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Preparation method of isobutene-alkyl styrene random copolymer

A technology of alkyl styrene and random copolymer, which is applied in the field of preparation of isobutylene and alkyl styrene random copolymer, can solve the problems such as difficulty in controlling the activity of the initiating system, and achieves reducing molecular weight distribution, increasing reaction temperature, The effect of increasing molecular weight

Inactive Publication Date: 2016-05-25
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The initiator in the file is directly added to the reaction system without aging, which makes it difficult to control the activity of the initiator system

Method used

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  • Preparation method of isobutene-alkyl styrene random copolymer
  • Preparation method of isobutene-alkyl styrene random copolymer
  • Preparation method of isobutene-alkyl styrene random copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Reactor feed: at -90°C, add 184g of methyl chloride, 40.5g of isobutylene and 2.6g of p-methylstyrene into the reactor, mix well to form a mixed solution; in the mixed solution, isobutene and p-methylstyrene The total mass concentration of allyl styrene is 18.98wt%;

[0038] (2) Initiator system preparation: take 1.8ml trichlorotriethyl aluminum (0.4M) and 1.8ml CH 2 Cl 2 (0.12M) saturated aqueous solution (the main initiator is water), fully mixed (the amount ratio of the main initiator and the co-initiator is 1:3.3), then add 25ml of methyl chloride solvent to dilute, the main initiator after dilution The concentration is 0.0075mol / L, and then aged at -90°C for 5 minutes to form an initiating system;

[0039] (3) Synthesis of random copolymers: at -90°C, squeeze the initiator system into the reactor to initiate polymerization. After 5 minutes of polymerization, add 20ml of pre-cooled methanol to terminate the reaction, and dry in vacuum to obtain isobutylene and...

Embodiment 2

[0041] (1) Reactor feed: At -90°C, add 184g of methyl chloride, 40.5g of isobutylene and 2.6g of p-tert-butylstyrene to the reactor to form a mixed solution. In the mixed solution, isobutylene and p-tert-butyl The total mass concentration of styrene is 18.98wt%; then add 1.5ml ethyl acetate (0.1M) and mix well;

[0042] (2) Initiator system preparation: take 1.8ml trichlorotriethyl aluminum (0.4M) and 1.8ml CH 2 Cl 2 (0.12M) saturated aqueous solution (the main initiator is water), fully mixed (the ratio of the substance of the main initiator and the co-initiator is 1:3.3), then add 25ml of methyl chloride to dilute, the concentration of the main initiator after dilution is 0.0091mol / L, then aged at -90°C for 5min;

[0043] (3) Synthesis of random copolymer: at -90°C, squeeze the initiator system into the reactor to initiate polymerization. After 5 minutes of polymerization, add 20ml of pre-cooled methanol to terminate the reaction, and dry in vacuum to obtain isobutylene an...

Embodiment 3

[0045](1) Reactor feed: At -90°C, add 184g of methyl chloride, 40.5g of isobutylene and 2.6g of m-methylstyrene into the reactor, mix well to form a mixed solution, and the mixture of isobutene and m-methylstyrene in the mixed solution The total mass concentration of allyl styrene is 18.98wt%;

[0046] (2) Initiator system preparation: take 1.8ml trichlorotriethyl aluminum (0.4M) and 1.8ml CH 2 Cl 2 (0.12M) saturated aqueous solution (the main initiator is water), fully mixed (the amount ratio of the main initiator and the co-initiator is 1:3.3), add 25ml methyl chloride and dilute, the concentration of the main initiator after dilution is 0.0091mol / L, then add 1.5ml ethyl acetate (0.1M), the final concentration of ethyl acetate after mixing is 0.0042mol / L, and age at -90°C for 5min to form an initiating system;

[0047] (3) Polymer synthesis: At -90°C, squeeze the initiator system into the reactor to initiate polymerization. After 5 minutes of polymerization, add 20ml of pr...

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Abstract

The invention discloses a preparation method of an isobutene-alkyl styrene random copolymer, and belongs to the technical field of macromolecular copolymer synthesizing methods. The preparation method comprises the steps of reactor feeding, initiator system preparing and polymer synthesizing and particularly comprises the two forms that a third component is added into a reactor along with a monomer raw material or the third component is added into the reactor after being aged together with a coinitiator and a main initiator. According to the preparation method, an ester compound or a ketone compound is taken as the cationic copolymerization third component, therefore, the cationic activity center can be stabilized, the reaction speed can be controlled, the molecular weight of the polymer can be increased, the molecular weight distribution can be reduced, and the reaction temperature can be increased, so that a reaction is performed at the higher temperature to achieve the effects of energy conservation and emission reduction. The property of the synthesized isobutene-alkyl styrene random copolymer is the same as that of a copolymer synthesized at the lower temperature, and the isobutene-alkyl styrene random copolymer can serve as a tire inner liner and a vibration-absorptive material or damping material.

Description

technical field [0001] The invention belongs to the technical field of polymer copolymer synthesis methods, and in particular relates to a preparation method of a random copolymer of isobutylene and alkylstyrene. Background technique [0002] Traditional butyl rubber (IIR) has excellent air tightness, low glass transition temperature, excellent damping and aging resistance, and is widely used in automobiles, biomedicine and other fields. But traditional butyl rubber also has many deficiencies. For example, traditional butyl rubber has poor compatibility with other rubbers, which is not conducive to blending and mixing with other rubbers. Moreover, the molecular chain contains unsaturated double bonds, which are easy to cross-link and cause scorch during the post-processing of rubber. [0003] In the random copolymer of isobutylene and alkylstyrene synthesized by using alkylstyrene as the second monomer, the content of isobutylene structural unit is greater than 90%, which h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/10C08F212/12C08F4/54C08F4/16
CPCC08F210/10C08F212/12C08F4/54C08F4/16
Inventor 伍一波张涛郭文莉李树新杨丹常金杰商育伟张彦
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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