Method of raising the stability of isobutene polymer slurry

A technology of isobutylene polymer and slurry method, which is applied in the field of improving the stability of isobutylene polymer slurry, and can solve problems such as aggregation and agglomeration, increased cost, and adverse effects of isobutylene polymer production

Inactive Publication Date: 2004-06-23
中国石油化工股份有限公司北京燕山分公司研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the slurry method is widely used in the industrial production of isobutylene polymers, the slurry method also has the following disadvantages: using the slurry method, when the local microscopic temperature of the polymerization reaction system fluctuates and rises, the surface of the butyl rubber particles is easily sticky and lumpy
Boron trichloride can initiate the cationic polymerization of isobutene, which may adversely affect the production of isobutene polymers
Obviously, this will complicate the process and increase the cost

Method used

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  • Method of raising the stability of isobutene polymer slurry
  • Method of raising the stability of isobutene polymer slurry
  • Method of raising the stability of isobutene polymer slurry

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Example 1 Preparation of slurry stabilizer precursor by cationic polymerization of p-methylstyrene monomer in methylene chloride:

[0032] Polymerization was carried out in a 100 ml tubular reactor. The reactor is first baked under vacuum, filled with nitrogen, and repeated several times. Then the reactor was placed in a cold bath, and a metered amount of initiator 1-phenylchloroethane (1-PhEtCl), additive n-Bu 4 N + Cl - , the monomer p-methylstyrene (pMSt) and the solvent methylene chloride. After the temperature reaches the predetermined reaction temperature, add the co-initiator SnCl 4 The polymerization reaction is started. After reacting for a predetermined time, the polymerization reaction is terminated with pre-cooled methanol to obtain a stabilizer precursor. After the monochloromethane volatilized, a certain amount of dichloromethane was added to dissolve the polymer, and then precipitated with methanol, filtered, vacuum-dried, weighed, and the conversio...

Embodiment 2

[0036] Example 2 Preparation of slurry stabilizer precursor by cationic polymerization of styrene monomer in methylene chloride:

[0037] Get a well-processed polymerization reactor as described in Example 1, place it in a cold bath, then add 20 milliliters of solvent monochloromethane, 3 milliliters of monomeric styrene, 28 milligrams of additives tetrabutylammonium bromide ( Consumption is 1% of styrene monomer quality), 25 microliters of initiator cumyl oxygen (consumption is 0.9% of styrene monomer quality), above-mentioned reactant is cooled to-80 ℃, then adds 75 microliters of co- Initiator SnCl4 (The consumption is 6% of the mass of styrene monomer), and the polymerization reaction starts. After 1 hour of reaction, methanol was added to terminate the reaction. Get about 1.08 grams of polystyrene (conversion rate about 40%), relative molecular mass =6500, relative molecular mass distribution index =1.53.

Embodiment 3

[0038] Example 3 Stabilization of Isobutylene Polymer Slurry by Indirect Addition of Stabilizer Precursor

[0039] Polymerization experiments of isobutylene copolymers were carried out in a 250 ml stirred tubular reactor. With 30 milliliters of diluent methylene chloride, 21 gram monomer isobutylene, 0.8 gram comonomer isoprene, 0.160 gram polyp-methylstyrene (numbering S1-4 in embodiment 1, relative molecular mass =13900, relative molecular mass distribution index =1.87, the dosage is about 0.75% of the monomer weight) into the reactor and cooled to -95°C. Then add 25 ml of AlCl 3 Chloromethane solution (which contains AlCl 3 about 18 mg). During the polymerization, the temperature inside the reactor rose to -75°C. The material in the reactor is a milky white dispersion, and there is no adhering polymer on the reactor wall, stirring blade and stirring shaft. After the agitation was stopped, no polymer agglomeration in the reactor was observed within 10 minutes. The c...

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Abstract

The method of raising the stability of isobutene polymer slurry includes adopting styrene polymer with C1 end group as the precursor for the stabilizer, and the precursor for polymer slurry stabilizer is prepared via cation polymerizing process. The monomer is at least one selected from styrene, p-methyl styrene and alpha-methyl styrene; the solvent is methane chloride; the initiator system includes initiator halohydrocarbon, co-initiator tin tetrahalide and additive quaternary ammonium salt; and the polymerization temperature is -110 deg.c to -40 deg.c.

Description

technical field [0001] The present invention relates to a kind of method that improves the stability of isobutylene polymer slurry, more specifically, the present invention relates to adopting the terminal group obtained by the polymerization of styrenic monomers in a methyl chloride solvent by cationic polymerization method is chlorine group ( Cl) the styrene-based monomer polymer is used as a stabilizer precursor, and the slurry in the isobutylene polymer is prepared by a stable slurry method. Background technique [0002] Isobutylene polymers generally include isobutylene homopolymers, copolymers of isobutylene and isoprene, or copolymers of isobutylene and p-methylstyrene. Copolymers of isobutylene and isoprene are commonly referred to as butyl rubber. The industrial production of isobutylene polymer mainly adopts low-temperature cationic polymerization process with Lewis acid as catalyst or co-initiator. Commonly used Lewis acids are aluminum tric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/00C08F10/10
Inventor 马育红程斌武冠英
Owner 中国石油化工股份有限公司北京燕山分公司研究院
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