Preparation method of butyl rubber

A butyl rubber and slurry technology, applied in the rubber field, can solve the problems of product quality fluctuation and production cost increase, etc.

Active Publication Date: 2021-02-26
山东京博中聚新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Frequent start-up and shutdown of production equipment will lead to increased production costs and large fluctuations in product quality

Method used

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

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preparation example Construction

[0035] The invention provides a kind of preparation method of butyl rubber, comprises the following steps:

[0036] a) mixing a monoolefin with a solvent to obtain a mixed solution;

[0037] b) dissolving the slurry stabilizer in diene to obtain a slurry stabilizer solution;

[0038] c) mixing and reacting the mixed solution, the slurry stabilizer solution and the catalyst solution to form butyl rubber;

[0039] Described slurry stabilizer has structure shown in formula (1):

[0040]

[0041] in,

[0042] R 1 , R 2 , R 3 and R 4 each independently selected from H, C1-C15 alkyl, vinyl, halogen, hydroxyl, halomethyl, haloethyl or α-methylvinyl;

[0043] Polymerization n 1 4~2000, n 2 0~2000, n 3 0~2000, n 4 0~2000, n 5 0~2000, n 6 It is 0~2000.

[0044] The present invention introduces the slurry stabilizer shown in formula (1) in the preparation process, which can effectively reduce the polymerization speed of cationic living polymerization, improve the dispers...

Embodiment 1

[0090] S1. At -70°C, weigh 22.5g of isobutene and add it to 127.5g of monochloromethane to obtain a mixed solution.

[0091] S2. Add the polymer represented by formula (1-1) into isoprene to obtain a 6.3 wt% slurry stabilizer solution.

[0092] S3. Add 1.07 g of the slurry stabilizer solution in step S2 to the mixed solution in step S1, and lower the temperature to -97.5° C. to obtain a reactant solution.

[0093] S4, take by weighing the normal hexane solution (mass fraction of 10%) of 0.2g ethyl aluminum sesquichloride, join in the monochloromethane solution (mass fraction of 0.025wt%) of 10gHCl, mix well, and in-97.5 Aging at ℃ for 30 min to obtain a catalyst solution.

[0094] S5. Add the catalyst solution in step S4 into the reactant solution in step S3, 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.

[0095] S6. Add 2 g of ethanol to termin...

Embodiment 2

[0097] S1. At -70°C, weigh 20 g of isobutene and add it to 113.5 g of monochloromethane to obtain a mixed solution.

[0098] S2. Add the polymer represented by formula (1-2) into isoprene to obtain a 4.4 wt% slurry stabilizer solution.

[0099] S3. Add 1.36 g of the slurry stabilizer solution in step S2 to the mixed solution in step S1, and lower the temperature to -97.5° C. to obtain a reactant solution.

[0100] S4. Weigh 0.15g of a n-hexane solution of diethylaluminum chloride (20% by mass fraction), add it into a chloromethane solution of 6gHCl (0.020wt% by mass fraction), mix well, and store at -97.5°C aging for 20 min to obtain a catalyst solution.

[0101] S5. Add the catalyst solution in step S4 into the reactant solution in step S3, and react at -97.5° C. for 10 min. During the polymerization process, the temperature rises slowly, and the obtained slurry is uniformly dispersed in the form of particles.

[0102] S6. Add 2 g of ethanol to terminate the reaction, move...

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Abstract

The invention provides a preparation method of butyl rubber. The preparation method provided by the invention comprises the following steps: a) mixing monoolefine with a solvent to obtain a mixed solution; b) dissolving a slurry stabilizer in diene to obtain a slurry stabilizer solution; and c) mixing the mixed solution, the slurry stabilizer solution and a catalyst solution for reaction to form butyl rubber. In the preparation process, the slurry stabilizer shown in the formula (1) is introduced, so that the polymerization speed of cationic active polymerization can be effectively reduced, the dispersion state of butyl rubber in a polymerization system is improved, product agglomeration is inhibited, the mass and heat transfer of the polymerization system is enhanced, the blockage of a reaction kettle is reduced, and the reaction period is prolonged; and finally, the product molecular weight is improved, the molecular weight distribution is broadened, and the product quality is improved.

Description

technical field [0001] The invention relates to the field of rubber, in particular to a preparation method of butyl rubber. Background technique [0002] Butyl rubber is a kind of synthetic rubber, which is mainly made of isobutylene and a small amount of isoprene by cationic polymerization at low temperature (about -100°C) under the initiator system. Butyl rubber has good chemical stability and thermal stability, the most prominent is air tightness and water tightness. Due to its unique properties, it is widely used in many aspects such as manufacturing inner tubes, anti-vibration rubber, industrial rubber sheets, medical rubber, etc. . [0003] At present, the butyl rubber polymerization process adopts the slurry polymerization method, using methyl chloride as the solvent, Lewis acid as the main catalyst, and protonic acid as the co-catalyst, which is a typical cationic polymerization. The reaction has the characteristics of fast reaction speed, concentrated heat release...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F236/08C08F2/14
CPCC08F210/12C08F236/08C08F2/14
Inventor 李立霞栾波任学斌王衍金
Owner 山东京博中聚新材料有限公司
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