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Catalysis system and method for preparing diolefin copolymer elastomer

A catalytic system and elastomer technology, applied in the field of catalytic systems, can solve the problems of difficult separation and removal of solvents, low cis content, etc., and achieve the effects of good stability, high orientation and high catalytic activity

Active Publication Date: 2011-01-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1295087A adds m-xylene (m-xylene / rare earth salt=130) to the catalytic system, and the intrinsic viscosity of the copolymerized elastomer prepared is reduced from 7.3dL / g to 5.2dL / g, but the structure of butadiene and isoprene The unit cis content is relatively low, 97.6% and 95.3%, respectively, and the large amount of m-xylene makes it difficult to separate and remove the solvent in the post-treatment process

Method used

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  • Catalysis system and method for preparing diolefin copolymer elastomer
  • Catalysis system and method for preparing diolefin copolymer elastomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Under the protection of nitrogen, add 0.031mmol of neodymium isooctanoate, 0.77mmol of triisobutylaluminum, 0.023mmol of dibutylaluminum hydride, 0.93mmol of chloroform, and 0.025mmol of ethyl trichloroacetate into the dry catalyst preparation device , 0.009 mmol of octanoic acid and 0.09 mmol of ethanol were evenly mixed and then aged at 30° C. for 50 min to prepare a homogeneous catalyst system for future use.

[0026] Add 23 mL of butadiene / isoprene hexane solution (wherein [Bd]=3.1mol / L, [Ip]=1.3mol / L) into the dry polymerization reactor under the protection of nitrogen, and then add the above-prepared Catalyst solution, the molar ratio of catalyst component A (neodymium isooctanoate) to total monomer is 3.0×10 -4 . After polymerization for 3 hours at 50°C, add 1 wt% of 2,6-di-tert-butyl-p-methylphenol in ethanol solution to terminate the reaction, wash it and place it in a vacuum oven at 45°C to dry to constant weight. The yield of the copolymerization product is ...

Embodiment 2

[0028] Under the protection of nitrogen, add 0.16mmol neodymium octanoate, 0.082mmol ethanol, 1.52mmol triisobutylaluminum, 2.74mmol chloroform, 0.10mmol ethyl chloroacetate, 0.048mmol isooctanoic acid and 0.005mmol Mmol capric acid was mixed uniformly and then aged at 50°C for 1 h to prepare a homogeneous catalyst system for future use.

[0029] Under the protection of nitrogen, add 42 mL of butadiene / isoprene hexane solution (where [Bd]=2.3mol / L, [Ip]=0.5mol / L) into the dry polymerization reactor, and then add the above A good catalyst solution, the molar ratio of catalyst component A (neodymium octanoate) to monomer is 1.4×10 -3 . The polymerization was terminated after 1 hour at 50° C., and the termination and post-treatment methods were the same as in Example 1. The copolymerization product yield is 41%, M w 1.5×10 6 ,M w / M n is 2.4, [η] is 4.3dL / g, the cis-1 and 4 contents of butadiene and isoprene chain members are 99.0% and 99.6%, respectively, and the butadiene...

Embodiment 3

[0031] Add 0.028mmol neodymium naphthenate, 0.003mmol ethanol, 0.92mmol triisobutylaluminum, 0.032mmol dibutylaluminum hydride, 0.08mmol chloroform and 0.008mmol isooctanoic acid to the dry catalyst preparation device under nitrogen protection , mixed evenly and aged at 10°C for 115h to prepare a homogeneous catalyst system for future use.

[0032] Add 42 mL of butadiene / isoprene hexane solution (wherein [Bd]=1.8mol / L, [Ip]=0.4mol / L) into the dry polymerization reactor under the protection of nitrogen, and then add the above prepared Catalyst solution, the molar ratio of catalyst component A (neodymium naphthenate) and monomer is 3.5 * 10 -4 . Polymerization was terminated at 50°C for 25 hours, and the termination and post-treatment methods were the same as in Example 1. Copolymerization product yield is 27%, M w 3.9×10 5 ,M w / M n is 2.9, [η] is 2.1dL / g, the cis-1 and 4 contents of butadiene and isoprene chain members are 98.0% and 98.8%, respectively, and the butadiene...

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Abstract

The invention relates to a catalysis system, in particular to a rear earth catalysis system for copolymerizing diolefin and a method for preparing diolefin copolymer elastomer. In the invention, a homogeneous catalysis system based on rare-earth carboxylate is adopted, and a bivinyl / methyl butane random copolymerization elastomer with excellent low-temperature elasticity can be prepared by changing the preparing conditions of the catalysis system and the technology conditions of polymerization under the condition of ensuring high catalytic activity and stable catalytic performance, wherein the bivinyl / methyl butane random copolymerization elastomer has the following advantages that the cis-form content of two structural units are both higher than 98% ( can be higher than 99% at the same time), the weight-average molecular weight (Mw) is 3.9*10<5> to 1.5*10<6>, and the molecular weight dispersion index (Mw / Mn) is 1.8 to 4.3.

Description

Technical field: [0001] The invention relates to a catalytic system, especially a rare earth catalytic system for diolefin copolymerization and a method for preparing diolefin copolymerized elastomer. Background technique: [0002] High cis-butadiene rubber (referred to as butadiene rubber) can be obtained under the action of nickel-based, titanium-based, cobalt-based and rare earth-based catalysts, and is suitable for the manufacture of tires and other elastic materials. However, butadiene rubber begins to crystallize at -30°C, resulting in poor elasticity, which limits its use. In order to improve the low-temperature elasticity of butadiene rubber, an appropriate amount of high-cis-isoprene structural units are randomly introduced into the high-cis-polybutadiene macromolecular chain, so that the copolymerized elastomer of butadiene and isoprene It does not crystallize at low temperature (such as: 0 ° C ~ -150 ° C), has excellent low temperature elastic properties, and at ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/00C08F4/54C08F236/06C08F236/08
Inventor 吴一弦赵姜维周为为朱寒
Owner CHINA PETROLEUM & CHEM CORP
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