CN101486637A - Method for extracting amber acid from fermentation liquor - Google Patents
Method for extracting amber acid from fermentation liquor Download PDFInfo
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- CN101486637A CN101486637A CNA2009100678343A CN200910067834A CN101486637A CN 101486637 A CN101486637 A CN 101486637A CN A2009100678343 A CNA2009100678343 A CN A2009100678343A CN 200910067834 A CN200910067834 A CN 200910067834A CN 101486637 A CN101486637 A CN 101486637A
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- succinic acid
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Abstract
The invention discloses a method for extracting succinic acid from a broth. The method comprises the following steps: a sodium succinate broth generated from microbial fermentation goes through a microfiltration membrane to conduct cross-flow filtration so as to remove thallus and other relatively large impurity particles; cross-flow filtration is carried out through a nanofiltration membrane to remove residual protein and pigment in the broth so as to get a clean filtrate; after the electrolysis, electrodialysis and electrolysis of the clean filtrate through a bipolar membrane, a succinic acid solution and a sodium hydroxide solution are obtained respectively; and the succinic acid solution is decompress-vaporized, cooled and crystallized, and therefore white succinic acid crystals are obtained. All working procedures in the method are closely connected, feed liquid always recycles under sealed condition, conditions through the whole technique process are mild, no organic solvent and any other organic compounds are added, the technique flow is short, steps are simple, the requirements on equipment are not high, the final product has high purity and the content of succinic acid is more than 99.0 percent through test.
Description
Technical field
The invention belongs to technical field of biochemical industry, relate to a kind of method of from fermented liquid, extracting Succinic Acid.
Background technology
Succinic Acid (succsinic acid) is a kind of important C4 hardware and software platform compound, is widely used in medicine, agricultural chemicals, dyestuff, spices, paint, food, plastics and photographic material industry.Be 1,4-butyleneglycol, tetrahydrofuran (THF), the basic material of important bulk chemical such as gamma-butyrolactone, PBT resin, N-Methyl pyrrolidone, hexanodioic acid and specialty chemicals.
The preparation method of Succinic Acid mainly contains chemical synthesis and microbe fermentation method.Chemical method mainly contains the electrolysis of ozone oxidation, MALEIC ANHYDRIDE or fumaric shortening and maleic acid of cyaniding hydrolysis, the cyclenes of paraffin oxidation, methyl chloroacetate.Producing Succinic Acid in the chemical synthesis can pollute environment, and the raw material of chemical synthesis is non-renewable petrochemicals, and its widespread use is restricted.The raw material of producing succinic acid by microbial fermentation is a renewable resources, as corn steep liquor, sugarcane, glucose etc., in addition, absorbs CO in the fermentation engineering
2, from the utilization of environmental protection and resource, the fermentative Production Succinic Acid be a kind of emerging, very the friendly process of development potentiality arranged.At present microbial fermentation preferably level be that the content of Succinic Acid in the fermented liquid is about 50g/L.So contained composition also comprises thalline, particulate state nutrient media components, solubility biomacromolecule, small organic molecule and organic acid (formic acid, acetate etc.) etc. in the fermented liquid except that Succinic Acid.Therefore the Succinic Acid in the microbial fermentation solution is carried out aftertreatment and Study on Purification significant.
The method of extracting Succinic Acid from microbial fermentation solution mainly contains calcium salt method, ammonia salt method, solvent extration, conventional electroosmose process, membrane separation process.
U.S. Pat 5143833, US5168055 discloses the method that a kind of calcium salt extracts Succinic Acid, in fermented liquid, add calcium hydroxide, produce the precipitation of calcium succinate, filter the back acidifying, obtain Succinic Acid solution after removing calcium sulfate, but the yield of this method is lower, have a large amount of calcium sulfate waste of generation in the leaching process, the acid and alkali consumption amount is big, the defective that energy consumption is big.
U.S. Pat 5958744 discloses the method that a kind of ammonia salt extracts Succinic Acid, and the pH that regulates fermented liquid with sodium hydroxide is greater than 6.5 earlier, and then adds monoammonium sulfate, carries out crystallization, at last by the methyl alcohol purifying.The ammonium salt process route is long, needs with a large amount of solvents, and crystallization condition is difficult for grasping, and step is more numerous, and difficulty is big, process cost height, the cost height of aftertreatment.
U.S. Pat 503415 discloses removes most of salt through the desalination electrodialysis again after the conventional electrodialysis and obtains the higher Succinic Acid solution of purity.But the electroosmose process route is long, the energy consumption height, and handling foreign ion has significant limitation, big to facility investment as not handling divalent ion, operational difficulty.
Lee SY (Proess Biochem, 2006,41:1461-1465), Wang Dawei (colleges and universities' chemical engineering journal, 1994,8 (2); 143.Reported with the method for solvent and extracted Succinic Acid, but in the process of extracting, need to consume a large amount of expensive organic solvents, cause cost for purification higher, the toxicity of residual solvent has detrimentally affect to the quality of food grade and pharmaceutical grade product simultaneously, and this method also is not suitable for the fermented liquid system of high-strength ionic strength.
Chinese patent CN1887843 discloses a kind of employing micro-filtrate membrane filtration, use ultrafiltration membrance filter then, use activated carbon decolorizing again, concentrate, the method for Succinic Acid is extracted in crystallization, but this method can not be converted into Succinic Acid with succinate, also to be acidified with acid at last, can cause introducing in the solution a large amount of salt, the result can cause comparatively difficulty of refined product, and yield is lower.
Chinese patent CN101348428A and CN101348429A disclose a kind of method with yin, yang resin purification Succinic Acid, it can consume a large amount of water in the process of ion-exchange, make that the evaporation cost is higher, increased energy consumption cost, and the regenerated process can produce a large amount of waste water.Be used for fermented liquid saltiness height simultaneously, cause resin stain serious, the regeneration difficulty, shorten resin life.
In the said extracted method or have aftertreatment cost for purification height, or the agents useful for same material is comparatively expensive, and operational path is long, or method complexity too, and the problem that energy consumption is big is unfavorable for the large-scale production of fermentative Production Succinic Acid.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of processing condition gentleness is provided, do not add any organic solvent and other organic compound, technical process is short, and step is simple, and cost is low, selectivity is good, the method for extracting Succinic Acid from fermented liquid that quality product is high.
Technical scheme of the present invention is summarized as follows:
From fermented liquid, extract the method for Succinic Acid, form by following step:
(1) Soduxin fermented liquid that will be by Production by Microorganism Fermentation is at 0.03～0.3MPa, 10～60 ℃, by the aperture is that the microfiltration membrane of 0.1～0.5um is carried out cross flow filter, cycles of concentration is 15～25 times, leaching requirement is 10%～50% of a fermentating liquid volume, holds back and removes thalline and the bigger impurity particle of other particles;
(2) filtrate that will obtain through step (1) is at 1～5MPa, 20～60 ℃, by molecular weight cut-off is that 500～2000 nanofiltration membrane is carried out cross flow filter, 20～40 times of cycles of concentration, leaching requirement is 10%～30% of a fermentating liquid volume, hold back and remove protein residual in the fermented liquid and pigment, obtain clarifying filtrate;
(3) with described clarifying filtrate at 5～40 ℃, by the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively;
(4) with described Succinic Acid solution decompression evaporation, decrease temperature crystalline obtains white Succinic Acid crystal.
Described step (1) is preferably: Soduxin fermented liquid that will be by Production by Microorganism Fermentation is at 0.12MPa, 30 ℃, by the aperture is that the microfiltration membrane of 0.3um is carried out cross flow filter, cycles of concentration is 20 times, leaching requirement is 20%～40% of a fermentating liquid volume, holds back and removes thalline and the bigger impurity particle of other particles.
Described step (2) is preferably: the filtrate that will obtain through step (1) is at 2MPa, 40 ℃, by molecular weight cut-off is that 800～1000 nanofiltration membrane is carried out cross flow filter, 35 times of cycles of concentration, leaching requirement is 20% of a fermentating liquid volume, hold back and remove protein residual in the fermented liquid and pigment, obtain clarifying filtrate.
The used fermented liquid of the present invention is to be the fermented liquid that contains Soduxin that fermenting raw materials obtains by glucose, sucrose, W-Gum hydrolysis syrup, agricultural crop straw lignocellulose hydrolysis syrup or sweet sorghum straw syrup.
Beneficial effect of the present invention: the present invention has adopted microfiltration membrane to remove thalline and the bigger impurity particle of particle, and filtered liquid is limpid.That quality is better than obviously that conventional fermentation liquor treatment adopts is centrifugal, flocculation and press filtration method, and operating process do not have the parts of running up, and has reduced energy consumption and labour intensity.The nanofiltration membrane that adopts has annexed the step of decolouring and removal of impurities, has saved traditional decolorization, has avoided the absorption of gac to Succinic Acid, has reduced operation steps, has improved yield simultaneously.The Bipolar Membrane electrolytic electro-dialysis that adopts has been avoided traditional and has been adjusted the pH value with soda acid, has reduced the content of salt in the system, makes that Succinic Acid crystalline purity is higher, makes that simultaneously the sodium salt in the system is recycled, and has reduced the pollution to environment.Series connection closely between each operation of the present invention, feed liquid circulates under airtight condition all the time, whole technological process mild condition, do not add any organic solvent and other organic compound, technical process is short, and step is simple, and is not high to equipment requirements, last product purity height is analyzed Succinic Acid content after testing greater than 99.0%.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
From fermented liquid, extract the method for Succinic Acid, form by following step:
Is that the microfiltration membrane of 0.3um is carried out cross flow filter with the Soduxin fermented liquid that contains Succinic Acid 50.1g/L of 20L Production by Microorganism Fermentation by the aperture, remove thalline and granule foreign, working pressure 0.12MPa, 30 ℃ of temperature, cycles of concentration is 19 times, and leaching requirement is 4L, and the clear liquid behind the micro-filtration is 500 nanofiltration membrane cross flow filter through molecular weight cut-off, remove protein residual in the fermented liquid and pigment, working pressure 2MPa, 40 ℃ of temperature, 35 times of cycles of concentration, leaching requirement is 2L, obtain clarifying filtrate, clarifying filtrate again 35 ℃ through the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively, sodium hydroxide solution reclaims, Succinic Acid solution is at 60 ℃ of reduction vaporizations, and the mass concentration of Succinic Acid is filtered greater than 20% back decrease temperature crystalline, oven dry obtains the Succinic Acid finished product of 804.6g white, yield 80.3%.Check and analysis Succinic Acid content is 99.2%.
Embodiment 2
From fermented liquid, extract the method for Succinic Acid, form by following step:
(1) with the Soduxin fermented liquid of 20L by Production by Microorganism Fermentation at 0.12MPa, 60 ℃ is that the microfiltration membrane of 0.1um is carried out cross flow filter by the aperture, cycles of concentration is 20 times, leaching requirement is 8L, holds back and removes thalline and the bigger impurity particle of other particles;
(2) filtrate that will obtain through step (1) is at 2MPa, and 40 ℃ is that 800 nanofiltration membrane is carried out cross flow filter by molecular weight cut-off, 30 times of cycles of concentration, and leaching requirement is 4L, holds back and removes protein residual in the fermented liquid and pigment, obtains clarifying filtrate;
(3) with described clarifying filtrate at 5 ℃, by the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively;
(4) with described Succinic Acid solution at 60 ℃ of reduction vaporizations, decrease temperature crystalline obtains white Succinic Acid crystal.
Embodiment 3
From fermented liquid, extract the method for Succinic Acid, form by following step:
(1) with the Soduxin fermented liquid of 20L by Production by Microorganism Fermentation at 0.03MPa, 40 ℃ is that the microfiltration membrane of 0.5um is carried out cross flow filter by the aperture, cycles of concentration is 15 times, leaching requirement is 2L, holds back and removes thalline and the bigger impurity particle of other particles;
(2) filtrate that will obtain through step (1) is at 1MPa, and 60 ℃ is that 1000 nanofiltration membrane is carried out cross flow filter by molecular weight cut-off, 20 times of cycles of concentration, and leaching requirement 2L holds back and removes protein residual in the fermented liquid and pigment, obtains clarifying filtrate;
(3) with described clarifying filtrate at 40 ℃, by the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively;
(4) with described Succinic Acid solution decompression evaporation, decrease temperature crystalline obtains white Succinic Acid crystal.
Embodiment 4
From fermented liquid, extract the method for Succinic Acid, form by following step:
(1) with the Soduxin fermented liquid of 20L by Production by Microorganism Fermentation at 0.3MPa, 10 ℃ is that the microfiltration membrane of 0.3um is carried out cross flow filter by the aperture, cycles of concentration is 25 times, leaching requirement is 10L, holds back and removes thalline and the bigger impurity particle of other particles;
(2) filtrate that will obtain through step (1) is at 5MPa, and 20 ℃ is that 2000 nanofiltration membrane is carried out cross flow filter by molecular weight cut-off, 40 times of cycles of concentration, and leaching requirement is 6L, holds back and removes protein residual in the fermented liquid and pigment, obtains clarifying filtrate;
(3) with described clarifying filtrate at 30 ℃, by the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively;
(4) with described Succinic Acid solution decompression evaporation, decrease temperature crystalline obtains white Succinic Acid crystal.
Claims (3)
1. from fermented liquid, extract the method for Succinic Acid, it is characterized in that forming by following step:
(1) Soduxin fermented liquid that will be by Production by Microorganism Fermentation is at 0.03～0.3MPa, 10～60 ℃, by the aperture is that the microfiltration membrane of 0.1～0.5um is carried out cross flow filter, cycles of concentration is 15～25 times, leaching requirement is 10%～50% of a fermentating liquid volume, holds back and removes thalline and the bigger impurity particle of other particles;
(2) filtrate that will obtain through step (1) is at 1～5MPa, 20～60 ℃, by molecular weight cut-off is that 500～2000 nanofiltration membrane is carried out cross flow filter, 20～40 times of cycles of concentration, leaching requirement is 10%～30% of a fermentating liquid volume, hold back and remove protein residual in the fermented liquid and pigment, obtain clarifying filtrate;
(3) with described clarifying filtrate at 5～40 ℃, by the electrolysis of Bipolar Membrane electrolytic electro-dialysis, obtain Succinic Acid solution and sodium hydroxide solution respectively;
(4) with described Succinic Acid solution decompression evaporation, decrease temperature crystalline obtains white Succinic Acid crystal.
2. a kind of method of from fermented liquid, extracting Succinic Acid according to claim 1, it is characterized in that described step (1) is: Soduxin fermented liquid that will be by Production by Microorganism Fermentation is at 0.12MPa, 30 ℃, by the aperture is that the microfiltration membrane of 0.3um is carried out cross flow filter, cycles of concentration is 20 times, leaching requirement is 20%～40% of a fermentating liquid volume, holds back and removes thalline and the bigger impurity particle of other particles.
3. a kind of method of from fermented liquid, extracting Succinic Acid according to claim 1, it is characterized in that described step (2) is: the filtrate that will obtain through step (1) is at 2MPa, 40 ℃, by molecular weight cut-off is that 800～1000 nanofiltration membrane is carried out cross flow filter, 35 times of cycles of concentration, leaching requirement is 20% of a fermentating liquid volume, holds back and removes protein residual in the fermented liquid and pigment, obtains clarifying filtrate.
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| CNA2009100678343A CN101486637A (en) | 2009-02-09 | 2009-02-09 | Method for extracting amber acid from fermentation liquor |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021604A (en) * | 2010-10-15 | 2011-04-20 | 福建师范大学 | Method for preparing succinic acid based on alloy wire mesh-bipolar film combined electrode technology |
| CN102020620B (en) * | 2009-09-18 | 2012-11-21 | 劲牌有限公司 | Method for separating and purifying effective constituents from salvia miltiorrhiza extracting solution by applying membrane technology |
| CN103012106A (en) * | 2012-11-27 | 2013-04-03 | 青岛琅琊台集团股份有限公司 | Method for extracting succinic acid by applying membrane technology |
| CN101665428B (en) * | 2009-10-09 | 2013-08-07 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting succinic acid from succinic acid fermentation liquor |
| CN103420826A (en) * | 2012-05-15 | 2013-12-04 | 常茂生物化学工程股份有限公司 | Method for extracting succinic acid from fermentation broth |
| CN103524327A (en) * | 2013-10-16 | 2014-01-22 | 江阴奥瑞诺生物技术有限公司 | Method for extracting succinic acid from succinic acid fermentation liquor by using electrodialysis method |
| CN103554065A (en) * | 2013-10-16 | 2014-02-05 | 江阴奥瑞诺生物技术有限公司 | Method for preparing tetrahydrofuran by using succinic acid fermentation broth |
| CN105452474A (en) * | 2013-03-08 | 2016-03-30 | 希乐克公司 | Upgrading process streams |
| CN105503578A (en) * | 2014-09-26 | 2016-04-20 | 常茂生物化学工程股份有限公司 | Method for extracting succinic acid from fermentation broth by use of extractant |
| CN106316836A (en) * | 2015-07-01 | 2017-01-11 | 中国石化扬子石油化工有限公司 | Method for preparing butanedioic acid |
| CN107033020A (en) * | 2017-06-10 | 2017-08-11 | 唐雪平 | A kind of method that theanine is extracted from tealeaves |
| CN107245032A (en) * | 2017-07-08 | 2017-10-13 | 桂林理工大学 | A kind of method that butanedioic acid is isolated and purified in the zymotic fluid from Bt |
| CN110141969A (en) * | 2019-05-27 | 2019-08-20 | 常茂生物化学工程股份有限公司 | A kind of two compartment method electrolytic separation of Bipolar Membrane anode membrane continuously prepares L-TARTARIC ACID method |
| CN117263794A (en) * | 2023-09-19 | 2023-12-22 | 安徽固德生物工程有限公司 | Succinic acid purifying and refining method |
-
2009
- 2009-02-09 CN CNA2009100678343A patent/CN101486637A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020620B (en) * | 2009-09-18 | 2012-11-21 | 劲牌有限公司 | Method for separating and purifying effective constituents from salvia miltiorrhiza extracting solution by applying membrane technology |
| CN101665428B (en) * | 2009-10-09 | 2013-08-07 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting succinic acid from succinic acid fermentation liquor |
| CN102021604A (en) * | 2010-10-15 | 2011-04-20 | 福建师范大学 | Method for preparing succinic acid based on alloy wire mesh-bipolar film combined electrode technology |
| CN102021604B (en) * | 2010-10-15 | 2012-07-25 | 福建师范大学 | Method for preparing succinic acid based on alloy wire mesh-bipolar film combined electrode technology |
| CN103420826A (en) * | 2012-05-15 | 2013-12-04 | 常茂生物化学工程股份有限公司 | Method for extracting succinic acid from fermentation broth |
| CN103012106A (en) * | 2012-11-27 | 2013-04-03 | 青岛琅琊台集团股份有限公司 | Method for extracting succinic acid by applying membrane technology |
| CN105452474B (en) * | 2013-03-08 | 2020-05-01 | 希乐克公司 | Upgrading process streams |
| CN105452474A (en) * | 2013-03-08 | 2016-03-30 | 希乐克公司 | Upgrading process streams |
| CN103554065B (en) * | 2013-10-16 | 2015-08-26 | 江阴奥瑞诺生物技术有限公司 | A kind of method using succinic acid fermentation liquor to prepare tetrahydrofuran (THF) |
| CN103554065A (en) * | 2013-10-16 | 2014-02-05 | 江阴奥瑞诺生物技术有限公司 | Method for preparing tetrahydrofuran by using succinic acid fermentation broth |
| CN103524327A (en) * | 2013-10-16 | 2014-01-22 | 江阴奥瑞诺生物技术有限公司 | Method for extracting succinic acid from succinic acid fermentation liquor by using electrodialysis method |
| CN105503578A (en) * | 2014-09-26 | 2016-04-20 | 常茂生物化学工程股份有限公司 | Method for extracting succinic acid from fermentation broth by use of extractant |
| CN105503578B (en) * | 2014-09-26 | 2018-03-02 | 常茂生物化学工程股份有限公司 | A kind of method for extracting succinic acid from zymotic fluid with extractant |
| CN106316836A (en) * | 2015-07-01 | 2017-01-11 | 中国石化扬子石油化工有限公司 | Method for preparing butanedioic acid |
| CN107033020A (en) * | 2017-06-10 | 2017-08-11 | 唐雪平 | A kind of method that theanine is extracted from tealeaves |
| CN107245032A (en) * | 2017-07-08 | 2017-10-13 | 桂林理工大学 | A kind of method that butanedioic acid is isolated and purified in the zymotic fluid from Bt |
| CN107245032B (en) * | 2017-07-08 | 2020-06-05 | 桂林理工大学 | Method for separating and purifying succinic acid from Bt fermentation liquor |
| CN110141969A (en) * | 2019-05-27 | 2019-08-20 | 常茂生物化学工程股份有限公司 | A kind of two compartment method electrolytic separation of Bipolar Membrane anode membrane continuously prepares L-TARTARIC ACID method |
| CN117263794A (en) * | 2023-09-19 | 2023-12-22 | 安徽固德生物工程有限公司 | Succinic acid purifying and refining method |
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