CN104876817A - Method for extracting succinic acid by employing succinic acid fermentation liquor - Google Patents
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Abstract
The invention relates to a method for extracting a succinic acid by employing a succinic acid fermentation liquor. The method comprises the following steps: (1) preparing a succinic acid fermentation liquor; (2) transforming succinate into succinic acid diammonium and acidizing the succinic acid fermentation liquor; (3) extracting the succinic acid; and (4) introducing a magnesium-salt ammonia production process and an acid and alkali recovery technology based on bipolar membrane electrodialysis, and recycling evaporable water, an ammonia gas, a magnesium carbonate suspension liquid and a hydrochloric acid. Clean production in the process is realized by intermediate products of the succinic acid diammonium; meanwhile, the problem that the succinic acid diammonium is transformed into the succinic acid by virtue of resin exchange in a traditional technological process, so that the discharge amount of wastewater is high is avoided; the process difficulty is lowered; and the method is a closed clean production process.
Description
Technical field
The present invention relates to a kind of use succinic acid fermentation liquor, through the method for succinic acid two ammonium procedure extraction succinic acid.The invention belongs to technical field of biochemical industry.
Background technology
Succinic acid (succinic acid) has another name called succsinic acid, is extensively present in organism, is a kind of important binary organic carboxyl acid, is also the important meta-bolites of microorganism tricarboxylic acid cycle glycolytic pathway.At present, succinic acid can be prepared by fermentable and obtain.
Fermentable is prepared in the process of succinic acid, according to the kind of microorganism and the difference of zymotechnique, creates the processing method of many different rear extractions.
The process of separation and purification removes insoluble impurities exactly, and succinate is converted into free succinic acid, and its concentration is brought up to required process.It is very crucial that the separation-extraction technology that a kind of route is short, cost is low, pollution-free, easy and simple to handle produces succinic acid for industrial fermentation.
The process of separation and purification removes insoluble impurities exactly, and succinate is converted into free succinic acid, and its concentration is brought up to required process.It is very crucial that the separation-extraction technology that a kind of route is short, cost is low, pollution-free, easy and simple to handle produces succinic acid for industrial fermentation.
Several extraction processes of current research have liquid-liquid extraction method, calcium salt perfectly crystallization process, ammonium sulfate cracking partition method and membrane separation process etc.
Liquid-liquid extraction method is a kind of respond well, widely used method in chemical industry, but employs a large amount of organic solvent in leaching process, its application in medicine food industry of the toxic effect of residual solvent.
Calcium salt method need consume a large amount of sulfuric acid, calcium oxide or calcium hydroxide, and can not recycle.
Embrane method extraction efficiency is high, but easily blocks in process, and flow process is unstable.
US5168055 discloses one and does not consume a large amount of reagent, the production of a large amount of by product and the technique of succinic acid purification is not produced yet, by product ammonium sulfate in production process can realize recycle, thus the cleaner production process that formation one is closed, succinic acid crystal is unique product, but this crystallisation process operational condition is harsher, and difficulty is larger.
CN101665428 provides a kind of method extracting succinic acid, employs ammonia, volatile salt or bicarbonate of ammonia and succinate is converted into succinic acid two ammonium, re-use Zeo-karb and be converted into succinic acid; Wherein the scavenging solution of cation regenerant exchange resin prepares ammonium salt as fertilizer application, and reuse magnesium precipitate thing is to fermentation system.The method use the traditional technology process of resins exchange, cause quantity of wastewater effluent large, and reclaim the whole evaporate to dryness of water needing when can be used as the ammonium salt of chemical fertilizer to clean, cost recovery is high.Whole flow process is failed to realize closed, and the salts substances that cannot use in removal process and hydrochloric acid, cause auxiliary material waste and problem of environmental pollution.This method is unsuitable for industrialization production requirements.
Summary of the invention
The object of the invention is to overcome defect of the prior art, a kind of method using succinic acid fermentation liquor to extract succinic acid is provided.
The present invention is achieved by the following technical programs.
Use succinic acid fermentation liquor to extract a method for succinic acid, its extracting method is as follows:
(1) preparation of succinic acid fermentation liquor
1. in fermentation cauldron, use seed culture medium to cultivate Actinobacillus succinogenes, the moiety of described seed culture medium is counted by mass concentration: peptone 5g/L, corn steep liquor 20g/L, glucose 20g/L, potassium primary phosphate 1.5g/L, Sodium phosphate dibasic 1.5g/L, yeast extract paste 5g/L, deionized water is prepared, the per minute volume intake needing carbonic acid gas in described fermentation cauldron is the fermenter volume of 0.1% ~ 0.5%, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, and maintenance system pH value is stabilized in 6.0-7.0;
2. the Actinobacillus succinogenes cultivated through seed culture medium is moved in fermention medium, carry out cultivating to obtain succinic acid fermentation liquor in fermentation cauldron, the moiety of described fermention medium is counted by mass concentration: peptone 5g/L, corn steep liquor 10g/L, glucose 100g/L, potassium primary phosphate 2.5g/L, Sodium phosphate dibasic 2.5g/L, yeast extract paste 5g/L, sodium acetate 5g/L, configure with deionized water, the per minute volume intake needing carbonic acid gas in described fermentation cauldron is the fermenter volume of 0.1% ~ 0.5%, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, maintenance system pH value is stabilized in 6.0-7.0, now the main component of succinic acid fermentation liquor is the substratum residue of succinic acid magnesium and fermenting process,
(2) process of succinic acid fermentation liquor
1. succinic acid fermentation liquor is entered ceramic film component by pump delivery, filter to obtain clear liquid;
2. proceeded to by clear liquid in succinic acid two ammonium conversion tank, ammonia enters bottom conversion tank, and after pH value to 10 ~ 10.2, reaction is complete, stops ammonia entering, reacts to obtain conversion fluid;
3. conversion fluid is entered ceramic film component by pump delivery and carry out secondary filtration, be separated succinic acid two ammonium and magnesium hydroxide solid, must contain clear liquid and the magnesium hydroxide suspension liquid of succinic acid two ammonium, magnesium hydroxide suspension liquid mass concentration reaches 20%;
4. proceeded in acidifying still by the clear liquid containing succinic acid two ammonium, the hydrochloric acid conditioning solution pH value adding 5% is 2, generates succinic acid and ammonium chloride mixing solutions;
(3) extraction of succinic acid
1. the mixing solutions after step (2) 4. processes is entered evaporator tower by pump delivery, in solution, water vapour flows out from evaporator tower top, and it is 25% ~ 30% that strength of solution is concentrated into succinic acid content, obtains concentrated solution;
2. concentrated solution is proceeded to crystallizer, mixing speed is 20 ~ 30rpm, and after control temperature is reduced to 8 ~ 10 DEG C, stop 4 hours, crystallization is complete;
3. the solution after step (3) 2. processes is proceeded to whizzer, centrifugal succinic acid crystal product and crystalline mother solution;
(4) Collection and utilization of by product
1. the Collection and utilization of vaporize water: the water vapour 1. flowed out through step (3) is reclaimed vaporize water through supercooler, can be used for needing arbitrarily water step;
2. the Collection and utilization of ammonia: the magnesium hydroxide suspension solution that crystalline mother solution step (3) 3. reclaimed and step (2) 3. reclaim mixes and proceeds to ammonia generation tank and react, control temperature is 120 ~ 130 DEG C, pressure 1.5 ~ 2kg/cm2, pH value is 9 ~ 10, the ammonia generated can proceed to step (2) and 2. utilize, crystalline mother solution and magnesium hydroxide suspension solution obtain reacting phase after completion of the reaction, and reacting phase is the magnesium chloride solution of mass concentration 20 ~ 25%;
3. the Collection and utilization of magnesiumcarbonate suspension liquid: sodium hydroxide solution is loaded injector, proceeds to after absorbing carbon dioxide in bipolar membrane electrodialysis equipment and generates hydrochloric acid and sodium carbonate; Proceed to magnesiumcarbonate generation tank by through step (4) reacting phase 2., mix with the sodium carbonate reclaimed in bipolar membrane electrodialysis equipment and generate the magnesiumcarbonate suspension liquid that the magnesia amount concentration of carbonic acid is 20%, magnesiumcarbonate suspension liquid can proceed to step (1) and 2. utilize;
4. the Collection and utilization of hydrochloric acid: recycling step (4) 3. generates hydrochloric acid in bipolar membrane electrodialysis equipment, can proceed to step (2) and 4. utilize.
Use succinic acid fermentation liquor to extract a method for succinic acid, wherein, in described succinic acid fermentation liquor, the mass percentage content of succinic acid magnesium is 8% ~ 12%.
Beneficial effect of the present invention is:
The preparation using Actinobacillus succinogenes (Actinobacillus succinogenes) CGMCC 1593 anaerobically fermenting to carry out succinic acid is one efficient method very reliably.Using magnesiumcarbonate as the PH conditioning agent in fermenting process, then in fermented liquid, main component is the substratum residue of succinic acid magnesium and fermenting process.
Be conducive to the process for cleanly preparing in implementation procedure through the intermediate product of succinic acid two ammonium in leaching process, other chemical involved in appropriate change process, reduction process difficulty, the requirement of suitability for industrialized production can be reached, and in process, adopt acidization that succinic acid two ammonium is converted into succinic acid, avoid in traditional technology process and employ resins exchange, cause the problem that quantity of wastewater effluent is large.
Find in experiment, if introduce the technique of magnesium salts Ammonia Process and bipolar membrane electrodialysis recovery soda acid in process, make the cleaning procedure that process reaches closed, reduce process difficulty simultaneously, such as, avoid the step etc. of pyrolytic decomposition monoammonium sulfate.Whole technological process, creates succinic acid crystal product, and vaporize water, ammonia, magnesiumcarbonate suspension liquid, hydrochloric acid are all recyclable with utilization, generate without other by products.
It should be noted that, due to fermentable feature, have a small amount of acetic acid to generate in fermented liquid, therefore acetic acid can be accumulated during the course, but this does not affect technological process and the method for this patent proposition.
Embodiment
Embodiment one
Use succinic acid fermentation liquor to extract a method for succinic acid, its extracting method is as follows:
(1) preparation of succinic acid fermentation liquor
1. peptone 5kg is taken, corn steep liquor 20kg, glucose 20kg, potassium primary phosphate 1.5kg, Sodium phosphate dibasic 1.5kg, yeast extract paste 5kg, deionized water 947kg is configured to the seed culture medium that total mass is 1000kg, uses seed culture medium to cultivate Actinobacillus succinogenes in fermentation cauldron, and the per minute volume intake needing carbonic acid gas in described fermentation cauldron is 10L, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, and maintenance system pH value is stabilized in 6.0-7.0;
2. peptone 50kg is taken, corn steep liquor 100kg, glucose 1000kg, potassium primary phosphate 25kg, Sodium phosphate dibasic 25kg, yeast extract paste 50kg, sodium acetate 50kg, deionized water 8700kg is configured to the fermention medium that total mass is 10000kg, the Actinobacillus succinogenes cultivated through seed culture medium is moved in fermention medium, ferment to obtain succinic acid fermentation liquor, now the main component of succinic acid fermentation liquor is the substratum residue of succinic acid magnesium and fermenting process, the mass percent concentration of succinic acid magnesium is 10%, the per minute volume intake needing carbonic acid gas in described fermentation cauldron is 10L, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, maintenance system pH value is stabilized in 6.0-7.0,
(2) process of succinic acid fermentation liquor
1. succinic acid fermentation liquor is entered ceramic film component by pump delivery, filter to obtain clear liquid;
2. proceeded to by clear liquid in succinic acid two ammonium conversion tank, ammonia enters bottom conversion tank, and after pH value to 10, reaction is complete, stops ammonia entering, reacts to obtain conversion fluid;
3. conversion fluid is entered ceramic film component by pump delivery and carry out secondary filtration, be separated succinic acid two ammonium and magnesium hydroxide solid, must contain clear liquid and the magnesium hydroxide suspension liquid of succinic acid two ammonium, magnesium hydroxide suspension liquid mass concentration reaches 20%;
4. proceeded in acidifying still by the clear liquid containing succinic acid two ammonium, add 5% hydrochloric acid 10 tons, mixing generates the mixing solutions of succinic acid 845kg and ammonium chloride 739kg;
(3) extraction of succinic acid
1. the mixing solutions after step (2) 4. processes is entered evaporator tower by pump delivery, in solution, water vapour flows out from evaporator tower top, and it is 25% that strength of solution is concentrated into succinic acid content, obtains concentrated solution;
2. concentrated solution is proceeded to crystallizer, mixing speed is 30rpm, and after control temperature is reduced to 10 DEG C, stop 4 hours, crystallization is complete;
3. the solution after step (3) 2. processes is proceeded to whizzer, centrifugal succinic acid crystal product 709kg and crystalline mother solution 2266kg;
(4) Collection and utilization of by product
1. the Collection and utilization of vaporize water: the water vapour 1. flowed out through step (3) is reclaimed vaporize water through supercooler, can be used for needing arbitrarily water step;
2. the Collection and utilization of ammonia: the magnesium hydroxide suspension solution that crystalline mother solution step (3) 3. reclaimed and step (2) 3. reclaim mixes and proceeds to ammonia generation tank and react, control temperature is 120 ~ 130 DEG C, pressure 1.5 ~ 2kg/cm2, pH value is 9 ~ 10, the ammonia generated can proceed to step (2) and 2. utilize, crystalline mother solution and magnesium hydroxide suspension solution obtain reacting phase 3324kg after completion of the reaction, and reacting phase is the magnesium chloride solution of mass concentration 20%;
3. the Collection and utilization of magnesiumcarbonate suspension liquid: sodium hydroxide solution is loaded injector, proceeds to after absorbing carbon dioxide in bipolar membrane electrodialysis equipment and generates hydrochloric acid and sodium carbonate; Proceed to magnesiumcarbonate generation tank by through step (4) reacting phase 2., mix with the sodium carbonate reclaimed in bipolar membrane electrodialysis equipment and generate the magnesiumcarbonate suspension liquid 2957kg that the magnesia amount concentration of carbonic acid is 20%, magnesiumcarbonate suspension liquid can proceed to step (1) and 2. utilize;
4. the Collection and utilization of hydrochloric acid: recycling step (4) 3. generates hydrochloric acid in bipolar membrane electrodialysis equipment, can proceed to step (2) and 4. utilize.
As can be seen from the above-described embodiment, the process for cleanly preparing in process is achieved through the intermediate product of succinic acid two ammonium, avoid in traditional technology process simultaneously and employ resins exchange succinic acid two ammonium is converted into succinic acid, cause the problem that quantity of wastewater effluent is large, and in process, introduce the technique of magnesium salts Ammonia Process and bipolar membrane electrodialysis recovery soda acid, make the cleaning procedure that process reaches closed, reduce process difficulty simultaneously; Whole technological process creates succinic acid crystal product, and vaporize water, ammonia, magnesiumcarbonate suspension liquid, hydrochloric acid are all recyclable with utilization, generate without other by products.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments, and therefore, the present invention is not by the restriction of the present embodiment, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (2)
1. use succinic acid fermentation liquor to extract a method for succinic acid, it is characterized by, its extracting method is as follows:
(1) preparation of succinic acid fermentation liquor
1. in fermentation cauldron, use seed culture medium to cultivate Actinobacillus succinogenes, the moiety of described seed culture medium is counted by mass concentration: peptone 5g/L, corn steep liquor 20g/L, glucose 20g/L, potassium primary phosphate 1.5g/L, Sodium phosphate dibasic 1.5g/L, yeast extract paste 5g/L, deionized water is prepared, the per minute volume intake needing carbonic acid gas in described fermentation cauldron is the fermenter volume of 0.1% ~ 0.5%, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, and maintenance system pH value is stabilized in 6.0-7.0;
2. the Actinobacillus succinogenes cultivated through seed culture medium is moved in fermention medium, carry out cultivating to obtain succinic acid fermentation liquor in fermentation cauldron, the moiety of described fermention medium is counted by mass concentration: peptone 5g/L, corn steep liquor 10g/L, glucose 100g/L, potassium primary phosphate 2.5g/L, Sodium phosphate dibasic 2.5g/L, yeast extract paste 5g/L, sodium acetate 5g/L, configure with deionized water, the per minute volume intake needing carbonic acid gas in described fermentation cauldron is the fermenter volume of 0.1% ~ 0.5%, in process, stream adds the magnesiumcarbonate suspension liquid that magnesiumcarbonate mass concentration is 20%, maintenance system pH value is stabilized in 6.0-7.0, now the main component of succinic acid fermentation liquor is the substratum residue of succinic acid magnesium and fermenting process,
(2) process of succinic acid fermentation liquor
1. succinic acid fermentation liquor is entered ceramic film component by pump delivery, filter to obtain clear liquid;
2. proceeded to by clear liquid in succinic acid two ammonium conversion tank, ammonia enters bottom conversion tank, and after pH value to 10 ~ 10.2, reaction is complete, stops ammonia entering, reacts to obtain conversion fluid;
3. conversion fluid is entered ceramic film component by pump delivery and carry out secondary filtration, be separated succinic acid two ammonium and magnesium hydroxide solid, must contain clear liquid and the magnesium hydroxide suspension liquid of succinic acid two ammonium, magnesium hydroxide suspension liquid mass concentration reaches 20%;
4. proceeded in acidifying still by the clear liquid containing succinic acid two ammonium, the hydrochloric acid conditioning solution pH value adding 5% is 2, generates succinic acid and ammonium chloride mixing solutions;
(3) extraction of succinic acid
1. the mixing solutions after step (2) 4. processes is entered evaporator tower by pump delivery, in solution, water vapour flows out from evaporator tower top, and it is 25% ~ 30% that strength of solution is concentrated into succinic acid content, obtains concentrated solution;
2. concentrated solution is proceeded to crystallizer, mixing speed is 20 ~ 30rpm, and after control temperature is reduced to 8 ~ 10 DEG C, stop 4 hours, crystallization is complete;
3. the solution after step (3) 2. processes is proceeded to whizzer, centrifugal succinic acid crystal product and crystalline mother solution;
(4) Collection and utilization of by product
1. the Collection and utilization of vaporize water: the water vapour 1. flowed out through step (3) is reclaimed vaporize water through supercooler, can be used for needing arbitrarily water step;
2. the Collection and utilization of ammonia: the magnesium hydroxide suspension solution that crystalline mother solution step (3) 3. reclaimed and step (2) 3. reclaim mixes and proceeds to ammonia generation tank and react, control temperature is 120 ~ 130 DEG C, pressure 1.5 ~ 2kg/cm2, pH value is 9 ~ 10, the ammonia generated can proceed to step (2) and 2. utilize, crystalline mother solution and magnesium hydroxide suspension solution obtain reacting phase after completion of the reaction, and reacting phase is the magnesium chloride solution of mass concentration 20 ~ 25%;
3. the Collection and utilization of magnesiumcarbonate suspension liquid: sodium hydroxide solution is loaded injector, proceeds to after absorbing carbon dioxide in bipolar membrane electrodialysis equipment and generates hydrochloric acid and sodium carbonate; Proceed to magnesiumcarbonate generation tank by through step (4) reacting phase 2., mix with the sodium carbonate reclaimed in bipolar membrane electrodialysis equipment and generate the magnesiumcarbonate suspension liquid that the magnesia amount concentration of carbonic acid is 20%, magnesiumcarbonate suspension liquid can proceed to step (1) and 2. utilize;
4. the Collection and utilization of hydrochloric acid: recycling step (4) 3. generates hydrochloric acid in bipolar membrane electrodialysis equipment, can proceed to step (2) and 4. utilize.
2. a kind of method using succinic acid fermentation liquor to extract succinic acid as claimed in claim 1, the mass percentage content that it is characterized by succinic acid magnesium in described succinic acid fermentation liquor is 8% ~ 12%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566096A (en) * | 2015-12-18 | 2016-05-11 | 江西科技师范大学 | Technique for separating and purifying succinic acid from microbial fermentation liquid |
| CN110373432A (en) * | 2018-04-12 | 2019-10-25 | 中国科学院过程工程研究所 | It is a kind of using synthesis gas as the system and its processing method of raw material coproduction succinic acid and alcohols |
| CN114540433A (en) * | 2022-02-17 | 2022-05-27 | 山东飞扬化工有限公司 | Process method for producing succinic acid and purification method thereof |
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| US5168055A (en) * | 1986-06-11 | 1992-12-01 | Rathin Datta | Fermentation and purification process for succinic acid |
| CN101348428A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | Method for extracting amber acid in fermentation liquor by anion resin adsorption |
| CN101748161A (en) * | 2010-01-19 | 2010-06-23 | 南京工业大学 | Process for purifying succinic acid by anaerobic fermentation |
| 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 |
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| US5168055A (en) * | 1986-06-11 | 1992-12-01 | Rathin Datta | Fermentation and purification process for succinic acid |
| CN101348428A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | Method for extracting amber acid in fermentation liquor by anion resin adsorption |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105566096A (en) * | 2015-12-18 | 2016-05-11 | 江西科技师范大学 | Technique for separating and purifying succinic acid from microbial fermentation liquid |
| CN105566096B (en) * | 2015-12-18 | 2018-11-16 | 江西科技师范大学 | A kind of technique isolating and purifying succinic acid from microbial fermentation solution |
| CN110373432A (en) * | 2018-04-12 | 2019-10-25 | 中国科学院过程工程研究所 | It is a kind of using synthesis gas as the system and its processing method of raw material coproduction succinic acid and alcohols |
| CN114540433A (en) * | 2022-02-17 | 2022-05-27 | 山东飞扬化工有限公司 | Process method for producing succinic acid and purification method thereof |
| CN114540433B (en) * | 2022-02-17 | 2023-07-25 | 山东飞扬化工有限公司 | Technological method for producing succinic acid and purification method thereof |
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