Method for preparing monoolefine-conjugated diene copolymer solution for halogenating

A technology of conjugated diolefins and monoolefins, which is applied in the field of preparation of halogenated monoolefin-conjugated diene copolymer solutions for halogenation, can solve the problems of high content and poor product quality, reduce production costs, improve quality, The effect of simplifying the preparation and production process

Active Publication Date: 2019-07-02
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem that the existing method for preparing halogenated butyl rubber solution has a relatively high gel content of the copolymer and a relatively high content of low-molecular-weight oligomers with a weight-average molecular weight of less than 20,000, which leads to poor product quality. Problem, provide a new preparation method of monoolefin-conjugated diene copolymer solution for halogenation

Method used

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  • Method for preparing monoolefine-conjugated diene copolymer solution for halogenating
  • Method for preparing monoolefine-conjugated diene copolymer solution for halogenating
  • Method for preparing monoolefine-conjugated diene copolymer solution for halogenating

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preparation example Construction

[0026] The invention provides a method for preparing a monoolefin-conjugated diene copolymer solution for halogenation, the method comprising:

[0027] (1) Mix the terminator solution cooled below -35°C with the monoolefin-conjugated diene copolymer slurry to obtain a monoolefin-conjugated diene copolymer slurry that has lost catalytic activity, wherein the terminator The agent solution contains C 1 -C 2 Halogenated alkanes and saturated fatty alcohols A and optionally C 5 -C 8 The aliphatic alkanes, the saturated fatty alcohol A is C 1 -C 5 Saturated monohydric fatty alcohol, C 2 -C 4 One or more of saturated dibasic fatty alcohols and saturated fatty alcohols shown in formula (1),

[0028]

[0029] Formula (1), R 1 for C 2 -C 3 straight-chain or branched-chain alkyl,

[0030] (2) Use at least one replacement solvent to replace the haloalkane in the monoolefin-conjugated diene copolymer slurry that has lost catalytic activity and remove unreacted monomers to obt...

preparation example 1

[0105] A low-pressure liquid ethylene at -115°C is introduced into the internal cooling pipe of the polymerization reactor, and methylene chloride, isobutene and isoprene are mixed in a certain proportion to form a mixed monomer solution, wherein the moles of isobutene and isoprene The ratio is 45:1, the total monomer concentration is 35wt%, and the mixed monomer solution is gradually cooled to -98°C through propylene and ethylene respectively. The catalyst solution formed by mixing the catalysts ethylaluminum dichloride and methylene chloride in a certain proportion is also gradually cooled to -95°C through propylene and ethylene respectively, and the catalyst concentration is 0.25wt%. The cooled monomer solution and catalyst solution are respectively sent to the polymerization reactor under flow control, and contact in the polymerization reactor to carry out cationic polymerization reaction. The polymerization heat is removed by -115°C low-pressure liquid ethylene, and the po...

preparation example 2

[0108] A low-pressure liquid ethylene at -115°C is introduced into the internal cooling pipe of the polymerization reactor, and methylene chloride, isobutene and isoprene are mixed in a certain proportion to form a mixed monomer solution, wherein the moles of isobutene and isoprene The ratio is 99:1, the total monomer concentration is 40wt%, and the mixed monomer solution is gradually cooled to -98°C through propylene and ethylene respectively. The catalysts, ethylaluminum dichloride and methylene chloride, are mixed in a certain proportion and gradually cooled to -95° C. through propylene and ethylene respectively, wherein the concentration of the catalyst is 0.25 wt%. The cooled monomer solution and catalyst solution are respectively sent to the polymerization reactor under flow control, and contact in the polymerization reactor to carry out cationic polymerization reaction. The polymerization heat is removed by -115°C low-pressure liquid ethylene, and the polymerization temp...

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Abstract

The present invention relates to a method for preparing monoolefine-conjugated diene copolymer solution for halogenating. The method comprises: (1) mixing a terminant solution which has been cooled tobe below 35 DEG C with monoolefine-conjugated diene copolymer slurry, wherein the terminator solution contains C1-C2 haloalkanes and saturated aliphatic alcohols A and optionally C5-C8 aliphatic alkanes, the saturated aliphatic alcohols A is one or several kinds of C1-C5 saturated mono fatty alcohol, one or several kinds of C2-C4 saturated dihydric fatty alcohol and one or several kinds of saturated fatty alcohols shown in the formula (1), (2) replacing the halogenated alkane in the solution by at least one replacement solvent and removing the unreacted monomer, wherein the replacement solvent is selected from C5-C8 aliphatic alkanes. The halogenating butyl rubber obtained by the method has the characteristic of low gel content, and the low molecular weight oligomer content in the halogenated butyl rubber having a weight average molecular weight of less than 20,000 is low.

Description

technical field [0001] The invention relates to the technical field of monoolefin-conjugated diene copolymers for halogenation, in particular to a method for preparing a solution of halogenated monoolefin-conjugated diene copolymers for halogenation. Background technique [0002] On the basis of maintaining the original properties of butyl rubber, halogenated butyl rubber (HIIR) has a fast vulcanization speed, can be co-vulcanized with general-purpose elastomers, has good bonding performance, and has better heat resistance. The material of choice for innerliners of tubeless radial tires. At present, the production technology of halogenated butyl rubber is mainly carried out by solution method, that is, saturated alkane (such as hexane) is used as a solvent to dissolve butyl rubber to obtain a certain concentration of glue, and then carry out halogenation reaction. The production process of solution method halogenated butyl rubber includes three parts: (1) production of basi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F6/02C08F6/10C08F6/06C08F8/20C08F210/12
CPCC08F6/003C08F6/02C08F6/06C08F8/20C08L23/283C08F210/12
Inventor 孟伟娟邱迎昕张雷周新钦
Owner CHINA PETROLEUM & CHEM CORP
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