CN106673996A - Method for purifying long-chain dicarboxylic acid - Google Patents
Method for purifying long-chain dicarboxylic acid Download PDFInfo
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- CN106673996A CN106673996A CN201510751395.3A CN201510751395A CN106673996A CN 106673996 A CN106673996 A CN 106673996A CN 201510751395 A CN201510751395 A CN 201510751395A CN 106673996 A CN106673996 A CN 106673996A
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- 238000000034 method Methods 0.000 title claims abstract description 53
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000047 product Substances 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 3
- 238000000855 fermentation Methods 0.000 claims description 27
- 230000004151 fermentation Effects 0.000 claims description 27
- 150000001991 dicarboxylic acids Chemical class 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 11
- 230000009514 concussion Effects 0.000 claims description 9
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 7
- 238000005374 membrane filtration Methods 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000002207 metabolite Substances 0.000 claims description 4
- 244000005700 microbiome Species 0.000 claims description 4
- 241000894006 Bacteria Species 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 claims description 2
- 238000001728 nano-filtration Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 6
- 102000004169 proteins and genes Human genes 0.000 abstract description 6
- 108090000623 proteins and genes Proteins 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 3
- 241000233866 Fungi Species 0.000 abstract 1
- 239000010413 mother solution Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 11
- -1 dicarboxylic acids sodium salt Chemical class 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000012065 filter cake Substances 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 6
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 241000222178 Candida tropicalis Species 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 235000021463 dry cake Nutrition 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004925 denaturation Methods 0.000 description 3
- 230000036425 denaturation Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 235000012970 cakes Nutrition 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- IIYFAKIEWZDVMP-UHFFFAOYSA-N linear paraffin C13 Natural products CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 229940094933 n-dodecane Drugs 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 102000039446 nucleic acids Human genes 0.000 description 2
- 108020004707 nucleic acids Proteins 0.000 description 2
- 150000007523 nucleic acids Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for purifying long-chain dicarboxylic acid. The method comprises the following steps: I, heating and demulsifying terminated fermented liquid, and separating unreacted alkane; II, removing solid impurities such as fungi residues to obtain fermented clear liquid; III, adding at least one of acetone and acetonitrile and activated carbon, oscillating, mixing and then filtering; IV, adding filtrate obtained in the step III and inorganic acid into heating and evaporating equipment for acidifying, separating an organic solvent from a fermented mother solution by using heating in an acidifying process, condensing distilled organic solvent and recovering; crystallizing dicarboxylic acid, separating out, cooling, filtering and drying to obtain a refined dicarboxylic acid product. The method disclosed by the invention adopts a method of precipitating the organic solvent, so that the contents of impurities such as protein in a dicarboxylic acid product are effectively reduced, and further a high-purity dicarboxylic acid product is obtained.
Description
Technical field
The present invention relates to a kind of method of purification long chain dicarboxylic acid, the method that high purity long chain dicarboxylic acids is particularly obtained from microbial fermentation solution.
Background technology
Long chain dicarboxylic acid general molecular formula is CnH2n-2O4, wherein n is 10-18, is microorganism metabolite obtained from the fermentation such as liquid wax.Its zymotic fluid is complicated heterogeneous system, secretion wherein containing unreacted carbon source, microbial cell and fragment, the culture medium not utilized and metabolite and microorganism etc., especially wherein grade impurity containing a large amount of protein, pigment and ash, purity and the application of product are had a strong impact on, and the extraction to the species dicarboxylic acids brings difficulty with refined.
The method for extracting long chain dicarboxylic acid at present is generally divided into solvent method and Aqueous phase.Although solvent method can solve the above problems, because solvent method is present, investment is big, and equipment corrosion is serious, and the problems such as solvent and alkane and production security and environmental pollution is remained in product, and the use of the method is greatly limited.Although traditional water phase method of purification overcomes the defect of solvent method, but its product purity and yield can not be reached compared with high target.
In long chain dicarboxylic acid process for purification disclosed in CN01142806.6, with long chain dicarboxylic acid dry powder as raw material, using acetone, methyl alcohol and ethanol as solvent refining long-chain dicarboxylic acids.Dicarboxylic acids elder generation in method zymotic fluid first is Jing after charcoal absorption, then acidizing crystal, filters, washes and be dried dicarboxylic acid crystallizates filter cake and obtain long chain dicarboxylic acid dry powder, is then refined using organic solvent.The refined raw material of the method is that aqueous filter cake obtains after drying dicarboxylic acids dry powder, and the restriction to feed moisture content reduces the operating flexibility of the method, increased the equipment that thick acid is dried, and causes this technological process longer, increased production cost.And the method is in the aqueous solution for obtaining the alkaline dicarboxylic acids sodium salt before dicarboxylic acid crystallizates filter cake and in solvent refining processes, the process of charcoal absorption twice has been carried out altogether, those skilled in the relevant art know about, increase an activated carbon processing procedure, equipment investment and production cost can be increased, and activated carbon dosage is directly proportional to the loss of product, and activated carbon dosage is bigger, the yield of product is lower.And in the refined dicarboxylic acids of organic solvent, can typically reach the requirement of decolouring using adsorbent, but still more difficult removing small molecular protein therein, make total nitrogen content undesirable.
CN1255483A discloses a kind of method that Aqueous phase separates dicarboxylic acids：Zymotic fluid heating will be terminated and remove unreacted alkane, then add diatom filtration sterilization；Filtrate Jing adjusts pH value to obtain sour cake and filtrate；Filtrate adds activated carbon decolorizing again, then filters；The sour cake obtained dissolved with the filtrate after decolouring again before, acidifying；Crystallization is finally obtained, drying obtains dicarboxylic acid product.The method complex operation step, running cost is high, and dicarboxylic acid product yield is too low, and purity is not also high, and the alkane rate of recovery is low.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of method of purification long chain dicarboxylic acid.The inventive method effectively reduces the content of the impurity such as albumen in dicarboxylic acid product, so as to obtain highly purified dicarboxylic acid product using the method for organic solvent deposit.
A kind of method of purification long chain dicarboxylic acid of the present invention, including herein below：
I, zymotic fluid heating demulsification type will be terminated, separate unreacted alkane；
The solid impurities such as II, removing bacteria residue, obtain fermentation clear liquid；
III, at least one and activated carbon in fermentation clear liquid in addition acetone, acetonitrile, are filtered after concussion mixing；
IV, inorganic acid is added to be acidified in heating evaporation equipment the filtrate obtained by III, can realize that organic solvent is separated with fermentation mother liquor using heating in acidization, reclaim after the organic solvent condensate for distilling out, dicarboxylic acid crystallizates are separated out, and cooled down, are filtered, being dried to obtain refined dicarboxylic acid product.
In the inventive method, it is microorganism metabolite obtained from liquid wax fermentation that zymotic fluid is terminated described in step I, wherein the dicarboxylic acid molecule formula for containing is CnH2n-2O4, wherein n is 10-18, and dicarboxylic acids can be a kind of single dicarboxylic acids, or mixed dicarboxylic acid.
In the inventive method, step II can adopt the conventional methods such as centrifugation or membrane filtration and equipment to carry out removing the operation of the impurity such as thalline.
In the inventive method, preferably it is initially charged activated carbon in fermentation clear liquid and is adsorbed, absorption adds at least one in acetone, acetonitrile after terminating, filtered after concussion mixing.The preferred Powdered Activated Carbon of described activated carbon, addition is the 1% ~ 10% of zymotic fluid theory acid content, and adsorption time is 30 ~ 60min.Addition in acetone and/or acetonitrile is the 5% ~ 40% of fermentation clear liquid volume.Concussion 20 ~ 60min of incorporation time.
In the inventive method, step III can also add appropriate picric acid, preferably add simultaneously with least one in acetone, acetonitrile, and addition is 2 ~ 5 wt% of the theoretical acid content of zymotic fluid.Picric acid, acetone and/or acetonitrile, activated carbon collective effect, improve the contamination precipitation effects such as albumen.
In the inventive method, the preferred ultrafiltration of filtration or nanofiltration equipment described in step III is separated.
In the inventive method, the pH value being acidified described in step IV is 2.0 ~ 4.0, and heating-up temperature is 80 ~ 95 DEG C, atmospheric operation condition.The organic solvent that condensation is reclaimed can be reused.Acid used by the above-mentioned acidifying of the present invention can be the H of any concentration2SO4、HNO3, HCl or H3PO4。
Till crystallisation by cooling temperature generally makes dicarboxylic acids sufficient crystallising in step IV, temperature is generally 10 DEG C～30 DEG C.
The inventive method can obtain the dicarboxylic acid product of highly purified single kind, it is also possible to obtain mixed dicarboxylic acid product.
Compared with prior art, the present invention has advantages below：
The inventors discovered that, although terminating zymotic fluid during heat inactivation and breakdown of emulsion by the denaturation of the impurity such as Partial Protein to precipitate, and remove with preliminary filtration, but follow-up acidifying is separated out during dicarboxylic acids, due to the acute variation of pH value, remaining a large amount of water-solubility proteins still can the denaturation during acidifying, separate out in the lump with dicarboxylic acids, be embedded in crystal thus have a strong impact on product quality.
The present invention is using impurity such as unmodified albumen, nucleic acid in organic solvent and picric acid co-precipitation zymotic fluid, then precipitation is filtered to remove so that the impurity such as most albumen in zymotic fluid is removed；Water miscible picric acid can form compound and precipitate with the alkaline functional group of the biomolecule such as albumen, polysaccharide, nucleic acid, then be removed by filtration, will not introduce other impurity.Water-solubility protein denaturation remaining in zymotic fluid when avoiding follow-up acidifying is separated out, and affects product quality, so as to obtain highly purified dicarboxylic acids essence product.The characteristics of there is the inventive method process is simple to be easily achieved, product yield is high, under less material consumption energy consumption input, can obtain the polymer grade product that purity is high, total nitrogen content is low, is more suitable for industrialized production.
Specific embodiment
Further the inventive method is explained below by embodiment.
Embodiment 1
With n-dodecane hydrocarbon as substrate, using the carbon dicarboxylic acids of candida tropicalis fermenting and producing 12.Dicarboxyl acid concentration is 150g/L during fermentation ends, and pH is 7.2.Zymotic fluid 1000ml is taken, 80 DEG C are heated to, is stood to room temperature, divide the liquid wax for going solution to remain, be filtered to remove thalline, 1.5g Powdered Activated Carbons are added in fermentation clear liquid, stir decolouring 30min.Continue to add 80ml acetone in fermentation clear liquid, concussion mixing 60min, is 10 with membrane aperture-2μm membrane filtration, remove the precipitation such as activated carbon and albumen, adjust filtrate pH to 3 with the sulfuric acid of 6M, 85 DEG C are heated in heating and evaporating unit, distill acetone solvent, the acetone condensation for distilling out is reclaimed.Crystallizing at room temperature is at the uniform velocity down to 15 DEG C/h, dicarboxylic acids filter cake is filtered to obtain, neutrality is washed to, dry cake obtains product.Product quality is shown in Table 1.
Embodiment 2
With n-dodecane hydrocarbon as substrate, using the carbon dicarboxylic acids of candida tropicalis fermenting and producing 12.Dicarboxyl acid concentration is 158 g/L during fermentation ends, and pH is 7.3.Zymotic fluid 1000ml is taken, 90 DEG C are heated to, is stood to room temperature, divide the liquid wax for going solution to remain, be filtered to remove thalline, 2.5g Powdered Activated Carbons are added in fermentation clear liquid, stir decolouring 40min.Continue to add 200ml acetonitriles in fermentation clear liquid, concussion mixing 60min, is 10 with membrane aperture-2μm membrane filtration, remove the precipitation such as activated carbon and albumen, adjust filtrate pH to 4 with the sulfuric acid of 10M, 90 DEG C are heated in heating and evaporating unit, distill acetonitrile solvent, the acetonitrile condensation for distilling out is reclaimed.
Crystallizing at room temperature is at the uniform velocity down to 20 DEG C/h, dicarboxylic acids filter cake is filtered to obtain, neutrality is washed to, dry cake obtains product.Product quality is shown in Table 1.
Embodiment 3
With n-tridecane hydrocarbon as substrate, using the carbon dicarboxylic acids of candida tropicalis fermenting and producing 13.Dicarboxyl acid concentration is 154.3 g/L during fermentation ends, and pH is 7.5.Zymotic fluid 1000ml is taken, 85 DEG C are heated to, is stood to room temperature, divide the liquid wax for going solution to remain, be filtered to remove thalline, 5g Powdered Activated Carbons are added in fermentation clear liquid, stir decolouring 60min.Continue to add 300ml acetone and 3.2g picric acid in fermentation clear liquid, concussion mixing 60min, is 10 with membrane aperture-3μm membrane filtration, remove the precipitation such as activated carbon and albumen, adjust filtrate pH to 2 with the sulfuric acid of 8M, 95 DEG C are heated in heating and evaporating unit, distill acetone solvent, the acetone condensation for distilling out is reclaimed.Crystallizing at room temperature is at the uniform velocity down to 18 DEG C/h, dicarboxylic acids filter cake is filtered to obtain, neutrality is washed to, dry cake obtains product.Product quality is shown in Table 1.
Embodiment 4
With n-tridecane hydrocarbon as substrate, using the carbon dicarboxylic acids of candida tropicalis fermenting and producing 13.Dicarboxyl acid concentration is 163.0 g/L during fermentation ends, and pH is 7.1.Zymotic fluid 1000ml is taken, 90 DEG C are heated to, is stood to room temperature, divide the liquid wax for going solution to remain, be filtered to remove thalline, 15g Powdered Activated Carbons are added in fermentation clear liquid, stir decolouring 60min.Continue to add 350ml acetonitriles and 8g picric acid in fermentation clear liquid, concussion mixing 40min, is 10 with membrane aperture-3μm membrane filtration, remove the precipitation such as activated carbon and albumen, adjust filtrate pH to 3 with the sulfuric acid of 7M, 90 DEG C are heated in heating and evaporating unit, distill acetonitrile solvent, the acetonitrile condensation for distilling out is reclaimed.Crystallizing at room temperature is at the uniform velocity down to 15 DEG C/h, dicarboxylic acids filter cake is filtered to obtain, neutrality is washed to, dry cake obtains product.Product quality is shown in Table 1.
Comparative example 1
1.5g Powdered Activated Carbons are only added in fermentation clear liquid, and is added without acetone, remaining is with embodiment 1.Product quality is shown in Table 1.
The long chain dicarboxylic acid product quality of table 1
Claims (12)
1. it is a kind of purification long chain dicarboxylic acid method, it is characterised in that：Including herein below：
I, zymotic fluid heating demulsification type will be terminated, separate unreacted alkane；
II, removing bacteria residue solid impurity, obtain fermentation clear liquid；
III, at least one and activated carbon in fermentation clear liquid in addition acetone, acetonitrile, are filtered after concussion mixing；
IV, inorganic acid is added to be acidified in heating evaporation equipment the filtrate obtained by III, realize that organic solvent is separated with fermentation mother liquor using heating in acidization, reclaim after the organic solvent condensate for distilling out, dicarboxylic acid crystallizates are separated out, and Jing is cooled down, filtered, being dried to obtain refined dicarboxylic acid product.
2. method according to claim 1, it is characterised in that：It is microorganism metabolite obtained from liquid wax fermentation to terminate zymotic fluid described in step I, and the dicarboxylic acid molecule formula for containing is CnH2n-2O4, wherein n is 10-18, and dicarboxylic acids is single dicarboxylic acids or for mixed dicarboxylic acid.
3. method according to claim 1, it is characterised in that：Step II removes bacteria residue solid impurity using centrifugation or membrane filtration.
4. method according to claim 1, it is characterised in that：Activated carbon is added to be adsorbed in fermentation clear liquid in step III, absorption adds at least one in acetone, acetonitrile after terminating, filtered after concussion mixing.
5. method according to claim 4, it is characterised in that：Described activated carbon is Powdered Activated Carbon, and addition is the 1% ~ 10% of zymotic fluid theory acid content, and adsorption time is 30 ~ 60min.
6. method according to claim 4, it is characterised in that：The addition of acetone and/or acetonitrile is the 5% ~ 40% of fermentation clear liquid volume, shakes 20 ~ 60min of incorporation time.
7. method according to claim 1, it is characterised in that：Appropriate picric acid is added in step III, addition is 2 ~ 5 wt% of the theoretical acid content of zymotic fluid.
8. method according to claim 1, it is characterised in that：Picric acid is with least one addition simultaneously in acetone and/or acetonitrile.
9. method according to claim 1, it is characterised in that：Ultrafiltration or nanofiltration are filtered into described in step III.
10. method according to claim 1, it is characterised in that：The pH value being acidified described in step IV is 2.0 ~ 4.0, and heating-up temperature is 80 ~ 95 DEG C.
11. methods according to claim 1, it is characterised in that：It is H that acid used is acidified in step IV2SO4、HNO3、HCl、H3PO4In at least one.
12. methods according to claim 1, it is characterised in that：Crystallisation by cooling temperature is 10 DEG C～30 DEG C in step IV.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507129A (en) * | 2020-10-28 | 2022-05-17 | 中国石油化工股份有限公司 | Refining method of organic acid in fermentation liquor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147016A (en) * | 1995-10-05 | 1997-04-09 | 中国石油化工总公司 | Method for treatment of alpha, omega dibasic acid fermentation liquor |
| CN1326463A (en) * | 1998-11-20 | 2001-12-12 | 雀巢制品公司 | Method for continuously isolating active proteins |
| CN1388242A (en) * | 2001-05-25 | 2003-01-01 | 广东省微生物研究所 | Method of separating and collecting bacterial cell from fermented liquid |
| CN1460671A (en) * | 2003-06-02 | 2003-12-10 | 大连理工大学 | Method for extracting and separating 1,3-propylene glycol from microbial fermented liquor |
-
2015
- 2015-11-09 CN CN201510751395.3A patent/CN106673996A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147016A (en) * | 1995-10-05 | 1997-04-09 | 中国石油化工总公司 | Method for treatment of alpha, omega dibasic acid fermentation liquor |
| CN1326463A (en) * | 1998-11-20 | 2001-12-12 | 雀巢制品公司 | Method for continuously isolating active proteins |
| CN1388242A (en) * | 2001-05-25 | 2003-01-01 | 广东省微生物研究所 | Method of separating and collecting bacterial cell from fermented liquid |
| CN1460671A (en) * | 2003-06-02 | 2003-12-10 | 大连理工大学 | Method for extracting and separating 1,3-propylene glycol from microbial fermented liquor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507129A (en) * | 2020-10-28 | 2022-05-17 | 中国石油化工股份有限公司 | Refining method of organic acid in fermentation liquor |
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Application publication date: 20170517 |