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Method for preparing polyisobutylene with high reaction activity

A high-reactivity, polyisobutylene technology, applied in the field of preparation of high-reactivity polyisobutylene, can solve problems such as equipment corrosion and damage, achieve the effects of reducing acidity, increasing the content of α-double bonds, and reducing the possibility

Active Publication Date: 2009-12-30
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When the polymerization product of fluorine-containing impurities is used to synthesize fuel additives or lubricating oil additives, and is further applied to the engine, HF will be released to cause corrosion damage to equipment

Method used

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  • Method for preparing polyisobutylene with high reaction activity

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Under the protection of high-purity nitrogen, add 0.62 mmol of 2-ethylhexanol and 0.44 mmol of AlCl to 20 ml of a solution containing isobutene (IB) and dichloromethane ([IB]=2.0 mol / L) 3 The complex initiates the polymerization of isobutylene, reacts at 0°C for 20min, and adds 1ml of 0.1g / 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. IB conversion was 46%. The number-average molecular weight of polymerization product 2700g / mol, molecular weight distribution index (M w / M n ) was 1.9, and the terminal α-double bond content was 90%.

Embodiment 2

[0021] Under the protection of high-purity nitrogen, add 0.66mmol of 2-ethylbutanol and 0.44mmol of AlCl to the solution of 20ml of IB and methylene chloride ([IB]=2.0mol / L) 3 The complex initiates the polymerization of isobutylene, reacts at 0°C for 20min, adds 1ml of 0.1g / 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. IB conversion was 45%. The number-average molecular weight of polymerization product 1800g / mol, molecular weight distribution index (M w / M n ) was 1.8, and the terminal α-double bond content was 92%.

Embodiment 3

[0023] Under the protection of high-purity nitrogen, add 0.57mmol of n-hexanol and 0.44mmol of AlCl to the solution of 20ml of IB and dichloromethane ([IB]=2.0mol / L) 3 The complex initiates the polymerization of isobutylene, reacts at 0°C for 20min, adds 1ml of 0.1g / 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 IB conversion rate was 42. The number average molecular weight of the polymerized product was 1700 g / mol, and the terminal α-double bond content was 80%.

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Abstract

The invention provides a method for preparing polyisobutylene with high reaction activity. In a polymerization system of a liquid-phase isobutylene raw material, the polymerization of isobutylene is initiated by adopting a complex catalyst consisting of AlCl3 and oxygen-containing organic compound complex, wherein the organic compound complex is one or mixture of more than one of alcohol compounds of 6 to 12C; and the adopted complex catalyst initiation system can effectively control the polymerization of the isobutylene and selectively remove protons so as to remarkably improve the content of polyisobutylene terminal alpha-double bonds, and has narrow molecular weight distribution. The content of chain terminal alpha-double bonds is generally improved to over 80 mol percent, and the majority reaches over 90 mol percent; and the number-average molecular weight of the prepared polyisobutylene with the high reaction activity is 800 to 5,000 Dalton. The method for preparing the polyisobutylene with high activity has the advantages of simple production process, good repeatability and low production cost, and is easy for industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of highly reactive polyisobutene, especially for isobutene, hydrocarbon mixture of isobutene or mixed light C containing isobutene 4 A method for preparing polyisobutene with high reactivity by carbocation polymerization of fractions in liquid phase. The high reactivity polyisobutene with the terminal α-double bond content of the polyisobutene higher than 80 mol % and the number average molecular weight of 800-5000 Daltons can be prepared. Background technique [0002] Due to the chemical structure characteristics, polyisobutene (PIB) can only be prepared from isobutene (IB) through cationic polymerization process, and the terminal α-double bond content in polyisobutene molecular chain is the most important quality standard in reactive polyisobutene products, usually The polyisobutene whose terminal α-double bond content is less than 10mol% is called ordinary polyisobutene; when its termina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/10C08F4/14
Inventor 吴一弦刘强张瑜
Owner BEIJING UNIV OF CHEM TECH
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