(19)
(11)EP 3 242 100 B1

(12)EUROPEAN PATENT SPECIFICATION

(45)Mention of the grant of the patent:
26.06.2019 Bulletin 2019/26

(21)Application number: 17177667.7

(22)Date of filing:  28.10.2013
(51)International Patent Classification (IPC): 
F26B 17/10(2006.01)
F26B 25/10(2006.01)
B01D 1/18(2006.01)
F26B 21/00(2006.01)
F26B 25/18(2006.01)

(54)

A METHOD FOR CONTROLLED CONCENTRATION AND SOLIDS RECOVERY

VERFAHREN ZUR KONTROLLIERTEN KONZENTRATION UND RÜCKGEWINNUNG VON FESTSTOFFEN

MÉTHODE DE CONCENTRATION CONTRÔLÉE ET DE RÉCUPÉRATION DE SOLIDES


(84)Designated Contracting States:
AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

(30)Priority: 01.11.2012 IN 3175MU2012

(43)Date of publication of application:
08.11.2017 Bulletin 2017/45

(62)Application number of the earlier application in accordance with Art. 76 EPC:
13818368.6 / 2914914

(73)Proprietor: Shah, Janak Ramanlal
Mumbai 400 056 Maharashtra (IN)

(72)Inventors:
  • Tiwari, Manoj Shyamnarayan
    421501 Thane, Maharashtra (IN)
  • Shah, Janak Ramanlal
    400 056 Mumbai, Maharashtra (IN)

(74)Representative: Engelhard, Markus 
Boehmert & Boehmert Anwaltspartnerschaft mbB Pettenkoferstrasse 22
80336 München
80336 München (DE)


(56)References cited: : 
JP-A- H05 220 314
JP-A- 2006 266 552
  
      
    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 Invention



    [0001] The present invention relates to a method for one pot solids recovery from solutions, slurries, gels, semisolids, and their like. Further the method can be used for controlled concentration of solutions, slurries, gels, semisolids, and their like. Such a method is known from JP-H-05220314A.

    Background of the Invention



    [0002] Recovery of solids from solutions, slurries, dispersions, emulsions, gels, semisolids, and their like involves the removal of the solvent and / or the carrier medium by diverse processes that involve evaporation, reverse osmosis, ultrafiltration, pervaporation, freeze concentration, clathration etc. Such processes are generally carried out using various types of equipments such as spray driers, drum driers, freeze driers, foam-mat, fluid bed driers, etc.

    [0003] Spray driers are routinely used for recovery of solids from solutions / slurries. Similarly fluid bed driers are routinely used to dry wet solids but cannot be used for recovery of solids from solutions, dispersions, slurries, emulsions, gels, semisolids and their like.

    [0004] The challenges in technologies related to the treatment of solutions, dispersions, slurries, emulsions, gels, semisolids and their like for the recovery of substantially dry solids are in providing cost effective equipments / systems that enable easy to operate energy efficient processes. The present inventions address this technology gap.

    Definition



    [0005] The term "substantially dry solids" when used herein shall mean the "loss on drying" to be less than 10% by weight of the solids, preferably less than 5% by weight of the solids, more preferably less than 2% by weight of the solids and most preferably less than 1% by weight of the solids depending on the type and nature of the material and the method used for its determination.

    Objects of the Invention



    [0006] The main object of the invention is to provide a solid recovery method for the recovery of substantially dry solids from solutions, dispersions, slurries, emulsions, gels, semisolids and their like that enables easy to operate cost effective energy efficient processes.

    [0007] Another object of the invention is to provide a method for a single pot process for the concentration of solutions, slurries, dispersions, emulsions, gels, semisolids, and further substantially drying the solids for their recovery.

    [0008] Another object of the invention is to provide a method to enhance the contact between the liquid phase and the gaseous medium used in the process for effective heat transfer for controlled concentration and / or recovery of substantially dry solids from solutions, slurries, dispersions, emulsions, gels, semisolids, and their like.

    [0009] Yet another object of the invention is to provide a method of using the said system for controlled concentration and / or recovery of substantially dry solids in applications related to foods, nutraceuticals, natural products, pharmaceuticals, chemicals, etc.

    [0010] Thus in accordance with the invention, a method in accordance with claim 1 is provided.

    [0011] The liquid medium (solution / dispersion / emulsion / slurry / gel / semisolid and their like) is filled in the said third container, and pressurized gas (for example air) is made to flow from the base of the said first container through the said first annular space into the said second annular space and further from the passages in the base of the said third container to mix with the liquid medium, causing the solvent to evaporate and further dry the formed solids in the same system for recovery.

    [0012] In an embodiment of the process, the hot pressurized gas such as air of appropriate temperature and humidity may be used depending on the nature of the solvent / carrier in the solution, slurry, gel, dispersion, emulsion, semisolid etc.

    Detailed Description of the Invention



    [0013] Features and advantages of the invention will become apparent in the following detailed description and the preferred embodiments with reference to the accompanying drawings.

    [0014] The schematic of the system used in the method of the invention is illustrated in Figure 1. It comprises of a container module 10, gas pressurizing means 11, expansion chamber 12, filter housing 13, vapor exhaust (extraction) port 14.

    [0015] The schematic of the container module 10 is illustrated in Figure 2. It comprises of first container 1 that is provided with perforated base or perforated gas distribution plate 20 for gas passage. The flow path of the gas such as pressurized air is indicated in the Figure 2 by arrow 21 for better understanding. The second container 2 is disposed in the said first container 1 so as to define first annular space 22 between first and the second container as well as to define space 23 between the base 20 of the said first container and base 24 of the said second container 2.

    [0016] The said first annular space 22 is closed on the top side 25 as illustrated in the Figure 2. The base 24 of the said second container 2 is substantially flat or is provided with a substantially flat plate. The third container 3 is disposed inside the said second container 2 to define second annular cavity / space 26 as well as to define the space 29 between the base 28 of the said third container and the base 24 of the said second container. The said second annular space 26 is closed from top side 27 as illustrated in the Figure 2. The base 28 of the said third container 3 is provided with a set of perforations/ passages or is provided with a gas distribution plate with a set of perforations/ passages.

    [0017] In one of the embodiments, the said first, second and third containers 1, 2 and 3 respectively are of frusto-conical geometry.

    [0018] The base 20 of the said first container 1 is operably connected with the outlet of the gas pressurizing means such as compressor or blower. The said container module 10 is operably connected to the expansion chamber 12 and further to the filter housing 13 as depicted in Figure 1.

    [0019] In operation, the solution/ dispersion/ emulsion / slurry / gel / semisolid and their like is filled in the said third container 3. The pressurized gas flows from the base 20 of the said first container 1 through the said space 23 and further through the first annular space 22 into the said second annular space 26. It further passes from the passages in the base 28 of the said third container 3 to mix with the solution / dispersion/ emulsion / slurry / gel / semisolid and their like, cause the solvent to evaporate and the dry the resulting solids for final recovery.

    [0020] In one of the embodiments, the said third container 3 is provided with a set of inclined passages configured to distribute gas in the bulk of the liquid medium (solution / dispersion/ emulsion / slurry / gel / semisolid and their like) to create turbulence for enhancement of contact between the gas and the liquid medium for improved heat transfer. In one of the variants of this embodiment, the passages are inclined to the horizontal at 15° to 85°, preferably 25° to 75°.

    [0021] One of the configurations of the said passages in the said base 28 is depicted in Figure 3. As an illustration, only quarter of the gas distribution plate is indicated with the configuration of the passages (individual passage is indicated by numeral 50). The said passages may be of any shape such as oval, flat oval, rectangular, circular, square, elliptical, or combinations thereof. The ratio of thickness of the said base 28 to the length of the passage is in the range of 0.250 to 0.999.
    The ratio of total area of the passages to the area of the base is in the range of 0.01 to 0.50, preferably 0.03 to 0.30, more preferably 0.05 to 0.10.

    [0022] In an embodiment of the invention, the said passages are provided with internal serrations to provide swirling motion to the gas passing through it.

    [0023] In yet another embodiment the passages provided in the base of the said third container are of diverse cross section such as round, oval, flat oval, rectangular, square etc.

    [0024] In yet another embodiment plurality of passages are provided on the sides of the said third container.

    [0025] In another embodiment there are more than three containers disposed so as to create more than two annular spaces between them.

    [0026] The invention further provides non-limiting examples.

    Example 1:



    [0027] A solution of 6 kg of sucrose was prepared in 25 kg of water and 5 kg of acetone and filled in third container. The third container was provided with gas distribution plate with passages inclined to the horizontal at 55°. The system was preheated with a stream of hot and dehumidified air. Pressurized hot air was introduced into the system from the bottom of first container and process was run for about 1.5 hours with exhaust kept on to remove the evaporated solvent vapors from the system. The inlet air temperature was about 60°C to 90°C resulting in bed temperature of about 30°C to 55°C and outlet air/vapor temperature of about 30°C to 45°C. The solution gradually got concentrated with the emergence of the solids which got dried as a fluidized bed till the solvent was completely removed and the substantially dry solids were obtained. The solid material was removed and weighed. The yield of the process was 96.3% and the moisture content in the solids was ∼0.7%.

    Example 2:



    [0028] 5 kg of non-pareil seeds was added to 25 kg of purified water. The mixture was stirred to obtain a dispersion which was charged in the third container. The third container was provided with gas distribution plate with passages inclined to the horizontal at 55° The process described in example 1 was carried out. At the end of the process, solid material was removed and weighed. The yield of the process was -95% and the moisture content in the solids was less than 1.5%.

    Example 3:



    [0029] 0.400 kg of starch was added to 1.5 kg of isopropyl alcohol. The mixture was stirred to obtain a dispersion which was filled in third container. The third container was provided with a gas distribution plate with passages inclined to the horizontal at 25°. The system was preheated with a stream of hot and dehumidified air. Pressurized hot air was introduced into the system from the bottom of first container and process was run for about 1 hours with exhaust kept on to remove the evaporated solvent vapors from the system. The inlet air temperature was about 60°C resulting in bed temperature of about 15°C to 55°C and outlet air/vapor temperature of about 20°C to 45°C. The solution gradually got concentrated with the emergence of the solids which got dried as a fluidized bed till the solvent was completely removed and the substantially dry solids were obtained. The solid material was removed and weighed. The yield of the process was ∼81% and the moisture content in the solids was about 5.2 %.

    Example 4:



    [0030] 0.300 kg of povidone K30 was added to 0.13 kg of purified water. The mixture was stirred to obtain a gel. The third container was provided with gas distribution plate with passages inclined to the horizontal at 75°. Purified talc (0.007 kg) was sprinkled (applied) to the inner walls of third container and the upper surface of gas distribution plate. The prepared gel was filled in third container. The system was preheated with a stream of hot remove the evaporated solvent vapors from the system. The inlet air temperature was about 65°C to 85°C resulting in bed temperature of about 35°C to 70°C and outlet air/vapor temperature of about 40°C to 65°C. The solution gradually got concentrated with the emergence of the solids which got dried as a fluidized bed till the solvent was completely removed and the substantially dry solids were obtained. The solid material was removed and weighed. The yield of the process was 90% and the moisture content in the solids was about 2.8%.

    Example 5:



    [0031] 0.400 kg of lactose was added to 4.89 kg of purified water. The mixture was stirred to obtain a solution which was filled in third container. The third container was provided with gas distribution plate with passages inclined to the horizontal at 35°. The system was preheated with a stream of hot and dehumidified air. Pressurized hot air was introduced into the system from the bottom of first container and process was run for about 3.5 hours with exhaust kept on to remove the evaporated solvent vapors from the system. The inlet air temperature was about 45°C to 90°C resulting in bed temperature of about 25°C to 75°C and outlet air/vapor temperature of about 30°C to 60°C. The solution gradually got concentrated with the emergence of the solids which got dried as a fluidized bed till the solvent was completely removed and the substantially dry solids were obtained. The solid material was removed and weighed. The yield of the process was 91.75% and the moisture content in the solids was 0.62%.

    [0032] The invention described demonstrates the effectiveness of the designed systems that enables a one pot solids recovery from solutions, emulsions, dispersions, slurries, gels, semisolids, and their like. Further the equipment and the process can be used for controlled concentration of solutions, slurries, dispersions, emulsion, semisolids, and gels and materials of their like.


    Claims

    1. A method for controlled concentration and/or recovery of substantially dry solids,
    wherein the method comprises:

    a) providing a system for the recovery of substantially dry solids, said system comprising a container module (10), gas pressurizing means (11), vapor extraction means, and optional filters, wherein said container module comprises a first container (1) that is provided with perforated base (20) for passage of pressurized gas, a second container (2) disposed in said first container (1) so as to form a first continuous annular space (22) on the sides as well as to define space (23) between the base (20) of said first container and the base (24) of said second container (2) to enable gas flow,
    wherein said first annular space (22) is closed on the top (25), wherein the base (24) of said second container (2) has a substantially flat bottom, a third container (3) disposed inside said second container (2) to define a second continuous annular space (26) on the sides as well as to define the space (29) between the base of said third container (3) and the base of said second container (2),
    wherein said second annular space (26) is closed from top (27), the base of said third container (3) being provided with perforations or passages;
    the base (20) of said first container (1) is operably connected with the outlet of the pressurized gas source,
    said container module (10) is integrated in a housing (13) with vapor extraction means at the top and an optional filter;

    b) filling a liquid medium selected from solution, dispersion, emulsion, slurry, gel or semisolid into said third container (3);

    c) making a pressurized gas to flow from the base (20) of said first container (1) through said first continuous annular space (22) into said second continuous annular space (26) and further from the passages in the base of said third container (3) to mix with said liquid medium;

    d) causing the solvent to evaporate to concentrate the liquid medium and drying the solids in said system for recovery.


     
    2. The method according to claim 1, wherein the liquid medium is a solution.
     
    3. The method according to claim 1, wherein the liquid medium is a dispersion.
     
    4. The method according to claim 1, wherein the liquid medium is a gel.
     
    5. The method according to any of claims 1 - 4, wherein, by a set of inclined passages in said third container, said pressurized gas is distributed in the bulk of the liquid medium to create turbulence for enhancement of contact between the gas and the liquid medium for improved heat transfer.
     
    6. The method according to any of claims 1 - 5, wherein said gas pressurizing means is a compressor or blower.
     
    7. The method according to any of the foregoing claims, wherein said pressurized gas is air.
     


    Ansprüche

    1. Verfahren zur kontrollierten Aufkonzentrierung und/oder Rückgewinnung von im Wesentlichen trockenen Feststoffen, wobei das Verfahren umfasst:

    a) Bereitstellen eines Systems zur Rückgewinnung von im Wesentlichen trockenen Feststoffen, wobei das System ein Behältermodul (10), Gasdruckmittel (11), Dampfextraktionsmittel und optionale Filter umfasst, wobei das Behältermodul umfasst:

    einen ersten Behälter (1), der mit einer perforierten Basis (20) zum Durchlass von Druckgas versehen ist,

    einen zweiten Behälter (2), der in dem ersten Behälter (1) so angeordnet ist, dass er einen ersten kontinuierlichen ringförmigen Raum (22) an den Seiten bildet und dass er einen Raum (23) zwischen der Basis (20) des ersten Behälters und der Basis (24) des zweiten Behälters (2) definiert, um einen Gasstrom zu ermöglichen,

    wobei der erste ringförmige Raum (22) oben (25) geschlossen ist, wobei die Basis (24) des zweiten Behälters (2) einen im Wesentlichen flachen Boden aufweist, einen dritten Behälter (3), der innerhalb des zweiten Behälters (2) angeordnet ist, um einen zweiten kontinuierlichen ringförmigen Raum (26) an den Seiten zu definieren und um den Raum (29) zwischen der Basis des dritten Behälters (3) und der Basis des zweiten Behälters (2) zu definieren,

    wobei der zweite ringförmige Raum (26) von oben (27) geschlossen ist, wobei die Basis des dritten Behälters (3) mit Perforationen oder Durchlässen versehen ist; die Basis (20) des ersten Behälters (1) funktionsfähig mit dem Auslass der Druckgasquelle verknüpft ist,

    das Behältermodul (10) in ein Gehäuse (13) mit einem Dampfextraktionsmittel oben und einem optionalen Filter integriert ist;

    b) Füllen eines flüssigen Mediums, ausgewählt aus Lösung, Dispersion, Emulsion, Schlamm, Gel oder Halbfeststoff, in den dritten Behälter (3);

    c) Strömenlassen eines Druckgases von der Basis (20) des ersten Behälters (1) durch den ersten kontinuierlichen ringförmigen Raum (22) in den zweiten kontinuierlichen ringförmigen Raum (26) und weiter von den Durchlässen in der Basis des dritten Behälters (3), um sich mit dem flüssigen Medium zu vermischen;

    d) Bewirken des Verdampfens des Lösungsmittels, um das flüssige Medium zu konzentrieren, und Trocknen der Feststoffe in dem System zur Rückgewinnung.


     
    2. Verfahren nach Anspruch 1, wobei das flüssige Medium eine Lösung ist.
     
    3. Verfahren nach Anspruch 1, wobei das flüssige Medium eine Dispersion ist.
     
    4. Verfahren nach Anspruch 1, wobei das flüssige Medium ein Gel ist.
     
    5. Verfahren nach einem der Ansprüche 1 - 4, wobei durch eine Reihe von geneigten Durchlässen in dem dritten Behälter das Druckgas in der Masse des flüssigen Mediums verteilt wird, um Turbulenzen zur Verbesserung des Kontakts zwischen dem Gas und dem flüssigen Medium für eine verbesserte Wärmeübertragung zu erzeugen.
     
    6. Verfahren nach einem der Ansprüche 1 - 5, wobei das Gasdruckmittel ein Kompressor oder Gebläse ist.
     
    7. Verfahren nach einem der vorangehenden Ansprüche, wobei das Druckgas Luft ist.
     


    Revendications

    1. Procédé de concentration contrôlée et/ou de récupération de solides sensiblement secs, dans lequel le procédé comprend :

    a) la fourniture d'un système pour la récupération de solides sensiblement secs, ledit système comprenant un module récipient (10), des moyens de mise sous pression de gaz (11), des moyens d'extraction de vapeur et des filtres optionnels, dans lequel ledit module récipient comprend un premier récipient (1) qui est doté d'une base (20) perforée pour le passage de gaz sous pression, un deuxième récipient (2) disposé dans ledit premier récipient (1) de sorte à former un premier espace annulaire continu (22) sur les côtés ainsi qu'à définir un espace (23) entre la base (20) dudit premier récipient et la base (24) dudit deuxième récipient (2) pour permettre l'écoulement de gaz,
    dans lequel ledit premier espace annulaire (22) est fermé sur le dessus (25), dans lequel la base (24) dudit deuxième récipient (2) a une partie inférieure sensiblement plane, un troisième récipient (3) disposé à l'intérieur dudit deuxième récipient (2) pour définir un second espace annulaire continu (26) sur les côtés ainsi que pour définir un espace (29) entre la base dudit troisième récipient (3) et la base dudit deuxième récipient (2),
    dans lequel ledit second espace annulaire (26) est fermé depuis le dessus (27), la base dudit troisième récipient (3) étant dotée de perforations ou de passages ;
    la base (20) dudit premier récipient (1) est raccordée opérationnellement à l'orifice de sortie de la source de gaz sous pression,
    ledit module récipient (10) est intégré dans un boîtier (13) doté de moyens d'extraction de vapeur sur le dessus et d'un filtre optionnel ;

    b) l'introduction d'un milieu liquide choisi parmi une solution, une dispersion, une émulsion, une bouillie, un gel ou un semi-solide dans ledit troisième récipient (3) ;

    c) le fait de faire s'écouler un gaz sous pression depuis la base (20) dudit premier récipient (1) à travers ledit premier espace annulaire continu (22) dans ledit second espace annulaire continu (26) et en outre depuis les passages dans la base dudit troisième récipient (3) pour se mélanger avec ledit milieu liquide ;

    d) le fait d'amener le solvant à s'évaporer pour concentrer le milieu liquide et le séchage des solides dans ledit système pour récupération.


     
    2. Procédé selon la revendication 1, dans lequel le milieu liquide est une solution.
     
    3. Procédé selon la revendication 1, dans lequel le milieu liquide est une dispersion.
     
    4. Procédé selon la revendication 1, dans lequel le milieu liquide est un gel.
     
    5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel, grâce à un ensemble de passages inclinés dans ledit troisième récipient, ledit gaz sous pression est diffusé dans la masse du milieu liquide pour créer une turbulence pour intensifier le contact entre le gaz et le milieu liquide pour un transfert thermique amélioré.
     
    6. Procédé selon l'une quelconque des revendications 1 à 5, dans lequel ledit moyen de mise sous pression du gaz est un compresseur ou un ventilateur.
     
    7. Procédé selon l'une quelconque des revendications précédentes, dans lequel ledit gaz sous pression est de l'air.
     




    Drawing














    Cited references

    REFERENCES CITED IN THE DESCRIPTION



    This list of references cited by the applicant is for the reader's convenience only. It does not form part of the European patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be excluded and the EPO disclaims all liability in this regard.

    Patent documents cited in the description