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Iron-contained type load catalyst polymerized by utilizing reverse atom to transfer free radical and its application

A supported catalyst and atom transfer technology, applied in the field of polymer synthesis, can solve problems such as low catalyst residue and difficult separation, and achieve the effects of avoiding separation and processing work, avoiding environmental pollution, and saving energy

Inactive Publication Date: 2004-07-28
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem of separation difficulties in existing reverse atom transfer radical polymerization catalysts, and to propose an easily separated supported catalyst, which can be used to control polymerization and prepare polymers with specified molecular weight and narrow distribution. The biggest feature of the catalyst is that after the catalytic polymerization reaction is over, it can be completely separated by simple filtration, and the residual amount of the catalyst is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparing the complex supported carrier of the catalyst. After washing the cross-linked polyacrylic acid resin with water, pass through an appropriate amount of 3% NaOH solution to change the ion exchange resin from the hydrogen form to the sodium form, then wash it with deionized water until pH = 9, dry it in vacuum at 80°C, and pass it through a ball mill Pulverize and dry in vacuum to obtain cross-linked polyacrylic acid ion exchange resin powder PAA(N).

[0021] (2) Preparation of supported catalyst. Dissolve 1 part of ferric chloride in 10 parts of methanol, add 3 parts of cross-linked polyacrylic acid ion exchange resin powder, stir and reflux at 70°C for 3 hours, remove methanol and vacuum dry to obtain PAA-FeCl 3 Crude. The crude product was eluted with methanol until it was colorless, and after vacuum drying, PAA-FeCl 3 , which is a catalyst for catalyzing reverse atom transfer radical polymerization.

[0022] (3) Get the azobisisobutyronitrile initiato...

Embodiment 2

[0024] (1) Preparing the complex supported carrier of the catalyst. After washing the cross-linked polyacrylic acid resin with water, pass through an appropriate amount of 2% NaOH solution to change the ion exchange resin from the hydrogen form to the sodium form, then wash it with deionized water until pH = 9, dry it in vacuum at 80°C, and pass it through a ball mill Pulverize and dry in vacuum to obtain cross-linked polyacrylic acid ion exchange resin powder PAA(N).

[0025](2) Preparation of supported catalyst. Dissolve 1 part of ferric chloride in 10 parts of methanol, add 3 parts of cross-linked polyacrylic acid ion exchange resin powder, stir and reflux at 70°C for 3 hours, remove methanol and vacuum dry to obtain PAA-FeCl 3 Crude. The crude product was eluted with methanol until it was colorless, and after vacuum drying, PAA-FeCl 3 , which is a catalyst for catalyzing reverse atom transfer radical polymerization.

[0026] (3) get the initiator dibenzoyl peroxide and...

Embodiment 3

[0028] (1) Preparing the complex supported carrier of the catalyst. After washing the cross-linked polyacrylic acid resin with water, pass through an appropriate amount of 5% NaOH solution to change the ion exchange resin from the hydrogen form to the sodium form, then wash it with deionized water until pH = 9, dry it in vacuum at 80°C, and pass it through a ball mill Pulverize and dry in vacuum to obtain cross-linked polyacrylic acid ion exchange resin powder PAA(N).

[0029] (2) Preparation of supported catalyst. Dissolve 1 part of ferric tribromide in 10 parts of methanol, add 3 parts of cross-linked polyacrylic acid ion exchange resin powder, stir and reflux at 70°C for 3 hours, remove methanol and vacuum dry to obtain PAA-FeBr 3 Crude. The crude product was eluted with methanol until it was colorless, and after vacuum drying, PAA-FeBr 3 , which is a catalyst for catalyzing reverse atom transfer radical polymerization.

[0030] (3) get the azobisisobutyronitrile initia...

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Abstract

The present invention relates to an iron-contained type load catalyst for reverse atomic transfer free radical polymolization and its application. It uses high specific area cross-linked polyacrylic acid ion-exchange resin as load carrier of catalyst, and uses iron trihalide to make coordination and complexation to form load catalyst, the load catalyst and conventional azo initiator, monomer and solvent are formed into a solid-liquid reaction system according to a certain proportion, the system can be used for catalyzing controllable free radical polymerization. The catalyst has no need of using halid with strong poisonou property as initiator, after having been activated it can be circularly used.

Description

Technical field: [0001] The invention relates to the manufacture of a novel iron-containing supported catalyst for reverse atom transfer radical polymerization, which can be used to prepare homopolymers and copolymers with a specified molecular weight and a narrow distribution, and the reaction system only needs simple The catalyst can be removed by centrifugation. The invention belongs to the technical field of polymer synthesis. technical background: [0002] Living polymerization is an important means to achieve molecular design and synthesize polymers with specific structures and properties. Due to the harsh reaction conditions of commonly used living polymerization methods, such as anionic polymerization, cationic polymerization, and group transfer polymerization, there are fewer applicable monomers. In contrast, free radical polymerization has a wide application prospect because it can adapt to a wide range of monomers, the conditions are mild, and the requirements f...

Claims

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Application Information

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IPC IPC(8): C08F4/02C08F4/80C08F20/10
Inventor 张永明李忠辉薛敏钊张春刘燕刚
Owner SHANGHAI JIAO TONG UNIV
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