CN1107116C - Regenerating liquid and method for ionic exchange resin to decolor sugar solution - Google Patents

Regenerating liquid and method for ionic exchange resin to decolor sugar solution Download PDF

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Publication number
CN1107116C
CN1107116C CN00130871A CN00130871A CN1107116C CN 1107116 C CN1107116 C CN 1107116C CN 00130871 A CN00130871 A CN 00130871A CN 00130871 A CN00130871 A CN 00130871A CN 1107116 C CN1107116 C CN 1107116C
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China
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liquid
sugar
ion exchange
liter
exchange resin
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CN1298952A (en
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于淑娟
高大维
李国基
秦志荣
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The present invention relates to ion exchange resin regeneration liquid of sugar liquor decoloration, which is composed of calcium oxide, calcium chloride and sugar, or calcium chloride and sugar, or aluminum hydroxide and sugar. In the regeneration method, eluant through regeneration treatment under certain conditions is carbonated by CO2 or added with phosphoric acid so that calcium ions precipitate to generate calcium carbonate or calcium phosphate; after filtration, the eluant is repeatedly used, or the eluant directly returns to main flow paths without treatment. Because the eluant after the regeneration method mainly contains sugar and calcium salt which are recovered into the main flow path without generating pollution; in addition, the consumption of regeneration reagents and washing water is greatly reduced, and the environment is protected.

Description

The ion exchange resin regeneration liquid and the renovation process thereof of liquid glucose decolouring
The present invention relates to be used for the decolouring of carbohydrate goods industry liquid glucose, comprise the decolouring of sucrose, beet sugar, Dian Fentang, biological polyoses, functional oligose and various monose.
The refining material of spent ion exchange resin is a kind of effective ways of food and biochemical industrial application, though absorption impurity is simple operation, desorption has certain degree of difficulty, causes ion exchange technique to be restricted in industrial application.The main method that makes resin regeneration at present is chemical method-sodium-chlor or alkaline sodium chloride solution method of reproduction, though this method consumption simple to operate pharmaceutical chemicals is many, blowdown flow rate is big.Usually use the alkaline NaCl solution of 4-10% in the tradition sugar refining technology, not only can not effectively remove the pigment on the resins exchange base with this regenerator but also produce a large amount of waste liquids, so seriously polluted owing to contain in the alkaline NaCl elutriant that a large amount of coloring matters and sodium salt cause COD and BOD too high levels.
The objective of the invention is to shortcoming at the prior art existence, a kind of ion exchange resin regeneration liquid of liquid glucose decolouring is provided, can effectively removes the pigment on the resins exchange base, can be used for after the use in sugaring or the sugar refinery technical process, thereby consumption is few, and does not produce waste liquid and pollution.
The present invention also aims to provide a kind of ion exchange resin regeneration method of liquid glucose decolouring.
The ion exchange resin regeneration liquid of liquid glucose decolouring of the present invention is made up of calcium oxide, calcium chloride and sugar; Or calcium chloride and sugar composition; Or aluminium hydroxide and sugar composition.
The regenerated liquid consumption that calcium oxide and sugar are formed is a calcium oxide 1-50 grams per liter, sugared 20-600 grams per liter.Optimum amount is a calcium oxide 5-10 grams per liter, sugared 100-150 grams per liter.
The regenerated liquid consumption that calcium chloride and sugar are formed is chlorion (Cl -) concentration 2-40mol/ liter, sugared 20-600 grams per liter.Optimum amount is chlorion (Cl -) concentration 10-20mol/ liter, sugared 100-150 grams per liter.
The regenerated liquid consumption that aluminium hydroxide and sugar are formed is aluminum ion (Al 3-) concentration 0.002-0.05mol/ liter.Optimum amount is aluminum ion (Al 3+) concentration 0.008-0.01mol/ liter, sugared 100-150 grams per liter.
Above-mentioned regenerated liquid is the aqueous solution.
Raw materials used calcium oxide or the natural matters such as calcium chloride or aluminium hydroxide and sugar of comprising of above-mentioned regenerated liquid, work in-process and finished product, the restriction with kind of not originated.
The ion exchange resin regeneration method of liquid glucose decolouring of the present invention comprises
---liquid glucose enters from an end of ion exchange column, and the other end flows out, and decolours, and the liquid glucose in the decolouring back water backwash post when syrup concentration is reduced to and equates with sugar concentration in the regenerated liquid in the post, is regenerated;
---during regeneration, regenerated liquid is added from an end of ion exchange column, the other end flows out, with 1-3 times of resin bed volume/hour velocity flow cross resin column, temperature is controlled at 40-70 ℃, the regenerated liquid consumption be the resin bed volume 1-4 doubly.---the elutriant CO that comes out after the manipulation of regeneration 2Full charge or add phosphoric acid and make calcium ion precipitation generate lime carbonate or calcium phosphate is filtered the back and is reused.The perhaps not treated main flow of directly getting back to of elutriant.
The present invention compared with prior art has following advantage and effect:
1, the present invention with alkaline calcium salt or aluminium salt with liquid glucose as regenerated liquid, calcium salt and aluminium salt regenerator improve than traditional alkaline salt solution greatly to the pigment elutive power that anchors on the exchanger, its reason is Ca 2-Or Al 3-Existence increased substantially Cl in the pigment negatively charged ion of solid phase adsorption and the liquid phase -Switching performance.
2, the elutriant after the manipulation of regeneration mainly contains sugar part and calcium salt, can be recovered in the main flow and does not produce pollution, and can significantly reduce regeneration reagent and washing water consumption, helps environment protection.
3, under the less salt state, the over-drastic pucker ﹠ bloat does not take place in ion exchange resin, can effectively prolong the work-ing life of resin.
4, this Ca (OH) that has 2Or Al (OH) 3Regenerated liquid can be used in and the secondary sugar of low-purity, also can calcium ion be removed by carbonation or the method that adds phosphoric acid precipitates, directly reclaim and be used as regenerated liquid.
Below by embodiment the present invention is further described.
Embodiment 1
Material: JRA900C (A Bulaite 900C type) strongly basic anion exchange resin, the former syrup of 50 hammer degree.
Pack into through pretreated resin at 70 ℃ of following 200ml and to be with the exchange column of insulation jacket, filter the remelt syrup of 40 times of resin bed volume 50 hammer degree in advance, liquid glucose adds from the top of ion exchange column, flow out the bottom, make the abundant adsorpting pigment of resin, liquid glucose in the decolouring back water backwash post, when syrup concentration in the post is reduced to when equating with sugar concentration in the regenerated liquid, with 4 times of resin bed volumes/hour the distilled water of flow velocity by 5 times of resin bed volumes, use lime saccharate solution regenerating resin again, the pigment on the wash-out resin.Lime saccharate solution is pressed sucrose: 20 grams per liters; CaO 50 grams per liters; Cl -Concentration 2mol/ liter, with 1 times of ion exchange resin bed volume/hour velocity flow cross resin column, collecting the every 20ml of elutriant is a sample, serial sampling is surveyed its absorbancy respectively and is calculated reduction coefficient.Be eluted to colourless with distilled water.Carry out next round-robin operation.
Come out after the manipulation of regeneration elutriant CO 2Full charge or add phosphoric acid and make calcium ion precipitation generate lime carbonate or calcium phosphate is filtered the back and is reused.
Embodiment 2
Material: D201 strongly basic anion exchange resin, the evaporating sugar-molasses syrup of 45 hammer degree.Pack into through pretreated resin at 60 ℃ of following 200ml and to be with the exchange column of insulation jacket, filter the remelt syrup of 40 times of resin bed volume 45 hammer degree in advance, liquid glucose adds from the top of ion exchange column, flow out the bottom, make the abundant adsorpting pigment of resin, liquid glucose in the decolouring back water backwash post, when syrup concentration in the post is reduced to when equating with sugar concentration in the regenerated liquid, the flow velocity of 3 resin bed volume/h is crossed the distilled water of 4 times of resin bed volumes, use lime saccharate solution regenerating resin again, pigment on the wash-out resin, lime saccharate solution is pressed sucrose: 600 grams per liters; CaO 1 grams per liter; Cl -Concentration 40mol/ liter is crossed resin column with the velocity flow of 2 times of resin bed volume/h, and collecting the every 20ml of elutriant is a sample, and serial sampling is surveyed its absorbancy respectively and calculated reduction coefficient.Be eluted to colourless with distilled water.Carry out next round-robin operation.So operate 50 cycles, syrup decolorization rate average out to 90%, than the high 15-20% of prior art (sodium-chlor or alkaline sodium chloride solution method of reproduction), the ion exchange resin regeneration rate reaches 90%, the not treated main flow of directly getting back to of elutriant.
Embodiment 3
Material: EDABF weakly basic anion exchange fibre, the clear juice of 15 hammer degree
(1) juice is heated to 40 ℃ clearly, advances post, when the pan feeding of exchange column equates with discharging hammer degree effluent liquid is collected.
(2) syrup flows into the flow velocity of 4 times of resin bed volume/hr, and 40 times of resin bed volume sugar juice decolorings are one-period.
40 ℃ of deionized water back scrubbing of (3) 2 times of resin bed volumes.
1. regeneration:
Solution 0.01mol/L Al (OH) 3Sucrose 20 grams per liters.
2. above solution flows into exchange column successively.With flow velocity 1-4BV/hr, temperature flows into exchange column for 40 ℃;
The regeneration back is washed till pH neutrality with deionized water.
3.752 type ultraviolet spectrophotometer 420nm surveys absorbancy down.
Elutriant colour=absorbancy * 1000 * extension rate.The detection method of elutriant colour.
The not treated main flow of directly getting back to of elutriant.
Embodiment 4
Material: D296 strongly basic anion exchange resin
(1) syrup is heated to 60 ℃, advances post, when the pan feeding of exchange column equates with discharging hammer degree effluent liquid is collected.
(2) syrup flows into the 35BV/hr flow velocity, and the 30BV sugar juice decoloring is an one-period.
(3) 4 times of resin bed volume/60 ℃ of deionized water back scrubbing of hr BV.
2. regeneration:
Solution 0.008mol/L Al (OH) 3Sucrose 600 grams per liters.
3. above solution flows into exchange column successively.With 2.5 times of resin bed volume/hr of flow velocity, temperature flows into exchange column for 60 ℃; The regeneration back is washed till pH neutrality with deionized water.
Come out after the manipulation of regeneration elutriant CO 2Full charge or add phosphoric acid and make calcium ion precipitation generate lime carbonate or calcium phosphate is filtered the back and is reused.

Claims (8)

1, a kind of ion exchange resin regeneration liquid of liquid glucose decolouring is characterized in that described regenerated liquid is the aqueous solution by calcium oxide, calcium chloride and sugar or calcium chloride and sugar or aluminium hydroxide and sugared the composition.
2, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 1 is characterized in that the regenerated liquid consumption of being made up of calcium oxide, calcium chloride and sugar is calcium oxide 1-50 grams per liter, chlorine ion concentration 2-40mol/ liter, sugared 20-600 grams per liter.
3, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 2 is characterized in that calcium oxide 5-10 grams per liter, chlorion 2-40mol/ liter, sugared 100-150 grams per liter.
4, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 1 is characterized in that the regenerated liquid consumption of being made up of calcium chloride and sugar is chlorine ion concentration 2-40mol/ liter, sugared 20-600 grams per liter.
5, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 4 is characterized in that chlorine ion concentration 10-20mol/ liter, sugared 100-150 grams per liter.
6, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 1 is characterized in that the regenerated liquid consumption of being made up of aluminium hydroxide and sugar is aluminium ion concentration 0.002-0.05mol/ liter, sugared 20-600 grams per liter.
7, the ion exchange resin regeneration liquid of liquid glucose decolouring according to claim 6 is characterized in that aluminium ion concentration 0.008-0.01mol/ liter, sugared 100-150mol/ liter.
8, use the described regenerated liquid of claim 1 to carry out the method for the ion exchange resin regeneration of liquid glucose decolouring, it is characterized in that comprising:
---liquid glucose enters from an end of ion exchange column, and the other end flows out, and decolours, and liquid glucose in the decolouring back water backwash post when sugar concentration is reduced to and equates with sugar concentration in the regenerated liquid in the post, is regenerated;
---during regeneration, regenerated liquid is added from an end of ion exchange column, the other end flows out, with 1-3 times of resin bed volume/hour velocity flow cross resin column, temperature is controlled at 40-70 ℃, the regenerated liquid consumption be the resin bed volume 1-4 doubly;
---the elutriant CO that comes out after the manipulation of regeneration 2Full charge or add phosphoric acid and make calcium ion precipitation generate lime carbonate or calcium phosphate is filtered the back and is reused; The perhaps not treated main flow of directly getting back to of elutriant.
CN00130871A 2000-12-20 2000-12-20 Regenerating liquid and method for ionic exchange resin to decolor sugar solution Expired - Fee Related CN1107116C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9592540B2 (en) 2011-02-02 2017-03-14 Bio-Rad Laboratories, Inc. Apatite surface neutralization with alkali solutions
CN104507952B (en) * 2012-05-30 2018-08-10 生物辐射实验室股份有限公司 The in situ of chromatography resin based on apatite restores
CN103801196B (en) * 2012-11-13 2016-01-20 山东百龙创园生物科技有限公司 A kind of method reclaimed from handing over sugar in post washing lotion
CN111955584A (en) * 2020-08-06 2020-11-20 广东省农业科学院蚕业与农产品加工研究所 Recovery process of sugar liquid in preserved fruit production
CN112795710A (en) * 2020-12-08 2021-05-14 武汉美味源生物工程有限公司 Regeneration method of ion exchange resin in sugar production process
CN114195292B (en) * 2021-12-16 2023-08-25 山东省鲁洲食品集团有限公司 Method for removing phosphorus from starch sugar rabbet sewage

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3791866A (en) * 1972-08-07 1974-02-12 Rohm & Haas Recovery of waste brine regenerant
FR2732358A1 (en) * 1995-03-27 1996-10-04 Resindion Srl Regeneration of cationic ion-exchange resin used to treat sugar soln. from sugar beet,

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3791866A (en) * 1972-08-07 1974-02-12 Rohm & Haas Recovery of waste brine regenerant
FR2732358A1 (en) * 1995-03-27 1996-10-04 Resindion Srl Regeneration of cationic ion-exchange resin used to treat sugar soln. from sugar beet,

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