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Method for preparing vinyl monomer polymer using metallorene free-radical polymerization catalyst

A technology of metallocene compounds and vinyl monomers, applied in the field of active radical polymerization catalysts, can solve the problems of slow reaction speed and no active polymerization, and achieve the effect of easy storage

Inactive Publication Date: 2004-01-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Korean Hee-Gweon Woo (Bull Korean Chem.Soc.2002, 23, 1343) reported that the metallocene compound catalyzed the free radical thermal polymerization of acrylic acid under the initiation of several halogenated hydrocarbons, but did not obtain active polymerization. As a result, and the slow response

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 57mg of cobaltocene into a 100mL Schlenk reaction bottle equipped with a stirring magnet, add 5mL of toluene, 6.858g of styrene and 62mg of ethyl α-bromoisobutyrate through injection technology, and the system is frozen-vacuumized-frozen three times cycle, and finally filled with argon. The reaction system was reacted at 60° C. for 96 hours, and the monomer conversion rate was 37.7%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 16900, the molecular weight distribution (MWD) was 1.58, and the predicted molecular weight of the product was 7540.

Embodiment 2

[0023] Put 57mg of cobaltocene in a 100mL Schlenk reaction bottle equipped with a stirring magnet, add 5mL of toluene, 6.314g of styrene and 60mg of ethyl α-bromoisobutyrate through injection technology, and the system is frozen-vacuumized-frozen three times cycle, and finally filled with argon. The reaction system was reacted at 70° C. for 97 hours, and the monomer conversion rate was 66.6%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 26800, the molecular weight distribution (MWD) was 1.55, and the predicted molecular weight of the product was 13300.

Embodiment 3

[0025] Put 57mg of cobaltocene in a 100mL Schlenk reaction bottle equipped with a stirring magnet, add 5mL of toluene, 6.151g of styrene and 62mg of ethyl α-bromoisobutyrate through injection technology, and the system is frozen-vacuumized-freezing Three cycles, finally filled with argon. The reaction system was reacted at 80° C. for 48 hours, and the monomer conversion rate was 74.5%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 32900, the molecular weight distribution (MWD) was 1.56, and the predicted molecular weight of the product was 14410.

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PUM

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Abstract

The method for preparing vinyl monomer polymer by using metallocene free radical polymerization catalyst is characterized by that in the presence of dicyclopentadienyl type metallocene compound catalyst, initiating agent and inert gas and in the organic solvent the vinyl monomer polymerization reaction can be made, the ratio of described halogenated organic compound initiating agent and catalyst is 1-3, it adopts orgon protection, its polymerization reaction temp. is 60-90 deg.C, and the general vinyl monomer can be undergone the process of active free radical polymerization reaction to obtain the polymer whose molecular weight is in the range of 1000-100000, molecular weight can be controlled and molecular weight distribution is narrow and the polymer with controllable block and graft structure, so that it provides good condition for industrization of active free radical polymerization reaction.

Description

technical field [0001] The invention relates to a novel active radical polymerization catalyst, in particular to a method for preparing a vinyl monomer polymer by using a metallocene radical polymerization catalyst. Background technique [0002] Because living polymerization can control the structure of polymer compounds and synthesize various useful polymer materials with special structures and properties, its industrialization has huge social and economic benefits. Among many living polymerization methods, free radical living polymerization has many obvious advantages, such as a wide range of monomers, mild implementation conditions, and favorable industrial production. Therefore, this technology has been highly valued in recent years. In 1995, American KrzysztofMatyjaszewski (J.Am.Chem.Soc.1995,117,5614) and Japanese Mitsuo Sawamoto (Macromolecules 1995,28,1721) took the lead in reporting the synthesis of styrene and methyl methacrylate with transition metal catalysts. L...

Claims

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Application Information

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IPC IPC(8): C08F4/80C08F10/02
Inventor 王佰全庄岩雒雄雄徐善生
Owner CHINA PETROLEUM & CHEM CORP