Two-component cobalt-based catalyst and its application in solution or suspension polymerization of 1,3-butadiene

A technology of suspension polymerization and butadiene, which is applied in the field of two-component catalysts, can solve the problems of low activity of rare earth catalysts, high Nd content, and low catalytic activity, and achieve excellent catalytic activity, high product cis-selectivity, and wide industrial The effect of applying the foreground

Active Publication Date: 2015-12-23
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, there are also evaluations that the activity of the supported rare earth catalyst is low, and the residual Nd content in the polymerization product is high (Adv. Polym. Sci., 2006, 204, 1–154)
[0010] Therefore, to realize the heterogeneous polymerization production of butadiene rubber, it is still necessary to solve the problems of low catalytic activity and easy agglomeration of polymer particles during the polymerization process.

Method used

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  • Two-component cobalt-based catalyst and its application in solution or suspension polymerization of 1,3-butadiene
  • Two-component cobalt-based catalyst and its application in solution or suspension polymerization of 1,3-butadiene
  • Two-component cobalt-based catalyst and its application in solution or suspension polymerization of 1,3-butadiene

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Experimental program
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Embodiment 1

[0032] Under nitrogen protection, take 3.3 mg (5.0 μmol) of the main catalyst CoCl 2 (PPh 3 ) 2 In a Schlenk bottle, seal it with a rubber stopper, vacuumize and blow nitrogen three times, and add 5 mL of purified toluene solvent. Then, add 0.5 mL of cocatalyst sesquiethylaluminum chloride (EASC, 0.4 mol / L n-hexane solution) with a syringe, so that [Al] / [Co] is 80 (molar ratio, the same below), the catalyst The composition was stirred and aged at 25°C for two minutes, and then 1.4mL of 1,3-butadiene (1.86mol / L toluene solution) was added with a syringe to make the monomer 1,3-butadiene and the main catalyst The molar ratio of metal cobalt in the medium is 500, and the polymerization reaction starts to proceed. After one hour, a uniform and transparent reaction solution was obtained, and the reaction solution was poured into 200mL terminator to terminate the polymerization. as an antioxidant). The precipitated polybutadiene rubber (PBD) was filtered, washed several times w...

Embodiment 2

[0034] The specific operation steps are the same as in Example 1, taking 3.3 mg (5.0 μmol) of the main catalyst CoCl 2 (PPh 3 ) 2 , add 5mL of purified benzene solvent, and add 5.5mL of 1,3-butadiene (1.85mol / L benzene solution) with a syringe, so that the mole of monomer 1,3-butadiene and metal cobalt in the main catalyst The ratio was 2000, the polymerization temperature was 25° C., and the polymerization time was one hour.

Embodiment 3

[0036] The specific operation steps are the same as in Example 1, taking 3.3 mg (5.0 μmol) of the main catalyst CoCl 2 (PPh 3 ) 2 , add 5mL of purified ethylbenzene solvent, and add 8.5mL of 1,3-butadiene (1.84mol / L ethylbenzene solution) with a syringe, so that the monomer 1,3-butadiene and the metal cobalt in the main catalyst The molar ratio is 3000, the polymerization temperature is 25°C, and the polymerization time is one hour.

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Abstract

The invention discloses a two-component cobalt catalyst and application thereof in solution polymerization or suspension polymerization of 1,3-butadiene. The cobalt catalyst comprises: (1) a main catalyst, wherein the general formula of the main catalyst is CoCl2(PR<1>nR<2>(3-n))2, and R1 and R2 are independently selected from hydrogen, alkyl group, naphthene group, benzyl group and aryl group; (2) a cocatalyst, wherein the cocatalyst is an alkyl aluminum chloride compound, including diethylaluminium chloride, ethylaluminium dichloride and sesquiethyl aluminum chloride. The main catalyst and the cocatalyst of the cobalt catalyst are mixed and aged for a period of time in a solvent according to a proportion or are supported on inert powder to be prepared into a supported catalyst; the 1,3-butadiene is added to perform solution polymerization or suspension polymerization. The two-component cobalt catalyst shows superior catalytic activity and high product cis-form selectivity in the polymerization of the 1,3-butadiene, and has wide industrial application prospect.

Description

technical field [0001] The invention relates to a two-component catalyst composed of a cobalt-based main catalyst containing a free phosphine ligand and an alkylaluminum chloride co-catalyst and its application, in particular to a two-component cobalt-based catalyst and its application in 1,3-butyl Applications in solution or suspension polymerization of dienes. Background technique [0002] The polymerization methods of 1,3-butadiene include 1,4-polymerization and 1,2-polymerization to generate cis-1,4, trans-1,4 or 1,2-vinyl polybutadiene respectively ( PBDs), whose performance mainly depends on the microstructure of the polymer. Among these different isomers, high cis-1,4 polybutadiene has become an important industrial product because of its excellent rubber properties, that is, butadiene rubber. High-cis 1,4-polybutadiene rubber (butadiene rubber, BR) has particularly excellent cold resistance, wear resistance and elasticity, and also has good aging resistance; it is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/70C08F136/06C08F2/06C08F2/18
Inventor 介素云李伯耿周勤灼
Owner ZHEJIANG UNIV
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