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Preparation method and application of polymerization inhibitor

A technology of polymerization inhibitors and uses, which is applied in the field of preparation of polymerization inhibitors, can solve the problems of inability to meet the requirements of new industrial green environmental protection, high toxicity, etc., and achieve the effects of low toxicity, excellent polymerization inhibition effect and good stability

Inactive Publication Date: 2020-09-22
宜兴金兑化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the prior art, dinitrophenol is usually used as the main polymerization inhibitor in the production of styrene, but because of its high toxicity, it cannot meet the requirements of new industrial green environmental protection

Method used

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  • Preparation method and application of polymerization inhibitor
  • Preparation method and application of polymerization inhibitor
  • Preparation method and application of polymerization inhibitor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: a kind of preparation method of inhibitor, specifically comprises:

[0026] Step 1: Preparation of Type I Mixed Matrix

[0027] Mix 2,4-dinitro-6-sec-butylphenol and N,N-dibenzylhydroxylamine evenly to prepare a type I mixed matrix; among them, 2,4-dinitro-6-sec-butylphenol The mixing molar ratio with N,N-dibenzylhydroxylamine is 0.5:1.3; the reaction temperature in step 1 is 28°C, and the reaction time is 3h;

[0028] Step 2: Preparation of Type II Mixed Matrix

[0029] Diethylhydroxylamine and 2-thiomethyl ether phenothiazine are mixed and cross-linked in the presence of triethylamine to obtain II mixed matrix; wherein, the mixing molar ratio of diethylhydroxylamine and 2-thiomethyl ether phenothiazine It is 2.6:1; step 2 reaction temperature is 85 ℃, and reaction time is 6h;

[0030] Step 3: Preparation of premix

[0031] The type I mixed matrix and the II mixed matrix are mixed and reacted to form a premix; then deionized water is added to the prem...

Embodiment 4

[0035] Embodiment 4: a kind of preparation method of inhibitor, specifically comprises:

[0036] Step 1: Preparation of Type I Mixed Matrix

[0037] Mix 2,4-dinitro-6-sec-butylphenol and N,N-dibenzylhydroxylamine evenly to prepare a type I mixed matrix; among them, 2,4-dinitro-6-sec-butylphenol The mixing molar ratio with N,N-dibenzylhydroxylamine is 0.6:1.3; the reaction temperature in step 1 is 30°C, and the reaction time is 3.5h;

[0038] Step 2: Preparation of Type II Mixed Matrix

[0039] Diethylhydroxylamine and 2-thiomethyl ether phenothiazine are mixed and cross-linked in the presence of triethylamine to obtain II mixed matrix; wherein, the mixing molar ratio of diethylhydroxylamine and 2-thiomethyl ether phenothiazine It is 2.8:1; step 2 reaction temperature is 90 ℃, and reaction time is 12h;

[0040] Step 3: Preparation of premix

[0041] The type I mixed matrix and the II mixed matrix are mixed and reacted to form a premix; then deionized water is added to the p...

Embodiment 3

[0045] Embodiment 3: a kind of preparation method of inhibitor, specifically comprises:

[0046] Step 1: Preparation of Type I Mixed Matrix

[0047] Mix 2,4-dinitro-6-sec-butylphenol and N,N-dibenzylhydroxylamine evenly to prepare a type I mixed matrix; among them, 2,4-dinitro-6-sec-butylphenol The mixing molar ratio with N,N-dibenzylhydroxylamine is 0.8:1.3; the reaction temperature in step 1 is 32°C, and the reaction time is 4h;

[0048] Step 2: Preparation of Type II Mixed Matrix

[0049] Diethylhydroxylamine and 2-thiomethyl ether phenothiazine are mixed and cross-linked in the presence of triethylamine to obtain II mixed matrix; wherein, the mixing molar ratio of diethylhydroxylamine and 2-thiomethyl ether phenothiazine It is 3.2:1; step 2 reaction temperature is 95 ℃, and reaction time is 14h;

[0050] Step 3: Preparation of premix

[0051] The type I mixed matrix and the II mixed matrix are mixed and reacted to form a premix; then deionized water is added to the pre...

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Abstract

The invention provides a preparation method and application of a polymerization inhibitor. The preparation method comprises the following steps of: uniformly mixing 2, 4-dinitro-6-sec-butyl phenol with N, N-dibenzyl hydroxylamine to prepare a class I mixed matrix; mixing diethylhydroxylamine and 2-thiomethyl ether phenothiazine, performing mixing in the presence of triethylamine, and carrying outcrosslinking to obtain a mixed matrix II; mixing and reacting the class I mixed matrix with the mixed matrix II to form a premix; adding deionized water into the premix, and uniformly mixing the substances to prepare a premix aqueous solution; adding benzyl methacrylate into the premix aqueous solution, adding sodium hydroxide, and performing standing to obtain the polymerization inhibitor; the method is simple in preparation process and relatively low in preparation cost; the polymerization inhibitor prepared by the method has the advantages of favorable stability, low toxicity and excellentenvironment friendliness.

Description

technical field [0001] The invention relates to the technical field of chemical products, in particular to a preparation method and application of a polymerization inhibitor. Background technique [0002] Styrene is a widely used chemical raw material, and its monomer is easy to polymerize, which can be polymerized at room temperature. In the production of styrene, in order to reduce the self-polymerization of styrene, in addition to using negative pressure operation to reduce the rectification temperature, it is usually necessary to add a high-efficiency polymerization inhibitor. [0003] However, in the prior art, dinitrophenol is usually used as the main polymerization inhibitor in the production of styrene, but because of its high toxicity, it cannot meet the requirements of new industrial green environmental protection. [0004] There is an urgent need for an environmentally friendly polymerization inhibitor to be used in the production of styrene. Contents of the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D279/20C07C7/20C07C15/46
CPCC07C7/20C07D279/20C07C15/46
Inventor 杨巍路竹强
Owner 宜兴金兑化工有限公司