CN104892693A - Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution - Google Patents
Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution Download PDFInfo
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- CN104892693A CN104892693A CN201510293920.1A CN201510293920A CN104892693A CN 104892693 A CN104892693 A CN 104892693A CN 201510293920 A CN201510293920 A CN 201510293920A CN 104892693 A CN104892693 A CN 104892693A
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Abstract
The invention relates to a method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution, belonging to a coiled membrane filtration process. The method comprises the following steps: a, pretreating gulonic acid crystal mother solution; b, separating with an acid-resistant coiled ultrafiltration membrane; c, separating with an acid-resistant coiled nanofiltration membrane; and d, introducing the penetrate liquid treated through the acid-resistant coiled nanofiltration membrane into a cation exchanging step in the course of the main production process of 2-one-L-gulonic acid, removing residual cations for further purification, and carrying out vacuum concentration and crystallization on the purified 2-one-L-gulonic acid. According to the method disclosed by the invention, by virtue of a two-stage coiled membrane filtration method, 2-one-L-gulonic acid is separated from impurities such as carbohydrates with different molecular weights, pigments and colloid; the recovery rate of gulonic acid can reach 90-95%; the obtained gulonic acid solution is high in purity and can be directly returned to the original production flow; the process can be conveniently controlled in a fully automatic way and is simple and reliable to operate; the advantages of improving yield, reducing consumption and relieving pollution are achieved.
Description
Technical field
The present invention is a kind of method reclaiming KGA from 2-KLG crystalline mother solution, is specifically related to adopt the method for organic rolled film KGA and the impurity in mother liquor to be carried out the technique be separated.
Background technology
KGA (being called for short 2-KLG) is the important as precursors of producing vitamins C (also known as L-AA), mainly contain two kinds of production methods at present: one is chemical synthesis, also known as " Lai Shi method ", obtain 2-KLG by L-sorbose through ketonize and oxidation; Another kind is fermentation method, and being fermented by L-sorbose obtains 2-KLG.The KGA of current domestic production of vitamin C factory is all fermentative Production.
The existing extraction process of fermentative Production KGA is essentially: obtain 2KGA-Na solution after the fermentation such as L-sorbose, corn steep liquor, calcium carbonate, heat sterilization body, clear liquid is through Zeo-karb, remove sodium ion, become KGA solution, again through vacuum concentration, crystallisation by cooling, centrifugation obtains KGA crystal.Crystalline mother solution, through again concentrating, can separate out a small amount of 2-KLG again.Owing to there is the impurity such as a large amount of colloid, albumen, pigment, organic heteroacid in mother liquor, though wherein also containing the 2-KLG (about 20% ~ 25%) of higher concentration, uncrystallizable go out qualified product, be discharged, pollute and waste.
In order to obtain the 2-KLG in crystalline mother solution, the impurity in mother liquor must be removed, the method reported has ion-exchange-resin process, electroosmose process, simulation moving-bed resin method etc., though this several method all has certain practical value and feature, but still there is the deficiency such as complex operation, inefficiency.
Summary of the invention
Technical problem: in order to solve Problems existing in production reality, the object of the present invention is to provide a kind of method reclaiming KGA from 2-KLG crystalline mother solution, the method technological operation is simple, equipment is simple, separation efficiency is high, and level of automation is high, pollutes few.
Technical scheme: 2-KLG crystalline mother solution treatment process of the present invention is specific as follows:
A, the pre-treatment of 2-KLG crystalline mother solution: the cloth envelop collector filtration by 2-KLG crystalline mother solution pore size filter being 5 microns, remove the graininess impurity that wherein may exist, obtain ultrafiltration stock liquid, for subsequent use;
B, acidproof spiral wound membrane sepn: above-mentioned solution and ultrafiltration stock liquid are entered ultra-filtration membrane device and filters, by the governor valve control working pressure in setting device, when ultrafiltration stock liquid is by ultra-filtration membrane, be separated into trapped fluid and permeate two parts, when trapped fluid volume to ultrafiltration stock liquid volume 1/10 time, in trapped fluid, add pure water dialyse, amount of water equals the volume of trapped fluid, stop when continuing to be filtered to former trapped fluid volume filtering, collect permeate; Main containing macromole pigment, albumen, colloidal impurity in trapped fluid, send into wastewater treatment operation and carry out biochemical treatment;
C, acidproof rolling nanofiltration membrane separation: the permeate through above-mentioned ultra-filtration filters is called nanofiltration stock liquid, then enter acidproof rolling nanofiltration membrane and filter, by the governor valve control working pressure in conditioning equipment; When nanofiltration stock liquid is by nanofiltration membrane, be separated into trapped fluid and permeate two parts, when this trapped fluid volume to nanofiltration stock liquid volume 1/10 time, in this trapped fluid, add pure water dialyse, amount of water is 2 times of these trapped fluid volumes, stop when continuing to be filtered to this trapped fluid volume filtering, collect permeate; Main containing small molecules pigment, residual sugar and part high volence metal ion impurity in remaining trapped fluid, send into wastewater treatment operation and carry out biochemical treatment;
D, the cation-exchange step be incorporated to through the permeate of above-mentioned nanofiltration membrane treatment in the main production process of KGA, remove remaining positively charged ion to purify further, KGA after purifying, carry out vacuum concentration and crystallization subsequently.
Beneficial effect: the present invention is to provide a kind of new treatment process reclaiming KGA from 2-KLG crystalline mother solution---wound membrane filtration technique, thus improve yield, reduce and consume, decreasing pollution.
Owing to present invention employs the method for two-stage wound membrane filtration, by the magazins' layout such as sugar, pigment, colloid of KGA and different molecular weight, the rate of recovery of 2-KLG can reach 90 ~ 95%, the 2-KLG solution purity obtained is better, directly can get back in original production flow process and go, both reduce the difficulty of wastewater treatment, again saved production cost, this technique can realize full automatic control easily simultaneously, and operation is simple and reliable.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail.
Embodiment 1:
The main component of 2-KLG crystalline mother solution is: KGA 20%, protein 4%, residual sugar 2.5%, pigment, other organic acid, PH=1.1, brownish black.
Get above mother liquor 100L; after filtering out the large granular impurity that may exist with 5 micron cloth bag, enter acidproof rolling ultrafiltration membrane and filter, when trapped fluid volume is 10L; in trapped fluid, add total 10L pure water dialyse, when trapped fluid volume is shut down for during 10L again in batches.Film device is joined the acidproof rolling organic membrane of 1 2540 specification, filtration MW is 3000Da, and working pressure is 15-20bar, and filtration flux is 22.3L/m
2.h; Enter acidproof nanofiltration membrane after being collected by ultrafiltration membrane permeate liquid 100L to filter, when trapped fluid volume is 10L, in trapped fluid, adds total 20L pure water in batches dialyse, when trapped fluid volume is shut down for during 10L again.Film device is joined the acidproof rolling organic membrane of 1 2540 specification, filtration MW is 700Da, and working pressure is 15bar, and filtration flux is 14.4L/m
2.h.Collect nanofiltration membrane permeate, clear, brown color, KGA content 17.2%.This solution carries out cationic exchange, vacuum concentration, crystallization, obtains KGA crystal.
Embodiment 2:
The main component of 2-KLG crystalline mother solution is: KGA 25%, protein 4.2%, residual sugar 2.6%, pigment, other organic acid, PH=0.6, aterrimus.
Get above mother liquor 100L; after filtering out the large granular impurity that may exist with 5 micron cloth bag, enter acidproof rolling ultrafiltration membrane and filter, when trapped fluid volume is 10L; in trapped fluid, add total 10L pure water dialyse, when trapped fluid volume is shut down for during 10L again in batches.Film device is joined the acidproof rolling organic membrane of 1 2540 specification, filtration MW is 3000Da, and working pressure is 15-20bar, and filtration flux is 18.7L/m
2.h; Enter acidproof nanofiltration membrane after being collected by ultrafiltration membrane permeate liquid 100L to filter, when trapped fluid volume is 10L, in trapped fluid, adds total 20L pure water in batches dialyse, when trapped fluid volume is shut down for during 10L again.Film device is joined the acidproof rolling organic membrane of 1 2540 specification, filtration MW is 700Da, and working pressure is 15bar, and filtration flux is 13.2L/m
2.h.Collect the permeate of nanofiltration membrane, clear, brown color, KGA content 20.6%.This solution carries out cationic exchange, vacuum concentration, crystallization, obtains KGA crystal.
Claims (1)
1. from 2-KLG crystalline mother solution, reclaim a method for KGA, it is characterized in that the method comprises the steps:
A, the pre-treatment of 2-KLG crystalline mother solution: the cloth envelop collector filtration by 2-KLG crystalline mother solution pore size filter being 5 microns, remove the graininess impurity that wherein may exist, obtain ultrafiltration stock liquid, for subsequent use;
B, acidproof spiral wound membrane sepn: above-mentioned solution and ultrafiltration stock liquid are entered ultra-filtration membrane device and filters, by the governor valve control working pressure in setting device, when ultrafiltration stock liquid is by ultra-filtration membrane, be separated into trapped fluid and permeate two parts, when trapped fluid volume to ultrafiltration stock liquid volume 1/10 time, in trapped fluid, add pure water dialyse, amount of water equals the volume of trapped fluid, stop when continuing to be filtered to former trapped fluid volume filtering, collect permeate; Main containing macromole pigment, albumen, colloidal impurity in trapped fluid, send into wastewater treatment operation and carry out biochemical treatment;
C, acidproof rolling nanofiltration membrane separation: the permeate through above-mentioned ultra-filtration filters is called nanofiltration stock liquid, then enter acidproof rolling nanofiltration membrane and filter, by the governor valve control working pressure in conditioning equipment; When nanofiltration stock liquid is by nanofiltration membrane, be separated into trapped fluid and permeate two parts, when this trapped fluid volume to nanofiltration stock liquid volume 1/10 time, in this trapped fluid, add pure water dialyse, amount of water is 2 times of these trapped fluid volumes, stop when continuing to be filtered to this trapped fluid volume filtering, collect permeate; Main containing small molecules pigment, residual sugar and part high volence metal ion impurity in remaining trapped fluid, send into wastewater treatment operation and carry out biochemical treatment;
D, the cation-exchange step be incorporated to through the permeate of above-mentioned nanofiltration membrane treatment in the main production process of KGA, remove remaining positively charged ion to purify further, KGA after purifying, carry out vacuum concentration and crystallization subsequently.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510293920.1A CN104892693A (en) | 2015-06-01 | 2015-06-01 | Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution |
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| CN201510293920.1A CN104892693A (en) | 2015-06-01 | 2015-06-01 | Method for recovering 2-one-L-gulonic acid from gulonic acid crystal mother solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588641A (en) * | 2016-12-20 | 2017-04-26 | 宁夏启元药业有限公司 | Method for reclaiming primary crystallized mother liquor of gulonic acid |
| CN109851491A (en) * | 2019-04-16 | 2019-06-07 | 同舟纵横（厦门）流体技术有限公司 | A kind of method and device of gulonate feed liquid decoloration removal of impurities |
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| CN1594266A (en) * | 2004-06-23 | 2005-03-16 | 徐昌洪 | Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor |
| CN1754869A (en) * | 2004-09-28 | 2006-04-05 | 三达膜科技（厦门）有限公司 | Process for extracting gulonic acid |
| CN101704737A (en) * | 2009-10-10 | 2010-05-12 | 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 |
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2015
- 2015-06-01 CN CN201510293920.1A patent/CN104892693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1594266A (en) * | 2004-06-23 | 2005-03-16 | 徐昌洪 | Method for recovering 2-keto-L-gluconic acid from gluconic acid crystallization mother liquor |
| CN1754869A (en) * | 2004-09-28 | 2006-04-05 | 三达膜科技（厦门）有限公司 | Process for extracting gulonic acid |
| CN101704737A (en) * | 2009-10-10 | 2010-05-12 | 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 |
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| 朱银惠等: "纳滤浓缩古龙酸提取液的研究", 《中国酿造》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588641A (en) * | 2016-12-20 | 2017-04-26 | 宁夏启元药业有限公司 | Method for reclaiming primary crystallized mother liquor of gulonic acid |
| CN106588641B (en) * | 2016-12-20 | 2019-10-22 | 宁夏启元药业有限公司 | A kind of recovery method of 2-KLG primary crystallization mother liquor |
| CN109851491A (en) * | 2019-04-16 | 2019-06-07 | 同舟纵横（厦门）流体技术有限公司 | A kind of method and device of gulonate feed liquid decoloration removal of impurities |
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Application publication date: 20150909 |