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A kind of titanium tetrachloride co-initiation system and its method for preparing highly reactive polyisobutene

A titanium tetrachloride and co-initiation technology, applied in the field of titanium tetrachloride co-initiation system and its use in the preparation of highly reactive polyisobutylene, can solve the problems of high polymer molecular weight and low initiating activity

Active Publication Date: 2016-08-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

[0022] Under the protection of high-purity nitrogen at -28°C, in 20 mL of a mixed solution containing isobutene, n-hexane, water and HCl ([H 2 O]=0.64mmol / L; [HCl]=40.5mmol / L; [IB]=3.0mol / L) add 3.84mmol 2-phenylethanethiol and 9.6mmol TiCl in sequence 4 , mix well, and then add, so that TiCl 4 with H 2 The molar ratio of O is 750, HCl and TiCl 4 The molar ratio of 2-phenylethanethiol to TiCl is 0.08 4 The molar ratio is 0.4, TiCl 4 The molar ratio to isobutene is 0.16, and the molar ratio of 2-phenylethanethiol to isobutene is 0.066. After 30 min of polymerization reaction, 3 mL of 0.1 g / L 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 70%, number average molecular weight (M n ) is 3200, the molecular weight distrib...

Embodiment 2

[0024] Under the protection of high-purity nitrogen at -32 ° C, in 20 mL of mixed C containing isobutene, butane, butene, water and HCl 4 Fraction ([H 2 O]=0.35mmol / L; [HCl]=40.5mmol / L; [IB]=2.9mol / L) solution was added in sequence of 5.8mmol of 2-phenylethanethiol and 12mmol of TiCl 4 , mixed well so that the TiCl 4 with H 2 The molar ratio of O is 1765, HCl and TiCl 4 The molar ratio of 2-phenylethanethiol to TiCl is 0.07 4 The molar ratio is 0.48, TiCl 4 The molar ratio to isobutene is 0.21, and the molar ratio of 2-phenylethanethiol to isobutene is 0.099. After 40 minutes of reaction, the polymerization was terminated, and the termination method and polymer post-treatment method were the same as in Example 1. The yield of HRPIB is 21%, M n It is 1500, PDI is 1.2, and the terminal α double bond content is 91%.

Embodiment 3

[0026] Under the protection of high-purity nitrogen at -30 ° C, in 20 mL of mixed C containing isobutene, butane, butene, water and HCl 4 Fraction ([H 2 O]=0.35mmol / L; [HCl]=46.5mmol / L; [IB]=1.6mol / L) were added 1.44mmol of n-dodecyl mercaptan and 8mmol of TiCl in sequence 4 , mixed well so that the TiCl 4 with H 2 The molar ratio of O is 1176, HCl and TiCl 4 The molar ratio of n-dodecylmercaptan to TiCl is 0.12 4 The molar ratio is 0.18, TiCl 4 The molar ratio to isobutene is 0.25, and the molar ratio of n-dodecylmercaptan to isobutene is 0.046. Polymerization was terminated after 50 min of reaction, and the termination method and polymer post-treatment method were the same as in Example 1. The yield of HRPIB is 18%, M n It is 2000, PDI is 1.2, and the terminal α double bond content is 89%.

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Abstract

The invention relates to a titanium tetrachloride co-initiation system, and a method for preparing high-reaction-activity polyisobutylene by using it. The system is suitable for the preparation of the high-reaction-activity polyisobutylene through cationic polymerization of isobutene, an isobutene and inert solvent mixed solution or an isobutene-containing mixed light C4 fraction. An organic compound additive can be introduced into the polymerization system to efficiently and selectively remove beta-H on -CH3 adjacent to a carbonium ion at the end of an active chain in order to generate a polyisobutylene chain end alpha-double bond structure, so the high yield and high-reaction-activity polyisobutylene can be directly prepared, and the chain end alpha-double bond content can reaches above 90%.

Description

technical field [0001] The invention relates to a co-initiation system of titanium tetrachloride and a method for preparing polyisobutene with high reactivity by using the co-initiation system to initiate the polymerization of isobutene, especially for isobutene, isobutene inert solvent mixture or mixed light C containing isobutene 4 Cationic polymerization of fractions to prepare highly reactive polyisobutene with terminal α-double bond content of more than 90%. Background technique [0002] The preparation of polyisobutene from isobutene is a typical cationic polymerization reaction. 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. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/10C08F4/16
Inventor 吴一弦郭安儒杨小健徐会超
Owner BEIJING UNIV OF CHEM TECH
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