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Method for preparing N,N-dialkylacrylamide

A technology of dialkylacrylamide and dialkylaminopropionamide is applied in the field of new polymer monomer N, which can solve the problems of low industrialization value, high reaction temperature, many by-products, etc., so as to reduce the activation energy and reduce the reaction time, the effect of reducing by-products

Inactive Publication Date: 2008-03-19
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Subsequently, the German CPC company proposed to use 3-methoxy-N, N-dimethylpropionamide pyrolysis preparation method, but this type of method has complicated steps, high reaction temperature, and N, N-dimethylacrylamide is easy to produce Polymerization, many by-products, low yield, low industrial value

Method used

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  • Method for preparing N,N-dialkylacrylamide
  • Method for preparing N,N-dialkylacrylamide
  • Method for preparing N,N-dialkylacrylamide

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Weigh N,N-dimethyl-(3-dimethylamino)-propionamide 5g and add in the reactor, add 0.005g polymerization inhibitor 4010NA (0.1%), 0.05 gram hydrochloric acid (1%) simultaneously, control reaction The temperature was 140°C, the reaction pressure was kept at 400 mmHg, and the reaction was carried out for 3 hours, with a yield of 23.2%.

Embodiment 2

[0022] Weigh N,N-dimethyl-(3-dimethylamino)-propionamide 5g into the reactor, add 0.01g polymerization inhibitor 4010NA (0.2%), 0.1 gram p-toluenesulfonic acid (2%) , control the reaction temperature at 160°C, keep the reaction pressure at 300mmHg, react for 5h, and the yield is 54.6%.

Embodiment 3

[0024] Take by weighing N, N-dimethyl-(3-dimethylamino)-propionamide 5g adds in the reactor, adds 0.015g stopper hydroquinone (0.3%) simultaneously, 0.1 gram zinc chloride (2 %), control the reaction temperature at 180°C, keep the reaction pressure at 200mmHg, react for 8h, and the yield is 78.7%.

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Abstract

The invention discloses a preparation method of new polymer monomer N, N-dialkyl acrylamide and the improvement of a process route, that is, under the existance of polymerization inhibitor and the function of catalyst, the 3-dialkyl amidocyanogen propanamide shown in the formula (I) goes through thermal cracking reaction for two the twenty hours under the conditions of temperature between 100 DEG C and 280 DEG C and pressure between 200 mmHg and 760 mmHg, and after a cracking product is processed, the N, N-dialkyl acrylamide shown in the formula (II) is obtained. Because acid as catalyst is added into the reaction system, the activation energy of the thermal cracking reaction is lowered, the reactive selectivity and the reactive yield rate are increased, and therefore energy consumption is reduced. Compared with the original cracking technique, the temperature of cracking is lowered, the time of reaction is shortened, that is, the time of reaction is shortened to a few hours from over twenty hours, the yield rate of cracking is increased, and byproducts are reduced.

Description

(1) Technical field [0001] The invention relates to the development of new industrial technology for N,N-dialkylacrylamide, a new type of polymer monomer, in particular to the selection of catalysts, the optimization of reaction conditions and the optimization of process routes in catalytic thermal cracking reactions. (2) Background technology [0002] There are mainly two methods for the synthesis of N, N-dialkylacrylamides: (1) retain the double bond and directly replace the carbonyl compound of the propylene skeleton; (2) first protect the double bond and synthesize the carbonyl compound of the propylene skeleton with multiple substituents, Then thermal decomposition removes the redundant substituents and restores the double bond to obtain the product. The research on N, N-dialkylacrylamide abroad has become increasingly in-depth and extensive. Al-colac Co.Ltd in the United States, Kohjin in Japan, Mitsui Toatsu Chemicals (Mitsui Toatsu Chemicals) and Bimax in the United ...

Claims

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Application Information

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IPC IPC(8): C07C233/09C07C231/12
Inventor 李郁锦韩亮高建荣盛卫坚贾建洪王敏韩非
Owner ZHEJIANG UNIV OF TECH
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