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Solution method for synthesizing butyl rubber

A technology of butyl rubber and solution method, which is applied in the field of butyl rubber synthesis by solution method, which can solve the problems of complex preparation process, difficulty in dissolving aluminum trichloride, difficulty in catalyst dispersion, etc., and achieve good control of polymerization reaction and narrow molecular weight distribution , the effect of high number average molecular weight

Active Publication Date: 2014-08-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of these technologies are that aluminum trichloride is difficult to dissolve in non-polar solvents when the initiation system is formulated, and the catalyst is difficult to disperse and the dispersion is poor.
This complicates the preparation process

Method used

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  • Solution method for synthesizing butyl rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 131ml of hexane with 54ml of methyl chloride, 124ml of isobutylene and 4.4ml of isoprene, take 33μL of water, add 6ml of sesqui-aluminum and dilute with 13ml of hexane to prepare an initiator system and age it for 15min. The prepared initiator system contains a large amount of white precipitation. After the initiation system was added to the polymerization at -80°C for 40 minutes, 10 ml of pre-cooled methanol solution was added to terminate. Precipitate by methanol solution, wash, and dry the product in vacuum.

Embodiment 2

[0028] Mix 131ml of hexane with 54ml of methyl chloride, 124ml of isobutene and 4.4ml of isoprene, then add to 0.3ml of CH 2 Cl 2 (Water content: 1600μg / g) was added 0.8ml of ethylaluminum dichloride and diluted with 9ml of hexane to prepare the trigger system and aged for 15min, the trigger system was light yellow, clear and free of white precipitate. After the initiation system was added to the polymerization at -80°C for 50 minutes, 10 ml of pre-cooled methanol solution was added to terminate it. Precipitate by methanol solution, wash, and dry the product in vacuum.

Embodiment 3

[0030] Mix 131ml of hexane with 54ml of methyl chloride, 124ml of isobutene and 4.4ml of isoprene, then mix 0.1ml of N,N-dimethylethanolamine with 0.3ml of CH 2 Cl 2 (water content: 1600μg / g) mixed, add 0.8ml of dichloroethylaluminum and dilute with 9ml of hexane to prepare the initiator system to age for 15min, add the initiator system to polymerization at -80°C for 50min, then add 10ml of pre-cooled methanol solution termination. Precipitate by methanol solution, wash, and dry the product in vacuum.

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Abstract

The invention relates to a solution method for synthesizing butyl rubber. A mixture of C4-C8 monoolefine monomers and C4-C14 polyene hydrocarbon monomers is taken as a raw material, and in a system that hexane and chloromethane are solvents, polymerization reaction is initiated by an initiating system to prepare butyl rubber polymer, wherein the reaction pressure is normal pressure, the reaction temperature ranges from 0 to -90DEG C, and the initiating system has the concentration of 0.01-0.001mol / L, and is prepared by dissolving a main initiator, namely deionized water and a coinitiator, namely aluminum alkyl dihalide by using a polar solvent CH2Cl2 for mixing, and adding alkylol amines; the molar ratio of the coinitiator to the main initiator is 1:1-10:1, and the molar ratio of a third component to the main initiator is 1:10-1:25; and the adding amount of the mixed solvent is 1 to 50 times volume of the polymerization monomers. According to the method, reaction is mild, polymerization temperature is improved, the stability and initiation efficiency of the initiators are high, and the molecular weight distribution of the product is narrow.

Description

technical field [0001] The invention relates to a method for synthesizing butyl rubber by a solution method. Background technique [0002] Butyl rubber is considered a copolymer of an isoolefin and one or more, preferably conjugated, multiolefins as comonomers. Butyl rubber polymer generally has two preparation methods: solution method and slurry method. The solution method is to prepare butyl rubber polymer in solution, using an aluminum trihalide catalyst system, and using aluminum trichloride or aluminum tribromide alone. system. The disadvantages of these technologies are that aluminum trichloride is difficult to dissolve in non-polar solvents when the initiation system is formulated, and the dispersion of the catalyst is difficult and poor. [0003] Canadian Patent 1,019,095 proposes the use of alkylaluminum halides such as ethylaluminum sesquichloride (C 2 h 5 ) 2 AlCl·Cl 2 AlC 2 h 5 , an industrial process for the preparation of butyl rubber in solution using ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/12C08F2/38C08F4/54
Inventor 潘广勤郭文莉张耀亨李树新刘秀兰伍一波焦宏宇胡开放钱锦华刘志琴刘栓祥武冠英何春赵小龙李彤霞齐永新李冬红黄英王兴刚盛艳闽晓兵
Owner PETROCHINA CO LTD
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