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Preparation method of poly(3,4-ethylene dithio-thiofuran) aqueous dispersion

A technology of ethylene dithiothiophene and dispersion, which is applied in the field of preparation of polythiophene derivative poly(3,4-ethylene dithiothiophene) aqueous dispersion, which can solve unsuitable scale synthesis, limited processing and application , unstable state and other problems, to achieve the effect of low equipment requirements, simple preparation method, and mild production conditions

Inactive Publication Date: 2012-05-09
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wherein the chemical oxidative polymerization method prepares the polymer solid powder, although its solubility property is better than the PEDOT powder obtained under the same conditions, it can be partially dissolved in some organic solvents or completely dissolved in N-methylpyrrolidone, but these organic The toxicity, corrosiveness, volatility or high boiling point of the solvent greatly limit its processing and application; electrochemical polymerization can only obtain a very small amount of polymer, which is not suitable for large-scale synthesis; although solid-state polymerization avoids the oxidant in the polymerization process The influence of the use of solvents and solvents on the purity of the final polymer, but the polymer is an unstable solid powder, which limits its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A kind of preparation method of poly(3,4-ethylenedithiothiophene) aqueous dispersion

[0017] Under the protection of nitrogen, 0.6134 g (3.517 mmol) of monomer 3,4-ethylenedithiothiophene was added dropwise to 1.5 wt% polystyrene sulfonic acid (weight average molecular weight M w 75,000, 1.231 g) in an aqueous solution, mechanically stirred at a speed of 500 rpm under the condition of a water bath at 25 °C, after 15 minutes, add the oxidant sodium persulfate with a molar ratio of 1.2:1 to the monomer, after 5 minutes, Add ferric sulfate with a molar ratio of 1:0.005 to sodium persulfate, and continue stirring for 24 hours. After the reaction is over, add twice the volume of deionized water to the reaction system to dilute, then add anion (201×7 type) and cation (001×7 type) ion exchange resins in sequence, and keep stirring for 7 hours each time. The sand core funnel was suction filtered to obtain the polymer aqueous dispersion, which was subjected to rotary evaporat...

Embodiment 2

[0019] Preparation of Poly(3,4-Ethylenedithiothiophene) Conductive Thin Film

[0020] The aqueous dispersion of poly(3,4-ethylenedithiothiophene) prepared in Example 1 was used to spread on the substrate by casting film coating method, and the polymer film was obtained after drying treatment. The adopted substrate is PP or PET plastic substrate. The drying conditions used were drying in a blast oven at a temperature of 80 °C for 12 hours. The thickness of the obtained polymer film is 5-10 microns, which can be peeled off from the base material and cut into various shapes. The conductivity of the film is tested by the four-electrode method, and the value is 1.0×10 -4 ~4.5×10 -3 Siemens / cm.

Embodiment 3

[0022] Preparation of poly(3,4-ethylenedithiothiophene) conductive coating

[0023] This embodiment is similar to Embodiment 3, except that the film coating method used is spin coating, and the substrate used is ITO glass. The spin-coating parameters adopted are: cloth glue (600 rpm, 10 seconds), uniform glue (2200 rpm, 18 seconds). The heating conditions adopted are: heating by electric heating plate, the temperature is 60°C, and the heating time is 30-80 seconds. The thickness of the obtained conductive coating is 100-200 nanometers, and the conductivity is 8.0×10 -5 ~3.0×10 -4 Siemens / cm, visible light transmittance 80% to 90%.

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Abstract

The invention relates to a preparation method of a poly(3,4-ethylene dithio-thiofuran) aqueous dispersion. The preparation method comprises the steps of: dropwise adding a monomer 3,4-ethylene dithio-thiofuran to an aqueous solution containing a surfactant, adding an oxidant, and persistently stirring and reacting, wherein the molar ratio of the aqueous solution containing the surfactant to the monomer is (1-3):1; adding deionized water, the volume of which is two times that of the reacted system, to the reacted system for diluting, and then sequentially passing through anion and cation exchange resin columns; carrying out suction filtering by a sand core funnel; and carrying out rotary evaporation on the aqueous dispersion, concentrating, homogenizing and emulsifying to obtain a stable nanoscale poly(3,4-ethylene dithio-thiofuran) aqueous dispersion. The preparation method provided by the invention has the advantages that: the preparation method is simple and easy, the production conditions are mild, the requirements on instruments and equipment are not high, and the finally obtained aqueous dispersion can be easily processed into a conductive film or coating on a substrate.

Description

technical field [0001] The invention belongs to the field of conductive polymer materials, in particular to a method for preparing a polythiophene derivative poly(3,4-ethylenedithiothiophene) aqueous dispersion. Background technique [0002] Conductive polymers are a class of polymer compounds with a conjugated π bond structure. After chemical or electrochemical doping with anions or cations, special conductive polymer materials are formed, including polyacetylene, polythiophene, and polypyrrole. , polyaniline, polyparaphenylene, polycarbazole, polyfluorene, etc. The outstanding advantages of conductive polymers are that they not only have the photoelectric properties of metals and semiconductor materials, but also have good stability and mechanical properties of polymers, are relatively light in weight, and are easy to process. At present, the most successful conductive polymers in the industrial field are polyaniline and polythiophene, especially poly(3,4-ethylenedioxythi...

Claims

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Application Information

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IPC IPC(8): C08J3/03C08G61/12
Inventor 徐景坤陈帅卢宝阳段学民祝丹华郭亮
Owner JIANGXI SCI & TECH NORMAL UNIV
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