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

A high-reactivity, polyisobutylene technology is applied in the field of initiating systems for preparing high-reactivity polyisobutylene and its copolymers, and achieves the effects of reducing the formation of tertiary chlorine end groups, wide adjustment range and lowering production costs.

Active Publication Date: 2013-03-13
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, add H 2 O, ethanol and FeCl 3 The initiator system initiates the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [ethanol]=6mmol / L, [FeCl 3 ] = 5 mmol / L. React at 0°C for 10 min, add 1 mL of 0.1 g / L NaOH / C 2 h 5 OH solution to terminate the reaction. The polymer 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 is 42%, number average molecular weight (M n ) is 800, the molecular weight distribution index (M w / M n ) was 1.9, and the terminal α-double bond content was 85%.

Embodiment 2

[0030] Example 2: Under the protection of high-purity nitrogen, add H 2 O, isopropanol and FeCl 3 Initiate the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [isopropanol]=5mmol / L, [FeCl 3 ] = 5 mmol / L. React at 0°C for 10 minutes. 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 isobutylene product is 1300, molecular weight distribution index (M w / M n ) was 2.1, and the terminal α-double bond content was 87%.

Embodiment 3

[0031] Example 3: Under the protection of high-purity nitrogen, add H 2 O, butanone and FeCl 3 Initiate the polymerization of isobutylene, where [H 2 O]=1.1mmol / L, [butanone]=4.8mmol / L, [FeCl 3 ] = 5 mmol / L. React at 0°C for 10 minutes. Termination and post-processing methods are the same as in Example 1. The yield of polyisobutylene product is 62%, M n for 850, M w / M n is 2.1. The isobutene product has a terminal α-double bond content of 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. The repeatability is high. The environmental pollution is light. And the industrial application is easy.

Description

technical field [0001] The invention relates to an initiation system for preparing highly reactive polyisobutylene and its copolymers, in particular to an initiating system containing FeCl 3 The initiator system composed of compounding agent is used for cationic polymerization of isobutene and isobutene hydrocarbon mixture to prepare highly reactive polyisobutene and its copolymers. It can prepare polyisobutene terminal α-double bond content higher than 75mol%, especially It is a highly reactive polyisobutylene and its copolymer with a number average molecular weight of 500-6000 g / mol. Background technique [0002] Isobutene (IB) can be prepared by cationic polymerization polyisobutene (PIB). According to different chain termination methods, after the deprotonation reaction at the end of the polyisobutylene molecular chain, it can generally generate: α-double bond (exo-olefin), β-double bond (endo-olefin). [0003] [0004] Wherein R is the head end group, such as hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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