CN101665428B - Method for extracting succinic acid from succinic acid fermentation liquor - Google Patents
Method for extracting succinic acid from succinic acid fermentation liquor Download PDFInfo
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- CN101665428B CN101665428B CN 200910178134 CN200910178134A CN101665428B CN 101665428 B CN101665428 B CN 101665428B CN 200910178134 CN200910178134 CN 200910178134 CN 200910178134 A CN200910178134 A CN 200910178134A CN 101665428 B CN101665428 B CN 101665428B
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Abstract
The invention provides a method for extracting succinic acid from succinic acid fermentation liquor. The method includes that succinic acid fermentation liquor produced by anaerobic fermentation is filtered, filtrate directly reacts with ammonia water, ammonium carbonate or ammonium bicarbonate, the obtained filtrate is treated by resin, the obtained solution is subject to decolouration, concentration and centrifugal separation, thus obtaining succinic acid crystal. The method of the invention has the characteristics of low raw material consumption, simpler technology, short operational process, easy control and low cost.
Description
Technical field
The present invention relates to a kind of separating and extracting method of Succinic Acid, specifically, relate to a kind of method of from the Succinic Acid fermented liquid, extracting Succinic Acid.
Background technology
Succinic Acid claims succsinic acid again, is widely used in medicine, agricultural chemicals, fuel, spices, paint, food, plastics and photographic material industry.Succinic Acid is a kind of outstanding chemical platform product as a kind of tetra-carbonic, and it can replace a lot of commodity based on benzene and petrochemical industry intermediate product, and this can reduce the produced pollution in surpassing the production and consumption process of 250 kinds of phenyl chemical preparationss.The preparation method of Succinic Acid mainly contains two kinds at present: the one, and by petrification production, the 2nd, with Production by Microorganism Fermentation.Petrification production cost height, seriously polluted, limited significantly; But advantages such as raw materials cost is cheap and renewable, fermenting process absorbing carbon dioxide, environmental protection that the Production by Microorganism Fermentation Succinic Acid has are furtherd investigate widely.The method of extracting Succinic Acid at present is generally: fermented liquid is removed thalline by pre-treatment, extracts by methods such as ion-exchange, electrodialysis or solvent extractions then.
US Patent No. 5168055 discloses the method for calcium salt method extraction Succinic Acid, and its shortcoming is for producing the calcium sulfate waste.The method that US Patent No. 5958744 adopts ammonium salt to extract Succinic Acid needs Pintsch process vitriol, complex process, running cost height.US Patent No. 5034105 discloses the method for electroosmose process extraction Succinic Acid, this method energy consumption height, and can not handle divalent cation.Chinese patent CN1887843A discloses the method for acidifying extraction Succinic Acid, and there are a large amount of inorganic salt in this method in crystallisation process, be unfavorable for the carrying out of crystallisation process.Chinese patent CN101348429A discloses the method that a kind of resin cation exchange is extracted Succinic Acid in the fermented liquid, carries out wash-out with bicarbonate of ammonia in its production process, need the sodium bicarbonate that obtains is removed ammonia, and resin regeneration is loaded down with trivial details.Chinese patent CN101348428A discloses the method that a kind of resin anion(R.A) extracts Succinic Acid in the fermented liquid, and its resin absorption amount is little, does not possess industrial value.Solvent extration needs to consume a large amount of expensive organic solvents in the process of extracting, the toxicity of residual solvent has detrimentally affect to quality product.
In sum, extract the method production cost height of Succinic Acid at present in the Succinic Acid fermented liquid, complex process is unfavorable for suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of processing condition and simplify, easy and simple to handle, cost is low, good product quality, the Succinic Acid separating and extracting method that no waste produces.
In order to realize the object of the invention, a kind of method of from the Succinic Acid fermented liquid, extracting Succinic Acid of the present invention, it comprises the steps:
1) earlier the Succinic Acid filtering fermentation liquor is removed thalline, obtain clear filtrate;
2) then filtrate is reacted with ammoniacal liquor, volatile salt or bicarbonate of ammonia or its mixture each other, filter magnesium salts and ammonium succinate solution;
3) again with ammonium succinate solution through Zeo-karb handle Succinic Acid.
Wherein, described Succinic Acid fermented liquid is that anaerobion obtains the glucide conversion, because magnesium salts is beneficial to the microorganism synthesizing succinic acid, contains the solution that magnesium salts is the master so its tunning mostly is, and its filter type can adopt modes such as flocculation filtration or membrane filtration to carry out.
Described flocculation filtration mode, its flocculation agent that adopts is polyacrylamide, consumption is 10-80ppm, stirs 5-30min and carry out centrifugation under temperature is 70-95 ℃.
Described membrane filtration mode, it adopts the aperture is that the film of 0.05-0.2um specification is handled under 70-90 ℃.
Step 2) ammoniacal liquor, volatile salt or bicarbonate of ammonia or its mixture each other are as reagent in, consumption is the equivalent proportioning between its Succinic Acid magnesium solution and the reagent, temperature of reaction is 10-85 ℃, and the reaction times is 0.5-2h, and reagent is good to select volatile salt.
Step 2) filters the magnesium salts or the magnesium hydroxide that obtain in and can carry out recycling for the fermentation of Succinic Acid.
Zeo-karb is used for removing the ammonium succinate ammonium ion in the step 3), and it adopts storng-acid cation exchange resin or weakly acidic cation-exchange resin.
The used Zeo-karb of the present invention can carry out manipulation of regeneration, such as adopting organic acid or mineral acid to carry out manipulation of regeneration as eluent, with the ammonium ion in the absorption exchange resin column.Be good with sulfuric acid or hydrochloric acid wherein.
The ammonium salt (ammonium sulfate or ammonium chloride) that absorption obtains also can use as the nitrogenous source of fermention medium or as farm crop fertilizer through the ammonium salt finished product that concentrates, crystallization obtains.
The Succinic Acid solution that step 3) obtains further through the technology of this area routine decolour, concentrate, crystallization obtains the Succinic Acid finished product.
Such as, can adopt Succinic Acid solution is heated to 50-60 ℃, add the powder activity carbon decoloring 30-60min that treats de-inking solution volume 0.3-1.0%, remove gac with Plate Filtration, after the destainer that obtains had been concentrated into the crystal appearance, the beginning decrease temperature crystalline was separated out the Succinic Acid crystal.The Succinic Acid magma liquid of gained obtains the Succinic Acid crystal through centrifugation.
After Succinic Acid fermented liquid of the present invention is handled after filtration, neutralize with ammoniacal liquor or volatile salt or bicarbonate of ammonia or its mixture, obtain magnesium hydroxide or magnesiumcarbonate or both mixtures through centrifugation, and the ammonium succinate that obtains exchanged with Zeo-karb, effluent liquid is Succinic Acid, through decolouring, concentrate, crystallization obtains the Succinic Acid product.It is low that the present invention has consumption of raw and auxiliary materials, is convenient to take continuous operation, and work simplification, and operating process is few, is easy to characteristics such as control.
The present invention adopts the Succinic Acid fermented liquid that contains magnesium ion is extracted, its magnesium hydroxide that obtains, magnesiumcarbonate can be directly used in the upstream fermentation procedure, the ammonium succinate that obtains can obtain Succinic Acid solution through the direct processing of resin, the while producing ammonium sulfate byproduct, this technological operation is simple, be convenient to control, product yield has higher economy, environment protection significance to high.
Description of drawings
Fig. 1 extracts the process flow diagram of Succinic Acid from the Succinic Acid fermented liquid for the present invention.
Embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
Obtain the Succinic Acid fermented liquid through microbiological anaerobic fermenting carbohydrate material.
With Succinic Acid fermented liquid 30L, add flocculation agent polyacrylamide 0.9g, in 85 ℃ of stirring 30min, centrifugation obtains filtrate--Succinic Acid magnesium fermentation clear liquid.Be that 17% ammonia soln slowly is added in the Succinic Acid magnesium fermentation clear liquid that 35L concentration is 5.6% (g/100ml) with mass volume ratio (g/100ml), its add-on is 2.8L, kept 1 hour, and centrifugation, and use the less water washing leaching cake.The gained magnesium hydroxide can use for the Succinic Acid fermentation.
The ammonium succinate solution 35.6L that obtains after centrifugal, flow velocity by 1.5BV/h pumps into 001 * 7 cationic exchange coloum, and effluent liquid is Succinic Acid solution, uses less water drip washing then behind the friendship post, dilution heat of sulfuric acid with 4% (g/100ml) is regenerated, and regenerated liquid is ammoniumsulphate soln.
Succinic Acid solution adds the gac of its volume 0.3% in 60 ℃ of decolourings 1 hour.Again 60 ℃ of temperature, be concentrated into crystal under vacuum tightness-0.095mpa and occur, obtain the Succinic Acid finished product with the speed decrease temperature crystalline of 2 ℃/h.The Succinic Acid yield is 86.3%, the magnesium rate of recovery 91.5%.
Embodiment 2
Obtain the Succinic Acid fermented liquid through microbiological anaerobic fermenting carbohydrate material.
With Succinic Acid fermented liquid 30L, add flocculation agent polyacrylamide 0.9g, in 85 ℃ of stirring 20min, centrifugation obtains Succinic Acid magnesium fermentation clear liquid.The ammonium carbonate solution of 30% (g/100ml) slowly is added in the Succinic Acid magnesium fermentation clear liquid that 35L concentration is 5.8% (g/100ml), and its add-on is 4.3L, kept 1 hour, and centrifugation, and use the less water washing leaching cake.Gained magnesiumcarbonate uses for the Succinic Acid fermentation.
The ammonium succinate solution 37.1L that obtains after centrifugal pumps into 001 * 7 cationic exchange coloum by the flow velocity of 1.5BV/h, and effluent liquid is Succinic Acid solution., regenerate with 4% dilution heat of sulfuric acid behind the friendship post with less water drip washing, regenerated liquid is ammoniumsulphate soln.
Succinic Acid solution adds the gac of its volume 0.5% in 50 ℃ of decolourings 1 hour.Obtain the Succinic Acid finished product through concentrated, crystallization again.The Succinic Acid yield is 88.6%, the magnesium rate of recovery 93.1%.
Embodiment 3
Obtain the Succinic Acid fermented liquid through microbiological anaerobic fermenting carbohydrate material.
With Succinic Acid fermented liquid 30L, the employing aperture is that the film of 0.05um specification filters under 70 ℃, obtains Succinic Acid magnesium fermentation clear liquid.Ammonium bicarbonate aqueous solution with 30% slowly is added in the Succinic Acid magnesium fermentation clear liquid that 36L concentration is 5.4% (g/100ml), and its add-on is 7.8L, kept 1 hour, and centrifugation, and use the less water washing leaching cake.Gained magnesiumcarbonate uses for the Succinic Acid fermentation.
The ammonium succinate solution 40.8L that obtains after centrifugal pumps into 001 * 7 cationic exchange coloum by the flow velocity of 1.5BV/h, and effluent liquid is Succinic Acid solution., regenerate with 4% dilution heat of sulfuric acid behind the friendship post with less water drip washing, regenerated liquid is ammoniumsulphate soln.
Succinic Acid solution adds the gac of its volume 0.8% in 60 ℃ of decolourings 1 hour.Obtain the Succinic Acid finished product through concentrated, crystallization again.The Succinic Acid yield is 86.3%, the magnesium rate of recovery 90.6%.
Embodiment 4
Obtain the Succinic Acid fermented liquid through microbiological anaerobic fermenting carbohydrate material.
With Succinic Acid fermented liquid 30L, add flocculation agent polyacrylamide 1.2g, in 85 ℃ of stirring 25min, centrifugation obtains Succinic Acid magnesium fermentation clear liquid.The volatile salt of 17% ammoniacal liquor and 30% slowly was added to after the proportioning in the Succinic Acid magnesium fermentation clear liquid that 37.6L concentration is 5.2% (g/100ml) by 1: 3, and its add-on is 3.8L, kept 1 hour, and centrifugation, and use the less water washing leaching cake.Gained magnesiumcarbonate uses for the Succinic Acid fermentation.
The ammonium succinate solution 38.2L that obtains after centrifugal pumps into the exchange column that 001 * 8 resin cation (R.C.) is housed by the flow velocity of 1.5BV/h, and effluent liquid is Succinic Acid solution., regenerate with 4% dilution heat of sulfuric acid behind the friendship post with less water drip washing, regenerated liquid is ammoniumsulphate soln.Succinic Acid solution adds the gac of its volume 0.3% in 60 ℃ of decolourings 0.5 hour.Obtain the Succinic Acid finished product through concentrated, crystallization again.The Succinic Acid yield is 87.7%, the magnesium rate of recovery 92.5%.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (3)
1. a method of extracting Succinic Acid from the Succinic Acid fermented liquid is characterized in that, is made up of following steps:
1) earlier the Succinic Acid filtering fermentation liquor is removed thalline, obtain filtrate; Wherein, the flocculation filtration mode is adopted in described filtration, and the flocculation agent of employing is polyacrylamide, and consumption is 10-80ppm, stirs 5-30min and carry out centrifugation under temperature is 70-95 ℃;
2) then filtrate is reacted with ammoniacal liquor, volatile salt or bicarbonate of ammonia or its mixture each other, filter magnesium salts and ammonium succinate solution;
3) again with ammonium succinate solution through storng-acid cation exchange resin or weakly acidic cation-exchange resin handle Succinic Acid;
Wherein, described Succinic Acid fermented liquid is to contain magnesium salts;
Wherein, described storng-acid cation exchange resin or weakly acidic cation-exchange resin adopt organic acid or mineral acid to carry out manipulation of regeneration as eluent.
2. method according to claim 1 is characterized in that step 2) in ammoniacal liquor, volatile salt or bicarbonate of ammonia or its mixture each other be that equivalent reacts with the filtrate reaction, temperature of reaction is 10-85 ℃, the reaction times is 0.5-2h.
3. method according to claim 1 is characterized in that, the Succinic Acid that step 3) obtains further decolours, concentrates, crystallization obtains the Succinic Acid finished product.
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| CN102617325B (en) * | 2011-01-27 | 2014-12-24 | 中国科学院过程工程研究所 | Method for decoloration of succinic acid fermentation broth by ion exchange resin |
| CN102323263A (en) * | 2011-08-19 | 2012-01-18 | 南宁奕德环境科技有限公司 | Method for rapidly detecting succinic acid content in fermentation broth |
| CN102321682B (en) * | 2011-09-13 | 2013-01-23 | 南京工业大学 | Method for recycling water from separation process of succinic acid by fermentation |
| CN103012107B (en) * | 2013-01-21 | 2015-07-08 | 江阴奥瑞诺生物技术有限公司 | Method for preparing succinic acid amine from fermentation liquor for preparing succinic acid |
| TWI525074B (en) * | 2014-04-30 | 2016-03-11 | 財團法人工業技術研究院 | Method for purifying an organic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1860237A (en) * | 2003-09-30 | 2006-11-08 | 味之素株式会社 | Method for purifying succinic acid from fermentation broth |
| CN1887843A (en) * | 2006-07-18 | 2007-01-03 | 南京工业大学 | Process of separating and extracting succinic acid from anaerobic fermented liquid |
| CN101348429A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | Method for extracting amber acid in fermentation liquor by cationic resin exchange |
| CN101486637A (en) * | 2009-02-09 | 2009-07-22 | 常茂生物化学工程股份有限公司 | Method for extracting amber acid from fermentation liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1860237A (en) * | 2003-09-30 | 2006-11-08 | 味之素株式会社 | Method for purifying succinic acid from fermentation broth |
| CN1887843A (en) * | 2006-07-18 | 2007-01-03 | 南京工业大学 | Process of separating and extracting succinic acid from anaerobic fermented liquid |
| CN101348429A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | Method for extracting amber acid in fermentation liquor by cationic resin exchange |
| CN101486637A (en) * | 2009-02-09 | 2009-07-22 | 常茂生物化学工程股份有限公司 | Method for extracting amber acid from fermentation liquor |
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