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Method for preparing vinyl monomer polymer by using cobalt diphosphine dihalide as catalyst

A vinyl monomer and catalyst technology, applied in the field of free radical polymerization, can solve the problems of unsuitability for large-scale industrial production, large amount of catalyst, complex post-treatment, etc., achieve good industrial application conditions and prospects, high catalyst activity, and preparation easy effect

Inactive Publication Date: 2008-07-09
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, multiple transition metal organic compounds have been used in controlled free radical polymerization (Chem.Rev.2001, 101, 2921; Chem.Rev.2001, 101, 3689), but there are still many problems, such as: the amount of catalyst Larger, complex post-processing, higher cost, etc., not suitable for large-scale industrial production

Method used

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  • Method for preparing vinyl monomer polymer by using cobalt diphosphine dihalide as catalyst
  • Method for preparing vinyl monomer polymer by using cobalt diphosphine dihalide as catalyst
  • Method for preparing vinyl monomer polymer by using cobalt diphosphine dihalide as catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 223.0mg of bis(triphenylphosphine)cobalt dibromide and 25mg of azobisisobutyronitrile into a 100mL Schlenk reaction flask equipped with a stirring magnet, add 10mL of toluene, 6.120g of methyl methacrylate by injection technique . The system went through three cycles of freezing-vacuumizing-freezing, and finally filled with argon. The reaction system was reacted at 80° C. for 2.5 hours, and the monomer conversion rate was 69%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 45000, and the molecular weight distribution (MWD) was 1.34.

Embodiment 2

[0033] 22.3 mg of bis(triphenylphosphine) cobalt dibromide and 25 mg of azobisisobutyronitrile were added to a 100 mL Schlenk reaction bottle equipped with a stirring magnet, and 10 mL of toluene and 6.112 g of methyl methacrylate were added by injection technique. The system went through three cycles of freezing-vacuumizing-freezing, and finally filled with argon. The reaction system was reacted at 80° C. for 3 hours, and the monomer conversion rate was 60%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 52000, and the molecular weight distribution (MWD) was 1.31.

Embodiment 3

[0035] 22.3 mg of bis(triphenylphosphine) cobalt dibromide and 25 mg of azobisisobutyronitrile were added to a 100 mL Schlenk reaction bottle equipped with a stirring magnet, and 10 mL of toluene and 3.126 g of methyl methacrylate were added by injection technique. The system went through three cycles of freezing-vacuumizing-freezing, and finally filled with argon. The reaction system was reacted at 80° C. for 4 hours, and the monomer conversion rate was 71%. The obtained polymer was analyzed by gel permeation chromatography (GPC), and the molecular weight was 33000, and the molecular weight distribution (MWD) was 1.33.

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Abstract

The invention relates to a process for utilizing catalyst such as diphosphonic dihalide cobalt to prepare vinyl monomer polymer. The catalyst of the invention is a compound such as diphosphonic dihalide cobalt which has the structure of the general formula (I) (II). The process for preparing vinyl monomer polymer of the invention comprises leading the vinyl monomer to have a polymerization reaction in organic solvent under the protecting of the catalyst (I) or (II), initiating agent and inactive gas. The mole ratio of the initiating agent and the catalyst is 0.5-50, the temperature of polymerization reaction is 60-90 DEG C, the general vinyl monomer can have free radical polymerization reaction which can be controlled to get polymers whose molecular weight is between the scope of 5000-100000, and the molecular weight can be controlled and the distribution thereof is narrow, and get the polymer whose block, graft and super graft can be controlled. The invention has a certain prospect of industrialization application.

Description

【Technical field】 [0001] The invention belongs to the technical field of free radical polymerization, and relates to a novel controllable free radical polymerization catalyst and a polymerization method thereof, in particular to a method for preparing vinyl monomer polymers with low-cost diphosphine cobalt dihalide catalysts. 【Background technique】 [0002] Free radical polymerization is the most widely used polymerization method in industry. It is suitable for a wide range of monomers, has mild reaction conditions, various synthesis processes, and is easy to realize industrial production. Since controlled free radical polymerization can synthesize various polymer materials with different structures and properties, research and development of new controlled free radical polymerization system and industrialization will have huge social and economic benefits. Transition metal-organic The compound catalyzes the atom transfer radical polymerization of styrene and methyl methac...

Claims

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Application Information

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IPC IPC(8): C08F4/26C08F4/04C08F4/34C08F20/00C08F16/36C08F120/14
Inventor 王佰全雒雄雄徐善生
Owner NANKAI UNIV