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Load catalyst containing nickel and iron and its application

A technology for supporting catalysts and catalysts, which is applied to catalyst carriers, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of difficult separation and low catalyst residues, achieve simple regeneration treatment, good industrialization prospects, and avoid separation. difficult effect

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

[0006] The purpose of the present invention is to present the difficult problem of separating in existing ATRP catalyst, propose a kind of easily separable nickel-iron-containing supported catalyst, use this catalyst to control polymerization, prepare the polymer of specified molecular weight, narrow distribution, the catalyst's The biggest feature is that after the catalytic polymerization reaction is completed, all of them can be separated by simple filtration, and the residual amount of catalyst is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparing the complex supported carrier of the catalyst. Use cross-linked polyacrylic acid ion exchange resin as the carrier of catalyst iron halide, wash with 5% lye, change the ion exchange resin from hydrogen form to sodium form, then wash with deionized water to pH = 9, and vacuum dry at 80°C Afterwards, pulverized by a ball mill, and then vacuum-dried to obtain a cross-linked polyacrylic acid ion exchange resin powder PAA(Na).

[0024] (2) Preparation of supported passivator. Take 1 part of ferric trichloride FeCl 3 After dissolving 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 .

[0025] (3) Preparation of loaded activator. Take 1 part NiCl 2 After being placed in 10 parts of methanol and fully stirred, add ...

Embodiment 2

[0029] (1) Preparing the complex supported carrier of the catalyst. Use cross-linked polyacrylic acid ion exchange resin as the carrier of catalyst iron halide, wash with 3% lye, change the ion exchange resin from hydrogen form to sodium form, then wash with deionized water to pH = 9, and vacuum dry at 80°C Afterwards, pulverized by a ball mill, and then vacuum-dried to obtain a cross-linked polyacrylic acid ion exchange resin powder PAA(Na).

[0030] (2) Preparation of supported passivator. Take 1 part of iron tribromide FeBr 3 After dissolving 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 .

[0031] (3) Preparation of loaded activator. Take 1 part NiBr 2 After being placed in 10 parts of methanol and fully stirred, add 30 ...

Embodiment 3

[0035] (1) Preparing the complex supported carrier of the catalyst. Use cross-linked polyacrylic acid ion exchange resin as the carrier of catalyst iron halide, wash with 4% lye, change the ion exchange resin from hydrogen form to sodium form, then wash with deionized water to pH = 9, and vacuum dry at 80°C Afterwards, pulverized by a ball mill, and then vacuum-dried to obtain a cross-linked polyacrylic acid ion exchange resin powder PAA(Na).

[0036] (2) Preparation of supported passivator. Take 1 part of iron tribromide FeBr 3 After dissolving 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 .

[0037] (3) Preparation of loaded activator. Take 1 part NiCl 2 After being placed in 10 parts of methanol and fully stirred, add 30 ...

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Abstract

The present invention relates to a load type catalyst containing nickel and iron and its application. It uses high specific area cross-linked polyacrylic ion-exchange resin powder body as load carrier of catalyst, and makes it and nickel dihalide and iron trihalide undergo the process of coordinative complexation reaction to form the load catalyst. The load catalyst can be mixed with initiator, monomer and solvent according to a certain ratio, and formed into a solid-liquid reaction systm which can be used for catalyzing controllable free radical polymerization. After the reaction is completed, then reaction product and catalyst can be simply separated, and the metal catalyst residue in the product is less, and said catalyst can be recovered and reused.

Description

Technical field: [0001] The invention relates to a nickel-iron-containing supported catalyst for active / controllable polymerization. The catalyst can be used to prepare narrow-distribution homopolymers and copolymers with specified molecular weights. The reaction system only needs simple centrifugation. The catalyst is removed. Compared with other supported catalysts of the same type, the supported catalyst of the invention is simple to regenerate, can be recycled, and avoids environmental pollution. The invention belongs to the technical field of polymer synthesis. Background technique: [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 polym...

Claims

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Application Information

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IPC IPC(8): B01J27/128B01J32/00C08F4/70
Inventor 张永明李忠辉薛敏钊张春刘燕刚
Owner SHANGHAI JIAO TONG UNIV
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