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Preparation method of hyperbranched butyl rubber with ultra-wide molecular weight distribution

A technology of wide molecular weight distribution and molecular weight distribution, applied in the field of ultra-broad molecular weight distribution and the preparation of hyperbranched butyl rubber, can solve the problems of small extrusion expansion effect of stress relaxation rate and slow stress relaxation rate.

Active Publication Date: 2021-12-24
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problems of extrusion swell and slow stress relaxation rate that butyl rubber is prone to occur during processing, so that ultra-wide molecular weight distribution, hyperbranched butyl rubber can obtain fast stress relaxation rate and extrusion rate during processing. Excellent processability with small swelling effect, while ensuring sufficient raw rubber strength and good air tightness of butyl rubber, achieving a balance between physical and mechanical properties and processability

Method used

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  • Preparation method of hyperbranched butyl rubber with ultra-wide molecular weight distribution
  • Preparation method of hyperbranched butyl rubber with ultra-wide molecular weight distribution
  • Preparation method of hyperbranched butyl rubber with ultra-wide molecular weight distribution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Preparation of grafting agent:

[0046] a Preparation of coupling agent: First, in a jacketed 4L stainless steel polymerization kettle, replace with argon for 3 times, then add 600g of deionized water and 58g of 3,9-dioxo[5.5]spirocyclodecane to the polymerization kettle One alkane, 320g liquid bromine, 18g HCl-CH 3 OH solution (the molar concentration of HCl is: 0.7mol / L), the temperature is raised to 70° C., after reacting for 3.0 hours, adding 300 g of mass concentration is 15% NaOH aqueous solution to terminate the reaction, and finally adding 800 g of monochloromethane for extraction, separation, washing, The coupling agent 1,5-dibromo-3,3 bis(2-bromoethyl)pentane was obtained by drying (yield 93%).

[0047] b Preparation of grafting agent: In a 15L stainless steel polymerization kettle A with a jacket, the system was replaced by argon for 3 times, and 1610g cyclohexane, 160g styrene, and 80g 1,3-butane were sequentially added to the polymerization kettle Die...

Embodiment 2

[0050] (1) Preparation of grafting agent:

[0051] The preparation of a coupling agent: with embodiment 1.

[0052] b Preparation of grafting agent: In a 15L stainless steel polymerization kettle A with a jacket, the system was replaced by argon for 3 times, and 1720g cyclohexane, 180g styrene, and 90g 1,3-butane were sequentially added to the polymerization kettle Diene, 1.2g THF, heat up to 50°C, add 25.1mmol n-butyllithium to start the reaction, the temperature gradually rises from 50°C to 80°C within 70min, the heating rate is 0.5°C / min, and the reaction takes 70min to form a wide vinyl content Distributed -SBR- segment, then heated up to 85°C, added 240mmol 1,5-dibromo-3,3 bis(2-bromoethyl)pentane, and carried out coupling reaction for 70min; at the same time in 15L stainless steel polymerization kettle B In the process, the system was replaced by argon for 3 times, 1740g cyclohexane, 185g styrene, 85g 1,3-butadiene, 1.1g THF were added in sequence, the temperature was r...

Embodiment 3

[0055] (1) Preparation of grafting agent:

[0056] The preparation of a coupling agent: with embodiment 1.

[0057]b Preparation of grafting agent: In a 15L stainless steel polymerization kettle A with a jacket, the system was replaced by argon for 3 times, and 1920g cyclohexane, 200g styrene, 100g 1,3-butane were sequentially added to the polymerization kettle Diene, 1.3g THF, heat up to 50°C, add 27.5mmol n-butyllithium to start the reaction, the temperature gradually rises from 50°C to 80°C within 80min, the heating rate is 0.4°C / min, and react for 80min to form a wide vinyl content Distributed -SBR- segment, then heated to 85°C, added 270mmol 1,5-dibromo-3,3 bis(2-bromoethyl)pentane, and carried out coupling reaction for 75min; at the same time, in 15L stainless steel polymerization kettle B During the process, the system was replaced by argon for 3 times, 1900g cyclohexane, 195g styrene, 92g 1,3-butadiene, 1.3g THF were added in sequence, the temperature was raised to 55...

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Abstract

The invention relates to a preparation method of hyperbranched butyl rubber with ultra-wide molecular weight distribution, which comprises the following steps of: preparing four chain segments with different wide vinyl content distribution and wide molecular weight distribution by using binary reaction monomers of styrene and butadiene through four-kettle reaction and variable-temperature polymerization; preparing a binary four-miktoarm star-shaped copolymer [-B-SBR-] n [-BR1-PS-B-] n Y [-BR-SBR-B-] n [-PS-B-] n with a four-miktoarm star-shaped structure through coupling of a synthesized novel coupling agent 1, 5-dihalo-3, 3-bis (2-haloethyl) pentane; and performing cationic polymerization on the binary four-miktoarm star copolymer as a grafting agent, isobutene and isoprene in a catalytic system compounded by alkyl aluminum halide and protonic acid to obtain hyperbranched butyl rubber with ultra-wide molecular weight distribution.

Description

technical field [0001] The invention relates to a preparation method of ultra-wide molecular weight distribution and hyperbranched butyl rubber, in particular to a binary tetraheteroarm star-shaped copolymer synthesized from styrene and butadiene as a grafting agent with isobutylene and isoprene A process for the preparation of ultra-broad molecular weight distribution, hyperbranched butyl rubber by cationic polymerization of dienes. 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 automob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F287/00C08F210/12C08F236/08C08F293/00
CPCC08F287/00C08F293/00C08F210/12C08F236/08Y02T10/86
Inventor 徐典宏牛承祥孟令坤翟云芳朱晶燕鹏华
Owner PETROCHINA CO LTD