CN1887843A - Process of separating and extracting succinic acid from anaerobic fermented liquid - Google Patents

Process of separating and extracting succinic acid from anaerobic fermented liquid Download PDF

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CN1887843A
CN1887843A CN 200610086003 CN200610086003A CN1887843A CN 1887843 A CN1887843 A CN 1887843A CN 200610086003 CN200610086003 CN 200610086003 CN 200610086003 A CN200610086003 A CN 200610086003A CN 1887843 A CN1887843 A CN 1887843A
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succinic acid
fermented liquid
separating
filtration
extracting
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CN100445257C (en
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姚忠
吴昊
刘辉
李松
姜岷
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The present invention discloses process of separating and extracting succinic acid from anaerobic fermented liquid. The process includes filtering the fermented liquid of succinic acid with microfiltering membrane, filtering with ultrafiltering membrane, decolorizing and depurating with active carbon to obtain clarified succinic acid solution, concentrating, and crystallizing to obtain succinic acid product. The process has the features of mild condition, simple operation, short separating path, low cost, high selectivity and high product quality.

Description

A kind of from anaerobic fermented liquid the method for separating and extracting succinic acid
Technical field
The present invention relates to a kind of separating and extracting method of Succinic Acid, particularly relate to a kind of method of utilizing membrane sepn, activated carbon decolorizing and crystallization technique separating and extracting succinic acid from the fermented liquid of Unareobic fermentation preparation.
Background technology
Succinic Acid (Succinic Acid, Butanedioic Acid) is called succsinic acid again, is a kind of binary organic acid, and it is a kind of important C 4The hardware and software platform compound can be used as the intermediate that synthesizes complex organic compound, is widely used in pharmacy, food-processing, synthetic plastics, rubber, protective coating, dyestuff and other industry.
The preparation method of Succinic Acid mainly contains two kinds, and the one, by petrification production, the 2nd, with Production by Microorganism Fermentation.Petrification produce succinic acid traditionally is subjected to bigger restriction because of reasons such as cost and environmental pollution make the industrial scale of Succinic Acid and use.The Production by Microorganism Fermentation Succinic Acid is because its efficient height, numerous advantages such as cost is low, pollution is little; studied extensively and profoundly; large-scale production has abroad been arranged; the domestic research starting evening that fermentation method is prepared Succinic Acid; be not applied to actual production as yet; but, be that the fermentation method of raw material prepares the Succinic Acid technology and is subjected to just day by day paying close attention to widely with the renewable resources along with the minimizing day by day of fossil resource.
At present, Succinic Acid commonly used produces bacterium to be had and separates from cud, as Ruminocoddus flavefaciens and Fibrobacter succinogenes, Anaerobiospirillum succiniciproducens (ATCC 53488) utilizes the glucide metabolism to produce the representative of the cud bacterium of Succinic Acid.Typical stomach bacterium: E.coli, Pectinatus sp., Bacteroides sp.; The cud bacterium is as Mannheimia succiniciproducens MBEL55E, Prevotellaruminicola (ATCC 19188), Succinimonas amylolytica (ATCC 19716), Ruminobacteramylophilus (DSM 1361) also is the bacterial strain that can accumulate Succinic Acid.
National Engineering Research Center for Biotechnology (Nanjing) utilizes product succsinic acid actinobacillus (Actinobacillussuccinogenes) NJ113 (to be preserved in China Committee for Culture Collection of Microorganisms common micro-organisms center at present, deposit number is CGMCC No.1716, preservation date is on 05 18th, 2006, the annex submission as No. 200610085415.9 patent applications to State Intellectual Property Office of preservation proof) fermentation method prepares the Succinic Acid aspect and is attended by the most momentous results, and the separation and Extraction work of Succinic Acid has been become the emphasis of research.
The above-mentioned various system of utilizing microbe fermentation method to prepare Succinic Acid all has some common features, promptly be anaerobically fermenting, contained main component comprises thalline, particulate state nutrient media components, solubility biomacromolecule, small organic molecule and organic acid (formic acid, acetate, Succinic Acid etc.) etc. in the fermented liquid.Therefore, preparing the Succinic Acid system at the mentioned microorganism fermentation method carries out the downstream Study on Technology and has important practice significance.
The patent of utilizing the microbial fermentation preparation to extract Succinic Acid at present has: US5034105 (1991), US5168055 (1992), US5143834 (1992), US5958744 (1999) etc.; its patent protection content relates generally to fermentation bacterial classification, zymotechnique and extraction process, and the domestic patent report that does not also have at the Succinic Acid separating and extracting method that adopts the fermentation method preparation.
In above-mentioned disclosed patent, the method of separating the purification Succinic Acid from fermented liquid is generally described as: fermented liquid is removed thalline etc. by pre-treatment, extract by methods such as ion-exchange or electrodialysis or solvent extractions then, condensing crystal obtains the pure product of Succinic Acid then.For example patent US5168055 adopts the calcium salt method separating and extracting succinic acid, adopts at first during the fermentation and adds calcium hydroxide adjusting pH value, and crystallization goes out calcium succinate in fermented liquid.Fermented liquid obtains the mixed precipitation of insoluble substance such as thalline, albumen and calcium succinate after filtration, then by constantly washing, removes materials such as thalline in the precipitation and albumen; Crystal after washing changes soluble Succinic Acid and insoluble calcium sulfate (gypsum) into by adding the vitriol oil; The free Succinic Acid after filtration, two secondary ions hand over resin purification to remove the negative and positive foreign ion respectively, and then obtain Succinic Acid by crystallization, and the content of Succinic Acid is 80~99% in the product.
Adopt these technologies separating and extracting succinic acid from fermented liquid to have following problem:
Control normally carrying out of fermentation owing to need to add a large amount of calcium magnesium salts in the fermenting process, so high-content ionic substance quickening resin is saturated, increases the resin regeneration number of times, causes problems such as quantity of wastewater effluent is big.
The employing calcium salt method, because salts contg height in the fermented liquid, resin stain is serious, and the regeneration difficulty is not suitable for ion exchange method and handles, and needs in addition to handle a large amount of solids and slurries, and produces a large amount of gypsum offscum pollutions, and the acid and alkali consumption amount is big.Adopt electroosmose process, route is long, the energy consumption height, and the processing foreign ion has significant limitation, and big to facility investment, operational difficulty.Adopt solvent extration, need to consume a large amount of expensive organic solvents in leaching process, the toxicity of residual solvent has detrimentally affect to the quality of food grade and pharmaceutical grade product, and this method is not suitable for the fermented liquid system of high ionic strength simultaneously.The crystallisation process operational condition of ammonium salt process route length is relatively harsher, also needs Pintsch process vitriol, complex steps, and difficulty is big.The operational path that all exists of above patent is grown (6~8 step lock out operation unit), process cost height in a word; implement shortcomings such as difficulty is big, environmental pollution is serious; increased running cost, be unfavorable for that fermentation method prepares the large-scale production of Succinic Acid, has weakened competition capability.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of processing condition gentleness is provided, easy and simple to handle, route is short, cost is low, and selectivity is good, the method for utilizing membrane sepn, activated carbon decolorizing and crystallization technique separating and extracting succinic acid from anaerobic fermented liquid that quality product is high.
The objective of the invention is to realize by following technical measures:
Provided by the invention from anaerobic fermented liquid the basic step of the method for separating and extracting succinic acid be will produce through anaerobically fermenting the Succinic Acid fermented liquid adopt little (hole) membrane filtration, to remove thalline and the bigger contaminant particles of other particles, use the ultra-filtration membrane ultrafiltration then, remove the macromolecular substance such as protein that exist in the fermented liquid, use decolorization and impurity removal by active carbon again, remove small molecular weight impurity and residual proteins such as pigment, obtain clarifying Succinic Acid solution, concentrating under reduced pressure, the formic acid that is contained in the separation solution, impurity organic acids such as acetate, crystallization obtain high-quality Succinic Acid product (wherein the content of Succinic Acid reaches more than 99.5%).
A kind of from anaerobic fermented liquid the method for separating and extracting succinic acid, this method may further comprise the steps:
To adopt micro-filtrate membrane filtration through the Succinic Acid fermented liquid that anaerobically fermenting is produced, and use the ultra-filtration membrane ultrafiltration then, and use decolorization and impurity removal by active carbon again, and obtain clarifying Succinic Acid solution, and concentrate, crystallization obtains the Succinic Acid product.
The method of described separating and extracting succinic acid, wherein adopting micro-filtrate membrane filtration is that the Succinic Acid fermented liquid through anaerobically fermenting production is diluted with water to 1.25~2 times of original volume, and regulate fermented liquid pH to acid, by the aperture is that the microfiltration membrane of 0.1~0.5 μ m is carried out cross flow filter, working pressure is 0.05~0.1MPa, service temperature is 15~40 ℃, 10~20 times of cycles of concentration, the dialysis water yield account for dilution secondary fermentation liquid long-pending 20~70%.
The method of described separating and extracting succinic acid, wherein to be diluted with water to the multiple of original volume be 1.25~1.75 times to the Succinic Acid fermented liquid, the aperture of microfiltration membrane is 0.1~0.2 μ m, the micro-filtration working pressure is 0.05~0.08MPa, service temperature is 20~35 ℃, cycles of concentration is 15~20 times, the dialysis water yield account for dilution secondary fermentation liquid long-pending 20~50%.
The method of described separating and extracting succinic acid, be that to adopt molecular weight cut-off be that 6000~10000 daltonian ultra-filtration membranes carry out cross flow filter for Succinic Acid fermented liquid after filtering with microporous membrane is handled wherein with the ultra-filtration membrane ultrafiltration, ultrafiltration pressure 0.1~0.5MPa, temperature is 15~40 ℃, 30~40 times of cycles of concentration, the dialysis water yield accounts for 5~20% of micro-filtrate volume.
The method of described separating and extracting succinic acid is 8000~10000 with the ultra-filtration membrane molecular weight that dams wherein, and ultrafiltration pressure is 0.1~0.4MPa, and service temperature is 20~40 ℃, and cycles of concentration is 35~40 times, and the dialysis water yield accounts for 5~10% of micro-filtrate volume.
The method of described separating and extracting succinic acid, be to adopt Powdered Activated Carbon to remove pigment and removal of impurities the Succinic Acid fermented liquid after the ultrafiltration wherein with decolorization and impurity removal by active carbon, operational condition is under 200 rev/mins mixing speed, the Powdered Activated Carbon addition is counted 0.3~0.5% of ultrafiltrated volume with the quality volume percent, bleaching temperature is 40~60 ℃, decoloured 30~45 minutes, carry out press filtration, filter cake is with 30~50 ℃ pure water circulation cleaning 3 times, pure water washing consumption account for activated carbon decolorizing liquid long-pending 5~15%, to decolour filtrate and wash water merges, and obtains clarifying Succinic Acid solution.
The method of described separating and extracting succinic acid, wherein the Powdered Activated Carbon addition is counted 0.3~0.4% of ultrafiltrated volume with the quality volume percent, service temperature is 40~50 ℃, and bleaching time is 30 minutes, filter cake pure water washing consumption account for activated carbon decolorizing liquid long-pending 5~10%.
The method of described separating and extracting succinic acid, wherein the method for the condensing crystal of fermented liquid is that the Succinic Acid feed liquid behind the decolouring purifying is transferred to pH2.0~3.5, reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 55~70 ℃, 4~6 times of cycles of concentration, crystallisation by cooling obtains the Succinic Acid crystal again.
By regulating pH is that acidity makes organic acid impurity be molecular state, can make its boiling point lowering.Because formic acid, acetate, the boiling point of Succinic Acid is respectively 100.8 ℃, 118.1 ℃, 235 ℃, formic acid wherein, the boiling point of acetate and the boiling point of water are approaching, the part formic acid that in concentrating under reduced pressure, can remove in the solution to be contained, VFA impurity such as acetate, (Succinic Acid solubleness in water is 68g/L (20 ℃) according to the dissolubility difference of Succinic Acid and other solubility organic acid impurity then, and formic acid, acetate can dissolve each other with arbitrary proportion with water), therefore adopt the crystallisation by cooling method promptly can be with Succinic Acid and formic acid, organic acid impurity such as acetate separate effectively.
Beneficial effect of the present invention:
The technology of employing membrane sepn, activated carbon decolorizing and the crystallization technique separating and extracting succinic acid from anaerobic fermented liquid that the present invention relates to, first membrane sepn, activated carbon decolorizing and crystallization technique being introduced Unareobic fermentation produces in the extraction of Succinic Acid, and, set up a cover stage trapping system according to the distribution situation of impurity granularity in the fermented liquid.The membrane sepn that the present invention relates to, activated carbon decolorizing and crystallization technique have mild condition, easy and simple to handle, separating step is few, cost is low, and selectivity is good, the characteristics that quality product is high, the optimum combination stage trapping system of utilizing this technology to set up simultaneously, overcome the defective that complex steps, solvent consumption are many, blowdown flow rate is big, Product Safety is poor, yield is not high and productive labor intensity is big that prior art exists, the Succinic Acid production cost is obviously reduced, yield and quality product significantly improve.
Compare with existing Technology, the superiority of utilizing technology of the present invention to have is as follows:
1. the present invention adopts microfiltration membrane to remove solid substances such as thalline, centrifugal, the flocculation that has changed that conventional fermentation liquor treatment adopts and the method for press filtration, and operating process does not have the parts of running up, and has reduced energy consumption, maintenance cost and labour intensity.Through micro-filtrate membrane filtration, thalline separates fully with feed liquid, crosses the cleaner liquid clarification, methods such as that the filtrate quality significantly is better than is centrifugal, flocculation.
2. the present invention adopts ultra-filtration membrane and activated carbon treatment, and small molecular weight impurities such as macromole such as protein and pigment are removed in a large number, makes the fermented liquid purifying for clarification and near colourless Succinic Acid solution.
3. series connection closely between each operation of technology of the present invention, fermented liquid circulates under airtight condition all the time, avoided the secondary pollution of the impurity in the external environment to Succinic Acid, and technological process mild condition, do not add any organic solvent and other organic compound, have the Succinic Acid loss that is caused by chemical reaction hardly, so adopt the Succinic Acid yield of technology separation and Extraction of the present invention obviously to improve, Product Safety is good.
4. adopt the most outstanding superiority of technology of the present invention to be technical process short (only 4 step lock out operation unit), step is few, after finishing, fermentation liquor treatment impurity organic acids such as formic acid, acetate are removed fully and the while concentrated product by reduction vaporization is concentrated, direct crystallization can obtain product, analyzing Succinic Acid content through high performance liquid chromatography (HPLC) reaches more than 99.5%, do not contain impurity such as formic acid, acetate, other index meets the FCC-IV standard, quality good (and the Succinic Acid product content of other bibliographical information is 80~99%, partly still contains impurity such as acetate).
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The used Succinic Acid fermented liquid of following examples is all by following method fermentative preparation:
NJ113 (has been preserved in China Committee for Culture Collection of Microorganisms common micro-organisms center with succinic acid-producing actinobacillus (Actinobacillus succinogenes), deposit number is CGMCC No.1716) be inoculated in the fermention medium in the 5L fermentor tank, volume is 2~4L, inoculum size is 3~7% (v/v) (seed liquor and substratum ratios), temperature is 35~40 ℃, and fermentor tank feeds and contains N 2And CO 2Gas mixture (ratio is 4: 1), to keep the anaerobic environment of fermentation system, mixing speed is at 100~300rpm, fermenting process adopts carbonate, ammoniacal liquor, NaOH, urea, organic or inorganic acid control pH 6.0~7.4, fermentation time is 30~48h, obtain Succinic Acid fermented liquid through anaerobically fermenting production, standby.
Wherein:
(1) seed culture medium adds agar for the conventional liq substratum that carbon source, nitrogenous source and inorganic salt can be provided that contains carbohydrate of pH 6.0~8.0 during slant culture; Fermention medium is the conventional liq substratum that carbon source, nitrogenous source and inorganic salt can be provided that contains carbohydrate of pH 6.0~8.0, and adds VITAMIN; VITAMIN is folic acid, vitamin H, vitamins B 12, Thioctic Acid, nicotinic acid, pantothenic acid, VitB1 or vitamins B 6In one or more.
(2) inclined-plane and seed culture condition are:
Slant culture: with deposit number is the bacterial strain of CGMCC No.1716 carries out plate streaking in slant medium after, to cultivate in the anaerobism incubator, and incubator contains N 2, CO 2And H 2Mixed gas (N 2: CO 2: H 2=8: 1: 1), temperature is 30~40 ℃, cultivates 24~48h, is used for seed culture medium inoculation and bacterial strain and preserves;
Seed culture: seed culture medium is 20~80mL in the 100ml serum bottle, feeds to contain N 2And CO 2Gas mixture (N 2: CO 2=4: 1), 115~121 ℃ of sterilization 15~30min, the deposit number that slant culture is inserted in the cooling back is the bacterial strain of CGMCCNo.1716, culture temperature is 30~40 ℃, shaking speed 100~200r/min, incubation time are 10~16h, and the seed liquor of gained is used for the fermention medium inoculation.
Used Succinic Acid fermented liquid also can adopt other succinic acid-producing bacterial strains to prepare through anaerobically fermenting according to the method for introducing in the prior art among the present invention.
Embodiment 1
1.25 times that will be diluted with water to original volume through the Succinic Acid fermented liquid of anaerobically fermenting production are 10L, regulate fermented liquid pH to acid, microfiltration membrane cross flow filter through 0.2 μ m, remove thalline and granule foreign, working pressure is 0.05MPa, and temperature is 35 ℃, 20 times of cycles of concentration, dialysis water yield 3L, account for dilution secondary fermentation liquid long-pending 30%.The micro-filtration clear liquid is 8000 ultra-filtration membrane cross flow filter through the molecular weight that dams, and working pressure is 0.1MPa, and service temperature is 20 ℃, and cycles of concentration is 40 times, and the dialysis water yield is 1L, accounts for 8.3% of micro-filtrate volume.(this ratio is the mass volume ratio of activated carbon and ultrafiltrated to add 0.4% in the ultrafiltration clear liquid, be that activated carbon is 0.4g in every 100ml ultrafiltrated, gac down together), under 200 rev/mins mixing speed, decoloured 30 minutes, bleaching temperature is 50 ℃, carry out press filtration, add pure water (account for destainer volume the 5.6%) washing leaching cake of 0.7L, the decolouring filtrate after the merging transfers to pH3.5, directly reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 65 ℃, 4 times of cycles of concentration, crystallisation by cooling, dry Succinic Acid finished product 276g, the results are shown in Table 1.
Table 1:
Transmittance (430nm) Volume (L) Succinic Acid concentration (g/L) Yield (%)
Fermented liquid after the dilution 0.3 10.0 39.1
The micro-filtration clear liquid 40.1 12.0 31.2 95.8
The ultrafiltration clear liquid 52.4 12.5 29.6 98.8
Decolouring filtrate 93.3 13.0 28.3 99.5
Primary crystallization 75.0
Embodiment 2
1.5 times that will be diluted with water to original volume through the Succinic Acid fermented liquid of anaerobically fermenting production are 10L, regulate fermented liquid pH to acid, microfiltration membrane cross flow filter through 0.1 μ m, remove thalline and granule foreign, working pressure is 0.05MPa, and temperature is 35 ℃, 20 times of cycles of concentration, dialysis water yield 2L, account for dilution secondary fermentation liquid long-pending 20%.The micro-filtration clear liquid is 10000 ultra-filtration membrane cross flow filter through the molecular weight that dams, and working pressure is 0.2MPa, and service temperature is 35 ℃, and cycles of concentration is 40 times, and the dialysis water yield is 1L, accounts for 9.1% of micro-filtrate volume.Add 0.35% gac in the ultrafiltration clear liquid, under 200 rev/mins mixing speed, decoloured 30 minutes, bleaching temperature is 50 ℃, carry out press filtration, add pure water (account for destainer volume the 8.7%) washing leaching cake of 1L, the decolouring filtrate after the merging transfers to pH2.5, directly reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 65 ℃, 4 times of cycles of concentration, crystallisation by cooling, dry Succinic Acid finished product 288g, the results are shown in Table 2.
Table 2
Transmittance (430nm) Volume (L) Succinic Acid concentration (g/L) Yield (%)
Fermented liquid after the dilution 0.8 10.0 37.5
The micro-filtration clear liquid 52.3 11.0 33.3 97.7
The ultrafiltration clear liquid 60.4 11.5 31.3 98.5
Decolouring filtrate 94.5 12.3 29.2 99.8
Primary crystallization 80.5
Embodiment 3
1.75 times that will be diluted with water to original volume through the Succinic Acid fermented liquid of anaerobically fermenting production are 17.5L, regulate fermented liquid pH to acid, microfiltration membrane cross flow filter through 0.3 μ m, remove thalline and granule foreign, working pressure is 0.1MPa, and temperature is 20 ℃, 20 times of cycles of concentration, dialysis water yield 5L, account for dilution secondary fermentation liquid long-pending 28.6%.The micro-filtration clear liquid is 8000 ultra-filtration membrane cross flow filter through the molecular weight that dams, and working pressure is 0.4MPa, and service temperature is 20 ℃, and cycles of concentration is 40 times, and the dialysis water yield is 2L, accounts for 9.5% of micro-filtrate volume.Add 0.3% gac in the ultrafiltration clear liquid, under 200 rev/mins mixing speed, decoloured 30 minutes, bleaching temperature is 40 ℃, carry out press filtration, add pure water (account for destainer volume the 8.9%) washing leaching cake of 2L, the decolouring filtrate after the merging transfers to pH3.0, directly reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 65 ℃, 5 times of cycles of concentration, crystallisation by cooling, dry Succinic Acid finished product 453g, the results are shown in Table 3.
Table 3:
Transmittance (430nm) Volume (L) Succinic Acid concentration (g/L) Yield (%)
Fermented liquid after the dilution 1.7 17.5 33.7
The micro-filtration clear liquid 57.2 21.0 27.0 96.1
The ultrafiltration clear liquid 62.6 22.5 25.6 99.2
Decolouring filtrate 95.0 24.2 23.8 100.0
Primary crystallization 78.6
Embodiment 4
1.5 times that will be diluted with water to original volume through the Succinic Acid fermented liquid of anaerobically fermenting production are 10L, regulate fermented liquid pH to acid, microfiltration membrane cross flow filter through 0.2 μ m, remove thalline and granule foreign, working pressure is 0.05MPa, and temperature is 20 ℃, 15 times of cycles of concentration, dialysis water yield 2L, account for dilution secondary fermentation liquid long-pending 20%.The micro-filtration clear liquid is 10000 ultra-filtration membrane cross flow filter through the molecular weight that dams, and working pressure is 0.3MPa, and service temperature is 20 ℃, and cycles of concentration is 40 times, and the dialysis water yield is 1L, accounts for 9.1% of micro-filtrate volume.Add 0.35% gac in the ultrafiltration clear liquid, under 200 rev/mins mixing speed, decoloured 30 minutes, bleaching temperature is 50 ℃, carry out press filtration, add pure water (account for destainer volume the 8.7%) washing leaching cake of 1L, the decolouring filtrate after the merging transfers to pH2.0, directly reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 65 ℃, 4 times of cycles of concentration, crystallisation by cooling, dry Succinic Acid finished product 268g, the results are shown in Table 4.
Table 4:
Transmittance (430nm) Volume (L) Succinic Acid concentration (g/L) Yield (%)
Fermented liquid after the dilution 0.7 10.0 38.0
The micro-filtration clear liquid 52.3 11.0 32.8 95.0
The ultrafiltration clear liquid 60.4 11.5 30.7 97.9
Decolouring filtrate 94.8 12.2 28.8 99.6
The primary crystallization yield 76.3

Claims (8)

1. the method for a separating and extracting succinic acid from anaerobic fermented liquid is characterized in that this method may further comprise the steps:
To adopt micro-filtrate membrane filtration through the Succinic Acid fermented liquid that anaerobically fermenting is produced, and use the ultra-filtration membrane ultrafiltration then, and use decolorization and impurity removal by active carbon again, and obtain clarifying Succinic Acid solution, and concentrate, crystallization obtains the Succinic Acid product.
2. the method for separating and extracting succinic acid according to claim 1, it is characterized in that adopting micro-filtrate membrane filtration is that the Succinic Acid fermented liquid through anaerobically fermenting production is diluted with water to 1.25~2 times of original volume, and regulate fermented liquid pH to acid, by the aperture is that the microfiltration membrane of 0.1~0.5 μ m is carried out cross flow filter, working pressure is 0.05~0.1MPa, service temperature is 15~40 ℃, 10~20 times of cycles of concentration, the dialysis water yield account for dilution secondary fermentation liquid long-pending 20~70%.
3. the method for separating and extracting succinic acid according to claim 2, it is characterized in that the multiple that the Succinic Acid fermented liquid is diluted with water to original volume is 1.25~1.75 times, the aperture of microfiltration membrane is 0.1~0.2 μ m, the micro-filtration working pressure is 0.05~0.08MPa, service temperature is 20~35 ℃, cycles of concentration is 15~20 times, the dialysis water yield account for dilution secondary fermentation liquid long-pending 20~50%.
4. the method for separating and extracting succinic acid according to claim 1, it is characterized in that with the ultra-filtration membrane ultrafiltration it being that to adopt molecular weight cut-off be that 6000~10000 daltonian ultra-filtration membranes carry out cross flow filter for Succinic Acid fermented liquid after micro-filtrate membrane filtration is handled, ultrafiltration pressure 0.1~0.5MPa, temperature is 15~40 ℃, 30~40 times of cycles of concentration, the dialysis water yield accounts for 5~20% of micro-filtrate volume.
5. the method for separating and extracting succinic acid according to claim 4, it is characterized in that with the ultra-filtration membrane molecular weight that dams be 8000~10000, ultrafiltration pressure is 0.1~0.4MPa, and service temperature is 20~40 ℃, cycles of concentration is 35~40 times, and the dialysis water yield accounts for 5~10% of micro-filtrate volume.
6. the method for separating and extracting succinic acid according to claim 1, it is characterized in that with decolorization and impurity removal by active carbon it being to adopt Powdered Activated Carbon to remove pigment and removal of impurities the Succinic Acid fermented liquid after the ultrafiltration, operational condition is under 200 rev/mins mixing speed, the Powdered Activated Carbon addition is counted 0.3~0.5% of ultrafiltrated volume with the quality volume percent, bleaching temperature is 40~60 ℃, decoloured 30~45 minutes, carry out press filtration, filter cake is with 30~50 ℃ pure water circulation cleaning 3 times, pure water washing consumption account for activated carbon decolorizing liquid long-pending 5~15%, to decolour filtrate and wash water merges, and obtains clarifying Succinic Acid solution.
7. the method for separating and extracting succinic acid according to claim 6, it is characterized in that the Powdered Activated Carbon addition counts 0.3~0.4% of ultrafiltrated volume with the quality volume percent, service temperature is 40~50 ℃, bleaching time is 30 minutes, filter cake pure water washing consumption account for activated carbon decolorizing liquid long-pending 5~10%.
8. the method for separating and extracting succinic acid according to claim 1, the method that it is characterized in that the condensing crystal of fermented liquid is that the Succinic Acid feed liquid behind the decolouring purifying is transferred to pH2.0~3.5, reduction vaporization concentrates, working pressure is-0.08~-0.1MPa, service temperature is 55~70 ℃, 4~6 times of cycles of concentration, crystallisation by cooling obtains the Succinic Acid crystal again.
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CN101215583B (en) * 2008-01-18 2010-11-10 南京工业大学 Method for preparing succinic acid by coupling fermentation and film separation unit
CN101348428B (en) * 2008-09-05 2011-01-05 江南大学 Method for extracting amber acid in fermentation liquor by anion resin adsorption
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CN108047022A (en) * 2017-12-12 2018-05-18 河北科莱维生物科技有限公司 A kind of method for preparing succinic acid
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CN101215583B (en) * 2008-01-18 2010-11-10 南京工业大学 Method for preparing succinic acid by coupling fermentation and film separation unit
CN101348428B (en) * 2008-09-05 2011-01-05 江南大学 Method for extracting amber acid in fermentation liquor by anion resin adsorption
CN101348429B (en) * 2008-09-05 2011-03-16 江南大学 Method for extracting amber acid in fermentation liquor by cationic resin exchange
CN101475464B (en) * 2009-02-09 2011-08-31 南京工业大学 Method for separating and extracting amber acid from amber acid fermentation liquor by nanofiltration
CN102573526A (en) * 2009-09-30 2012-07-11 生物琥珀酸有限公司 Processes for removing color during production of runway deicer
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
US20150057425A1 (en) * 2009-11-24 2015-02-26 Dsm Ip Assets B.V. Process for the crystallization of succinic acid
US20120238722A1 (en) * 2009-11-24 2012-09-20 Roquette Freres Sa Process for the crystallization of succinic acid
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CN101792778A (en) * 2010-03-25 2010-08-04 南京工业大学 Method for fermentation production of succinic acid by circulating utilization of recombinant Bacillus coli cells
CN101792778B (en) * 2010-03-25 2013-06-19 南京工业大学 Method for fermentation production of succinic acid by circulating utilization of recombinant Bacillus coli cells
CN102731288B (en) * 2011-03-31 2014-04-02 中国石油化工股份有限公司 Method for separating high-purity succinic acid from fermentation broth
CN102731288A (en) * 2011-03-31 2012-10-17 中国石油化工股份有限公司 Method for separating high-purity succinic acid from fermentation broth
CN102952008A (en) * 2011-08-26 2013-03-06 中国石油化工股份有限公司 Method for extracting succinic acid from anaerobic fermentation broth
CN102321682A (en) * 2011-09-13 2012-01-18 南京工业大学 Method for recycling water from separation process of succinic acid by fermentation
CN102503804A (en) * 2011-11-04 2012-06-20 南京工业大学 Method for continuously discoloring succinic acid fermentation liquor by using activated carbon
CN102503804B (en) * 2011-11-04 2013-09-18 南京工业大学 Method for continuously discoloring succinic acid fermentation liquor by using activated carbon
CN102363594A (en) * 2011-11-09 2012-02-29 中国科学院过程工程研究所 Method for separating and purifying succinic acid from fermentation broth
CN102690189A (en) * 2012-06-12 2012-09-26 南京工业大学 Method for extracting and separating succinic acid from succinic acid fermentation solution or succinic acid crystallization mother solution
CN102942472A (en) * 2012-11-22 2013-02-27 天津工业生物技术研究所 Method of extracting succinic acid from microorganism fermentation liquor
CN102942472B (en) * 2012-11-22 2015-03-11 中国科学院天津工业生物技术研究所 Method of extracting succinic acid from microorganism fermentation liquor
CN103420827A (en) * 2013-08-21 2013-12-04 江南大学 Method for extracting succinic acid from fermentation broth through two aqueous phase extraction
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
CN107835798A (en) * 2015-07-14 2018-03-23 普拉克生化公司 The method for manufacturing butanedioic acid
CN107835798B (en) * 2015-07-14 2021-11-23 普拉克生化公司 Process for producing succinic acid
CN109206313A (en) * 2017-07-05 2019-01-15 中国石化扬子石油化工有限公司 The method that succinate anaerobic fermented liquid prepares succinic acid
CN109206313B (en) * 2017-07-05 2021-06-11 中国石化扬子石油化工有限公司 Method for preparing succinic acid by succinate anaerobic fermentation liquid
CN108047022A (en) * 2017-12-12 2018-05-18 河北科莱维生物科技有限公司 A kind of method for preparing succinic acid
CN111138272A (en) * 2019-12-19 2020-05-12 上海凯赛生物技术股份有限公司 Extraction method and system of long-chain dibasic acid
US11999689B2 (en) 2019-12-19 2024-06-04 Cathay Biotech Inc. Method and system for extracting long chain dicarboxylic acid
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Inventor after: Yao Zhong

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