Conductive poly 3,4-ethylene dioxy thiophene film and preparation method thereof

A technology of ethylenedioxythiophene and conductive polymerization, which is applied in the direction of electrolytic components, electrolytic process, electrolytic organic production, etc., can solve the problems of unfavorable product separation, unsuitable for large-scale production, human body and environmental hazards, and achieve convenient polymerization speed Effects of regulation, ease of separation and purification, and improved polymerization efficiency

Inactive Publication Date: 2012-08-29
WUHAN UNIV
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

"Non-aqueous system" polymerization: that is, using organic solvents (cyanide is the most common) or ionic liquids as solvents, dissolving both the supporting electrolyte and the monomers in this solvent for polymerization, however, due to the choice of organic solvents or preparation of ionic liquids The raw materials have certain toxicity, which will cause harm to the human body and the environment, and the cost of supporting electrolytes used in these systems is relatively high, so "non-aqueous system polymerization" is facing environmental and economic pressures
"Emulsion system" polymerization: that is, to form an emulsion by adding surfactants or ultrasound to increase the solubility of monomers in water, which can promote efficient polymerization and avoid the use of toxic reagents. However, due to surface activity The participation of additives is not conducive to the separation of products. Although the ultrasonic emulsification method does not introduce any foreign substances and has high polymerization efficiency, the emulsion has a short stable time and is only suitable for small-scale production in a short period of time.
[0004] The traditional homogeneous system electrochemical polymerization can effectively control the synthesis of conductive polymers by adjusting the electrode potential. The product components are simple and easy to separate, but the polymerization is limited to the surface of the working electrode, and the size and shape of the generated conductive polymer film are directly affected by It is controlled by the selected working electrode, and because the generated polymer adheres to the surface of the working electrode, it needs to be used together with the working electrode or scraped off the polymer from the surface of the working electrode, which is not suitable for large-scale production, and also faces Choice of solvent and supporting electrolyte

Method used

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  • Conductive poly 3,4-ethylene dioxy thiophene film and preparation method thereof
  • Conductive poly 3,4-ethylene dioxy thiophene film and preparation method thereof
  • Conductive poly 3,4-ethylene dioxy thiophene film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 carries out electrochemical polymerization at the liquid-liquid interface formed by dichloromethane and water

[0026] First take a certain amount of monomer ethylenedioxythiophene (EDOT) and supporting electrolyte lithium perchlorate (LiClO 4 ) were dissolved in the organic solvent chloroform and water respectively to prepare 0.01 mol / L EDOT chloroform solution and 0.1 mol / L LiClO 4 aqueous solution; sequentially take a certain volume of EDOT chloroform solution and LiClO 4 aqueous solution in figure 1 In the single-port polymerization device shown, a clear liquid-liquid interface is formed; then a certain length of platinum wire working electrode (0.5 mm in diameter) is vertically and slowly inserted into the liquid-liquid interface, and the platinum wire is ensured to slightly exceed the liquid-liquid interface and penetrate deep into the liquid-liquid interface. The oil phase is about 0.5 mm, and the platinum auxiliary electrode and saturated calomel ...

Embodiment 1 and comparative example 1

[0030] Embodiment 1 is in 0.01 mol / L EDOT trichloromethane solution and 0.1 mol / L LiClO 4 The liquid-liquid interface formed by the aqueous solution, in comparative example 1, was polymerized by cyclic voltammetry in 0.01 mol / L EDOT aqueous solution, the potential range: 0.2 V ~ 1.6 V, and the scanning speed: 20 mV / s. The cyclic voltammetry curve in the polymerization process of embodiment 1 and the macroscopic appearance of the conductive polymer film of generation see respectively image 3 a, b, the ring voltammetry curve of comparative example 1 polymerization process sees Figure 4 (The arrows in the figure indicate the direction and trend of current change).

[0031] Compared image 3 a and Figure 4It can be clearly seen that the cyclic voltammetry curve of the process of preparing the conductive polymer in the present invention shows a very different behavior from that of the polymerization in the traditional homogeneous system, especially in the oxidation potential ...

Embodiment 2

[0033] First take a certain amount of monomer ethylenedioxythiophene (EDOT) and supporting electrolyte perchloric acid (HClO 4 ) were dissolved in organic solvent dichloroethane and water respectively, and made into 1 mol / L EDOT dichloroethane solution and 2 mol / L HClO 4 aqueous solution; sequentially take a certain volume of EDOT dichloroethane solution and HClO 4 aqueous solution in figure 1 In the single-port polymerization device shown, a clear liquid-liquid interface is formed; then a certain length of platinum wire working electrode (0.5 mm in diameter) is vertically and slowly inserted into the liquid-liquid interface, and the platinum wire is ensured to slightly exceed the liquid-liquid interface and penetrate deep into the liquid-liquid interface. The oil phase is about 0.5 mm, and the platinum auxiliary electrode and saturated calomel (SCE) reference electrode are inserted into the upper layer of HClO 4 In aqueous solution; using a constant potential of 1.4V ( vs...

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Abstract

The invention discloses a conductive poly 3,4-ethylene dioxy thiophene film and a preparation method thereof. The method is characterized by comprising the following steps: resolving a poly 3,4-ethylene dioxy thiophene monomer in an organic solvent, resolving supporting electrolyte into water, and preparing into solutions; transferring the two solutions stepwise into an reactor, thus forming a liquid-liquid interface; inserting a working electrode in the liquid-liquid interface; placing an auxiliary electrode and a reference electrode in the supporting electrolyte solution; and carrying out electrochemical polymerization by utilizing an electrochemistry means. The invention has the advantages that the prepared poly 3,4-ethylene dioxy thiophene film has good conductivity, and the topography has obvious dual character. One side, which is close to the water phase, of the conductive poly 3,4-ethylene dioxy thiophene film is a nano smooth film; the other side, which is close to the oil phase, of the conductive poly 3,4-ethylene dioxy thiophene film is a micrometer ordered cellular porous film; and a high reaction area is revealed, and the conductive poly 3,4-ethylene dioxy thiophene film can be used for positive electrode materials and negative electrode materials of super capacitors and batteries, electromagnetic shielding materials and the like.

Description

technical field [0001] The invention relates to a conductive poly-3,4-ethylenedioxythiophene film and its preparation method, in particular to a conductive poly-3,4-ethylenedioxythiophene film with a unique micro-nano structure and its preparation method, belonging to polymer materials field. Background technique [0002] Conjugated conductive polymers such as polypyrrole, polyaniline, polythiophene and their derivatives have unique structural characteristics, doping mechanism, and excellent physical and chemical properties, making them a hot field of materials science in the late 20th century. widespread attention from science and industry. Poly(3,4-ethylenedioxythiophene) (abbreviated as PEDOT), developed by Bayer Company in Germany in the late 1980s, has attracted much attention due to its excellent properties such as high conductivity, high stability, and high transparency. [0003] At present, the preparation methods of conductive polymers mainly include chemical poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L65/00C08G61/12C25B3/00B82Y30/00B82Y40/00
Inventor 汪的华高丽丽朱华
Owner WUHAN UNIV
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