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Method used for preparing isobutene and alkyl styrene and/or isoprene random copolymer via water phase cationic suspension polymerization

A technology of alkyl styrene and random copolymers, which is applied in the field of polymer material preparation to achieve the effect of reducing costs and expanding the scope of application

Active Publication Date: 2017-03-22
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above studies are all related to the research method of isobutylene copolymer prepared by cationic suspension in water phase, and the third component that stabilizes the active center is not added.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] At -100°C, add 100g of water, 115g of LiCl, H 2 SO 4 2ml, HBF 4 10ml, 1.0g of sodium lauryl sulfate, 100mL of a mixture of isobutylene and p-methylstyrene (wherein 10mol% of p-methylstyrene), and a monomer concentration of 36.3wt%. Sodium dialkyl sulfate is 1.41wt% by weight of the monomer. Under stirring, add 2mL of hydrogen chloride 0.4M, 2mL of ethyl acetate as the third component 0.4M into the system, add 32mL of tris(pentafluorophenyl)gallium (Ga(C 6 f 5 ) 3 ) solution 1M to initiate polymerization, wherein the molar ratio of hydrogen chloride, ethyl acetate and tris(pentafluorophenyl)gallium is 1:1:40. The polymerization reaction system is milky white and uniformly dispersed. After 20 minutes of polymerization reaction, NaOH / ethanol solution was added to terminate the reaction. The reaction system is washed several times with lye and water successively to remove residual monomers, dispersants, additives, reaction media, etc., to obtain a polymer, and to ob...

Embodiment 2

[0027] At -80°C, add 100g of water, 2.5g of trimethyldodecyl ammonium bromide, 10g of LiCl, HBF to the polymerization kettle 4 5ml, 50mL mixed solution of isobutylene and p-tert-butylstyrene (5mol% of p-tert-butylstyrene), monomer concentration 36.3wt%. Trimethyl dodecyl ammonium bromide is 7wt% by weight of the monomer. Under stirring, add 2mL 2-chloro-2,4,4-trimethylpentane 0.4M, 4mL N,N-dimethylformamide as the third component 0.4M into the system, add 16mL tris(pentafluorobenzene base) gallium (Ga(C 6 f 5 ) 3 ) solution 1M to initiate polymerization, wherein the molar ratio of 2-chloro-2,4,4-trimethylpentane TMPCl, N,N-dimethylformamide and tris(pentafluorophenyl)gallium is 1:2: 20. The polymerization reaction system is milky white and uniformly dispersed. After 20 minutes of polymerization reaction, NaOH / ethanol solution was added to terminate the reaction. The reaction system is washed several times with lye and water successively to remove residual monomers, dis...

Embodiment 3

[0029] At -60°C, add 100g of water, 2.5g of trifluoromethanesulfonic acid, 10g of LiCl, HBF to the polymerization kettle 4 10ml, 35mL mixture of isobutylene and m-methylstyrene (2mol% m-methylstyrene), monomer concentration 36.3wt%. Trifluoromethanesulfonic acid is 10 wt% of the monomer mass. Under stirring, add 2 mL of cumyl chloride 0.4 M, 1 mL of acetone as the third component 0.4 M into the system, add 4 mL of tris(pentafluorophenyl) gallium (Ga(C 6 f 5 ) 3 ) solution 1M to initiate polymerization, wherein the molar ratio of cumyl chloride, acetone and tris(pentafluorophenyl)gallium is 1:0.5:5. The polymerization reaction system is milky white and uniformly dispersed. After 20 minutes of polymerization reaction, NaOH / ethanol solution was added to terminate the reaction. The reaction system is washed several times with lye and water successively to remove residual monomers, dispersants, additives, reaction media, etc., to obtain a polymer, and to obtain a polymer after...

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PUM

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Abstract

The invention belongs to the technical field of high molecular material preparation, and discloses a method used for preparing an isobutene and alkyl styrene and / or isoprene random copolymer via water phase cationic suspension polymerization. According to the method, Lewis acids with high water resistance, such as tri(pentafluorophenyl)gallium (Ga(C6F5)3) and tri(pentafluorophenyl)aluminum (Al(C6F5)3) are taken as coinitiators of cationic polymerization, cationic copolymerization is adopted to synthesize the isobutene and alkyl styrene and / or isoprene random copolymer. The molecular weight and molecular weight distribution of the isobutene and alkyl styrene and / or isoprene random copolymer are preferable; living polymerization can be realized via adding of a third component in water phase cationic polymerization. The method is green, and is friendly to the environment.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, in particular to a method for preparing random copolymers of isobutylene and alkylstyrene and / or isoprene by cationic suspension polymerization in water phase, more specifically a polymer A green and environment-friendly synthetic method of the copolymer. That is to use water as the reaction medium, and realize the copolymerization of isobutylene and alkylstyrene or, and isoprene through the water-phase cationic suspension method, and prepare high-molecular-weight isobutylene, alkylstyrene, or, and isoprene random copolymerization way of things. Background technique [0002] At present, the above-mentioned isobutylene homopolymers and copolymers can only be prepared by cationic polymerization of isobutene monomers, which are usually required to be carried out in a dry organic reaction medium under the conditions of almost no oxygen, no water and high-purity inert gas protect...

Claims

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Application Information

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IPC IPC(8): C08F210/10C08F212/12C08F236/10C08F2/18
CPCC08F210/10C08F212/12C08F2500/03C08F236/10C08F2/18
Inventor 伍一波张经瀚郭文莉李树新商育伟杨丹王浩张敏
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY