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Preparation method of branched halogenated butyl rubber

A halogenated butyl rubber, butyl rubber technology, applied in the rubber field, can solve the problems of slow stress relaxation, poor processing performance, good damping and so on

Pending Publication Date: 2021-11-12
山东京博中聚新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, it is precisely because of the tight arrangement of IIR / HIIR molecules that the damping property is good, the stress relaxation is slow, and the processability is poor.

Method used

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  • Preparation method of branched halogenated butyl rubber

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preparation example Construction

[0033] The invention provides a kind of preparation method of branched halogenated butyl rubber, comprising:

[0034] S1) mixing the isomonoolefin, the conjugated diene and the first diluent to obtain a reactant solution;

[0035] Mixing the branching agent with the second diluent to obtain a branching agent solution;

[0036] S2) Mixing the reactant solution, the branching agent solution and the catalyst solution after low-temperature aging for polymerization reaction to obtain branched butyl rubber; the catalyst solution includes a Lewis acid, a cocatalyst and an aliphatic hydrocarbon;

[0037] S3) mixing branched butyl rubber with aliphatic hydrocarbons to obtain glue;

[0038] S4) mixing the glue solution and the wetting agent evenly, and then reacting it with a halogenating agent under the condition of avoiding light to obtain a reacted emulsion;

[0039] S5) mixing and reacting the reacted emulsion with the acid-binding agent to obtain a reaction solution;

[0040] S6...

Embodiment 1

[0063] 1.1 At -85°C, weigh 40g of isobutene and 1.5g of isoprene into 100g of methylene chloride to obtain a mixed material.

[0064] 1.2 Prepare 50 g of 1 wt % SBS / chloromethane solution, and pass HCl gas for 30 minutes to obtain hydrochloric acid acidified SBS / chloromethane solution.

[0065] 1.3 Add the hydrochloric acid acidified SBS / chloromethane solution obtained in step 1.2 to the mixed material obtained in 1.1, and then add 0.02 g of 1-hexene to obtain a solution to be reacted.

[0066] 1.4 Weigh 0.3g of n-hexane solution (mass fraction: 20%) of ethyl aluminum dichloride, add it to 12g HCl in dichloromethane solution (mass fraction: 0.020wt%), mix well, and age at -97.5°C After 30 min, the catalyst solution was obtained.

[0067] 1.5 Add the catalyst solution in step 1.4 to the solution to be reacted in step 1.3, and react at -97.5°C for 20 minutes. During the polymerization process, the temperature rises slowly, and the obtained slurry is uniformly dispersed in the ...

Embodiment 2

[0077] 2.1 At -85°C, weigh 40g of isobutene and 1.5g of isoprene into 100g of methylene chloride to obtain a mixed material.

[0078] 2.2 Prepare 50 g of 1 wt % SBS / chloromethane solution, and pass HCl gas for 30 minutes to obtain hydrochloric acid acidified SBS / chloromethane solution.

[0079] 2.3 Add the hydrochloric acid acidified SBS / chloromethane solution obtained in step 2.2 to the mixed material to obtain a solution to be reacted.

[0080] 2.4 Weigh 0.3g of n-hexane solution (mass fraction: 20%) of ethyl aluminum dichloride, add it to 12g HCl in dichloromethane solution (mass fraction: 0.020wt%), mix well, and age at -97.5°C After 30 min, the catalyst solution was obtained.

[0081] 2.5 Add the catalyst solution in step 2.4 to the solution to be reacted in step 2.3, and react at -97.5°C for 20 minutes. During the polymerization process, the temperature rises slowly, and the obtained slurry is uniformly dispersed in the form of particles.

[0082] 2.6 Add 2 mL of cold...

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Abstract

The invention provides a preparation method of branched halogenated butyl rubber. Compared with the prior art, the molecular weight of the synthesized branched butyl rubber is in bimodal distribution, the molecular weight distribution is widened, and the mechanical properties such as tensile strength are obviously improved, so that the processability of the butyl rubber is effectively improved; according to the branched butyl rubber halogenation method provided by the invention, the neutralization efficiency is improved, the possibility of incomplete neutralization is reduced, the conversion from a secondary allyl bromide substitution product to a primary allyl bromide substitution product is effectively inhibited, and the obtained brominated butyl rubber is excellent in various indexes and more stable in structure; meanwhile, the preparation method is easy to operate, easy in condition control and low in cost, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of rubber, in particular to a preparation method of branched halogenated butyl rubber. Background technique [0002] Butyl rubber (IIR) is copolymerized from isobutylene and a small amount of isoprene. Due to its molecular structure has a large methyl group and the molecules are tightly arranged, it has excellent airtightness. It is used in tires and sealing materials The application has irreplaceable advantages. However, its poor adhesion, slow vulcanization speed, and difficulty in blending with other rubbers also limit its application. [0003] Halogenated butyl rubber (HIIR) is divided into chlorinated butyl rubber (CIIR) and brominated butyl rubber (BIIR), which are prepared by adding chlorine or bromine to butyl rubber. HIIR not only maintains the excellent characteristics of butyl rubber, but also overcomes the disadvantages of butyl rubber, and can be used in the inner liner of car radial tires and...

Claims

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Application Information

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IPC IPC(8): C08F8/22C08F210/12
CPCC08F8/22C08F210/12C08F2500/05
Inventor 李立霞谢晴荆帅林栾波王孝海任学斌王耀伟
Owner 山东京博中聚新材料有限公司
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