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Catalyst system and preparation method for norbornene and isoprene copolymer

A technology of isoprene and norbornene, applied in the field of norbornene-isoprene copolymer and its preparation, can solve the problems of unavailable materials and few related researches, and achieve narrow molecular weight distribution and monomer conversion The effect of high rate and single active center

Inactive Publication Date: 2013-05-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among them, the cationic or free radical polymerization method, due to the rearrangement and chain transfer reactions in the polymerization, obtains low molecular weight oligomers (molecular weight <1000) connected at the 2-, 7-position, which cannot be used as materials, and related researches are relatively limited. few

Method used

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  • Catalyst system and preparation method for norbornene and isoprene copolymer
  • Catalyst system and preparation method for norbornene and isoprene copolymer
  • Catalyst system and preparation method for norbornene and isoprene copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Under the protection of argon, add 1ml norbornene toluene solution (concentration 0.4g / ml) and 0.7ml isoprene toluene solution (concentration 0.4g / ml), the ratio of norbornene to isoprene monomer is 1:1. Under the protection of argon, inject 0.26×10 -5 mol of triisobutylaluminum and 0.53×10 -6 mol of TiCl 4 , fill the polymerization bottle with argon gas, seal it, and put it in a 40°C water bath for 6 hours of polymerization. After the reaction, add acidified industrial alcohol (containing 5% HCl) to terminate the reaction, and precipitate the product. Dry to constant weight in a vacuum drying oven; the yield of copolymer is 87%, and the molecular weight is 3.4×10 4 g / mol, molecular weight distribution index 2.6, norbornene structure content 49mol%.

Embodiment 2

[0026] Under the protection of argon, add 1ml norbornene toluene solution (concentration 0.4g / ml) and 0.7ml isoprene toluene solution (concentration 0.4g / ml), the ratio of norbornene to isoprene monomer is 1:1. Under the protection of argon, inject 0.26×10 -5 mol of triisobutylaluminum and 0.52×10 -6 mol of TiCl 4 , fill the polymerization bottle with argon gas, seal it, and put it in a 40°C water bath for 6 hours of polymerization. After the reaction, add acidified industrial alcohol (containing 5% HCl) to terminate the reaction, and precipitate the product. Dry to constant weight in a vacuum oven; the yield of the copolymer is 75%.

Embodiment 3

[0028] Under the protection of argon, add 1ml norbornene toluene solution (concentration 0.4g / ml) and 0.7ml isoprene toluene solution (concentration 0.4g / ml), the ratio of norbornene to isoprene monomer is 1:1. Under the protection of argon, inject 0.52×10 -5 mol of triisobutylaluminum and 0.52×10 -6 mol of TiCl 4 , fill the polymerization bottle with argon gas, seal it, and put it in a 40°C water bath for 6 hours of polymerization. After the reaction, add acidified industrial alcohol (containing 5% HCl) to terminate the reaction, and precipitate the product. Dry to constant weight in a vacuum oven; yield of copolymer is 52%.

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Abstract

The invention discloses a catalyst system and a polymerization method for preparing norbornene and isoprene copolymer under the existence of titanium catalyst and Lewis acid by means of coordination polymerization. The composition of the polymerization catalyst system is simple, the yield of the obtained copolymer can be as high as about 90 percent, and the composition structure of the copolymer can be controlled within a certain range by changing polymerization conditions. By means of copolymerization, a product, the structure and properties of which are different from the structures and properties of homopolymer and two types of homopolymer blends, can be obtained, and promises to be applied as a novel material.

Description

technical field [0001] The invention relates to a copolymer of norbornene and isoprene and a preparation method thereof. Background technique [0002] Bicyclo[2,2,1]hept-2-ene (norbornene) has the following three polymerization methods: ring-opening metathesis polymerization, addition polymerization and cationic or free radical polymerization (Scheme1). [0003] [0004] Among them, the cationic or free radical polymerization method, due to the rearrangement and chain transfer reactions in the polymerization, obtains low molecular weight oligomers (molecular weight <1000) connected at the 2-, 7-position, which cannot be used as materials, and related researches are relatively limited. few. The first report on the polymerization of norbornene was in 1954, and Andersen and Merkling of DuPont used TiCl 4 / LiAlR 4 The ring-opening metathesis polymerization of norbornene was carried out in the system to obtain a polymer with double bonds in the main chain. With the in-d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F232/08C08F236/08C08F4/642
Inventor 倪旭峰李欣沈之荃
Owner ZHEJIANG UNIV