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Method for preparing polyacrylonitrile resin with narrow molecular weight distribution

A technology of polyacrylonitrile resin and narrow molecular weight distribution, which is applied in the field of preparation of polyacrylonitrile resin with narrow molecular weight distribution, can solve the problems of poisonous, difficult to obtain, and sensitive initiator halides, and achieves the goal of overcoming atom transfer radical polymerization, The effect of the preparation method is simple and easy

Inactive Publication Date: 2009-08-26
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two major defects in conventional atom transfer radical polymerization: on the one hand, the initiator halide used is poisonous, difficult to obtain, and difficult to preserve; moisture sensitive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1: 0.071 gram of anhydrous FeCl 3 , 0.114 grams of itaconic acid were dissolved in 50.0 milliliters of N,N-dimethylformamide, 0.072 grams of azobisisobutyronitrile was dissolved in 23.0 milliliters of acrylonitrile, and added to the reaction flask in turn, and the nitrogen filling was repeated 4 times In addition to oxygen removal, the reaction bottle was placed in a constant temperature oil bath at 65 degrees Celsius to carry out polymerization. After reacting for 16 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0011] The conversion rate of the polymerization reaction was 74.6%, the number average molecular weight of the obtained polyacrylonitrile resin was 16180, and the molecular weight distribution was 1.18.

Embodiment 2

[0012] Embodiment 2: 1.458 grams of anhydrous FeCl 3 1.17 grams of itaconic acid were dissolved in 50.0 milliliters of N,N-dimethylformamide, 0.492 grams of azobisisobutyronitrile was dissolved in 19.7 milliliters of acrylonitrile, and then added to the reaction flask in turn, and nitrogen filling was repeated 4 times In addition to oxygen removal, the reaction bottle was placed in a constant temperature oil bath at 55 degrees Celsius to carry out polymerization. After reacting for 10 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0013] The conversion rate of the polymerization reaction was 40.2%, the number average molecular weight of the obtained polyacrylonitrile resin was 1250, and the molecular weight distribution was 1.21.

Embodiment 3

[0014] Embodiment 3: 0.142 gram of anhydrous FeCl 3 , 0.341 g of itaconic acid was dissolved in 50.0 ml of N, N-dimethylformamide, 0.144 g of azobisisobutyronitrile was dissolved in 23.0 ml of acrylonitrile, and added to the reaction flask in turn, and nitrogen filling was repeated 4 times In addition to oxygen removal, the reaction bottle was placed in a constant temperature oil bath at 60°C for polymerization. After reacting for 6 hours, the product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried.

[0015] The conversion rate of the polymerization reaction was 30.6%, the number average molecular weight of the obtained polyacrylonitrile resin was 3520, and the molecular weight distribution was 1.16.

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Abstract

The invention discloses a preparation method of polyacrylonitrile resin with narrow molecular weight distribution. It is characterized in that the metal halide anhydrous ferric trichloride (FeCl3) and the ligand itaconic acid (IA) are dissolved in the solvent N, N-dimethylformamide (DMF); the initiator azobisisobutyl Nitrile (AIBN) was dissolved into monomer acrylonitrile (AN), nitrogen was passed through repeatedly to deoxygenate 4 times, and reverse atom transfer radical living polymerization was carried out. The reaction was at least 6 hours. The product was precipitated, filtered with suction, washed with concentrated hydrochloric acid, and dried. By means of the preparation method disclosed in the present invention, the polyacrylonitrile resin with a molecular weight distribution of 1.14-1.21 can be obtained.

Description

(1) Technical field: [0001] The invention relates to a method for preparing polyacrylonitrile resin with narrow molecular weight distribution, in particular to a method for preparing polyacrylonitrile resin by reverse atom transfer radical active polymerization using a conventional initiator and a high-valence metal halide as a catalytic system. (two) background technology: [0002] Polyacrylonitrile resin is an important precursor in the field of polymer materials, with excellent light resistance, weather resistance, insect resistance, and radiation resistance. The distribution of polymer molecular weight has a great influence on the production process and product quality of polymer materials. Discussing the molecular weight distribution of polymers has very important practical significance for improving the performance of polymer materials, optimizing molding process conditions, and improving product quality. At present, the preparation of polyacrylonitrile resin with narr...

Claims

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Application Information

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IPC IPC(8): C08F120/44C08F2/00C08F4/04
Inventor 陈厚曲荣君王春华周文英纪春暖孙昌梅
Owner LUDONG UNIVERSITY