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Method for preparing thermostable syndiotactic 1,2-polybutadiene thermoplastic elastomer

A technology of thermoplastic elastomer and polybutadiene, which is applied in the field of thermal stability, can solve problems such as high viscosity, difficulty and complexity of anti-aging agents, and achieve excellent thermal stability and improve thermal stability.

Active Publication Date: 2011-05-04
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the molecular chain of syndiotactic 1,2-polybutadiene thermoplastic elastomer has a large number of tertiary hydrocarbons and side vinyl groups, it is difficult to avoid branching and crosslinking during high-temperature polymerization; the operation of adding anti-aging agent at high temperature is more complicated , due to the high viscosity of the polymerization liquid even at a high temperature of 80 ° C, it is difficult to disperse the anti-aging agent evenly in the polymer, and high temperature operation will cause high energy consumption during industrial production

Method used

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  • Method for preparing thermostable syndiotactic 1,2-polybutadiene thermoplastic elastomer
  • Method for preparing thermostable syndiotactic 1,2-polybutadiene thermoplastic elastomer

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Under the protection of nitrogen, add 50 ml of dry hexane and 7 g of dry butadiene to the single-port 100 ml reaction flask that has been baked and dried, and then add the catalyst components in the following order: 2,6-di-tert-butyl- 0.12mmol of 4-(dimethylaminomethyl)phenol, 0.010mmol of iron isooctanoate, 0.025mmol of diethyl phosphite, 0.050mmol of triisobutylaluminum, 0.200mmol of triethylaluminum; put it in a constant temperature water bath at 50°C Polymerize for 6 hours, then stir and pulverize the mixture of polymer and solvent, add alcohol / hexane mixed solution containing 0.5ml alcohol to terminate, separate the polymer, remove the solvent and put it in a vacuum drying oven to dry under vacuum, the polymer Sample 6.0g, yield 86%. According to DSC analysis, the glass transition temperature of the polymer is -10.9°C, and the melting temperature is 118.3°C; the 1,2-structure content of the polymer is 83.4 by 1H-NMR analysis; the syndiotacticity of the polymer is a...

Embodiment 2～4

[0028] Except that the amounts of triisobutylaluminum and triethylaluminum are shown in Table 1, all the other are the same as in Example 1.

[0029] Table 1

[0030] Example

[0031] Triethylaluminum / triisobutylaluminum (molar ratio)

Embodiment 5

[0033]Under the protection of nitrogen, add 50ml of dry heptane and 7g of dry butadiene into the single-port 100ml reaction flask that has been baked and dried, and then add the catalyst components in the following order: iron acetylacetonate 0.010mmol, diphosphite Ethyl ester 0.025mmol, triisobutylaluminum 0.050mmol, triethylaluminum 0.200mmol, 2,6-di-tert-butyl-4-(dimethylaminomethyl)phenol 0.12mmol; put in a constant temperature water bath at 50°C Polymerize for 6 hours, then stir and pulverize the mixture of polymer and solvent, add alcohol / hexane mixed solution containing 0.5ml alcohol to terminate, separate the polymer, remove the solvent and put it in a vacuum drying oven to dry under vacuum, the polymer Sample 6.4g, yield 91%. According to DSC analysis, the glass transition temperature of the polymer is -10.5°C, and the melting temperature is 117.9°C; 1 The 1,2-structure content of polymer analyzed by H-NMR is 84.1; 13 C-NMR analysis showed that the syndiotacticity o...

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Abstract

The invention provides a method for preparing thermo-stable syndiotactic 1, 2-polybutadiene thermoplastic elastomers. The method takes a compound with anti-aging function as a component of a catalyst, and can cause an age inhibitor to be evenly dispersed in the irregular 1, 2-polybutadiene thermoplastic elastomers. The syndiotactic 1, 2-polybutadiene thermoplastic elastomers prepared have excellent thermal stability. The thermo-stable syndiotactic 1, 2-polybutadiene thermoplastic elastomers prepared through the method have 1, 2-structure with content over 80 percent, and have a syndiotactic degree larger than 70 percent and the fusing temperature between 115 DEG C to 150 DEG C.

Description

technical field [0001] The invention belongs to the manufacturing method of thermally stable syndiotactic 1,2-polybutadiene thermoplastic elastomer. Background technique [0002] Syndiotactic 1,2-polybutadiene thermoplastic elastomer is a unique material with both plastic and rubber properties. Syndiotactic 1,2-polybutadiene thermoplastic elastomer is a high-vinyl polybutadiene polymer, and its side vinyl groups are arranged alternately on both sides of the main chain of the polymer molecule. The syndiotactic 1,2-polybutadiene thermoplastic elastomer refers to a syndiotactic 1,2-polybutadiene polymer having a degree of crystallinity in the range of 5% to 50%. When the crystallinity of syndiotactic 1,2-polybutadiene is lower than 5%, it is a kind of rubber, not thermoplastic; when the crystallinity of syndiotactic 1,2-polybutadiene is higher than 50%, it is a rubber Thermoplastic resin, but not elastic. [0003] In the 1970s, the industrial production of syndiotactic 1,2-p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/06C08F4/70
Inventor 毕吉福张学全姜连升蔡洪光王蓓
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI