(19)
(11)EP 1 212 379 B1

(12)EUROPEAN PATENT SPECIFICATION

(45)Mention of the grant of the patent:
11.02.2004 Bulletin 2004/07

(21)Application number: 00982602.5

(22)Date of filing:  13.09.2000
(51)Int. Cl.7C09B 67/10, B29B 7/00
(86)International application number:
PCT/US2000/040884
(87)International publication number:
WO 2001/019926 (22.03.2001 Gazette  2001/12)

(54)

PROCESS FOR PREPARING PIGMENT FLUSH

VERFAHREN ZUR HERSTELLUNG VON EINEM PIGMENTFLUSH

PREPARATION DE PIGMENTS PAR PIGMENT FLUSH


(84)Designated Contracting States:
AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

(30)Priority: 17.09.1999 US 397801

(43)Date of publication of application:
12.06.2002 Bulletin 2002/24

(73)Proprietor: Flint Ink Corporation
Ann Arbor, MI 48105-2773 (US)

(72)Inventors:
  • AFFELDT, Donald, C.
    Warren, MI 48091 (US)
  • CUNIGAN, Robert, John
    Elizabethtown, KY 42701 (US)
  • PRICE, Joseph, B.
    Birmingham, MI 48009 (US)

(74)Representative: Lind, Urban et al
Awapatent AB, P.O. Box 11394
404 28 Göteborg
404 28 Göteborg (SE)


(56)References cited: : 
EP-A- 0 255 667
US-A- 4 309 223
US-A- 4 747 882
DE-A- 2 437 510
US-A- 4 474 473
US-A- 5 151 026
  
      
    Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


    Description

    FIELD OF THE INVENTION



    [0001] The present invention relates to processes for preparing pigment flushes, particularly pigment flushes for ink compositions. The present invention also relates to methods for preparing ink bases and finished ink compositions.

    BACKGROUND OF THE INVENTION



    [0002] Syntheses of many organic pigments include a coupling step in a dilute aqueous medium to produce a slurry of the pigment product, which is typically followed by filtering the slurry in a filter press to concentrate the pigment. The press cake that results is then either dried to provide a dry, particulate pigment or else is "flushed" with an organic medium such as an oil and/or resin to transfer the pigment particles from the aqueous press cake to the oil or resin phase. Flushing assists in keeping pigment particles non-agglomerated and easier to use in making inks or coatings. The flushing process requires additional time and materials over simply drying the pigment. If the pigment is used in an ink or coating composition, however, it must first be well-dispersed in an appropriate organic medium in order to achieve the desired color development and stability, and thus the flushing process is advantageous because it accomplishes the transfer without intermediate steps of drying the pigment and grinding the pigment in the organic medium to produce the pigment dispersion.

    [0003] In the past, pigment flushes have usually been prepared by batch processes in which the press cake is kneaded with an organic phase such as an oil and/or a resin, for example in a sigma blade mixer or dough mixer, to flush the pigment particles from the water phase to the organic medium phase and displace the water as a separate aqueous phase. The displaced water is separated and the dispersion of the pigment in the varnish can be used as a pigment paste in preparing an ink or paint.

    [0004] The batch process has many shortcomings. First, the steps of adding varnish, kneading the dough to displace the water, and pouring off the water must usually be repeated a number of times in order to obtain the optimum yield and a product with the desired low water content. This is a labor-intensive process that requires careful monitoring. Further, in order to remove the residual water, the batch must be further treated, such as by heating and stripping under vacuum. For many pigments, the heat history from processing to remove the residual water may result in a color shift. Further, the process is time-consuming and inefficient. Finally, it is difficult to reduce the water content below about 3% by weight, even with the vacuum stripping.

    [0005] Continuous flush processes have been suggested in the past, but those processes have also had shortcomings. Higuchi et al., U.S. Patent No. 4,474,473, describe a process for continuously flushing pigment press cake on equipment that includes a co-rotating, twin screw extruder. The process requires a press cake that has a pigment content of 35 weight percent or more. The '473 patent discloses that press cakes having a pigment content of from 15 to 35 weight percent cannot be used in the continuous process because of problems with obtaining constant flow feeding. The range of 15 to 35 weight percent, however, is the range of pigment content that is typically obtained for press cakes. While dilution of the press cake with water to form a liquid slurry of low pigment content was previously suggested, the '473 patent takes the opposite direction of increasing pigment content to 35% or more to provide a "lump cake" that is apparently suitable for constant flow feeding as a free-flowing solid. Increasing the pigment content of the manufactured press cake, however, requires a time-consuming process of shaping the press cake and drying it with circulating air until the desired water content is obtained.

    [0006] An example of the methods using diluted press cake is Rouwhorst et al., U.S. Patent No. 4,309,223. This patent discloses a process of preparing a pigment flush from a press cake using a single screw extruder. The process uses a slurry containing only about 0.5% to 10% by weight pigment. When so much water is added during the flushing process it is difficult to get a clean break or separation between the phases. In addition, more aqueous waste is produced. Finally, it is often the case that the single screw extruder does not provide a sufficient amount of mixing shear to adequately flush the press cake.

    [0007] Document EP 0 255 667 also relates to a method and equipment for manufacturing pigment dispersion in a continuous process. It is stated that both fluid pigment slurry as well as compact press cakes could be used, with a water content in the range of 20-90%. When press cakes with thoxotropic flow properties are used, it is proposed to use an additional pump or extruder segment for the feeding of the press cakes. However, this scheme does not provide a sufficient solution for the feeding problem, since the filter cake will still not flow in to the entrance of the extruder segment or into the inlet of the pump.

    [0008] Anderson et al., U.S. Patent No. 5,151,026, discloses an extruder apparatus for removing liquid from an aqueous mass of comminuted solids such as crumb rubber, wood pulp, and ground plastic materials that are cleansed during recycling processes. The water is squeezed out of the aqueous mass in a pinch point. The pinch point pressure results from applying a backward force by means of a reverse-threaded section of the screw immediately at the liquid extraction location. The Anderson process removes from water relatively large solid pieces that do not appear to associate or agglomerate. Unlike the Anderson process, the pigment flush process concerns transfer of fine pigment particles from aqueous press cake to an organic phase, usually including a resin, followed by separation of the two liquid phases (aqueous and organic). Two key considerations in the flush process are clean separation of the organic and aqueous phases and good dispersion of the pigment particles. The pinch point method is unsuitable for the two-phase pigment flushing process because the pinching force would interfere with the necessary phase separation between aqueous and organic phases. The pigment particles also have a tendency to agglomerate. The pinch point would thus be unsuitable for the additional reason that squeezing the pigment would cause undesirable agglomeration of the pigment particles, which would in turn impair dispersion of the pigment.

    SUMMARY OF THE INVENTION



    [0009] The invention provides a process for continuous production of pigment flush from conventional press cake. In a first step, at least one pigment press cake is homogenized to a fluidized mass. In a second step, the homogenized press cake is fed at a controlled rate into a twin screw extruder. The twin screw extruder may receive more than one stream of fluidized press cake. An organic medium, which may include organic components selected from solvent, varnish, oil, and/or resin, is also fed into the extruder, and the press cake and organic medium are mixed in a first zone of the extruder to wet the pigment with the organic medium, displacing water from the press cake and producing a crude pigment flush. The displaced water is removed in a second zone of the extruder. The second zone of the extruder includes a port for removing the displaced water, especially by draining the water, and preferably includes a dam that retains the pigment flush in the second zone for a time sufficient to allow most of the displaced water to be removed from the crude flush mass. The extruder preferably includes a third zone that has one or more vacuum ports to draw off residual water clinging to the pigment flush.

    [0010] The invention also provides a method for continuous production of an ink base or a finished ink from a pigment press cake. The method includes the steps just outlined for the process of the invention for producing a pigment flush and at least one an additional step of introducing into the extruder, at some point before the pigment dispersion is discharged, preferably after the optional vacuum zone, one or more additional ink components, such as a varnish, pigmented tinting or toning compositions, solvent, and/or additives, to make an ink base or a finished ink composition.

    [0011] The invention further provides an apparatus that includes a press cake feed system and a twin screw extruder. The press cake feed system is used to fluidize the press cake and feed the fluidized press cake to the extruder. The press cake feed system applies shear to the press cake to convert the crumbly, agglomerating material into a smooth, fluid dispersion. The feed system then transfers the fluidized press cake to the twin screw extruder. The twin screw extruder of the apparatus has at least two zones. In a first zone, the fluidized press cake and an organic medium are fed into the extruder and mixed. The action of the first zone transfers the pigment to the organic medium and produces a separate water phase. In a second zone of the extruder, the water phase is at least partially removed. In an optional third zone, a residual portion of water is removed from the pigment flush by vacuum. The extruder may also optionally have a fourth zone with at least one addition port by which additional ingredients are added and which provides additional mixing to prepare an ink base or finished ink composition.

    [0012] The invention offers an advantage over previous processes in that it provides continuous processing of conventional press cakes. Press cakes are usually prepared having pigment contents of from about 15% to about 35%. Because the present invention can process press cakes as prepared, it is possible to eliminate a cumbersome preliminary evaporation step to increase pigment content of the press cake to the point at which the press cake can be flushed or a diluting step in which the press cake is reduced to a very low solids slurry for processing using the prior art methods.

    [0013] The invention offers a further advantage of providing more control for a continuous flushing process, which results in increased consistency of color and other properties of the pigment dispersion.

    [0014] The invention offers a still further advantage of providing a continuous process for manufacturing ink base or a finished ink product from a continuous feed of conventional press cake.

    BRIEF DESCRIPTION OF THE DRAWINGS



    [0015] 

    FIG. 1 is a schematic diagram of one embodiment of the press cake feed system of the invention.

    FIG. 2 is a schematic diagram of an alternative embodiment of the press cake feed system of the invention.

    FIG. 3 is a schematic diagram of one embodiment of the twin screw extruder of the present invention.

    FIG. 4 is a partial schematic view of the water separation zone of the invention.

    FIG. 5 is a partial schematic view of an alternative embodiment of the extruder showing the fourth zone.


    DETAILED DESCRIPTION



    [0016] The invention provides a process in which a pigment in press cake form is flushed by transferring the pigment particles from the aqueous press cake to an organic medium, especially to an oil or resin phase. The press cake may be from the synthesis of any of a number of organic pigments. Examples of suitable press cakes include, without limitation, press cakes of diarrylide yellow pigments (e.g., Pigment Yellow 12), phthalocyanine pigments, calcium lithol red, alkali blue, barium lithol red, rhodamine yellow, rhodamine blue, and so on. Press cakes of organic pigments typically have a water content by weight of from about 12% to about 30%, although press cakes such as those of certain blue pigments may have a water content as high as 45%.

    [0017] The invention further provides an apparatus that includes at least one press cake feed system, a preferred embodiment of which is shown in FIG. 1, and a twin screw extruder, a preferred embodiment of which is shown in FIG. 3. The press cake feed system fluidizes the press cake and feeds the fluidized press cake to the twin screw extruder. The press cake feed system may include two components that carry out these actions, a fluidizing component such as 1 in FIG. 1 and a feed component such as 2 in FIG. 1. The fluidizing component applies shear to the press cake to break up the bridging between the individual particles that gives the press cake its pasty or plaster-like consistency. The amount of shear is sufficient to produce a fluidized press cake. The amount of shear should not be excessive, as too much shear will beat air into the fluidized press cake, making it difficult again to feed into the extruder. Suitable examples of the fluidizing component are, without limitation, a ribbon mixer, a paddle mixer, an auger screw, and a helical mixer. FIG 1 shows as one preferred embodiment of the fluidizing component a paddle mixer 3 driven by motor 13. Paddle mixer 3 shows ten paddle mixing elements 4, but the size of the paddle mixer and the number of mixing elements can be varied widely to suit the particular situation, such as the desired throughput of the continuous process. Scrapers 10 may be included to scrape the walls and keep the press cake inside the mixer. If necessary, the mixer may be cooled with the aid of a cooling jacket (not shown), by air cooling, or otherwise.

    [0018] The fluidizing component has a orifice 5 through which the fluidized press cake exits the fluidizing component. The fluidized press cake may be discharged from the fluidizing component by pushing the fluidized press cake through the orifice with a valve 6, as is shown in FIG. 1, to control the flow of fluidized press cake from the fluidizing component. Alternatively, the fluidized press cake may be drawn from the fluidizing component with vacuum or pumped from the fluidizing component. In a preferred embodiment, the fluidized press cake is fed into a holding tank 7 as shown in FIG. 1. Holding tank 7 is equipped with a blade 8 that rotates along the perimeter and serves both to prevent re-bridging between the pigment particles of the fluidized press cake and to aid in feeding the press cake to feed pump 9. Feed pump 9 provides fluidized press cake to the extruder. Holding tank 7 allows the fluidizing operation taking place in paddle mixer 3 to be carried out in a batch or semi-batch manner, with all or part of the fluidized press cake in the mixer being emptied to the holding tank at intervals. Thus, press cake can be fluidized in a batch method with a portion of press cake being introduced to the mixer, mixed until fluidized, then the fluidized portion passed on to the holding tank. The mixer may then be charged with a new batch of press cake, which is fluidized. The fluidized press cake may be immediately introduced to the holding tank or held in the mixer for a desired time and then introduced to the holding tank. Alternatively, a semi-batch process may be employed in which at certain intervals a part of the fluidized press cake is passed from the mixer to the holding tank, after which additional press cake is added to the material remaining in the mixer.

    [0019] It is also possible to forego the holding tank in the press cake fluidizing component. In this embodiment (not shown), the fluidized press cake is passed at a continuous rate from the mixer through the pump to the extruder. In this embodiment of the invention, new press cake is fed into the mixer at a rate sufficient to insure that the mixer does not empty and that the average dwell time of the press cake in the mixer is adequate to fluidize the press cake.

    [0020] The feed component of the press cake feed system feeds the fluidized press cake to the extruder. Preferably, the feed component includes a pump. The pump may be any type suitable for the viscosity of the fluidized press cake. Examples of suitable pumps include, without limitation, lobe pumps, gear pumps, or other positive displacement pumps.

    [0021] In the alternative preferred embodiment shown in FIG. 2, the press cake feed system has a fluidizing component that includes a conical container 101 that preferably rotates by gear 102 driven by motor 111 and a stationary two-screw auger 103 (front screw shown) with motor 113 that applies shear to the press cake. The press cake is fluidized by the action of the two-screw auger. The auger also serves to convey the fluidized press cake to an orifice 105 at the bottom of the conical container. The fluidized press cake expelled from the orifice is fed to the extruder, again for example by pump 109, with or without a holding tank for the fluidized material, as in the first embodiment.

    [0022] The feed component introduces the fluidized press cake to port 19 at the beginning of an extruder shown in the preferred example of FIG. 3. The extruder has at least two zones, and optionally has a third and/or a fourth zone. In a first zone, represented in the figure by sections 1 through 5, the fluidized press cake and organic medium are fed into the extruder and then mixed to flush the pigment from the aqueous phase to the organic phase. In a second zone, represented by sections 6 through 8, at least a portion the water displaced during the flushing operation is removed by draining or drawing the liquid from the extruder. In a third zone, which is optional but preferred, represented by sections 9 through 11, residual water is removed (as water vapor) by vacuum dehydrating the pigment flush through one or more vacuum ports. In the fourth zone, also optional, represented by sections 12 through 14, the flush is further mixed and one or more other ink components may be added and mixed with the pigment flush. The optional fourth zone can be used to produce an ink base or finished ink composition product.

    [0023] The extruder is a twin-screw extruder, with the screws being driven by motor 18. The screws are preferably co-rotating. At least one fluidized press cake is fed into the extruder through port 19. In one preferred embodiment, a second fluidized press cake is fed into the extruder through a port 19 or through a second port 119. A liquid organic medium, preferably including at least an oil, a resin, or resin solution, is also fed into the extruder, which may be through port 19 or through a second port 119. The liquid organic medium is sufficiently hydrophobic to allow a non-aqueous phase to form in the process. Types of organic materials that are suitable to prepare pigment are well-known in the art. If the extruder has two different fluidized press cake feeds by ports 19 and 119, the organic medium may be fed through either or through yet another separate port.

    [0024] Typical kinds of resins and oils that may be used for flushing varnishes include, without limitation, alkyd resins, phenolic resins, polyesters, hydrocarbon resins, maleic resins, rosin-modified varnishes of any of these, polyamide resins, polyvinyl chloride resins, vinyl acetate resins, vinyl chloride/vinyl acetate copolymer resins, chlorinated polyolefins, polystyrene resins, acrylic resins, polyurethane resins, ketone resins, vegetable oils including linseed oil, soybean oil, neatsfoot oil, coconut oil, tung oil, mineral oils, and so on. Combinations of such resins and oils may also be employed. The resin, oil, or combination thereof may be combined with a hydrophobic organic solvent or liquid, including high boiling petroleum distillates.

    [0025] As mentioned, the organic medium may be introduced in the same barrel, or section, of the extruder as the fluidized press cake, whether in the same port or a different port. Alternatively, the organic medium may be introduced in another section close to the front of the extruder in the first zone, as shown in FIG. 3 by the port 119. The organic medium may be fed from a line or tank, which may have a stirrer, and may be metered in with, for example, a pump. Preferably, the organic medium and the fluidized press cake are each introduced at fairly constant rates. The relative amounts of the organic medium and the fluidized press cake for optimum processing can be determined based upon the particular materials chosen, but in general the amounts remain the same as those expected for conventional batch processing. For example, the amount of organic medium introduced per unit of time may be from about 0.6 to about 2 times the amount of solid pigment introduced in the same unit of time. The ratio of organic medium to solid pigment may be adjusted according to factors known in the art, such as the type of pigment and the type of organic medium.

    [0026] The fluidized press cake and organic medium are mixed in one or more sections of the first zone of the extruder to wet the pigment with the organic medium, displacing water from the press cake and producing a crude pigment flush. A special screw section with a plurality of kneading disks may be used in the first zone where the flushing takes place. In one preferred embodiment of the invention, the screw profile in the first zone tapers from a deep channel used in the section or sections having a feeding port gradually to a shallow channel in a later (downstream) section or section of the first zone. The length of the first zone of the extruder in which the fluidized press cake and the organic medium are mixed is sufficiently long so that the pigment is flushed completely. The rotational speed of the screw also is a factor for efficient flushing. A preferred range for rotational speed of the screw is from about 150 to about 550 rpm, and a more preferred range for rotational speed is from about 450 to about 550 rpm.

    [0027] The displaced water and the crude pigment flush continue in the extruder to the second zone of the extruder where at least a portion of the displaced water is removed. In the second zone, preferably a major portion of the displaced water is removed, more preferably at least about 80%, still more preferably at least about 90%, and even more preferably all but a residual amount of water that clings to the pigment flush is removed. Referring to FIG. 3, the second zone of the extruder includes sections 6-8. The second zone of the extruder includes a port or vent 20 for removing, preferably by draining off, the displaced water. While the water may be withdrawn by other means, gravity draining is the simplest and is therefore preferred. The port 20 shown in the figure is connected on the other side to a section 21 having therein a screw turned by motor 22 that drives the relatively viscous pigment-containing flush back into the section 6 while letting the water drain out of section 6. Collected water is drained via valve 23.

    [0028] One important feature of the second zone is a dam that retains the pigment flush for a time sufficient to allow most of the displaced water to drain from the crude flush mass. The dam causes the kneaded press cake / organic medium to dwell over the port long enough to allow more of the displaced water to drain from the kneaded pigment. A portion of the mixture of press cake and organic medium is carried into the dammed section of the extruder and remains in that section until the portion works its way out of the pocket of retained material and is carried into the next section by the grabbing action of the screw. The dam is shown in more detail in FIG. 4. FIG. 4 shows the screw sections in sections 6 to 8 of the second zone. The features of section 6 are the port 20, side section 21 (shown in part) containing screw 121, and screw section 130. Screw section 130 has relatively tight threads to remove material from the mixing zone. Screw sections 131 and 132 in marked barrels 6 and 7a have threads that are less tight to increase residence time and allow open room for water to drain. The screw sections designated by 133 are reverse threaded in a tight thread to provide sufficient reverse flow to cause the material to fill a section of 7a (for example, about 30 mm). The reverse flow force that causes the damming effect is limited so that there is no squeezing, as squeezing would tend to produce an emulsion of the aqueous and organic phases, impairing the desired separation of water from organic phase. Because the draining port 20 is relatively far upstream from the reverse screws, the effect of the reverse flow is to cause material to accumulate before eventually flowing over the created dam and/or being pulled on by forward-turning screws located further downstream. The water is not engaged by the forward screws and does not flow over the accumulated material. Instead, the water is held in the second zone to drain.

    [0029] Because more of the water is drained from the flush in a liquid phase instead of being evaporated, as compared to prior methods, the final product contains a lower concentration of salts. The dam thus improves the purity of the product.

    [0030] The third zone of the extruder, which is optional but preferred, includes one or more vacuum ports 24 connected to vacuum at valves 25 to draw off residual water clinging to the pigment flush. The water is drawn off as water vapor. Suitable vacuum ports are known to be used with extruders and typically can include a section 26 containing a screw turned by motor 27 in the vacuum port to help retain the flush in the extruder. A vacuum pump is typically connected to the vacuum port to provide the reduced pressure. The profile of the screw used for the vacuum section preferably has a shallow channel, which tends to increase the efficiency of vacuum dehydration by shaping the material in a thin layer form. FIG. 3 shows identical vacuum ports on consecutive extruder sections.

    [0031] The present process is particularly advantageous for preparing flushes of pigments that are heat-sensitive, including, without limitation, diarrylide and rhodamine pigments such as diarrylide yellow, rhodamine yellow, and rhodamine blue. Because the time during which the pigment is exposed to higher temperatures is minimized by the process of the invention, pigments that may discolor when exposed to heat may be made more reproducibly and without significant color degradation.

    [0032] The pigment flush produced by the inventive process may be used to prepare an ink composition according to usual methods. Additional resins, oils, solvents or other components of the organic medium may be added after the vacuum port to adjust the composition of the pigment flush. FIG. 5 shows an alternative fourth zone having ports 130 and 131 for addition of one or more further materials.

    [0033] Alternatively, the pigment flush may be made into an ink base or a finished ink composition as a further step of the continuous process of the invention by introducing additional materials such as varnish, other resins, organic solvent and/or additives into the extruder at some point before the pigment flush is discharged, preferably after the vacuum zone, such as into port 130 or port 131. The flushed pigment dispersion and other ink component(s) are combined in the extruder so that the output from the extruder is an ink base or ink composition. Typical resins used as ink varnishes that may be added include, without limitation, alkyd resins, polyesters, phenolic resins, rosins, cellulosics, and derivatives of these such as rosin-modified phenolics, phenolic-modified rosins, hydrocarbon-modified rosins, maleic modified rosin, fumaric modified rosins; hydrocarbon resins, vinyl resins including acrylic resins, polyvinyl chloride resins, vinyl acetate resins, polystyrene, and copolymers thereof; polyurethanes, polyamide resins, and so on. Combinations of such resins may also be employed. Suitable example of organic solvents that may be added include, without limitation, aliphatic hydrocarbons such as petroleum distillate fractions and normal and isoparaffinic solvents with limited aromatic character. Any of the many additives known in the art that may be included in the ink compositions of the invention, so long as such additives do not significantly detract from the benefits of the present invention. Illustrative examples of these include, without limitation, pour point depressants, surfactants, wetting agents, waxes, emulsifying agents and dispersing agents, defoamers, antioxidants, UV absorbers, dryers (e.g., for formulations containing vegetable oils), flow agents and other rheology modifiers, gloss enhancers, and anti-settling agents. When included, additives are typically included in amounts of at least about 0.001% of the ink composition, and the additives may be included in amounts of up to about 7% by weight or more of the ink composition.

    [0034] The invention is illustrated by the following example. The example is merely illustrative and does not in any way limit the scope of the invention as described and claimed. All parts are parts by weight unless otherwise noted.

    Example of the Invention



    [0035] A twin screw co-rotating extruder with a screw diameter of 44mm, L/D of 56, and a speed of 450 rpm was used to produce the pigment flush. The table below summarizes the addition points, rates and temperatures of the extruder depicted in FIG. 3.
    Barrels123-56-87b-11121314
    Function add add mixing water break vacuum dehydration mixing let down mixing
    Feed wet cake, alkyd varnish - - - - varnish and oil -
    Jacket none heat heat heat heat heat cool cool
    Temp - - 99 C (210 F) - 102 C (215 F) 127 C (260 F) - 60 C (140 F)


    [0036] First, a 22% lithol rubine press cake was fluidized to a homogenous mixture in a 5 hp ribbon mixer. After mixing, the fluidized press cake was put into a feeder (a 25 hp helical mixer). The fluidized press cake was fed at 56 kg/h (124 lbs/hr) using a gear pump, through a mass flow meter and into barrel 1. The alkyd varnish was feed at 3,2 kg/h (7 lbs/hr) into barrel 1 using a gear pump. A first hydrocarbon varnish was charged into barrel 2 at 13 kg/h (29 lbs/hr). This mass was then mixed through the end of barrel 5.

    [0037] The water was drained from the pigment/varnish mass in barrels 6-8. The water was fairly clear and exited at 99°C (210°F). Barrels 7b-11 were the vacuum dehydration zone. Vacuum ports were installed at barrels 9 and 11.

    [0038] The flush was further mixed in Section 12. In Section 13, the pigment flush was reduced by addition of 5 kg/h (11 lbs/hr) of a hydrocarbon varnish and 1,5 kg/h (3.3 lbs/hr) of a hydrocarbon oil and allowed to cool. The pigment flush, hydrocarbon varnish and hydrocarbon oil were further mixed and cooled in Section 14. The resulting product was a shade converted flush with less than 2% water content. \


    Claims

    1. An apparatus, comprising
       a press cake feed system, wherein said press cake feed system includes a shear component for fluidizing a press cake and a feed component for feeding the fluidized press cake;
       a twin screw extruder connected to the feed component, wherein said twin screw extruder includes
          a first zone with a port that receives the fluidized press cake from the feed component and mixes the fluidized press cake with an organic medium; and
          a second zone downstream of the first zone comprising an outlet for at least partially removing the water phase.
     
    2. An apparatus according to claim 1, wherein said extruder further includes a third zone downstream of the second zone comprising at least one vacuum port.
     
    3. An apparatus according to claim 1, wherein said second zone comprises a partial dam that impedes the progress of the pigment flush out of the second zone for a desired time.
     
    4. An apparatus according to claim 3, wherein said partial dam comprises a reverse threaded screw section.
     
    5. An apparatus according to claim 1, wherein said first zone includes a plurality of kneading disks.
     
    6. An apparatus according to claim 2, wherein the twin screw extruder further comprises a fourth zone downstream of the third zone that includes at least one addition port.
     
    7. An apparatus according to claim 1, wherein the apparatus includes more than one press cake feed systems, each connecting to a port in the first zone.
     
    8. An apparatus according to claim 7, wherein each press cake feed system connects to the same port in the first zone.
     
    9. An apparatus according to claim 7, wherein each press cake feed system connects to a different port in the first zone.
     
    10. An apparatus according to claim 1, wherein the press cake feed system further comprises a reservoir for maintaining the fluidized press cake upstream of the feed component.
     
    11. A process for continuous flush of a pigment press cake, comprising steps of:

    (a) applying shear to the press cake to produce a fluidized press cake;

    (b) continuously feeding the fluidized press cake into a twin screw extruder;

    (c) mixing the fluidized press cake with a liquid organic medium in the extruder to produce an organic flush phase and a water phase; and

    (d) removing at least part of the water phase from the extruder through one or more ports of the extruder.


     
    12. A process according to claim 11, wherein the press cake has about 15 to about 35 percent by weight of pigment.
     
    13. A process according to claim 11, wherein the press cake has up to about 45% by weight pigment.
     
    14. A process according to claim 11, wherein the feeding of step (a) is carried out at a substantially constant rate.
     
    15. A process according to claim 11, wherein the fluidized press cake from step (a) is conveyed to a reservoir and the fluidized press cake is continuously fed in step (c) from said reservoir.
     
    16. An process for continuous flush of a pigment press cake, comprising steps of:

    (a) fluidizing an aqueous pigment press cake to produce a fluidized pigment press cake;

    (b) feeding the fluidized pigment press cake and a hydrophobic organic medium into a first zone of a twin screw extruder having rotating adjacent parallel screws to move the contents of the extruder downstream;

    (c) kneading said fluidized pigment press cake and said organic medium between the pair of screws to flush pigment from the water phase into the organic medium;

    (c) moving the water phase and pigment flush of the pigment in the organic medium downstream to a second zone in which a majority of the water phase is removed through at least one vent, said second zone including an impediment to downstream movement causing the contents of the extruder to dwell in the separation section for a desired period of time.


     
    17. A process according to claim 16, further comprising a step:

    (d) applying vacuum downstream of the second zone to remove a residual portion of water from the pigment flush.


     
    18. A process according to claim 17, wherein the vacuum of step (d) is applied through two or more vacuum ports in the extruder.
     
    19. A process according to claim 16, wherein the screws are rotated at from about 150 to about 550 rpm.
     
    20. A process of preparing an ink product, comprising steps of:

    (a) applying shear to a pigment press cake to produce a fluidized press cake;

    (b) continuously feeding fluidized press cake to a twin screw extruder;

    (c) mixing the fluidized press cake with a liquid organic medium in the extruder to produce an organic flush phase and a water phase;

    (d) removing the water phase from the extruder through one or more ports of the extruder to produce a pigment flush; and

    (e) mixing the pigment flush with at least one additional material to produce an ink product.


     
    21. A process according to claim 20, wherein the mixing of step (e) is carried out in the extruder.
     
    22. A process according to claim 20, wherein at least one material mixed with the pigment flush in step (e) is selected from the group consisting of ink varnishes, organic solvents, ink additives, and combinations thereof.
     
    23. A process according to claim 20, wherein two different fluidized press cakes are fed to the extruder in step (b).
     


    Ansprüche

    1. Vorrichtung, umfassend
    ein Presskuchen-Zufuhrsystem, wobei Presskuchen-Zufuhrsystem eine Scherkomponente zum Fluidisieren eines Presskuchens und eine Zufuhrkomponente zum Zuführen des fluidisierten Presskuchens beinhaltet;
    einen Doppelschneckenextruder, der an die Zufuhrkomponente angeschlossen ist, wobei der Doppelschneckenextruder Folgendes beinhaltet:

    eine erste Zone mit einem Anschluss, der den fluidisierten Presskuchen von der Zufuhrkomponente erhält und den fluidisierten Presskuchen mit einem organischen Medium mischt; und

    eine zweite Zone stromabwärts von der ersten Zone, umfassend einen Auslass, um die Wasserphase zumindest teilweise zu entfernen.


     
    2. Vorrichtung nach Anspruch 1, wobei der Extruder weiterhin eine dritte Zone stromabwärts von der zweiten Zone enthält, umfassend mindestens einen Vakuumanschluss.
     
    3. Vorrichtung nach Anspruch 1, wobei die zweite Zone einen teilweisen Damm umfasst, der das Weiterkommen des Pigmentflushs aus der zweiten Zone eine gewünschte Zeit lang verhindert.
     
    4. Vorrichtung nach Anspruch 3, wobei der teilweise Damm einen gegenläufigen Schneckenabschnitt umfasst.
     
    5. Vorrichtung nach Anspruch 1, wobei die erste Zone mehrere Knetscheiben umfasst.
     
    6. Vorrichtung nach Anspruch 2, wobei der Doppelschneckenextruder weiterhin eine vierte Zone stromabwärts von der dritten Zone umfasst, die mindestens einen Beimenganschluss aufweist.
     
    7. Vorrichtung nach Anspruch 1, wobei die Vorrichtung mehr als ein Presskuchen-Zufuhrsystem aufweist, von denen jedes an einen Anschluss in der ersten Zone anzuschliessen ist.
     
    8. Vorrichtung nach Anspruch 7, wobei jedes Presskuchen-Zufuhrsystem an denselben Anschluss in der ersten Zone anzuschliessen ist.
     
    9. Vorrichtung nach Anspruch 7, wobei jedes Presskuchen-Zufuhrsystem an einen anderen Anschluss in der ersten Zone anzuschliessen ist.
     
    10. Vorrichtung nach Anspruch 1, wobei das Presskuchen-Zufuhrsystem einen Behälter umfasst, um den fluidisierten Presskuchen stromaufwärts von der Zufuhrkomponente zu halten.
     
    11. Verfahren zum kontinuierlichen Flushen eines Pigmentpresskuchens, das folgende Schritte umfasst:

    (a) Anwenden von Scheren auf den Presskuchen, um einen fluidisierten Presskuchen herzustellen;

    (b) kontinuierliches Zuführen des fluidisierten Presskuchens in einen Doppelschneckenextruder;

    (c) Mischen des fluidisierten Presskuchens mit einem flüssigen organischen Medium in dem Extruder, um eine organische Flushphase und eine Wasserphase herzustellen; und

    (d) Entfernen von mindestens eines Teils der Wasserphase aus dem Extruder durch einen oder mehrere Anschlüsse des Extruders.


     
    12. Verfahren nach Anspruch 11, wobei der Presskuchen ungefähr 15 bis ungefähr 35 Prozent nach Gewicht Pigment hat.
     
    13. Verfahren nach Anspruch 11, wobei der Presskuchen bis zu ungefähr 45 % nach Gewicht Pigment hat.
     
    14. Verfahren nach Anspruch 11, wobei das Zuführen von Schritt (a) bei einer im Wesentlichen konstanten Geschwindigkeit ausgeführt wird.
     
    15. Verfahren nach Anspruch 11, wobei der fluidisierte Presskuchen von Schritt (a) zu einem Behälter befördert wird, und der fluidisierte Presskuchen aus dem Behälter kontinuierlich in Schritt (c) zugeführt wird.
     
    16. Verfahren zum kontinuierlichen Flushen eines Pigmentpresskuchens, das folgende Schritte umfasst:

    (a) Fluidisieren eines wässrigen Pigmentpresskuchens, um einen fluidisierten Pigmentpresskuchen herzustellen;

    (b) Zuführen des fluidisierten Pigmentpresskuchens und eines hydrophoben organischen Mediums in eine erste Zone eines Doppelschneckenextruders, der rotierende benachbarte parallele Schnecken aufweist, um den Inhalt des Extruders stromabwärts zu bewegen;

    (c) Kneten des fluidisierten Pigmentpresskuchens und des organischen Mediums zwischen dem Schneckenpaar, um Pigment von der Wasserphase in das organische Medium zu flushen;

    (c) Bewegen der Wasserphase und des Pigmentflushs des Pigments in das organische Medium stromabwärts zu einer zweiten Zone, in welcher eine Mehrheit der Wasserphase durch mindestens eine Öffnung entfernt wird, wobei die zweite Zone ein Hindernis zu der Stromabwärtsbewegung aufweist, das bewirkt, dass der Inhalt des Extruders eine gewünschte Zeit lang in dem Trennabschnitt verbleibt.


     
    17. Verfahren nach Anspruch 16, des Weiteren umfassend einen Schritt:

    (d) Anwenden von Vakuum stromabwärts von der zweiten Zone, um einen Restanteil von Wasser aus dem Pigmentflush zu entfernen.


     
    18. Verfahren nach Anspruch 17, wobei das Vakuum von Schritt (d) durch zwei oder mehr Vakuumanschlüsse im Extruder angewendet wird.
     
    19. Verfahren nach Anspruch 16, wobei die Schnecken im Bereich von ungefähr 150 bis ungefähr 550 UpM rotieren.
     
    20. Verfahren zum Bereiten eines Farbprodukts, das folgende Schritte umfasst:

    (a) Anwenden von Scheren auf einen Pigmentpresskuchen, um einen fluidisierten Presskuchen herzustellen;

    (b) kontinuierliches Zuführen des fluidisierten Presskuchens in einen Doppelschneckenextruder;

    (c) Mischen des fluidisierten Presskuchens mit einem flüssigen organischen Medium in dem Extruder, um eine organische Flushphase und eine Wasserphase herzustellen;

    (d) Entfernen der Wasserphase aus dem Extruder durch einen oder mehrere Anschlüsse des Extruders, um einen Pigmentflush herzustellen; und

    (e) Mischen des Pigmentflushs mit mindestens einem zusätzlichen Material, um ein Farbprodukt herzustellen.


     
    21. Verfahren nach Anspruch 20, wobei das Mischen von Schritt (e) im Extruder ausgeführt wird.
     
    22. Verfahren nach Anspruch 20, wobei mindestens ein Material. das mit dem Pigmentflush in Schritt (e) gemischt ist, ausgewählt ist aus der Gruppe, bestehend aus Farblacken, organischen Lösungen, Farbadditiven und Kombinationen davon.
     
    23. Verfahren nach Anspruch 20, wobei zwei verschiedene fluidisierte Presskuchen dem Extruder in Schritt (b) zugeführt werden.
     


    Revendications

    1. Appareil comprenant
    un système d'alimentation en gâteau de presse, dans lequel ledit système d'alimentation en gâteau de presse comprend un composant de cisaillement destiné à fluidifier un gâteau de presse et un composant d'alimentation destiné à charger le gâteau de presse fluidifié ;
    une extrudeuse à deux vis connectée au composant d'alimentation, dans lequel ladite extrudeuse à deux vis comprend
    une première zone avec un orifice qui reçoit le gâteau de presse fluidifié du composant d'alimentation et mélange le gâteau de presse fluidifié avec un milieu organique ; et
    une seconde zone en aval de la première zone, comprenant un orifice de sortie destiné à retirer au moins partiellement la phase aqueuse.
     
    2. Appareil selon la revendication 1, dans lequel ladite extrudeuse comprend en outre une troisième zone en aval de la seconde zone, comprenant au moins un orifice d'aspiration.
     
    3. Appareil selon la revendication 1, dans lequel ladite seconde zone comprend un barrage partiel qui empêche la progression du broyage humide de pigment dans une seconde zone pendant une période de temps souhaitée.
     
    4. Appareil selon la revendication 3, dans lequel ledit barrage partiel comprend une section de vis à filetage inverse.
     
    5. Appareil selon la revendication 1, dans lequel ladite première zone comprend une pluralité de disques de malaxage.
     
    6. Appareil selon la revendication 2, dans lequel l'extrudeuse à deux vis comprend en outre une quatrième zone en aval de la troisième zone qui comprend au moins un orifice d'addition.
     
    7. Appareil selon la revendication 1, dans lequel l'appareil comprend un ou plusieurs systèmes d'alimentation en gâteau de presse, chacun se connectant à un orifice dans la première zone.
     
    8. Appareil selon la revendication 7, dans lequel chaque système d'alimentation en gâteau de presse se connecte au même orifice dans la première zone.
     
    9. Appareil selon la revendication 7, dans lequel chaque système d'alimentation en gâteau de presse se connecte à un orifice différent dans la première zone.
     
    10. Appareil selon la revendication 1, dans lequel le système d'alimentation en gâteau de presse comprend en outre un réservoir destiné à maintenir le gâteau de presse fluidifié en amont du composant d'alimentation.
     
    11. Processus de broyage continu par voie humide d'un gâteau de presse de pigment, comprenant les étapes consistant à :

    (a) appliquer un cisaillement au gâteau de presse pour produire un gâteau de presse fluidifié ;

    (b) charger de manière continue le gâteau de presse fluidifié dans une extrudeuse à deux vis ;

    (c) mélanger le gâteau de presse fluidifié avec un milieu organique liquide dans l'extrudeuse pour produire une phase organique de broyage humide et une phase aqueuse ; et

    (d) retirer au moins une partie de la phase aqueuse de l'extrudeuse par un ou plusieurs orifices de l'extrudeuse.


     
    12. Processus selon la revendication 11, dans lequel le gâteau de presse a environ 15 à environ 35 % en poids de pigment.
     
    13. Processus selon la revendication 11, dans lequel le gâteau de presse a jusqu'à environ 45 % en poids de pigment.
     
    14. Processus selon la revendication 11, dans lequel la charge à l'étape (a) est réalisée à une vitesse sensiblement constante.
     
    15. Processus selon la revendication 11, dans lequel le gâteau de presse fluidifié de l'étape (a) est acheminé à un réservoir et le gâteau de presse fluidifié est continuellement chargé à l'étape (c) à partir dudit réservoir.
     
    16. Processus de broyage continu d'un gâteau de presse de pigment comprenant les étapes consistant à :

    (a) fluidifier un gâteau de presse de pigment pour produire un gâteau de presse de pigment fluidifié ;

    (b) charger le gâteau de presse de pigment fluidifié et un milieu organique hydrophobe dans une première zone d'une extrudeuse à deux vis ayant des vis parallèles adjacentes rotatives pour retirer les contenus de l'extrudeuse en aval ;

    (c) malaxer ledit gâteau de presse de pigment fluidifié et ledit milieu organique entre une paire de vis pour transférer le pigment de la phase aqueuse au milieu organique ;

    (d) déplacer la phase aqueuse et le broyage humide de pigment du pigment dans le milieu organique en aval vers une seconde zone dans laquelle une majorité de la phase aqueuse est retirée par au moins un conduit d'évacuation, ladite seconde zone comprenant une entrave au mouvement en aval obligeant le contenu de l'extrudeuse à rester dans la section de séparation pendant une période de temps souhaitée.


     
    17. Processus selon la revendication 16, comprenant en outre l'étape consistant à :

    (e) appliquer un vide en aval de la seconde zone pour aspirer une partie résiduelle d'eau du broyage humide de pigment.


     
    18. Processus selon la revendication 17, dans lequel le vide de l'étape (d) est appliqué par deux orifices d'aspiration ou plus dans l'extrudeuse.
     
    19. Processus selon la revendication 16, dans lequel les vis pivotent à environ 150 à 550 tr/min.
     
    20. Processus de préparation d'un produit d'encre, comprenant les étapes consistant à :

    (a) appliquer un cisaillement à un gâteau de presse de pigment pour produire un gâteau de presse fluidifié ;

    (b) continuellement charger le gâteau de presse fluidifié à une extrudeuse à deux vis ;

    (c) mélanger le gâteau de presse fluidifié avec un milieu organique liquide dans l'extrudeuse pour produire une phase organique de broyage humide et une phase aqueuse ;

    (d) retirer la phase aqueuse de l'extrudeuse par un ou plusieurs orifices de l'extrudeuse pour produire un broyage humide de pigment ; et

    (e) mélanger le broyage humide de pigment à au moins un matériau supplémentaire pour produire un produit d'encre.


     
    21. Processus selon la revendication 20, dans lequel l'étape de mélange (e) est réalisée dans l'extrudeuse.
     
    22. Processus selon la revendication 20, dans lequel au moins un matériau mélangé avec le broyage humide de pigment à l'étape (e) est choisi dans le groupe comprenant les vernis pour encre, les solvants organiques, les additifs pour encre, et des combinaisons de ceux-ci.
     
    23. Processus selon la revendication 20, dans lequel deux différents gâteaux de presse fluidifiés sont chargés à l'extrudeuse dans l'étape (b).
     




    Drawing