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A kind of synthetic method of high isoprene content butyl rubber

A technology of high isoprene and butyl rubber, which is applied in the field of synthesizing high isoprene content butyl rubber, can solve the problems of excessive heat release, etc., to solve the problem of excessive heat release, inhibit activity and reduce production. cost effect

Active Publication Date: 2019-01-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Another object of the present invention is to introduce nitro compounds into the process of synthesizing butyl rubber by the solution method, in order to realize the controlled reaction of butyl rubber and solve the problem of excessive heat release in the synthesis process

Method used

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  • A kind of synthetic method of high isoprene content butyl rubber
  • A kind of synthetic method of high isoprene content butyl rubber

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preparation example Construction

[0040] Catalyst preparation

[0041] The reaction flask was pumped and filled with nitrogen three times. Add 90ml of isopentane to a 1000ml polymerization bottle under the protection of high-purity nitrogen, add 200μl of water at room temperature, stir to make it evenly mixed, add 20ml of ethylaluminum sesquichloride, then add 1g of triethylaluminum and 1g of nitroethane, and aged at this temperature for 60min, thereby making a catalyst solution. The whole process was carried out in a glove box under a dry nitrogen atmosphere.

Embodiment 1

[0043] Add 200ml of monomer mixture (volume ratio of isobutylene to isoprene: 97:3) into 200ml of pre-prepared solvent (volume ratio of methyl chloride to n-hexane: 3:7) at -80°C, and then stir 15 ml of the catalyst described in Example 1 were added in the case of . After 30 min, 8 ml of methanol solution was added to terminate the reaction. The polymer was precipitated with 100 ml of methanol, then washed with water, filtered and dried at 50°C to constant weight. Butyl rubber polymer yield is 65.38%, and the number average molecular weight of product is 26.47 * 10 4 g / mol, the molecular weight distribution index is 1.98, and the degree of unsaturation is 1.6.

Embodiment 2

[0045] Except that the volume ratio of the polymerization solvent methyl chloride to n-hexane is 2:5; the volume ratio of isobutylene to isoprene is 92:8, the steps of Example 2 are repeated, and the yield of butyl rubber polymer is 62.6%. The number average molecular weight is 25.12×10 4 g / mol, the molecular weight distribution index is 1.95, and the degree of unsaturation is 3.6.

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Abstract

The invention relates to a synthesis method of high-isoprene butyl rubber. The method comprises the following steps: dissolving a polymerization monomer in a solvent at -80 ~ -20 DEG C, uniformly stirring, adding a catalyst mixture, polymerizing the monomer for 10-90min, adding a methanol solution to end the reaction, washing the obtained product with water, filtering the washed product, and drying to obtain the high-isoprene butyl rubber. The butyl rubber obtained through adopting the synthesis method has high reaction yield and high unsaturated degree; and a nitro compound is added in the preparation process to effectively inhibit the activity of an initiation system, so the controlled reaction of the butyl rubber is realized.

Description

technical field [0001] The invention relates to a method for synthesizing butyl rubber with high isoprene content. Background technique [0002] In 1943, the United States first adopted the slurry method for the industrial production of butyl rubber. The method adopts aluminum trichloride initiation system, methyl chloride is used as diluent, and a small amount of water or hydrogen chloride is added at the same time. Under strong stirring, isobutylene and isoprene are copolymerized at about -100 ° C to obtain diluent-insoluble The polymerization product - butyl rubber, makes the polymerization system present a slurry state. When the polymerization reaction temperature is higher than -85°C or the size of the colloidal particles in the reaction system reaches a certain value, the particles in the slurry system will aggregate into agglomerates, and the speed of forming aggregates will increase rapidly. These aggregates will settle in the reaction system and stick to the place....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/12C08F2/06
Inventor 潘广勤焦宏宇刘秀兰刘志琴胡开放王兴刚王春磊徐海燕彭仁苹王福善张耀亨李彤霞徐惠俭齐永新柏海见王彤宋阳张春梅
Owner PETROCHINA CO LTD
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