Preparation method of long-chain branched cis-rich polybutadiene

A technology of polybutadiene and long-chain branching, which is applied in the field of preparation of long-chain branched high-cis-polybutadiene, which can solve the problems of low coupling efficiency, many short-chain branched products, and harsh polymerization temperature preparation requirements, etc. problems, to achieve the effect of improving mixing uniformity, improving physical and mechanical properties, and improving dynamic mechanical properties

Active Publication Date: 2014-12-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are three methods for preparing branched polybutadiene rubber: (1) Direct polymerization method: Copolymerize butadiene with low molecular weight polybutadiene macromonomer to prepare polybutadiene grafted with short chain branches , but due to the short polybutadiene branch chain, the cold flow resistance and physical and mechanical properties of polybutadiene rubber have not been effectively improved, see Polymer Science, Ser.B, 2006, 48, 61-65; patent WO2009121516A1 Discloses a method by adjusting the polymerization temperature and H in the catalytic system 2 The O/Nd molar ratio is a method for directly preparing branched polybutadiene, but this method has strict requirements on the polymerization temperature and the preparation of the catalyst, and the branched structure of the prepared branched polybutadiene is difficult to control; (2) the chain end Coupling reaction: the active chain end of linear polybutadiene and organic halides, organometallic compounds, carboxylic acids

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1:

[0019] In N 2 Under the protection, add 37.5mL of butadiene / hexane solution (in which the monomer mass concentration is 20%) and containing neodymium octoate, triisobutylaluminum, diisobutylaluminum hydride, trichloromethane and A catalyst solution composed of 2-phenyl-2-chloropropane, the molar ratio of the amount of catalyst to butadiene is 2×10 -4 , Start the polymerization, and after reacting at 40°C for 2.5 hours, add a hexane solution containing 0.1% by mass of 2,6-di-tert-butyl-p-cresol to terminate the polymerization to obtain a hexane solution of linear high-cis polybutadiene. The weight average molecular weight of high cis polybutadiene (M w ) Is 45.6×10 4 , Molecular weight distribution (M w / M n ) Is 2.5, and the cis-1,4 structure content is 97.7%. By adding a certain amount of hexane, the polymer solution concentration was adjusted to 40g / L, and azobisisoheptonitrile and 1,3-dimercaptopropane were added in an air atmosphere to make 1,3-dimercaptop...

Example Embodiment

[0020] Example 2:

[0021] The preparation method, branching reaction method and treatment method of the linear high-cis polybutadiene / hexane solution are the same as in Example 1, except that the mass ratio of 1,10-dimercaptodecane to polybutadiene is 0.025%. The molar ratio of azodiisoheptanonitrile to 1,10-dimercaptodecane is 1:1. The obtained long-chain branched high cis polybutadiene M w 46.9×10 4 , M w / M n Is 2.5, cis-1,4 structure content is 97.6%, g is 0.95.

Example Embodiment

[0022] Example 3:

[0023] The preparation method, branching reaction method and treatment method of the linear high-cis polybutadiene / hexane solution are the same as in Example 1, except that the mass ratio of 4,4'-dimercaptodiphenyl sulfide to polybutadiene is 0.03 %, the molar ratio of azobisisoheptonitrile to 4,4'-dimercaptodiphenyl sulfide is 1:1, and the reaction is 5 minutes. The obtained long-chain branched high cis polybutadiene M w 43.2×10 4 , M w / M n It is 2.4, cis-1,4 structure content is 97.7%, g is 0.97.

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Abstract

The invention relates to a preparation method of long-chain branched cis-rich polybutadiene. The preparation method specifically comprises the following step of: reacting linear or linear short-chain branched cis-rich polybutadiene with a bifunctional or polyfunctional organic compound in the presence of a radical initiator, so that long-chain branched cis-rich polybutadiene is prepared. Compared with linear or linear short-chain branched cis-rich polybutadiene, the thermal stability, cold flow resistance, and mixing uniformity with packing, and the like, of the long-chain branched cis-rich polybutadiene are obviously improved, and the physical and mechanical properties and dynamic mechanical properties of vulcanized rubber are also obviously improved.

Description

Technical field: [0001] The invention relates to a preparation method of long-chain branched high-cis-polybutadiene, specifically, in the presence of a free radical initiator, linear or linear short-chain branched high-cis-polybutadiene is combined with a bifunctional group or Multifunctional organic compounds are reacted to prepare long chain branched high cis polybutadiene. Background technique: [0002] The rolling resistance, wet skid resistance and wear resistance of tires are important indicators for evaluating tire performance. Only tires that achieve "triangular balance" can achieve the best energy-saving effect. High-cis polybutadiene rubber has a series of advantages such as good elasticity, good wear resistance, good low-temperature performance, low heat generation, and low rolling resistance. It is the second largest synthetic rubber variety and is widely used in tire manufacturing, but usually high The cis-polybutadiene has a linear structure or a linear short-...

Claims

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Application Information

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IPC IPC(8): C08C19/28C08F136/06
Inventor 吴一弦高晓满朱寒楼金帅王迎春
Owner CHINA PETROLEUM & CHEM CORP
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