EP0832986A1 - Verfahren zur Regenerierung von Ionaustauschharzen im Verfahren zur Entfernung des Kalzium aus Zuckersaften - Google Patents

Verfahren zur Regenerierung von Ionaustauschharzen im Verfahren zur Entfernung des Kalzium aus Zuckersaften Download PDF

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Publication number
EP0832986A1
EP0832986A1 EP97402149A EP97402149A EP0832986A1 EP 0832986 A1 EP0832986 A1 EP 0832986A1 EP 97402149 A EP97402149 A EP 97402149A EP 97402149 A EP97402149 A EP 97402149A EP 0832986 A1 EP0832986 A1 EP 0832986A1
Authority
EP
European Patent Office
Prior art keywords
molasses
ion exchange
exchange resin
regeneration
sent
Prior art date
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Granted
Application number
EP97402149A
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English (en)
French (fr)
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EP0832986B1 (de
Inventor
Gérard Rousseau
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.)
SAINT-LOUIS SUCRE S.A.
Original Assignee
GENERALE SUCRIERE SA
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Publication of EP0832986A1 publication Critical patent/EP0832986A1/de
Application granted granted Critical
Publication of EP0832986B1 publication Critical patent/EP0832986B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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 present invention relates to a process for softening a sweet juice aqueous containing sugar and calcium ions and relates more particularly to a process for regenerating ion exchange resins in the process of decalcification of candy juices.
  • the juice is treated obtained by diffusion, from sugar beets transformed into cossettes, with lime.
  • the spent pods are pressed to give pulp.
  • Lime introduced into the juice is transformed, by introduction of carbon dioxide, into calcium carbonate.
  • the calcium carbonate is removed by filtration.
  • this elimination is only partial and a certain amount of calcium compounds remains dissolved in the juice in the form of soluble calcium salts.
  • These calcium salts have a certain solubility which decreases when the concentration of dry matter increases, which occurs during evaporation and crystallization stages. In precipitating, these calcium salts scale up the material and lower the coefficient of heat transfer, which causes partial disturbances in the equilibrium of the economy of the sugar refinery. In addition, they create a cloud in the crystallized sugar obtained during the process.
  • the Akzo process consisting of a regeneration with soda, results in a significant expenditure of soda and an increase in the coloring of purified juices.
  • the present invention overcomes the problems of regeneration techniques of prior art.
  • molasses is used for the regeneration of ion exchange resins in the juice decalcification process of candy.
  • the present invention therefore provides a process for decalcifying purified sugar juice from a sugar manufacturing process, originating from the filtration stages, in which said juice, containing calcium ions, is sent to a strong cationic ion exchange resin. in Na + or K + form , where calcium ions are replaced by sodium and / or potassium ions, and in which said ion exchange resin is then subjected to regeneration (or washing), said process being characterized in that diluted molasses are used to effect said regeneration (or said washing) of said ion exchange resin.
  • This molasses is advantageously part of the molasses obtained during of the sugar making process.
  • the installation includes a distillery
  • all the products leaving the decalcification and used for regeneration are sent directly to the distillery. There is no recycling of eluate in purification.
  • the first variant described below will be advantageously used.
  • the diluted fractions are used for diluting turbinated molasses (for regeneration).
  • second variant described below will preferably be used.
  • the molasses is sent in the step co-current regeneration.
  • the molasses is preferably diluted to around 70 to 80 brix (percent dry matter), better yet at around 76 brix, before being sent to the decalcification stage to regenerate the ion exchange resin.
  • molasses is advantageously reheated to a temperature of about 80 to 90 ° C, better still at about 85 ° C, before being sent to the decalcification step to regenerate the resin ion exchange.
  • the regeneration of the resin ion exchange is carried out while the resin is dry, i.e. the resin bed has been drained and is therefore dry.
  • An ion exchange resin is said to be "dry” when it does not include interstitial fluid (water or, in this case, juice).
  • a molasses cake is formed which is sent to the resin in order to to eliminate with the minimum of mixing, i.e. dilution, the diluted juice contained in the resin.
  • the resin after regeneration, the resin is brought to dryness, by a total emptying of the resin can, and the resin is washed dry with a cake of purified juice.
  • the calcified molasses used to regenerate the ion exchange resin of the decalcification step is mixed with molasses from the process, i.e. turbinated molasses, to obtain a concentration equal to approximately 80% of dry matter, and is sent to storage.
  • the molasses is sent in the step counter-current regeneration.
  • the molasses is preferably diluted to around 60 to 65 brix, better still to around 62 brix, before being sent to the decalcification step to regenerate the ion exchange resin.
  • molasses is advantageously sent at a temperature of about 50 to 60 ° C, better still at about 55 ° C, before being sent to the decalcification step to regenerate the resin ion exchange.
  • the resins undergo a total emptying then are washed dry with a small amount of water (about 0.2 BV).
  • the washing of the exchange resin ion is carried out while the resin is dry, i.e. the resin bed has been drained and is therefore dry.
  • An ion exchange resin is said to be "dry” when it does not includes no interstitial fluid (water).
  • the calcified molasses used to regenerate the ion exchange resin of the decalcification step is mixed with molasses from the process, i.e. turbinated molasses, to obtain a concentration equal to approximately 80% of dry matter, and is sent to storage.
  • lime salts can be removed from the calcified molasses from the regeneration of the ion exchange resin by carbonating simply said molasses and separating the calcium carbonate formed.
  • the process of the present invention can be used both in the beet sugar as in cane sugar.
  • the purified juices JE originating from the filtration stages (generally two in number), containing sodium, potassium and calcium ions, are sent by 1 to a DK decalcification stage, designated by 2.
  • a DK decalcification stage the calcified juices pass over an ion exchange resin (not shown).
  • the juices, free of calcium ions and still containing sodium and potassium ions, leaving the decalcification by 3, are about 15% dry matter.
  • These juices before evaporation are designated by JAE.
  • the JAEs are sent by 3 in an evaporation step with several effects 4, generally five in number (not shown), from which emerges by 5 a syrup with approximately 72 to 74% of dry matter.
  • This syrup receives the redesigns of sugar from third spray and possibly from second spray, as will be shown below, to constitute Standard Liquor 1 (LS1), which will feed the first crystallization spray.
  • the LS1 is sent by 5 in a first jet cooking appliance 6, containing the Masse Cuite I (MC I ).
  • the MC I leaving at 7 from the first jet cooking appliance 6 is sent to a discontinuous first jet turbine 8 where it is added with water H 2 O at 9.
  • first-throw sugar, Sucre I or S I is recovered, as well as in 11, a mother liquor of MC I , designated by Poor Sewer I (EP1).
  • This EP1 also constitutes the LS2 (Standard Liquor 2).
  • the EP1 (or LS2) is sent to a second jet cooking appliance 12, containing the Masse Cuite II (MC II ).
  • the MC II leaving through 13 from the second jet cooking appliance 12 is sent to a continuous second jet turbine 14.
  • second jet sugar Si is recovered, as well as 16 a mother liquor of MC II , designated by Poor Sewer II (EP2).
  • the second jet sugar S II is recycled by 15 'in the standard liquor LS1.
  • the EP2 is sent by 16 in a third jet cooking appliance 17 containing the Massecuite III (MC III ) ⁇
  • the MC III leaving by 18 of the third jet cooking appliance 17 is sent in a block of vertical mixers 19, generally three in number (not shown individually), then by 20 on a continuous turbine 21.
  • we recover by 22 brown sugar SR which is returned to the Standard Liquor 1 by 22 ', and, by 23, turbines molasses M T.
  • part of the turbines molasses M T is diluted with dilution juice of JDM molasses originating by 24 from washing the resin. ion exchange up to about 35 brix, and sent by 25 to the decalcification step 2 to regenerate the co-current ion exchange resin.
  • the calcified molasses M C leaving the decalcification 2 by 26 after regenerating the ion exchange resin is mixed with the turbinated molasses M T to obtain a molasses having a concentration greater than about 78 to 80% of dry matter which is sent to the storage by 27.
  • the purified JE juices coming from the filtration stages (generally two in number), containing sodium, potassium and calcium ions, are sent by 1 to a DK decalcification stage, designated by 2.
  • a DK decalcification stage the calcified juices pass over an ion exchange resin (not shown).
  • These juices before evaporation are designated by JAE.
  • the JAEs are sent by 3 in an evaporation step with several effects 4, generally five in number (not shown), from which emerges by 5 a syrup with approximately 72 to 74% of dry matter.
  • This syrup receives the redesigns of sugar from third spray and possibly from second spray, as will be shown below, to constitute Standard Liquor 1 (LS1), which will feed the first crystallization spray.
  • the LS1 is sent by 5 in a first jet cooking appliance 6, containing the Masse Cuite I (MC I ).
  • the MC I leaving at 7 from the first jet cooking appliance 6 is sent to a discontinuous first jet turbine 8 where it is added with water H 2 O at 9.
  • first-throw sugar, Sucre I or S I is recovered, as well as in 11, a mother liquor of MC I , designated by Poor Sewer I (EP1).
  • This EP1 also constitutes the LS2 (Standard Liquor 2).
  • the EP1 (or LS2) is sent to a second jet cooking appliance 12, containing the Masse Cuite II (MC II ).
  • the MC II leaving through 13 from the second jet cooking appliance 12 is sent to a continuous second jet turbine 14.
  • sugar from the second jet S II is recovered, as well as in 16 a mother liquor of MC II , designated by Poor Sewer II (EP2).
  • the second jet sugar S II is recycled by 15 'in the standard liquor LS1.
  • the EP2 is sent by 16 in a third jet cooking appliance 17 containing the Mace III (MC III )
  • the MC III leaving by 18 from the third jet cooking appliance 17 is sent in a block of vertical mixers 19 , generally three in number (not shown individually), then by 20 on a continuous turbine 21.
  • we recover by 22 brown sugar SR which is returned to the Standard Liquor 1 by 22 ' , and, by 23, turbinated molasses M T.
  • part of the turbines molasses M T is diluted with dilution juice of JDM molasses originating by 24 from washing the resin. ion exchange, and sent by 25 to the decalcification step 2 to regenerate the ion exchange resin against the current.
  • the calcified molasses M C leaving the decalcification 2 by 26 after regenerating the ion exchange resin is mixed with the turbinated molasses M T to obtain a molasses having a concentration greater than about 78 to 80% of dry matter which is sent to the storage by 27.
  • Phases a), b), c) and d) above are then repeated.
  • Phases a), b), c) and d) are then repeated.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Non-Alcoholic Beverages (AREA)
  • Saccharide Compounds (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
EP97402149A 1996-09-18 1997-09-17 Verfahren zur Regenerierung von Ionaustauschharzen im Verfahren zur Entfernung des Kalzium aus Zuckersaften Expired - Lifetime EP0832986B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9611373A FR2753456B1 (fr) 1996-09-18 1996-09-18 Procede de regeneration de resines echangeuses d'ions dans le processus de decalcification des jus de sucrerie
FR9611373 1996-09-18

Publications (2)

Publication Number Publication Date
EP0832986A1 true EP0832986A1 (de) 1998-04-01
EP0832986B1 EP0832986B1 (de) 2003-11-19

Family

ID=9495848

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97402149A Expired - Lifetime EP0832986B1 (de) 1996-09-18 1997-09-17 Verfahren zur Regenerierung von Ionaustauschharzen im Verfahren zur Entfernung des Kalzium aus Zuckersaften

Country Status (9)

Country Link
US (1) US5958142A (de)
EP (1) EP0832986B1 (de)
AT (1) ATE254668T1 (de)
DE (1) DE69726237T2 (de)
DK (1) DK0832986T3 (de)
ES (1) ES2210474T3 (de)
FR (1) FR2753456B1 (de)
PT (1) PT832986E (de)
WO (1) WO1998012356A1 (de)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998001533A1 (en) 1996-07-08 1998-01-15 Burstein Laboratories, Inc. Cleavable signal element device and method
FR3094724B1 (fr) * 2019-04-05 2021-04-23 Novasep Process Procédé de traitement de sucre
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
CN115595383B (zh) * 2022-08-31 2024-07-26 新疆冠农股份有限公司 一种糖浆稀汁脱钙工艺

Citations (5)

* 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
EP0016992A1 (de) * 1979-03-15 1980-10-15 Giuseppe Assalini Verfahren und Anlage zur Regenerierung von Ionenaustauscherharzen bei der Zuckersaftbehandlung
EP0032263A1 (de) * 1979-12-28 1981-07-22 Akzo N.V. Verfahren zur Regenerierung eines Sorbens
EP0629707A2 (de) * 1993-06-11 1994-12-21 Applexion Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern
EP0655507A2 (de) * 1993-11-12 1995-05-31 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft

Patent Citations (5)

* 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
EP0016992A1 (de) * 1979-03-15 1980-10-15 Giuseppe Assalini Verfahren und Anlage zur Regenerierung von Ionenaustauscherharzen bei der Zuckersaftbehandlung
EP0032263A1 (de) * 1979-12-28 1981-07-22 Akzo N.V. Verfahren zur Regenerierung eines Sorbens
EP0629707A2 (de) * 1993-06-11 1994-12-21 Applexion Verfahren zur Enthartung von zuckerenthaltenden Säften wie Melasse und Verwendung desselben zu einem Verfahren zur Gewinnung der in dieser Melasse enthaltenden Zuckern
EP0655507A2 (de) * 1993-11-12 1995-05-31 Applexion Verfahren zur Herstellung von Kristallzucker aus einem wässrigen Zuckersaft, z.B. Zuckerrohr-oder Zuckerrübesaft

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
E.GRYLLUS ET AL.: "Das BMA-Zsigmond-Gryllus Verfahren - ein neuses Verfahren zur Dünnsaftentkalkung", ZEITSCHRIFT FÜR DIE ZUCKERINDUSTRIE, vol. 25, no. 9, 20 September 1975 (1975-09-20), pages 493 - 501, XP002031417 *

Also Published As

Publication number Publication date
PT832986E (pt) 2004-04-30
FR2753456A1 (fr) 1998-03-20
FR2753456B1 (fr) 1998-12-31
DK0832986T3 (da) 2004-03-29
WO1998012356A1 (fr) 1998-03-26
DE69726237T2 (de) 2004-09-23
ES2210474T3 (es) 2004-07-01
ATE254668T1 (de) 2003-12-15
US5958142A (en) 1999-09-28
EP0832986B1 (de) 2003-11-19
DE69726237D1 (de) 2003-12-24

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