CN1096447C - Production method of N-ethyl-alpha-pyrrolidone - Google Patents
Production method of N-ethyl-alpha-pyrrolidone Download PDFInfo
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- CN1096447C CN1096447C CN99114241A CN99114241A CN1096447C CN 1096447 C CN1096447 C CN 1096447C CN 99114241 A CN99114241 A CN 99114241A CN 99114241 A CN99114241 A CN 99114241A CN 1096447 C CN1096447 C CN 1096447C
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- pyrrolidone
- ethyl
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Abstract
The present invention relates to a production method of N-ethyl-a-pyrrolidone, which comprises condensation reaction and purification. The present invention is characterized in that an auxiliary organic acid condensation agent is added into ethylamine solution, and the adding quantity of the auxiliary organic acid condensation agent is from 0.3% to 1% of the volume of the ethylamine solution, r-butyrolactone and the mixture are continuously pumped into a tubular reactor by a high pressure measuring pump according to the mole proportioning of 1: 1.0 to 1.6 to react. The reactor is controlled by a control system under the protection of nitrogen, the crude product is cooled and depressurized, and an auxiliary strong alkali and weak acid salt agent is added according to the proportion of 0.3 to 1% of the crude product to purify. The N-ethyl-a-pyrrolidone produced by the present invention has the advantages of high quality and stable quality.
Description
The present invention relates to a kind of production technique of heterogeneous ring compound, exactly is the production method of a kind of N-ethyl-a-pyrrolidone.
Chinese patent CN1199730A disclosed " production technique of 1-ethyl-2-aminomethyl Pyrrolidine and intermediate product N-ethyl-a-pyrrolidone ", the N-ethyl-a-pyrrolidone that utilizes this production technique to obtain, its quality product is lower, and stable inadequately.
The object of the present invention is to provide a kind of quality product height and production method stay-in-grade, that be fit to the N-ethyl-a-pyrrolidone of scale production.
Technical solution of the present invention is: the production method of a kind of N-ethyl-a-pyrrolidone is characterized in that: with the low-carbon (LC) alkanoic acid by the 0.3-1% of-ethylamine solution join concentration be 50-70%-ethylamine solution in; R-butyrolactone with 〉=99.0% and said mixture are by 1: the mole proportioning of 1.0-1.6 is squeezed into the duct type high-pressure reactor continuously with high-pressure metering pump and is reacted; The reaction pressure of this reactor is controlled under nitrogen protection by a Controlling System; Reacted crude product is through the cooling release, and the crude product groove of moving into is pressed the 0.3-1% interpolation strong base weak acid salt assitant of crude product amount.
Production method of the present invention makes and has added the strong base weak acid salt assitant when refining by r-butyrolactone sufficient reacting owing to added the low-carbon (LC) alkanoic acid in starting material, makes the products production steady quality, the quality height, and adopt pipeline reactor, practicable scale production.This production method technology advanced person, reasonable, easy to operate, cost is low.N-ethyl-a-pyrrolidone that production method provided by the invention is produced, has high-solvency, characteristics such as low vapor pressure and specific inductivity are low, industrial solvent and the refined oil that can be used as macromolecular material also can be used as the solvent and the extraction agent of engineering plastics, coating resin.
The invention will be further described below in conjunction with embodiment.
Concentration be 70%-add 0.3% left and right sides low-carbon (LC) alkanoic acid in the ethylamine solution; then with its mixture and 〉=the 99.0%r-butyrolactone is respectively with 40L/hr; 36L/hr squeezes into the duct type high-pressure reactor with high-pressure metering pump; this reactor reaction pressure is controlled under nitrogen protection by a Controlling System, and control pressure is 7.8MPa, and temperature is controlled by a Controlling System; about 275 degree; carry out successive reaction, reacted material is delivered to the crude product groove continuously through the release that cools.With thick NEP product in the crude product groove, throw the yellow soda ash of crude product amount 0.5%, and take off-ethamine and water after it is pumped into distillation system, rectification under vacuum obtains NEP again, and this product structural formula is:
Product purity 〉=99.0%, r-butyrolactone≤0.1%, acidity≤0.1% refractive index 1.4664, density d
n 200.994.
Claims (2)
1, the production method of a kind of N-ethyl-a-pyrrolidone, comprise condensation reaction and refining, it is characterized in that: the 0.3-1% by-ethylamine solution joins in the monoethylamine solution that concentration is 50-70% with the low-carbon (LC) alkanoic acid, and r-butyrolactone with 〉=90.0% and said mixture are by 1: the mole proportioning of 1.0-1.6 is squeezed into the duct type high-pressure reactor continuously with high-pressure metering pump and reacted; The reaction pressure of this reactor is controlled under nitrogen protection by a Controlling System; Reacted crude product is through the cooling release, and the crude product groove of moving into is pressed the 0.3-1% interpolation strong base weak acid salt assitant of crude product amount.
2, the production method of a kind of N-ethyl according to claim 1-a-pyrrolidone, it is characterized in that: described strong base weak acid salt assitant is a yellow soda ash.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114241A CN1096447C (en) | 1999-05-27 | 1999-05-27 | Production method of N-ethyl-alpha-pyrrolidone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99114241A CN1096447C (en) | 1999-05-27 | 1999-05-27 | Production method of N-ethyl-alpha-pyrrolidone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1237578A CN1237578A (en) | 1999-12-08 |
| CN1096447C true CN1096447C (en) | 2002-12-18 |
Family
ID=5277347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99114241A Expired - Fee Related CN1096447C (en) | 1999-05-27 | 1999-05-27 | Production method of N-ethyl-alpha-pyrrolidone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1096447C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATE451354T1 (en) | 2006-05-16 | 2009-12-15 | Basf Se | METHOD FOR CONTINUOUS PRODUCTION OF N-ETHYL-2-PYRROLIDONE (NEP) |
| CN102001986A (en) * | 2010-12-23 | 2011-04-06 | 上海化学试剂研究所 | Method for improving quality of industrial N-methylpyrrolidone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4814464A (en) * | 1987-03-30 | 1989-03-21 | Amoco Corporation | Process for making N-alkylpyrrolidones |
| CN1199730A (en) * | 1998-04-22 | 1998-11-25 | 邱国祥 | Production technology of 1-ethyl-2-aminomethyl tetrahydropyrrole and its intermediate product N-ethyl-a-pyrrolidone |
-
1999
- 1999-05-27 CN CN99114241A patent/CN1096447C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4814464A (en) * | 1987-03-30 | 1989-03-21 | Amoco Corporation | Process for making N-alkylpyrrolidones |
| CN1199730A (en) * | 1998-04-22 | 1998-11-25 | 邱国祥 | Production technology of 1-ethyl-2-aminomethyl tetrahydropyrrole and its intermediate product N-ethyl-a-pyrrolidone |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1237578A (en) | 1999-12-08 |
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Effective date of registration: 20081205 Address after: No. 1084 South Jinzhai Road, Anhui, Hefei Patentee after: Anhui Harvest Fine Chemical Industry Co., Ltd. Address before: No. 1084 South Jinzhai Road, Anhui, Hefei Patentee before: Hefei Jianghuai Chemical Fertilizer General plant |
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Address after: No. 12 Qi Road, Hefei, Anhui Patentee after: CNSG Anhui Hong Sifang Co., Ltd. Address before: No. 1084 South Jinzhai Road, Anhui, Hefei Patentee before: Anhui Harvest Fine Chemical Industry Co., Ltd. |
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