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Preparation method of high-conversion-rate and high-purity N-vinyl acetamide without catalyst.

A technology of vinylacetamide and high conversion rate, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of high thermal cracking temperature, increase the yield, and avoid acid-base neutralization The effect of dealing with the problem

Inactive Publication Date: 2022-01-28
山东瑞博龙化工科技股份有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0013] In order to solve the existing problems in the preparation process of N-vinylacetamide that need to use catalysts, need acid-base neutralization, and high thermal cracking temperature, the present invention proposes a catalyst-free, high-conversion, high-purity N-vinyl The preparation method of acetamide

Method used

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  • Preparation method of high-conversion-rate and high-purity N-vinyl acetamide without catalyst.

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preparation example Construction

[0031] The first aspect of the present invention provides a catalyst-free, high-conversion, high-purity N-vinylacetamide preparation method, including at least one of the following two methods:

[0032] High-temperature and high-pressure method: using acetaldehyde, acetamide, and ethanol as raw materials, under airtight conditions, first preheating at low temperature, then heating at high temperature, and reacting to obtain N-vinylacetamide;

[0033] Or use a pipeline reactor: use acetaldehyde, acetamide, and ethanol as raw materials, react in a pipeline reactor, and then obtain N-vinylacetamide by distillation under normal pressure and under reduced pressure.

[0034] The two methods belong to the same technical idea, and both improve the conversion rate and purity of N-vinylacetamide by controlling physical parameters.

[0035] In the high temperature and high pressure method:

[0036] It is carried out in a closed environment with high temperature and high pressure, such a...

experiment example 1

[0087] Low temperature and normal pressure method: Add 41.8g of acetaldehyde, 28g of acetamide, 25g of ethanol, and 0.5g of concentrated sulfuric acid (catalyst) into a 250mL three-necked flask, put it in a water bath, the temperature of the water bath is 6°C, and after stirring for 12 hours, GC analysis shows , the reaction cannot proceed, and there is no reaction between the substances.

experiment example 2

[0089] High temperature and normal pressure method: Add 42g of acetaldehyde, 28.3g of acetamide, 25.1g of ethanol, 0.5g of concentrated sulfuric acid (catalyst) into a 250mL three-necked flask, put it in an oil bath, set the temperature of the oil bath to 200°C, and stir for 12 hours , GC analysis showed that although there was a reaction between the various substances, the conversion rate of acetamide was only 11.3%. Since this reaction is an equilibrium reaction, the reaction cannot continue to the right under this condition.

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Abstract

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of high-conversion-rate and high-purity N-vinyl acetamide without a catalyst. In order to solve the problems that in the existing preparation process of N-vinyl acetamide, a catalyst is needed, acid-base neutralization is needed, and the thermal cracking temperature is too high, the invention provides a preparation method of high-conversion-rate and high-purity N-vinyl acetamide without a catalyst. According to the invention, N-vinyl acetamide is prepared by a one-pot method through a high-temperature and high-pressure method by adopting a physical means, and the conversion rate of raw materials and the purity of the N-vinyl acetamide can be realized without a catalyst; and when a pipeline reactor is selected as a reaction container, the thermal cracking temperature can be obviously reduced, the thermal cracking reaction can be completed when the temperature is 200-250 DEG C, the energy consumption is low, the reaction time is shorter, the generation of more byproducts can be avoided, and the conversion rate is relatively higher.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a catalyst-free, high-conversion, high-purity N-vinylacetamide preparation method. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] At present, there are two main synthetic routes of N-vinylacetamide (NVA): [0004] (1) N-(a-alkoxyethyl)-carboxamide cleavage method: [0005] The first step of hydroxyethylation: using acetaldehyde and acetamide as raw materials, adding a solvent (methanol, cyclohexane, etc.), and generating an intermediate under the action of a basic catalyst; [0006] The second step of etherification: add ethanol and a certain amount of concentrat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/08C07C233/05
CPCC07C231/08C07C233/05
Inventor 王红乐卢禄姚慧玲杨双庆穆佃鹏李田田张新民李晓璇郑万强
Owner 山东瑞博龙化工科技股份有限公司
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