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Carbonyl-containing covalent organic framework KT-Tp COFs material as well as preparation method and application thereof

A covalent organic framework and carbonyl technology, applied in the field of carbonyl-containing covalent organic framework materials, can solve problems such as poor durability and low capacitance

Active Publication Date: 2020-05-29
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most electrodes based on COFs face the challenge of relatively low capacitance or poor durability.

Method used

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  • Carbonyl-containing covalent organic framework KT-Tp COFs material as well as preparation method and application thereof
  • Carbonyl-containing covalent organic framework KT-Tp COFs material as well as preparation method and application thereof
  • Carbonyl-containing covalent organic framework KT-Tp COFs material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation method of 2,7-diaminopyrene-4,5,9,10-tetraketone (I-2), comprises the steps:

[0050] 1) Synthesis of pyrene-4,5,9,10-tetraketone (II):

[0051] Pyrene reacts with potassium periodate and ruthenium chloride to generate pyrene-4,5,9,10-tetraketone (II); according to the literature J.Org.Chem.2005,70,707-708.

[0052] 2) Synthesis of 2,7-dinitropyrene-4,5,9,10-tetraketone (III):

[0053] Weigh pyrene-4,5,9,10-tetraketone (II, 5g, 3.8mmol) into a 250mL two-neck round bottom flask, add concentrated sulfuric acid (50mL), then slowly add fuming nitric acid (50mL ). The device was placed in an oil bath at 85°C and refluxed for 45 minutes. After the reaction solution was cooled to room temperature, it was poured into a beaker filled with ice. After the ice was completely melted, it was suction filtered. The filter cake was washed with water and dried in vacuum at room temperature. , to obtain light yellow solid 2,7-dinitropyrene-4,5,9,10-tetraketone (III) (5....

Embodiment 2

[0060] A method for preparing a carbonyl-containing covalent organic framework KT-Tp COFs material ((IV-1), abbreviated as 2KT-Tp COF), comprising the following steps:

[0061] In a 10 mL Schlenk tube, mix 2,7-diamino-9,10-phenanthrenequinone (I-1, 17.9 mg, 0.075 mmol) and 1,3,5-triformylphloroglucinol (V, 10.5 mg, 0.05mmol) was dispersed in a mixed solution of 1,4-dioxane (0.2mL) and mesitylene (0.8mL); sonicated for 2min to obtain a uniform dispersion, and then 0.1mL of 36% acetic acid was added Aqueous solution, sonicated for 2 minutes, frozen and degassed under argon three times, placed the Schlenk tube at 120°C for 3 days, cooled to room temperature, filtered to collect the precipitate, and successively washed with N,N-dimethylacetamide, Washed with tetrahydrofuran and acetone, dried in vacuo to give a black powder (IV-1, 26 mg, yield 91%).

[0062]

[0063] figure 2 The powder XRD diffraction pattern of 2KT-Tp COF prepared in Example 2 proves that 2KT-Tp COF is a t...

Embodiment 3

[0065] A method for preparing a carbonyl-containing covalent organic framework KT-Tp COFs material ((IV-2), abbreviated as 4KT-Tp COF), comprising the following steps:

[0066] In a 10 mL Schlenk tube, mix 2,7-diaminopyrene-4,5,9,10-tetraketone (I-2, 21.9 mg, 0.075 mmol) and 1,3,5-triformylphloroglucinol ( V, 10.5mg, 0.05mmol) was dispersed in 1,4-dioxane (10mL); sonicated for 2min to obtain a uniform dispersion, then added 0.2mL of 36% acetic acid aqueous solution, sonicated for 2min, and frozen And degas three times under argon, put the Schlenk tube at 120 ° C for 3 days, after cooling to room temperature, filter to collect the precipitate, wash with N,N-dimethylacetamide, tetrahydrofuran and acetone successively, and vacuum dry , to obtain a black powder (IV-2, 29 mg, yield 89%).

[0067]

[0068] image 3 The powder XRD diffraction pattern of 4KT-Tp COF prepared in Example 3 proves that 4KT-Tp COF is a two-dimensional covalent organic framework material with good crys...

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Abstract

The invention discloses a carbonyl-containing covalent organic framework KT-Tp COFs material as well as a preparation method and application thereof. The carbonyl-containing covalent organic frameworkKT-Tp COFs material has a structure represented by a formula (IV), wherein m is equal to 0-2, and n is equal to 2; an o-quinone structure is introduced into a COFs skeleton, and experimental resultsshow that the COFs skeleton with the o-quinone structure has better energy storage performance than COFs with only isolated carbonyl, and the carbonyl-containing covalent organic framework KT-Tp COFsmaterial is applied to capacitors.

Description

technical field [0001] The invention belongs to the field of macromolecular organic porous materials, in particular to a class of carbonyl-containing covalent organic framework material KT-Tp COFs, a preparation method and application. Background technique [0002] Currently, electrochemical energy is considered as one of the promising sustainable energy sources due to its efficient storage and conversion. Representative electrochemical energy storage devices include batteries, fuel cells, and supercapacitors, etc. In the mid-term, supercapacitors have received extensive attention due to their advantages such as ultra-fast charge and discharge, high energy density, excellent specific capacity and long service life. Electrode materials play a crucial role in the performance of supercapacitors. So far, great progress has been made in the development of carbon-based electrode materials, but carbon-based materials usually exhibit low capacitance due to the lack of redox groups...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C225/34C07C221/00C08G73/00H01G11/24H01G11/30
CPCC07C225/34C08G73/00H01G11/24H01G11/30
Inventor 陈龙李淼刘婧娟
Owner TIANJIN UNIV
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