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Application of oxygen-nitrogen free radical group containing triphenylamine derivate polymer containing as electrochromic material

A free radical and triphenylamine technology, which is applied in the field of triphenylamine derivative polymers, can solve the problems of poor uniformity of film formation, increased production costs, and complex chemical preparation processes, achieving low cost, short response time, and good stability Effect

Active Publication Date: 2016-03-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All of the above are triphenylamine derivative polymer films prepared by chemical polymerization, but the preparation process of chemical method is relatively complicated, which increases the preparation cost, and the uniformity of film formation is relatively poor.

Method used

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  • Application of oxygen-nitrogen free radical group containing triphenylamine derivate polymer containing as electrochromic material
  • Application of oxygen-nitrogen free radical group containing triphenylamine derivate polymer containing as electrochromic material
  • Application of oxygen-nitrogen free radical group containing triphenylamine derivate polymer containing as electrochromic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1: the electrochemical synthesis of PTPAT

[0054] (1) Synthesis of 4-diphenylaminobenzonitrile

[0055] Add 50 mL of anhydrous N,N-dimethylformamide (DMF) to a pre-dried 250 mL three-neck flask, followed by sodium hydride (1.5 g), and stir well to remove a large number of bubbles generated during the dissolution process. When no bubbles are generated, diphenylamine (III) (5.1 g) is added and the temperature is raised to 110° C., the reaction solution turns green tea green, then p-fluorobenzonitrile (IV) (4.5 g) is added, and the reaction solution turns dark red. in N 2 Under the protection of the reaction 12h to reach the end of the reaction. The crude reaction product was washed and extracted with dichloromethane and water, and the oil phase extract was dried, and then the solvent was removed by a rotary evaporator, and the remaining product after rotary evaporation was separated and purified by column chromatography. The stationary phase was 300 mesh sil...

Embodiment 2

[0066] Example 2: Electrochromism of PTPAT in Acetonitrile

[0067] The PTPAT polymer thin film that is attached to the ITO glass prepared in embodiment 1 is put into three-electrode electrolytic cell, is dissolved with 10 in the cell -2 mol / LLiClO 4 / acetonitrile solution as the electrolytic solution, wherein the working electrode is ITO glass with PTPAT polymer film, the counter electrode is platinum wire, and the reference electrode is silver-silver chloride electrode. Cyclic voltammetry was used for scanning, the scanning voltage range was 0.4V-1.2V, the scanning speed was 100mV / s, and the scanning was performed for 300 cycles. It can be observed with the naked eye that the film changes from yellow to dark green as the voltage increases, and when the voltage decreases, the color turns back to yellow, and so on. The relationship between the redox peak on the cyclic voltammetry curve and the color of the polymer film was recorded. See Table 1:

[0068] Table 1 The relati...

Embodiment 3

[0070] Embodiment 3: the electrochromic response speed and contrast of PTPAT in acetonitrile The PTPAT polymer thin film that is attached on the ITO glass prepared in embodiment 1 is put into the three-electrode electrolytic cell, is dissolved with 10 -2 mol / LLiClO 4 / acetonitrile solution as the electrolytic solution, wherein the working electrode is ITO glass with PTPAT polymer film, the counter electrode is platinum wire, and the reference electrode is silver-silver chloride electrode. The combined technology of electrochemical workstation and ultraviolet spectrometer is adopted. The electrochemical workstation is set to multi-potential step method, the ultraviolet spectrum is set to ultraviolet absorption, and the scanning range is 1100-300nm. The final data obtained as Figure 5 as shown, Figure 5 It can be seen that under the condition of neutral state 0V, PTPAT has an absorption peak at 409nm, which is attributed to the π-π of the polymer main chain. * The characte...

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Abstract

The invention discloses an application ofoxygen-nitrogen free radical group containing triphenylamine derivate polymer as an electrochromic material. The structure of the triphenylamine derivate polymer is shown as the formula (1), and in the formula (1), n represents the average degree of polymerization, and n ranges from 10 to 2,000. Compared with other existing electrochromic materials, the prepared electrochromic material has short response time, the large color contrast ratio and good stability, when the electrochromic material is tested at the position of the visible wavelength of 1,100 nm, the contrast ratio is 47.3%, the response time is 0.43 s, and 96.8% of initial electrochemical activity is still kept after cyclic voltammetry continuous scanning is carried out for 300 circles. The formula I is shown in the specification.

Description

technical field [0001] The invention belongs to the technical field of electrochromic materials, and in particular relates to the application of a triphenylamine derivative polymer containing oxygen and nitrogen free radical groups as an electrochromic material, and the electrochromic polymer can be used in electrochromic devices . Background technique [0002] Electrochromism refers to the reversible transformation of the optical properties of materials in the visible wavelength range through the injection and extraction of carriers under the action of an external electric field. Since Deb.S.K first discovered WO in 1969 3 Since the electrochromic phenomenon of thin films and the mechanism of "oxygen vacancy color center" were proposed, a large number of electrochromic materials have been studied. Early research on electrochromic materials mainly focused on inorganic electrochromic materials, such as WO 3 , IrO 2 , NiO and other transition metal oxides, followed by Prus...

Claims

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Application Information

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IPC IPC(8): C09K9/02C08G61/12C25B3/10C25B3/29
CPCC09K9/02C08G61/122C08G2261/3162C08G2261/44C08G2261/54C09K2211/1466C25B3/29
Inventor 张诚纪律律苏畅徐立环吕耀康欧阳密杨芳戴玉玉蔡志威朱晓刚何晖晖
Owner ZHEJIANG UNIV OF TECH
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