EP0832986B1 - 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
EP0832986B1
EP0832986B1 EP97402149A EP97402149A EP0832986B1 EP 0832986 B1 EP0832986 B1 EP 0832986B1 EP 97402149 A EP97402149 A EP 97402149A EP 97402149 A EP97402149 A EP 97402149A EP 0832986 B1 EP0832986 B1 EP 0832986B1
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EP
European Patent Office
Prior art keywords
molasses
ion exchange
process according
exchange resin
regeneration
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.)
Expired - Lifetime
Application number
EP97402149A
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English (en)
French (fr)
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EP0832986A1 (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 SA
Original Assignee
Saint-Louis Sucre SA
Saint Louis Sucre SA
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Publication of EP0832986A1 publication Critical patent/EP0832986A1/de
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/14—Purification of sugar juices using ion-exchange materials
    • C13B20/144—Purification 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, coming 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 regeneration is carried out dry, in contrast to the methods described in EP 0 016 992, EP 0 655 507, and Gryllus and Delavier, Z. Zuckerind. 1975, 25 (9): 493-501.
  • 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 warmed 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 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 the third jet and possibly from the second jet, as will be shown below, to constitute the Standard Liquor 1 (LS1), which will feed the first crystallization jet.
  • the LS1 is sent by 5 in a first jet cooking appliance 6, containing the Masse Cuite I (MC I ).
  • the MC l 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.
  • At outlet 10 from the first jet turbine 8 first-throw sugar, Sugar 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 via 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 Masse Cuite III (MC III ).
  • the MC III leaving by 18 from the third jet cooking appliance 17 is sent to a block of vertical mixers 19, generally three in number (not shown individually), then by 20 to 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 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 juices JE 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 the third jet and possibly from the second jet, as will be shown below, to constitute the Standard Liquor 1 (LS1), which will feed the first crystallization jet.
  • the LS1 is sent by 5 in a first jet cooking appliance 6, containing the Masse Cuite I (MC I ).
  • the MC l 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.
  • At outlet 10 from the first jet turbine 8 first-throw sugar, Sugar 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 via 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 Masse Cuite III (MC III ).
  • the MC III leaving by 18 from the third jet cooking appliance 17 is sent to a block of vertical mixers 19, generally three in number (not shown individually), then by 20 to 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 obtained 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)
  • Treatment Of Water By Ion Exchange (AREA)
  • Saccharide Compounds (AREA)

Claims (15)

  1. Verfahren zur Entkalkung von gereinigten Zuckerfabrik-Säften aus einem Verfahren zur Herstellung von Zucker, in dem die Säfte, die Calciumionen enthalten, über ein starkes Kationenaustauscherharz in Na+- oder K+-Form geführt werden, in dem die Calciumionen durch Natrium- oder Kaliumionen ersetzt werden, und in dem das Ionenaustauscherharz dann einer Regeneration (oder einem Waschen) unterworfen wird, wobei das Verfahren dadurch gekennzeichnet ist, dass die Regeneration des Ionenaustauscherharzes trocken mit verdünnter Melasse durchgeführt wird.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Melasse Teil der Melasse ist, die in dem genannten Verfahren zur Herstellung von Zucker erhalten wird.
  3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die verkalkte Melasse, die zur Regeneration des Ionenaustauscherharzes dient, mit der Melasse des Verfahrens unter Erhalt einer Konzentration von etwa 80% Trockensubstanz vermischt wird, um dann der Lagerung zugeführt zu werden.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Melasse im Gleichstrom über das Ionenaustauscherharz geführt wird.
  5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass die Melasse auf etwa 70-80 Brix (% Trockensubstanz) verdünnt wird.
  6. Verfahren nach Anspruch 4 oder 5, dadurch gekennzeichnet, dass die Melasse wieder auf eine Temperatur von etwa 80-90°C erwärmt wird.
  7. Verfahren nach einem der Ansprüche 4 bis 6, dadurch gekennzeichnet, dass zur Regeneration die Melasse über das Ionenaustauscherharz in Form einer Scheibe geführt wird.
  8. Verfahren nach einem der Ansprüche 4 bis 7, dadurch gekennzeichnet, dass das Ionenaustauscherharz nach Regeneration getrocknet wird und trocken in Scheibenform durch den gereinigten Saft gewaschen wird.
  9. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Melasse im Gegenstrom über das Ionenaustauscherharz geführt wird.
  10. Verfahren nach Anspruch 9, dadurch gekennzeichnet, dass die Melasse auf etwa 60-65 Brix verdünnt wird.
  11. Verfahren nach Anspruch 9 oder 10, dadurch gekennzeichnet, dass die Melasse bei einer Temperatur von etwa 50-60°C durchgeführt wird.
  12. Verfahren nach einem der Ansprüche 9 bis 11, dadurch gekennzeichnet, dass das Ionenaustauscherharz nach Regeneration getrocknet wird und trocken mit Wasser gewaschen wird.
  13. Verfahren nach einem der Ansprüche 9 bis 12, dadurch gekennzeichnet, dass die Kalksalze aus der verkalkten Melasse, die aus der Regeneration des Ionenaustauscherharzes stammt, eliminiert werden, indem die Melasse mit Kohlendioxid gesättigt wird und das gebildete Calciumcarbonat abgetrennt wird.
  14. Verwendung des Verfahrens nach einem der vorangehenden Ansprüche 1 bis 3 bei der Herstellung von Zuckerrübenzucker.
  15. Verwendung des Verfahrens nach einem der Ansprüche 1 bis 13 bei der Herstellung von Rohrzucker.
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
FR9611373 1996-09-18
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

Publications (2)

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

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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)

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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
NZ333907A (en) 1996-07-08 2000-09-29 Burstein Lab Inc Cleavable optically detectable elements on substrate for microanalysis of chemical species
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
CN115595383A (zh) * 2022-08-31 2023-01-13 新疆冠农果茸股份有限公司（Cn） 一种糖浆稀汁脱钙工艺

Family Cites Families (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
IT1124013B (it) * 1979-03-15 1986-05-07 Assalini Giuseppe Procedimento ed impianto per il ripristino delle resine scambiatrici i ioni nel processo alcali magnesio tramite rigenerazione con melasso proveniente da detto processo arrichito con sale rigenerante fresco
NL7909337A (nl) * 1979-12-28 1981-07-16 Akzo Nv Werkwijze voor de regeneratie van sorbentia, in het bijzonder ionenuitwisselaars.
US5443650B2 (en) * 1993-06-11 2000-05-30 Univ Louisiana State Process for softening a sugar-containing aqueous solution such as sugar juice or molasses
US5554227A (en) * 1993-11-12 1996-09-10 Societe Nouvelle De Recherches Et D'applications Industrielles D'echangeurs D'ions Applexion Process of manufacturing crystal sugar from an aqueous sugar juice such as cane juice or sugar beet juice

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PW VAN DER POEL, H SCHIWECK, T SCHWARTZ: "Sugar technology: Beet and cane sugar manufacture", BARTENS, ? *

Also Published As

Publication number Publication date
ES2210474T3 (es) 2004-07-01
DE69726237T2 (de) 2004-09-23
WO1998012356A1 (fr) 1998-03-26
PT832986E (pt) 2004-04-30
US5958142A (en) 1999-09-28
DK0832986T3 (da) 2004-03-29
DE69726237D1 (de) 2003-12-24
FR2753456B1 (fr) 1998-12-31
ATE254668T1 (de) 2003-12-15
FR2753456A1 (fr) 1998-03-20
EP0832986A1 (de) 1998-04-01

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