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Method for preparing butyl rubber by catalytic polymerization

A butyl rubber, catalytic polymerization technology, applied in the field of butyl rubber prepared by catalytic polymerization, can solve problems such as difficulty in using homogeneous polymerization, instability, etc.

Active Publication Date: 2012-10-17
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are certain risks in the reaction process of water and alkyl aluminum halides at room temperature, and the catalyst composition formed at the same time is a heterogeneous mixture, which is unstable and not easy to use for homogeneous polymerization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The method of Comparative Example 1 was repeated, except that the reaction flask containing the catalyst solution I was cooled to -20°C, and under stirring, 0.001 ml of water was added dropwise to the reaction flask, so that the water was quickly dispersed into the solution to form fine particles. After the addition of ice crystals, the reaction flask was reacted at room temperature for 2 hours to form a homogeneous catalyst composition III, which was used immediately. 1.8 ml of catalyst composition III was used to initiate the reaction. The polymer yield was 39.6%, Mn=226900, Mw=567400, and the mole fraction of isoprene in the rubber was 1.9.

Embodiment 2

[0021] The procedure of Example 1 was repeated except that the reaction time to form a homogeneous catalyst composition IV was 24 hours and 1.8 ml of catalyst composition IV was used to initiate the reaction. The polymer yield was 39.6%, Mn=226700, Mw=567300, and the mole fraction of isoprene in the rubber was 1.9.

Embodiment 3

[0023] The method of Example 1 was repeated, except that 0.0015 ml of water was added dropwise to the reaction flask to form a homogeneous catalyst composition VI. 1.8 ml of catalyst composition VI was used to initiate the reaction. The polymer yield was 52.8%, Mn=211800, Mw=508300, and the mole fraction of isoprene in the rubber was 2.1.

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PUM

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Abstract

The invention relates to a method for preparing butyl rubber by catalytic polymerization. The method comprises the following steps: contacting an isobutene monomer with an isoprene monomer at the temperature of minus 75 DEG C-minus 50 DEG C in the presence of an aliphatic series hydrocarbon diluent and a catalyst composite so as to carry out a cationic polymerization reaction, wherein the amount of added isobutene is 80-85% of the total volume, and the weight of added isoprene is 2.90-2.97% of that of isobutene, the allowance is the aliphatic series hydrocarbon diluent based on volume, the content of aluminium diethyl monochloride in the added catalyst composite is 0.13-0.23% of the mass of isobutene, the addition weight of ethylaluminum dichloride is 8.2% of that of aluminium diethyl monochloride, and the addition mass of water is 10-16% of that of the added diethylaluminum. The catalyst composite is stable in property, and butyl rubber with high dialkene content and molecular weightis formed at the polymerization reaction rate.

Description

technical field [0001] The invention relates to a method for preparing butyl rubber by catalytic polymerization with a cationic polymerization catalyst composition. Background technique [0002] Almost all butyl rubber production worldwide uses methyl chloride as a diluent. Methyl chloride can cause liver, kidney, nervous system and central nervous system damage. The search for alternative reaction medium in butyl rubber has been paid much attention. The method of producing butyl rubber in hydrocarbon solvent (such as hexane) has become an important direction in the research and development of butyl rubber. Combining this method with the method for producing halogenated butyl rubber, the dissolving step can be omitted, and it has a good application prospect. [0003] The method for producing butyl rubber in a hydrocarbon solvent such as hexane (solution butyl method) mainly employs an aluminum trihalide catalyst system. As described in US Pat. Nos. 2,844,569 and 2,772,25...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/12C08F4/52
Inventor 张红江王硕蔡小平陈可佳李秀梅陈万友李江利
Owner PETROCHINA CO LTD