EP0629707A2 - Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern - Google Patents

Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern Download PDF

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Publication number
EP0629707A2
EP0629707A2 EP94401313A EP94401313A EP0629707A2 EP 0629707 A2 EP0629707 A2 EP 0629707A2 EP 94401313 A EP94401313 A EP 94401313A EP 94401313 A EP94401313 A EP 94401313A EP 0629707 A2 EP0629707 A2 EP 0629707A2
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EP
European Patent Office
Prior art keywords
ions
resin
sugars
liquid effluent
sweet juice
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP94401313A
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English (en)
French (fr)
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EP0629707A3 (de
EP0629707B1 (de
Inventor
Xavier Lancrenon
Michael Saska
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Applexion SAS
Louisiana State University
Original Assignee
Applexion SAS
Louisiana State University
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Publication of EP0629707A3 publication Critical patent/EP0629707A3/de
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Publication of EP0629707B1 publication Critical patent/EP0629707B1/de
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Classifications

    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B35/00Extraction of sucrose from molasses
    • C13B35/02Extraction of sucrose from molasses by chemical means
    • C13B35/06Extraction of sucrose from molasses by chemical means using ion exchange
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00Purification of sugar juices
    • C13B20/14Purification of sugar juices using ion-exchange materials
    • C13B20/144Purification of sugar juices using ion-exchange materials using only cationic ion-exchange material

Definitions

  • the subject of the present invention is a process for softening a sweet juice such as a candy molasses and its use in a process for recovering the sugars contained in this sweet juice.
  • the sugar cane or sugar beet industry produces significant amounts of non-crystallizable sweet juice known as candy molasses. Since this molasses has a non-negligible sugar content, it is usual to subject it to an appropriate treatment in order to extract the major part of the sugars which it contains. This treatment consists in particular in subjecting the molasses to an ion exclusion chromatography using a fixed support constituted by a strong cationic resin, in the Na+ and / or K+ form.
  • the sugar molasses contains significant quantities of dissolved calcium and / or magnesium salts, the said resin becomes charged with Ca2+ and / or Mg2+ ions during the chromatography operation and sees this makes its separation power decrease relatively quickly. This requires the periodic interruption of the chromatography operation to regenerate the cationic resin, which implies the consumption of a regeneration reagent and a decrease in productivity.
  • the regeneration step of the process according to the invention makes astute use of one of the liquid effluents available in a sugar refinery installation, namely the so-called raffinate fraction generated during the separation by chromatography of the sugars from a sweetened sweetened juice loaded with Na+ and / or K+ ions, a fraction which was usually purely and simply rejected out of this installation.
  • raffinate fraction generated during the separation by chromatography of the sugars from a sweetened sweetened juice loaded with Na+ and / or K+ ions
  • the liquid effluent (raffinate) used in step (b) advantageously consists of that produced during the separation by chromatography of the sugars from the sweetened sweet juice obtained in step (a).
  • the invention it is also advantageous to concentrate the liquid effluent (raffinate) before its implementation in step (b), since the degree of regeneration is all the higher as the concentration of Na ions + and / or K+ of this effluent is higher. It is also advantageous according to the invention, that before bringing said resin into contact with said liquid effluent in step (b), Na+ and / or K+ ions are added to said effluent, which will further improve regeneration.
  • the cation exchange resin used in step (a) will preferably be a strong cationic resin in the Na+ and / or K+ form and that the chromatography producing the liquid effluent (raffinate) used in step (b) is preferably carried out on a strong cationic resin in the Na+ and / or K+ form with elution with water.
  • a strong cationic resin it is possible to choose in particular any resin comprising a polymer matrix, for example of the polystyrene or polyacrylate type, crosslinked by a crosslinking agent such as divinylbenzene, matrix on which are grafted cation exchange groups, such as acid groups. strongly acid sulfonic. Particular preference is given to IR 200 resin (trademark of a resin sold by Rohm and Haas).
  • the present invention further extends to sweetened sweet juice as obtained by the softening process described above.
  • said first liquid effluent (raffinate) is preferably concentrated before its use in step (iii), that Na+ and / or K+ ions may be added to said first liquid effluent before the use of the latter in step (iii), that the cation exchange resin used in step (i) is preferably a strong cationic resin in the Na+ and / or K+ form and that the chromatography used in step (ii) is preferably carried out on a strong cationic resin in the Na+ and / or K+ form with elution with water.
  • a strong cationic resin use can be made of those already mentioned above in connection with the softening process.
  • the present invention further extends to the liquid effluent enriched in sugars as obtained by the recovery process described above.
  • the installation shown by way of example in this figure comprises, in a manner known per se, two softening units 1, 2 each consisting of a column filled with a strong cationic resin, in the form Na+ and / or K +, for example the IR®200 resin sold by Rohm and Haas. These columns are each provided, at their upper part, with a conduit 3,4 for supplying candy molasses (aqueous sweet juice) previously clarified and diluted with deionized water.
  • the clarification can be carried out by any known method, for example by implementing the clarification process described in US-A-5 110 363. As for dilution, it is carried out so that the dry matter content of the molasses after dilution or preferably of the order of 10 to 70% by weight.
  • the molasses thus clarified and diluted essentially comprises sugars, mineral salts of sodium, potassium, calcium and optionally magnesium and colorings.
  • Each softening column 1, 2 is further provided, at its lower part, with a conduit 5,6 for softened molasses outlet, the conduits 5,6 both leading to a three-way valve 7 from which a conduit 8, the free end of which opens out at the top of a chromatography column 9.
  • a circulation pump 10, 11 can be provided on each conduit 5.6.
  • Each column 1,2 is finally provided, at its upper part, with a conduit 12, 13 for supplying resin regeneration liquid and, at its lower part, with a conduit 12 a , 13 a for outlet from spent regeneration liquid carrying respectively a shut-off valve 12 b , 13 b .
  • the chromatography column 9 is of the type comprising a fixed support constituted by a strong cationic resin, in the Na+ and / or K+ form, the elution liquid being of the water brought into the upper part of the column by a pipe 14.
  • This same column 9 also comprises, at its lower part, a pipe 15 for extracting a liquid effluent (raffinate) rich in sugars and a pipe 16 d extraction of a liquid effluent poor in sugars.
  • the concentration unit can be constituted by an evaporator operating under reduced pressure. It may, for example, be a simple or multiple effect falling-stream evaporator, well known in the art considered.
  • the outlet 22 ensures the evacuation of the condensates formed during the evaporation.
  • valve 7 is positioned to communicate the conduit 8 with the conduits 5 and 6, the pumps 10, 11, 18 and 24 are in operation, the pump 27 is stopped and the valves 12 b , 13 b and 28 are closed.
  • the clarified and diluted molasses (10 to 70% by weight of dry matter) is brought through conduits 3 and 4 into columns 1 and 2 where it undergoes a cation exchange, the Na+ and / or K+ ions of the resin arranged in these columns being progressively replaced by the Ca2+ and / or Mg2+ ions present in the molasses.
  • molasses is enriched in Na / and / or K+ ions and is depleted in Ca2+ and / or Mg2+ ions, while the resin is enriched in Ca2+ and / or Mg2+ ions and s 'depleted in Na+ and / or K+ ions.
  • the molasses from the columns 1,2 is then brought via the conduits 5,6, the pumps 10, 11, the valve 7 and the conduit 8 in the chromatography column 9.
  • the molasses is subjected to a separation there under the effect resin and water supplied via line 14 as an eluent.
  • the first eluted fractions (constituting the raffinate) poor in sugars and rich in sodium and / or potassium salts and dyes, are extracted via line 16 and poured into tank 20.
  • the following fractions, poor in sodium salts and / or potassium and rich in sugars are extracted via line 15.
  • the raffinate recovered in the tank 20 is brought via the conduit 19, the pump 18 and the pipe 17 into the evaporation unit 21.
  • the concentrated raffinate (preferably at 10-70% by weight of dry matter ) produced in this unit 21 is extracted from the latter by the conduit 23 and the pump 24 and poured into the tank 25.
  • the ion-exchange resin of one of the columns 1 and 2 is regenerated, for example the resin of column 1.
  • the supply of molasses to be softened is stopped, the pump 10 is stopped, valve 7 is positioned to communicate conduit 8 only with conduit 6, valve 12b is open, valve 28 is positioned to communicate conduit 26 only with conduit 29 and pump 27 is brought into operation.
  • the concentrated raffinate from tank 25 is brought via conduits 26, 29 and 12 to column 1 where said concentrated raffinate, rich in Na+ and / or K+ ions, will pass through the resin contained in the column 1 and regenerate it, the Na+ and / or K+ ions of said concentrated raffinate progressively replacing the Ca2+ and / or Mg2+ ions of the resin.
  • the concentrated raffinate which, during its passage through the resin, is enriched in Ca2+ and / or Mg2+ ions is then evacuated via line 12 a .
  • the second and third cycles are then repeated at regular time intervals.
  • the flow of clarified and diluted molasses (10 to 70% by weight of dry matter) through each column 1,2 may be of the order 0.1 to 5 times the volume of the resin bed / hour and that during the regeneration operation, the flow rate of regeneration liquid (concentrated raffinate present in the tank 25 and containing 10 to 70% by weight of dry matter) through each column 1.2 may be of the order of 0.1 to 5 times the volume of the resin bed / hour.
  • these flow rates will be chosen according to the dry matter content of the liquid used.
  • the higher the dry matter content of the molasses the lower the molasses flow rate through the columns 1,2 will be for the softening operation.
  • the higher the dry matter content of the regeneration liquid (concentrated raffinate) the lower the flow rate of this liquid through the columns 1,2.
  • the temperature of the regeneration liquid will be adjusted so as to have a liquid having a viscosity suitable for the regeneration operations; this may be in the range of 20 to 70 ° C depending on the dry matter content.
  • Na+ and / or K+ ions in the form of NaCl and / or KCl for example
  • the concentrated raffinate for example at the level of tank 25.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Saccharide Compounds (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
EP94401313A 1993-06-11 1994-06-10 Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern Expired - Lifetime EP0629707B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US75634 1993-06-11
US08075634 US5443650B2 (en) 1993-06-11 1993-06-11 Process for softening a sugar-containing aqueous solution such as sugar juice or molasses

Publications (3)

Publication Number Publication Date
EP0629707A2 true EP0629707A2 (de) 1994-12-21
EP0629707A3 EP0629707A3 (de) 1995-02-15
EP0629707B1 EP0629707B1 (de) 1999-03-24

Family

ID=22127050

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94401313A Expired - Lifetime EP0629707B1 (de) 1993-06-11 1994-06-10 Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern

Country Status (18)

Country Link
US (1) US5443650B2 (de)
EP (1) EP0629707B1 (de)
CN (1) CN1043903C (de)
AT (1) ATE178099T1 (de)
AU (1) AU668305B2 (de)
CA (1) CA2125749A1 (de)
CZ (1) CZ289046B6 (de)
DE (1) DE69417292T2 (de)
DK (1) DK0629707T3 (de)
ES (1) ES2130375T3 (de)
GR (1) GR3030118T3 (de)
MA (1) MA23222A1 (de)
PH (1) PH31548A (de)
PL (1) PL303771A1 (de)
RU (1) RU2122031C1 (de)
SK (1) SK280574B6 (de)
UA (1) UA27814C2 (de)
ZA (1) ZA944017B (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0655507A3 (de) * 1993-11-12 1996-03-20 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft.
FR2732358A1 (fr) * 1995-03-27 1996-10-04 Resindion Srl Procede pour le traitement par une resine echangeuse d'ions cationique d'une solution sucree issue de la betterave
FR2753456A1 (fr) * 1996-09-18 1998-03-20 Generale Sucriere Sa Procede de regeneration de resines echangeuses d'ions dans le processus de decalcification des jus de sucrerie

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU726559C (en) * 1997-07-24 2001-08-30 Commonwealth Scientific And Industrial Research Organisation Process for the purification of nutrients from food process streams
AUPO821397A0 (en) * 1997-07-24 1997-08-14 Commonwealth Scientific And Industrial Research Organisation Process for the purification of nutrients from food process streams
WO2000021546A1 (fr) * 1998-10-09 2000-04-20 Mitsui Sugar Co., Ltd Prophylactiques/medicaments pour l'infection, agents anti-endotoxine, adjuvants de vaccin et promoteurs de croissance
MXPA01010051A (es) * 1999-04-07 2003-07-14 White Strap Molasses Technolog Tratamiento de jugo de azucar.
IL147529A0 (en) * 2002-01-09 2002-08-14 Oladur Ltd A method for the production of soybean sugars and the product produced thereof
FR2844209B1 (fr) * 2002-09-06 2007-10-19 Applexion Ste Nouvelle De Rech Procede de purification par nanofiltration d'une solution aqueuse sucree contenant des anions et cations monovalents et polyvalents
FR2844151B1 (fr) * 2002-09-06 2006-05-26 Applexion Ste Nouvelle De Rech Procede de decalcification d'une solution aqueuse et utilisation de ce procede pour la decalcification de lactoserum ou d'un permeat d'ultrafiltration de lactoserum
US6790245B2 (en) * 2002-10-07 2004-09-14 Benetech, Inc. Control of dust
FR2907687B1 (fr) * 2006-10-30 2008-12-26 Applexion Procede de purification de sialyllactose par chromatographie
US8273181B2 (en) * 2007-08-30 2012-09-25 Iogen Energy Corporation Process of removing calcium and obtaining sulfate salts from an aqueous sugar solution
CN101403017B (zh) * 2008-10-31 2011-06-08 华南理工大学 一种二混蜜脱钾钠树脂的再生方法
WO2012106761A1 (en) 2011-02-08 2012-08-16 Horizon Science Pty Ltd Sugar extracts
US9017767B2 (en) 2012-06-13 2015-04-28 Benetech, Inc. Method of suppressing dust in piles and railcars using plasticized cellulose ethers
US9267063B2 (en) 2012-11-19 2016-02-23 Benetech, Inc. Dust suppression formulas using plasticized cellulose ethers
RU2621995C1 (ru) * 2016-09-21 2017-06-08 Федеральное государственное бюджетное научное учреждение "Краснодарский научно-исследовательский институт хранения и переработки сельскохозяйственной продукции" (ФГБНУ КНИИХП) Способ очистки диффузионного сока
CN112795710A (zh) * 2020-12-08 2021-05-14 武汉美味源生物工程有限公司 制糖过程中离子交换树脂的再生方法
CN112593017A (zh) * 2020-12-15 2021-04-02 新疆冠农果茸股份有限公司 一种用于甜菜制糖糖分高效分离方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1404591A (fr) * 1964-05-21 1965-07-02 Magyar Cukoripar Ki Procédé pour régénérer les échangeurs d'ions et pour réduire la teneur en ions alcalins des jus de sortie des sucreries, en vue de leur utilisation pour l'adoucissement des jus dilués, au moyen d'un échange d'ions
FR2304673A2 (fr) * 1975-03-19 1976-10-15 Sueddeutsche Zucker Ag Procede perfectionne pour separer le sucre des melasses
US4519845A (en) * 1984-02-09 1985-05-28 Uop Inc. Separation of sucrose from molasses
US5110369A (en) * 1990-10-24 1992-05-05 Mobil Solar Energy Corporation Cable interconnections for solar cell modules

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2362211C3 (de) * 1973-12-14 1978-05-11 Sueddeutsche Zucker Ag, 6800 Mannheim Verfahren zur Aufarbeitung von Melassen
US4140541A (en) * 1977-03-25 1979-02-20 Karel Popper Treatment of crude sugar juices by ion exchange

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1404591A (fr) * 1964-05-21 1965-07-02 Magyar Cukoripar Ki Procédé pour régénérer les échangeurs d'ions et pour réduire la teneur en ions alcalins des jus de sortie des sucreries, en vue de leur utilisation pour l'adoucissement des jus dilués, au moyen d'un échange d'ions
FR2304673A2 (fr) * 1975-03-19 1976-10-15 Sueddeutsche Zucker Ag Procede perfectionne pour separer le sucre des melasses
US4519845A (en) * 1984-02-09 1985-05-28 Uop Inc. Separation of sucrose from molasses
US5110369A (en) * 1990-10-24 1992-05-05 Mobil Solar Energy Corporation Cable interconnections for solar cell modules

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0655507A3 (de) * 1993-11-12 1996-03-20 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft.
FR2732358A1 (fr) * 1995-03-27 1996-10-04 Resindion Srl Procede pour le traitement par une resine echangeuse d'ions cationique d'une solution sucree issue de la betterave
FR2753456A1 (fr) * 1996-09-18 1998-03-20 Generale Sucriere Sa Procede de regeneration de resines echangeuses d'ions dans le processus de decalcification des jus de sucrerie
WO1998012356A1 (fr) * 1996-09-18 1998-03-26 Saint Louis Sucre Procede de regeneration de resines echangeuses d'ions dans le processus de decalcification des jus de sucrerie
EP0832986A1 (de) * 1996-09-18 1998-04-01 Generale Sucriere, S.A. Verfahren zur Regenerierung von Ionaustauschharzen im Verfahren zur Entfernung des Kalzium aus Zuckersaften

Also Published As

Publication number Publication date
ZA944017B (en) 1995-02-09
CN1043903C (zh) 1999-06-30
DK0629707T3 (da) 1999-10-11
ATE178099T1 (de) 1999-04-15
PL303771A1 (en) 1995-01-09
MA23222A1 (fr) 1994-12-31
CZ289046B6 (cs) 2001-10-17
AU668305B2 (en) 1996-04-26
US5443650B2 (en) 2000-05-30
CZ139394A3 (en) 1995-02-15
GR3030118T3 (en) 1999-07-30
EP0629707A3 (de) 1995-02-15
PH31548A (en) 1998-11-03
US5443650A (en) 1995-08-22
CA2125749A1 (fr) 1994-12-12
SK70594A3 (en) 1995-03-08
DE69417292D1 (de) 1999-04-29
EP0629707B1 (de) 1999-03-24
AU6467694A (en) 1994-12-15
SK280574B6 (sk) 2000-04-10
CN1111678A (zh) 1995-11-15
ES2130375T3 (es) 1999-07-01
US5443650B1 (en) 1998-05-26
RU2122031C1 (ru) 1998-11-20
DE69417292T2 (de) 1999-09-02
UA27814C2 (uk) 2000-10-16

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