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Multi-arm star-type thermoplastic elastomer synthesizing method

A technology of thermoplastic elastomer and synthesis method, which is applied in the field of synthesis of known polymer compounds, can solve the problems of wide molecular weight distribution of block polymers, few properties of thermoplastic elastomers, poor physical properties, etc., and achieve low homopolymer content , high molecular weight and excellent product performance

Inactive Publication Date: 2005-02-16
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method of polyisobutylene thermoplastic elastomer is prepared by active cationic polymerization technology. For example, WO95 / 10554 patent provides a method for synthesizing block copolymers using end-capping agents, using tert-butyl dicumyl chloride and tricumyl chloride base chloride; with TiCl 4 For the initiating system, use 40:60 (V:V) mixed solvent of methyl chloride and HX; carry out living polymerization of isobutylene at -80°C, then add end-capping agent 1.1-diphenylethylene, and then add isopropoxy acid Phthalophthalein, finally add p-methylstyrene to synthesize a tri-block copolymer of polyp-methylstyrene-polyisobutylene-poly-p-methylstyrene, and WO91 / 11468 patent provides polyisobutylene as the rubber soft segment, with Styrene, indene or derivatives of both are thermoplastic elastomers with hard segments, using dicumyl ether or tricumyl ether and TiCl 4 As an initiating system, the block polymer obtained by the above method has a wide molecular weight distribution and poor physical properties. In the synthesis of block polymers, there are very few properties related to thermoplastic elastomers.

Method used

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  • Multi-arm star-type thermoplastic elastomer synthesizing method
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  • Multi-arm star-type thermoplastic elastomer synthesizing method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Example 1: Linear polyisobutylene-polystyrene block thermoplastic elastomer

[0039] At normal pressure, reaction temperature -75--80°C, under the protection of dry nitrogen, add 1L mixed solvent, 1×10 -3 mol / L Benzoyl Chloride, 0.04mol / L TiCl 4 , 1.2×10 -3 mol / L hexahydropyridine was aged for 15 minutes, and wasobutene was added to keep the concentration at 2.8mol / L. After reacting for 1 hour, the end-capping agent 1,1-diphenylethylene was added, and the concentration was 6×10 -3 mol / L, age for 15 minutes, add plastic hard segment monomer or its concentration is 0.6mol / L, continue to react for 1 hour, add methanol dissolved in 5% HCl to the system to terminate, pour the solution after termination The product precipitated out in ethanol solution, was filtered and dried.

[0040] The block thermoplastic elastomer product has a number average molecular weight of 25,000, a molecular weight distribution of 1.19, a glass transition temperature of 197°C, a tensile strength o...

Embodiment 2

[0041] Embodiment 2: multi-arm star polyisobutylene-polystyrene block thermoplastic elastomer

[0042] At normal pressure, reaction temperature -75--80°C, under the protection of dry nitrogen, add 1L mixed solvent, 1×10 -3 mol / L pyromellitic acid chloride, TiCl 4 The concentration of 0.16mol / L, the concentration of hexahydropyridine is 1.2×10 -3 mol / L, the concentration of isobutylene is 11.2mol / L, the concentration of end-capping agent 1,1-diphenylethylene is 0.024mol / L, and the concentration of plastic hard segment monomer styrene is 2.4mol / L.

[0043] The block thermal elastomer product has a number average molecular weight of 220,000, a molecular weight distribution of 1.26, a tensile strength of 26 MPa, and an elongation of 750%.

[0044] While applying for a patent for the synthesis method of the present invention, a patent for the initiation system was also applied for.

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Abstract

This invention refers to a kind of synthetic method of poly-armed star-like polyolefin thermoplastic elastomer, which belongs to high molecular compound of carbon-and-carbon dangling bond reaction. The synthetic method is as follows: under the ordinary pressure, low temperature and the protection of dry nitrogen gas, get the soft section of active cation polyisobutylene synthetic rubber, hard section monomer of plastic and terminator from the component solvent, initiator, coinitiator and soft section monomer, then get the 4-armed star-like block thermoplastic elastomer, whose relative molecular weight is between 180000 and 250000 and whose molecular weight distributes between 2.0 and 3.5. The advantage of the invention lies in the high molecular weight and excellent performance and refers to many thermoplastic elastomers.

Description

technical field [0001] The invention relates to a synthesis method of a class of known polymer compounds; more specifically, the invention relates to a new synthesis method of a class of multi-arm star-shaped polyolefin thermoplastic elastomers. Background technique [0002] Thermoplastic elastomers are similar to vulcanized rubber at room temperature, and can be melt-processed like thermoplastics; they meet people's special requirements for material properties and processing, and develop rapidly. [0003] At present, the synthesis method of polyisobutylene thermoplastic elastomer is prepared by active cationic polymerization technology. For example, WO95 / 10554 patent provides a method for synthesizing block copolymers using end-capping agents, using tert-butyl dicumyl chloride and tricumyl chloride base chloride; with TiCl 4 For the initiating system, use 40:60 (V:V) mixed solvent of methyl chloride and HX; carry out living polymerization of isobutylene at -80°C, then add ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F295/00
Inventor 李树新郭文莉金玉顺商育伟吴天斌刘红升
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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