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Process for preparing polyanilinechloride

A technology of polyaniline and chlorination, which is applied in the field of preparation of chlorinated polyaniline, and can solve problems such as poor yield

Inactive Publication Date: 2004-01-07
NO 63971 TROOPS PLA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above literatures use haloaniline monomers to directly synthesize polyhaloanilines through free radical polymerization. The chemical structure is relatively clear, but the yield is not good.

Method used

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  • Process for preparing polyanilinechloride

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Experimental program
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Effect test

Embodiment 1

[0012] Add 3.0g (33mmol) polyaniline, 11.0g (82mmol) anhydrous aluminum trichloride and 13ml (165mmol) sulfur monochloride successively in 250ml three-neck round bottom flask, then add dropwise 100ml anhydrous acetonitrile, then slowly heat, Continue to stir and reflux for 10h. After the reaction is completed, filter, extract with carbon disulfide ladder for 10 hours, wash 30ml×20 times with 1mol / L hydrochloric acid solution, soak in 0.1mol / L ammonia water (pH=8~9) overnight, wash 20ml×15 times with 0.1mol / L ammonia water , and finally vacuum-dried at 60° C. for 24 hours to obtain 6.0 g of black powdery solid chlorinated polyaniline with a yield of 93%. The elemental analysis results (wt%) are: C 37.64, N 7.66, H1.10, S 3.18, Cl 50.32. FT-IR (KBr, cm -1 ): 3375, 3057, 1671, 1582, 1474, 1359, 1223, 1127, 1080, 1036, 866, 819, 574. The scanning electron microscope spectrum of chlorinated polyaniline is shown in the accompanying drawing.

Embodiment 2

[0014] Add 4.50g (49.5mmol) of polyaniline, 36.5g (272mmol) of anhydrous aluminum trichloride and 24ml (165mmol) of sulfur monochloride successively into a 250ml three-neck round bottom flask, then add 150ml of anhydrous DMF dropwise, and then slowly heat , Continue stirring and reflux reaction for 12h. After the reaction is complete, filter, wash with ether 100ml×5 times, carbon disulfide 50ml×8 times, deionized distilled water 50ml×10 times, then soak with 250ml 1mol / L ammonia water (pH=8~9) overnight, and then wash with 0.1mol / L ammonia water washing 50ml×10 times, and finally vacuum drying at 80° C. for 48 hours to obtain 9.3 g of black powdery solid chlorinated polyaniline with a yield of 97%. The elemental analysis results (wt%) are: C 33.83, N6.86, H 0.92, S 5.20, Cl 48.36. FT-IR (KBr, cm -1 ): 3380, 1586, 1477, 1230, 1128, 1079, 1037, 945, 825, 707, 481.

Embodiment 3

[0016] Add 3.5g of polyaniline, 3.8ml of phenylhydrazine, and 100ml of anhydrous ether into a 150ml round bottom flask, and react at room temperature for 8h. After the reaction, filter, wash with ether 30ml x 6 times, and then vacuum-dry at 80°C for 6h to obtain 3.5g black powdery solid reduced polyaniline.

[0017] Add 0.50 g of reduced polyaniline, 3.30 g of anhydrous aluminum trichloride and 2.2 ml of sulfur monochloride to a 100 ml single-necked round-bottom flask in sequence, then add dropwise 30 ml of anhydrous acetonitrile, and then continue stirring and heating under reflux for 10 h. After the reaction is completed, filter, extract with carbon disulfide ladder for 10 hours, wash 30ml×20 times with 1mol / L hydrochloric acid, soak in 150ml 0.1mol / L ammonia water for 24h, then wash 30ml×15 times with 0.1mol / L ammonia water, and finally vacuum-dry at 60°C After 24 hours, 1.0 g of black powdery solid chlorinated polyaniline was obtained with a yield of 95%. The elemental an...

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Abstract

The present invention relates to a preparation method of chloropolyaniline, and is characterized by that the polyailine and sulfur monochloride are heated and returned under the action of lewis acid catalysis in the polar aprotic solvent so as to obtain the invented chloropolyaniline. Every 6 carbon atoms of the chloropolyaniline contain 2-3 chlorine atoms, and its yield rate is up to 93-97%, it can be used as precursor raw material of positive material of lithium secondary cell.

Description

Technical field [0001] The invention relates to a preparation method of chlorinated polyaniline, especially a preparation method of polychlorinated polyaniline. Background technique [0002] Since the first chemical synthesis of conductive polyaniline by MacDiarmid A.G. et al. in 1987, people have carried out extensive and in-depth research on polyaniline and its derivatives, but there are few reports on polyaniline derivatives containing electron-withdrawing halogen functional groups on the benzene ring. Korean Kang D.P. et al. used 2-chloroaniline and 2-fluoroaniline monomers to prepare poly-2-chloroaniline and poly-2-fluoroaniline through free radical polymerization under the oxidation of chromic acid. No reaction product was introduced. rate, but dissected the impact of the monomer structure on the polymerization reaction. The author believes that the greater the electronegativity of the substituent group contained on the monomeric benzene ring, the lower the oxidation ...

Claims

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Application Information

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IPC IPC(8): C08G73/02
Inventor 苑克国杨裕生王安邦
Owner NO 63971 TROOPS PLA
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