Preparation method for N-methylolacrylamide

A technology of -methylol acrylamide and acrylic acid amine, which is applied in the field of preparation of N-methylol acrylamide, can solve the problems of inconvenient operation, low yield, complicated technological process, etc., so as to improve product yield and improve product quality. the quality of the effect

Inactive Publication Date: 2012-01-04
WUJIANG BEISHE SHENGYUAN TEXTILE PROD AUXILIARIES PLANT
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Problems solved by technology

[0004] Therefore, the preparation method of N-methylolacrylamide at the present stage either has extremely low yield, or complicated technological process and inconvenient operation

Method used

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Embodiment Construction

[0010] The technical solutions of the present invention will be described in detail below in conjunction with examples.

[0011] The preparation method of N-methylolacrylamide of the present invention, the reagent that adopts has: acrylamide crystal, paraformaldehyde, ethyl acetate, triethylamine, dilute sulfuric acid and composite polymerization inhibitor, wherein, acrylamide crystal and The molar ratio of paraformaldehyde is 1.1.05; the operation process is: first put a certain amount of ethyl acetate in the reaction container, then add acrylamide crystals to the ethyl acetate, and heat to control the reaction temperature between 38-42 ℃ to promote the dissolution of acrylamide in ethyl acetate; then add a compound inhibitor to the ethyl acetate in which acrylamide is dissolved, the compound inhibitor is composed of hydroquinone and diphenylamine, and then slowly add alkali The catalyst is triethylamine and paraformaldehyde. The purpose of adding triethylamine is to control ...

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Abstract

The present invention discloses a preparation method for N-methylolacrylamide. The method comprises the following steps: firstly adding acrylamide crystal to acetic ether; then heating to a temperature of 38-42 DEG C; then adding a composite polymerization inhibitor and trioxymethylene, wherein the composite polymerization inhibitor comprises hydroquinone and diphenylamine; adopting an alkaline catalyst of triethanolamine to adjust the pH value of the reaction solution to 9.5-9.6; carrying out the reaction for 1.5-2.5 hours at the temperature of 38-42 DEG C after completing the material adding; carrying out filtering while the solution is hot after completing the reaction; adopting dilute sulfuric acid to adjust the pH value of the filtrate to the neutral pH value; carrying out cooling and crystallization for the neutral filtrate to obtain the crude N-methylolacrylamide product. According to the present invention, the product having the content more than 97% and the yield more than 98% can be obtained; compared to the prior art, the product yield and the product quality are effectively improved through the method provided by the present invention.

Description

technical field [0001] The invention relates to a preparation method of N-methylolacrylamide. Background technique [0002] N-methylolacrylamide is a white crystalline powder with a melting point of 74-75°C, easily soluble in water and hydrophilic solvents, soluble in fatty acid lipids, but almost insoluble in hydrophobic solvents such as hydrocarbons and halogenated hydrocarbons . The molecular structure of N-methylolacrylamide contains two active groups, a double bond that can be polymerized and a methylol group that can be condensed, and has the characteristics of an interwoven monomer. Therefore, N-methylolacrylamide is used in textiles, It is widely used in adhesives, plastics, coatings and other industries. [0003] At present, there are many methods for synthesizing N-methylolacrylamide at home and abroad. An Yuanchu used 36% formaldehyde and acrylamide to synthesize N-methylolacrylamide with a yield of 44% at a low temperature of 0-5°C; British scholars used paraf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/20C07C231/12
Inventor 钱华张宁荣
Owner WUJIANG BEISHE SHENGYUAN TEXTILE PROD AUXILIARIES PLANT
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