Production method of 1-acetyl-2-pyrrolidone

A technology for pyrrolidone and its production method, which is applied in the production field of 1-acetyl-2-pyrrolidone, can solve the problems of cumbersome operation process, decreased safety factor, high equipment requirements, etc., and achieve prolongation of reaction time, short reaction time and high activity Effect

Inactive Publication Date: 2019-12-20
MAIQI CHEM CO LTD
View PDF11 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the characteristics of short reaction time and high yield, but reducing the material at 240°C to 0-5°C in a short period of time requires high equipment requirements. At the same time, micro-reaction, as an emerging technology, has relatively high investment costs , the effect is not stable, also can find that its yield is the highest more than 90% from its embodiment, minimum only has 43.7%
[0005] The Chinese patent with the notification number CN105237456B discloses a production method of pyrrolidone products. It introduces the direct production of pyrrolidone by using 1,4-butanediol as a raw material through one-step reaction. , 4-butanediol is converted into pyrrolidone series products in one reaction unit through dehydrogenation-amination reaction. This method is completed in two reactors in one reaction unit. The first stage of reaction is 1,4 - Dehydrogenation of butanediol is mainly used to produce γ-butyrolactone, and the second-stage reaction is mainly based on the amination of γ-butyrolactone to synthesize pyrrolidones. The reaction temperature of the first-stage reactor is 190-260°C and the reaction pressure is 0.5- 8.0MPa, the reaction temperature of the second-stage reactor is 230-290°C, and the reaction pressure is 5-15.0MPa. Therefore, this patent is equipped with a buffer tank, a booster pump, Filters and heaters have complex structures and cumbersome operations, reducing the safety factor of workers during operations

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Production method of 1-acetyl-2-pyrrolidone
  • Production method of 1-acetyl-2-pyrrolidone
  • Production method of 1-acetyl-2-pyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A production method of 1-acetyl-2-pyrrolidone, comprising the following steps:

[0034] (1) Dissolve copper nitrate, bismuth nitrate and silver nitrate in deionized water to form a 1.5mol / L solution A, then add polyethylene glycol with a polymerization degree of 2000, stir, and transfer to a microwave hydrothermal parallel synthesizer Under the condition of 80 ℃, react for 6h to obtain the mixed solution B containing Cu / Bi / Ag; 2 o 3 and TiO 2 Use ultrasonic waves to disperse in deionized water to form solution C; use ultrasonic waves to disperse the nano-scale carrier in deionized water to form solution D; mix solutions B, C, and D in parallel, stir for 24 hours, and add a precipitant dropwise to control The pH at the end point is 6.8, let stand, filter, wash, and vacuum-dry the filter cake, then roast at 500°C for 10 hours to obtain the catalyst;

[0035] (2) Pre-pack the catalyst obtained in step (1) in a tubular fixed-bed reactor, use nitrogen to replace the react...

Embodiment 2

[0046] A production method of 1-acetyl-2-pyrrolidone, comprising the following steps:

[0047] (1) Dissolve copper nitrate, bismuth nitrate and silver nitrate in deionized water to prepare 1mol / L solution A, then add polyethylene glycol with a degree of polymerization of 8000, stir, and move to a microwave hydrothermal parallel synthesizer Under the condition of 90°C, react for 5h to obtain a mixed solution B containing Cu / Bi / Ag; 2 o 3 and TiO 2 Use ultrasonic waves to disperse in deionized water to form solution C; use ultrasonic waves to disperse the nano-scale carrier in deionized water to form solution D; mix solutions B, C, and D in parallel, stir for 20 hours, and add a precipitant dropwise to control The end point pH is 6.7, let stand, filter, wash, vacuum-dry the filter cake and roast at 550°C for 8 hours to obtain the catalyst;

[0048] (2) Pre-pack the catalyst obtained in step (1) in a tubular fixed-bed reactor, use nitrogen to replace the reactor, and hydrogen t...

Embodiment 3

[0059] A production method of 1-acetyl-2-pyrrolidone, comprising the following steps:

[0060] (1) Dissolve copper nitrate, bismuth nitrate and silver nitrate in deionized water to make solution A of 1.5mol / L, then add polyethylene glycol with a polymerization degree of 6000, stir, and transfer to microwave hydrothermal parallel synthesizer Under the condition of 80 ℃, react for 8h to obtain the mixed solution B containing Cu / Bi / Ag; 2 o 3 and TiO 2 Use ultrasonic waves to disperse in deionized water to form solution C; use ultrasonic waves to disperse the nano-scale carrier in deionized water to form solution D; mix solutions B, C, and D in parallel, stir for 24 hours, and add a precipitant dropwise to control The pH at the end point is 7.0, let stand, filter, wash, vacuum-dry the filter cake and then roast at 550°C for 10 hours to obtain the catalyst;

[0061] (2) Pre-pack the catalyst obtained in step (1) in a tubular fixed-bed reactor, use nitrogen to replace the reactor...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
densityaaaaaaaaaa
boiling pointaaaaaaaaaa
water contentaaaaaaaaaa
Login to view more

Abstract

The invention discloses a production method of 1-acetyl-2-pyrrolidone. The method includes the steps of: taking 1, 3-propylene glycol, ammonia water, methyl acetate and methyl formate as the raw materials, carrying out amination, addition and cyclization reactions in a tubular fixed bed reactor under the action of a copper-based catalyst to obtain a 1-acetyl-2-pyrrolidone crude product, and further performing purification to obtain the 1-acetyl-2-pyrrolidone. The method provided by the invention has the characteristics of high catalyst catalytic activity, mild reaction conditions and simple technological operation, and the obtained product has yield of greater than or equal to 98.4%, selectivity of greater than or equal to 99.0%, purity of higher than or equal to 99.9%, a water content ofsmaller than or equal to 40ppm, and an ammonia content of less than or equal to 2ppm, thus meeting the requirements of downstream medicine, fine chemical intermediates and other fields.

Description

technical field [0001] The invention belongs to the field of production of fine chemical products, and in particular relates to a production method of 1-acetyl-2-pyrrolidone. Background technique [0002] 1-acetyl-2-pyrrolidone, molecular weight 127.4, density 1.15g / cm 3 , with a boiling point of 231°C, has a special smell, and has high biological activity. It can be used to synthesize acetylpyrrolidine, acetylpyrrole, etc. It is an important starting material in organic synthesis, so it is widely used in pharmaceutical chemical industry, fine chemical industry, Pesticide chemical, fragrance and cosmetic additive field. [0003] In the prior art, the catalysts used to synthesize pyrrolidone by amination of γ-butyrolactone are generally solid superacids, heteropolyacids or modified molecular sieves, such as: Zhang Zhide, etc. (refer to literature: Zhang Zhide, Lin Fengzhen, etc., 1-cyclohexyl- Synthesis of 2-pyrrolidone [J], Fine Chemical Industry, 2005, Volume 22, Issue 9)...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/27B01J29/46B01J35/10B01J37/18B01J37/03
CPCB01J29/46B01J35/1004B01J37/031B01J37/18B01J2229/18C07D207/27
Inventor 吴彦彬闫广学宋国全吴正岭肖强杨理梁斌周淑飞李清霞
Owner MAIQI CHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products