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Controllable cation polymerizing method of vinyl monomers

A vinyl monomer and cationic polymerization technology, which is applied in the field of vinyl monomer carbocation controllable polymerization, can solve the problems such as narrowing of the molecular weight of the polymerization product, and achieve the effects of improving the initiation efficiency, reducing the dosage, and reducing the production cost

Active Publication Date: 2011-03-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the disclosed technology, there is no mention of the method of adding 1,1-diphenylethylene and its application to the controlled polymerization method of vinyl monomers in the preparation process of the initiation system, so as to improve the initiation efficiency, reduce side reactions and Narrow the molecular weight of the polymer product

Method used

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  • Controllable cation polymerizing method of vinyl monomers
  • Controllable cation polymerizing method of vinyl monomers
  • Controllable cation polymerizing method of vinyl monomers

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Under the condition of -80℃ and high-purity nitrogen protection, the H 2 O (0.014mmol), AlCl 3 (0.033mmol), dichloromethane (5mL), 1,1-diphenylethylene (0.0033mmol) and triphenylamine (0.0033mmol) were added to the dry initiation system preparation device and mixed evenly to obtain blood red homogeneous transparent triggering system.

[0027] Under the protection of high-purity nitrogen, add 20mL of monomer mixed solution of isobutylene (IB) / n-hexane / dichloromethane to the polymerization reactor (the volume ratio of n-hexane / dichloromethane is 3.2, and the molar concentration of monomer is 0.8mol / L), then add the above-mentioned initiation system, so that in the polymerization system [AlCl 3 ] / [IB]=2.1×10 -3 . After the polymerization reaction at -80° C. for 1 h, a precooled 5 mL NaOH / ethanol mixed solution (the mass fraction of NaOH was 5%) was added to terminate the polymerization. The solvent and unreacted monomers were removed, and the polymer product was obta...

Embodiment 2

[0029] The preparation method, polymerization reaction and post-treatment method of the initiation system are as described in Example 1, but the amount of 1,1-diphenylethylene (0.043mmol) is changed, that is, [1,1-diphenylethylene]:[AlCl 3 ] = 1.3. Polyisobutylene product yield 76%, M n 7.5×10 4 ,M w / M n is 1.8.

Embodiment 3

[0031] The preparation method of the initiation system, the polymerization process and the post-treatment method are as in Example 1, only changing the amount of 1,1-diphenylethylene (0.132mmol), [1,1-diphenylethylene]:[AlCl 3 ]=4. Polyisobutylene product yield is 20%, M n 2.7×10 4 ,M w / M n is 1.7.

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Abstract

The invention relates to a controllable cation polymerizing method, which can be used for cation polymerization of vinyl monomers and preparing polymers of the vinyl monomers. In the invention, Lewis acid is used as a co-initiation system for carrying out the cation polymerization reaction of the vinyl monomers (including isobutene, styrene, a-alkyl styrene or p-alkyl styrene and isoprene) in alkane, halohydrocarbon or a mixed solvent of the alkane and the halohydrocarbon. Generally through adding a proper amount of 1,1-diphenylethylene in the initiation system, the initiation efficiency can be improved effectively, the consumption of initiation initiators and co-initiators can be reduced, and secondary reaction can be reduced so that the molecular weight distribution of polymerisates is obviously narrowed.

Description

Technical field: [0001] The invention relates to a method for the controllable cationic polymerization of vinyl monomers, in particular to a method for the controllable carbocationic polymerization of vinyl monomers. By adding an appropriate amount of 1,1-diphenylethylene during the preparation of the initiation system, it can Effectively improve the initiation efficiency, reduce the amount of initiator and co-initiator, and reduce side reactions, so that the polymer molecular weight distribution is significantly narrowed. Background technique: [0002] Polyisobutylene (PIB) or butyl rubber (copolymer of isobutylene and a small amount of isoprene, IIR) is the largest industrialized product of cationic polymerization, with excellent air tightness, water tightness, oxidation resistance, electrical insulation, chemical Stability, heat resistance, low temperature performance. Its application fields are closely related to its molecular weight. According to different molecular we...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/00C08F2/06C08F10/10C08F12/08C08F12/06C08F36/08
Inventor 吴一弦黄强刘强任慧宁
Owner BEIJING UNIV OF CHEM TECH
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