A controllable preparation method based on covalent organic framework and its application in energy storage

A covalent organic framework and mechanical technology, applied in the direction of hybrid capacitor electrodes, can solve the problems that the shape and size of COFs materials cannot be precisely controlled, and the advantages of microstructure cannot be fully utilized, so as to improve the shape of the amorphous and growth process. control effect

Active Publication Date: 2021-06-22
LANZHOU JIAOTONG UNIV
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  • 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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  • A controllable preparation method based on covalent organic framework and its application in energy storage
  • A controllable preparation method based on covalent organic framework and its application in energy storage
  • A controllable preparation method based on covalent organic framework and its application in energy storage

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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 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, 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 spe...

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 Figure 6 As shown, M-COFs can be seen assembled into...

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Abstract

The present invention provides a controllable preparation method based on a covalent organic framework and its application in energy storage to β ‑ Ketoamide-linked covalent organic framework COFs materials are the main materials. Through the design of its topology and the selection of the prepolymerization environment of polymerized monomers, the successful introduction of energy storage components in COFs materials and the effective control of microscopic morphology have been achieved. As an energy storage component, anthraquinone molecules can make COFs materials exhibit obvious electrochemical energy storage activities. At the same time, through the double induction of mechanical grinding and different reaction solvents in the prepolymerization process of organic framework unit molecules, COFs materials in different dimensions have been realized. Oriented growth, and finally obtain the covalent organic crystal material G‑S‑COFs energy storage material with a rod-clustered microscopic morphology; directly use the solvent method to polymerize, and finally obtain the flower-shaped covalent organic crystal material C‑S composed of nanosheets -COFs. The advantage of the present invention is that on the basis of ensuring the energy storage activity of the COFs material, it effectively improves the shortcomings of the COFs material's amorphous morphology and uncontrollable growth process under solvothermal conditions.

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 Patents(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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