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Preparation method for polyisobutylene with high reaction activity

A high-reactivity, polyisobutylene technology, applied in the field of preparation of high-reactivity polyisobutylene, can solve the problems of high polymer molecular weight, low initiation activity, complicated process, etc., achieve stable production process and product quality, reduce isomerization and the effect of side reactions such as rearrangement

Inactive Publication Date: 2014-08-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In US5122572 and US5169914, it is proposed to use a tertiary alkyl compound as an initiator and a Lewis acid (boron trifluoride or titanium tetrachloride) as a co-initiator. Highly reactive polyisobutene can only be obtained after further removal of hydrogen chloride, the process is complicated, and the process of removing hydrogen chloride will inevitably produce by-products containing internal double bonds
CN101062962A discloses the use of alcohols or ether organic compounds as complexing agents and TiCl 4 A complex catalyst is formed to initiate the polymerization of isobutylene, wherein the selected alcohol complexing agent is selected from C 1 ~C 3 Alcohols, such as: methanol, ethanol, propanol; ether complexing agents only selected from C 3 ~C 4 Ethers, such as: methyl ethyl ether and diethyl ether, can directly prepare HRPIB, but for non-polar polymerization systems, usually the initiation activity is low and the molecular weight of the polymer is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under the protection of high-purity nitrogen at -32°C, in 20 mL of a mixed solution containing isobutene, n-hexane, dichloromethane and water ([H 2 O]=0.95mmol / L; [IB]=2.3mol / L) add 5.0mmol of cyclopentanol, mix well, then add 9.6mmol of TiCl 4 , so that TiCl 4 with H 2 The molar ratio of O is 510, cyclopentanol and TiCl 4 The molar ratio is 0.52, H 2 The molar ratio of O to isobutene is 4.1×10 -4 , TiCl 4 The molar ratio to isobutene was 0.21. After 60 min of polymerization reaction, 1 mL of 0.1 gL NaOH / ethanol solution was added to terminate 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 obtain a highly reactive polyisobutylene (HRPIB) product. The yield of HRPIB is 84%, number average molecular weight (M n ) is 2800, the molecular weight distribution index (PDI) is 1.9, and the terminal α double bond content is 75%.

Embodiment 2

[0022] At -30°C and under the protection of high-purity nitrogen, in 20mL of mixed C containing isobutene, butane, butene and water 4 Fraction ([H 2 O] = 0.7mmol / L; [IB] = 3.0mol / L) in the solution followed by 9.6mmol of isoamyl alcohol, and 9.6mmol of TiCl 4 , mixed well so that the TiCl 4 with H 2 The molar ratio of O is 738, isoamyl alcohol to TiCl 4 The molar ratio is 1.0, H 2 The molar ratio of O to isobutene is 2.3×10 -4 , TiCl 4 The molar ratio to isobutene was 0.16. The polymerization was terminated after 60 min of reaction. Termination method and polymer post-treatment method are the same as in Example 1. The yield of HRPIB is 75%, M n It is 1700, PDI is 1.5, and the terminal α double bond content is 75%.

Embodiment 3

[0024] Under the protection of high-purity nitrogen at 0°C, in 20 mL of a mixed solution containing isobutene, water and n-hexane ([H 2 O]=0.45mmol / L; [IB]=3.0mol / L) were added in turn 6.7mmol of isoamyl alcohol and 9.6mmol of TiCl 4 , mixed well so that the TiCl 4 with H 2 The molar ratio of O is 1050, isoamyl alcohol and TiCl 4 The molar ratio is 0.7, TiCl 4 The molar ratio to isobutene is 0.16, H 2 The molar ratio of O to isobutene is 1.5×10 -4 . The polymerization was terminated after 40 min of reaction. Termination method and polymer post-treatment method are the same as in Example 1. The yield of HRPIB is 73%, M n It is 2300, PDI is 1.8, and the terminal α double bond content is 75%.

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Abstract

The invention relates to a preparation method for polyisobutylene with high reaction activity, and the method is especially suitable for carbocation polymerization of isobutylene, an alkane mixture of isobutylene or a mixed light C4 fraction containing isobutylene to prepare polyisobutylene with high reaction activity. According to the method, in the presence of an organic compound of alcohol, phenol and / or ether, isobutylene cationic polymerization can be co-initiated by TiCl4 to prepare the polyisobutylene with high reaction activity, and by adjusting the proportion of alcohol, phenol or ether and the counter-ion steric hindrance, the polyisobutylene with high reaction activity can be obtained directly. The method can improve the conversion rate, increase the content of the polyisobutylene chain end alpha-double bond to over 90%, and lower the molecular weight distribution, with the distribution index reaching 1.2, thereby improving the product quality.

Description

technical field [0001] The invention relates to a preparation method of highly reactive polyisobutene, especially suitable for isobutene, alkane mixture of isobutene or mixed light C containing isobutene 4 The distillate was subjected to carbocationic polymerization to prepare highly reactive polyisobutene. Background technique [0002] Polyisobutene is a product obtained by carbocationic polymerization of isobutene (IB). In the cationic polymerization reaction, the carbocations at the end of the active chain are unstable, and a series of side reactions such as removal of β-H, transfer to monomers or other substances, and intramolecular isomerization are prone to occur. Therefore, the prepared polyisobutene terminal α- The double bond content is usually less than 10% (mol), known as ordinary polyisobutylene (referred to as PIB). Only by changing the nature of the counterion around the active chain-terminal carbocation, resulting in a chain-terminal -CH 3 The efficient and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/10C08F210/10C08F4/16
Inventor 吴一弦杨小健郭安儒严鹏飞
Owner BEIJING UNIV OF CHEM TECH
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