Catalyst composition for preparing 1,2-polybutadiene, and preparation method for 1,2-polybutadiene

A polybutadiene and catalyst technology, applied in the field of polymers, can solve problems such as unfavorable industrial production, reduced catalytic activity, complex components, etc., achieve strong thermodynamic stability and chemical stability, improve catalytic activity, and use less Effect

Inactive Publication Date: 2012-07-04
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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Problems solved by technology

However, the above-mentioned iron-based catalysts not only have complex components and high cost, but also their catalytic activity decreases significantly when the temperature is higher than 30°C, which is not conducive to the preparation of 1,2-polybutadiene, that is, the above-mentioned iron-based catalysts are only suitable for It is used in low temperature polymerization, which is not conducive to industrial production

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  • Catalyst composition for preparing 1,2-polybutadiene, and preparation method for 1,2-polybutadiene
  • Catalyst composition for preparing 1,2-polybutadiene, and preparation method for 1,2-polybutadiene

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preparation example Construction

[0052] The present invention also provides a kind of preparation method of 1,2-polybutadiene, comprises the following steps:

[0053] Under the action of the obtained catalyst composition for preparing 1,2-polybutadiene, 1,3-butadiene is polymerized in an organic solvent to obtain 1,2-polybutadiene.

[0054] The present invention is preferably under the protection of nitrogen, preferably adding 1,3-butadiene, an organic solvent and the catalyst composition for preparing 1,2-polybutadiene to an anhydrous and oxygen-free polymerizer to carry out the polymerization reaction, Then it is preferred to terminate the reaction with an ethanol solution of 1% 2,6-di-tert-butyl-p-cresol with a mass fraction, preferably to precipitate the polymer with ethanol, and preferably after washing with ethanol, extruding, and preferably vacuum-drying to constant Weight, to obtain polybutadiene product.

[0055] Wherein, the present invention uses the obtained catalyst composition for the preparati...

Embodiment 1

[0062] Under nitrogen protection, iron and dimethyl phosphite (C 2 h 7 PO 3 ) in a molar ratio of 1:3, iron trifluoromethanesulfonate and dimethyl phosphite were added to the reactor, and 40 mL of tetrahydrofuran was added as a solvent to obtain a mixed solution, and then the mixed solution was condensed and refluxed in a boiling state for 24 hours After evaporating the solvent, and drying to constant weight, the chemical formula is [Fe(CF 3 SO 3 ) 3 (C 2 h 7 PO 3 ) 3 ] of iron complexes.

[0063] Under the protection of nitrogen, 4×10 -5 mol obtained iron complex, 1.6mL hexane and 0.4mL Al(i-Bu) with a concentration of 2.0mol / L 3 hexane solution to obtain a concentration of 2 x 10 -5 mol / mL is used to prepare the catalyst composition of 1,2-polybutadiene, wherein, Al(i-Bu) 3 The molar ratio of iron in the obtained iron complex is 20:1.

[0064] Under the protection of nitrogen, add 20mL concentration of 20g / 100mL 1,3-butadiene hexane solution to an anhydrous and ...

Embodiment 2

[0067] Under nitrogen protection, iron and diethyl phosphite (C 4 h 11 PO 3 ) in a mol ratio of 1:3, ferrous trifluoromethanesulfonate and diethyl phosphite were added to the reactor, and then 40mL of tetrahydrofuran was added as a solvent to obtain a mixed solution, then the mixed solution was condensed and refluxed in a boiling state, After 24h, the solvent was evaporated and dried to constant weight to obtain the chemical formula [Fe(CF 3 SO 3 ) 2 (C 4 h 11 PO 3 ) 3 ] of iron complexes.

[0068] Under the protection of nitrogen, 4×10 -5 mol obtained iron complex, 0.4mL 1,3-butadiene hexane solution with a concentration of 1.0mol / L, 1.5mL hexane and 0.1mL Al(i-Bu) with a concentration of 2.0mol / L 2 H in hexane to obtain a concentration of 2 x 10 -5mol / mL is used to prepare the catalyst composition of 1,2-polybutadiene, wherein, the mol ratio of 1,3-butadiene and iron in the obtained iron complex is 10:1, Al(i-Bu) 2 The molar ratio of H to iron in the obtained iro...

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Abstract

The invention provides a catalyst composition for preparing 1,2-polybutadiene. The catalyst composition comprises alkyl aluminum, and iron complex with the chemical formula shown as a formula (I): [Fe(CF3SO3)x(L)y], wherein L is ligand which is a phosphorus compound, a nitrogenous compound, a sulfur compound, or an oxygen compound; x is 2 or 3; and y is more than or equal to 1 and less than or equal to 10. The catalyst composition has high catalytic activity at high temperature, has a wide application temperature range, and can be produced industrially. The invention also provides a preparation method for the 1,2-polybutadiene. The preparation method comprises the following steps of: performing polymerization on 1,3-butadiene in an organic solvent under the action of the catalyst composition for preparing the 1,2-polybutadiene to obtain the 1,2-polybutadiene. A small amount of the catalyst composition is adopted in the preparation method, a preparation process is stable, a reaction condition is mild, and the method is easy to operate and low in production cost.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a catalyst composition for preparing 1,2-polybutadiene and a preparation method of 1,2-polybutadiene. Background technique [0002] 1,2-Polybutadiene is an olefin polymer with vinyl side groups on the main molecular chain. It has good wet skid resistance, aging resistance and low heat generation. It is ideal for manufacturing high-performance tires, green tires and One of the ideal materials for automobiles, etc. With the rapid development of the automotive industry, the demand for 1,2-polybutadiene is also increasing. [0003] When preparing 1,2-polybutadiene, catalysts such as lithium-based catalysts, cobalt-based catalysts, molybdenum-based catalysts, and iron-based catalysts can be used. Among them, iron-based catalysts are a better catalyst and have become a current research focus. one. The prior art discloses a variety of iron-based catalysts for the preparation of 1,2-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/06C08F4/70
Inventor 代全权唐月张学全白晨曦蔡洪光张春雨张贺新毕吉福那丽华
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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