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Initiating system for preparing high-reaction activity polyisobutene and copolymer of polyisobutene

A technology of high reactivity and initiation system, which is applied in the field of preparation of initiation system of high reactivity polyisobutylene and its copolymers, to achieve the effects of reducing the formation of tertiary chlorine end groups, wide adjustment range and reducing production cost

Active Publication Date: 2011-01-26
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

FeCl is not currently used 3 Co-initiated cationic polymerization of isobutene, one-step direct access to highly reactive polyisobutene and its copolymers reported in the literature

Method used

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  • Initiating system for preparing high-reaction activity polyisobutene and copolymer of polyisobutene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Under the protection of high-purity nitrogen, to 20 mL of a solution containing isobutylene (IB) and dichloromethane ([IB]=2.0mol / L) was added H 2 O, ethanol and FeCl 3 The initiation system initiates the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [ethanol]=6mmol / L, [FeCl 3 ]=5mmol / L. React for 10min at 0℃, add 1mL 0.1g / L NaOH / C 2 H 5 The OH solution terminates the reaction. The polymerized product was precipitated with ethanol, washed repeatedly with deionized water and ethanol, and finally dried in a vacuum oven at 40°C for 24 hours to remove volatile impurities. The yield of polyisobutylene product was 42%, and the number average molecular weight (M n ) Is 800, and the molecular weight distribution index (M w / M n ) Is 1.9, and the terminal α-double bond content is 85%.

Embodiment 2

[0030] Example 2: Under the protection of high-purity nitrogen, H was added to 20 mL of a solution containing isobutylene (IB) and dichloromethane ([IB]=2.0mol / L) 2 O, isopropanol and FeCl 3 Initiate the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [isopropanol]=5mmol / L, [FeCl 3 ]=5mmol / L. React for 10 min at 0°C. The termination and post-processing methods are the same as in Example 1. The yield of polyisobutylene product was 39%. The number average molecular weight of the isobutylene product is 1300, and the molecular weight distribution index (M w / M n ) Is 2.1 and the terminal α-double bond content is 87%.

Embodiment 3

[0031] Example 3: Under the protection of high-purity nitrogen, add H to 20 mL of a solution containing isobutylene (IB) and dichloromethane ([IB]=2.0mol / L) 2 O, butanone and FeCl 3 Initiate the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [Butanone]=4.8mmol / L, [FeCl 3 ]=5mmol / L. React for 10 min at 0°C. The termination and post-processing methods are the same as in Example 1. The yield of polyisobutylene product is 62%, M n 850, M w / M n Is 2.1. The terminal α-double bond content of the isobutylene product is 89%.

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Abstract

The invention relates to an initiating system for preparing high-reaction activity polyisobutene and a copolymer of polyisobutene, which comprises an initiator for initiating the cationic polymerization of an isobutene-containing material, a coinitiator and a compounding ingredient, wherein the coinitiator is FeCl3; the compounding ingredient is an oxygen- or sulfur-containing organic compound; the molar mixing ratio of the FeCl3 and the isobutene raw material ranges from 0.01 to 3.0; the molar mixing ratio of the initiator to the FeCl3 ranges from 0.1 to 2.0; and the molar mixing ratio of the compounding ingredient to the FeCl3 ranges from 0.1 to 3.4. In the invention, the FeCl3 is used as the compounding ingredient to be compounded with the oxygen- or sulfur-containing compounding ingredient to promote a reaction for removing active central carbocations beta-H, thus the high-reaction activity polyisobutene and the copolymer of polyisobutene, which have terminal alpha-double bond content of more than 75mol percent (even over 90 percent) and narrow molecular weight distribution, can be obtained by a one-step method. The process steps are simplified. The production cost is low. Therepeatability is high. The environmental pollution is light. And the industrial application is easy.

Description

Technical field [0001] The invention relates to an initiating system for preparing high-reactivity polyisobutylene and its copolymers, in particular to an initiation system containing FeCl 3 Initiation system composed of compounding agent and used for cationic polymerization of isobutylene and isobutylene hydrocarbon mixture to prepare high-reactivity polyisobutylene and its copolymers. It can prepare polyisobutylene with a terminal alpha-double bond content of more than 75mol%, especially It is a highly reactive polyisobutylene and its copolymers with a number average molecular weight of 500 to 6000 g / mol. Background technique [0002] Isobutylene (IB) can be prepared from polyisobutylene (PIB) by cationic polymerization. According to different chain termination methods, the proton removal reaction at the end of the polyisobutylene molecular chain generally produces: α-double bond (exo-olefin), β-double bond (endo-olefin). [0003] [0004] Where R is the head group, such as hydr...

Claims

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Application Information

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IPC IPC(8): C08F10/10C08F4/26
Inventor 吴一弦刘强严鹏飞
Owner BEIJING UNIV OF CHEM TECH
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