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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- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 239000001384 succinic acid Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000855 fermentation Methods 0.000 title claims abstract description 22
- 230000004151 fermentation Effects 0.000 title claims abstract description 21
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 39
- 239000000047 product Substances 0.000 claims description 12
- NHJPVZLSLOHJDM-UHFFFAOYSA-N azane;butanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCC([O-])=O NHJPVZLSLOHJDM-UHFFFAOYSA-N 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005189 flocculation Methods 0.000 claims description 8
- 230000016615 flocculation Effects 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000003729 cation exchange resin Substances 0.000 claims description 6
- 159000000003 magnesium salts Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000011347 resin Substances 0.000 abstract description 8
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001099 ammonium carbonate Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract description 2
- 235000012501 ammonium carbonate Nutrition 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- LZNBFGXYVFUAQM-UHFFFAOYSA-N butanedioic acid;magnesium Chemical compound [Mg].OC(=O)CCC(O)=O LZNBFGXYVFUAQM-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 6
- 235000011130 ammonium sulphate Nutrition 0.000 description 6
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000001095 magnesium carbonate Substances 0.000 description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 5
- 235000014380 magnesium carbonate Nutrition 0.000 description 5
- 229960001708 magnesium carbonate Drugs 0.000 description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000001166 ammonium sulphate Substances 0.000 description 4
- 150000001720 carbohydrates Chemical class 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 4
- 239000000347 magnesium hydroxide Substances 0.000 description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 4
- 230000002906 microbiologic effect Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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 in 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 |
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| 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 | Method for separating and extracting succinic acid from anaerobic fermentation broth |
| CN101348429A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | A kind of cationic resin exchange extracts the method for succinic acid in fermented liquid |
| 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 |
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| 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 | Method for separating and extracting succinic acid from anaerobic fermentation broth |
| CN101348429A (en) * | 2008-09-05 | 2009-01-21 | 江南大学 | A kind of cationic resin exchange extracts the method for succinic acid in fermented liquid |
| 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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