(19)
(11)EP 1 849 751 A1

(12)EUROPEAN PATENT APPLICATION
published in accordance with Art. 158(3) EPC

(43)Date of publication:
31.10.2007 Bulletin 2007/44

(21)Application number: 06712163.2

(22)Date of filing:  23.01.2006
(51)International Patent Classification (IPC): 
C02F 11/04(2006.01)
C02F 11/00(2006.01)
B01D 9/02(2006.01)
C02F 11/14(2006.01)
(86)International application number:
PCT/JP2006/300947
(87)International publication number:
WO 2006/078012 (27.07.2006 Gazette  2006/30)
(84)Designated Contracting States:
DE NL

(30)Priority: 21.01.2005 JP 2005013551
21.01.2005 JP 2005013552

(71)Applicant: EBARA CORPORATION
Ohta-ku, Tokyo 144-8510 (JP)

(72)Inventors:
  • SHIMAMURA, Kazuaki
    a-ku, Tokyo, 1448510 (JP)
  • HAGINO, Takao
    a-ku, Tokyo, 1448510 (JP)
  • UEDA, Noriko
    a-ku, Tokyo, 1448510 (JP)
  • ISHIKAWA, Hideyuki
    a-ku, Tokyo, 1448510 (JP)
  • FUCHU, Yuichi
    a-ku, Tokyo, 1448510 (JP)

(74)Representative: Geyer, Ulrich F. 
WAGNER & GEYER, Patentanwälte, Gewürzmühlstrasse 5
80538 München
80538 München (DE)

  


(54)APPARATUS FOR TREATING WASTEWATER AND SLUDGE


(57) In a system for separating crystals from sludge, or from separated water generated in a sludge concentration process or a dewatering process, both phosphorus removal and phosphorus recovery can be satisfactorily achieved, and MAP having a high degree of purity can be recovered. Also, stable treatment can be performed such that the MAP recovery rate is high and blocking of a liquid cyclone do not occur. An aspect of the present invention is a crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludgeconcentration process or a dewatering process, comprising a liquid cyclone for separating the crystals from the sludge or separated water introduced into the liquid cyclone, and a return pipe A for returning an overflow from the liquid cyclone to a supplying portion of said sludge or said separated water.




Description

FIELD OF THE INVENTION



[0001] The present invention relates to an apparatus and method for separating and concentrating crystals from anaerobic or aerobic digestion sludge, separated water generated in a sludge concentration process or dewatering process, or various kinds of waste water. The present invention also relates to an apparatus and method for treating digested sludge generated when organic wastes or waste water is subjected to anaerobic digestion.

BACKGROUND ART



[0002] In a treatment facility for treating organic waste water containing phosphorus and nitrogen, such as sewage, waste water, and human waste, first the raw sludge (also referred to as preliminary sludge hereafter) is subjected to liquid/solid separation in a preliminary sedimentation tank, whereupon the separated supernatant is subjected to activated sludge treatment to remove organic matters. During the activated sludge treatment, the propagated activated sludge is discharged as excess sludge. Incidentally, when raw sludge or organic wastes such as excess sludge, human waste, or garbage is subjected to anaerobic digestion, the organic matter in the waste matter is degraded by the working of acidogenic bacteria and methanogenic bacteria, as a result of which the amount of sludge is reduced and gas containing methane, carbon dioxide, and the like is generated together with waste water having high nitrogen and phosphorus concentrations. Nowadays, a great deal of research is being conducted into the utilization of generated methane as a heat source, as well as the generation of MAP from supernatant liquor obtained through the dewatering of digested sludge and the effective use of this MAP in fertilizers, chemical raw materials, and so on (Japanese Unexamined Patent Application Publication No. 2003-117306).

[0003] Moreover, improvements are currently being made in the efficiency of anaerobic digestion tanks from the viewpoints of energy recovery and sludge volume reduction. For example, by subjecting raw sludge, excess sludge, or mixed sludge of raw sludge and excess sludge to physical/mechanical treatment, chemical liquefaction treatment, heating treatment, and so on such that the sludge is solubilized, improvements have been achieved in the methane recovery rate and sludge reduction rate during a subsequent anaerobic digestion process. The aforementioned physical/mechanical treatment includes ultrasonic treatment and crushing treatment using a mill. Chemical liquefaction treatment includes treatment using ozone, hydrogen peroxide, acid, and alkali. Heating treatment includes treatment using thermophilic bacteria. For example, Japanese Unexamined Patent Application Publication No. 2002-336898 describes a method of solubilizing sludge by treating the sludge in an ultrasonic treatment process.

[0004] As the efficiency of anaerobic digestion increases in the manner described above, waste water having ever higher nitrogen and phosphorus concentrations is generated. Original organic wastes contain elements such as nitrogen, phosphorus, and also magnesium and the like, and when the organic wastes are solubilized, these elements move to a solution. When waste water containing such high concentrations of nitrogen and phosphorus is returned to a water treatment system, the nitrogen and phosphorus loads on the water treatment system increase, causing deterioration in the quality of the treated water.

[0005] Hence, as a known technique, MAP is generated by subjecting the digested sludge or digested sludge liquor to aeration treatment, and a part of the sludge that settles in the sedimentation tank is returned to the aeration tank to serve as seed crystal, resulting in reduction in the phosphorus concentration of the return water , and the phosphorus can be recovered easily as MAP. In Japanese Examined Patent Application Publication No. H7-115979, digested sludge is decarbonated, whereupon a magnesium compound is added to precipitate MAP, thereby reducing the phosphorus concentration of the dewatered liquid. In both cases, the phosphorus concentration of the liquid is reduced by precipitating MAP, and as a result, phosphorus can be prevented from circulating endlessly between water treatment process and sludge treatment process.

[0006] Nowadays, in order to achieve effective utilization and efficient treatment of digested sludge, in some areas, all wastewater treatment plants and the like are connected by sewers (pipes), and generated digested sludge is transported through the sewers, gathered to a single treatment plant for collective treatment. Similarly, in order to treat the supernatant that is generated by dewatering digested sludge efficiently, in some areass, all wastewater treatment plants are connected by sewers, and the generated supernatant liquor is transported through the sewers to be treated collectively in a single treatment plant. The construction cost of the sewers is cheaper than that of treatment facilities, and since the advantage of scale effects to sludge treatment facilities (i.e. the unit cost thereof decreases as the scale increases), sewers are considered to be more economical in locations such as urban areas, where buildings are in close proximity.

[0007] By the way, when digested sludge or the supernatant liquor thereof is transported through pipes, so-called MAP precipitate is generated when the magnesium ions in the sludge chemically react with the phosphate ions and ammonium ions, leading to possible blockings of the pipe.

[0008] To solve this problem, a method of transporting the sludge through a pipe after removing and recovering the MAP by aerating the digested sludge in a reactor in advance to generate MAP particulates, and then subjecting the sludge containing the MAP particulates to centrifugal separation, is known. Further, a part or all of the MAP particulates is returned to the reactor following centrifugal separation to serve as kernels for generating new MAP particulates in the reactor. By performing such an operation, problems such as blockings of the sludge pipes caused by MAP particulates can be avoided.

DISCLOSURE OF THE INVENTION


PROBLEMS TO BE SOLVED BY THE INVENTION



[0009] As noted above, as the efficiency of anaerobic digestion increases, waste water having ever higher nitrogen and phosphorus concentrations is produced. Originally, organic wastes contain elements such as nitrogen, phosphorus, and also magnesium and the like, and when the organic wastes are solubilized, these elements migrate into the solution. Nitrogen, phosphorus, and magnesium are the constituent components of MAP, and at high concentrations in liquid, or when the pH rises, the nitrogen, phosphorus, and magnesium easily equal or exceed the solubility product of the MAP such that the MAP precipitates spontaneously in a digestion tank. When the MAP precipitates into a draft tube in the digestion tank, the flow of the digested sludge deteriorates, and scale trouble such as pipe blockings during pump extraction occurs frequently. Moreover, the MAP is disposed of together with the dewatered sludge rather than being recovered, and hence there is demand for an efficient MAP recovery method.

[0010] When MAP is precipitated by decarbonating the digested sludge or adding a magnesium compound thereto, the phosphorus concentration of the dewatered liquid decreases, and therefore the phosphorus load on the water treatment system is reduced so that the treated water can be maintained at a favorable quality. However, this method focuses on phosphorus removal rather than the recovery of phosphorus resources, and hence there is demand for a treatment method which satisfies aspects of both phosphorus removal and phosphorus recovery.

[0011] Moreover, when MAP is recovered through aeration and centrifugal separation, the recovered matter contains digested sludge and screen residues as well as the MAP, and hence it is not always possible to recover MAP having a high degree of purity. When recycling phosphorus, purity is required, and hence there is demand for a method of recovering MAP having a high degree of purity.

[0012] Furthermore, when MAP is recovered by subjecting the MAP to centrifugal separation using a liquid cyclone and the concentration of MAP or other inorganic solids introduced into the liquid cyclone is high, the liquid cyclone itself may become blocked. In certain cases, the MAP concentration in an overflow riser may also increase, leading to deterioration in the recovery rate. Hence, there is demand for a separating method enabling treatment to be performed with stability and a high MAP recovery rate.

[0013] Further, when digested sludge containing MAP is transported by pipe to a facility for treating sludge collectively, a large amount of MAP scale is generated in the pipe, leading to deterioration in the efficiency with which the sludge is transported. Following its initial generation, MAP scale continues to grow. If MAP scale is left on the inside of the pipe, the entire sewer eventually becomes covered in MAP scale, making sludge transportation difficult, and hence washing and complicated maintenance must be performed periodically.

[0014] Nowadays, due to the spread of sewerage, advancements in advanced treatment, and so on, the amount of sewage-treated sludge is increasing. In order to achieve detoxification and volume reduction of the sludge, sludge slagging combustion treatment is becoming more widely used. However, when sewage sludge is subjected to slagging combustion treatment at a high temperature between 1200 and 1400°C, a part of the phosphorus contained in the sludge is emitted into the slag without solidifying, and as a result, the phosphorus becomes stuck during an exhaust gas treatment process, leading to problems such as machinery corrosion, an increase in the phosphorus load of the return water produced by exhaust gas wet washing, and so on. Hence, there is demand for a technique for removing phosphorus from sludge in advance.

[0015] As for crystallization reactors, when attempts have been made in the past to reduce the size of the crystallization reactor, the concentration ability of the liquid cyclone has posed a problem since it becomes difficult to maintain the MAP in the crystallization reactor at a high concentration.

[0016] An object of the present invention is to solve the problems illustrated above by providing a treatment method and apparatus which satisfactorily achieve both phosphorus removal and phosphorus recovery at the same time, to enable the recovery of MAP having a high degree of purity, and stable treatment in which the MAP recovery rate is high and blockings of a liquid cyclone do not occur.

[0017] The present invention may be applied not only to the separation and recovery of MAP crystals from anaerobically digested sludge and the like, as described above, but also to the separation and recovery of various types of crystal from various types of waste water. For example, the present invention may be applied to the recovery of calcium phosphate (Ca3(PO4)2) crystals or hydroxyapatite (Ca10 (PO4)6 (OH)2 : HAP) crystals from waste water such as return water obtained from the secondary treated water of sewage or a sludge treatment system; the recovery of calcium fluoride (CaF2) crystals from the waste water of a semiconductor factory or the like; the recovery of calcium carbonate crystals from service water using ground water as a raw water, waste water, and refuse leachate; the recovery of calcium carbonate (CaCO3) crystals from hard water containing a large amount of carbonate ions; the recovery of manganese carbonate (MnCO3) crystals generated from Mn in the form of an impurity contained in running tap water; and so on.

[0018] This specification mainly describes an example in which MAP crystals are separated and recovered from anaerobically digested sludge and the like.

MEANS FOR SOLVING THE PROBLEMS



[0019] As means for achieving the object described above, an aspect of the present invention provides the crystal separation apparatus illustrated below.

[0020] 1. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a liquid cyclone for separating said crystals from said sludge or said separated water introduced into said liquid cyclone; and

a return pipe A for returning an overflow from said liquid cyclone to a supplying portion of said sludge or said separated water.



[0021] 2. The crystal separation apparatus as defined in the above-mentioned item 1, further comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water provided upstream of said liquid cyclone, and

a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclone to said crystallization reactor.



[0022] 3. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water;

a liquid cyclone for separating said crystals from said sludge or said separated water introduced into said liquid cyclone after being treated by said crystallization reactor; and

a return pipe C for returning an overflow from said liquid cyclone to said crystallization reactor.



[0023] 4. The crystal separation apparatus as defined in the above-mentioned item 3, further comprising a return pipe A for returning said overflow from said liquid cyclone to a supplying portion of said sludge or said separated water.

[0024] 5. The crystal separation apparatus as defined in the above-mentioned item 3 or 4, further comprising a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclone to said crystallization reactor.

[0025] 6. The crystal separation apparatus as defined in any one of the above-mentioned items 2 to 5, further comprising discharge pipe for discharging said crystals from the bottom of said crystallization reactor,
wherein, when a feed rate of said sludge or raw water to be supplied to said crystallization reactor is Q1, a feed rate of said chemical to be added to said crystallization reactor is Q2, a feed rate of said crystals separated or concentrated by said liquid cyclone to be returned to said crystallization reactor is Q3, and a feed rate of said crystals to be discharged by said discharge pipe is Q4, Q1+Q2+Q3<Q4.

[0026] 7. The crystal separation apparatus as defined in any one of the above-mentioned items 2 to 6, wherein a horizontal cross section of the bottom of said crystallization reactor is smaller than a horizontal cross section of the upper end of said crystallization reactor.

[0027] 8. The crystal separation apparatus as defined in any one of the above-mentioned items 1 to 7, wherein a recovery pipe for recovering said crystals separated or concentrated by said liquid cyclone is connected to the bottom of said liquid cyclone.

[0028] 9. The crystal separation apparatus as defined in any one of the above-mentioned items 2 to 8, wherein a washing pipe for washing said liquid cyclone is connected to said return pipe B or said recovery pipe.

[0029] 10. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water;

a plurality of liquid cyclones arranged in parallel for separating said crystals from said sludge or said separated water introduced into said liquid cyclones after being treated by said crystallization reactor; and

a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclones to said crystallization reactor.



[0030] 11. The crystal separation apparatus as defined in the above-mentioned item 10, further comprising:

a flow meter for measuring a flow rate of said sludge or said separated water installed in a pipe for introducing said sludge or said separated water into said crystallization reactor, and

means for determining a number of liquid cyclones to be operated from a measured value of said flow meter and a predetermined relationship between a flow rate range and a number of operational liquid cyclones.



[0031] 12. The crystal separation apparatus as defined in the above-mentioned item 10, further comprising:

a sludge concentration meter installed in said crystallization reactor, and

means for determining a number of liquid cyclones to be operated according to a detected value of said sludge concentration meter.



[0032] 13. The crystal separation apparatus as defined in the above-mentioned item 10, further comprising:

means for monitoring a phosphorus concentration and a pH (hydrogen ion concentration) value of said sludge or said separated water treated by said crystallization reactor and said liquid cyclones;

means for calculating a supersaturation ratio from said phosphorus concentration and said pH value measured by said monitoring means; and

means for determining a feed rate of magnesium to be added and a number of liquid cyclones to be operated according to said supersaturation ratio.


BREIF DESCRIPTION OF THE DRAWINGS



[0033] 

Fig. 1 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 2 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 3 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 4 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 5 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 6 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 7 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 8 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 9 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 10 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 11 is a graph showing the relationship between a MAP amount in a crystallization reactor and a phosphorus recovery rate;

Fig. 12 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 13 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 14 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 15 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 16 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 17 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 18 is a treatment flow diagram pertaining to an embodiment of the present invention;

Fig. 19 is a graph showing the relationship between a sludge circulation ratio in a liquid cyclone and a MAP concentration following circulation, determined in example 3;

Fig. 20 is a flow diagram of apparatuses used in comparative example 1;

Fig. 21 is a flow diagram of apparatuses used in comparative example 2;

Fig. 22 is a flow diagram of apparatuses used in example 4;

Fig. 23 is a flow diagram of apparatuses used in example 5;

Fig. 24 is a flow diagram of apparatuses used in comparative example 3;

Fig. 25 is a flow diagram of apparatuses used in comparative example 4;

Fig. 26 is a flow diagram of apparatuses used in example 6;

Fig. 27 is a flow diagram of apparatuses used in example 7;

Fig. 28 is a flow diagram of apparatuses used in example 8;

Fig. 29 is a flow diagram of apparatuses used in example 9;

Fig. 30 is a flow diagram of apparatuses used in example 10;

Fig. 31 is a flow diagram of apparatuses used in example 11;

Fig. 32 is a flow diagram of apparatuses used in comparative example 5;

Fig. 33 is a flow diagram of apparatuses used in example 14;

Fig. 34 is a flow diagram of apparatuses used in comparative example 6;

Fig. 35 is a flow diagram of apparatuses used in comparative example 7; and

Fig. 36 is a flow diagram of a comparative flow in example 16.


DESCRIPTION OF THE PREFERRED EMBODIMENTS



[0034] Embodiments of the present invention will now be described in detail with reference to the drawings. However, it is to be understood that the present invention is not limited to these embodiments. As noted above, the present invention may be applied to the separation and recovery of various types of crystal from various types of waste water, but in the following description, an example is mainly used in which MAP crystals are separated and recovered from anaerobically digested sludge or the like.

[0035] In the drawings, constitutional elements having identical functions may be described using identical reference numerals. Furthermore, where appropriate, description relating to constitutional elements having identical functions has been omitted. The technical matter relating to each constitutional element described in relation to the flow of each drawing may be applied to identical constitutional elements in the flows of the other drawings.

[0036] Examples of the MAP-containing sludge which is treated in the present invention include human waste, septic tank sludge, sewage sludge, agricultural sludge, livestock waste, garbage, and waste foodstaffs. The organic wastes are typically in liquid slurry form, or has a high moisture content when in solid form. To enable smooth treatment, it is preferable to introduce waste water or the like into non-slurry form waste matter such that the waste matter is treated in slurry form. The present invention may also be applied to separated water obtained by concentrating or dewatering the sludge. In the following descriptions, an example will be used in which sludge obtained by subjecting excess sewage sludge to anaerobic digestion is employed as the MAP-containing sludge.

[0037] Fig. 1 shows a treatment flow in which anaerobically digested sludge is used as raw sludge 1, MAP 3 in the sludge 1 is concentrated using a liquid cyclone 2 and discharged via a particulate discharge pipe 4, and the sludge from which the MAP 3 has been removed is caused to overflow through a sludge discharge pipe (also referred to as an overflow riser) 5.

[0038] The lower portion structure of the liquid cyclone 2. shown in Fig. 1 takes an inverted conical form with a liquid cyclone inflow pipe 6 (also referred to as an introduction pipe) provided on the side portion, the particulate discharge pipe 4 provided on the lower portion, and the overflow riser 5 provided on the upper portion. In the liquid cyclone 2, the digested sludge 1 containing the MAP 3 is transmitted through the liquid cyclone inflow pipe 6 by the pressure of a pump, and is then caused to swirl down the inverted cone-shaped wall surface in the interior of the liquid cyclone 2. Particulates containing the MAP 3, which have a greater specific gravity than the digested sludge, are collected and concentrated on a lower wall surface side by means of centrifugal force. The concentrated particulates are removed either continuously or intermittently through the particulate discharge pipe 4. Further, sludge (treated sludge) 8 from which the particulates containing the MAP 3 have been removed is extracted through the overflow riser 5 and discharged.

[0039] The pipe diameter of the particulate discharge pipe 4 and the pipe diameter of the overflow riser (sludge discharge pipe) 5 may be altered, and by altering both, the flow rate and particulate diameter distribution can be varied.

[0040] In the present invention, the sludge that flows out of the sludge discharge pipe of the liquid cyclone 2 is returned to the liquid cyclone inflow pipe 6 through a treated sludge return pipe 7 (return pipe A). The return amount may be set to a desired proportion of the raw sludge 1 introduction amount, but the return amount is preferably determined such that the MAP concentration of the sludge introduced into the liquid cyclone remains at or below a predetermined concentration, and the set value thereof is preferably varied according to the size of the liquid cyclone 2, the diameter of the sludge discharge pipe, and the diameter of the particulate discharge pipe. The particulate discharge speed in relation to the sectional area of the particulate discharge pipe (kg/mm2/hr) is a very important factor in determining whether or not the liquid cyclone will become blocked since the liquid cyclone becomes blocked when the discharge speed reaches or exceeds a certain speed. For example, a two-inch cyclone becomes blocked at approximately 10 kg/mm2/hr or more, although this differs according to factors such as the introduction pressure and the shape of the cyclone, and therefore the concentration of the MAP-containing particulates in the cyclone inflow pipe is preferably reduced such that the particulate discharge speed is no greater than 5 kg/mm2/hr, and more preferably no greater than 2kg/mm2/hr.

[0041] As will be described below in Example 3, the treated sludge return amount is preferably no less than 0.1 times the amount of introduced raw sludge 1, and although there is no specific upper limit, the return amount is preferably set to no more than 50 times the amount of introduced raw sludge 1 in order to achieve an economical circulation ratio.

[0042] The sludge that flows out of the sludge discharge pipe 5 may be returned to the cyclone inflow pipe 6 after being stored temporarily in a storage tank (not shown), or may be returned without passing through the storage tank. The remaining sludge is recovered as the treated sludge 8 and applied appropriately to a dewatering process or the like.

[0043] By returning the overflow from the liquid cyclone to the cyclone inflow pipe in this manner, the concentration of the MAP-containing particulates in the cyclone inflow pipe decreases, and as a result, blockings of the cyclone can be prevented. Moreover, by reducing the concentration of the MAP-containing particulates in the cyclone inflow pipe, the MAP concentration of the sludge that is discharged through the overflow riser also decreases, and thus the MAP recovery rate improves.

[0044] Fig. 2 shows the treatment flow of another embodiment of the present invention, comprisinga crystallization reactor 9 and the liquid cyclone 2.

[0045] In the crystallization reactor 9, MAP is precipitated by adding a magnesium compound 10 serving as a crystallization chemical to the digested sludge and digested sludge liquor 1 extracted from the anaerobic digestion tank, and by causing the magnesium compound 10 to react with PO4-P dissolved in the liquid. If aeration, decompression, or a similar process is also performed at this time, the sludge is decarbonated, leading to an increase in the pH, and hence MAP can be precipitated more efficiently. Needless to say, a chemical such as sodium hydroxide, magnesium hydroxide, or magnesium oxide may be added to raise the pH. Magnesium compounds 10, such as magnesium chloride, magnesium hydroxide, magnesium oxide, sea water, and the like may be added. As regards the amount of added magnesium, a molar ratio between 0.1 and 10, preferably between 0.5 and 3.0, and more preferably between 0.8 and 1.2 in relation to the aqueous o-phosphoric acid concentration of the digested sludge is suitable. The pH in the reaction may be between 7.0 and 11.0, and preferably between 7.5 and 8.5.

[0046] Seed crystals are preferably added to the crystallization reactor 9 to ensure that MAP is precipitated efficiently. The MAP precipitated by the crystallization reactor 9 or MAP precipitated in a separate reactor may be used as the seed crystals. Alternatively, MAP that precipitates spontaneously in the digestion tank may be used.

[0047] Particulates or the like containing the MAP 3, which are recovered by the liquid cyclone 2, may also be used. In this case, the particulates that are separated and recovered by the liquid cyclone 2 may be returned to the crystallization reactor 9 through a return pipe 11 (return pipe B). When separated water from the separation process, effluent water, or the like contains MAP, each of them may also be used.

[0048] Alternatively, a powder or granular substance such as rock phosphate, dolomite, bone charcoal, activated carbon, silica sand, or calcium silicate may be used. The particulate diameter of the seed crystals is arbitrary, but is preferably set between 0.05 and 3.0 mm, and more preferably between 0.1 and 0.5 mm. By precipitating new MAP on the surface of the seed crystals, subsequent separation of the digested sludge and MAP 3 in the liquid cyclone 2 can be performed well. The seed crystal charging amount is extremely important for precipitating MAP on the surface of the seed crystals. The charging amount is determined in consideration of the introduced phosphorus amount and the seed crystal particulate diameter such that the phosphorus introduction amount in relation to the seed crystal surface area (the phosphorus surface area load hereafter) is no more than 100 g-P/m2/d, preferably no more than 30 g-P/m2/d, and more preferably no more than 10 g-P/m2/d. In other words, when a high concentration of MAP is maintained in the reactor 9 in relation to a constant particulate diameter, the volume of the reactor can be reduced, enabling a reduction in initial costs.

[0049] There are no particular limitations on the form of the reactor 9 used in the crystallization process, and a complete mixing type reactor comprising a mechanical stirring apparatus, a jet stream type stirring reactor using a pump, a fluidized bed reactor charged with seed crystals at a high density, an internal circulation type reactor comprising a draft tube, an external circulation type reactor, or another reactor may be used.

[0050] The MAP precipitated in the crystallization process is discharged from the bottom of the crystallization reactor 9, introduced into the aforementioned liquid cyclone 2 through the liquid cyclone inflow pipe 6, and subjected to separation and recovery in the liquid cyclone 2. In this case also, the sludge that flows out from the overflow riser 5 of the liquid cyclone 2 is returned to the liquid cyclone inflow pipe 6 through the return pipe 7 (return pipe A). By diluting the MAP concentration, which was maintained at a high level in the crystallization process, with the treated sludge 8, blockinge of the cyclone 2 can be prevented, and a stable treatment performance with a high MAP recovery rate can be obtained. Note that in Fig. 2, 10 denotes a Mg compound. An Mg compound for generating MAP is added to the crystallization reactor, and therefore MAP generation occurs in the crystallization reactor 9. Sludge may be introduced into the liquid cyclone 2 either continuously or intermittently.

[0051] Fig. 3 is a flow diagram showing an example of another embodiment of the present invention, in which a screen residue removal apparatus 11 is provided before the sludge 1 is introduced into the liquid cyclone 2. In the conventional art, no screen residue separation process is provided, and therefore problems such as blockings caused by screen residues and the like occur in the downstream liquid cyclone 2. As a result, long-term stable treatment is difficult. In the present invention, screen residues are removed, enabling a dramatic improvement in the stability of MAP particulate separation using the liquid cyclone. Moreover, by separating screen residues in advance, MAP with a high degree of purity can be obtained. The screen residue removal apparatus 11 may also be attached midway along the liquid cyclone inflow pipe 6.

[0052] The removed screen residues may be discharged outside of the system or introduced into a dewatering process for dewatering the treated sludge 8. In the latter case, the dewatering performance is preferably enhanced.

[0053] The crystallization process and the screen residue separation process may performed in any order. The crystallization process may precede the screen residue separation process, or the screen residue separation process may precede the crystallization process.

[0054] A method for separating the screen residues may employ a centrifugal settler, a sedimentation tank employing gravity separation, and so on, and a particulate separation method using differences in particulate diameter may employ a vibrating screen, a drum screen, a filter layer, a classification layer type separation layer, and so on.

[0055] A further embodiment of the present invention is illustrated in Figs. 4 through 6.

[0056] Fig. 4 shows a treatment flow, comprising the crystallization reactor 9 comprising a stirring apparatus, the liquid cyclone 2, and a circulating water tank 55.

[0057] To ensure that the particulates and liquid are mixed together well in the crystallization reactor 9, stirring is preferably performed to maintain a favorable particulate current. The stirring method may employ a mechanical stirring apparatus equipped with a motor, or stirring may be performed with the use of an air supply.

[0058] The crystallization reactor 9 is connected to a raw water 1 supply pipe, a chemical 10 supply pipe, a return pipe 51 whose lower portion communicates with the reactor, an discharge pipe 52 for discharging sludge and particulates from the interior of the reactor, and a discharge pipe 53 for discharging particulates from the liquid cyclone, while a circulating water effluent pipe 54 is connected to the return pipe 51. The sludge of the raw water contains between 100 and 600 mg/L of phosphate ions, and between 50 and 3000 mg/L of ammonia nitrogen. A magnesium source for generating MAP is supplied as the chemical 10. Magnesium chloride, magnesium hydroxide, magnesium oxide, and so on may be employed as the magnesium source.

[0059] The crystallization reactor 9 is preferably structured such that the horizontal cross section of the bottom is smaller than the horizontal cross section of the upper end. Furthermore, the planar cross section from the top end to a predetermined lower position preferably has a constant shape and a constant sectional area, and from the predetermined position downward, the cross section preferably decreases steadily. As shown in Fig. 4, for example, the base portion preferably takes an inverted conical form. The angle of the inverted cone is preferably no less than 45° in relation to the horizontal, and more preferably no less than 60°. By setting the angle in this manner, the MAP particulates which settle inside the crystallization reactor 9 become concentrated at a single point in the base portion of the reactor, which is preferable. Furthermore, the particulate discharge pipe 52 is preferably connected to the vicinity of the point at which the settled particulates concentrate. As a result; blockings caused by sediment can be prevented.

[0060] The particulate discharge pipe 53 of the liquid cyclone 2 is used to discharge the MAP particulates that are concentrated by the cyclone 2 from the bottom of the cyclone 2 and to return these MAP particulates to the crystallization reactor 9. By returning the MAP particulates concentrated by the liquid cyclone 2 to the crystallization reactor 9, the MAP particulate concentration in the reactor can be raised, and as a result, the MAP particulate surface area can be maintained at a high level. The crystallization reaction is constituted by a particulate nucleation phenomenon and a growth phenomenon, but as the particulate surface area increases, the growth phenomenon takes precedence over the nucleation phenomenon, thereby facilitating solid/liquid separation. A recovery pipe 56 for recovering the concentrated MAP particulates may also be connected to the bottom of the liquid cyclone 2 or the particulate discharge pipe 53.

[0061] An important characteristic feature of the embodiment shown in Fig. 4 is the return pipe 51 which is disposed in the crystallization reactor 9. The return pipe 51 is connected to the overflow riser 5 of the liquid cyclone 2 and the circulating water inflow pipe 54, and also communicates with the crystallization reactor 9 at the bottom. Following the removal of MAP particulates in the liquid cyclone 2, the sludge passes through the overflow riser 5 and is supplied in its entirety to the return pipe 51. The return pipe 51 maintains an identical water level to the water surface of the reactor 9 such that a part of the returned sludge is returned to the reactor 9, while the remainder is supplied to the circulating water tank 55 through the circulating water inflow pipe 54.

[0062] The inflow rate into the liquid cyclone is determined principally according to the size of the employed cyclone. With a two-inch cyclone, an inflow rate of approximately 4 m3/hr is available, and with a four-inch cyclone, an inflow rate of approximately 20 m3/hr is available. When the actual inflow rate is larger or smaller than a predetermined flow rate, the treatment performance varies. In a conventional crystallization reactor, return pipe 51 is not provided, and it is therefore difficult to match the sum total of the raw water 1 supply rate, the under flow rate of the liquid cyclone (the flow rate of the particulate discharge pipe 53 at the bottom of the reactor), and the chemical 10 supply rate with the extraction rate from the discharge pipe 52. This leads to increases or decreases in the water surface of the reactor 9. Hence, in the conventional art, a level meter or the like must be provided to control the water level. In the embodiment shown in Fig. 4, this problem can be solved by providing the return pipe 51 in the crystallization reactor 9. More specifically, when the return pipe 51 communicates with the reactor 9 such that the sludge discharged from the overflow riser 5 of the liquid cyclone 2 is returned to the reactor 9 via the return pipe 51, and when an amount of sludge corresponding to the raw water supply amount and chemical supply amount is caused to overflow by the return pipe 51 constantly, the water level of the reactor 9 can be maintained at a constant level. As a result, level meter may be omitted, and continuous introduction into the cyclone can be performed. Also, the water level is stabilized enough to enable stable treatment.

[0063] The sludge which overflows from the return pipe 51 is led to the circulating water tank 55 via the circulating water inflow pipe 54. A part of the sludge overflows and is discharged as the treated sludge 8, while the remainder is introduced into the liquid cyclone 2 through the liquid cyclone inflow pipe 6.

[0064] The MAP particulates in the reactor 9 are discharged via the discharge pipe 52 at a predetermined flow rate, and introduced into the liquid cyclone 2 via the liquid cyclone inflow pipe 6. An important characteristic feature is the discharge pipe 52 which isconnected to the liquid cyclone inflow pipe 6 such that the MAP particulates are introduced into the cyclone after the particulate concentration in the discharge pipe 52 is diluted by circulating water (sludge) from the circulating water tank 55. The concentration of the MAP particulates introduced into the liquid cyclone is an important operational factor affecting the treatment performance of the liquid cyclone, and therefore to prevent reductions in the particulate concentration of the treated water and blockings of the cyclone under (cyclone base portion), the concentration is preferably as low as possible.

[0065] When the raw water supply feed rate supplied to the crystallization reactor 9 is defined as Q1, the chemical supply feed rate supplied to the crystallization reactor 9 is defined as Q2, the return feed rate of MAP crystals separated in the liquid cyclone 2 and then returned to the crystallization reactor 9 is defined as Q3, and the extraction feed rate of MAP crystal particulates discharged from the discharge pipe 52 of the crystallization reactor 9 is defined as Q4, a relationship of


is preferably maintained. By maintaining this relationship, the flow direction of a return water feed rate Q5 passing through the return pipe 51 can be maintained in a direction heading toward the crystallization reactor 9, and the MAP particulates in the crystallization reactor 9 can be prevented from flowing out through the circulating water effluent pipe.

[0066] When the pH, water temperature, or sludge concentration in the reactor varies, a pH meter 57, water temperature meter, sludge concentration meter, or the like is preferably provided, and in accordance with the measured value, a pH adjusting agent is preferably added, or a heating/cooling operation or sludge concentration adjustment operation is preferably performed.

[0067] The lower portion structure of the liquid cyclone 2 preferably takes an inverted conical form. The liquid cyclone inflow pipe 6, particulate discharge pipe 53, and overflow riser (sludge discharge pipe) 5 are connected to the liquid cyclone 2. In the liquid cyclone 2, sludge containing MAP particulates is introduced through the liquid cyclone inflow pipe 6 by the pressure of a pump, and is then caused to swirl down the inverted cone-shaped wall surface of the liquid cyclone 2. The MAP-containing particulates, which have a greater specific gravity than the sludge, are collected and concentrated on a lower wall surface side by means of centrifugal force. The concentrated particulates are returned to the reactor either continuously or intermittently via the particulate discharge pipe 53. Alternatively, the particulates may be recovered via the recovery pipe 56 appropriately.

[0068] The concentration of the particulates in the liquid cyclone inflow pipe 6 is an important operational factor affecting the treatment performance of the liquid cyclone 2, and to prevent reductions in the particulate concentration of the treated water and blockings of the cyclone under, the concentration is preferably as low as possible. The degree to which the particulate concentration should be reduced varies according to the concentration performance of the cyclone, but a preferable concentration is approximately several tens of grams per liter.

[0069] As described above, sludge from which MAP particulates have been removed flows out from the overflow riser 5. The overflow riser 5 is connected to the return pipe 51 of the crystallization reactor 9, and hence all of the sludge from which the MAP particulates have been removed is supplied to the return pipe 51.

[0070] In the liquid cyclone 2, the pipe diameter of the particulate discharge pipe and the pipe diameter of the sludge discharge pipe may be altered, and by altering both, the flow rate and particulate diameter distribution can be varied.

[0071] The circulating water inflow pipe 54, which is connected to the return pipe 51 of the crystallization reactor 9, the liquid cyclone inflow pipe 6, and the treated water (sludge) 8 discharge pipe are connected to the circulating water tank 55. A part 8 of the sludge that flows into the circulating water tank 55 through the circulating water inflow pipe 54 overflows into the treated water discharge pipe. The circulating water tank 55 stores circulating water (having identical properties to the treated water) temporarily, and its size may be determined arbitrarily. Needless to say, a stirring apparatus may be provided to ensure that the circulating water is mixed evenly.

[0072] A screen residue removal apparatus may be provided in the discharge pipe 52, which is connected to the sludge 1 supply pipe and/or the bottom of the crystallization reactor 9. By removing screen residue, a dramatic improvement in the stability of MAP particulate separation using the liquid cyclone 2 can be achieved. Moreover, by separating screen residues in advance, MAP with a high degree of purity can be obtained.

[0073] In the example shown in Fig. 5, the circulating water tank 55 is disposed directly above the return pipe 51. In so doing, the circulating water inflow pipe 54 of the embodiment in Fig. 4 can be omitted.

[0074] As shown in Fig. 6, the crystallization reactor 9 may be provided with a bottom having a columnar or other shape below the inverted conical part, and the discharge pipe 52 may be connected to this columnar part.

[0075] As shown in Figs. 4 to 6, the particulate recovery pipe 56 for recovering the MAP particulates concentrated by the liquid cyclone 2 may be connected to the bottom of the liquid cyclone 2 or the particulate discharge pipe 53. Typically, the MAP particulate concentration in the crystallization reactor 9 increases as the crystallization reaction progresses, and hence by discharging the MAP particulates from the liquid cyclone 2 appropriately, the MAP particulate concentration in the crystallization reactor 9 can be maintained at a constant concentration. The MAP particulates concentrated by the liquid cyclone 2 are returned to the crystallization reactor 9 through the particulate discharge pipe 53, and hence by connecting the recovery pipe 56 to the particulate discharge pipe 53, a part of the concentrated MAP particulates can be discharged to the outside through the recovery pipe 56. The concentrated MAP particulates may be discharged by means of valve switching, for example. The valve may be switched in accordance with a fixed timer setting, or the particulate concentration in the crystallization reactor 9 may be detected so that the valve is switched according to the detected value.

[0076] The recovered MAP particulates may be subjected to a process such as washing, dewatering, or drying in preparation for reuse.

[0077] Further, a washing pipe (not shown) for supplying washing water to clean the liquid cyclone may be connected to the particulate discharge pipe 53 or the recovery pipe 56. To ensure that the under (base portion) of the liquid cyclone 2 does not become blocked, measures such as removing large particulates in advance and reducing the concentration of the particulates that are introduced into the liquid cyclone 2 are usually taken. Even so, in certain cases blockings occur. In such cases, washing water may be supplied to flow in an upward flow from the cyclone under (base portion) so as to push the particulates out to the cyclone main body side. When supplying washing water, the particulate discharge pipe and recovery pipe may be closed using a valve or the like.

[0078] A further embodiment of the present invention provides a treatment system in which a plurality of liquid cyclones are connected in parallel so that the crystallization reactor can be reduced in size, blockings of the liquid cyclone can be eliminated, and stable treatment maintaining a high MAP particulate concentration in the crystallization reactor can be performed. An example of this embodiment is shown in Figs. 7 to 10.

[0079] Fig. 7 shows a treatment flow in which the crystallization reactor 9 is used to crystallize phosphorus dissolved in the raw sludge 1, and the liquid cyclone 2 is used to concentrate the MAP contained in the sludge and to discharge the concentrated MAP through the particulate discharge pipe 53 such that the sludge 8 from which MAP has been removed overflows from the sludge discharge pipe (overflow riser).

[0080] Contaminants such as screen residues are preferably removed from the raw sludge 1 in advance by using a screen residue removal apparatus (also referred to as a contaminant removal apparatus). A centrifugal settler, a sedimentation tank employing gravity separation, and so on may be employed as the screen residue removal apparatus, while a vibrating screen, a bar screen, a drum screen, a filter layer, a classification layer-type separation tank, and so on, or an apparatus combining the principles thereof, may be employed as a particulate separation method using differences in particulate diameter. By disposing the screen residue removal apparatus before the crystallization reactor 9 and/or the liquid cyclone 2, contaminants can be prevented from becoming caught in the stirring apparatus inside the crystallization reactor 9, and hence blockings of the liquid cyclone 2 can be prevented. As a result, treatment can be stabilized, and the frequency with which washing and maintenance must be performed can be reduced. Moreover, by separating screen residues in advance, MAP having a high degree of purity can be obtained. Note that the screen residue removal apparatus may be disposed in the liquid cyclone inflow pipe 6, which is connected to the bottom of the crystallization reactor 9.

[0081] The crystallization reactor 9 is connected to the raw sludge 1 supply pipe, the magnesium 10 supply pipe, the particulate discharge pipe 53 of the liquid cyclone 2, and the sludge discharge pipe (overflow riser) 5. In certain cases, a pH meter and pH adjusting agent supply pipe are also provided in the crystallization reactor 9. There are no particular limitations on the form of the reactor, and a complete mixing type reactor comprising a mechanical stirring apparatus, a jet stream type stirring reactor using a pump, a fluidized bed reactor charged with seed crystals at a high density, an internal circulation type reactor comprising a draft tube, an external circulation type reactor, or another reactor may be used.

[0082] When sludge is a subject to be treated, a complete mixing type reactor comprising a mechanical stirring apparatus which is capable of applying a strong shearing force is preferably employed.

[0083] In the crystallization reactor 9, MAP is precipitated by adding the magnesium compound 10 to the sludge or the separated water 1 that is generated as a result of sludge concentration or dewatering treatment. If aeration, decompression, or a similar process is also performed at this time, the sludge is decarbonated, leading to an increase in the pH, and hence MAP can be precipitated more efficiently. Needless to say, a chemical such as sodium hydroxide, magnesium hydroxide, or magnesium oxide may be added to raise the pH. Magnesium compounds, such as magnesium chloride, magnesium hydroxide, magnesium oxide, sea water, and the like, may be added. As regards the feed rate of added magnesium, a molar ratio between 0.1 and 10, preferably between 0.5 and 3.0, and more preferably between 0.8 and 1.2 in relation to the aqueous o-phosphoric acid concentration of the digested sludge is suitable. The pH in the reaction should be between 7.0 and 11.0, and preferably between 7.5 and 8.5.

[0084] Seed crystals are preferably added to the crystallization reactor 9 to ensure that MAP is generated efficiently. The MAP that precipitates spontaneously in the digestion tank, the MAP that precipitates in the crystallization reactor 9, the MAP that is concentrated by using the liquid cyclone 2, MAP precipitated in a separate crystallization reactor, and so on may be used as the seed crystals.

[0085] Alternatively, a powder or granular substance such as rock phosphate, dolomite, bone charcoal, activated carbon, silica sand, or calcium silicate may be used. The particulate diameter of the seed crystals is arbitrary, but is preferably set between 0.05 and 3.0 mm, and more preferably between 0.1 and 0.5 mm. By precipitating new MAP on the surface of the seed crystals, separation of the digested sludge and MAP in a subsequent separation process can be performed well. The seed crystal charging amount is extremely important for precipitating MAP on the surface of the seed crystals.

[0086] Fig. 11 shows the relationship between the MAP amount in the crystallization reactor and the phosphorus recovery rate. As is evident from Fig. 11, the recovery rate rises as the MAP charging amount increases, and therefore by setting the MAP amount charged into the reactor to at least 10 g/L, at least 30% of the phosphorus can be recovered.

[0087] Further, the phosphorus introduction amount in relation to the seed crystal surface area (referred to as the phosphorus surface area load, hereafter) should be set to no more than 100 g-P/m2/d, preferably no more than 30 g-P/m2/d, and more preferably no more than 10 g-P/m2/d.

[0088] The MAP concentration in the crystallization reactor is determined according to the raw sludge supply amount and the concentration of the MAP contained in the raw sludge, the amount and concentration of the MAP that is concentrated by the liquid cyclone and returned to the crystallization reactor, and the crystallization amount of the reactor. As noted above, it is important to increase the crystal surface area by raising the MAP concentration in the reactor, but since the MAP concentration of the raw sludge is approximately 1/10 to 1/500 that of the MAP which is concentrated by the liquid cyclone, the MAP concentrated by the liquid cyclone is diluted by the raw sludge. As a result, it becomes more and more difficult to maintain the MAP in the reactor at a high concentration as the raw sludge amount increases.

[0089] Hence, in the embodiment shown in Figs. 7 to 10, a plurality of the liquid cyclones 2 are disposed in parallel such that each liquid cyclone is capable of independent control. Further, the MAP that is concentrated by each liquid cyclone 2 is returned partially or entirely to the crystallization reactor 9 by the particulate discharge pipe 53. By employing such an embodiment, the MAP concentration in the crystallization reactor 9 can be maintained at a desired concentration, and since a larger amount of the MAP concentrated by the liquid cyclones 2 is returned, the MAP concentration in the crystallization reactor 9 can be maintained at a high concentration. Consequently, this greatly contributes to downsizing of the crystallization reactor 9.

[0090] The number of liquid cyclones 2 may be set at a desired number of two or more. The number of liquid cyclones 2 may be determined in consideration of the concentration flow rate of the liquid cyclones, the concentration of the concentrated MAP, and the desired MAP concentration in the crystallization reactor.

[0091] Further, in the embodiment shown in Figs. 7 to 10, the MAP concentration in the reactor can be adjusted by connecting the recovery pipe 56 to the bottom of the liquid cyclones 2 or the particulate discharge pipe 53 and discharging a part of the MAP concentrated by the liquid cyclones, as shown above in Fig. 4 and so on. The concentrated MAP particulates may be discharged intermittently or continuously from a specific cyclone, each cyclone in sequence, or all of the cyclones simultaneously. The discharged MAP may be put to effective use as a fertilizer, an inorganic chemical, a chemical raw material, and so on.

[0092] Note that a part of the sludge 8 that flow out from the overflow riser 5 of the liquid cyclones following recovery of the particulates may be returned to the liquid cyclone inflow pipe 6. In this case, the sludge 8 preferably passes through a relay tank. When a plurality of liquid cyclones are disposed in parallel, the number of operational liquid cyclones may be controlled in accordance with the raw water flow rate, for example as shown in Fig. 8. More specifically, a flow meter 71 is disposed on the raw sludge 1 supply pipe to monitor the inflow rate of raw sludge into the crystallization reactor 9. By determining a number of operational pumps disposed at the inflow portion of each liquid cyclone 2 from the relationship between a preset flow rate range and the number of operational liquid cyclones 2, the number of operational liquid cyclones 2 can be determined whereby the interior of the crystallization reactor 9 can be maintained at a desired MAP concentration even when the raw sludge inflow rate varies.

[0093] The number of operational liquid cyclones 2 can be also controlled in accordance with the MAP concentration in the crystallization reactor, as shown in Fig. 9. The MAP concentration in the crystallization reactor 9 can be measured using a concentration meter 73 employing a transmitted light/scattered light method, a laser light diffusion method, an ultrasonic method, a microwave method, a near infrared method, or another method. The MAP concentration may be measured together with the organic matter concentration, and since there is little variation in the organic matter concentration in the crystallization reactor 9, the MAP concentration may be calculated by creating a calibration curve.

[0094] Further, as shown in Fig. 10, by monitoring the phosphorus concentration and pH (hydrogen ion concentration) of the sludge or separated water treated in the crystallization reactor and liquid cyclones, that is, the sludge or separated water 8 that flows out from the overflow riser 5 of the liquid cyclones 2, using a phosphorus concentration meter 74 and a pH meter 75, the supersaturation ratio can be calculated on the basis of the resultant measurement data, and in accordance with the supersaturation ratio, the magnesium addition amount and the number of operational liquid cyclones can be controlled.

[0095] The pH and phosphorus concentration can be measured using an arbitrary analytical instrument, and monitoring may be performed continuously or at fixed time intervals. It is preferable that the total phosphorus, including the phosphorus dissolved in the sludge and particulates as well as the soluble phosphorus, be measured.

[0096] The supersaturation ratio is calculated by a calculation apparatus using the pH and phosphorus concentration obtained as a result of the monitoring. A typical example of the calculation apparatus includes a personal computer, which may comprise an input apparatus, a display apparatus and the like.

[0097] The supersaturation ratio will now be described. The supersaturation ratio is calculated as follows.



[0098] Hereinafter, SP denotes the solubility product of MAP, which is 10-12.6 (General Water Quality Chemistry; Kyoritsu Shuppan Ltd.). [Mg2+] and [NH3+] denote the molarities of respective ions, which vary according to the pH, and hence the number of unknown quantities for calculating the supersaturation ratio is four. The supersaturation may be expressed in other ways such as


or


In all cases, deviation in the solubility product is used as an index. Here, calculation is performed using the supersaturation ratio of Equation (1) as an index.

[0099] When the supersaturation ratio is 1 in Equation (1), this indicates that the sludge or liquid is in a state of equilibrium, and hence even if local crystallization and dissolution are occurring repetitively, as a whole crystallization is not underway. When the supersaturation ratio is greater than 1, this indicates a state of supersaturation, i.e. a region in which the concentration which exceeds the ionic product is crystallized such that MAP scale is generated. MAP scale is generated until a state of equilibrium is achieved, and the amount of MAP scale increases as the supersaturation ratio increases. When the supersaturation ratio is no more than 1, this indicates a state of unsaturation, i.e. a region in which MAP scale is not generated.

[0100] The ammonium ion concentration in the anaerobically digested sludge of the sewage sludge also varies according to regionality and treatment method, but is set at a fixed value between approximately 500 and 3000 mg/L.

[0101] The magnesium concentration and phosphorus concentration are preferably measured in a similar manner, and since magnesium is added as a chemical such that Mg/P=1.0, the concentration of the remaining Mg can be estimated between 10 and 100 mg/L.

[0102] MAP scale is less likely to occur as the supersaturation ratio, calculated in the manner described above, decreases, and therefore a supersaturation ratio of no greater than 30, preferably no greater than 10, and more preferably no greater than 5 is desirable.

[0103] Based on the supersaturation ratio calculated in this manner, the number of operational liquid cyclones can be controlled. As noted above, when the MAP concentration in the crystallization reactor decreases, the MAP recovery rate falls, and hence the supersaturation ratio of the treated sludge 8 increases. In this case, when the number of operational liquid cyclones is increased such that the MAP concentration in the crystallization reactor rises, the phosphorus concentration of the treated sludge decreases, leading to a reduction in the supersaturation ratio, and hence scale generation can be suppressed to a minimum.

[0104] The feed rate of magnesium to be added to the crystallization reactor can also be controlled by calculating the supersaturation ratio. More specifically, in a case where the supersaturation ratio is calculated by measuring the soluble phosphorus concentration, the phosphorus concentration is high when the supersaturation ratio is high, and hence the phosphorus concentration can be reduced by increasing the magnesium addition amount.

[0105] Although not shown in Figs. 7 to 10, the treated sludge from which MAP particulates have been removed, which flows out from the overflow riser 5 of the liquid cyclones 2, may be returned to the inflow pipe 6 of the liquid cyclones 2, as described above in the flow of Figs. 2 to 6. Also, the particulate slurry concentrated by the liquid cyclones 2 may be extracted and recovered appropriately.

[0106] A plurality of liquid cyclones and controlling operations thereof may be provided likewise in a flow having the constitution shown in Figs. 2 to 6, or flows having the constitutions shown in Figs. 12 to 17 and Fig. 18 to be described below, for example.

[0107] According to a still further aspect of the present invention, there is provided a treatment process for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising steps for: decarbonating the digested sludge or crystallizing MAP from the digested sludge; removing screen residues from the digested sludge; and separating or concentrating crystals containing MAP from the digested sludge after the digested sludge is treated by the steps for decarbonating or crystallizing and removing the screen sludge. Also, the present invention includes the following aspects.

[0108] 14. A digested sludge treatment apparatus for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising:

an apparatus for decarbonating said digested sludge;

a removal apparatus for removing screen residues from said digested sludge; and

an apparatus for separating or concentrating crystals containing magnesium ammonium phosphate from said digested sludge after said digested sludge is treated by said decarbonation apparatus and said removal apparatus.



[0109] 15. A digested sludge treatment apparatus for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising:

a crystallization reactor for precipitating magnesium ammonium phosphate from said digested sludge;

a removal apparatus for removing screen residues from said digested sludge; and

an apparatus for separating or concentrating crystals containing magnesium ammonium phosphate from said digested sludge after said digested sludge is treated by said crystallization reactor and said screen residue removal apparatus.



[0110] 16. The digested sludge treatment apparatus as defined in the above-mentioned item 14 or 15, wherein said removal apparatus is a wet-type vibrating screen equipped with two or more types of sieve bodies having different openings.

[0111] 17. The digested sludge treatment apparatus as defined in any one of the above-mentioned items 14 to 16, further comprising an apparatus for washing the separated crystals containing magnesium ammonium phosphate.

[0112] According to a further aspect of the present invention, there is provided a method of preventing scale from forming on the inside of a pipe when digested sludge generated by subjecting organic wastes to anaerobic digestion is transported via the pipe, wherein the digested sludge is treated in a decarbonation process and a screen residue removal process, particulates containing MAP are separated from the digested sludge following decarbonation and screen residue removal, and following removal of these particulates, the digested sludge is transported via the pipe.

[0113] In this method of the present invention, following particulate removal, the digested sludge is preferably subjected to processing to lower the pH and/or processing to reduce at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration, and then transported via the pipe. The anaerobic digestion may be performed following a discharge process for discharging phosphate ions from the organic wastes and a concentration process for concentrating the organic wastes following the discharge process. Further, the digested sludge that is transported via the pipe may have a magnesium ion concentration of no more than 20 mg/L, and preferably no more than 5 mg/L.

[0114] A further aspect of the present invention provides an apparatus for preventing scale from forming on the inside of a pipe when digested sludge generated by treating organic wastes in an anaerobic digestion tank is transported via the pipe, comprising: an apparatus for decarbonating the digested sludge; a removal apparatus for removing screen residues from the digested sludge; and an apparatus for separating particulates containing MAP from the digested sludge after the digested sludge is treated by the decarbonation apparatus and screen residue removal apparatus.

[0115] This apparatus of the present invention preferably further comprises a chemical adding apparatus for lowering the pH of the digested sludge following particulate removal, and/or a chemical adding apparatus for reducing at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration thereof. Further, discharging means for discharging phosphate ions from the organic wastes and a concentration apparatus for concentrating the organic wastes following the discharge process may be disposed before the anaerobic digestion tank.

[0116] A further aspect of the present invention provides a digested sludge treatment method for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, wherein the digested sludge is treated in a crystallization process for precipitating MAP by adding a magnesium compound and screen residue removal process for removing screen residues such as night soil residue from the digested sludge, particulates containing MAP are recovered from the digested sludge in a separation process following the crystallization process and screen residue removal process, and following removal of these particulates, the digested sludge is dewatered in a dewatering process. In this method of the present invention, the MAP-containing particulates recovered in the separation process, or a portion or all of MAP-containing effluent generated in the separation process, may be returned to the crystallization process, and a portion or all of the screen residues removed in the screen residue removal process may be supplied to the dewatering process. Further, following particulate removal, the digested sludge is preferably subjected to processing to lower the pH and/or processing to reduce at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration, and then transported to the dewatering process.

[0117] A further aspect of the present invention provides a digested sludge treatment apparatus for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising: a crystallization apparatus having adding means for adding a magnesium compound in order to precipitate MAP during treatment of the digested sludge; a screen residue removal apparatus for removing screen residues from the digested sludge; a separation apparatus for recovering particulates containing MAP from the digested sludge after the digested sludge is treated by the crystallization apparatus and screen residue removal apparatus; and a dewatering apparatus for dewatering the digested sludge following removal of the particulates. In this apparatus of the present invention, a return path may be provided for returning a portion or all of the MAP-containing particulates recovered by the separation apparatus to the crystallization apparatus, and supply means may be provided for supplying a portion or all of the screen residues removed by the screen residue removal apparatus to the dewatering apparatus. Further, a chemical adding apparatus for lowering the pH of the digested sludge following particulate removal, and/or a chemical adding apparatus for reducing at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration thereof, may be provided after the separation apparatus.

[0118] According to the present invention, by employing the embodiment described above, MAP scale on the inside of a pipe for transporting digested sludge can be reduced greatly, and/or phosphorus can be recovered efficiently from the inside of a digestion tank.

[0119] Embodiments of the present invention will be illustrated hereinafter with reference to Figs. 12 to 17. In Figs. 12 to 17 and Figs. 33 to 35 that will be mentioned hereinafter, each of reference numerals in the drawings denotes the following meaning.
101:
introduced sludge
102:
anaerobic digestion tank
103:
digested sludge (extracted sludge)
104:
decarbonation process
105:
screen residue removal process
106:
screen residues
107:
process for separating particulates containing MAP
108:
recovery of particulates containing MAP
109:
out of the system
110:
pH adjustor
111:
concentrated excess sludge
112:
phosphorus discharge tank
113:
BOD source
114:
concentration process
115:
separated water
116:
dewatering process
117:
concentration-adjusted water
118:
sludge liquor
201:
introduced sludge
202:
anaerobic digestion tank
203:
extracted sludge (digested sludge)
204:
crystallization process
205:
Mg compound
206:
screen residue removal process
207:
screen residues
208:
process for separating particulates containing MAP
209:
recovery of particulates containing MAP
210:
dewatering process
211:
sludge liquor
212:
out of the system
213:
particulate transportation pipe
214:
screen residue transportation pipe
Fig. 12 is a flow diagram showing an example of a treatment flow according to the present invention, which is constituted by an anaerobic digestion tank 102, a decarbonation process 104 for decarbonating digested sludge, a screen residue separation process 105, and a particulate separation process 107 for separating and recovering particulates containing MAP.

[0120] Excess sludge and/or primary sludge are introduced into the anaerobic digestion tank 102. The interior of the anaerobic digestion tank is heated and maintained at a temperature of approximately 55°C or approximately 35°C. In the anaerobic digestion tank, the sludge is broken down into a gas such as methane, carbon dioxide, hydrogen sulfide; water-soluble nitrogen and phosphorus, and so on by the action of acid-fermentative bacteria and methanogenic bacteria. The generated methane gas may be recovered and used as energy. The amount of generated methane gas is increased by introducing easily-decomposable raw sludge in addition to excess sludge. As the sludge decomposes, phosphorus, magnesium, and ammonium are dissolved into the liquid side, and thus MAP is generated spontaneously in the anaerobic digestion tank. As a result of this MAP precipitation, scale trouble occurs on the draft tube, the bottom of the anaerobic digestion tank, the sludge discharge pipe, and so on.

[0121] The ratio of the phosphorus, magnesium, and ammonium in the digested sludge is generally phosphorus : magnesium : ammonium = 100 to 500: several to several tens : 1000, and hence the magnesium concentration is overwhelmingly lower than the phosphorus and ammonium concentrations. During MAP generation in the digestion tank, the magnesium concentration clearly serves as a rate control.

[0122] The digested sludge contains particulates containing MAP, and has a pH in the vicinity of 7, a phosphorus concentration between 100 and 500 mg/L, a magnesium concentration between several and several tens of mg/L, and an ammonium concentration between 500 and 4000 mg/L. Conventionally, a large amount of MAP scale is generated in a sewer when digested sludge having these properties is transported via pipe, leading to problems such as blockings.

[0123] As a result of intensive research into the phenomenon of scale generation, performed by the present inventors and others, it was ascertained that pH variation and gas phase intermixing inside the pipe leads to decarbonation, causing the generation of MAP and hence scaling. In other words, the digested sludge continues to possess a latent ability to generate MAP (referred to as MAP generation ability, hereinafter). To make matters worse, the MAP particulates generated spontaneously in the digested sludge act as seed crystals, promoting scale generation.

[0124] The present inventors focused on the remnant MAP generation ability described above, and thus discovered a need to reduce the remnant MAP generation ability before the digested sludge is introduced into a sewer. The present inventors discovered that the MAP generation ability of digested sludge is greatly reduced by decarbonating the digested sludge to raise the pH such that MAP is generated in advance, and then separating the MAP contained in the digested sludge and the MAP generated in the decarbonation process from the digested sludge, as in the present invention.

[0125] Aeration treatment or decompression treatment may be employed in the decarbonation process 104. Aeration treatment involves aerating the digested sludge such that the carbon gas in the sludge is dispersed into the gas phase, thereby raising the pH such that MAP is generated in a quantity corresponding to the amount of remaining magnesium. In decompression treatment, a degassing apparatus such as that disclosed in Japanese Unexamined Patent Application Publication H7-136406 (referred to as a thin film vacuum degassing apparatus hereafter) is preferably used. Specifically, a subject liquid is put in acceleration by the centrifugal force of a sifting body which has a base and is rotated in a vacuum container, whereby the subject liquid collides with the inner wall surface of the vacuum container such that the gas in the subject liquid is removed. As a result of the decompression treatment, decarbonation occurs, leading to an increase in the pH and the generation of MAP.

[0126] In the treatment described above, if the magnesium ion concentration of the liquid decreases, the MAP generation ability disappears, and hence scale generation is suppressed. For example, if the pH is raised from 7 to 8, the magnesium ion concentration of the digested sludge generally falls to 1/10 to 1/2. In the present invention, the magnesium ion concentration of the digested sludge is set at no more than 20 mg/L, and preferably no more than 5 mg/L. When the magnesium ion concentration is no more than 20 mg/L, almost no MAP supersaturation occurs even when the pH in the sewer varies, or when the gas phase is intermixed such that the pH rises, for example, and hence MAP precipitation can be prevented.

[0127] In addition to a decarbonation method by aeration and decompression, a decarbonation by chemical addition may be employed. Needless to say, these operations may be combined and performed in any order. The decarbonated digested sludge is then introduced into the screen residue removal process 105. In the conventional art, no screen residue separation process is performed, and therefore when a liquid cyclone is used in the subsequent particulate separation process 107, blockings caused by screen residues and the like occur. For this reason, there is demand for a treatment method exhibiting long-term stability. In the present invention, screen residues are sufficiently removed to achieve a significant improvement in the stability of the subsequent particulate separation process 107, particularly when this process employs a liquid cyclone.

[0128] The removed screen residues 106 may be discharged outside of the system or mixed into the digested sludge following the particulate separation process 107. When a dewatering process is provided, the screen residues 106 may be introduced in the dewatering process. In this case, the dewatering performance is enhanced, and it is therefore preferable to introduce the screen residues 106 into the dewatering process if such a process is provided.

[0129] Note that the decarbonation process 104 and screen residue removal process 105 may be performed in any order. The decarbonation process 104 may precede the screen residue removal process 105, or the screen residue removal process 105 may precede the decarbonation process 104, as shown in Fig. 12 and so on.

[0130] Following the decarbonation process 104 and screen residue removal process 105, the particulates containing MAP precipitated in the digestion tank and during the decarbonation process are separated from the digested sludge. A liquid cyclone, a centrifugal settler, a sedimentation tank employing gravity separation, and so on may be employed as a method of separating the particulates from the digested sludge using the specific gravity difference between the two, while a vibrating screen, a drum screen, a filter layer, a classification layer-type separation tank, and so on may be employed as a particulate separation method using differences in particulate diameter.

[0131] A liquid cyclone has a reverse conical-form lower portion structure, and is constituted by a liquid cyclone inflow pipe, a particulate discharge pipe, and a sludge discharge pipe. In the liquid cyclone, the digested sludge containing MAP is caused to swirl down the wall surface of the reverse conical form by the pressure of an extractor pump. The MAP-containing particulates, which have a greater specific gravity than the digested sludge, are collected and concentrated on a lower wall surface side by means of centrifugal force. The concentrated particulates are extracted either continuously or intermittently.

[0132] In the present invention, screen residues are separated before the MAP-containing particulate separation process 107, and therefore problems such as blockings of the liquid cyclone caused by screen residues and the like are solved. Having passed through the decarbonation process 104, screen residue separation process 105, and particulate separation process 107, the digested sludge is transported through a sewer to a collective sludge treatment facility, other type of sludge treatment facility, or a sludge treatment facility within the same premises. As a result of the processes described above, the magnesium ion concentration of the digested sludge is greatly reduced and MAP particulates are removed from the digested sludge. Hence, according to the present invention, the MAP generation ability is reduced even upon pH variation or gas phase intermixing, and therefore MAP scale generation is reduced greatly.

[0133] In the example shown in Fig. 13, processing to lower the pH and/or processing to reduce at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration are performed following the particulate separation process 107. A pH adjustor may be added as a method of reducing the pH. A chemical for lowering the pH of digested sludge, such as hydrochloric acid, sulfuric acid, aluminum salt, or iron salt, is used as the pH adjustor. With aluminum salt and iron salt, the soluble phosphorus contained in the digested sludge is fixed, causing a reduction in the solubility concentration. Ammonia stripping, fixation by adhesive, and so on may be used as a method of reducing ammonium ions. MAP is precipitated when any of the phosphorus concentration, magnesium concentration, ammonium concentration, and pH rises. Conversely, as described above, when the pH of the digested sludge falls or at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration is reduced, the MAP generation ability deteriorates. According to the present invention, the MAP generation ability deteriorates, reducing the likelihood of MAP scale generation. Note that with the addition of iron salt, the generation of hydrogen sulfide and the like from the digested sludge can be suppressed.

[0134] In the example shown in Fig. 14, excess sludge or concentrated excess sludge 111 is introduced into a phosphorus discharge tank 112. Phosphorus is discharged from the sludge by adding a BOD under anaerobic conditions. As a BOD source 113, organic wastes containing raw sludge, a portion of the solubilized sludge that is generated when sludge solubilization treatment is performed, or a portion of the organic waste water from which the excess sludge is generated is used. Also, a chemical such as methanol may be added as a BOD source. In the phosphorus discharge tank 112, phosphorus is discharged from the excess sludge and concentrated excess sludge, and a part of the magnesium contained in the sludge is also eluted to the liquid side. Particularly when a biological dephosphorylation method such as an anaerobic/aerobic process is performed in a water treatment system, the phosphorus concentration and magnesium concentration of the liquid increase dramatically. When phosphorus is discharged from concentrated excess sludge, the phosphorus concentration and magnesium concentration of the liquid fall to approximately 50 to 400 mg/L and 50 to 200 mg/L, respectively. Meanwhile, ammonium elution is small, leading to an ammonium concentration of approximately 50 to 150 mg/L. Having undergone this phosphorus discharge treatment, the discharged sludge is separated into concentrated sludge 101 and concentrated sludge liquor 115 in a sludge concentration apparatus 114, or separated into sludge cake and sludge liquor in a dewatering apparatus. The sludge concentration apparatus 114 is used for a method such as flotation separation, gravity separation, or mechanical separation. The dewatering apparatus is used for a dewatering method such as centrifugal dewatering, belt pressing, or screw pressing.

[0135] The separated liquid and supernatante liquor 115 contain concentrated phosphorus, and it is of course desirable that the phosphorus be removed and recovered by precipitating a phosphorus compound from this waste water. In the anaerobic digestion tank 102, the sludge is broken down such that the phosphorus, magnesium, and ammonium migrate to the liquid side, but by discharging the phosphorus and magnesium from the sludge in advance, before introduction into the anaerobic digestion tank, such that the phosphorus and magnesium concentrations decrease, as in the present invention, the amount of MAP that is generated spontaneously in the anaerobic digestion tank can be reduced. As a result, scale trouble caused by MAP and the like can be suppressed. Moreover, the amount of MAP that is discharged together with the digested sludge can be reduced. In Fig. 14, the digested sludge is decarbonated, screen residues are removed, and then the MAP-containing particulates are separated. The effects of these processes are as described above.

[0136] Another example of the treatment flow according to the present invention is illustrated in Fig. 15. The flow in Fig. 15 is constituted by an anaerobic digestion tank 202, a crystallization process 204, a screen residue removal process 206, a particulate separation process 208, and a dewatering process 210. Note that in the flow illustrated in Fig. 15 and the following Figs. 16 and 17, the dewatering process 210 is not essential, and may be omitted.

[0137] Excess sludge and/or primary sludge 201 are introduced into the anaerobic digestion tank 202. The interior of the anaerobic digestion tank is heated and maintained at a temperature of approximately 55°C or approximately 35°C. In the anaerobic digestion tank, the sludge is broken down into methane, carbon dioxide, a gas such as hydrogen sulfide, water-soluble nitrogen, phosphorus, and so on by the action of acid-fermentative bacteria and methanogenic bacteria. The generated methane gas may be recovered and used as energy. The amount of generated methane is increased by introducing easily-decomposable raw sludge in addition to the excess sludge. As the sludge decomposes, phosphorus, magnesium, and ammonium migrate to the liquid side. When the respective ion concentrations thereof reach or exceed the MAP solubility product, MAP is generated spontaneously in the anaerobic digestion tank. As a result of this MAP precipitation, scale trouble occurs on the draft tube, the bottom of the anaerobic digestion tank, the sludge discharge pipe, and so on.

[0138] Normally, the ratio of the phosphorus, magnesium, and ammonium in the digested sludge is generally phosphorus : magnesium : ammonium = 100 to 500: several to several tens : 1000. The magnesium concentration is overwhelmingly lower than the phosphorus and ammonium concentrations, and therefore during MAP generation in the digestion tank, the magnesium concentration clearly serves as a rate control.

[0139] In the following crystallization process 204, MAP is precipitated by adding a magnesium compound to the digested sludge and digested sludge liquor extracted from the anaerobic digestion tank 202. If aeration, decompression, or the like is also performed at this time, the sludge is decarbonated, leading to an increase in the pH, and hence MAP can be precipitated more efficiently. Needless to say, a chemical such as sodium hydroxide, magnesium hydroxide, or magnesium oxide may be added to raise the pH. Magnesium compounds, such as magnesium chloride, magnesium hydroxide, magnesium oxide, sea water, and the like, may be added. As regards the amount of added magnesium, a molar ratio between 0.1 and 10, preferably between 0.5 and 3.0, and more preferably between 0.8 and 1.2 in relation to the aqueous o-ophosphoric acid concentration of the digested sludge is suitable. The pH in the reaction should be between 7.0 and 11.0, and preferably between 7.5 and 8.5.

[0140] Seed crystals are preferably added to the crystallization process 204 to ensure that MAP is generated efficiently. The MAP that precipitates spontaneously in the digestion tank, the MAP that precipitates in the crystallization process 204, or MAP precipitated in a separate reactor may be used as the seed crystals.

[0141] As shown in another flow diagram of the present invention in Fig. 15, MAP-containing particulates and so on recovered in the separation process 208 may be supplied to the crystallization process 204 through a pipe 213 and be used as seed crystals. Separated water generated midway through the separation process or MAP contained in effluent or the like may also be used.

[0142] Alternatively, a powder or granular substance such as rock phosphate, dolomite, bone charcoal, activated carbon, silica sand, or calcium silicate may be used as seed crystals. The particulate diameter of the seed crystals is arbitrary, but is preferably set between 0.05 and 3.0 mm, and more preferably between 0.1 and 0.5 mm. By precipitating new MAP on the surface of the seed crystals, separation of the digested sludge and MAP in the subsequent separation process can be performed well. The seed crystal charging amount is extremely important for precipitating MAP on the surface of the seed crystals. The charging amount is determined in consideration of the introduced phosphorus amount and the seed crystal particulate diameter such that the phosphorus introduction amount in relation to the seed crystal surface area (the phosphorus surface area load hereafter) is no more than 100 g-P/m2/d, preferably no more than 30 g-P/m2/d, and more preferably no more than 10 g-P/m2/d.

[0143] Next, the digested sludge is introduced into the screen residue removal process 206. In the conventional art, no screen residue separation process is performed, and therefore when a liquid cyclone is used in the subsequent particulate separation process, blockings caused by screen residues and so on occur. For this reason, there is demand for a treatment method exhibiting long-term stability. In the present invention, screen residues are sufficiently removed to achieve a significant improvement in the stability of the subsequent particulate separation process 208, particularly when this process employs a liquid cyclone. Furthermore, when a sedimentation tank is used, the screen residues, digested sludge, and MAP are mixed together, and hence in the past it has been impossible to obtain MAP having a high degree of purity. In the present invention, MAP with a high degree of purity can be obtained by separating the screen residues in advance. The separated screen residues may be discharged outside of the system or may be introduced into the dewatering process 210 through a pipe 214, as shown in another flow diagram of the present invention in Fig. 17. In this case, the dewatering performance is enhanced, and hence the screen residues 106 are preferably introduced into the dewatering process.

[0144] The crystallization process 204 and screen residue separation process 206 may be performed in any order. The crystallization process 204 may precede the screen residue separation process 206, as shown in Fig. 15, or the screen residue separation process 206 may precede the crystallization process 204, as shown in Fig. 16.

[0145] Following the crystallization process 204 and screen residue removal process 206, the particulates containing MAP precipitated in the digestion tank and during the crystallization process are separated from the digested sludge. A liquid cyclone, a centrifugal settler, a sedimentation tank employing gravity separation, and so on may be employed as a method of separating the particulates from the digested sludge using the specific gravity difference between the two, while a vibrating screen, a drum screen, a filter layer, a classification layer-type separation layer, and so on may be employed as a particulate separation method using differences in particulate diameter. The digested sludge is viscous, making it difficult to separate the MAP from the digested sludge through natural sedimentation, and therefore a mechanical separation method using a liquid cyclone or the like is preferable. A liquid cyclone has a reverse conical-form lower portion structure, and it comprises a liquid cyclone inflow pipe, a particulate discharge pipe, and a sludge discharge pipe. In the liquid cyclone, the digested sludge containing MAP is caused to swirl down the wall surface of the reverse conical form by the pressure of an extractor pump. The MAP-containing particulates, which have a greater specific gravity than the digested sludge, are collected and concentrated on a lower wall surface side by means of centrifugal force. The concentrated particulates are extracted either continuously or intermittently.

[0146] In the present invention, screen residues are separated before the MAP-containing particulate separation process 208, and therefore problems such as blockings of the liquid cyclone caused by screen residues and the like are solved.

[0147] In the dewatering process 210, the digested sludge separated from the MAP-containing particulates is dewatered. Belt pressing, screw pressing, filter pressing, centrifugal dewatering, and so on may be used as a dewatering method. As noted above, by introducing the screen residues separated in the screen residue separation process 206 into the dewatering process 210, the dewatering effect can be improved, and hence this is preferable.

[0148] To prevent pipe blockings from being caused by MAP scale following this process, treatments of lowering the pH and/or reducing at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration are preferably performed following the particulate separation process 208. A pH adjustor may be added as a method of reducing the pH. A chemical for lowering the pH of digested sludge, such as hydrochloric acid, sulfuric acid, aluminum salt, or iron salt, is used as the pH adjustor. With aluminum salt and iron salt, the soluble phosphorus contained in the digested sludge is fixed, causing a reduction in the solubility concentration.

[0149] Ammonia stripping, fixation by adhesive, and so on may be used as a method of reducing ammonium ions. MAP is precipitated when any of the phosphorus concentration, magnesium concentration, ammonium concentration, and pH rises. Conversely, as described above, when the pH of the digested sludge falls or at least one of the magnesium ion concentration, phosphate ion concentration, and ammonium ion concentration is reduced, the MAP generation ability deteriorates. According to the present invention, the MAP generation ability deteriorates, reducing the likelihood of MAP scale generation. Note that with the addition of iron salt, the generation of hydrogen sulfide and the like from the digested sludge can be suppressed. Needless to say, each of the above processes may be performed in the same treatment facility, or the sludge may be piped to a different treatment facility for each process.

[0150] By means of the above processes, phosphorus can be recovered efficiently from the digested sludge. In the past, it has been particularly difficult to recover MAP generated spontaneously in a digestion tank, but with the present system, MAP can be recovered easily.

[0151] The crystallization reactor and liquid cyclone of the various embodiments illustrated above in Figs. 1 to 10 may be employed as the apparatuses used in a crystallization process and a particulate separation process of the flows shown in Figs. 12 to 17.

[0152] Furthermore, in the present invention a wet-type vibrating screen comprising two or more sieve bodies having different openings may be used as a screen residue removal apparatus. Fig. 18 shows an example of a treatment flow using a two-stage, wet-type vibrating screen comprising two or more sieve bodies having different openings.

[0153] Fig. 18 illustrates a treatment system in which anaerobically digested sludge generated in a sewage treatment plant serves as raw sludge 1. In this treatment system, pre-existing MAP is recovered from the sludge, further MAP is generated using phosphate ions and ammonia ions, which are soluble components of the sludge, as substrates, and the generated MAP is recovered efficiently.

[0154] According to an investigation made by the inventors, when an iron or aluminum additive is not used in the water treatment system, the anaerobically digested sludge of sewage may contain MAP particulates having a particulate diameter within a range of 0.1 to 2.0 mm at approximately 0.8 g/L on average. In addition to these MAP particulates, the sludge is also intermixed with a large amount of contaminant particulates having a comparatively large particulate diameter of at least 1.0 mm, such as screen residues, plant seed particulates, hair, straw, and wood waste. The flow shown in Fig. 18 is constituted by a two-stage vibrating screen 81, the crystallization reactor 9, the liquid cyclone 2, a MAP washing apparatus 82, and a cleaned MAP slurry dewatering apparatus 83. First, the sludge 1 is introduced into the two-stage vibrating screen 81 comprising two sieves having different openings. A first stage sieve 81a having coarse holes and a second stage sieve 81b having narrow holes are provided in the two-stage vibrating screen 81. The first stage sieve 81a is used to separate contaminants such as screen residues, while the second stage sieve 81b is used to separate MAP particulates having a large particulate diameter for recovery. The matter introduced into the two-stage vibrating screen 81 is divided into three types: contaminant particulates 85 recovered by the first stage sieve 81a, such as screen residues, which have a comparatively large particulate diameter of approximately 0.8 to 3.0 mm or greater and are not to be recovered; particulates 86 composed mainly of MAP that is to be recovered, which pass through the first stage sieve 81a and are recovered by the second stage sieve 81b, and have a particulate diameter of approximately 1.0 mm; and sludge 87 containing particulates having a particulate diameter of approximately 0.3 to less than 1.2 mm, which passes through the second sieve. Following separation from the sludge, the contaminant particulates 85 such as screen residues which are separated by the upper stage coarse sieve 81a may eventually be added to the particulates of separated sludge following recovery of these particulates by the liquid cyclone 2, and may be discharged. By separating contaminants such as screen residues and the like, pipe blockings in the liquid cyclone 2 and the like can be prevented, and an improvement in the purity of the recovered MAP can be achieved. By adding the contaminant particulates 85 to the particulates of separated sludge, deterioration of the treatment performance during dewatering of the discharged sludge can be prevented. The particulates 86 composed mainly of MAP, which are separated by the lower stage narrow sieve 81b, may be recovered as MAP particulates without passing through the downstream crystallization reactor 9. Alternatively, when the amount of seed crystals in the crystallization reactor 9 is insufficient during system start-up or the like, the particulates 86 composed mainly of MAP that are separated by the lower stage narrow sieve may be introduced into the crystallization reactor 9. The sludge 87 containing particulates which passes through the lower stage narrow sieve is introduced entirely into the downstream crystallization reactor 9. By separating the particulates 86 composed mainly of MAP from the sludge, the particulate diameter of the MAP particulates in the downstream crystallization reactor 9 can be controlled, and MAP accumulation or pipe blockings in the reactor 9 can be suppressed.

[0155] A magnesium source and a pH adjusting agent are added to the crystallization reactor 9 as needed, and MAP crystallization is performed using the phosphate ions and ammonia ions dissolved in the sludge as substrates. When the sludge flowing into the reactor 9 contains a large amount of comparatively large MAP particulates having a particulate diameter of at least 1.0 mm, the crystallization reaction in the reactor 9 causes these MAP particulates to grow even larger such that the particulate diameter of a part of the MAP particulates may increase to several millimeters or more. When the MAP particulate diameter reaches several millimeters or more, the MAP particulates may accumulate in the reactor 9 or on the bottom of the pipes, causing blockings. Furthermore, a catalytic function for promoting the MAP crystallization reaction exists on the MAP particulate surface, and therefore MAP generation is promoted as the total surface area of the MAP particulates in the sludge inside the reactor 9 increases. However, as the proportion of MAP particulates having a large particulate diameter in the sludge inside the reactor 9 increases, the MAP surface area decreases in relation to the MAP mass, and hence the reaction promotion effect may decrease in relation to the MAP mass. On the other hand, when the proportion of MAP particulates having a small particulate diameter increases, the MAP particulate recovery rate in the subsequent MAP particulate separation operation performed by the liquid cyclone 2 and so on may decrease. Hence, the MAP particulates in the reactor 9 are preferably controlled to an appropriate size, which is not too small and not too large. In the flow shown in Fig. 18, the MAP particulate diameter in the MAP crystallization reactor 9 may be controlled by adjusting the particulate diameter of the MAP particulates which flow into the crystallization reactor 9, from among the pre-existing MAP particulates in the inflowing sludge. The sludge 87 containing particulates which pass through the lower stage narrow sieve following separation and removal of the large MAP particulates by the upper stage coarse sieve are introduced entirely into the crystallization reactor 9, but since the particulate diameter of the MAP particulates in this sludge is no greater than a predetermined particulate diameter, the likelihood of the MAP particulates accumulating in the bottom of the crystallization reactor 9 or the pipes is extremely small.

[0156] The openings of the two sieves used in the two-stage wet-type vibrating screen must be selected correctly in accordance with the proportion of MAP intermixed in the contaminant particulates 85, the MAP purity of the mainly MAP particulates 86, the filtration resistance and required filtration area of the sieves, the relationship between the MAP particulate diameter and the amount of accumulated MAP in the crystallization reaction tank, and so on. Specifically, in most cases an opening of approximately 0.8 to 3.0 mm is appropriate for the first stage sieve 81a for separating the contaminant particulates, and an opening of approximately 0.3 to 1.2 mm is appropriate for the second stage sieve 81b for separating the mainly MAP particulates. In general, the mainly MAP particulates 86 separated by the second stage sieve 81b are recovered without passing through the downstream crystallization reactor 9, but if necessary, in certain cases it is effective to supply the crystallization reactor 9 with a part of the mainly MAP particulates 86 in accordance with changes in the MAP particulate diameter and the total MAP surface area in the crystallization reaction tank. Also, a part or all of the sludge containing MAP particulates in the crystallization reactor 9 may be circulated back to the upstream two-stage vibrating screen 81 as needed so that MAP particulates which have grown extremely large in the crystallization reactor 9 can be separated as a part of the mainly MAP particulates and be prevented from entering the crystallization reactor 9.

[0157] Note that the particulates 86 composed mainly of MAP that are separated by the second stage sieve 81b may be introduced into the MAP particulate washing apparatus 82 and subjected to classification and washing treatment.

[0158] The sludge containing MAP particulates that is generated in the crystallization reactor 9 is introduced into the liquid cyclone 2 through the liquid cyclone inflow pipe 6, and the MAP particulates are concentrated. The MAP particulate slurry concentrated by the liquid cyclone 2 may be returned to the crystallization reactor 9 through the return pipe 11, or may be discharged appropriately via the particulate discharge pipe 4 as needed in order to adjust the MAP particulate concentration in the crystallization reactor 9. A part or all of the concentrated MAP slurry from the liquid cyclone 2 may be introduced into the downstream MAP washing apparatus 82.

[0159] In the MAP washing apparatus 82, the MAP particulates in the concentrated MAP slurry are separated from other particulates, and the MAP particulates are cleaned by washing water 84. An apparatus which is capable of performing particulate classification and washing simultaneously, such as a flowing film separation and classification apparatus used in a mine or the like, for example, may be employed as the MAP washing apparatus 82.

[0160] The sludge slurry 91 from which MAP particulates have been removed by the MAP washing apparatus 82 may be treated as discharged sludge 88, together with the contaminants 85 such as screen residues, which are separated by the first stage sieve 81a of the two-stage vibrating screen described above, and the sludge following MAP particulate separation that flows out from the overflow riser 5 of the liquid cyclone 2, and accordingly, this sludge may be subjected to treatment such as dewatering.

[0161] The MAP particulates cleaned by the MAP washing apparatus 82 may be directly subjected to dewatering by the dewatering apparatus 83 to produce recovered matter 89. Alternatively, the MAP particulates may be returned to the vibrating screen or be treated in a separation apparatus such as a magnetic separating apparatus or jig to enhance the MAP purity, and then subjected to a drying process to produce recovered matter in a dried, solid form.

[0162] Liquid 90 generated by the dewatering apparatus 83 may be returned as is to the water treatment system as waste water or subjected to dewatering treatment or the like together with the discharged sludge 88.

[0163] When heavy metal particulates other than MAP particulates exist in the liquid 90, sludge containing these heavy metal particulates is preferably separated from the liquid 90 by subjecting the liquid 90 to sedimentation separation treatment prior to dewatering and so on such that only the supernatant liquid is introduced into the dewatering process and so on. By taking these measures, the effective utility value of the resultant dewatered sludge cake may be increased.

[0164] Note that in the flow in Fig. 18, the MAP washing apparatus 82 and dewatering apparatus 83 are not essential components, and may be omitted.

[0165] A combination of three or more types of sieve having different openings may be used as the wet-type vibrating screen.

[0166] As described above, contaminants such as screen residues are removed from the sludge with the two-stage vibrating screen in advance, and prior to subsequent treatment by the crystallization reactor 9 and liquid cyclone 2, MAP particulates having a large particulate diameter pre-existing in the sludge are separated and recovered from the sludge slurry containing MAP particulates having a small particulate diameter whereby control of the particulate diameter of the MAP particulates in the crystallization reactor 9 can be performed easily. As a result, in the absence of blockings of the liquid cyclone, MAP particulates can be separated from the sludge and concentrated with stability.

[0167] The multi-stage wet-type vibrating screen described above may be used as the screen residue removal apparatus of the flow illustrated in Figs. 12 to 17, and may also be used as a screen residue removal apparatus in the various embodiments illustrated in Figs. 1 to 10. Furthermore, the MAP particulate washing apparatus 82 and dewatering apparatus 83 described above may be used as treatment apparatuses in the various embodiments described previously.

Examples



[0168] The present invention will now be described more specifically and in further detail using examples.

[0169] Examples 1 to 3 and Comparative examples 1 and 2 correspond to the embodiment described above with reference to Figs. 1 to 3.

Example 1



[0170] In this example, a performance test was performed on a liquid cyclone using raw sludge obtained by adding MAP prepared in advance to anaerobically digested sludge at 80 g/liter. The apparatus treatment flow is shown in Fig. 1.

[0171] A two-inch cyclone was used as the liquid cyclone 2. To increase the MAP concentration rate, the diameter of the sludge discharge pipe was set at 15 mm and the diameter of the particulate discharge pipe was set at 5 mm. The flow rate of the sludge introduced into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa. The supply rate of the raw sludge 1 was set at 0.6 m3/hr, the circulation rate of the sludge treated by the liquid cyclone 2 (the amount circulated by the pipe 7) was set at 3.4 m3/hr, and the circulation ratio (treated sludge circulation rate/raw sludge supply rate) was set at 5.7. The MAP concentration of the treated sludge 8 was 0.2 g/liter, as opposed to a MAP concentration of 80 g/liter in the raw sludge 1, and hence the MAP recovery rate was 99.8%. The discharge speed (kg/mm2/hr) of the particulates in the particulate discharge pipe was 2.4 kg/mm2/hr, and by keeping the discharge speed low, it was possible to perform treatment well without blockings.

Example 2



[0172] In this example, a phosphorus removal test was performed on digested sludge extracted from a digestion tank of a sewage treatment plant. The treatment flow is shown in Fig. 3.

[0173] The treatment flow was constituted by the sieve method screen residue removal apparatus 11, the crystallization reactor 9, and the liquid cyclone 2. The digested sludge 1 was treated by a vibrating screen having an aperture of 2.0 mm serving as the screen residue removal apparatus 11 to remove screen residues, and then introduced into the crystallization reactor 9. Magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. The MAP concentration in the crystallization reactor 9 was maintained at 40 g/liter. Sludge obtained by mixing together a part of the sludge 6 in the crystallization reactor 9 and a part 7 of the treated sludge of the liquid cyclone 2 was supplied continuously to the liquid cyclone 2.

[0174] A two-inch cyclone was used as the liquid cyclone 2. To increase the MAP concentration rate, the diameter of the sludge discharge pipe was set at 15 mm and the diameter of the particulate discharge pipe was set at 5 mm. The flow rate of the sludge introduced into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa.

[0175] In this example, and in following examples and comparative examples in which the crystallization reactor 9 and liquid cyclone 2 are used in combination, the crystal slurry concentrated by the liquid cyclone was generally returned to the crystallization reactor, and then discharged through a discharge pipe and recovered in an appropriate amount at appropriate intervals (for example, once or plural times a day) on the basis of the MAP precipitation amount, which was predicted in accordance with properties such as the phosphorus concentration of the raw water.

[0176] The supply rate of the raw sludge 1 was set at 0.25 m3/hr. The supply rate of the sludge 6 in the crystallization reactor was 0.5 m3/hr while the circulation rate of the sludge treated by the cyclone 2 was 3.5 m3/hr, and hence the total sludge supply rate to the liquid cyclone 2 was 4 m3/hr. The circulation ratio was set at 7.

[0177] In relation to 800 mg/liter of T-P and 300 mg/liter of PO4-P in the raw sludge 1, the treated sludge 8 contained 350 mg/liter of T-P and 10 mg/liter of PO4-P, and hence the phosphorus recovery rate was 56%. At least 95% of the recovered matter was MAP. In this case, the discharge speed (kg/mm2/hr) of the particulates in the particulate discharge pipe was 1.0 kg/mm2/hr, and by keeping the discharge speed low, it was possible to perform treatment well without blockings.

Example 3



[0178] In this example, a blocking condition was confirmed by circulating raw sludge having a MAP concentration of 55 g/L at a modified circulation ratio (circulated sludge amount/raw sludge amount). The treatment flow shown in Fig. 1 was employed. A two-inch cyclone was used as the liquid cyclone 2, the over diameter (the diameter of the sludge discharge pipe) was set at 14 mm, and the under diameter (the diameter of the particulate discharge pipe) was set at 5 mm. The flow rate of the sludge introduced into the cyclone 2 was set at 4 m3/hr, i.e. the sum total of the circulated sludge 7 amount and the raw sludge amount.

[0179] Fig. 19 shows the relationship between the circulation ratio and the MAP concentration following circulation (the MAP concentration of the sludge that is introduced into the cyclone 2). At circulation ratios of 0.01 and 0.05, the cyclone under (the base portion of the cyclone 2 and the particulate discharge pipe) was blocked, and in this case no treatment could be performed. At a circulation ratio of 0.1 or greater, it was possible to perform treatment well with no blockings. Thus it was found that the sludge circulation ratio is preferably set to 0.1 or more.

Comparative Example 1 (comparative example with Example 1)



[0180] This comparative example corresponds to Example 1. Similarly to Example 1, a performance test was performed on the liquid cyclone using raw sludge containing MAP at a concentration of 80 g/liter. The apparatus flow is shown in Fig. 20.

[0181] A similar liquid cyclone to that of Example 1 was used as the liquid cyclone 2. The raw sludge 1 supply rate was set at 4 m3/hr, and the treated sludge 8 of the liquid cyclone 2 was not returned such that the circulation rate (treated sludge circulation rate/raw sludge supply rate) was zero. A blocking occurred within one minute of the beginning of raw sludge 1 supply to the liquid cyclone 2, rendering separation impossible. The cause of the blocking was determined to be the high MAP concentration of the raw sludge 1. In this case, the discharge speed (kg/mm2/hr) of the particulates in the particulate discharge pipe was 16 kg/mm2/hr, and since the circulation ratio was zero, it is believed that the high discharge speed caused the blocking.

Comparative Example 2 (comparative example with Example 2)



[0182] This comparative example corresponds to Example 2. Similar sludge to that of Example 2 was used as the raw sludge. The treatment flow is shown in Fig. 21. Similarly to Example 2, the treatment flow was constituted by the screen residue removal apparatus 11, the crystallization reactor 9, and the liquid cyclone 2.

[0183] Similarly to Example 2, magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. The MAP concentration in the crystallization reactor 9 was maintained at 40 g/liter.

[0184] The raw sludge feed rate was set at 0.25 m3/hr, the circulation ratio (treated sludge circulation rate/raw sludge feed rate) was set at zero, and the sludge in the crystallization reactor 9 was supplied to the liquid cyclone 2 intermittently at 4 m3/hr.

[0185] The raw sludge contained 800 mg/liter of T-P and 300 mg/liter of PO4-P, whereas the treated sludge 8 contained 900 mg/liter of T-P and 10 mg/liter of PO4-P, and hence the phosphorus recovery rate was -13%. Since the T-P content of the treated sludge was greater than the T-P content of the raw sludge, it is believed that MAP in the reactor flowed out into the treated sludge. In this case, the discharge speed (kg/mm2/hr) of the particulates in the particulate discharge pipe was 8.0 kg/mm2/hr, and although blockings did not occur, the high discharge speed caused MAP particulates to flow out into the treated sludge, resulting in a low recovery rate.

Example 4



[0186] Examples 4 to 8 and Comparative Examples 3 and 4 correspond to the embodiment described above with reference to Figs. 4 to 6.

[0187] In Example 4, a test was performed on digested sludge extracted from a digestion tank of a sewage treatment plant to recover phosphorus in the form of magnesium ammonium phosphate. The treatment flow is shown in Fig. 22.

[0188] The treatment flow was constituted by the sieve method screen residue removal apparatus 11, the crystallization reactor 9, the liquid cyclone 2, and the circulating water tank 55. The digested sludge 1 was treated by a vibrating screen having an aperture of 2.0 mm serving as the screen residue removal apparatus 11 to remove screen residues, and then introduced into the crystallization reactor 9.

[0189] Magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0 while monitoring the pH in the reactor 9 using the pH meter 57. The MAP concentration in the crystallization reactor 9 was maintained at 80 g/liter.

[0190] Particulates discharged from the particulate discharge pipe 52 connected to the bottom of the reactor 9 were supplied to the liquid cyclone inflow pipe 6, and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone 2. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The introduction rate into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa. All of the effluent water from the overflow riser 5 of the liquid cyclone was returned to the return pipe 51 connected to the crystallization reactor 9.

[0191] The sludge supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the sludge extraction rate from the crystallization reactor 9 was set at 1.5 m3/hr.

[0192] The raw sludge 1 contained 800 mg/liter of T-P and 300 mg/liter of PO4-P, whereas the treated sludge 8 had a T-P content of 350 mg/liter and a PO4-P content of 10 mg/liter, and hence the phosphorus recovery rate was 56%. At least 95% of the recovered matter was MAP.

Example 5



[0193] In this example, refuse leachate was treated to remove calcium chloride by precipitating calcium carbonate particulates. The treatment apparatuses were constituted by the crystallization reactor 9, the liquid cyclone 2, and the circulating water tank 55. The treatment flow is shown in Fig. 23.

[0194] In the crystallization reactor 9, refuse leachate (referred to as raw water hereafter) was supplied to the bottom of the reactor 9, and a 5% sodium carbonate aqueous solution was also supplied to the bottom of the reactor 9. The sodium carbonate addition amount was set so as to obtain a C/Ca molar ratio of 1:1 in relation to the calcium concentration of the sludge introduced into the crystallization reactor 9. The reaction pH was set at 8.0. The calcium carbonate concentration in the crystallization reactor 9 was maintained at 80 g/L.

[0195] The particulates discharged from the particulate discharge pipe 52 of the crystallization reactor 9 were supplied to the liquid cyclone inflow pipe 6 and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone 2. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The introduction rate into the liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa.

[0196] The raw sludge supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the extraction rate of the sludge containing MAP particulates from the crystallization reactor 9 was set at 1.5 m3/hr.

[0197] The raw water 1 had a pH of 7.2 and a Ca concentration of 3000 mg/L, whereas the treated water 8 had a pH of 8.0 and a Ca concentration of 100 mg/L. Hence, a calcium removal rate of at least 95% was obtained.

Comparative Example 3 (comparative example of Example 4)



[0198] This comparative example corresponds to Example 4. Similar sludge to that of Example 4 was used as the raw sludge. The treatment flow is shown in Fig. 24. Similarly to Example 4, the treatment flow was constituted by the screen residue removal apparatus 11, the crystallization reactor 9, and the liquid cyclone 2. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 4 was performed.

[0199] Similarly to Example 4, magnesium chloride was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. Prior to the operation, the MAP concentration in the crystallization apparatus was set at 80 g/L.

[0200] The raw sludge 1 supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the sludge in the crystallization reactor 9 was supplied to the liquid cyclone 2 intermittently via the discharge pipe 52 at 4 m3/hr. Sludge supply to the liquid cyclone 2 was on-off controlled in accordance with the numerical value of a level meter (L).

[0201] The raw sludge contained 800 mg/L of T-P and 300 mg/L of PO4-P, whereas the treated sludge had a T-P content of 900 mg/L and a PO4-P content of 10 mg/L, and hence the phosphorus recovery rate was -13%. Three hours after the beginning of the operation, a blocking occurred in the cyclone under (the particulate discharge pipe). With this system, it was difficult to perform stable treatment.

Comparative Example 4 (comparative example with Example 4)



[0202] This comparative example corresponds to Example 4. Similar sludge to that of Example 4 was used as the raw sludge. The treatment flow is shown in Fig. 25. The treatment flow was constituted by the screen residue removal apparatus 11, the crystallization reactor 9, the liquid cyclone 2, and the circulating water tank 55. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 4 was performed.

[0203] Magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. The MAP concentration in the crystallization apparatus was maintained at 80 g/L.

[0204] The particulates discharged from the particulate discharge pipe 52 at the bottom of the crystallization reactor 9 were supplied to the liquid cyclone inflow pipe 6 and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone 2. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The introduction rate into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa. Introduction water supply to the liquid cyclone was on-off controlled in accordance with the numerical value of a level meter (L) provided in the crystallization reactor 9. All of the sludge flowing out from the overflow riser 5 of the liquid cyclone was supplied to the circulating water tank.

[0205] The raw sludge 1 supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the sludge extraction rate from the crystallization reactor 9 was set at 1.5 m3/hr.

[0206] .The raw sludge 1 had a T-P content of 800 mg/L and a PO4-P content of 300 mg/L, whereas the treated sludge 8 had a T-P content of 400 mg/L and a PO4-P content of 10 mg/L, and hence the phosphorus recovery rate was 50%. At least 95% of the recovered matter was MAP.

[0207] In comparison to Example 4, the recovery rate was lower, and moreover stability was insufficient due to variation in the water level, variation in the treated water quality caused by variation in the particulate concentration inside the reactor, and so on.

Example 6



[0208] In this example, a test was performed on digested sludge extracted from a digestion tank of a sewage treatment plant to recover phosphorus in the form of magnesium ammonium phosphate (MAP). The treatment flow is shown in Fig. 26. An improvement in the MAP particulate recovery rate was intended by disposing two liquid cyclones in parallel.

[0209] The treatment flow was constituted by the sieve method screen residue removal apparatus 11, the crystallization reactor 9, the two liquid cyclones 2, 2', and the circulating water tank 55. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 4 was performed.

[0210] Magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. The MAP concentration in the crystallization apparatus was maintained at 80 g/L.

[0211] The MAP particulates discharged from the particulate discharge pipe 52 from the bottom of the crystallization reactor 9 were supplied to the liquid cyclone inflow pipe 6 and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone 2. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The inflowing water introduction rate into the liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa. All of the sludge flowing out from the overflow riser 5 of the liquid cyclone was returned to the return pipe 51 connected to the crystallization reactor 9.

[0212] The raw sludge 1 supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the sludge extraction rate from the crystallization reactor 9 was set at 1.5 m3/hr.

[0213] An identical two-inch cyclone to the first stage cyclone 2 was used as the second stage cyclone 2'. The second stage cyclone 2' was provided with the aim of recovering the particulates that flow out from the overflow riser 5 of the first stage liquid cyclone 2. Effluent water from the circulating water tank 55 was introduced into the second stage cyclone 2'. The inflow rate into the second stage cyclone 2' was set at 4 m3/hr, and the introduction operation was performed intermittently.

[0214] The raw sludge 1 had a T-P content of 800 mg/L and a PO4-P content of 300 mg/L, whereas the treated sludge 8 had a T-P content of 320 mg/L and a PO4-P content of 10 mg/L, and hence the phosphorus recovery rate was 60%. By providing two cyclones in parallel, an improvement in the phosphorus recovery rate was achieved.

Example 7



[0215] In this example, a test was performed to recover phosphorus in the form of hydroxyapatite from separated water (raw water hereafter) obtained in a process for concentrating the excess sludge of a sewage treatment plant. The treatment flow is shown in Fig. 27.

[0216] The treatment flow was constituted by the crystallization reactor 9, the liquid cyclone 2, and the circulating water tank 55. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 4 was performed.

[0217] In the crystallization reactor 9, rock phosphate was floated in advance as seed crystals. Calcium chloride was added to obtain a Ca/P weight ratio of 5.6 in relation to the o-phosphate ion concentration of the raw water, and a pH adjusting agent was added to adjust the pH to 8.3. The phosphate rock concentration in the crystallization reactor 9 was maintained at 80 g/L.

[0218] The particulates discharged from the particulate discharge pipe 52 from the bottom of the crystallization reactor 9 were supplied to the liquid cyclone inflow pipe 6 and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The inflow rate into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa.

[0219] The raw water supply rate to the crystallization reactor 9 was set at 0.25 m3/hr, and the sludge extraction rate from the crystallization reactor 9 was set at 1.5 m3/hr. All of the sludge flowing out from the overflow riser 5 of the liquid cyclone was returned to the return pipe 51 connected to the crystallization reactor 9.

[0220] In relation to 46 mg/L of T-P and 45 mg/L of PO4-P in the raw water, treated water contained 3.2 mg/L of T-P and 2.0 mg/liter of PO4-P, and hence the phosphorus recovery rate was 93%.

Example 8



[0221] In this example, a test was performed to recover fluorine in the form of calcium fluoride from the waste water (referred to as raw water hereinafter) of a semiconductor manufacturing factory. The treatment flow is shown in Fig. 28.

[0222] The treatment flow was constituted by the crystallization reactor 9, the liquid cyclone 2, and the circulating water tank 55.

[0223] In the crystallization reactor 9, calcium fluoride crystals were floated in advance as seed crystals. Calcium chloride was added to obtain a Ca/F weight ratio of 1.5 in relation to the fluorine ion concentration of the raw water, and a pH adjusting agent was added to adjust the pH to 6.5. The calcium fluoride concentration in the crystallization reactor 9 was maintained at 80 g/L.

[0224] The particulates discharged from the particulate discharge pipe 52 from the bottom of the crystallization reactor 9 were supplied to the liquid cyclone inflow pipe 6 and then supplied to the liquid cyclone 2 continuously together with circulated water. A two-inch cyclone was used as the liquid cyclone 2. The diameter of the sludge discharge pipe of the liquid cyclone 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 9.4 mm. The inflow rate into the liquid cyclone 2 was set at 4 m3/hr, and the introduction pressure was set at 0.40 MPa.

[0225] The raw water 1 supply rate to the crystallization reactor 9 was set at 0.15 m3/hr, and the rate at which the particulate-containing sludge was extracted from the crystallization reactor 9 was set at 1.5 m3/hr.

[0226] The raw water 1 had a fluorine concentration of 600 mg/L, whereas the treated water 8 had a fluorine concentration of 8 mg/L, and hence the fluorine recovery rate was at least 95%.

Example 9



[0227] Examples 9 to 11 and Comparative Example 5 correspond to the embodiment described above with reference to Figs. 7 to 10. A phosphorus removal test was performed on digested sludge extracted from a digestion tank of a sewage treatment plant. Prior to introduction into the crystallization reactor, screen residues were removed from the sludge using an identical screen residue removal apparatus to that of Example 2.

[0228] The treatment flow of Example 9 is shown in Fig.29. The treatment flow was constituted by the crystallization reactor 9 and two liquid cyclones 2 disposed in parallel.

[0229] Following treatment by the sieve method screen residue removal apparatus, the digested sludge was introduced into the crystallization reactor 9. Magnesium chloride 10 was added to the crystallization reactor 9 to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. Two-inch cyclones were used as the liquid cyclones 2. The diameter of the sludge discharge pipe of the liquid cyclones 2 was set at 14 mm and the diameter of the particulate discharge pipe was set at 8 mm. Sludge obtained by mixing together the sludge 6 extracted from the bottom of the crystallization reactor 9 and a part of the treated sludge flowing out from the overflow riser 5 of the liquid cyclones was supplied continuously to the liquid cyclones 2 via the return pipe 7. The flow rate of the sludge introduced into one liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa.

[0230] The inflow rate of the raw sludge was monitored by the flow meter 71, and on-off control was performed by a pump 72 such that when the inflow rate of the raw sludge 1 fell to or below 0.25 m3/hr, only one of the liquid cyclones was activated, and when the inflow rate of the raw sludge 1 was between 0.25 and 0.5 m3/hr, both of the liquid cyclones were activated.

[0231] The MAP concentration in the crystallization reactor 9 was maintained at no less than 100 g/L regardless of variation in the inflow rate of the raw sludge 1 between 0.15 and 0.50 m3/hr. The raw sludge 1 had a T-P content of 800 mg/liter and a PO4-P content of 300 mg/liter, whereas the treated sludge 8 had a T-P content of 350 mg/liter and a PO4-P content of 10 mg/liter, and hence the phosphorus recovery rate was 56%. At least 95% of the recovered matter was MAP.

Example 10



[0232] In this example, the sludge concentration meter 73 was disposed in the crystallization reactor 9, and the number of operational liquid cyclones 2 was controlled by monitoring the sludge concentration in the reactor 9. The treatment is shown in Fig. 30. Note that the sludge concentration measured by monitoring was converted into a MAP concentration using a calibration curve prepared in advance.

[0233] The treatment flow was constituted by the crystallization reactor 9 and two liquid cyclones 2. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 9 was performed.

[0234] The crystallization reactor 9 and liquid cyclones 2 employed in this example were similar to those of Example 9. Sludge obtained by mixing together the sludge 6 extracted from the bottom of the crystallization reactor and a part of the treated sludge flowing out from the overflow riser 5 of the liquid cyclones was supplied continuously to the liquid cyclones 2 via the return pipe 7. The inflow rate into one liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa.

[0235] Control was performed by the pump 72 such that when the MAP concentration in the reactor 9 fell to or below 100 g/L, both of the liquid cyclones 2 were operated, and when the MAP concentration exceeded 100 g/L, one of the liquid cyclones was halted and the other was operated.

[0236] The properties of the treated sludge remained stable regardless of variation in the flow rate of the raw sludge between 0.15 and 0.50 m3/hr. The raw sludge had a T-P content of 800 mg/L and a PO4-P content of 300 mg/L, whereas the treated sludge had a T-P content of 350 mg/L and a PO4-P content of 10 mg/L, and hence the phosphorus recovery rate was 56%. At least 95% of the recovered matter was MAP.

Example 11



[0237] In this example, treatment was performed using a treatment flow such as that shown in Fig. 31. Digested sludge 1 obtained by subjecting excess sludge to anaerobic digestion in an anaerobic digestion tank at 35°C was used as the raw sludge. The pH and phosphorus concentration of the treated sludge flowing out from the overflow riser of the liquid cyclone were monitored, and a supersaturation value was calculated. The number of operational liquid cyclones was then controlled on the basis of the calculation value.

[0238] The treatment flow was constituted by the crystallization reactor 9 and two liquid cyclones 2. In the following, where specific description to the contrary is not provided, it is assumed that identical treatment to that of Example 9 was performed.

[0239] The crystallization reactor 9 and liquid cyclones 2 employed in this example were similar to those of Example 9. Sludge obtained by mixing together the sludge 6 extracted from the bottom of the crystallization reactor and a part of the treated sludge flowing out from the overflow riser 5 of the liquid cyclones was supplied continuously to the liquid cyclones 2 via the return pipe 7. The inflow rate into one liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa.

[0240] The pH and phosphorus concentration of the treated sludge 8 flowing out from the overflow riser 5 of the liquid cyclones were monitored using the phosphorus concentration meter 74 and pH meter 75. The pH and the phosphate-phosphorus ion concentration were measured by a monitoring apparatus using a pH electrode and a colorimetric method. Note that the phosphate-phosphorus concentration was measured by dissolving MAP at a sludge pH of 3. The elution of biological phosphorus at pH 3 was not detected.

[0241] The supersaturation ratio was calculated using the pH and phosphate-phosphorus ion concentration measured by the monitoring apparatus, together with ammonia nitrogen at 600 mg/L and Mg at 50 mg/L. When the supersaturation ratio was 25 or less, one liquid cyclone was made operational, and when the supersaturation ratio exceeded 25, two liquid cyclones were made operational.

[0242] The properties of the treated sludge remained stable regardless of variation in the raw sludge flow rate between 0.15 and 0.50 m3/hr. The raw sludge had a T-P content of 800 mg/L and a PO4-P content of 300 mg/L, whereas the treated sludge had a T-P content of 350 mg/L and a PO4-P content of 10 mg/L, and hence the phosphorus recovery rate was 56%. At least 95% of the recovered matter was MAP. The high supersaturation ratio was due to the large number of precipitated MAP particulates. In this case, two liquid cyclones were made operational in order to raise the MAP concentration in the crystallization reactor, and as a result the recovery rate increased.

Comparative Example 5 (comparative example with Example 9)



[0243] This example is a comparative example with Example 9, in which a similar phosphorus removal test to that of Example 9 was performed. The treatment flow is shown in Fig. 32.

[0244] The treatment flow was constituted by the crystallization reactor 9 and a single liquid cyclone 2.

[0245] Sludge introduction into the crystallization reactor 9, operation of the crystallization reactor 9, and operation of the liquid cyclone were performed in a similar manner to Example 9. Sludge obtained by mixing together the sludge 6 extracted from the bottom of the crystallization reactor 9 and a part of the treated sludge flowing out from the overflow riser 5 of the liquid cyclone was supplied continuously to the liquid cyclone 2 via the liquid cyclone inflow pipe 6. The inflow rate into the liquid cyclone was set at 4 m3/hr, and the introduction pressure was set at 0.45 MPa.

[0246] A single liquid cyclone was operated regardless of the flow rate of the raw sludge 1.

[0247] The raw sludge flow rate varied between 0.15 and 0.50 m3/hr, and the MAP concentration in the crystallization reactor 9 could not be maintained at or above 100 g/L. The raw sludge had a T-P content of 800 mg/L and a PO4-P content of 300 mg/L, while the T-P content of the treated sludge varied between 350 and 450 mg/L. Since the PO4-P content was substantially constant at 10 mg/L, it is believed that a large number of MAP particulates were precipitated when the MAP concentration in the reactor 9 decreased. Accordingly, treatment stability was lacking in comparison with Example 9.

Example 12



[0248] Examples 12 to 14 and Comparative Example 6 correspond to the embodiment described above with reference to Figs. 12 to 14.

[0249] In Example 12, treatment was performed using a treatment flow such as that shown in Fig. 12. The excess sludge of an anaerobic/aerobic process was used as the subject organic wastes. The treatment flow was constituted by an anaerobic digestion tank, an aeration tank serving as a decarbonation tank, a screen residue removal process, and a particulate separation process. The amount of sludge introduced into the anaerobic digestion tank was set at 90 L/d. Digestion took place over twenty days at a digestion temperature of 35°C. Approximately 90 L/d of digested sludge was discharged from the digestion tank as extracted sludge. The extracted sludge was aerated to raise the pH. Aeration took place over two hours at an air intake rate of 40 L/min. In the screen residue separation process, screen residues were removed using a vibrating screen with an aperture of 2.0 mm. Following decarbonation and screen residue removal, the digested sludge was separated into digested sludge and MAP-containing particulates using a 4-inch liquid cyclone.

[0250] Note that the decarbonation process, screen residue separation process, and particulate separation process were performed as semibatch operations. The water quality in each process is shown in Table 1.

[0251] Regarding the sludge introduced to anaerobic digestion (introduced sludge hereafter), TS was 42 g/L, VS was 35 g/L, and T-P was 920 mg/L. Following extraction from the anaerobic digestion tank, the sludge (extracted sludge hereafter) had a pH of 7.2, and contained 21 g/L of TS, 17 g/L of VS, 920 mg/L of T-P, 300 mg/L of soluble PO4-P, and 15 mg/L of soluble magnesium.

[0252] Following aeration of the extracted sludge to raise the pH to 8.2, the soluble magnesium concentration was measured and found to have decreased to 3 mg/L. The amount of MAP-containing particulates recovered in the particulate separation process was 1.9 g/L, of which 1.5 g/L was MAP.

[0253] After undergoing this treatment, a simulation was conducted in which the digested sludge was transferred continuously into a stainless steel pipe having an inner diameter of 130 mm. The sludge was retained in the pipe for 15 days. After approximately three months, no scale-like crystals could be found in the pipe. The amount of scale that had become adhered to a test piece provided in advance was only 2 g. Hence, it is determined that by performing the treatment described above, it is possible to prevent scale generation.

[0254] 
TABLE 1
 INTRODUCED SLUDGEEXTRACTED SLUDGEDECARBONATED DIGESTED SLUDGEDIGESTED SLUDGE FOLLOWING PARTICULATE SEPARATION
pH (-) - 7.2 8.5 8.5
TS (g/L) 42 21 21 19
VS (g/L) 35 17 17 17
T-P (mg/L) 920 920 920 720
PO4-P (mg/L) - 300 280 280
Mg (mg/L) - 15 2 2
AMOUNT OF RECOVERED ---PARTICULATES (g/L)       1.9

Example 13



[0255] In this example, treatment was performed using a treatment flow such as that shown in Fig. 12. The excess sludge of an anaerobic/aerobic process was used as the subject organic wastes. The treatment flow was constituted by an anaerobic digestion tank, decompression treatment serving as a decarbonation tank, a screen residue separation process, and a particulate separation process. The amount of sludge , introduced into the anaerobic digestion tank was set at 90 L/d. Digestion took place over twenty days at a digestion temperature of 35°C. Approximately 90 L/d of digested sludge was discharged from the digestion tank as extracted sludge.

[0256] The extracted sludge was decompressed to raise the pH. The degree of vacuum was set at -94 kPa, and the rotation speed of the rotary body was set at 1650 rpm.

[0257] In the screen residue separation process, screen residues were removed using a vibrating screen with an aperture of 2.0 mm. Following decarbonation and screen residue removal, the digested sludge was separated into digested sludge and MAP-containing particulates using a 4-inch liquid cyclone.

[0258] Note that the decarbonation process, screen residue separation process, and particulate separation process were performed as semibatch operations. The water quality in each process is shown in Table 2.

[0259] Regarding the sludge introduced to anaerobic digestion (introduced sludge hereafter), TS was 42 g/L, VS was 35 g/L, and T-P was 920 mg/L. Following extraction from the anaerobic digestion tank, the sludge (extracted sludge hereafter) had a pH of 7.2, and contained 21 g/L of TS, 17 g/L of VS, 920 mg/L of T-P, 300 mg/L of soluble PO4-P, and 15 mg/L of soluble magnesium.

[0260] Following aeration of the extracted sludge to raise the pH to 8.2, the soluble magnesium concentration was measured and found to have decreased to 3 mg/L. The amount of MAP-containing particulates recovered in the particulate separation process was 1.9 g/L, of which 1.5 g/L was MAP.

[0261] After undergoing this treatment, a simulation was conducted in which the digested sludge was transferred continuously into a stainless steel pipe having an inner diameter of 130 mm. The sludge was retained in the pipe for 15 days. After approximately three months, no scale-like crystals could be found in the pipe. The amount of scale that had become adhered to a test piece provided in advance was only 2 g. Hence, it may be determined that by performing the treatment described above, it was possible to prevent scale generation.

[0262] 
TABLE 2
 INTRODUCED SLUDGEEXTRACTED SLUDGEDECARBONATED DIGESTED SLUDGEDIGESTED SLUDGE FOLLOWING PARTICULATE SEPARATION
pH (-) - 7.2 8.2 8.2
TS (g/L) 42 21 21 19
VS (g/L) 35 17 17 17
T-P (mg/L) 920 920 920 720
PO4-P (mg/L) - 300 280 280
Mg (mg/L) - 15 3 3
AMOUNT OF RECOVERED PARTICULATES (g/L) - - - 1.9

Example 14



[0263] In this example, treatment was performed using a treatment flow such as that shown in Fig. 33. The excess sludge of an anaerobic/aerobic process was used as the subject organic wastes. The treatment flow was constituted by a phosphorus discharge tank, a dewatering process, a concentration adjustment process, an anaerobic digestion tank, a decarbonation tank (aeration tank), a screen residue separation process, and a particulate separation process. The excess sludge was retained in the phosphorus discharge tank for one day. The anaerobic digestion tank, decarbonation tank (aeration tank), screen residue separation process, and particulate separation process were performed similarly to those of Example 12. The water quality in each process is shown in Table 3.

[0264] Regarding the concentrated excess sludge, TS was 42 g/L, VS was 35 g/L, T-P was 920 mg/L, PO4-P was 20 mg/L, soluble Mg was 10 mg/L. At the outlet of the phosphorus discharge process, the soluble PO4-P and Mg had increased to 300 mg/L and 100 mg/L, respectively. Following phosphorus discharge, the concentrated excess sludge was dewatered, whereupon the TS of the sludge was adjusted to 42 g/L using secondary waste water effluent. Following this adjustment, the sludge contained 42 g/L of TS, 35 g/L of VS, 600 mg/L of TP, 60 mg/L of PO4-P, and 20 mg/L of soluble Mg.

[0265] Regarding the extracted sludge, TS was 20 g/L, VS was 17 g/L, T-P was 600 mg/L, PO4-P was 180 mg/L, and soluble Mg was 20 mg/L. Following aeration of the extracted sludge to raise the pH to 8.2, the soluble magnesium concentration was measured and found to have decreased to 3 mg/L.

[0266] The amount of MAP-containing particulates recovered in the particulate separation process was 0.3 g/L, of which 0.25 g/L was MAP.

[0267] After undergoing this treatment, a simulation was conducted in which the digested sludge was transferred continuously into a stainless steel pipe having an inner diameter of 130 mm. The sludge was retained in the pipe for 15 days. After approximately three months, no scale-like crystals could be found in the pipe. The amount of scale that had become adhered to a test piece provided in advance was only 2 g. Hence, it may be determined that by performing the treatment described above, it was possible to prevent scale generation.

[0268] 
TABLE 3
 INTRODUCED SLUDGEPHOSPHORUS DISCHARGE TANK OUTLETINTRODUCED SLUDGE (FOLLOWING TS CONCENTRATION ADJUSTMENT)EXTRACTED SLUDGEDECARBONATED DIGESTED SLUDGEDIGESTED SLUDGE FOLLOWING PARTICULATE SEPARATION
pH (-) - - - 7.2 8.2 8.2
TS (g/L) 42 38 42 20 20 19
VS (g/L) 35 31 35 17 17 17
T-P (mg/L) 920 830 600 600 600 560
PO4-P (mg/L) 20 300 60 180 160 160
Mg (mg/L) 10 100 20 20 3 3
AMOUNT OF RECOVERED PARTICULATES (g/L) - - - - - 0.3

Comparative Example 6



[0269] In the following, the results of a comparison with Example 12 will be illustrated. As shown in Fig. 34, this comparative example is identical to Eexample 12 except that the decarbonation process, screen residue separation process, and particulate separation process have been omitted. The water quality in each process is shown in Table 4.

[0270] Regarding the introduced sludge, TS was 42 g/L, VS was 35 g/L, and T-P was 920 mg/L. Regarding the extracted sludge, TS was 21 g/L, VS was 17 g/L, T-P was 920 mg/L, PO4-P was 300 mg/L, and soluble Mg was 9 mg/L. After undergoing treatment, a simulation was conducted in which the digested sludge was transferred continuously into a stainless steel pipe having an inner diameter of 130 mm. The sludge was retained in the pipe for 15 days. After approximately three months, scale having a thickness of approximately 3 mm had formed on the wall surface of the pipe. The scale was subjected to component analysis using an X-ray diffraction apparatus and a fluorescent X-ray apparatus, in which the scale was found to be MAP. It is believed that the MAP was generated due to MAP accumulation in the digested sludge and pH variation caused by decarbonation and the like in the pipe.

[0271] 
TABLE 4
 INTRODUCED SLUDGEEXTRACTED SLUDGE
pH (-) - 7.2
TS (g/L) 42 21
VS (g/L) 35 17
T-P (mg/L) 920 920
PO4-P (mg/L) - 300
Mg (mg/L) - 9
AMOUNT OF RECOVERED PARTICULATES (g/L) - -

Example 15



[0272] Example 15 and Comparative Example 7 correspond to the embodiment described above with reference to Figs. 15 to 17.

[0273] In Example 15, treatment was performed using a treatment flow such as that shown in Fig. 15. The excess sludge of an anaerobic/aerobic process was used as the subject organic wastes.

[0274] The treatment flow was constituted by an anaerobic digestion tank, a crystallization tank, a screen residue separation process, and a particulate separation process. The amount of sludge introduced into the anaerobic digestion tank was set at 90 L/d. Digestion took place over twenty days at a digestion temperature of 35°C. Approximately 90 L/d of digested sludge was discharged from the digestion tank as extracted sludge. Magnesium chloride was added to the crystallization tank to obtain an Mg/P molar ratio of 1 in relation to the o-phosphate ion concentration of the digested sludge, and a pH adjusting agent was added to adjust the pH to 8.0. Further, 7 kg of the MAP-containing particulates recovered in the particulate separation process was added as seed crystals.

[0275] A vibrating screen with an aperture of 2.0 mm was used in the screen residue separation process.

[0276] A 4-inch liquid cyclone was used in the particulate separation process.

[0277] Note that all processes other than that performed in the anaerobic digestion tank were performed as semi-batch operations. The water quality in each process is shown in Table 5.

[0278] Regarding the sludge introduced to anaerobic digestion (introduced sludge), TS was 42 g/L, VS was 35 g/L, and T-P was 920 mg/L. Following extraction from the anaerobic digestion tank, the sludge (extracted sludge: digested sludge) had a pH of 7.2, and contained 21 g/L of TS, 17 g/L of VS, 9.20 mg/L of T-P, and 300 mg/L of soluble PO4-P. The sludge discharged from the crystallization tank had a pH of 8.0, and contained 24 g/L of TS, 17 g/L of VS, 920 mg/L of T-P, and 10 mg/L of soluble PO4-P. The amount of MAP-containing particulates recovered in the particulate separation process was 4.3 g per liter of digested sludge, of which 4.0 g was MAP. The discharged sludge had a pH of 8.0, and contained 19 g/L of TS, 17 g/L of VS, 440 mg/L of T-P, and 10 mg/L of soluble PO4-P. Of the 920 mg/L phosphorus concentration introduced into the digested sludge, 480mg/L was recovered.

[0279] 
TABLE 5
 INTRODUCED SLUDGEEXTRACTED SLUDGEDECARBONATED DIGESTED SLUDGEDIGESTED SLUDGE FOLLOWING PARTICULATE SEPARATION
pH (-) - 7.2 8 8
TS (g/L) 42 21 24 19
VS (g/L) 35 17 17 17
T-P (mg/L) 920 920 920 440
PO4-P (mg/L) - 300 10 10
AMOUNT OF RECOVERED PARTICULATES (g/L) - - - 4.3

Comparative Example 7



[0280] In the following, the results of a comparison with Example 15 will be illustrated. As shown in Fig. 35, Comparative Example 7 is identical to the Example 15 except that the crystallization process, screen residue separation process, and particulate separation process have been omitted. The water quality in each process is shown in Table 6.

[0281] 
TABLE 6
 INTRODUCED SLUDGEEXTRACTED SLUDGE
PH (-) - 7.2
TS (g/L) 42 21
VS (g/L) 35 17
T-P (mg/L) 920 920
PO4-P (mg/L) - 300
AMOUNT OF RECOVERED PARTICULATES (g/L) - -


[0282] Regarding the introduced sludge, TS was 42 g/L, VS was 35 g/L, and T-P was 920 mg/L. The extracted sludge contained 21 g/L of TS, 17 g/L of VS, 920 mg/L of T-P, and 300 mg/L of PO4-P. The extracted sludge also contained 1.5 g/L of MAP. The MAP in the extracted sludge was not recovered, but dewatered and then incinerated.

[0283] The amount of recovered phosphorus in the comparative example described above was zero.

Example 16



[0284] In this example, sludge was treated using an identical flow to the treatment flow of Fig. 18 described above. The description relating to Fig. 18 should be referred to for details concerning this flow. The anaerobically digested sludge of a sewage treatment plant A was used as the subject sludge, and the MAP generated in this sludge was set as the subject recovered matter. The digested sludge treatment speed in this flow was set at 5 m3/day, and the operation was performed for three months.

[0285] The sieve openings of the two-stage vibrating screen 81 were set on the basis of the results of property analysis performed on the sludge of the sewage treatment plant A. The sieve opening of the upper stage sieve 81a was set at 2.0 mm, and the sieve opening of the lower stage sieve 81b was set at 0.5 mm. The separated matter (contaminants such as screen residues) 85 separated by the upper stage sieve 81a was added to MAP-separated sludge flowing out from the overflow riser 5 of the liquid cyclone 2 and the MAP-separated sludge 91 from the MAP particulate washing apparatus 82, and discharged as discharged sludge. The separated matter (particulates mainly containing MAP crystals) which passed through the upper stage sieve 81a but did not pass through the lower stage sieve 81b was introduced directly into the MAP washing apparatus 82. The separated matter (sludge slurry containing particulates) which passed through the lower stage sieve 81b was guided to the MAP crystallization reactor 9, where magnesium chloride and caustic soda were added as necessary to instigate a crystallization reaction. The sludge containing MAP particulates in the MAP crystallization reactor 9 was introduced appropriately into the two-inch liquid cyclone 2 through the liquid cyclone inflow pipe 6, the MAP particulates concentrated by the cyclone 2 were returned to the MAP crystallization reactor 9 through the return pipe 11, and a part thereof was introduced as appropriate into the MAP washing apparatus 82 through the particulate discharge pipe 4. A drum type flowing film separation and classification apparatus was used as the MAP washing apparatus 82, and hence MAP particulates were separated from the introduced MAP particulate-containing slurry, classified, and cleaned by the washing water 84. Following separation and washing, the MAP particulates were dewatered by the dewatering apparatus 83, and then recovered as the MAP crystals 89.

[0286] To provide a comparative flow, identical treatment was performed on identical subject sludge using a single-stage vibrating screen. Fig. 36 shows this comparative flow. In the comparative flow shown in Fig. 36, a single-stage sieve 91 having an opening of 2.0 mm was used as the vibrating screen, separated contaminants 92 such as screen residues were discharged as discharged sludge, and all of the sludge slurry 93 containing the MAP particulates that passed through the sieve was introduced into the crystallization reactor 9. All other conditions were identical to those of the flow shown in Fig. 18.

[0287] The results of Example 16 are shown in Table 7.

[0288] The aim of this system was to recover MAP from sewage sludge in as large a quantity as possible but with as high a purity as possible. Accordingly, the "MAP recovery amount per liter of digested sludge" and the "recovered MAP purity" were set as the two evaluation items of the system.

[0289] With the treatment flow using a two-stage sieve shown in Fig. 18, the average MAP recovery rate was 3.9 g/L and the average recovered MAP purity was 86.6%. With the treatment flow using a single-stage sieve shown in Fig. 36, the average MAP recovery rate was 3.5 g/L and the average recovered MAP purity was 82.7%. Hence, in the flow using the two-stage sieve, the MAP recovery rate increased by 0.4 g/L, which is an increase of more than 10% over the flow using the single-stage sieve, and the MAP purity increased by 4.2% over the flow using the single-stage sieve. With the method using the single-stage vibrating screen, MAP particulates, grown to several millimeters or more may partially settle in the system piping or the reaction tanks, which is believed to cause a reduction in the MAP recovery rate. Moreover, particulates other than MAP, for example refuse and wood waste having a particulate diameter of 2.0 mm or less, pass through the single-stage sieve and are introduced into the MAP crystallization reactor 9 together with the MAP particulates. As a result, crystallized MAP becomes adhered to the surfaces of the non-MAP particulates, and these newly formed particulates are recovered in the downstream MAP washing apparatus together with the MAP, leading to deterioration in the recovered MAP purity. Alternatively, the particulates may be discarded from the recovered matter, leading to deterioration in the MAP recovery rate. With the flow using the two-stage sieve, on the other hand, the non-MAP particulates such as refuse and wood waste which pass through the first-stage sieve having an opening of 2 mm are separated by the second-stage sieve together with the MAP particulates having a large particulate diameter. Since these particulates are transmitted directly to the MAP washing apparatus without passing through the crystallization reactor, they do not contribute to the reaction that takes place in the crystallization reactor. As a result, relatively favorable treatment results can be obtained in terms of both the MAP recovery rate and the MAP purity when a two-stage sieve is employed.

[0290] 
TABLE 7 TREATMENT RESULTS OF EXAMPLE 16
 FLOW USING TWO-STAGE SIEVEFLOW USING ONE-STAGE SIEVE
RAW SLUDGE pH (-) 7.2-7.6 (AVERAGE 7.4)
PO4-P (mg/L) 310-390 (AVERAGE 365)
MAP AMOUNT (g/L) 0.6-1.1 (AVERAGE 0.9)
MAP RECOVERY RATE (g/L OF SLUDGE) 3.5-4.3 (AVERAGE 3.9) 2.9-3.9 (AVERAGE 3.5)
RECOVERED MAP PURITY (%) 77.7-92.3 (AVERAGE 86.9) 71.6-88.9 (AVERAGE 82.7)


[0291] According to the present invention, during treatment for recovering phosphorus in the form of MAP particulates from sludge, blockings of a particulate separation apparatus such as a liquid cyclone are suppressed, and as a result, effects such as an improvement in the stability of the treatment and acquisition of MAP having a high degree of purity can be obtained. The present invention may be applied not only to treatment for recovering phosphorus in the form of MAP particulates from sludge, but also to the separation and recovery of various types of crystal from various types of waste water.


Claims

1. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a liquid cyclone for separating said crystals from said sludge or said separated water introduced into said liquid cyclone; and

a return pipe A for returning an overflow from said liquid cyclone to a supplying portion of said sludge or said separated water.


 
2. The crystal separation apparatus according to claim 1, further comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water provided upstream of said liquid cyclone, and

a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclone to said crystallization reactor.


 
3. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water;

a liquid cyclone for separating said crystals from said sludge or said separated water introduced into said liquid cyclone after being treated by said crystallization reactor; and

a return pipe C for returning an overflow from said liquid cyclone to said crystallization reactor.


 
4. The crystal separation apparatus according to claim 3, further comprising a return pipe A for returning said overflow from said liquid cyclone to a supplying portion of said sludge or said separated water.
 
5. The crystal separation apparatus according to claim 3 or 4, further comprising a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclone to said crystallization reactor.
 
6. The crystal separation apparatus according to any one of claims 2 to 5, further comprising discharge pipe for discharging said crystals from the bottom of said crystallization reactor,
wherein, when a feed rate of said sludge or raw water to be supplied to said crystallization reactor is Q1, a feed rate of said chemical to be added to said crystallization reactor is Q2, a feed rate of said crystals separated or concentrated by said liquid cyclone to be returned to said crystallization reactor is Q3, and a feed rate of said crystals to be discharged by said discharge pipe is Q4, Q1+Q2+Q3<Q4.
 
7. The crystal separation apparatus according to any one of claims 2 to 6, wherein a horizontal cross section of the bottom of said crystallization reactor is smaller than a horizontal cross section of the upper end of said crystallization reactor.
 
8. The crystal separation apparatus according to any one of claims 1 to 7, wherein a recovery pipe for recovering said crystals separated or concentrated by said liquid cyclone is connected to the bottom of said liquid cyclone.
 
9. The crystal separation apparatus according to any one of claims 2 to 8, wherein a washing pipe for washing said liquid cyclone is connected to said return pipe B or said recovery pipe.
 
10. A crystal separation apparatus for separating crystals from sludge, or from separated water generated in a sludge concentration process or a sludge dewatering process, comprising:

a crystallization reactor for precipitating said crystals by adding a chemical to said sludge or said separated water;

a plurality of liquid cyclones arranged in parallel for separating said crystals from said sludge or said separated water introduced into said liquid cyclones after being treated by said crystallization reactor; and

a return pipe B for returning all or a part of said crystals separated or concentrated by said liquid cyclones to said crystallization reactor.


 
11. The crystal separation apparatus according to claim 10, further comprising:

a flow meter for measuring a flow rate of said sludge or said separated water installed in a pipe for introducing said sludge or said separated water into said crystallization reactor, and

means for determining a number of liquid cyclones to be operated from a measured value of said flow meter and a predetermined relationship between a flow rate range and a number of operational liquid cyclones.


 
12. The crystal separation apparatus according to claim 10, further comprising:

a sludge concentration meter installed in said crystallization reactor, and

means for determining a number of liquid cyclones to be operated according to a detected value of said sludge concentration meter.


 
13. The crystal separation apparatus according to claim 10, further comprising:'

means for monitoring a phosphorus concentration and a pH (hydrogen ion concentration) value of said sludge or said separated water treated by said crystallization reactor and said liquid cyclones;

means for calculating a supersaturation ratio from said phosphorus concentration and said pH value measured by said monitoring means; and

means for determining a feed rate of magnesium to be added and a number of liquid cyclones to be operated according to said supersaturation ratio.


 
14. A digested sludge treatment apparatus for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising:

an apparatus for decarbonating said digested sludge;

a removal apparatus for removing screen residues from said digested sludge; and

an apparatus for separating or concentrating crystals containing magnesium ammonium phosphate from said digested sludge after said digested sludge is treated by said decarbonation apparatus and said removal apparatus.


 
15. A digested sludge treatment apparatus for treating digested sludge generated by subjecting organic wastes to anaerobic digestion, comprising:

a crystallization reactor for precipitating magnesium ammonium phosphate from said digested sludge;

a removal apparatus for removing screen residues from said digested sludge; and

an apparatus for separating or concentrating crystals containing magnesium ammonium phosphate from said digested sludge after said digested sludge is treated by said crystallization reactor and said screen residue removal apparatus.


 
16. The digested sludge treatment apparatus according to Claim 14 or 15, wherein said removal apparatus is a wet-type vibrating screen equipped with two or more types of sieve bodies having different openings.
 
17. The digested sludge treatment apparatus according to any one of Claims 14 to 16, further comprising an apparatus for washing the separated crystals containing magnesium ammonium phosphate.
 




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Cited references

REFERENCES CITED IN THE DESCRIPTION



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Patent documents cited in the description