CN1569315A - Method for recovering organic acid from organic solvent - Google Patents
Method for recovering organic acid from organic solvent Download PDFInfo
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- CN1569315A CN1569315A CN 200410037759 CN200410037759A CN1569315A CN 1569315 A CN1569315 A CN 1569315A CN 200410037759 CN200410037759 CN 200410037759 CN 200410037759 A CN200410037759 A CN 200410037759A CN 1569315 A CN1569315 A CN 1569315A
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- acid
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- organic solvent
- organic acid
- aqueous solution
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- 150000007524 organic acids Chemical class 0.000 title claims abstract description 56
- 239000003960 organic solvent Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 33
- 238000000909 electrodialysis Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 14
- -1 organic acid salt Chemical class 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000003411 electrode reaction Methods 0.000 claims abstract description 4
- 239000008267 milk Substances 0.000 claims description 29
- 210000004080 milk Anatomy 0.000 claims description 29
- 235000013336 milk Nutrition 0.000 claims description 29
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 12
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 8
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229940043265 methyl isobutyl ketone Drugs 0.000 claims description 8
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 6
- 239000001530 fumaric acid Substances 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 6
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 6
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 102100040653 Tryptophan 2,3-dioxygenase Human genes 0.000 claims description 4
- 101710136122 Tryptophan 2,3-dioxygenase Proteins 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 4
- 239000003011 anion exchange membrane Substances 0.000 claims description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 4
- 125000005270 trialkylamine group Chemical group 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 150000001243 acetic acids Chemical class 0.000 claims description 3
- 239000011260 aqueous acid Substances 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 3
- 238000010977 unit operation Methods 0.000 claims description 3
- 229940005605 valeric acid Drugs 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000004816 latex Substances 0.000 abstract 2
- 229920000126 latex Polymers 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 1
- 230000001360 synchronised effect Effects 0.000 abstract 1
- 238000006276 transfer reaction Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 description 1
- 208000035126 Facies Diseases 0.000 description 1
- YEJCDKJIEMIWRQ-UHFFFAOYSA-N Linopirdine Chemical compound O=C1N(C=2C=CC=CC=2)C2=CC=CC=C2C1(CC=1C=CN=CC=1)CC1=CC=NC=C1 YEJCDKJIEMIWRQ-UHFFFAOYSA-N 0.000 description 1
- 239000001744 Sodium fumarate Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- MSJMDZAOKORVFC-SEPHDYHBSA-L disodium fumarate Chemical compound [Na+].[Na+].[O-]C(=O)\C=C\C([O-])=O MSJMDZAOKORVFC-SEPHDYHBSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229940117955 isoamyl acetate Drugs 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229940005573 sodium fumarate Drugs 0.000 description 1
- 235000019294 sodium fumarate Nutrition 0.000 description 1
- 239000001540 sodium lactate Substances 0.000 description 1
- 229940005581 sodium lactate Drugs 0.000 description 1
- 235000011088 sodium lactate Nutrition 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
- 239000004324 sodium propionate Substances 0.000 description 1
- 235000010334 sodium propionate Nutrition 0.000 description 1
- 229960003212 sodium propionate Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a method for reclaiming organic acid from organic solvent in chemical mass transfer separation technology field. the organic solvent loaded with organic acid is mixed with aqueous solution of the organic acid salt and they are produced into latex liquid, then the latex and the aqueous solution containing the organic acid enters the negative chamber and positive chamber of the electrodialysis device, it realizes the synchronous extraction and condense of organic acid in the aqueous solution through electric transfer and electrode reaction. Compared with current technology, it has a high energy utilization rate, and low cost and side product.
Description
Technical field
The present invention relates to belong to chemical industry mass transfer isolation technique field, particularly a kind of organic acid method that from organic solvent, reclaims.
Background technology
Organic acid is a class basic chemical industry raw material, and fermentation method is to produce one of organic acid important method, but contains a large amount of impurity in the thick production fluid of fermentation method, and organic acid concentration and purity are all lower, obtain to have the product of commercial value, must separate and carry dense.
Solvent extration very is fit to optionally extract organic acid from the low concentration aqueous solution.U.S. Miles company uses the organic amine extraction agent, is reverse-extraction agent with hot water, has realized complete organic acid leaching process, this process is compared with the calcium salt method that extensively adopts at present, and yield is higher, material consumption and less side products, but production fluid concentration is very low, and further carrying dense then cost increases a lot.Therefore the organic acid high efficiency method is reclaimed in necessary development from organic solvent, and this relates in the dilute solution organic acid recovery and carry dense similar process significant equally for other, and as from waste water reclamation acetic acid, dilute formic acid solution is carried dense, or the like.
Summary of the invention
The purpose of this invention is to provide a kind of organic acid method that from organic solvent, reclaims, it is characterized in that: described to reclaim the organic acid method from organic solvent be at normal temperatures and pressures, load organic acid organic solvent and the aqueous solution that contains this organic acid salt are made milk sap, then with as cathode compartment and the anolyte compartment that this organic acid aqueous solution enters electrodialysis appts respectively that contain that receives mutually, realize organic acid simultaneous extraction in the organic solvent is concentrated by electromigration and electrode reaction.This method comprises the steps:
(1) adopt mechanical stirring, ultrasonic wave or microscale dispersing method that load is had organic acid organic solvent and the aqueous solution that contains organic hydrochlorate, make it to form milk sap, the lifetime of milk sap is suitable with the residence time of electrodialysis unit operation at least, and the mixed volume ratio is chosen in the scope of (1: 3)～(20: 1);
(2) use pump or other liquid transporting apparatus with the milk sap that obtains with as anolyte compartment and the cathode compartment that organic aqueous acid is transported to electrodialysis appts respectively that contain that receives mutually, electrodialysis operation is carried out in energising, and the organic acid concentration in the reception mutually is chosen in the scope of 0～15M;
(3) cathode compartment effluent liquid phase-splitting in clarification equipment, organic solvent obtain regeneration or partial regeneration, and water can be used as the aqueous solution that uses in the step 1;
(4) anolyte compartment's effluent liquid is made with extra care as production fluid or is concentrated, and the part production fluid can be that 0～15M mixes as the reception of using in the step 2 mutually with water by organic acid concentration.
Described organic solvent is the organic solvent that organic acid is had selective extraction capacity: trialkylamine, C12～C23 primary amine, TRPO, trialkyl phosphine acid esters, trialkyl phosphates, methyl iso-butyl ketone (MIBK), alkyl acetate, primary isoamyl alcohol or propyl carbinol.
Described organic acid is meant to dissociate in water becomes the organic compound of hydrogen ion and acid ion: citric acid, lactic acid, acetic acid, oxysuccinic acid, toxilic acid, fumaric acid, halogenated acetic acids, oxyacetic acid, oxoethanoic acid, oxalic acid, propionic acid, butyric acid or valeric acid.
Use anion-exchange membrane in the described electrodialysis appts.
Organic acid described in the step 1,2,3 refers to a kind of organic acid.
Can contain a small amount of organic acid in the aqueous solution described in the step 1.
Compared with prior art, advantage of the present invention and positively effect are: present method can effectively improve the current density and the current efficiency of two-phase electrodialysis process, significantly accelerate organic acid and reclaim and organic solvent regenerated process, obtain the higher aqueous solutions of organic acids of concentration.Simultaneously, the present invention is easy to operate, good operation stability, and material consumption and energy consumption are low, and the waste and the secondary pollution of generation are few.
Embodiment
The invention provides a kind of organic acid method that from organic solvent, reclaims, this method is at normal temperatures and pressures, load organic acid organic solvent and the aqueous solution that contains this organic acid salt are made milk sap, then with as cathode compartment and the anolyte compartment that this organic acid aqueous solution enters electrodialysis appts respectively that contain that receives mutually, realize organic acid simultaneous extraction in the organic solvent is concentrated by electromigration and electrode reaction.This method comprises the steps:
(1) adopt mechanical stirring, ultrasonic wave or microscale dispersing method that load is had organic acid organic solvent and the aqueous solution that contains organic hydrochlorate, make it to form milk sap, the lifetime of milk sap is suitable with the residence time of electrodialysis unit operation at least, and the mixed volume ratio is typically chosen in the scope of (1: 3)～(20: 1);
(2) use pump or other liquid transporting apparatus with the milk sap that obtains with as anolyte compartment and the cathode compartment that organic aqueous acid is transported to electrodialysis appts respectively that contain that receives mutually, electrodialysis operation is carried out in energising, and the organic acid concentration in the reception mutually is typically chosen in the scope of 0～15M;
(3) cathode compartment effluent liquid phase-splitting in clarification equipment, organic solvent obtain regeneration or partial regeneration, and water can be used as the aqueous solution that uses in the step 1;
(4) anolyte compartment's effluent liquid is made with extra care as production fluid or is concentrated, and the part production fluid can be that 0～15M mixes as the reception of using in the step 2 mutually with water by organic acid concentration.
Described organic solvent is the organic solvent that organic acid is had selective extraction capacity: trialkylamine, C12～C23 primary amine, TRPO, trialkyl phosphine acid esters, trialkyl phosphates, methyl iso-butyl ketone (MIBK), Isoamyl Acetate FCC, primary isoamyl alcohol or propyl carbinol.
Described organic acid is meant to dissociate in water becomes the organic compound of hydrogen ion and acid ion: citric acid, lactic acid, acetic acid, oxysuccinic acid, toxilic acid, fumaric acid, halogenated acetic acids, oxyacetic acid, oxoethanoic acid, oxalic acid, propionic acid, butyric acid or valeric acid.
Use anion-exchange membrane in the described electrodialysis appts.
Concrete implementation step comprises:
(1) takes the dress electrodialysis unit, be full of cathode compartment and anolyte compartment respectively, make the abundant swelling of mould material, to improve the stability of electrodialysis unit size and operation with organic solvent and water;
(2) in mixing vessel, add certain organic acid organic solvent of load and the aqueous solution that contains organic hydrochlorate in advance, start to stir and make it to mix formation milk sap, the content of organic acid salt can increase under the situation that solubleness allows as far as possible in its aqueous solution, thereby reduces cathode compartment resistance and consequent joule heating.
(3) with pump with milk sap with carry to cathode compartment and anolyte compartment respectively as the aqueous solutions of organic acids that receives mutually, power up to electrodialysis unit simultaneously, carry out electrodialysis operation, wherein the organic acid concentration in the reception mutually will be as the criterion with the conductive capability of assurance anolyte and the concentration requirement of production fluid;
(4) the cathode compartment effluent liquid enters the phase-splitting of branch facies unit, and water turns back to mixed cell, carries pending organic solvent with pump to mixing section simultaneously, guarantees the turnover material balance of mixed cell;
(5) with pump segment anode chamber effluent liquid is transported in the reception phase storage tank, to wherein adding entry, guarantees to receive the turnover material balance of phase storage tank simultaneously.
(6) move the sufficiently long time continuously, make system reach steady state operation.
Wherein, organic solvent need meet following standard:
A. to combine with organic acid be reversing process to organic solvent;
B. organic solvent is water insoluble or not soluble in water;
Adopt anion-exchange membrane in the electrodialysis unit, require this film to have less face resistance, not yielding, not by organic solvent dissolution.Can use porous support materials that film is supported receiving mutually a side, as non-woven fabrics etc.
The technology that the present invention mentions can be stopped in implementation process immediately, need not after the parking the feed liquid emptying in the device, and is longer as shutdown period, can be with the feed liquid emptying in the electrodialysis unit.Only the present invention is further specified below for 5 embodiment (all the other are basic identical).
Embodiment 1
Electrodialysis unit two-phase chamber size is 120mm * 50mm * 5mm, membrane area 60cm
2Make to receive phase with the aqueous citric acid solution of 0.730M, organic solvent is a trialkylamine, wherein the starting point concentration of citric acid is 0.561M, the water that preparation milk sap is used is the sodium citrate aqueous solution of 0.782M, the profit proportioning is 1: 3 (v/v) during preparation milk sap, the milk sap inlet flow rate is 3.08mL/min, receiving the phase inlet flow rate is 3.39mL/min, strength of current 0.504A, voltage 18V is after operation reaches stable state continuously, anolyte compartment's outlet is the aqueous citric acid solution of 0.775M, and flow is 3.58mL/min.Current efficiency 77.0%.
Embodiment 2
Electrodialysis unit two-phase chamber size is 120mm * 50mm * 5mm, membrane area 60cm
2Make to receive phase with the fumaric acid aqueous solution of 0.737M, organic solvent is a TRPO, wherein the starting point concentration of fumaric acid is 0.561M, the water that preparation milk sap is used is the sodium fumarate aqueous solution of 0.782M, the profit proportioning is 1: 1 (v/v) during preparation milk sap, the milk sap inlet flow rate is 3.08mL/min, receiving the phase inlet flow rate is 3.48mL/min, strength of current 0.498A, voltage 19.3V is after operation reaches stable state continuously, anolyte compartment's outlet is the fumaric acid aqueous solution of 0.774M, and flow is 3.55mL/min.Current efficiency is 59.0%.
Embodiment 3
Electrodialysis unit two-phase chamber size is 120mm * 50mm * 5mm, membrane area 60cm
2, to do to receive phase with the oxalic acid aqueous solution of 3.537M, organic solvent is a tributyl phosphate, the starting point concentration of its mesoxalic acid is 0.561M, the water that preparation milk sap is used is the sodium oxalate aqueous solution of 3.582M, and the profit proportioning is 1: 1 (v/v) during preparation milk sap, and the milk sap inlet flow rate is 3.08mL/min, receiving the phase inlet flow rate is 3.50mL/min, strength of current 1.10A, voltage 23.6V is after operation reaches stable state continuously, anolyte compartment's outlet is the oxalic acid aqueous solution of 0.824M, and flow is 3.76mL/min.Current efficiency 76.2%.
Embodiment 4
Electrodialysis unit two-phase chamber size is 120mm * 50mm * 5mm, membrane area 60cm
2, to do to receive phase with the propionic acid aqueous solution of 4.537M, organic solvent is a primary isoamyl alcohol, wherein the starting point concentration of propionic acid is 0.660M, the water that preparation milk sap is used is the Sodium Propionate aqueous solution of 4.565M, and the profit proportioning is 1: 1 (v/v) during preparation milk sap, and the milk sap inlet flow rate is 3.08mL/min, receiving the phase inlet flow rate is 3.40mL/min, strength of current 1.10A, voltage 22.8V is after operation reaches stable state continuously, anolyte compartment's outlet is the propionic acid aqueous solution of 0.838M, and flow is 3.65mL/min.Current efficiency 80.4%.
Embodiment 5
Electrodialysis unit two-phase chamber size is 120mm * 50mm * 5mm, membrane area 60cm
2, to do to receive phase with the lactic acid aqueous solution of 0.712M, organic solvent is a methyl iso-butyl ketone (MIBK).Wherein the starting point concentration of lactic acid is 0.520M, the water that preparation milk sap is used is the sodium lactate aqueous solution of 0.780M, the profit proportioning is 3: 1 (v/v) during preparation milk sap, the milk sap inlet flow rate is 3.08mL/min, and receiving the phase inlet flow rate is 3.38mL/min, strength of current 1.10A, voltage 23.1V, after operation reached stable state continuously, anolyte compartment's outlet was the lactic acid aqueous solution of 0.825M, and flow is 3.55mL/min.Current efficiency 76.0%.
Claims (6)
1. one kind is reclaimed the organic acid method from organic solvent, it is characterized in that: described to reclaim the organic acid method from organic solvent be at normal temperatures and pressures, load organic acid organic solvent and the aqueous solution that contains this organic acid salt are made milk sap, then with as cathode compartment and the anolyte compartment that this organic acid aqueous solution enters electrodialysis appts respectively that contain that receives mutually, realize organic acid simultaneous extraction in the organic solvent is concentrated by electromigration and electrode reaction.This method comprises the steps:
(1) adopts mechanical stirring, ultrasonic wave or microscale dispersing method that load is had organic acid organic solvent and the aqueous solution that contains organic hydrochlorate, make it to form milk sap;
(2) use pump or other liquid transporting apparatus with the milk sap that obtains with as anolyte compartment and the cathode compartment that organic aqueous acid is transported to electrodialysis appts respectively that contain that receives mutually, electrodialysis operation is carried out in energising;
(3) cathode compartment effluent liquid phase-splitting in clarification equipment, organic solvent obtain regeneration or partial regeneration;
(4) anolyte compartment's effluent liquid is made with extra care as production fluid or is concentrated.
2. according to the described organic acid method that reclaims from organic solvent of claim 1, it is characterized in that: described organic solvent is the organic solvent that organic acid is had selective extraction capacity: trialkylamine, C12～C23 primary amine, TRPO, trialkyl phosphine acid esters, trialkyl phosphates, methyl iso-butyl ketone (MIBK), alkyl acetate, primary isoamyl alcohol or propyl carbinol.
3. according to the described organic acid method that reclaims from organic solvent of claim 1, it is characterized in that: described organic acid is meant to dissociate in water becomes the organic compound of hydrogen ion and acid ion: citric acid, lactic acid, acetic acid, oxysuccinic acid, toxilic acid, fumaric acid, halogenated acetic acids, oxyacetic acid, oxoethanoic acid, oxalic acid, propionic acid, butyric acid or valeric acid.
4. according to the described organic acid method that from organic solvent, reclaims of claim 1, it is characterized in that: use anion-exchange membrane in the described electrodialysis appts.
5. according to the described organic acid method that from organic solvent, reclaims of claim 1, it is characterized in that: the lifetime of milk sap is suitable with the residence time of electrodialysis unit operation at least in the described step 1, and the mixed volume ratio can be chosen in the scope of (1: 3)～(20: 1).
6. according to the described organic acid method that reclaims from organic solvent of claim 1, it is characterized in that: organic acid concentration is between 0～15M in receiving mutually in the described step 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100377593A CN100427185C (en) | 2004-05-12 | 2004-05-12 | Method for recovering organic acid from organic solvent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100377593A CN100427185C (en) | 2004-05-12 | 2004-05-12 | Method for recovering organic acid from organic solvent |
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| Publication Number | Publication Date |
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| CN1569315A true CN1569315A (en) | 2005-01-26 |
| CN100427185C CN100427185C (en) | 2008-10-22 |
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| CNB2004100377593A Expired - Fee Related CN100427185C (en) | 2004-05-12 | 2004-05-12 | Method for recovering organic acid from organic solvent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102482693A (en) * | 2009-07-01 | 2012-05-30 | 诺维信北美公司 | Process for separating and recovering c4 dicarboxylic acids |
| CN109852987A (en) * | 2018-12-24 | 2019-06-07 | 万华化学集团股份有限公司 | A method of coupling reverse osmosis technology prepares sodiam glyoxlate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19545303C1 (en) * | 1995-12-05 | 1997-04-24 | Metallgesellschaft Ag | Process for the preparation of an organic acid |
| DE19849924A1 (en) * | 1998-10-29 | 2000-05-04 | Degussa | Electro-chemical process to remove organic acids from aqueous solution at reduced cost |
| CN1199976C (en) * | 2003-07-03 | 2005-05-04 | 华东理工大学 | Electrodialysis method for separating sugar and acid in biomass hydrolysate |
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2004
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102482693A (en) * | 2009-07-01 | 2012-05-30 | 诺维信北美公司 | Process for separating and recovering c4 dicarboxylic acids |
| CN109852987A (en) * | 2018-12-24 | 2019-06-07 | 万华化学集团股份有限公司 | A method of coupling reverse osmosis technology prepares sodiam glyoxlate |
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