A kind of polymerization inhibitor and its preparation method and application

A technology of polymerization inhibitor and initiator, which is applied in the application field of polymer homogeneous supported polymerization inhibitor and acrylate preparation, can solve the problems of easy entrainment, etc. Effect

Active Publication Date: 2021-07-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymerization inhibitor solves the problem of easy entrainment of conventional polymerization inhibitors while not affecting the polymerization inhibition effect, ensures the quality of the product, is suitable for preventing the reaction system of double bond monomer polymerization, and is especially suitable for high boiling point ( In the meth)acrylate reaction system

Method used

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  • A kind of polymerization inhibitor and its preparation method and application
  • A kind of polymerization inhibitor and its preparation method and application
  • A kind of polymerization inhibitor and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] (1) dissolve MHPD and benzyl trithiocarbonate propionic acid in dichloromethane, add catalyst 4-dimethylaminopyridine and N,N-dicyclohexylcarbodiimide, wherein benzyl trithio The molar ratio of carbonate-based propionic acid and MHPD is 1:1, the molar ratio of 4-dimethylaminopyridine and MHPD is 0.1:1, and the molar ratio of N,N-dicyclohexylcarbodiimide and MHPD is 1:1: 1. Under the condition of 20°C, react for 24h, filter after the reaction, concentrate by rotary evaporation, and precipitate twice with diethyl ether to obtain a light yellow solid, which is dried in vacuo to obtain the compound of formula I; The compound of formula I obtained is subjected to infrared analysis, and 1732cm appears -1 ester bond peaks.

[0065] (2) the compound of formula I and methyl methacrylate are dissolved in N,N-dimethylformamide, and the reaction is carried out under the initiation of 2,2'-azobisisobutyronitrile, wherein the initiator and formula I The molar ratio of the compound...

Embodiment 2

[0074] (1) dissolve MHPD and benzyl trithiocarbonate propionic acid in chloroform, add catalyst 4-dimethylaminopyridine and N,N-dicyclohexylcarbodiimide, wherein benzyl trithio The molar ratio of carbonate-based propionic acid and MHPD is 3:1, the molar ratio of 4-dimethylaminopyridine and MHPD is 0.3:1, and the molar ratio of N,N-dicyclohexylcarbodiimide and MHPD is 3:1 1. Under the condition of 50°C, react for 72h, filter after the reaction, concentrate by rotary evaporation, and precipitate twice with diethyl ether as a solvent to obtain a light yellow solid, which is dried in vacuo to obtain the compound of formula I; The obtained compound of formula I was subjected to infrared analysis, and 1737 cm appeared -1 ester bond peaks.

[0075] (2) the compound of formula I and methyl acrylate are dissolved in N,N-dimethylacetamide, and the reaction is carried out under the initiation of 2,2'-azobisisoheptanenitrile, wherein the initiator and the compound of formula I The mola...

Embodiment 3

[0085] (1) dissolve MHPD and benzyl trithiocarbonate propionic acid in solvent chloroform, add catalyst 4-dimethylaminopyridine and N,N-dicyclohexylcarbodiimide, wherein benzyl trisulfide The molar ratio of carbonate-based propionic acid and MHPD is 2:1, the molar ratio of 4-dimethylaminopyridine and MHPD is 0.2:1, and the molar ratio of N,N-dicyclohexylcarbodiimide and MHPD is 2 : 1, under the condition of 25 ℃, react for 48h, filter after the reaction, concentrate by rotary evaporation, and precipitate twice with diethyl ether to obtain a light yellow solid, which is dried in vacuo to obtain the compound of formula I; The obtained compound of formula I was subjected to infrared analysis, and 1725cm appeared -1 ester bond peaks.

[0086] (2) the compound of formula I and ethyl methacrylate are dissolved in N,N-dimethylacetamide, and the reaction is carried out under the initiation of 2,2'-azobisisobutyronitrile, wherein the initiator and formula I The molar ratio of the co...

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Abstract

The invention discloses a polymerization inhibitor, a preparation method and application thereof. The polymerization inhibitor comprises the compound of the following general structure and / or wherein, R 1 is H or methyl, R 2 Is methyl or ethyl, m=20-40, preferably 25-35, and, 1≤x≤m. The polymerization inhibitor is a polymer homogeneously supported type, and is suitable for high boiling point (meth)acrylate reaction systems. On the one hand, the polymerization inhibitor can effectively prevent the polymerization of raw materials and products, and during the separation process, it significantly reduces the entrainment effect of the product on the polymerization inhibitor, ensuring the purity of the product. It meets the requirements of downstream use and thus has a good application prospect.

Description

technical field [0001] The invention relates to the field of polymerization inhibition, in particular to a polymer homogeneous supported polymerization inhibitor and its application in the preparation of (meth)acrylates. Background technique [0002] Phenolic polymerization inhibitors, phenothiazine, nitroxide free radicals, and metal polymerization inhibitors are commonly used polymerization inhibitors in the industry, but these inhibitors still have many problems. In the high-temperature separation process, it is difficult for a single polymerization inhibitor to avoid product polymerization; on the other hand, rectification is a conventional means to remove polymerization inhibitors, but most of the polymerization inhibitors have low saturated vapor pressure (especially high-efficiency inhibitors, such as nitrogen and oxygen free radicals). Base), it is difficult to separate in high boiling point products, which affects the use effect of the product. [0003] In order to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F8/14C08F8/32C07C67/08C07C67/03C07C67/04C07C69/653
CPCC07C67/03C07C67/04C07C67/08C08F8/14C07C2601/14C07C2602/42C08F8/32C08F120/14C07C69/653
Inventor 郭华鞠昌迅郑京涛陆国太黎源
Owner WANHUA CHEM GRP CO LTD
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