Method for preparing isobutylene block copolymer by sequential initiation

A technology of block copolymer and isobutylene, applied in the field of preparation of block copolymer, can solve the problems of increased cost, complicated process, inability to realize active polymerization, etc.

Inactive Publication Date: 2004-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, since polyisobutene is insoluble in chlorinated hydrocarbon solvents such as chloromethane and methylene chloride, which are commonly used in cationic polymerization, at the temperature of cationic polymerization, the activity cannot be achieved in good solvents of polyisobutene (such as linear alkanes and aromatic hydrocarbons). Polymerization, so mixed solvents must be used
The existence of these problems greatly increases the cost, and at the same time complicates the process, especially the recovery and reprocessing

Method used

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  • Method for preparing isobutylene block copolymer by sequential initiation
  • Method for preparing isobutylene block copolymer by sequential initiation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 30ml of methyl chloride to a dry nitrogen-filled reactor, and then add about 60mg of n-Bu 4 N + Cl - , 2.06 g p-methylstyrene, 18 μl 1-phenylethyl chloride, the reaction mixture was cooled to -40 °C, and then 50 μl SnCl was added 4 Start the first phase of aggregation. After 1 hour of polymerization reaction, a small amount of sample was taken to determine the relative molecular mass of poly-p-methylstyrene. Then add 2.04g of isobutene, cool to -80°C, add 0.2ml of AlEt 2 Cl (10M hexane solution) for the second stage of polymerization. After 30 minutes of polymerization, 2 ml of methanol was added to terminate the polymerization, the polymer was precipitated with methanol, and about 4.0 g of the polymer was obtained after drying. The number average relative molecular mass measured by GPC was 19200 (MWD=1.46) for poly-p-methylstyrene, and 36600 (MWD=1.42) for poly-p-methylstyrene-b-polyisobutylene.

Embodiment 2

[0038] Add 20ml of methyl chloride to a dry nitrogen-filled reactor, then add about 25mg of n-Bu 4 N + Cl - , 1.5 g p-methylstyrene, 15 μl 1-phenylethyl chloride, the reaction mixture was cooled to -40 °C, and then 50 μl SnCl was added 4 The first stage of polymerization was started and the polymerization was carried out for 1 hour. Then add 1.8g of isobutene and 18 mg of divinylbenzene, cool to -80°C, add 0.1ml of AlEt 2 Cl (10M hexane solution) for the second stage of polymerization. After 30 minutes of polymerization, 2 ml of methanol was added to terminate the polymerization, the polymer was precipitated with methanol, and about 3.2 g of the polymer was obtained after drying. There are about 10% cyclohexane insoluble matter in the polymer product, and the number-average relative molecular mass of the soluble part measured by GPC is 25300 (MWD=4.13), and the GPC spectrum shows double peaks. This indicates that the poly(isobutylene-co-divinylbenzene) part has undergone ...

Embodiment 3

[0040] Add 30ml of dichloromethane into a dry nitrogen-filled reactor, and then add about 25mg of n-Bu 4 N + Cl - , 1.8 g styrene, 15 μl 1-phenylethyl chloride, the reaction mixture was cooled to -40 °C, and then 200 μl SnCl was added 4 The first stage of polymerization was started and the polymerization was carried out for 4 hours. Then add 1.8g of isobutylene and 100 mg of p-methylstyrene, cool to -80°C, add 0.1ml of AlEt 2 Cl (10M hexane solution) for the second stage of polymerization. After 30 minutes of polymerization, 2 ml of methanol was added to terminate the polymerization, the polymer was precipitated with methanol, and about 3.67 g of polymer was obtained after drying. The number average relative molecular mass measured by GPC is 35300 (MWD=1.65), 1 The p-methylstyrene content of the polyisobutylene block determined by H-NMR was about 5.2% by weight.

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Abstract

The present invention provides a method for preparing isobutene block copolymer by adopting sequence initiation. Said method successively includes the following steps: (1) first-stage polymerization: making styrene monomer (monomer A) implement 'controllable' or 'active' cationic homopolymerization or copolymerization; and (2) second-stage polymerization: using isobutene as monomer, using polymerization product of first-stage as macromolecular initiator, adding a novel Lewis acid as coinitiator and making homopolymerization of isobutene; or using isobutene as monomer, using polymerization product of first stage as macromolecular initiator, adding a novel Lewis acid as coinitiator and making copolymerization of copolymerization monomer of isobutene so as to obtain the invented block copolymer.

Description

technical field [0001] The present invention relates to a kind of preparation method of block copolymer, more specifically, the present invention relates to the cationic polymerization method of the block copolymer of preparation styrenic monomer and isobutylene, the isobutylene block copolymer prepared by this method and its functional derivatives. Background technique [0002] Block copolymers are a class of copolymers with a definite sequence structure and properties different from random copolymers. Each block in the copolymer has similar physical and mechanical properties to its homopolymer. Block copolymers are widely used as dispersants, surfactants, compatibilizers and thermoplastic elastomers. [0003] The preparation of block copolymers, especially copolymers containing polyisobutylene segments, by living cationic polymerization has been disclosed as follows. [0004] U.S. Patent No. 5,428,111 discloses a method for preparing isobutylene block copolymers, the me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F297/00
Inventor 马育红杨万泰武冠英
Owner CHINA PETROLEUM & CHEM CORP
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