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Method for preparing thermal-reversible cross-linking polyisobutene rubber capable of being processed repeatedly

An isobutylene-based, multiple-processing technology, which is applied in the field of preparation of thermally reversible cross-linked polyisobutylene-based rubber that can be processed multiple times, to solve the problem of reuse, improve resource utilization, and reduce waste emissions.

Inactive Publication Date: 2016-07-06
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymer cross-links at 50°C and dissolves when heated to 230°C, but this process can only be repeated twice

Method used

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  • Method for preparing thermal-reversible cross-linking polyisobutene rubber capable of being processed repeatedly
  • Method for preparing thermal-reversible cross-linking polyisobutene rubber capable of being processed repeatedly

Examples

Experimental program
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Effect test

example 1

[0021] Obtaining of reversible vulcanized rubber matrix: Brominated poly(isobutylene-co-p-methylstyrene) to obtain brominated poly(isobutylene-co-p-methylstyrene) with benzyl bromide contents of 1mol%, 1.5mol%, and 2mol%, respectively Styrene), dry and ready to use.

example 2

[0023] Thermally reversible cross-linking agent acquisition: Add 250ml DCPD raw material solution into a 500ml flask, carry out pyrolysis distillation, collect fractions at 41°C to obtain a colorless and clear liquid, and store in a sealed container. The gas in the dry reaction flask was replaced with nitrogen, 170ml of THF and 40g of NaOH were added, 20ml of newly distilled CPD was extracted, added into the reaction flask and stirred, reacted at 0°C until the product no longer increased, and the reaction was terminated. Then, under the condition of ice-water bath, CO was continuously introduced into the 2 , the product was suction filtered, washed with water, and dried to obtain a light yellow powder, namely DCPD(COONa) 2 .

[0024] DCPD (COONa) 2 Add hydrochloric acid to acidify to pH = 3, cool in an ice-water bath, then slowly pour KOH in methanol solution or KOH in ethanol solution to pH = 7, then remove the liquid phase by suction filtration, and dry the filter cake und...

example 3

[0027] Get example 1 benzyl bromide content and be brominated poly(isobutylene-co-p-methylstyrene) 100g, potassium salt of dicyclopentadiene dicarboxylate 0.5g, carbon black 20g of 1mol%, open mill mix uniformly, roll pitch 10mm film, after cooling at room temperature for 10 hours, using a flat vulcanizer, press at 100°C and 10Mpa pressure for 60 minutes, then press at 30°C and 10Mpa for cold pressing 60min to obtain a thermally reversible cross-linked rubber film. Cut the film into pieces, put it into the flat vulcanizing machine again, press at 130°C and 10Mpa pressure for 60 minutes, and then press at 30°C and 10Mpa for 60 minutes to obtain Rubber film. Cut the film into pieces again, in a flat vulcanizing machine, under the condition of hot pressing temperature of 160°C and pressure of 10Mpa, hold the pressure for 60 minutes, and then under the condition of cold pressing temperature of 30°C and pressure of 10Mpa, hold the pressure for 60 minutes, and process the film For...

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Abstract

The invention relates to a method for preparing thermal-reversible cross-linking polyisobutene rubber capable of being processed repeatedly. According to a rubber matrix, a bromination poly(isobutene-co-p-methylstyrene) copolymer containing benzyl bromide functional groups is adopted, and the benzyl bromide functional groups generate a cross-linking reaction with a cross-linking agent easily; dimeric cyclopentadiene carboxylic acid sodium salt or dimeric cyclopentadiene carboxylic acid kali salt is adopted, by the adoption of a blended vulcanization mode, the thermal-reversible cross-linking agent generates an esterification reaction with the rubber matrix to form a dicyclopentadiene cross-linking bridge key, and then the rubber is prepared after hot press is performed. The prepared rubber is equivalent to traditional vulcanized rubber in stretchability and heat resistance, the tensile strength of the rubber is stabilized to be about 70% of original performance, the elongation at break is stabilized to be about 60% of original performance, rubber raw materials can be obviously saved, meanwhile, leftover materials can be reprocessed to be finished products, reutilization of the leftover materials is achieved, in this way, the utilization rate of resources is increased, and environmental friendliness and saving are achieved.

Description

technical field [0001] The invention belongs to the technical field of polyisobutylene rubber, in particular to a preparation method of thermally reversible crosslinked polyisobutylene rubber that can be processed multiple times. Background technique [0002] Brominated poly(isobutylene-co-p-methylstyrene), referred to as BIMS, is a type of rubber product developed by EXXON in the 1990s to replace traditional butyl rubber. Since the molecular chain segment of this type of rubber is completely saturated, and it has vulcanizable benzyl bromide as the crosslinking point after bromination, it has better heat resistance, aging resistance, weather resistance, etc. than butyl rubber. Excellent performance. [0003] The vulcanized brominated poly(isobutylene-co-p-methylstyrene) has a multi-dimensional network, excellent mechanical properties, sealing properties, and friction resistance, and is widely used in the fields of automobile tires, medical bottle stoppers, and seals. Howev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/28C08K5/098C08K3/04C07C51/41C07C61/29
CPCC07C4/22C07C51/15C07C51/412C07F1/04C08K3/04C08K5/098C08L2201/08C08L2203/30C08L2312/00C08L23/283C07C13/15C07C61/29Y02P20/141
Inventor 李树新常金杰伍一波张涛郭文莉杨丹商育伟谢意袁星昊
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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