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Preparation method of polymerization inhibitor

The technology of a polymerization inhibitor and a polymerization inhibitor is applied in the field of preparation of the polymerization inhibitor, which can solve the problems of polymerization reaction, short polymerization time, short storage period of the polymerization inhibitor, etc. The effect of improving the polymerization inhibition performance

Inactive Publication Date: 2018-11-02
雷春生
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a preparation method of a polymerization inhibitor for the short storage period of the current polymerization inhibitor, the polymerization reaction is prone to occur, and the polymerization inhibition time is short

Method used

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Examples

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preparation example Construction

[0016] A method for preparing a polymerization inhibitor includes the following steps:

[0017] (1) Take copper bromide and add anisole with a mass ratio of 1:50~60, sonicate for 5~10min to obtain ultrasonic liquid, take the ultrasonic liquid and add methacrylic acid with a mass ratio of 10~15:3~7:1~3 -2,2,6,6-Tetramethyl-4-piperidinyl ester and pentamethyldiethylenetriamine, stir and mix at 35~40℃ for 30~40min, and then add ultrasonic liquid quality 2~5% 的2-bromoisobutyrate ethyl ester to obtain a mixture;

[0018] (2) Take cross-linked polystyrene microspheres and mix with liquid bromine at a mass ratio of 3:1 to obtain mixture A. Take the mixture and add mixture A and dilauric acid at a mass ratio of 10-20:1~3:0.3~0.5 Put butyl tin into nitrogen protection, stir and mix at 75~80℃ for 2~3h to obtain a stirred mixture. Take the stirred mixture and add n-hexane according to the mass ratio of 1:60~70, let stand for 40~50min, filter, and take the precipitate according to mass ratio ...

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Abstract

The invention discloses a preparation method of a polymerization inhibitor and belongs to the technical field of chemical industry. According to the preparation method, cross-linked polystyrene microspheres and liquid bromine are used as base materials; 2,2,6,6-tetramethyl-4-piperidyl methacrylate is added as a monomer to form a polymer; then 4,6-binitro-2-sec-butylphenol is added and compounded,so that on one hand, the activity of a hemi-ketone free radical generated by phenol with an electron-donating group is improved; furthermore, a peroxy free radical is easy to combine to generate quinone for inhibiting the polymerization of styrene; on the other hand, when the steric hindrance of a substituent group is relatively great, the generated hemi-ketone free radical is more stable; N,N-diethylhydroxylamine is added and easily reacts with 2,2'-azobisisobutyronitrile or a primary free radical in a system to generate an R2NO free radical under a polymerization condition; the stable free radical can be subjected to rapid chain transfer and has polymerization retardation performance; the stable free radical assists the polymerization inhibitor base materials to increase continuous action time and the polymerization inhibition efficiency is increased. By adopting the preparation method, the problems of a current polymerization inhibitor that the storage period is relatively short, polymerization reaction easily occurs and the polymerization inhibition action time is relatively short are solved.

Description

Technical field [0001] The invention belongs to the technical field of chemical engineering, and specifically relates to a preparation method of a polymerization inhibitor. Background technique [0002] Polymerization inhibitor is an industrial auxiliary, usually used to prevent the progress of polymerization. Inhibitor molecules react with chain free radicals to form non-radical substances or low-activity free radicals that cannot be initiated, thereby terminating the polymerization. In order to avoid polymerization of vinyl monomers during storage, transportation, etc., a small amount of polymerization inhibitor is often added to the monomers and then removed before use. Generally, the polymerization inhibitor is a solid substance with low volatility and can be removed when the monomer is distilled. The commonly used inhibitor hydroquinone can react with sodium hydroxide to form water-soluble sodium salt, so it can be removed by washing with 5%-10% sodium hydroxide solution. ...

Claims

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Application Information

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IPC IPC(8): C08F8/06C08F257/02C08F220/34C09K15/32
CPCC08F8/06C08F257/02C09K15/32C08F220/34
Inventor 雷春生庄文琴李莉
Owner 雷春生
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