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Preparation method of branched butyl rubber

A technology of butyl rubber and preparation process, applied in the field of preparation of branched butyl rubber, can solve the problems of slow stress relaxation rate of butyl rubber and the like

Active Publication Date: 2021-10-12
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention maintains a wide molecular weight distribution, which not only effectively solves the problem of slow stress relaxation rate of butyl rubber during processing, but also maintains sufficient raw rubber strength and good air tightness of butyl rubber, Endows butyl rubber with a balance of physical and mechanical properties and processing properties

Method used

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  • Preparation method of branched butyl rubber
  • Preparation method of branched butyl rubber
  • Preparation method of branched butyl rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of grafting agent: first in a jacketed 15L stainless steel reaction kettle, the argon gas is replaced twice, and 2820g cyclohexane, 560g styrene, 8.2g THF, 8.2mmol are added successively in the polymerization kettle n-Butyllithium was heated to 40°C and reacted for 50 minutes to form PS segments (the conversion rate of styrene monomer reached 100%); then 2905g cyclohexane, 290g styrene, and 301g butadiene were added to the polymerization kettle, 10.2g THF, heat up to 50°C, polymerize for 55 minutes to form -PS-SBR segment; finally add 35g of butadiene to the polymerization kettle, heat up to 60°C, react for 20 minutes, export the glue, and coagulate by wet method , drying, prepared with [-PS-SBR-B-] n Grafting agent for block structure copolymer (Mn is 11230, Mw / Mn is 1.12).

[0038] (2) Preparation of branched butyl rubber: first in a jacketed 4L stainless steel reaction kettle, nitrogen replacement was carried out 3 times, and in the polymerization ke...

Embodiment 2

[0040] (1) Preparation of grafting agent: at first in the 15L stainless steel reactor with jacket, lead to argon replacement 2 times, add 3020g hexamethylene successively in polymerization kettle, 601g styrene, 9.3g THF, 9.6mmol n-Butyllithium was heated to 45°C and reacted for 55min to form PS segments (the conversion rate of styrene monomer reached 100%); then, 3105g cyclohexane, 305g styrene, and 321g butadiene were added to the polymerization kettle, 12.1g THF, heat up to 52°C, polymerize for 57 minutes to form -PS-SBR segment; finally add 38g of butadiene to the polymerization kettle, heat up to 60°C, react for 22 minutes, export the glue, and coagulate by wet method , drying, prepared with [-PS-SBR-B-] n Grafting agent for block structure copolymers (Mn is 16310, Mw / Mn is 1.25).

[0041] (2) Preparation of branched butyl rubber: first in a jacketed 4L stainless steel reaction kettle, nitrogen replacement was carried out 3 times, and in the polymerization kettle, 574g of...

Embodiment 3

[0043] (1) Preparation of grafting agent: first in a jacketed 15L stainless steel reaction kettle, argon replacement is carried out 2 times, and 3168g cyclohexane, 635g styrene, 10.2g THF, 10.1mmol are added successively in the polymerization kettle n-Butyllithium was heated to 46°C and reacted for 57 minutes to form PS segments (the conversion rate of styrene monomer reached 100%); then, 3175g cyclohexane, 325g styrene, and 341g butadiene were added to the polymerization kettle, 15.7g THF, heat up to 54°C, polymerize for 59min to form -PS-SBR segment; finally add 40g of butadiene to the polymerization kettle, heat up to 65°C, react for 24min, export the glue, and coagulate by wet method , drying, prepared with [-PS-SBR-B-] n Grafting agent for block structure copolymer (Mn is 21400, Mw / Mn is 1.31).

[0044](2) Preparation of branched butyl rubber: first in a jacketed 4L stainless steel reaction kettle, nitrogen replacement was carried out 3 times, and in the polymerization k...

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Abstract

The invention aims to provide a preparation method of branched butyl rubber. The preparation method comprises the following steps of: synthesizing a [-PS-SBR-B-] n block copolymer serving as a grafting agent by taking lithium alkylide as an initiator, hydrocarbon as a solvent and an organic matter with certain polarity as a structure regulator and reaction monomers consisting of styrene and butadiene; and preparing the branched butyl rubber of a three-dimensional comb-shaped structure with PS and SBR grafted chain segments by adopting the grafting agent, isobutene and isoprene in a catalytic system compounded from Lewis acid and protonic acid through cationic polymerization. The branched butyl rubber has the advantages of high raw rubber strength rate, high air tightness, high stress relaxation rate and excellent viscoelasticity, and realizes the balance of physical and mechanical properties and processability. The preparation method of the branched butyl rubber provided by the invention has the characteristics of short process flow, controllable molecular weight, good product processability, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to a preparation method of branched butyl rubber, in particular to a method for preparing branched butyl rubber by grafting polyisobutylene with styrene / butadiene block copolymer. Background technique [0002] As we all know, butyl rubber (Butyl Rubber, IIR for short) is formed by cationic polymerization and copolymerization of isobutylene and a small amount of isoprene. Butyl rubber has a history of more than 70 years since it was industrialized by the American Exxon company in the 1940s. Due to its excellent air tightness, damping, heat aging resistance, ozone resistance and weather resistance, etc. Therefore, it is widely used in the fields of inner tubes, inner tubes, vulcanizing bladders and medical plugs of automobile tires, and has become one of the most important synthetic rubber varieties. [0003] However, the molecular chain of butyl rubber is mainly composed of carbon-carbon single bonds, the number of double bonds is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F287/00C08F210/12C08F297/04C08F2/38
CPCC08F287/00C08F297/04C08F2/38C08F210/12Y02T10/86
Inventor 徐典宏魏绪玲孟令坤翟云芳朱晶燕鹏华肖晔
Owner PETROCHINA CO LTD
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