CN104803870A - Method for extracting and recovering amide from aqueous solution - Google Patents
Method for extracting and recovering amide from aqueous solution Download PDFInfo
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- CN104803870A CN104803870A CN201510217136.2A CN201510217136A CN104803870A CN 104803870 A CN104803870 A CN 104803870A CN 201510217136 A CN201510217136 A CN 201510217136A CN 104803870 A CN104803870 A CN 104803870A
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- 150000001408 amides Chemical class 0.000 title claims abstract description 53
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 202
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 111
- 238000011084 recovery Methods 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 56
- 239000012071 phase Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 30
- 238000004064 recycling Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000007600 charging Methods 0.000 claims description 7
- 238000005191 phase separation Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000011027 product recovery Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 22
- 239000000126 substance Substances 0.000 description 14
- 238000005192 partition Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000000638 solvent extraction Methods 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 4
- 229960001701 chloroform Drugs 0.000 description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Pyrrole Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting and recovering amide from an aqueous solution. An amide aqueous solution is added into the bottom of an extraction tower at a normal temperature, a main extraction agent is added into the top of the extraction tower, a composite solvent consisting of a main extraction agent and an auxiliary extraction agent is added into a part at the height, 0.1-0.4 times away from the top of the tower, of the extraction tower, extraction and separation are finished through countercurrent contact of liquid-liquid phases, and a raffinate phase mainly containing water and an extraction phase containing amide are obtained from the top and bottom of the tower respectively. The extraction phase containing amide passes through a main extraction agent recovery tower, an auxiliary extraction agent recovery tower and a product recovery tower in sequence to obtain the main extraction agent, the auxiliary extraction agent and an amide product from the top of the tower respectively, and the main extraction agent and the auxiliary extraction agent are recirculated for extraction of the amide aqueous solution. The method increases the distribution coefficient of amide in the extraction agent under the action of the auxiliary extraction agent, and can remarkably reduce the consumption of the extraction agent, reduce the energy consumption of subsequent rectification separation, so as to achieve remarkable economic benefits.
Description
Technical field
The present invention relates to a kind of method adopting double solvents extraction and recovery acid amides from the aqueous solution, the fields such as a kind of chemical fibre, pharmacy that particularly relate to adopt amide substance to be obtain the continuous production method that the amides aqueous solution reclaims purification acid amides in solvent production process.
Background technology
Amide substance is the strong polar chemical material of a class generally used in Chemical Manufacture, and representative products has N,N-dimethylacetamide, DMF and N-Methyl pyrrolidone etc., is generally used as solvent in the field such as chemical fibre, pharmacy.Because such boiling point substance is general higher, and concentration is in aqueous not high, and conventional rectification separating and purifying method exists that energy consumption is higher, product purity is difficult to the unfavorable factors such as guarantee.The method substituted in current industry adopts extraction in conjunction with the separating technology of rectifying, the N-Methyl pyrrolidone in the recovery aramid fiber polymerization processes such as trichloromethane in mother liquor and N,N-dimethylacetamide is adopted as Chinese patent CN201010017119 and CN201410230676.Because the polarity of amide substance self is comparatively strong, comparatively large with the bonding force of water in aqueous, adopt the single extraction agent such as trichloromethane, methylene dichloride to need very high solvent load than obtaining desirable percentage extraction.
In addition, though trichloromethane is Conventional solvents, due to its temperature instability, easily decompose larger to equipment corrosion in follow-up rectifying separation process.Although methylene dichloride is comparatively stable also can be used as extraction agent, amide substance partition ratio is wherein general lower, and its solvent load is larger compared with trichloromethane, greatly can increase the cost of follow-up rectifying separation.
The present invention is high with existing solvent load existing in the industrial production, later separation energy consumption also high realistic problem for foundation, with improve extraction partition ratio, minimizing solvent load is for starting point, the complex solvent extraction proposing a kind of amide substance reclaims novel method, can be association area improvement of production process, reduces energy consumption and increase economic benefit.
Summary of the invention
The object of the invention is to the deficiency for existing production technology, provide a kind of method adopting double solvents extraction and recovery acid amides from the aqueous solution, the method can significantly improve the partition ratio of amide substance in solvent extraction, realizes higher extraction efficiency.
In solvent extraction process, the foundation of selective solvent measures its partition ratio, the partition ratio of solvent refers to and is extracted the composition of material in extraction phase and the ratio formed in extracting phase, its numerical value is larger, and illustrate that extract more easily enters extraction phase, solvent load is less.Because amide substance polarity is general comparatively large, also comparatively large with water binding, Conventional solvents is difficult to from water, acid amides be competed in the past, and especially for the aqueous solution that amide content is lower, the partition ratio of large multi-solvent is all very little.
The interaction of extraction agent and acid amides greatly can be strengthened by selecting the suitable extraction agent that helps, and then significantly improve the partition ratio of extraction, but help the bonding force of extraction agent often and between water molecules also stronger, certain meltage is had in water, it is unfavorable to bring to the precipitation of follow-up extracting phase, therefore needs to help the feed postition of extraction agent to make extraction process more rationally reliable by improving.In process program provided by the invention, can effectively suppress to help extraction agent to the problems of dissolution in water by the method adding extraction agent with two positions.
The object of the invention is to be achieved through the following technical solutions: the method for a kind of double solvents extraction and recovery acid amides from the aqueous solution, comprises the following steps:
Flow to be the mass concentration of 100 mass parts be 8 ~ 30% amide aqueous solution add at the bottom of the tower of extraction tower at normal temperatures, the main extraction agent carrying out 100 ~ 150 mass parts of autonomous extraction agent basin adds from the tower top of extraction tower at normal temperatures through main extractant feed pump, double solvents from 80 ~ 150 mass parts of double solvents basin adds from the extraction tower tower height apart from tower top 0.1 ~ 0.4 times at normal temperatures, and described double solvents is by main extraction agent and help extraction agent to form by the quality proportioning mixing of 80-60:20-40; The main component obtained from tower top after completing extracting and separating by the counter current contact of liquid-liquid diphase is that the extracting phase of water sends into extracting phase basin, and the extraction phase of the amide containing obtained at the bottom of tower sends into extraction phase basin; Described acid amides is N-Methyl pyrrolidone, N,N-dimethylacetamide or DMF; Described main extraction agent is methylene dichloride, helps extraction agent to be propyl alcohol or butanols;
Extraction phase in extraction phase basin sends into main extraction agent recovery tower through fresh feed pump, the mixing steam that main extraction agent recovery tower tower top obtains main extraction agent and water enters phase separation tank after overhead condenser condensation, phase separation tank upper part goes out aqueous phase, the top of extraction agent recovery tower is become owner of in the oil phase part backflow that bottom separates, another part sends into main extraction agent basin, circulates as the charging of extraction tower tower top; Main extraction agent recovery tower materials at bottom of tower is sent into through fresh feed pump and is helped extraction agent recovery tower, obtaining main component from helping extraction agent recovery tower tower top is help the steam of extraction agent to pass back into through overhead condenser condensation rear portion the top helping extraction agent recovery tower, another part is sent into and is helped extraction agent basin, sends into double solvents basin circulate as the double solvents charging of extraction tower with main extraction agent after allocating; The material at the bottom of extraction agent recovery tower tower is helped to send into Product recycling tower through fresh feed pump, amide products steam to pass back into Product recycling tower top through overhead condenser condensation rear portion is obtained from Product recycling column overhead, another part extraction as product, Product recycling tower materials at bottom of tower by height boil impurities outlet discharge high boiling material.
Described extraction tower is sieve-tray tower, packing tower, pulsed sieve plate column or pulsed packed tower, tower top atmospheric operation.Described main extraction agent recovery tower is plate distillation column or stuffing rectification column, tower top normal pressure or pressurized operation.The described extraction agent recovery tower that helps is stuffing rectification column, tower top normal pressure or decompression operation.Described Product recycling tower is stuffing rectification column, and reduced top column pressure operates.
Beneficial effect of the present invention is:
(1) the present invention helps extraction agent by interpolation, and can improve amide substance partition ratio in a solvent, partition ratio can reach 0.5 ~ 1.0, is significantly better than current traditional single solvent extraction processing method.
(2) the present invention is by dividing two bursts of chargings by main extraction agent, effectively can suppress the meltage helping extraction agent in water, is conducive to follow-up main extraction agent and the purification helping extraction agent.
(3) the present invention is owing to improve amide substance partition ratio in a solvent, can reduce the consumption of extraction agent, will significantly reduce the energy consumption of solvent loss and later separation purification.
(4) the present invention according to need of production, can regulate the relative usage of main extraction agent and double solvents easily, is also easy to realize the transformation to existing production equipment and expansion energy.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of acid amides extraction and recovery;
In figure, extraction tower 1, main extraction agent recovery tower 2, help extraction agent recovery tower 3, Product recycling tower 4, main extraction agent basin 5, help extraction agent basin 6, double solvents basin 7, extracting phase basin 8, extraction phase basin 9, phase separation tank 10, main extraction agent recovery tower condenser 11, main extraction agent recovery tower reboiler 12, help extraction agent recovery tower condenser 13, help extraction agent recovery tower reboiler 14, Product recycling tower condenser 15, Product recycling tower reboiler 16, main extractant feed pump 17, double solvents fresh feed pump 18, main extraction agent recovery tower fresh feed pump 19, help extraction agent recovery tower fresh feed pump 20, Product recycling tower fresh feed pump 21, amide aqueous solution opening for feed 22, main extractant feed mouth 23, double solvents opening for feed 24, aqueous phase outlet 25, oil phase outlet 26, products export 27, height boils impurities outlet 28.
Embodiment
The method of a kind of double solvents extraction and recovery acid amides from the aqueous solution that the present invention proposes, comprises the following steps:
Flow to be the mass concentration of 100 mass parts be 8 ~ 30% amide aqueous solution add from amide aqueous solution opening for feed 22 at the bottom of the tower of extraction tower 1 at normal temperatures, the main extraction agent carrying out 100 ~ 150 mass parts of autonomous extraction agent basin 5 adds from the main extractant feed mouth 23 of the tower top of extraction tower at normal temperatures through main extractant feed pump 17, double solvents from 80 ~ 150 mass parts of double solvents basin 7 adds from the extraction tower tower height double solvents opening for feed 24 apart from tower top 0.1 ~ 0.4 times at normal temperatures, described double solvents is by main extraction agent and help extraction agent to form by the quality proportioning mixing of 80-60:20-40, obtain from tower top the extracting phase feeding extracting phase basin 8 that main component is water after completing extracting and separating by the counter current contact of liquid-liquid diphase, the extraction phase of amide containing obtains at the bottom of tower sends into extraction phase basin 9, described acid amides is N-Methyl pyrrolidone, N,N-dimethylacetamide or DMF, described main extraction agent is methylene dichloride, helps extraction agent to be propyl alcohol or butanols,
Extraction phase in extraction phase basin 9 sends into main extraction agent recovery tower 2 through main extraction agent recovery tower fresh feed pump 19, the mixing steam that main extraction agent recovery tower 2 tower top obtains main extraction agent and water enters phase separation tank 10 after the condensation of main extraction agent recovery tower condenser 11, phase separation tank 10 upper part goes out aqueous phase and discharges from aqueous phase outlet 25, the oil phase that bottom separates is discharged from oil phase outlet 26, the top of extraction agent recovery tower 2 is become owner of in part backflow, another part sends into main extraction agent basin 5, circulates as the charging of extraction tower 1 tower top; Main extraction agent recovery tower 2 materials at bottom of tower helps extraction agent recovery tower 3 by helping extraction agent recovery tower fresh feed pump 20 to send into again after main extraction agent recovery tower reboiler 12 components vaporize, obtaining main component from helping extraction agent recovery tower 3 tower top is help extraction agent steam to pass back into through helping extraction agent recovery tower condenser 13 condensation rear portion the top helping extraction agent recovery tower 3, another part is sent into and is helped extraction agent basin 6, sends into double solvents basin 7 circulate as the double solvents charging of extraction tower 1 with main extraction agent after allocating; The material at the bottom of extraction agent recovery tower 3 tower is helped to send into Product recycling tower 4 by Product recycling tower fresh feed pump 21 again after helping extraction agent recovery tower reboiler 14 components vaporize, the higher amide products steam of purity to pass back into Product recycling tower 4 top through product recovery tower condenser 15 condensation rear portion is obtained from Product recycling tower 4 tower top, another part is through products export 27 extraction as product, and Product recycling tower 4 materials at bottom of tower discharges high boiling material by the height impurities outlet 28 that boils again after product recovery tower reboiler 16 components vaporize.
Described extraction tower 1 is sieve-tray tower, packing tower, pulsed sieve plate column or pulsed packed tower, tower top atmospheric operation; Described main extraction agent recovery tower 2 is plate distillation column or stuffing rectification column, tower top normal pressure or pressurized operation; The described extraction agent recovery tower 3 that helps is stuffing rectification column, tower top normal pressure or decompression operation; Described Product recycling tower 4 is stuffing rectification column, and reduced top column pressure operates.
According to described processing method, the partition ratio adopting complex solvent extraction of the present invention to reclaim acid amides can reach 0.5 ~ 1.0, is significantly better than current traditional single solvent extraction processing method.
Below by specific embodiment, the invention will be further described, but the present invention should be interpreted as and be only applicable to following case.
Embodiment 1
As shown in Figure 1, extraction tower 1 number of theoretical plate is 8, flow be 1000kg/h containing N, N-N,N-DIMETHYLACETAMIDE 8% (wt%) aqueous solution sends into the bottom amide aqueous solution opening for feed 22 of extraction tower 1 at 30 DEG C, main extraction agent methylene dichloride take flow as the main extractant feed mouth 23 in top that 1200kg/h sends into extraction tower 1 at 30 DEG C, and the double solvents of methylene dichloride and Virahol composition take flow as the double solvents opening for feed 24 that 1200kg/h (containing Virahol 30%) sends into the 3rd piece of theoretical stage place from the top down of extraction tower 1 at 30 DEG C.
After extraction tower 1 fully liquid liquid mass exchange, obtaining tower top extracting phase load is 856.4kg/h, and wherein residual N,N-dimethylacetamide content is 0.25%; Extraction phase load at the bottom of tower is 2543.6kg/h, and wherein N,N-dimethylacetamide content is 3.06%.Described per-cent is mass percent.
Embodiment 2
As shown in Figure 1, extraction tower 1 number of theoretical plate is 8, flow be 1000kg/h containing N, N-N,N-DIMETHYLACETAMIDE 25% (wt%) aqueous solution sends into the bottom amide aqueous solution opening for feed 22 of extraction tower 1 at 30 DEG C, main extraction agent methylene dichloride take flow as the main extractant feed mouth 23 in top that 1000kg/h sends into extraction tower 1 at 30 DEG C, and the double solvents of methylene dichloride and Virahol composition take flow as the double solvents opening for feed 24 that 1500kg/h (containing Virahol 20%) sends into the 3rd piece of theoretical stage place from the top down of extraction tower 1 at 30 DEG C.
After extraction tower 1 fully liquid liquid mass exchange, obtaining tower top extracting phase load is 588.1kg/h, and wherein residual N,N-dimethylacetamide content is 0.50%; Extraction phase load at the bottom of tower is 2344.5kg/h, and wherein N,N-dimethylacetamide content is 8.49%.Described per-cent is mass percent.
Embodiment 3
As shown in Figure 1, extraction tower 1 number of theoretical plate is 8, flow is the bottom amide aqueous solution opening for feed 22 sending into extraction tower 1 containing N-Methyl pyrrolidone 20% (wt%) aqueous solution at 30 DEG C of 1000kg/h, main extraction agent methylene dichloride take flow as the main extractant feed mouth 23 in top that 1500kg/h sends into extraction tower 1 at 30 DEG C, and the double solvents of methylene dichloride and isopropylcarbinol composition take flow as the double solvents opening for feed 24 that 1200kg/h (containing isopropylcarbinol 40%) sends into the 3rd piece of theoretical stage place from the top down of extraction tower 1 at 30 DEG C.
After extraction tower 1 fully liquid liquid mass exchange, obtaining tower top extracting phase load is 754.3kg/h, and wherein residual N-Methyl pyrrolidone content is 0.14%; Extraction phase load at the bottom of tower is 2945.7kg/h, and wherein N-Methyl pyrrolidone content is 6.75%.Described per-cent is mass percent.
Embodiment 4
As shown in Figure 1, extraction tower 1 number of theoretical plate is 8, flow is the bottom amide aqueous solution opening for feed 22 sending into extraction tower 1 containing N-Methyl pyrrolidone 10% (wt%) aqueous solution at 30 DEG C of 1000kg/h, main extraction agent methylene dichloride take flow as the main extractant feed mouth 23 in top that 1500kg/h sends into extraction tower 1 at 30 DEG C, and the double solvents of methylene dichloride and isopropylcarbinol composition take flow as the double solvents opening for feed 24 that 800kg/h (containing isopropylcarbinol 40%) sends into the 3rd piece of theoretical stage place from the top down of extraction tower 1 at 30 DEG C.
After extraction tower 1 fully liquid liquid mass exchange, obtaining tower top extracting phase load is 889.3kg/h, and wherein residual N-Methyl pyrrolidone content is 0.51%; Extraction phase load at the bottom of tower is 2410.7kg/h, and wherein N-Methyl pyrrolidone content is 3.96%.Described per-cent is mass percent.
Embodiment 5
As shown in Figure 1, extraction tower 1 number of theoretical plate is 8, flow be 1000kg/h containing N, dinethylformamide 30% (wt%) aqueous solution sends into the bottom amide aqueous solution opening for feed 22 of extraction tower 1 at 30 DEG C, main extraction agent methylene dichloride take flow as the main extractant feed mouth 23 in top that 1000kg/h sends into extraction tower 1 at 30 DEG C, and the double solvents of methylene dichloride and sec-butyl alcohol composition take flow as the double solvents opening for feed 24 that 1000kg/h (containing sec-butyl alcohol 20%) sends into the 3rd piece of theoretical stage place from the top down of extraction tower 1 at 30 DEG C.
After extraction tower 1 fully liquid liquid mass exchange, obtaining tower top extracting phase load is 587.3kg/h, and wherein residual DMF content is 0.35%; Extraction phase load at the bottom of tower is 2412.7kg/h, and wherein N,N-dimethylacetamide content is 12.35%.Described per-cent is mass percent.
Claims (5)
1. a method for double solvents extraction and recovery acid amides from the aqueous solution, is characterized in that, comprise the following steps:
Flow to be the mass concentration of 100 mass parts be 8 ~ 30% amide aqueous solution add at the bottom of the tower of extraction tower at normal temperatures, the main extraction agent carrying out 100 ~ 150 mass parts of autonomous extraction agent basin adds from the tower top of extraction tower at normal temperatures through main extractant feed pump, double solvents from 80 ~ 150 mass parts of double solvents basin adds from the extraction tower tower height apart from tower top 0.1 ~ 0.4 times at normal temperatures, and described double solvents is by main extraction agent and help extraction agent to form by the quality proportioning mixing of 80-60:20-40; The main component obtained from tower top after completing extracting and separating by the counter current contact of liquid-liquid diphase is that the extracting phase of water sends into extracting phase basin, and the extraction phase of the amide containing obtained at the bottom of tower sends into extraction phase basin; Described acid amides is N-Methyl pyrrolidone, N,N-dimethylacetamide or DMF; Described main extraction agent is methylene dichloride, helps extraction agent to be propyl alcohol or butanols;
Extraction phase in extraction phase basin sends into main extraction agent recovery tower through fresh feed pump, the mixing steam that main extraction agent recovery tower tower top obtains main extraction agent and water enters phase separation tank after overhead condenser condensation, phase separation tank upper part goes out aqueous phase, the top of extraction agent recovery tower is become owner of in the oil phase part backflow that bottom separates, another part sends into main extraction agent basin, circulates as the charging of extraction tower tower top; Main extraction agent recovery tower materials at bottom of tower is sent into through fresh feed pump and is helped extraction agent recovery tower, obtaining main component from helping extraction agent recovery tower tower top is help the steam of extraction agent to pass back into through overhead condenser condensation rear portion the top helping extraction agent recovery tower, another part is sent into and is helped extraction agent basin, sends into double solvents basin circulate as the double solvents charging of extraction tower with main extraction agent after allocating; The material at the bottom of extraction agent recovery tower tower is helped to send into Product recycling tower through fresh feed pump, amide products steam to pass back into Product recycling tower top through overhead condenser condensation rear portion is obtained from Product recycling column overhead, another part extraction as product, Product recycling tower materials at bottom of tower by height boil impurities outlet discharge high boiling material.
2. the method for double solvents extraction and recovery acid amides from the aqueous solution according to claim 1, it is characterized in that, described extraction tower is sieve-tray tower, packing tower, pulsed sieve plate column or pulsed packed tower, tower top atmospheric operation.
3. the method for double solvents extraction and recovery acid amides from the aqueous solution according to claim 1, it is characterized in that, described main extraction agent recovery tower is plate distillation column or stuffing rectification column, tower top normal pressure or pressurized operation.
4. the method for double solvents extraction and recovery acid amides from the aqueous solution according to claim 1, is characterized in that, described in help extraction agent recovery tower to be stuffing rectification column, tower top normal pressure or decompression operation.
5. the method for double solvents extraction and recovery acid amides from the aqueous solution according to claim 1, it is characterized in that, described Product recycling tower is stuffing rectification column, and reduced top column pressure operates.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646271A (en) * | 2015-12-08 | 2016-06-08 | 长春工业大学 | Method for recovering N,N-dimethyl acetamide from waste liquid generated in cefuroxime acid production through extraction |
| CN106565524A (en) * | 2016-09-22 | 2017-04-19 | 南通万顺化工科技有限公司 | A method of recovering dimethyl formamide |
| CN110357802A (en) * | 2018-03-26 | 2019-10-22 | 中国石油化工股份有限公司 | Solvent recovery process in a kind of cleaning solution waste liquid producing p-aramid fiber |
| CN111517532A (en) * | 2020-06-05 | 2020-08-11 | 宁夏泰益欣生物科技有限公司 | Sec-octanol wastewater treatment method and system |
| CN112574060A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
-
2015
- 2015-04-29 CN CN201510217136.2A patent/CN104803870B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646271A (en) * | 2015-12-08 | 2016-06-08 | 长春工业大学 | Method for recovering N,N-dimethyl acetamide from waste liquid generated in cefuroxime acid production through extraction |
| CN106565524A (en) * | 2016-09-22 | 2017-04-19 | 南通万顺化工科技有限公司 | A method of recovering dimethyl formamide |
| CN110357802A (en) * | 2018-03-26 | 2019-10-22 | 中国石油化工股份有限公司 | Solvent recovery process in a kind of cleaning solution waste liquid producing p-aramid fiber |
| CN110357802B (en) * | 2018-03-26 | 2023-02-03 | 中国石油化工股份有限公司 | Process for recovering solvent from washing liquid waste liquid in production of para-aramid |
| CN112574060A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Method for recovering N, N-dimethylacetamide |
| CN112574060B (en) * | 2019-09-29 | 2022-10-11 | 中国石油化工股份有限公司 | Recovery method of N, N-dimethylacetamide |
| CN111517532A (en) * | 2020-06-05 | 2020-08-11 | 宁夏泰益欣生物科技有限公司 | Sec-octanol wastewater treatment method and system |
| CN111517532B (en) * | 2020-06-05 | 2022-08-16 | 宁夏泰益欣生物科技有限公司 | Sec-octanol wastewater treatment method and system |
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| CN104803870B (en) | 2016-08-24 |
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