Preparation method of high-purity diacetone acrylamide

An acetone acrylamide, high-purity technology, applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of limited purity of diacetone acrylamide, no industrial value, and inability to reach electronic grades. , to achieve the effect of easy separation and purification, simple fractionation and purification, and low solubility

Active Publication Date: 2019-02-01
JINGCHU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Above 4 routes each have advantages and disadvantages, with acetone as raw material and acrylonitrile one-step synthesis method has simple technology, industrialization is easy to realize, less investment, the advantages of higher yield, the disadvantage is poor product quality (purity<99.0%)
Using acetone dimerization to form diacetone alcohol, and then reacting with acrylonitrile to synthesize diacetone acrylamide after purification is the main process put into production at present. It has the advantages of high yield, low cost and good quality, and it is undoubtedly the best route. Acetone acrylamide has limited purity and is not electronic grade
The other two routes have no industrial value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of high-purity diacetone acrylamide, its steps are:

[0026] 1. Add 255g of 96wt% concentrated sulfuric acid to 1000ml of four-port reaction, stir and cool down to -10°C, then add 55.6g of acrylonitrile dropwise, react at 0°C for 15min after dropping, then add 116g of diacetone dropwise Alcohol, after dropping, control the temperature of the system at 12°C and react for 3h, then raise the temperature to 40°C, continue to react for 5 hours, take a sample and detect it with gas chromatography, (chromatographic conditions: strong polar column, column temperature 100°C, heat preservation for 3 hours Minutes, 20°C / min, rise to 230°C, keep warm for 10 minutes, sample injection temperature 230°C, detector temperature 230°C), acrylonitrile content<1wt%, acrylamide content 2-3wt% is the reaction end point, and mixed solution, add 490ml of 17wt% ammonia water dropwise to the resulting mixed solution to neutralize to a pH value of 7.5, keep the tempera...

Embodiment 2

[0031] A kind of preparation method of high-purity diacetone acrylamide, its steps are:

[0032] 1. Add 255g of 96wt% concentrated sulfuric acid to 1000ml of four-port reaction, stir and cool down to -5°C, then add 55.6g of acrylonitrile dropwise, react at 5°C for 30min after dropping, then add 116g of diacetone dropwise Alcohol, after dropping, control the temperature of the system at 10°C and react for 4h, then raise the temperature to 45°C, continue to react for 4 hours, take a sample and detect it with gas chromatography, (chromatographic conditions: strong polar column, column temperature 100°C, heat preservation 3 Minutes, 20°C / min, rise to 230°C, keep warm for 10 minutes, sample injection temperature 230°C, detector temperature 230°C), acrylonitrile content<1wt%, acrylamide content 2-3wt% is the reaction end point, and mixed solution, add dropwise 490ml of 17wt% ammonia water to the resulting mixed solution to neutralize to a pH value of 8, keep the temperature of the s...

Embodiment 3

[0037] A kind of preparation method of high-purity diacetone acrylamide, its steps are:

[0038] 1. Add 255g of 96wt% concentrated sulfuric acid to 1000ml of four-port reaction variety, stir and cool down to -5°C, then add 55.6g of acrylonitrile dropwise, react at -5°C for 30min after dropping, then add dropwise 116g of bis Acetol, after dropping, control the temperature of the system at 10°C and react for 3h, then heat up to 45°C, continue to react for 4 hours, and take a sample to detect with gas chromatography, (chromatographic conditions: strong polar column, column temperature 100°C, heat preservation 3 minutes, 20°C / min, rise to 230°C, keep warm for 10 minutes, sample injection temperature 230°C, detector temperature 230°C), acrylonitrile content<1wt%, acrylamide content 2-3wt% is the reaction end point, obtained Mixed solution, add 490ml of 17wt% ammonia water dropwise to the obtained mixed solution to neutralize to a pH value of 8, keep the temperature of the system lo...

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Abstract

The invention discloses a preparation method of high-purity diacetone acrylamide. The preparation method comprises the following steps: 1, carrying out a one-step synthesis reaction on acrylonitrile and diacetone alcohol under catalysis of concentrated sulfuric acid, so as to obtain a diacetone acrylamide crude product; 2, hydrolyzing the diacetone acrylamide crude by using a liquid alkali to remove high-melting-point acrylamide; 3, carrying out reduced pressure fractionation after hydrolysis to obtain a colorless transparent molten liquid; and 4, adding the molten liquid into xylene for recrystallization, washing and replacing xylene with petroleum ether, and carrying out drying to obtain the high-purity diacetone acrylamide. The method is simple and environmentally friendly, the yield isup to 80% or above, and the purity of the obtained diacetone acrylamide is high and reaches 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing high-purity diacetone acrylamide. Background technique [0002] Diacetone acrylamide is the main raw material for the synthesis of cross-linking agents. It was mainly used in the preparation of hair spray in the past. In recent years, due to the extensive use of cross-linking agent diacetone acrylamide in water-based paints to improve the adhesion of paints, its dosage has increased. Its synthesis research is also gradually increasing, and the competition is fierce, thereby requiring higher quality, so it is of practical significance to find a kind of preparation method of high-purity diacetone acrylamide. [0003] The research on the synthesis of diacetone acrylamide began in the 1960s. It was first synthesized by using acetone as a raw material and acrylonitrile in a sulfuric acid catalyst. Later, the continuous synthesis method was reported in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/31C07C231/06C07C231/24
CPCC07C231/06C07C231/24C07C233/31
Inventor 胡莉萍胡冠丰
Owner JINGCHU UNIV OF TECH
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