CN104591996B - A kind of process for purification of organic acid - Google Patents
A kind of process for purification of organic acid Download PDFInfo
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- CN104591996B CN104591996B CN201310529516.0A CN201310529516A CN104591996B CN 104591996 B CN104591996 B CN 104591996B CN 201310529516 A CN201310529516 A CN 201310529516A CN 104591996 B CN104591996 B CN 104591996B
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- 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
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- 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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The invention discloses the process for purification of a kind of organic acid.The method includes: I, general terminate fermentation liquid heat inactivation；II, acidifying make organic acid crystallization separate out, it is thus achieved that organic acid crystallization liquid；III, organic acid crystallization liquid or the organic acid filter cake that is filtrated to get are mixed with organic solvent carry out hypergravity process, then carry out organic facies and aqueous phase separation；IV, separate after organic facies scrubbed after, add adsorbent, filtering and removing solid content；The organic facies that V, step IV obtain is cooled to organic acid crystallization and separates out, and through filtering, is dried to obtain refined organic acid production.The inventive method uses organic solvent and hypergravity to process refined organic acid, not only shortens technological process, saves equipment, time and energy consumption etc. and puts into, and can obtain the polymer grade product that purity is high, total nitrogen content is low, is more suitable for industrialized production.
Description
Technical field
The present invention relates to the process for purification of a kind of organic acid, the method particularly obtaining high-purity organic acid from fermentation liquid.
Background technology
The organic acid molecule formula of indication of the present invention is CnH2n-2O4, wherein n is 10-18, is that microorganism utilizes the fermentation such as liquid wax and the metabolite that obtains.Its fermentation liquid is complicated heterogeneous system, the culture medium wherein contain unreacted carbon source, microbial cell and fragment, not utilizing and metabolite and the secretions etc. of microorganism, wherein contain a large amount of protein, pigment and ash to grade impurity, have a strong impact on purity and the application of product, and bring difficulty with refined to the extraction of this kind organic acid.
At present, on market the highest to this kind organic acid purity requirement, the particularly purity requirement of polymer grade is higher, typically require that organic acid mono-acid purity is at more than 98.5wt%, total nitrogen ＜ 30 g/g, the most only purifies with organic solvent method and could obtain the polymer grade product meeting this requirement, and generally, even if purity reaches requirement, its total nitrogen content is still relatively inaccessible to requirement.
In CN01142806.6, with long-chain biatomic acid dry powder as raw material, use acetone, methanol and ethanol as solvent refining long-chain biatomic acid.Binary acid in this method first fermentation liquid is first after activated carbon adsorption, then acidizing crystal, filters, washes and be dried binary acid crystalli-zation cake and obtain long-chain biatomic acid dry powder, then uses organic solvent to refine.The raw material that the method refines is that aqueous filter cake obtains binary acid dry powder after drying, and raw aqueous quantitative limitation reduces the operating flexibility of the method, adds the equipment that thick acid is dried, causes this technological process longer, add production cost.And the method is in the aqueous solution of the alkaline binary acid sodium salt obtained before binary acid crystalli-zation cake and in solvent refining processes, carry out twice activated carbon adsorption altogether to process, 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 the biggest, the yield of product is the lowest.And when organic solvent refines binary acid, use adsorbent typically can reach the requirement of decolouring, but still more difficult removing small molecular protein therein, make total nitrogen content undesirable.
In long-chain biatomic acid process for purification disclosed in CN200410018255.7, first fermentation method reactant liquor is carried out pretreatment, to remove thalline therein and residual alkane or fatty acid, obtain organic acid clear liquid, then carrying out acidizing crystal, acidizing crystal liquid obtains organic acid crude product through filter press again；Finally by the crude product obtained is refined in high vacuum conditions by wiped film vaporization, short course distillation device or employing organic solvent refines.After the binary acid crude product that the method obtains and solvent mixed dissolution, the removings such as filtration are not taked to go the operating procedure of insoluble impurities, so during decrease temperature crystalline, insoluble impurities necessarily adsorbs crystal surface, have impact on product purity, brings bad impact to the application of product.And the solvent refining binary acid process in the method, include the solvent recrystallization operation of twice, solvent consumption is bigger, add the burden that solvent recovery is refined, cause operating process complex, and the highest only 98.75wt% of binary acid purity using solvent method to be refining to obtain, when production is slightly fluctuated, it is possible to can not get qualified product.
Summary of the invention
For the deficiencies in the prior art, the invention provides the process for purification of a kind of organic acid.Compared with prior art, the inventive method technique is simple, and energy consumption is low, and supplies consumption is few, and obtained organic acid purity is high, and the impurity content such as small protein and pigment is low, is more suitable for industrialized production.
The process for purification of a kind of organic acid of the present invention, including:
I, general terminate fermentation liquid heat inactivation；
II, acidifying make organic acid crystallization separate out, it is thus achieved that organic acid crystallization liquid；
III, organic acid crystallization liquid or the organic acid filter cake that is filtrated to get are mixed with organic solvent make organic acid dissolve, hypergravity equipment is heated to organic acid solution temperature, above-mentioned mixed system is carried out hypergravity process, hypergravity level be 10-650g(g be acceleration of gravity=9.8m/s2), the mean residence time that hypergravity processes is 0.2-10s, and mixed system carries out organic facies and aqueous phase separation after hypergravity processes；
After organic phase washed with water after IV, separation, add adsorbent, filtering and removing solid content；
The organic facies that V, step IV obtain is cooled to organic acid crystallization and separates out, and through filtering, is dried to obtain refined organic acid production.
In the inventive method, terminating fermentation liquid described in step I is the metabolite that microorganism utilizes that the fermentation of liquid wax obtains, and the organic acid molecule formula wherein contained is CnH2n-2O4, wherein n is 10-18, and organic acid can be single a kind of organic acid, it is also possible to be mixed organic acid.After terminating fermentation liquid heat inactivation, can carry out the impurity such as filtering and removing thalline, filtration can use the conventional methods such as membrane filtration and equipment.Can also in step III the impurity such as separation removal thalline.Heat inactivation temperature is generally 75 DEG C～100 DEG C.
In the inventive method, the acidifying described in step II can use conventional method to carry out.The pH value of described acidifying is 2.0 ~ 4.0, and heating-up temperature is 80 ~ 100 DEG C.The acid used by acidifying that the present invention is above-mentioned can be the H of any concentration2SO4、HNO3, HCl or H3PO4。
Organic solvent used by step III is one or more in alcohols, ketone, esters, ethers, alkane, cycloalkane, aromatic hydrocarbons, preferably in ethanol, dipropyl ketone, isobutyl acetate, dodecane, ethylcyclohexane, toluene, ether one or more.
In the inventive method, organic solvent is 1:1 ~ 15:1, preferably 2:1 ~ 7:1 with the weight ratio of organic acid butt.Organic acid crystallization liquid or organic acid filter cake dissolve the most in a heated condition with organic solvent, and heating-up temperature is generally 80 DEG C ~ 150 DEG C, preferably 90 ~ 120 DEG C, determine with specific reference to the boiling point selecting solvent, generally below the boiling temperature of used solvent.
In the inventive method, can carry out hypergravity process in step III mixed system after adding appropriate trinitrophenol, addition is 1 ~ 15wt% of organic acid butt weight (the theoretical acid content of fermentation liquid), preferably 2 ~ 5 wt%.Treatment effect, particularly ether organic solvent and trinitrophenol can be significantly improved after adding trinitrophenol and there is when being used in mixed way more preferably separating effect.
In the inventive method, hypergravity processes and carries out in hypergravity equipment, and hypergravity equipment includes the conventional hypergravity rotary apparatuss such as high gravity rotating packed bed, deflector type, screw path type, rotating compact disc formula and fixed-rotator type, preferably high gravity rotating packed bed.Hypergravity level refers to that supergravity reactor rotor rotates the size of the centrifugal acceleration produced, and generally represents with the multiple of gravity acceleration g, the most relevant with the internal-and external diameter of the rotating speed of rotor and rotor.
In the inventive method, step IV can add deionized water wash organic facies once or more, and isolate aqueous phase.
In the inventive method, the adsorbent in step IV is one or more in activated carbon, active hargil etc., preferably activated carbon, and addition is the 0.01wt% ~ 2.0wt% of organic acid butt weight, preferably 0.01wt% ~ 1.0wt%, and adsorption time is 30min
~60min。
In the inventive method, till in step V, crystallisation by cooling temperature generally makes organic acid sufficient crystallising, temperature is generally 10 DEG C～30 DEG C.
In the inventive method, the organic solvent filtrate obtained in step V, can recycle.
The inventive method can obtain the organic acid production of highly purified single kind, it is also possible to obtain mixed organic acid product.
Although it is this area conventional method that organic solvent method refines such organic acid, but the optimum solvent used in existing method and optimal process route, also can only obtain purity and be slightly above the purity of product quality indicator requirement (98.5%), this is disadvantageous to the steady production of commercial plant, when production is slightly fluctuated, it is possible to can not get qualified product.The inventors found that, organic facies containing organic acid can separate the impurity such as protein and pigment after hypergravity processes efficiently, impurity removes with the separation of aqueous phase, and more than 99.5% and total nitrogen is less than the organic acid production of 30 g/g the most only to use minimal amount of adsorbent to can be obtained by purity.In the art, it has been very difficult that purpose product quality reaches polymer grade index request, purity often improves 0.1 percentage point and total nitrogen 1 g/g of reduction on this basis is all the most difficult, and it is the most all significant and value, this is to ensureing commercial plant steady running, improving the aspects such as conforming product rate, have important effect, the quality impact on polymerization products such as follow-up synthesizing engineering plastics is also obviously.
The inventive method, while obtaining high-purity organic acid production, also has technical process simple, the advantages such as energy consumption is low, and supplies consumption is few.
Detailed description of the invention
The process for purification of the present invention is further illustrated below by embodiment.In the present invention, wt% is mass fraction.
In the inventive method, containing liquid wax, thalline, the culture medium not utilized, metabolite and microorganism secretion thing etc. in fermentation liquid, wherein contain the impurity such as a large amount of protein, pigment.Organic acid crystallization liquid can use this area usual way to obtain, as used at least one scheme following:
(1) being heated by termination fermentation liquid and stand, dividing the liquid wax going to upper strata, then cooling filtration sterilization, obtain filtrate and be acidified with acid to pH2.0 ~ 4.0, and heat simultaneously, obtain organic acid crystallization liquid, or aqueous solutions of organic acids is filtrated to get filter cake；
Actual conditions is: will terminate fermentation liquid and heat 75 DEG C ~ 100 DEG C, regulation pH value >=9, stand, then divide the liquid wax that upper strata remains, then be cooled to 60 DEG C ~ 80 DEG C, through microfiltration and or ultrafiltration apparatus, it is filtered to remove the impurity such as thalline and obtains clear liquid, the clear liquid obtained is added acid for adjusting pH value to 2.0 ~ 4.0, and is heated to 80 DEG C ~ 100 DEG C, obtain organic acid crystallization liquid, or aqueous solutions of organic acids is filtrated to get filter cake.
(2) fermentation liquid is heated to 75 DEG C ~ 100 DEG C, and is acidified to pH value 2.0 ~ 4.0, stand, separate and recover liquid wax, obtain organic acid crystallization liquid, or aqueous solutions of organic acids is filtrated to get filter cake.
(3) fermentation liquid is heated to 75 DEG C ~ 90 DEG C, enters microfiltration or ultrafiltration apparatus, remove thalline and liquid wax etc., the acidification of filtrate obtained to pH value 2.0 ~ 4.0, and be heated to 80 DEG C ~ 100 DEG C, obtain organic acid crystallization liquid, or aqueous solutions of organic acids is filtrated to get filter cake.
Embodiment 1
Take 200ml and obtained C by Candida tropicalis fermentation12H22O4Organic acid fermentation liquid, concentration is 160g/l.It is heated to 80 DEG C, uses H2SO4PH value is adjusted to 3.0, stands 2h, divide the liquid wax going solution to remain, obtain the C of mycetome12H22O4Organic acid crystallization liquid.
The C obtaining mycetome12H22O4Organic acid crystallization liquid and dipropyl ketone (dipropyl ketone and C12H22O4Weight ratio is 6:1) mixing, it is heated to 115 DEG C, after organic acid dissolves, mixed system is sent into and has been heated in the hypergravity equipment of 115 DEG C carrying out hypergravity process, hypergravity level is 50g, the mean residence time that hypergravity processes is 0.2s, the static 60min of mixed system that will process through hypergravity, point sub-cloud aqueous phase；In solvent phase, add 30ml deionized water wash organic facies again, again divide aqueous phase；With adding 0.2g activated carbon insulation decolouring 30min in backward organic facies, being then filtered to remove activated carbon, the organic facies after decolouring is cooled to 19 DEG C of crystallizations and obtains C12H22O4Organic acid, then obtain product through filtration drying step.Product quality is shown in Table 1.
Embodiment 2
Take 200ml and obtained C by Candida tropicalis fermentation12H22O4Organic acid fermentation liquid, concentration is 162g/l, regulation pH to 10.0, is heated to 80 DEG C, stands 2h, divide the liquid wax going solution to remain, lower floor's solution microfiltration equipment, is filtered to remove the impurity such as thalline and obtains clear liquid, and the clear liquid obtained is added acid for adjusting pH value to 3.5, and it is heated to 80 DEG C, obtain organic acid crystallization liquid.
The C obtained12H22O4Organic acid crystallization liquid and isobutyl acetate (isobutyl acetate and C12H22O4Weight ratio is 4:1) mixing, it is heated to 95 DEG C, after organic acid dissolves, mixed system is sent into and has been heated in the hypergravity equipment of 95 DEG C carrying out hypergravity process, hypergravity level is 150g, the mean residence time that hypergravity processes is 0.8s, the static 30min of mixed system that will process through hypergravity, point sub-cloud aqueous phase；In solvent phase, add 50ml deionized water wash organic facies again, again divide aqueous phase；Adding 0.16g activated carbon insulation decolouring 30min in organic facies, be then filtered to remove activated carbon, the organic facies after decolouring is cooled to 28 DEG C of crystallizations and obtains C12H22O4Organic acid, then obtain product through filtration drying step.Product quality is shown in Table 1.
Embodiment 3
Take 200ml and obtained C by Candida tropicalis fermentation13H24O4Organic acid fermentation liquid, concentration is 154g/l.Being heated to 70 DEG C, through ceramic micro filter membrane filtration, the liquid wax of removing thalline and remnants obtains filtrate.H is added in filtrate2SO4Regulation pH value is to 2.4, and is heated to 95 DEG C, obtains C13H24O4Organic acid crystallization liquid, is cooled to room temperature and is filtrated to get organic acid filter cake.
The C obtained13H24O4Organic acid filter cake and dodecane (dodecane and C13H24O4Weight ratio is 8:1) mixing, system is heated to 98 DEG C, after organic acid dissolves, mixed system is sent into and has been heated in the hypergravity equipment of 98 DEG C carrying out hypergravity process, hypergravity level is 300g, the mean residence time that hypergravity processes is 5s, the static 40min of mixed system that will process through hypergravity, point sub-cloud aqueous phase；In solvent phase, add 60ml deionized water wash organic facies again, again divide aqueous phase；Adding 0.3g activated carbon insulation decolouring 30min to organic facies, be then filtered to remove activated carbon, the organic facies after decolouring is cooled to 15 DEG C of crystallizations and obtains C13H24O4Organic acid, then obtain product through filtration drying step.Product quality is shown in Table 1.
Embodiment 4
Take the C that 200ml concentration is 145g/l14H26O4Organic acid fermentation liquid, is heated to 70 DEG C, and through ceramic micro filter membrane filtration, the liquid wax of removing thalline and remnants obtains filtrate.H is added in filtrate2SO4Regulation pH value is to 3.0, and is heated to 95 DEG C, obtains C14H26O4Organic acid crystallization liquid.
The C obtained14H26O4Organic acid crystallization liquid and ether (ether and C14H26O4Weight ratio is 6:1) mixing, after organic acid dissolves, mixed system is sent into hypergravity equipment carries out hypergravity process, hypergravity level is 500g, the mean residence time that hypergravity processes is 10s, the static 40min of mixed system that will process through hypergravity, point sub-cloud aqueous phase；In solvent phase, add 30ml deionized water wash organic facies again, again divide aqueous phase；Adding 0.15g activated carbon insulation decolouring 30min in organic facies, be then filtered to remove activated carbon, the organic facies after decolouring is cooled to 22 DEG C of crystallizations and obtains C14H26O4Organic acid, then obtain product through filtration drying step.Product quality is shown in Table 1.
Embodiment 5
Carrying out hypergravity process after adding 1.0g trinitrophenol in mixed system, remaining is with embodiment 4.Product quality is shown in Table 1.
Embodiment 6
Ether in embodiment 5 is changed to dipropyl ketone, and organic acid crystallization liquid makes organic acid dissolve with dipropyl ketone mixing post-heating to 115 DEG C, and hypergravity equipment is previously heated to 115 DEG C, and remaining is with embodiment 5.Product quality is shown in Table 1.
Embodiment 7
Carrying out hypergravity process after adding 1.5g trinitrophenol in mixed system, remaining is with embodiment 4.Product quality is shown in Table 1.
Comparative example 1
Mixed system does not carry out hypergravity process, and remaining is with embodiment 1, and product quality is shown in Table 1.
Table 1 organic acid production quality
Claims (15)
1. a process for purification for organic acid, including:
I, general terminate fermentation liquid heat inactivation；
II, acidifying make organic acid crystallization separate out, it is thus achieved that organic acid crystallization liquid；
III, organic acid crystallization liquid or the organic acid filter cake that is filtrated to get being mixed with organic solvent and make organic acid dissolve, above-mentioned mixed system carries out hypergravity process, hypergravity level is 10-650g, and wherein g is acceleration of gravity=9.8m/s2, the mean residence time that hypergravity processes is 0.2-10s, and mixed system carries out organic facies and aqueous phase separation after hypergravity processes；
After organic phase washed with water after IV, separation, add adsorbent, filtering and removing solid content；
The organic facies that V, step IV obtain is cooled to organic acid crystallization and separates out, and through filtering, is dried to obtain refined organic acid production；
Carrying out hypergravity process after it is characterized in that adding appropriate trinitrophenol in step III mixed system, addition is 1 ~ 15 wt% of organic acid butt weight.
The most in accordance with the method for claim 1, it is characterised in that organic solvent is one or more in alcohols, ketone, esters, ethers, alkane, cycloalkane, aromatic hydrocarbons.
The most in accordance with the method for claim 1, it is characterised in that described organic solvent is in ethanol, dipropyl ketone, isobutyl acetate, dodecane, ethylcyclohexane, toluene, ether one or more.
The most in accordance with the method for claim 1, it is characterised in that after adding appropriate trinitrophenol in step III mixed system, carry out hypergravity process, addition is 2 ~ 5wt% of organic acid butt weight.
The most in accordance with the method for claim 1, it is characterised in that hypergravity processes and carries out in hypergravity equipment, hypergravity equipment includes high gravity rotating packed bed, deflector type, screw path type, rotating compact disc formula and fixed-rotator type hypergravity rotary apparatus.
The most in accordance with the method for claim 1, it is characterised in that described organic acid molecule formula is CnH2n-2O4, wherein n is 10-18, and organic acid is single a kind of organic acid or is mixed organic acid.
The most in accordance with the method for claim 1, it is characterised in that step I heat inactivation temperature is 75 DEG C～100 DEG C.
The most in accordance with the method for claim 1, it is characterised in that described in step II, the pH value of acidifying is 2.0 ~ 4.0, and heating-up temperature is 80 ~ 100 DEG C, and the acid used by acidifying is the H of any concentration2SO4、HNO3, HCl or H3PO4。
The most in accordance with the method for claim 1, it is characterised in that in step III, organic solvent is 1:1 ~ 15:1 with the weight ratio of organic acid butt.
The most in accordance with the method for claim 1, it is characterised in that in step III, organic solvent is 2:1 ~ 7:1 with the weight ratio of organic acid butt.
11. in accordance with the method for claim 1, it is characterised in that in step III, and organic acid crystallization liquid or organic acid filter cake dissolve in a heated condition with organic solvent, and heating-up temperature is 80 DEG C ~ 150 DEG C.
12. in accordance with the method for claim 1, it is characterised in that the adsorbent in step IV is one or more in activated carbon, active hargil, and addition is the 0.01wt% ~ 2.0wt% of organic acid butt weight, and adsorption time is 30min ~ 60min.
13. in accordance with the method for claim 1, it is characterised in that the 0.01wt% ~ 1.0wt% that adsorbent addition is organic acid butt weight in step IV.
14. in accordance with the method for claim 1, it is characterised in that in step II, organic acid crystallization liquid employing at least one scheme following:
(1) termination fermentation liquid being heated to 75 DEG C ~ 100 DEG C and stands, dividing the liquid wax going to upper strata, then cooling filtration sterilization, obtain filtrate and be acidified with acid to pH2.0 ~ 4.0, and be simultaneously heated to 80 DEG C ~ 100 DEG C, obtain organic acid crystallization liquid；
(2) termination fermentation liquid is heated to 75 DEG C ~ 100 DEG C, and is acidified to pH value 2.0 ~ 4.0, stand, separate and recover liquid wax, obtain organic acid crystallization liquid；
(3) fermentation liquid being heated to 75 DEG C ~ 90 DEG C, enter microfiltration or ultrafiltration apparatus, removing thalline and liquid wax, the acidification of filtrate obtained is to pH value 2.0 ~ 4.0, and is heated to 80 DEG C ~ 100 DEG C, obtains organic acid crystallization liquid.
15. in accordance with the method for claim 1, it is characterised in that till in step V, crystallisation by cooling temperature is for making organic acid sufficient crystallising, and temperature is 10 DEG C～30 DEG C.
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Effective date of registration: 20230818 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |
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