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The preparation method of polyaniline

A polyaniline and aniline technology, applied in the field of electrode material preparation, can solve the problems of complex polyaniline preparation process, low product polymerization degree, narrow molecular weight distribution, etc., and achieve the effects of low cost, high electrochemical activity, and narrow molecular weight distribution

Active Publication Date: 2016-05-25
HARBIN INST OF TECH AT WEIHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to solve the technical problems of complex preparation process, low degree of product polymerization and poor electrical conductivity of the existing polyaniline, and provide a polyaniline polyaniline with high yield, large output, high electrochemical activity, good conductivity, low cost, and molecular weight distribution. Preparation method of narrow polyaniline

Method used

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  • The preparation method of polyaniline
  • The preparation method of polyaniline
  • The preparation method of polyaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 (the influence of temperature of reaction)

[0028] Taking the 70L reactor as an example, the effective reaction volume is 50L. First add 35L of 3mol / L hydrochloric acid to the reaction kettle, then add 7kg of lithium chloride, stir until it is completely dissolved and cool down to 0°C, then add 2.8kg of aniline, stir for 30min, add 1.05kg of manganese dioxide after cooling down to 0°C, Stir the reaction for 2 hours, then add dropwise 10L of ammonium persulfate solution with a concentration of 620g / L (containing 6.2kg of ammonium persulfate in total, the molar ratio of manganese dioxide to ammonium persulfate is 4:9, the molar ratio of the total amount of oxidant to aniline is 1.3︰1), the ammonium persulfate solution is also used to control the temperature below 5°C in an ice-water bath. The ammonium persulfate solution was added dropwise at a rate of 1 L / h, and the drop was completed in 10 hours, and then the stirring reaction was continued for 12 hours, ...

Embodiment 2

[0044] Embodiment 2 (the influence of oxidizing agent)

[0045] Taking the 70L reactor as an example, the effective reaction volume is 50L. Add 35L of 3mol / L hydrochloric acid into the reaction kettle, then add 7kg of lithium chloride, stir until it is completely dissolved and cool down to 0°C, then add 2.8kg of aniline, stir for 30min, cool down to 0°C, add manganese dioxide, The reaction was stirred for 2 hours, and then the ammonium persulfate solution was added dropwise, and the temperature of the ammonium persulfate solution was also controlled below 5°C with an ice-water bath. The ammonium persulfate solution was added dropwise at a rate of 1 L / h, and the drop was completed in 10 hours, and then the stirring reaction was continued for 12 hours, and the temperature of the reaction kettle was controlled at -15°C during the entire reaction process. After the reaction, use 800-mesh polypropylene filter cloth to suction filter, wash with deionized water, 50 L of water each t...

Embodiment 3

[0056] Embodiment 3 (the influence of hydrogen ion concentration)

[0057] The impact of table 5 hydrogen ion concentration on polyaniline yield and molecular weight

[0058]

[0059] It can be seen from Table 5 that when the concentration of hydrogen ions is 0.5 mol / L, due to the low concentration of hydrogen ions, aniline cations cannot be formed with aniline monomers, resulting in the aniline in the solution being in a molecular state, increasing various side reactions, and a large number of molecules State aniline was oxidized to quinones, resulting in a yield of only 41.9%, a mass-average degree of polymerization of 624, and a high dispersity of 10.23. As the hydrogen ion concentration increases to 1.5mol / L, it is enough to convert all the aniline monomers into aniline cations, and the reaction liquid system is acidic. At this time, aniline can strictly follow the 1,4-position polymerization reaction, and the side reactions are greatly reduced. , the yield increased b...

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Abstract

The invention relates to a preparation method for polyaniline, which solves the technical problems of complex process, low product polymerization degree and poor electric conductivity in existing polyaniline. The preparation method comprises the following steps: dispersing inorganic acid in water; adding an antifreezing agent into a mixture while stirring; cooling the mixture to a temperature below 0 DEG C and then adding aniline into the mixture; after a solution is stirred and reacted, adding manganese dioxide into the solution; uniformly dropwise adding a persulfate solution; then carrying out suction filtration; washing a product by using deionized water and hydrochloric acid, respectively; and drying the product in vacuum to obtain polyaniline. The preparation method for polyaniline can be widely used for preparation of electrode materials.

Description

technical field [0001] The invention relates to a preparation method of an electrode material, in particular to a preparation method of polyaniline. Background technique [0002] Conductive polymers, also known as conductive polymers, refer to compounds with a very large degree of polymerization, whose molecules are linked together by many small repeating structural units or monomers through covalent bonds, and at both ends of the compound When a voltage is applied, a directed movement of electrons occurs in the material. At present, the conductive polymers that have been studied more include polypyrrole, polythiophene, poly-p-phenylene, poly-p-toluene vinylene, and polyaniline. [0003] Among many conductive polymer materials, polyaniline has broad application prospects in practical application because of its cheap raw materials, simple synthesis process, good physical and chemical stability, high electrical conductivity and excellent electrochromic properties, and has bec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02
Inventor 韩家军林海亭程瑾宁仲建
Owner HARBIN INST OF TECH AT WEIHAI
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