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Preparation method of polyisobutylene

A technology of polyisobutylene and isobutylene, applied in the field of polyisobutylene preparation, can solve problems such as unavoidable internal double bond products, achieve the effect of simplifying the reaction process and reducing production costs

Active Publication Date: 2009-07-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Therefore, using TiCl 4 Co-initiation of living cationic polymerization of isobutylene cannot obtain highly reactive polyisobutene products in a simple one-step method, and usually only the obtained polyisobutene containing tertiary chlorine terminal groups can be further dehydrochlorinated to obtain highly reactive polyisobutene. , and the internal double bond products are inevitably produced during the dehydrochlorination process

Method used

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  • Preparation method of polyisobutylene

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Experimental program
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Effect test

Embodiment 1

[0021] Under the protection of high-purity nitrogen, add 0.15 mmol of methanol and 1.5 mmol of titanium tetrachloride to 25 mL of isobutene / hexane / dichloromethane monomer solution (the concentration of isobutene is 1.5 mol / L) to initiate polymerization, and react at -30 ° C After 10 min, add 1 mL of 0.1 g / L NaOH / ethanol solution to terminate the reaction, add ethanol to precipitate the polymer, and wash with ethanol repeatedly until it becomes clear and transparent. The monomer conversion rate was 73%, and a highly reactive polyisobutene with a number average molecular weight of 1400, a molecular weight distribution index of 1.6, an α-double bond content of 70%, and a tertiary chlorine end group content of 30% was obtained.

Embodiment 2

[0023] Under the protection of high-purity nitrogen, add 0.4 mmol of methanol and 1.5 mmol of titanium tetrachloride to 25 mL of isobutene / hexane / dichloromethane monomer solution (the concentration of isobutene is 1.5 mol / L) to initiate polymerization, at -30 ° C After reacting for 60 minutes, add 1 mL of 0.1 g / L NaOH / ethanol solution to terminate the reaction, add ethanol to precipitate the polymer, and wash with ethanol repeatedly until it becomes clear and transparent. The monomer conversion rate was 95.7%, and a highly reactive polyisobutene with a number average molecular weight of 1400, a molecular weight distribution index of 1.5, an α-double bond content of 87%, and a tertiary chlorine end group content of 13% was obtained.

Embodiment 3

[0025] Under the protection of high-purity nitrogen, add 0.45 mmol of isopropanol and 3.0 mmol of titanium tetrachloride to 25 mL of isobutene / hexane / dichloromethane monomer solution (the concentration of isobutene is 1.5 mol / L) to initiate polymerization, -30 ° C After reacting for 60 min, add 1 mL of 0.1 g / L NaOH / ethanol solution to terminate the reaction, add ethanol to precipitate the polymer, and wash with ethanol repeatedly until it becomes clear and transparent. The monomer conversion rate was 27.3%, and a highly reactive polyisobutene with a number average molecular weight of 1600, a molecular weight distribution index of 2.3, an α-double bond content of 79%, and a tertiary chlorine end group content of 21% was obtained.

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Abstract

The invention relates to a method for preparing polyisobutene. In a liquid-phase isobutene raw material system, alcohol or ether organic complexes and titanium tetrachloride are used to form an initiating system to initiate isobutene or a hydrocarbon mixture containing isobutene or a compound containing isobutene. Mix the isobutene component in the light C4 fraction for cationic polymerization, and directly prepare the high reactivity with a number average molecular weight of 500-6000 Daltons and a terminal α-double bond content of ≥70% mol, especially greater than 80% mol by one-step method Polyisobutylene products. The initiation system is not only cheap and easy to obtain, but also has high activity and adaptability to raw materials, can simplify the polymerization process and reduce production costs.

Description

technical field [0001] The present invention relates to a kind of method for preparing polyisobutene, especially use the initiation system containing titanium tetrachloride, to isobutene, the hydrocarbon mixture of isobutene or the mixed light C containing isobutene 4 A method for preparing polyisobutene with high reactivity by carbocation polymerization of fractions in liquid phase. Background technique [0002] Lewis acid co-initiated carbocationic polymerization of olefins to prepare polyisobutene (PIB) is a known process. Such Lewis acids are usually halides of aluminium, iron, zinc, titanium, tin, mercury or boron. However, in the process of carbocation polymerization, the stability of the carbocation active center is poor, and a series of side reactions such as monomer chain transfer reaction and intramolecular alkylation reaction are prone to occur, and the reaction is not easy to control. Therefore, the prepared polyisobutene terminal The chemically active α-double...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/10C08F4/16
Inventor 吴一弦叶晓林
Owner BEIJING UNIV OF CHEM TECH
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