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Polymer film PEFE with D-A-D structure and preparation method and application thereof

A D-A-D, structural polymer technology, applied in the direction of hybrid capacitor electrolyte, etc., to achieve the effect of high specific capacity and stability

Inactive Publication Date: 2020-03-31
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem of how to display the working state in the supercapacitor energy storage process, the object of the invention is to provide a D-A-D structure polymer film PEFE of a supercapacitor polymer film electrode material with obvious color change under its operating voltage range and Its preparation method and application

Method used

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  • Polymer film PEFE with D-A-D structure and preparation method and application thereof
  • Polymer film PEFE with D-A-D structure and preparation method and application thereof
  • Polymer film PEFE with D-A-D structure and preparation method and application thereof

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Effect test

Embodiment 1

[0027] refer to Figure 1 to Figure 5 , a D-A-D structure polymer film PEFE, prepared according to the following method:

[0028] (1) Synthesis of monomeric EFE

[0029] For 3,4-ethylenedioxythiophene (EDOT) tinning, EDOT (6mmol, 0.852g) was dissolved in dry tetrahydrofuran (40mL) at -78°C under N 2 Under the atmosphere, slowly add n-butyllithium (6.6mmol, 4.125mL, 1.6M) dropwise, slowly raise the temperature to -40°C, stir for 1h, then cool down to -78°C, slowly add dropwise tributyltin chloride (7.2mmol , 2.347g), and stirred at room temperature for 8h, filtered through a neutral alumina column to remove solid impurities, and obtained the product tributyl (2,3-dihydro[3,4-b][1,4]dioxin -5-yl) stannane, 2,7-dibromo-9 fluorenone (3mmol, 1.014g), tributyl(2,3-dihydro[3,4-b][1,4]diox In-5-yl) stannane (6mmol, 2.593g) and bistriphenylphosphine palladium dichloride (0.025mmol, 0.01755g) in N 2 Dissolve in 50ml of dry toluene under atmosphere, heat to 110°C and keep reflux for ...

Embodiment 2

[0035] A D-A-D structure polymer membrane PEFE is prepared according to the following method:

[0036] (1) Synthesis of monomeric EFE

[0037] For 3,4-ethylenedioxythiophene (EDOT) tinning, EDOT (6mmol, 0.852g) was dissolved in dry tetrahydrofuran (40mL) at -78°C under N 2 Under the atmosphere, slowly add n-butyllithium (6.6mmol, 4.125mL, 1.6M) dropwise, slowly raise the temperature to -40°C, stir for 1h, then cool down to -78°C, slowly add dropwise tributyltin chloride (7.2mmol , 2.347g), and stirred at room temperature for 8h, filtered through a neutral alumina column to remove solid impurities, and obtained the product tributyl (2,3-dihydro[3,4-b][1,4]dioxin -5-yl) stannane. 2,7-Dibromo-9-fluorenone (3mmol, 1.014g), tributyl(2,3-dihydro[3,4-b][1,4]dioxin-5-yl)stannane (6mmol, 2.593g) and bistriphenylphosphine palladium dichloride (0.025mmol, 0.01755g) in N 2 Dissolve in 50ml of dry toluene under atmosphere, heat to 110°C and keep reflux for 36 hours. After the system w...

Embodiment 3

[0043] A D-A-D structure polymer membrane PEFE is prepared according to the following method:

[0044] (1) Synthesis of monomeric EFE

[0045] For 3,4-ethylenedioxythiophene (EDOT) tinning, EDOT (6mmol, 0.852g) was dissolved in dry tetrahydrofuran (40mL) at -78°C under N 2 Under the atmosphere, slowly add n-butyllithium (6.6mmol, 4.125mL, 1.6M) dropwise, slowly raise the temperature to -40°C, stir for 1h, then cool down to -78°C, slowly add dropwise tributyltin chloride (7.2mmol , 2.347g), and stirred at room temperature for 8h, filtered through a neutral alumina column to remove solid impurities, and obtained the product tributyl (2,3-dihydro[3,4-b][1,4]dioxin -5-yl) stannane. 2,7-Dibromo-9-fluorenone (3mmol, 1.014g), tributyl(2,3-dihydro[3,4-b][1,4]dioxin-5-yl)stannane (6mmol, 2.593g) and bistriphenylphosphine palladium dichloride (0.025mmol, 0.01755g) in N 2 Dissolve in 50ml of dry toluene under atmosphere, heat to 110°C and keep reflux for 36 hours. After the system w...

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Abstract

The invention discloses a polymer film PEFE with a D-A-D structure. A preparation method for the polymer film PEFE comprises the following steps: (1) mixing 2,7-dibromo-9-fluorenone with pre-preparedtributyl(2,3-dihydro[3,4-b][1,4]dioxin-5-yl)stannane and bis(triphenylphosphine)palladium dichloride in proportion, dissolving the formed mixture in an organic solvent in a nitrogen environment, carrying out a reaction at a reflux temperature to obtain a reaction mixed solution, conducting extracting, and performing separating with a silica gel column to obtain a monomer EFE; and (2) dissolving aD-A-D monomer EFE and an electrolyte in a supporting electrolytic solvent to obtain an electrolyte, adding the electrolyte into an electrolytic tank three-electrode system, connecting the electrolytictank three-electrode system with an electrochemical workstation, carrying out an electrochemical CV polymerization reaction under polymerization voltage, cleaning a film with an organic solvent chromatographic-grade mixed solution, and carrying out drying. The invention further provides a preparation method and application of the polymer film PEFE with the D-A-D structure. The polymer film PEFE has obvious color change, and high specific capacity and stability.

Description

technical field [0001] The invention relates to a polymer film with high specific capacity and high stability, a preparation method and application thereof, which can be applied in the direction of electrochromic supercapacitors. Background technique [0002] In recent years, with the development of portability of electronic equipment, energy storage devices that can display working status have become more and more important. Electrochromism is a reversible change in the transmission or reflection of light by changing the magnitude of the operating voltage, and the material undergoes a redox reaction, which reflects a reversible change in color in appearance. It is a more feasible way to display the energy storage state of energy storage devices through color changes, but the preparation of materials with large specific capacity, high contrast and good stability that can meet this demand has become a major problem. [0003] In supercapacitors, compared with metal oxide mate...

Claims

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Application Information

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IPC IPC(8): C08G61/12C08J5/18H01G11/56
CPCC08G61/126C08J5/18H01G11/56C08G2261/11C08G2261/3243C08G2261/44C08G2261/54Y02E60/13
Inventor 刘军磊许若腾张诚罗俊涛
Owner ZHEJIANG UNIV OF TECH
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