CN1594266A - Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor - Google Patents
Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor Download PDFInfo
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- CN1594266A CN1594266A CN 200410041060 CN200410041060A CN1594266A CN 1594266 A CN1594266 A CN 1594266A CN 200410041060 CN200410041060 CN 200410041060 CN 200410041060 A CN200410041060 A CN 200410041060A CN 1594266 A CN1594266 A CN 1594266A
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Abstract
The invention provides a method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor which comprises, (1) preliminary treatment of 2-keto-L-gluconic acid crystallization mother liquor, (2) electrodialysis segregation, (3) cation exchange procedure, removing cation, converting into 2-keto-L-gluconic acid, vacuum concentration and crystallization.
Description
Technical field
The present invention is a kind of method that reclaims the ancient imperial acid of 2-ketone group-L-from the imperial acid crystal mother liquor of Gu, is specifically related to adopt electrodialytic method that the impurity in ancient dragon acid of 2-ketone group-L-and the mother liquor is carried out separation processes.
Background technology
The ancient dragon acid of 2-ketone group-L-(being called for short 2-KLG) is the important as precursors of producing vitamins C (claiming the L-xitix again), and mainly contain two kinds of production methods at present: a kind of is chemical synthesis, claims again " Lai Shi method " to obtain 2-KLG by the L-sorbose through ketonize and oxidation; Another kind is a fermentation method, is that China invented in nineteen seventies, and the fermentation of L-sorbose obtains 2-KLG.Chemical synthesis need consume a large amount of poisonous and inflammable and explosive chemical, and production plant needs higher investment, and the ancient imperial acid of 2-ketone group-L-of therefore present domestic production of vitamin C factory all is fermentative Production.
The existing technology of the ancient dragon acid of fermentative Production 2-ketone group-L-is: obtain 2-keto-L-gulonate solution after the fermentations such as L-sorbose, corn steep liquor, lime carbonate, the heat sterilization body, clear liquid is through Zeo-karb, remove sodium ion, become the ancient imperial acid solution of 2-ketone group-L-, again through vacuum concentration, crystallisation by cooling, centrifugation obtains the ancient imperial acid crystal of 2-ketone group-L-.Crystalline mother solution can be separated out a small amount of 2-KLG again through concentrating once more.Owing to have impurity such as a large amount of colloids, albumen, pigment, organic heteroacid in the mother liquor, though wherein also contain the 2-KLG (about 20%～25%) of higher concentration, uncrystallizablely go out qualified product, be discharged, pollute and waste.
In order to obtain the 2-KLG in the crystalline mother solution, must remove the impurity in the mother liquor, reported method has ion-exchange-resin process (" ion-exchange and absorption " 1998,14 (2), 175～179), this method adopts macropore strong acid ion exchange resin and macroreticular weakly base ion exchange resin to handle ancient imperial acid crystal mother liquor in succession, and to remove impurity, ancient imperial acid recovering rate is more than 80%; Through the ancient imperial acid solution after two kinds of plastic resin treatment, through decolouring, transition, crystallization, can obtain qualified 2-KLG, crystallization yield is 74.6%.Though this method has certain practical value, its shortcoming also is conspicuous: complex operation; Resin washing and regeneration will consume soda acid, and produce a large amount of waste water; Removal of impurity such as albumen, pigment is not high.
Summary of the invention
Technical problem: in order to solve the problem that exists in the production reality, the object of the present invention is to provide a kind of technological operation simple, equipment is simple, and the separation efficiency height pollutes few method that reclaims the ancient dragon acid of 2-ketone group-L-from the imperial acid crystal mother liquor of Gu.
Technical scheme: the ancient imperial acid crystal mother liquor treatment process of 2-ketone group of the present invention-L-is specific as follows:
The ancient imperial acid crystal mother liquor pre-treatment of a, 2-ketone group-L-: 2-ketone group-L-gulonic acid mother solution is adjusted to PH=4～8 with alkaline solution, standby;
B, electrodialysis separate: the freshwater room that above-mentioned solution enters electrodialysis unit carries out electrodialysis, adjusts the voltage and current of membrane stack by transformer.When the feed liquid specific conductivity drops to 2000～8000 μ s/cm, stop electrodialysis, collect ancient imperial hydrochlorate and see through liquid; Mainly contain impurity such as pigment, sugar, albumen in the remaining feed liquid, abandon it;
C, ancient imperial hydrochlorate see through liquid and incorporate cation-exchange step in the sour main production process of the ancient dragon of 2-ketone group-L-into, remove positively charged ion, change into the ancient dragon acid of 2-ketone group-L-, carry out vacuum concentration and crystallization subsequently;
In above-mentioned processing method, during the ancient imperial acid crystal mother liquor of 2-ketone group-L-at first need carry out and pre-treatment, with Gu dragon acid conversion salify, used alkali is: any in sodium hydroxide, potassium hydroxide, ammoniacal liquor, the yellow soda ash.
Beneficial effect: the present invention provides a kind of new treatment process---electrodialysis process that reclaims the ancient dragon acid of 2-ketone group-L-from the imperial acid crystal mother liquor of Gu, thereby improves yield, reduces consuming, and reduces and pollutes.
Because the present invention has adopted electrodialytic method, with the ancient dragon acid of ionogenic 2-ketone group-L-, to separate with impurity such as non-ionizing sugar, pigment, colloids, the rate of recovery of ancient dragon acid can reach 80～90%, and has simplified operation widely.The ancient imperial acid salt solution purity that obtains after the electrodialysis is better, can directly get back in the reason Production Flow Chart and go, and is workable.By adopting this technology, the total recovery that ancient dragon acid is produced can improve 4 percentage points, has reduced waste, reduces and pollutes, and has saved production cost.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail.
The ancient imperial acid crystal mother liquor treatment process of 2-ketone group of the present invention-L-is specific as follows:
The ancient imperial acid crystal mother liquor pre-treatment of a, 2-ketone group-L-: 2-ketone group-L-gulonic acid mother solution is transferred to PH=4～8 with alkaline solution, standby;
B, electrodialysis separate: the freshwater room that above-mentioned solution enters electrodialysis unit carries out electrodialysis, adjusts the voltage and current of membrane stack by transformer.When the feed liquid specific conductivity drops to 2000～8000 μ s/cm, stop electrodialysis, collect ancient imperial hydrochlorate and see through liquid; Mainly contain impurity such as pigment, sugar, albumen in the remaining feed liquid, abandon it;
C, ancient imperial hydrochlorate see through liquid and incorporate cation-exchange step in the sour main production process of the ancient dragon of 2-ketone group-L-into, remove positively charged ion, change into the ancient dragon acid of 2-ketone group-L-, carry out vacuum concentration and crystallization subsequently;
In above-mentioned processing method, used alkali is: any in sodium hydroxide, potassium hydroxide, ammoniacal liquor, the yellow soda ash.
Embodiment 1:
The main component of ancient imperial acid crystal mother liquor is: the ancient dragon acid 20% of 2-ketone group-L-, protein 4%, residual sugar 2.5%, pigment, other organic acid, PH=0.6, brownish black.
Get above mother liquor, stir adding 30% sodium hydroxide (or 40% potassium hydroxide solution) down, pH value is transferred to 6.5.The neutralizer specific conductivity is about 36000 μ s/cm, carries out electrodialysis.Electrodialyzer is made up of 12 pairs of anode membranes and cavity block, and control membrane stack voltage when the filtrate specific conductivity drops to 7600 μ s/cm, stops electrodialysis at 20～25V.Collect ancient dragon acid and see through liquid, clear, orange, the ancient imperial acid content 14.1% of 2-ketone group-L-.This solution carries out cationic exchange, vacuum concentration, and crystallization obtains the ancient imperial acid crystal of 2-ketone group-L-.
Embodiment 2:
The main component of ancient imperial acid crystal mother liquor is: the ancient dragon acid 25% of 2-ketone group-L-, protein 3.5%, residual sugar 2.2%, pigment, other organic acid, PH=1.2, brownish black.
Above mother liquor stirs adding 5% ammoniacal liquor (or 20% sodium carbonate solution) down, and pH value is transferred to 5.5.The neutralizer specific conductivity is about 34000 μ s/cm, carries out electrodialysis.Electrodialyzer is made up of 12 pairs of anode membranes and cavity block, and control membrane stack voltage when the filtrate specific conductivity drops to 6000 μ s/cm, stops electrodialysis at 23～26V.Collect ancient dragon acid and see through liquid, amount to 1.6 liters, clear, safran, the ancient imperial acid content 10.8% of 2-ketone group-L-.This solution carries out cationic exchange, vacuum concentration, and crystallization obtains the ancient imperial acid crystal of 2-ketone group-L-.
Claims (2)
1, a kind of method that reclaims the ancient dragon acid of 2-ketone group-L-from the imperial acid crystal mother liquor of Gu is characterized in that treatment process is specific as follows:
The ancient imperial acid crystal mother liquor pre-treatment of a, 2-ketone group-L-: 2-ketone group-L-gulonic acid mother solution is adjusted to PH=4～8 with alkaline solution, standby;
B, electrodialysis separate: the freshwater room that above-mentioned solution enters electrodialysis unit carries out electrodialysis, adjusts the voltage and current of membrane stack by transformer.When the feed liquid specific conductivity drops to 2000～8000 μ s/cm, stop electrodialysis, collect ancient imperial hydrochlorate and see through liquid; Mainly contain impurity such as pigment, sugar, albumen in the remaining feed liquid, abandon it;
C, ancient imperial hydrochlorate see through liquid and incorporate cation-exchange step in the sour main production process of the ancient dragon of 2-ketone group-L-into, remove positively charged ion, change into the ancient dragon acid of 2-ketone group-L-, carry out vacuum concentration and crystallization subsequently;
2, the method that from the imperial acid crystal mother liquor of Gu, reclaims the ancient dragon acid of 2-ketone group-L-according to claim 1, it is characterized in that used alkali is in the ancient imperial acid crystal mother liquor of 2-ketone group-L-carries out and in the pre-treatment: any in sodium hydroxide, potassium hydroxide, ammoniacal liquor, the yellow soda ash.
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| CN 200410041060 CN1273436C (en) | 2004-06-23 | 2004-06-23 | Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor |
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| CN 200410041060 CN1273436C (en) | 2004-06-23 | 2004-06-23 | Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717133B (en) * | 2009-12-14 | 2012-11-21 | 安徽丰原发酵技术工程研究有限公司 | Method for removing pigment in gulonic acid mother solution |
| CN101704737B (en) * | 2009-10-10 | 2013-01-30 | 安徽丰原发酵技术工程研究有限公司 | Method for separating gulonic acid from gulonic acid crystallization mother liquor by adopting ion exchange and bipolar electrodialysis membrane stack |
| CN104892693A (en) * | 2015-06-01 | 2015-09-09 | 南京鼎仕和膜科技有限公司 | Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution |
| CN105777533A (en) * | 2014-12-15 | 2016-07-20 | 宁夏启元药业有限公司 | Method for recovering gulonic acid from gulonic acid mother liquor |
| CN108774125A (en) * | 2018-05-28 | 2018-11-09 | 苏州澄江环境科技有限公司 | A kind of technique recycling raw material from gulonic acid mother solution |
| CN111592455A (en) * | 2019-02-21 | 2020-08-28 | 上海凯赛生物技术股份有限公司 | Decoloring method of mixed long-chain dibasic acid and mixed long-chain dibasic acid |
| CN112028766A (en) * | 2020-09-08 | 2020-12-04 | 山东鲁维制药有限公司 | Process for refining gulonic acid |
-
2004
- 2004-06-23 CN CN 200410041060 patent/CN1273436C/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704737B (en) * | 2009-10-10 | 2013-01-30 | 安徽丰原发酵技术工程研究有限公司 | Method for separating gulonic acid from gulonic acid crystallization mother liquor by adopting ion exchange and bipolar electrodialysis membrane stack |
| CN101717133B (en) * | 2009-12-14 | 2012-11-21 | 安徽丰原发酵技术工程研究有限公司 | Method for removing pigment in gulonic acid mother solution |
| CN105777533A (en) * | 2014-12-15 | 2016-07-20 | 宁夏启元药业有限公司 | Method for recovering gulonic acid from gulonic acid mother liquor |
| CN104892693A (en) * | 2015-06-01 | 2015-09-09 | 南京鼎仕和膜科技有限公司 | Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution |
| CN108774125A (en) * | 2018-05-28 | 2018-11-09 | 苏州澄江环境科技有限公司 | A kind of technique recycling raw material from gulonic acid mother solution |
| CN111592455A (en) * | 2019-02-21 | 2020-08-28 | 上海凯赛生物技术股份有限公司 | Decoloring method of mixed long-chain dibasic acid and mixed long-chain dibasic acid |
| CN112028766A (en) * | 2020-09-08 | 2020-12-04 | 山东鲁维制药有限公司 | Process for refining gulonic acid |
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| CN1273436C (en) | 2006-09-06 |
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