Uniform structure type polyisobutylene random copolymer and preparation method thereof

A polyisobutylene-based, random copolymer technology, applied in the field of isobutylene copolymer synthesis, can solve problems such as large difference in reactivity ratio, unstable product performance, and uneven copolymer structure, and achieves reduction of heat generation and prevention of glue The effect of particle bonding and control of polymerization rate

Active Publication Date: 2017-03-22
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The activity of these styrene derivatives is much greater than that of isobutylene. In the process of copolymerization, styrene derivatives are more likely to be polymerized first, and it is easy to form a homopolymer, resulting in a heterogeneous structure of the copolymer.
For example, in the copolymerization process of isobutylene and p-methylstyrene, compare the reactivity ratios of isobutylene and p-methylstyrene, the former reactivity ratio r 1 =0.99, the latter reactivity rate r 2 = 1.43, the reactivity ratios of the two have a large difference, which will easily lead to the formation of homopolymerized segments in the copolymerization process of p-methylstyrene, making the product performance unstable

Method used

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  • Uniform structure type polyisobutylene random copolymer and preparation method thereof
  • Uniform structure type polyisobutylene random copolymer and preparation method thereof
  • Uniform structure type polyisobutylene random copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At -95°C, add 184g of methyl chloride, 40.5g of isobutylene and 26g of p-methylstyrene into the reactor, and mix well. The concentration of isobutylene monomer is 16.2wt%, and the content of p-methylstyrene is 10.4wt%. . Take 1.8ml trichlorotriethyldialuminum chloride solution (0.4M), 1.8mg water and 2.2ml ethanol solution (0.1M) in methyl chloride solution (0.1M), mix and configure it as an initiating system, then add 25ml methyl chloride solution to dilute, in- Low-temperature aging at 95°C for 5 minutes. Squeeze the aged initiator system into the reactor to initiate polymerization, the polymerization time reaches 69 hours sticking to the kettle, add 20ml of pre-cooled methanol to terminate the reaction, and vacuum dry. The number average molecular weight was 320000 g / mol.

[0030] Such as figure 1 As shown, in the synthesis process of polyisobutylene-based random copolymer, under the same conditions, without adding the third component, the exothermic heat is parti...

Embodiment 2

[0033]At -95°C, add 184g of methyl chloride, 40.5g of isobutylene and 26g of p-tert-butylstyrene to the reactor, then add 1.5ml of ethanol in methyl chloride solution (0.1M), mix well, and the concentration of isobutylene monomer is 12.43wt%, and the content of p-tert-butylstyrene is 13wt%. Take 1.8ml of trichlorotriethyldialuminum chloride solution (0.4M) and 3.89mg of water, mix to configure the initiation system, then add 25ml of methyl chloride to dilute, and age at -95°C for 5min at low temperature. Squeeze the aged initiator system into the reactor to initiate polymerization, the polymerization time reaches 40 hours without sticking to the kettle, add 20ml of pre-cooled methanol to terminate the reaction, and dry in vacuum. The number average molecular weight is 60000 g / mol.

Embodiment 3

[0035] At -95°C, 184g of methyl chloride, 40.5g of isobutylene and 26g of m-methylstyrene were added to the reactor and mixed thoroughly, the concentration of isobutylene monomer was 16.2wt%, and the content of m-methylstyrene was 10.4wt%. Take 1.8ml trichlorotriethyldialuminum chloride solution (0.4M), 3.89mg water and 1.5ml ethanol solution (0.1M) and mix them to form an initiating system, then add 25ml methyl chloride solution for dilution, Under the condition of ℃, low-temperature aging for 5 minutes. Squeeze the aged initiator system into the reactor to initiate polymerization, the polymerization time reaches 40 hours without sticking to the kettle, add 20ml of pre-cooled methanol to terminate the reaction, and dry in vacuum. The number average molecular weight is 100000 g / mol.

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Abstract

The invention relates to a uniform structure type polyisobutylene random copolymer and a preparation method thereof. The preparation method is characterized in that the temperature condition is 60 to 100 DEG C; the solvent is chloromethane solvent; isobutene is treated as a first monomer, and a styrene derivative is treated as a second monomer; a main initiator and a co-initiator are aged and complexed to form an initiating system; alcohols or alcamines are added as a third component; on that basis, the copolymerizing is carried out through cationic slurry to obtain the uniform structure type polyisobutylene random copolymer. According to the preparation method, the reaction activity of the styrene derivative is effectively adjusted and controlled; the polymerizing rate is controlled, and the calorific value per unit of time in the polymerizing process is reduced, so that the colloidal particle adhering caused by the increased temperature in a reaction kettle can be prevented, and as a result, the problem of blocking of the reaction kettle can be effectively solved; in addition, the styrene derivative can be uniformly distributed in a polyisobutene main chain, and thus the uniform structural and stable polyisobutylene random copolymer can be obtained; meanwhile, the continuous production time of a single copolymerizing kettle can be prolonged to be 40 to 90 hours.

Description

technical field [0001] The invention belongs to the technical field of isobutylene copolymer synthesis, in particular to a polyisobutylene-based random copolymer with uniform structure and a preparation method thereof. Background technique [0002] There are two sets of production methods in the production technology of isobutylene in the world. One is synthesized by a solution method, which uses methyl chloride and hexane as reaction solvents, and the small rubber particles produced can be dissolved in hexane. Another method is the slurry method. The reaction solvent of this method is only methyl chloride, and the glue produced by the system cannot be dissolved in the solvent. This is the biggest difference between the two. Among the countries that produce isobutylene-based rubber in the world, only one factory in Togliatti, Sibur, Russia, adopts the solution preparation method, while the other factories all use the slurry method for the copolymerization of isobutylene and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/10C08F212/12C08F4/54
CPCC08F210/10C08F212/12C08F2500/03C08F4/54
Inventor 伍一波于小杰郭文莉李树新杨丹王浩胡月丽
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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