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Preparation method of PS-Cl and application thereof

A polystyrene, chlorine-based technology, applied in the chemical industry, can solve problems such as the influence of slurry stability

Inactive Publication Date: 2015-09-23
商巧玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Initiators such as SnCl4 and quaternary ammonium salts used in it, and additives all remain in the system, which will affect the stability of the slurry in the next step

Method used

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  • Preparation method of PS-Cl and application thereof
  • Preparation method of PS-Cl and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.5ml of styrene and 1ml of hexane into an anhydrous and oxygen-free polymerization bottle, add 1ml of cumyl chloride hexane solution (concentration: 0.007mol / L), and co-initiator AlCl 3 0.009g, reacted at -50°C for 30min, added to -50°C for 30min at a constant temperature, the monomer concentration prepared in a mixed solvent of dichloromethane and hexane (volume ratio: 4:6) was 20% isobutene (85g) and isoprene (2g) solution, add AlCl to the system 3 (2.6g), after reacting for 50min, add 2ml of ethanol solution containing 1wt% NaOH to terminate the polymerization, the product is milky white, no obvious aggregation of glue blocks, and no wall hanging phenomenon. The product was dried in a vacuum drying oven to constant weight, the polymerization conversion rate was 72%, the relative number average molecular weight was 230000, and the molecular weight distribution was 2.1.

Embodiment 2

[0022] Add 4.5ml of styrene and 10ml of hexane into an anhydrous and oxygen-free polymerization bottle, add 9ml of cumyl chloride hexane solution (concentration: 0.007mol / L), and co-initiator FeCl 3 0.012g, reacted at -110°C for 30min, added to -110°C for 30min at a constant temperature, and the monomer concentration prepared in a mixed solvent of methyl chloride and hexane (5:5 by volume) was 30% isobutylene (90g) and In the solution of isoprene (2.72g), add AlCl to the system 3 (5g), after reacting for 50min, add 2ml of ethanol solution containing 1wt% NaOH to terminate the polymerization, the product is milky white, no obvious aggregation of glue blocks, and no wall hanging phenomenon. The product was dried in a vacuum drying oven to constant weight, the polymerization conversion rate was 69%, the relative number average molecular weight was 180000, and the molecular weight distribution was 1.9.

Embodiment 3

[0024] Add 3ml of styrene and 10ml of hexane into an anhydrous and oxygen-free polymerization bottle, add 8ml of cumyl chloride hexane solution (concentration is 0.007mol / L), and co-initiator FeCl 3 0.012g, reacted at -90°C for 30min, added to -90°C for 30min at a constant temperature, and the monomer concentration prepared in a mixed solvent of methyl chloride and methylcyclohexane (volume ratio: 5:5) was 40% isobutene ( 90g) and isoprene (2.6g) solution, add AlCl to the system 3 (3.5g), after 50min of reaction, 2ml of ethanol solution containing 1Wt% NaOH was added to terminate the polymerization, the product was milky white, no obvious aggregation of glue blocks was found, and there was no wall hanging phenomenon. The product was dried in a vacuum drying oven to constant weight, the polymerization conversion rate was 75%, the relative number average molecular weight was 250,000, and the molecular weight distribution was 2.3.

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Abstract

The invention provides a preparation method of PS-Cl and the application thereof, wherein PS-Cl is used as a slurry stabilizer of IIR. The preparation method comprises the following steps that monomer styrene prepared by mixing solvents is placed in an oxygen-free water-free polymerization bottle, an inifer and coinitiator Lewis acid which are prepared through a hexane solution are placed in the polymerization bottle, a reaction is conducted for 30 min under the condition of -110 DEG C to -60 DEG C, a reaction product is added to an isobutene and isoprene solution prepared by mixing solvents at a constant temperature for 30 min, the Lewis acid is added to the system, after reaction is conducted for 50 min, 2 ml of an ethanol solution containing 1Wt% of NaOH is added to the system, and then polymerization is ended. A product is milky white, an obvious rubber block clustering phenomenon is not found, and a wall attachment phenomenon is avoided. A slurry stabilizing solution prepared through the method can directly achieve the slurry stabilizing function on IIR without after-treatment.

Description

technical field [0001] The present invention relates to the preparation of a chlorine-terminated polystyrene and its application as a slurry stabilizer. Specifically, the present invention uses a living cationic polymerization method to polymerize a chlorine-terminated polystyrene in a mixed solvent without the need for processing The invention can be added into the slurry polymerization process as a slurry stabilizer to stabilize the slurry of butyl rubber, and belongs to the technical field of chemical industry. technical background [0002] Butyl rubber (IIR) has good air tightness, electrical insulation, corrosion resistance, aging resistance and other advantages, and has been widely used in many fields such as tire inner tubes, automotive interiors, sealing and pharmaceutical products. Butyl rubber is a typical cationic polymerization process. Due to the fast initiation of cationic reactions, high activity, and various side reactions are prone to occur. At present, only...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F210/10C08F236/08C08F2/38C08F2/12
Inventor 商巧玲
Owner 商巧玲
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