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Method for preparing polybutadiene

A technology for polybutadiene and butadiene is applied in the field of preparation of polybutadiene, and can solve the problems of inapplicability of low molecular weight polybutadiene, low efficiency and low efficiency of lithium-based catalysts, etc.

Inactive Publication Date: 2010-08-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the efficiency of lithium-based catalysts is less than 100%
Traditional Ziegler-Natta catalysts are inefficient and unsuitable for the preparation of low molecular weight polybutadiene

Method used

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  • Method for preparing polybutadiene

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preparation example Construction

[0026] The invention provides a preparation method of polybutadiene, comprising: adding 1,3-butadiene monomer and catalyst into an alkane solvent in a molar ratio of 100 to 4000:1 for polymerization reaction to obtain Reaction solution; use ethanol to condense polybutadiene from the reaction solution. The catalyst is obtained by the following preparation method: the rare earth compound, butadiene and aluminum alkyl are mixed for reaction to obtain a mixed solution, and chloride is added to the The reaction is carried out in the mixed solution to obtain the catalyst.

[0027] The invention uses an anionic coordination polymerization mechanism to prepare polybutadiene with low molecular weight and narrow molecular weight distribution, and the polymerization environment is a solution. The catalyst used in the preparation method of the present invention is preferably a three-component homogeneous catalyst of rare earth compounds, and the raw materials include: rare earth compounds...

Embodiment 1

[0034] Under the protection of nitrogen, add neodymium neodecanoate, butadiene and diisobutylaluminum hydride to the dry catalyst reaction flask in sequence, and react at 50°C for 5 minutes, then add dimethyldichlorosilane, and then add dimethyldichlorosilane at 25 The reaction was carried out at ℃ for 30 minutes to obtain a rare earth catalyst for butadiene polymerization. In preparing the catalyst raw materials, the molar ratio of neodymium neodecanoate, butadiene, diisobutylaluminum hydride and dimethyldichlorosilane is 1:10:20:2.0.

[0035] Under nitrogen protection, 20 mL of a hexane solution of 1,3-butadiene monomer was added to a dry 50 mL reaction flask. Then add the prepared rare earth catalyst. The molar ratio of catalyst to 1,3-butadiene monomer is 1:400. Polymerization was carried out at 50°C. After 4 hours of polymerization reaction, terminate with ethanol solution containing 0.01 g / mL anti-aging agent 264. Coagulation with ethanol yields low molecular weight ...

Embodiment 2

[0041] Under the protection of nitrogen, add neodymium neodecanoate, butadiene and diisobutylaluminum hydride in sequence to the dry catalyst reaction bottle, and react at 50°C for 5 minutes, then add chlorobutylaluminum, and then add chlorobutylaluminum at 25°C The reaction was carried out for 30 minutes to obtain a rare earth catalyst for butadiene polymerization. In preparing the catalyst raw materials, the molar ratio of neodymium neodecanoate, butadiene, diisobutylaluminum hydride and chlorobutylaluminum is 1:10:20:2.0.

[0042] Under nitrogen protection, 20 mL of a hexane solution of 1,3-butadiene monomer was added to a dry 50 mL reaction flask. Then add the prepared rare earth catalyst. The molar ratio of catalyst to 1,3-butadiene monomer is 1:400. Polymerization was carried out at 50°C. After 4 hours of polymerization reaction, terminate with ethanol solution containing 0.01 g / mL anti-aging agent 264. Coagulation with ethanol yields low molecular weight butadiene. ...

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Abstract

The invention provides a method for preparing polybutadiene, which comprises: adding a 1,3-butadiene monomer and a catalyst into an alkane solvent in a molar ratio of 100-4,000:1 to perform polymerization to obtain reaction solution; and extracting polybutadiene from the reaction solution by using ethanol. A method for preparing the catalyst comprises: mixing a rare earth compound, butadiene, isoprene and alkylaluminium to perform a reaction to obtain a mixed solution; adding a chloride into the mixed solution to perform a reaction to obtain the catalyst. In the invention, the rare earth compound three-component homogeneous phase catalyst is used for catalyzing the reaction and part of the 1,3-butadiene monomer is pre-polymerized to serve as part of the catalyst, so an active center of the reaction is formed to stabilize polymerization; and by controlling the molar ratio of the 1,3-butadiene monomer to the catalyst, the polybutadiene with low molecular weight and narrow molecular weight distribution is prepared.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a preparation method of polybutadiene. Background technique [0002] Low-molecular-weight polybutadiene is a kind of liquid rubber. Low-molecular-weight polybutadiene and its modified products have excellent adhesion balance performance. It can be used as a reactive plasticizer and softener to improve the processing and operability of rubber The physical properties and processing properties of hard rubber products. Because low-molecular-weight polybutadiene has the above-mentioned excellent properties, low-molecular-weight polybutadiene is used in tires, wires and cables, sealing strips, hoses, seals, printing and textile rubber rollers, footwear, adhesives, etc. widely used. [0003] The low molecular weight polybutadiene generally has a number average molecular weight of 1,000 to 100,000. If one wants to obtain low-molecular-weight polybutadiene with uniform properties, the ...

Claims

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Application Information

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IPC IPC(8): C08F136/06C08F4/54C08F4/52C08F2/06C08F6/12
Inventor 张学全范长亮王佛松蔡洪光代全权毕吉福张春雨那丽华姜连升
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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