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Method for preparing polyacrylonitrile by single electron transfer active free radical polymerization

A single-electron transfer and polyacrylonitrile technology, which is applied in the field of preparation of polyacrylonitrile, can solve the problems of affecting the performance of the final polymer product, not being able to control the molecular weight and molecular weight distribution well, and achieve a simple and easy preparation method and excellent reaction conditions. mild effect

Inactive Publication Date: 2012-07-25
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional free radical polymerization method is a common method for preparing polyacrylonitrile, but because the traditional free radical polymerization is prone to chain transfer and chain termination reactions, it cannot control the molecular weight and molecular weight distribution well, which seriously affects the performance of the final polymer product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Dissolve 0.0064 grams of iron powder and 0.0799 grams of hexamethylenetetramine in 15.0 milliliters of N,N-dimethylformamide, dissolve 0.11 milliliters of carbon tetrachloride in 15.0 milliliters of acrylonitrile, and add them to the reaction flask in sequence , repeated nitrogen and deoxygenation 4 times, the reaction bottle was placed in a constant temperature oil bath at 65 degrees Celsius to carry out polymerization. After reacting for 36 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0012] The polyacrylonitrile obtained by the polymerization reaction had a number average molecular weight of 17557 and a molecular weight distribution of 1.15.

Embodiment 2

[0014] Dissolve 0.0318 g of iron powder and 0.3993 g of hexamethylenetetramine into 15.0 ml of N,N-dimethylformamide, dissolve 0.11 ml of carbon tetrachloride into 15.0 ml of acrylonitrile, and add them to the reaction flask in sequence , repeated nitrogen and deoxygenation 4 times, the reaction bottle was placed in a constant temperature oil bath at 65 degrees Celsius to carry out polymerization. After reacting for 20 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0015] The polyacrylonitrile obtained by the polymerization reaction has a number average molecular weight of 17028 and a molecular weight distribution of 1.12.

Embodiment 3

[0017] Dissolve 0.0318 grams of iron powder, 0.77 milliliters of 1,1,4,7,10,10-hexamethyltriethylenetetramine into 15.0 milliliters of N, N-dimethylformamide, and 0.11 milliliters of carbon tetrachloride Dissolve it in 15.0 ml of acrylonitrile, add it to the reaction flask in turn, repeatedly fill with nitrogen and remove oxygen 4 times, put the reaction flask into a constant temperature oil bath at 65 degrees Celsius, and carry out polymerization. After reacting for 24 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0018] The polyacrylonitrile obtained by the polymerization reaction has a number average molecular weight of 17028 and a molecular weight distribution of 1.12.

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Abstract

The invention discloses a method for preparing polyacrylonitrile by single electron transfer active free radical polymerization. The method is characterized by dissolving catalyst iron powder and a ligand in a solvent, namely N,N-dimethyl formamide, adding an initiator, namely carbon tetrachloride, into monomers, namely acrylonitrile, repeatedly introducing nitrogen for removing oxygen for at least three times, performing the single electron transfer active free radical polymerization at a certain temperature, washing a product by concentrated hydrochloric acid, settling, performing suction filtration, and drying. With the preparation method disclosed by the invention, the polyacrylonitrile with a molecular weight distribution of 1.10-1.17 can be obtained.

Description

technical field [0001] The invention relates to a method for preparing polyacrylonitrile, in particular to a method for preparing polyacrylonitrile by single electron transfer active radical polymerization. Background technique [0002] Polyacrylonitrile and its modification can be widely used in the fields of biomedicine, superabsorbent resin, ion exchange resin, pollution control, antibacterial and deodorizing, solid polymer electrolyte, filtration and separation, etc. [0003] The traditional free radical polymerization method is a common method for preparing polyacrylonitrile, but because the traditional free radical polymerization is prone to chain transfer and chain termination reactions, it cannot control the molecular weight and molecular weight distribution well, which seriously affects the performance of the final polymer product . [0004] In recent years, single electron transfer active radical polymerization catalyzed by copper powder or copper wire has been wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/44C08F4/80
Inventor 陈厚刘德龙王春华曲荣君陈玲芳
Owner LUDONG UNIVERSITY