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Method for synthesizing cyclopentadiene polymer

A cyclopentadiene and polymer technology, applied in the field of cyclopentadiene polymer synthesis, can solve the problem of low number-average molecular weight of cyclopentadiene homopolymers and copolymers, and little research on the detailed mechanism of co-catalysts , The research on the synthesis of new cyclopentadiene copolymers and the research on their properties are few problems, so as to achieve the effect of single component and clear structure

Active Publication Date: 2007-05-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main problems in the prior art are: (1) cyclopentadiene homopolymerization and copolymer number-average molecular weight are relatively low
(2) There is little research on the detailed mechanism of action of cocatalysts
(3) There are few studies on the synthesis and properties of cyclopentadiene-based new copolymers

Method used

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  • Method for synthesizing cyclopentadiene polymer
  • Method for synthesizing cyclopentadiene polymer
  • Method for synthesizing cyclopentadiene polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Replace the fully dried 100 ml polymerization reaction bottle with nitrogen twice under normal pressure, maintain the nitrogen atmosphere, add 0.05 moles of cyclopentadiene monomer, add 0.005 moles of methyl aluminoxane at -84 ° C, and keep - 84 DEG C reacted for 10 minutes, then added 20 milliliters of concentration and was 5% hydrochloric acid ethanol solution to terminate the reaction, and the polymer yield was 77%, and only contained 1,2- and 1, two kinds of chain structural units of 1,4-structure in the polymer, Wherein the 1,2-structure content is 50% ( 1 HNMR spectrogram analysis results, see accompanying drawing 1), number average molecular weight 32000.

Embodiment 2

[0025] Replace the fully dried 100 ml polymerization reaction bottle with nitrogen twice under normal pressure, maintain the nitrogen atmosphere, add 0.05 moles of cyclopentadiene monomer, add 0.005 moles of methyl aluminoxane at -84 ° C, and keep - 84 DEG C reacted for 12 hours, then added 20 milliliters of concentration and was 5% hydrochloric acid ethanol solution to terminate the reaction, and the polymer yield was 97%, and only contained 1,2- and 1, two kinds of chain structural units of 1,4-structure in the polymer, Among them, the 1,2-structure content is 57%, and the number average molecular weight is 43000.

Embodiment 3

[0027] Replace the fully dried 100 ml polymerization reaction bottle with nitrogen twice under normal pressure, maintain the nitrogen atmosphere, add 0.1 mole of cyclopentadiene monomer, 15 ml of toluene, and add 0.01 mole of methyl aluminoxane at 15 °C , keep the reaction at 15°C for 7 hours, then add 20 milliliters of 5% ethanol hydrochloric acid solution to terminate the reaction, the polymer yield is 45%, and the polymer only contains two chain structures of 1,2- and 1,4-structure unit, wherein the 1,2-structure content is 40%, and the number average molecular weight is 31000.

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Abstract

This invention relates to a synthesis method for cyclopentadienes polymers, involving an alkyl aluminoxane catalyst used for homopolymerization of cyclopentadienes monomers and copolymerization of cyclopentadienes monomers and styrene, norbornene and its derivatives. The polymerization catalyst is the single component of alkyl aluminoxane, including a C1-C4 alkyl, such as methylaluminoxane, triisobutylaluminoxane, methyl isobutyl aluminoxane or ethoxy diethyl aluminoxane. It can be a single catalyst, or a composite catalyst or a carried product. The catalyst component is single and easy to get, and the structure of the cyclopentadienes copolymer is clear, mainly as the two structural units of 1, 2-and 1, 4-chain structure. The copolymers of cyclopentadienes monomers and styrenes or norbornenes monomers can be obtained. Polymerization and copolymerization reaction rate and product structure can be controlled through regulating alkyl aluminoxane content, monomer concentration, solvents, polymerization temperature and time, etc. factors.

Description

technical field [0001] The present invention relates to the synthesizing method of cyclopentadiene type polymer, particularly a kind of alkyl aluminoxane catalyst is used for the homopolymerization of cyclopentadiene type monomer and cyclopentadiene type monomer and styrene, norbornanol Copolymerization of alkenes and their derivatives. Background technique [0002] At present, the synthesis of cyclopentadiene polymer is mainly by adding catalyst to cyclopentadiene monomer to initiate addition polymerization reaction. The catalyst used mainly includes Friedel-Crafts catalyst, such as: AlCl 3 , BF 3 , Oet 2 etc., cationic salt catalyst, such as: (C 6 h 5 ) 3 C+SbCl6-, etc., and transition metal coordination compound catalysts, including Pb, W, Ti, Mo, Mn, Fe, Cr, Ni, Cu, Zn, Co and other metal coordination compounds, metallocene catalysts and post-transition non- metallocene catalysts, etc. Metallocene catalysts and late-transition non-metallocene catalysts generally u...

Claims

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Application Information

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IPC IPC(8): C08F132/06C08F4/52
Inventor 林如海孙文华张东恒张德顺常飞王淑兰侯俊先乔福来袁大辉包世星刘忠恩刘枫林田炳全衣学飞孙建林白玉洁谢文华张艳丽张立军关伟宏任淑珍王秀文刘卫东
Owner PETROCHINA CO LTD
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