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A kind of initiator, preparation method and application

A technology of use and compound, applied in the field of initiators, can solve the problems of inconvenient storage and transportation, and achieve the effects of low cost, simple synthesis method, and safe use and storage

Active Publication Date: 2016-07-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The initiator with this structural formula overcomes the problem of inconvenient storage and transportation of general free radical initiators, and has low cost and simple operation, and can initiate acrylates, methacrylates or styrene: such as methyl methacrylate, Monomers such as ethyl methacrylate, methyl acrylate, ethyl acrylate and styrene are polymerized, and polymers with higher molecular weights are easily obtained; while expanding the free radical polymerization initiator system, it is also suitable for carbon-carbon bond type active initiators Effective attempts have been made to improve the system

Method used

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  • A kind of initiator, preparation method and application
  • A kind of initiator, preparation method and application
  • A kind of initiator, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add the phase transfer agent benzyltriethylammonium bromide (TEBAC) (4.587g, 0.02mol), NaOH solid (about 4g, 0.1mol) or an equivalent amount of KOH solid into 10ml of distilled water, and stir the chlorine Phenylethanol (2.81g, 0.02mol) and p-tolueneacetonitrile (2.94g, 0.02mol) were slowly added dropwise to the reaction system, and after reacting at 50-60°C for 8-10 hours, add an ice-water bath or stand still at room temperature to stop reaction. After extraction with dichloromethane solvent, extract the organic layer, and then use anhydrous MgSO 4 Dry, evaporate the solvent to dryness, and separate and purify by column chromatography to obtain Compound A.

Embodiment 2

[0028] Add 1g of methyl methacrylate monomer, 0.0252g of initiator A and 2ml of toluene solvent into the polymerization tube, mix evenly and seal it well. Nitrogen was repeated 5 times. The polymerization tube was placed in an oil bath at 80°C for 10 hours of reaction, and then the polymerization tube was taken out, and the reaction was terminated at low temperature. Then use petroleum ether or methanol / water=1:1 solvent to precipitate the polymer, and dry it in a vacuum oven at 50°C to a constant weight. The conversion rate is 36.45%, and the number average molecular weight (M n )=86020, molecular weight distribution width (PDI)=1.78. However, the blank group without initiator A under the same conditions did not polymerize at all.

Embodiment 3

[0030] Add 1g of methyl methacrylate monomer, 0.0252g of initiator A and 2ml of toluene solvent into the polymerization tube, mix evenly and seal it well. Nitrogen was repeated 5 times. The polymerization tube was placed in an oil bath at 85° C. for 10 h, and then the polymerization tube was taken out, and the reaction was terminated at low temperature. Then use petroleum ether or methanol / water=1:1 solvent to precipitate the polymer, and dry it in a vacuum oven at 50°C to a constant weight. The conversion rate is 39.48%, and the number average molecular weight of the polymer (M n )=87320, molecular weight distribution width (PDI)=1.84. However, the blank group without initiator A under the same conditions only had a small amount of polymerization.

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Abstract

The invention discloses an initiator, a preparation method and application, and belongs to the technical field of initiators. The structure of the initiator is as shown in the specification, and is used for polymerization of alkene monomers initiated by the initiator. The initiator is characterized in that the related polymerization method mainly is body polymerization or solution polymerization; the initializing polymerization temperature is 70-130 DEG C. A polymerization initiator system is expanded, and the polymer with high molecular weight is obtained.

Description

technical field [0001] The invention relates to an initiator, a preparation method and an application for initiating the polymerization of vinyl monomers, and belongs to the technical field of initiators. Background technique [0002] Free radical polymerization is an effective method for large-scale production of various vinyl polymers. In industrial production, more than 70% of vinyl polymers are realized by free radical polymerization. Vinyl free radical polymerization is due to the monomers used Diversity, simple polymerization method, good repeatability, and relatively mild reaction conditions have become an important technology for industrial production of polymer products. [0003] Although free radical polymerization is an important method for industrial production of polymer products, since traditional free radical initiators are mostly azo and peroxy compounds, there is a risk of explosion, which brings a lot of inconvenience to use, storage and transportation; and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/00C08F120/14C08F112/08C08F2/06C08F2/02C07C255/33C07C251/30
Inventor 程斌鲍彦广
Owner BEIJING UNIV OF CHEM TECH