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Catalyst for preparing syndiotactic polystyrene

A polystyrene and catalyst technology, applied in the field of catalysts for preparing syndiotactic polystyrene, can solve the problems of low catalytic activity and catalytic efficiency, etc.

Inactive Publication Date: 2005-06-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the problems of low catalytic activity and catalytic efficiency in the above-mentioned documents, and provide a new catalyst for preparing syndiotactic polystyrene, which has higher catalytic activity and catalytic efficiency

Method used

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  • Catalyst for preparing syndiotactic polystyrene
  • Catalyst for preparing syndiotactic polystyrene
  • Catalyst for preparing syndiotactic polystyrene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Catalyst preparation

[0040] In a dry 250ml three-necked bottle, N 2 Evacuate 3 times, add 1.016 grams of pentamethyl trichlorotitanocene and 70 milliliters of benzene, add dropwise a mixture of 30 milliliters of benzene, 1.35 grams of p-chlorophenol and 1.1 grams of triethylamine, drop it after 45 minutes, at room temperature After reacting for 1 hour, heat to benzene reflux temperature again, after reacting for 2 hours, stop heating, react at room temperature for 10 hours, heat and react again for 2 hours, filter, filtrate is drained, recrystallized repeatedly with toluene and hexane solution, drained, 1.74 g of yellow crystals were obtained, with a yield of 88%.

Embodiment 2

[0042] Catalyst preparation

[0043] In a dry 250ml three-necked bottle, N 2 Evacuate 3 times, add 2.10 g of pentamethyl trichlorotitanocene and 70 ml of benzene, add dropwise 50 ml of benzene, 2.79 g of p-chlorophenol and 2.4 g of triethylamine mixture, drop it after 45 minutes, heat Reacted for 4 hours, then reacted at room temperature for 10 hours, and finally heated for 4 hours again, filtered, the filtrate was drained, extracted with hexane, and drained to obtain 3.5 g of yellow crystals, with a yield of 85%.

Embodiment 3

[0045]In a baked and dried 50 ml two-necked bottle, use high-purity N 2 Evacuate 3 times, add 10 ml of refined styrene monomer, stir electromagnetically in an oil bath at 60°C for 20 minutes, inject 0.2 mmol of triisobutylaluminum, 0.4 mmol of MAO, and the titanocene of Example 1 with a syringe Catalyst 0.001 mmol reacts after 10 minutes, stops reaction with ethanol-hydrochloric acid solution, washes, and dries to obtain powder solid 3.53 grams, catalytic activity 443 kilograms polymer / (gram titanium.hour), syndiotacticity 96%, Mw=37× 10 4 .

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Abstract

The present invention relates to a catalyst for the preparation of syndiotactic polystyrene (sPS), comprising a metallocene titanium compound R 1 Ti(OR 2 R 3 ) 3 and alkylaluminoxanes, where R 1 Cyclopentadienyl or containing 1 to 5 C 1～4 Alkyl cyclopentadienyl, R 2 is an aryl group containing 6 to 12 carbon atoms, R 3 for halogen. When the catalytic system is used for the syndiotactic polymerization of styrene, it has high catalytic activity and catalytic efficiency, and the highest catalytic activity reaches 510 kg polymer / g titanium·hour, which can be used in industrial production.

Description

technical field [0001] This invention relates to catalysts for the preparation of syndiotactic polystyrene. Background technique [0002] Styrene polymers can be classified into atactic polystyrene (aPS), isotactic polystyrene (iPS) and syndiotactic polystyrene (sPS). The synthesis of syndiotactic polystyrene usually uses a catalytic system composed of organometallic titanium compounds and polymethylaluminoxane (MAO), in which the organometallic compounds are mainly titanocene compounds. Documents EP210615, US5252693, JP0291104 and EP389981 etc. report that the structure is CpTiCl 3 / MAO, Cp * TiCl 3 The / MAO catalytic system is used in the case of syndiotactic polymerization of styrene, but its catalytic activity and catalytic efficiency are not high, and it is not suitable for industrial applications. Contents of the invention [0003] The technical problem to be solved by the present invention is to overcome th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/642C08F112/08
Inventor 沈志刚林尚安周文乐祝方明赵薇薇卢文奎
Owner CHINA PETROLEUM & CHEM CORP