CN100406425C - Method for refining long-chain biatomic acid - Google Patents
Method for refining long-chain biatomic acid Download PDFInfo
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- CN100406425C CN100406425C CNB2003101049799A CN200310104979A CN100406425C CN 100406425 C CN100406425 C CN 100406425C CN B2003101049799 A CNB2003101049799 A CN B2003101049799A CN 200310104979 A CN200310104979 A CN 200310104979A CN 100406425 C CN100406425 C CN 100406425C
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- diprotic acid
- acid
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- long chain
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- 239000002253 acid Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000007670 refining Methods 0.000 title claims abstract description 12
- 238000005185 salting out Methods 0.000 claims abstract description 18
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000855 fermentation Methods 0.000 claims abstract description 8
- 230000004151 fermentation Effects 0.000 claims abstract description 8
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 43
- 239000000243 solution Substances 0.000 claims description 35
- 239000000047 product Substances 0.000 claims description 34
- 238000001914 filtration Methods 0.000 claims description 32
- 239000012065 filter cake Substances 0.000 claims description 23
- 150000007520 diprotic acids Chemical class 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 230000020477 pH reduction Effects 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 11
- 102000004169 proteins and genes Human genes 0.000 abstract description 11
- 108090000623 proteins and genes Proteins 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000012545 processing Methods 0.000 abstract description 6
- 239000012452 mother liquor Substances 0.000 abstract description 5
- 239000012188 paraffin wax Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 159000000000 sodium salts Chemical class 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 241000222178 Candida tropicalis Species 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- -1 diprotic acid basic metal Chemical class 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000002207 metabolite Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- BGHCVCJVXZWKCC-UHFFFAOYSA-N Tetradecane Natural products CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- YCOZIPAWZNQLMR-UHFFFAOYSA-N heptane - octane Natural products CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003248 secreting effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for extracting and refining long chain binary acid by a water phase method, and the long chain binary acid is extracted from C10 to C18 normal paraffin or mixed normal alkane fermentation liquor. The present invention overcomes the disadvantages of low purity and high chrominance of products prepared by the existing water phase method. The method effectively reduces impurity content in the products, such as protein, pigment, etc. and prepares the long chain binary acid products via being combined with the procedures of thalline separation, acid separation, crystallization, drying, etc., the total acid content of the long chain binary acid products is larger than 99 wt%, and the color of the long chain binary acid products is white. The present invention uses a combined technique of mono-salt crystallization and salting-out of the long chain binary acid, omits the binary acid recovery processing procedures of salting-out mother liquor or mono-salt filter liquor, saves processing cost and increases product yield.
Description
Technical field
The present invention relates to from fermented liquid, extract the also method of refining long-chain biatomic acid, particularly from one or more C
10～C
18Extract the also method of refining long-chain biatomic acid in the normal alkane fermentation liquor.
Background technology
Long-chain biatomic acid is to utilize the microbial fermentation normal paraffin and the meta-bolites that obtains.Its fermented liquid is the heterogeneous system of a complexity, wherein contain unreacted normal paraffin, microorganism cells and fragment, the substratum that does not utilize and the secretory product of meta-bolites and microorganism etc., especially wherein contain impurity such as a large amount of protein, pigment, influence the purity and the visual appearance of product.
The method of refining long-chain biatomic acid generally is divided into solvent method and water method two big classes at present.Though wherein solvent method can address the above problem, investment is big because solvent method exists, product residue alkane and problems such as solvent and production security, makes the use of this method be subjected to very big restriction.The water method has overcome the defective of solvent method, but the purity of its product and appearance luster can not reach higher index.A kind of method of refining long-chain biatomic acid has been proposed at CN1219530A as Fushun Petrochemical Research Institute, by the processing of saltouing of two salt, the purity of purified dicarboxylic acid product and color and luster are all fine, but the yield of product is lower, and, salting-out mother liquor also needs to recycle diprotic acid, has increased processing cost.CN1255483A has also proposed the method for three kinds of refining long-chain biatomic acids, only uses long-chain biatomic acid list sodium salt crystal technology, does not recycle under the situation of the diprotic acid in single salt filtrate, and the yield of product is below 90wt%, and the yield of product is lower; And under the situation of the diprotic acid in the single salt filtrate of recycling, the yield of product can reach 92wt%, but has increased this step of diprotic acid that recycles in single salt filtrate like this, thereby has increased processing cost.
Summary of the invention
The purpose of this invention is to provide and a kind ofly utilize single salt to saltout from one or more C
10～C
18Extract the also method of refining long-chain biatomic acid in the fermented liquid of normal paraffin, this method has been simplified operation steps, has improved the purity and the yield of product, has reduced the colourity of product.
The method of refining long-chain biatomic acid of the present invention may further comprise the steps:
I, will stop fermented liquid behind heating demulsification type, Separation and Recovery alkane, acidifying again, crystallization are filtered and are obtained the long-chain biatomic acid filter cake;
II, the alkalization of the diprotic acid wet cake of step I gained is mixed with diprotic acid list salts solution, adds salting-out agent simultaneously, and heating makes its whole dissolvings, be cooled to room temperature then and filter and obtain long-chain biatomic acid list salt crystal filter cake;
III, the long-chain biatomic acid list salt crystal filter cake of Step II gained is added alkali dissolution generate the two salts solutions of long-chain biatomic acid fully, and the filtering solid substance;
IV, make the filtrate acidifying of Step II I gained the two salt of long-chain biatomic acid all be converted into long-chain biatomic acid, obtain the long-chain biatomic acid product through crystallization, filtration, washing and drying step then.
Be acidified with acid and heat in this programme I step protein denaturation is separated out, make soluble proteins and partial pigment filtering by filtration then.Long-chain biatomic acid list salt in the II step is through salting-out crystallization, when filtering, because the ability of long-chain biatomic acid list salt adsorpting pigment is very weak, in long-chain biatomic acid list salt crystalline process, soluble protein and pigment are stayed in the mother liquor when the crystallization of long-chain biatomic acid list salt is filtered, more help the Partial Protein sex change to separate out, this process has the dual function that removes soluble protein and remove pigment, thereby improved the purity of long-chain biatomic acid product and reduced the colourity of product, improved the quality of product.
Wherein, the thalline in the fermented liquid can be removed in step I, or removes in Step II I.The I step also can not removed thalline, takes the direct acidifying filtration of fermented liquid, salting-out crystallization, but owing to the carrier alkalization, when single salt is saltoutd, pigment is deepened, and effect is also undesirable, so remove thalline in step I.
In Step II, the diprotic acid list concentration of salt solution of preparation should be preferably in 80～200g/l greater than 80g/l, and the effect of saltouing this moment is best, and the salting-out agent of adding and diprotic acid weight ratio are 1～3.Salting-out agent can adopt NaCl, Na
2SO
4Etc. neutral inorganic.Because the solubility with temperature of NaCl changes little, and NaCl content is low and cost is low in the room temperature salting-out crystallization thing, and effect is also better, so generally adopt NaCl.
Method of the present invention can prepare the diprotic acid basic metal list salts solution of any concentration by the thick diprotic acid filter cake of alkalization, adds salting-out agent simultaneously, through heating, cooling and crystallisation step long-chain biatomic acid list salt is all separated out.A little less than the discovery after deliberation, the ability of long-chain biatomic acid list salt adsorpting pigment, in long-chain biatomic acid list salt crystalline process, soluble protein and pigment are trapped in the mother liquor, and this process has the dual function that removes protein and pigment; At room temperature solubleness is very low because of single salt, thereby the salting-out agent that add can make single salt separate out fully, more helps the Partial Protein sex change to separate out simultaneously.The present invention adopts the salt crystallization of long-chain biatomic acid list and the technology of combining of saltouing, saved salting-out mother liquor or single salt filtrate recycling step of binary acid, saved processing cost, and further improved the purity of long-chain biatomic acid product and reduced the colourity of product, also improved the yield of product simultaneously.
Utilize the long-chain biatomic acid of present method preparation, total acid purity is greater than 99wt%, and nitrogen content is less than 40 μ g/g, and yield is greater than 94wt%, and colourity is less than 30, and product appearance is white in color.
Embodiment
The method of refining long-chain biatomic acid of the present invention specifically comprises the steps:
1, will stop fermented liquid heating demulsification type, Separation and Recovery alkane earlier after, to regulate the pH value be 2～4 in acidifying again, temperature is 75～90 ℃, cools the temperature to room temperature then, obtains the long-chain biatomic acid filter cake after filtration.
2, the long-chain biatomic acid filter cake that contains with step 1 gained mixes with water, adding alkali, to regulate the pH value be 6.0～7.0 to be prepared into certain density diprotic acid list salts solution, adding and diprotic acid weight ratio are 1～3 salting-out agent simultaneously, be heated to 85～95 ℃ of dissolvings fully then, be cooled to 75～85 ℃ of insulation 15～30min.Above-mentioned solution slowly is cooled to room temperature impels long-chain biatomic acid list salt salting-out crystallization, filter and obtain long-chain biatomic acid list salt filter cake.
3, the filter cake dissolving that step 2 is obtained also adds alkali to regulate pH value is 9～12, and slowly is heated to 50～70 ℃ and makes it to generate fully the two salts solutions of long-chain biatomic acid, and filter and obtain clarifying long-chain biatomic acid pair salt filtrates, and the filtering solid substance.
4, in the two salt filtrates of the long-chain biatomic acid that step 3 obtains, be acidified with acid, regulating the pH value is 2～4, heat 80～95 ℃, make the two salt of long-chain biatomic acid be converted into long-chain biatomic acid fully, under this temperature, be incubated 15～30min, then slowly cool to room temperature, after filtration, washing and drying step make the long-chain biatomic acid product.
The above-mentioned used acid of acidifying of the present invention can be H
2SO
4, HNO
3, HCl or H
3PO
4, used alkali can be alkali-metal oxyhydroxide such as NaOH, KOH etc.The handled long-chain biatomic acid of the present invention is C
10～C
18In the long-chain biatomic acid one or more.
The inventive method needs insulation 15～30min when long-chain biatomic acid list salt salting-out crystallization and final acidizing crystal, slowly cooling not only helps operation and filters to impel crystal growth again, and helps pigment and soluble protein is trapped in the filtrate.
Further specify method of the present invention below by specific embodiment.
Embodiment 1
Get 200mL and obtain tridecanyldicarboxylic acid by the fermentation of candida tropicalis bacterium, concentration is 130g/l, and the pH value is 7.6 fermented liquid, is heated to 80 ℃, and static 30min divides and removes alkane residual in the solution, removes thalline after filtration, and filtrate is used the H of 3mol/L
2SO
4The pH value is transferred to 4.0,, reduce to room temperature then, after filtration, washing obtains tridecanyldicarboxylic acid coarse filtration cake at 80 ℃ of insulation 30min.
Mix with thick acidleach cake with 130mL water, the NaOH solution with 10mol/L transfers to 6.2 with the pH value again, adds the NaCl of 26g simultaneously, be heated to 95 ℃, it is fully dissolved, be cooled to 80 ℃ again and keep 30min, slowly cool to room temperature then, filter and obtain tridecanyldicarboxylic acid list sodium salt filter cake.In the time of 50 ℃, it is 10 solution that the NaOH that filter cake adds 10mol/L is deployed into pH value, filters and obtains the two salts solutions of clarifying long-chain biatomic acid, the H of adding 3mol/L in solution
2SO
4, adjust pH to 4.0 is heated to 95 ℃, and insulation 30min is cooled to room temperature then, after filtration, washing and drying step obtain the tridecanyldicarboxylic acid product.Product property sees Table 1.
Embodiment 2
Getting 200mL concentration is 120g/l, and the pH value is 7.6 13 carbon and 14 carbon mixed dibasic acid fermented liquids, is heated to 80 ℃, and static 30min divides and removes 13 residual in solution carbon and n-tetradecane hydrocarbon, with the H of 3mol/L
2SO
4Adjust pH to 3.4 at 80 ℃ of following insulation 30min, is cooled to room temperature then, after filtration, washing obtains the mixed dibasic acid filter cake.
Mix with thick acidleach cake with 300mL water, the NaOH solution with 10mol/L transfers to 6.0 with the pH value again, adds the NaCl of 72g simultaneously, be heated to 90 ℃, it is fully dissolved, be cooled to 78 ℃ again and keep 30min, slowly cool to room temperature then, filter and obtain mixed dibasic acid list sodium salt filter cake.In the time of 60 ℃, it is 9 solution that the NaOH that filter cake adds 10mol/L is deployed into pH value, filters and obtains the two salts solutions of clarifying long-chain biatomic acid, the H of adding 3mol/L in solution
2SO
4, adjust pH to 3.0 is heated to 80 ℃ and be incubated 20min, is cooled to room temperature then, after filtration, washing and drying step obtain the tridecanyldicarboxylic acid product.
Embodiment 3
Getting 200mL concentration is 90g/l, and the pH value is 7.6 18 carbon dicarboxylic acid fermentation liquid, is heated to 80 ℃, and static 30min divides and removes alkane residual in the solution, removes thalline after filtration, uses the H of 3mol/L again
2SO
4Adjust pH to 3.4,80 ℃ down insulation 30min be cooled to room temperature then, after filtration, washing obtains 18 carbon dicarboxylic acid filter cakes.
Mix with thick acidleach cake with 200mL water, the NaOH solution with 10mol/L transfers to 6.0 with the pH value again, adds the NaCl of 36g simultaneously, be heated to 95 ℃, it is fully dissolved, be cooled to 80 ℃ again and keep 30min, slowly cool to room temperature then, filter and obtain mixed dibasic acid list sodium salt filter cake.In the time of 70 ℃, it is 10 solution that the NaOH that filter cake adds 10mol/L is deployed into pH value, filters and obtains the two salts solutions of clarifying long-chain biatomic acid, the H of adding 3mol/L in solution
2SO
4, adjust pH to 3.0 is heated to 95 ℃ and be incubated 30min, is cooled to room temperature then, after filtration, washing and drying step obtain 18 carbon dicarboxylic acid products.Product property sees Table 1.
Comparative Examples 1
Now, under the situation that does not reclaim long-chain biatomic acid list sodium salt filtering liquid, implement experiment with the second method (being the described method of claim 7) of patent CN1255483A.Get 200mL and obtain tridecanyldicarboxylic acid by the fermentation of candida tropicalis bacterium, concentration is 130g/l, and the pH value is 7.6 fermented liquid, is heated to 80 ℃, and static 30min divides and removes alkane residual in the solution, and filtrate is used the H of 3mol/L
2SO
4The pH value is transferred to 4.0,, reduce to room temperature then, after filtration, washing obtains mycetome tridecanyldicarboxylic acid coarse filtration cake at 80 ℃ of insulation 30min.
Mix with thick acidleach cake with 130mL water, the NaOH solution with 10mol/L transfers to 6.2 with the pH value again, is heated to 95 ℃, is cooled to 80 ℃ then and keeps 30min, slowly cools to room temperature then, filters to obtain mycetome tridecanyldicarboxylic acid list sodium salt filter cake.It is 10 solution that single sodium salt filter cake of mycetome, the NaOH that adds 10mol/L are deployed into pH value, and is heated to 60 ℃ and generates double sodium salts, adds 2% the abundant agitation and filtration of diatomite and obtains the two salts solutions of clarifying long-chain biatomic acid, the H of adding 3mol/L in solution
2SO
4, adjust pH to 4.0 is heated to 95 ℃, and insulation 30min is cooled to room temperature then, after filtration, washing and drying step obtain the tridecanyldicarboxylic acid product.Product property sees Table 1.
Comparative Examples 2
Now, under the situation that reclaims long-chain biatomic acid list sodium salt filtering liquid, implement experiment with the second method (being the described method of claim 7) of patent CN1255483A.Get 200mL and obtain tridecanyldicarboxylic acid by the fermentation of candida tropicalis bacterium, concentration is 130g/l, and the pH value is 7.6 fermented liquid, is heated to 80 ℃, and static 30min divides and removes alkane residual in the solution, and filtrate is used the H of 3mol/L
2SO
4The pH value is transferred to 4.0,, reduce to room temperature then, after filtration, washing obtains mycetome tridecanyldicarboxylic acid coarse filtration cake at 80 ℃ of insulation 30min.
Mix with thick acidleach cake with 130mL water, the NaOH solution with 10mol/L transfers to 6.2 with the pH value again, is heated to 95 ℃, is cooled to 80 ℃ then and keeps 30min, slowly cools to room temperature then, filters to obtain mycetome tridecanyldicarboxylic acid list sodium salt filter cake and filtrate.The gac of adding 2% in the filtrate, in 40 ℃ of decolouring 30min, the filtrate that filtration obtains is mixed with the tridecanyldicarboxylic acid list sodium salt filter cake of mycetome, it is 10 solution that the NaOH that adds 10mol/L is deployed into the pH value, and be heated to 60 ℃ and generate double sodium salts, add 2% the abundant agitation and filtration of diatomite and obtain the two salts solutions of clarifying long-chain biatomic acid, in solution, add the H of 3mol/L
2SO
4, adjust pH to 4.0 is heated to 95 ℃, and insulation 30min is cooled to room temperature then, after filtration, washing and drying step obtain the tridecanyldicarboxylic acid product.Product property sees Table 1.
The character of table 1 product
| Project | Total acid content, wt% | Product alkane content | Colourity | Nitrogen content, μ g/g | Product yield, wt% | Product appearance |
| Example 1 | 99.6 | Do not detect | 24 | 26.5 | 94.7 | White |
| Example 2 | 99.4 | Do not detect | 29 | 33.9 | 94.2 | White |
| Example 3 | 99.2 | Do not detect | 19 | 21.3 | 95.2 | White |
| Comparative Examples 1 | 98.6 | Do not detect | 33 | 43 | 83.2 | Pale yellow |
| Comparative Examples 2 | 99.3 | Do not detect | 28 | 37 | 92.6 | White |
Claims (8)
1. one kind from C
10～C
18In refining one or more C in one or more normal alkane fermentation liquor
10～C
18The method of diprotic acid may further comprise the steps:
I, termination fermented liquid are behind heating demulsification type, Separation and Recovery alkane, and acidifying again, crystallization are filtered and obtained one or more C
10～C
18The diprotic acid filter cake;
II, pH is made in the alkalization of the diprotic acid wet cake of step I gained is 6.0～7.0 diprotic acid list salts solution, adds salting-out agent simultaneously, and heating makes its whole dissolvings, is cooled to room temperature and filtration obtains one or more C after insulation
10～C
18Diprotic acid list salt crystal filter cake;
III, one or more C of Step II gained
10～C
18Diprotic acid list salt crystal filter cake adds alkali dissolution and generates one or more C fully
10～C
18The two salts solutions of diprotic acid, and filtering solid substance;
IV, the filtrate acidifying of Step II I gained is made one or more C
10～C
18The two salt of diprotic acid all are converted into one or more C
10～C
18Diprotic acid obtains one or more C through crystallization, filtration, washing and drying step then
10～C
18Dicarboxylic acid product.
2. in accordance with the method for claim 1, it is characterized in that I removes the thalline in the fermented liquid in the step.
3. in accordance with the method for claim 1, it is characterized in that the pH value after the acidifying is 2～4 in I step, temperature is 75～90 ℃.
4. according to claim 1 or 2 described methods, it is characterized in that the diprotic acid list concentration of salt solution that II prepared in the step is 80～200g/l.
5. according to claim 1 or 2 described methods, it is characterized in that II in the step salting-out agent be NaCl or Na
2SO
4, the salting-out agent of adding and the weight ratio of diprotic acid are 1～3.
6. according to claim 1 or 2 described methods, it is characterized in that II one or more C of heating for dissolving in the step
10～C
18The temperature of diprotic acid list salt is 85～95 ℃, and the dissolving back is incubated 15～30min down at 75～85 ℃ fully.
7. according to claim 1 or 2 described methods, it is characterized in that III generates one or more C in the step
10～C
18The pH value of the two salts solutions of diprotic acid is 9.0～12.0, and temperature is 50～70 ℃.
8. according to claim 1 or 2 described methods, it is characterized in that IV generates one or more C in the step
10～C
18The pH value of diprotic acid solution is 2.0～4.0, and temperature is 80～95 ℃, is incubated 15～30min after acidification reaction is finished under this temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108928A (en) * | 2006-07-20 | 2008-01-23 | 上海凯赛生物技术研发中心有限公司 | Powder paint solidifying agent and method of manufacturing used long chain carbon polyanhydride |
| CN102775292B (en) * | 2011-05-13 | 2015-03-11 | 中国科学院大连化学物理研究所 | Method for refining long chain dicarboxylic acid in n-alkane fermentation solution |
| CN102976917B (en) * | 2012-11-29 | 2014-06-11 | 中国石油化工股份有限公司 | Aqueous-phase refining method of long-chain dibasic acid |
| CN103497100A (en) * | 2013-09-23 | 2014-01-08 | 中国石油化工股份有限公司 | Double-stage purification method of long chain dicarboxylic acid aqueous phase |
| CN104591994B (en) * | 2013-11-03 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of method of refining long-chain biatomic acid |
| CN109824507A (en) * | 2019-02-20 | 2019-05-31 | 宁夏恒力生物新材料有限责任公司 | A kind of long-chain biatomic acid method of purification |
| CN111592457B (en) * | 2019-02-21 | 2023-06-30 | 上海凯赛生物技术股份有限公司 | Long-chain dibasic acid with concentrated particle size distribution and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5058284A (en) * | 1973-09-29 | 1975-05-21 | ||
| CN1079389C (en) * | 1998-12-03 | 2002-02-20 | 中国石油化工集团公司 | Process for refining long-chain biatomic acid |
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2003
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5058284A (en) * | 1973-09-29 | 1975-05-21 | ||
| CN1079389C (en) * | 1998-12-03 | 2002-02-20 | 中国石油化工集团公司 | Process for refining long-chain biatomic acid |
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| CN1611478A (en) | 2005-05-04 |
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