Controllable preparation method based on covalent organic framework and energy storage application thereof

A technology of covalent organic framework and covalent organic framework, which is applied in the direction of hybrid capacitor electrodes, etc., can solve the problems of inability to precisely control the morphology and size of COFs materials, and the inability to give full play to the advantages of microstructure, so as to improve the morphology and shape of amorphous materials. Uncontrollable effects of the growth process

Active Publication Date: 2019-11-22
LANZHOU JIAOTONG UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the lack of effective control of various factors in the solvothermal polymerization process, it is often impossible to accurately control the morphology and size of COFs materials in the actual preparation process, resulting in the inability to give full play to the advantages of its microstructure in the energy storage process.

Method used

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  • Controllable preparation method based on covalent organic framework and energy storage application thereof
  • Controllable preparation method based on covalent organic framework and energy storage application thereof
  • Controllable preparation method based on covalent organic framework and energy storage application thereof

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Embodiment 1

[0050] A controllable preparation method based on a covalent organic framework, adding 0.42 g (0.2 mmol) of trihydroxybenzenetricarbaldehyde and 0.65 g (0.3 mmol) of 2,6-diaminoanthraquinone into an agate mortar and grinding Add 6 μL of a mixed solvent of mesitylene and dioxane (1:1) and 0.1 μL of 6 mol / L acetic acid as a catalyst dropwise until the powder turns orange-red. Add the obtained orange-red powder into an ampoule (capacity about 25 mL, tube length 20 cm) containing 12 mL of mesitylene and dioxane (1:1) solution, ultrasonically disperse the mixture evenly, and add 0.6 mL of 6 mol / L acetic acid solution. Then the system was frozen with liquid nitrogen, the tube was sealed and evacuated, sealed with a flame spray gun and placed in an oven at 120 °C for 96 h to ensure that there was no interference. After the oven was cooled to room temperature, the ampoule was taken out, and the obtained product was washed repeatedly with tetrahydrofuran and dichloromethane, respectiv...

Embodiment 2

[0067] A controllable preparation method based on covalent organic framework, adding 0.42 g (0.2 mmol) of trihydroxybenzenetricarbaldehyde and 0.65 g (0.3 mmol) of 2,6-diaminoanthraquinone into a 12 mL mesitylene and dioxane (1:1) solution in an ampoule (capacity about 25 mL, tube length 20 cm), the mixture was ultrasonically dispersed, and 0.6 mL of 6 mol / L acetic acid solution was added dropwise. Then the system was frozen with liquid nitrogen, the tube was sealed and evacuated, sealed with a flame spray gun and placed in an oven at 120°C for 96 hours to ensure that there was no interference. After the oven was cooled to room temperature, the ampoule was taken out, and the obtained product was washed repeatedly with tetrahydrofuran and dichloromethane, and dried in a vacuum oven at 85°C for 12 h to obtain a C-S-COFs electrode material with a simulated flower shape.

[0068] Carry out performance test and characterization to embodiment 2 gained product:

[0069] 1. Infrared ...

Embodiment 3-5

[0084] Except that the polymerization solvent was different, other conditions were the same as in Example 2, and the influence of the polarity of the polymerization solvent on COFs was explored.

[0085] Add 0.42 g (0.2 mmol) of trihydroxybenzenetricarbaldehyde and 0.65 g (0.3 mmol) of 2,6-diaminoanthraquinone into an ampoule containing 12 mL of mesitylene solution (capacity about 25 mL, tube length 20 cm), the mixture was ultrasonically dispersed, and 0.6 mL of 6 mol / L acetic acid solution was added dropwise. Then the system was frozen with liquid nitrogen, the tube was sealed and evacuated, sealed with a flame spray gun and placed in an oven at 120 °C for 24 h without any disturbance. After the oven was cooled to room temperature, the ampoule was taken out, and the obtained product (M-COFs) was washed repeatedly with tetrahydrofuran and dichloromethane, respectively, and dried in a vacuum oven at 85 °C for 12 h. Such as Image 6 As shown, M-COFs can be seen assembled into ...

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Abstract

The invention provides a controllable preparation method based on a covalent organic framework and an energy storage application thereof. A covalent organic framework COFs material connected with beta-ketoamide is employed as a main material, and successful introduction of an energy storage component in the COFs material and effective control of the microstructure are realized by designing a topological structure of the COFs material and selecting a polymerization monomer prepolymerization environment of the COFs material; wherein anthraquinone molecules are used as an energy storage component, so that the COFs material can show obvious electrochemical energy storage activity; meanwhile, directional growth of the COFs material in different dimensions is achieved through mechanical grindingand the double induction effect of different reaction solvents in the organic framework unit molecule prepolymerization process, and finally the covalent organic crystal material G-S-COFs energy storage material with the rod cluster-shaped microstructure is obtained. Then, through a solvent-process polymerization step, the flower-shaped covalent organic crystal material C-S-COFs composed of nanosheets can be finally prepared. The method has the advantages that on the basis that the energy storage activity of the COFs material is guaranteed, the defects that the morphology of the COFs materialis amorphous and the growth process is uncontrollable under the solvothermal condition are effectively overcome.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a controllable preparation method based on covalent organic frameworks (COFs) and its energy storage application as a supercapacitor electrode material. Background technique [0002] COFs are a class of porous polymer materials with a periodic crystalline network framework structure formed by dynamic covalent chemical polymerization of light elements (hydrogen, boron, carbon, nitrogen, etc.). Since Professor Yaghi's research group successfully synthesized COFs materials for the first time in 2005, due to their great potential in structural characteristics and performance development, they have aroused strong research interest in the academic community and have been widely used in gas storage and separation, optoelectronic materials , catalysis and energy storage and other fields. [0003] Thanks to the ordered arrangement of structural units at the molec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00H01G11/24H01G11/48
CPCC08G83/008H01G11/24H01G11/48Y02E60/13
Inventor 安宁何媛媛邵珠航吕丽雯吴海超杨茗然胡中爱
Owner LANZHOU JIAOTONG UNIV
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