Spherical covalent organic framework material, preparation method and application thereof

A covalent organic framework, spherical technology, applied in the direction of hybrid capacitor electrodes, etc., can solve the problems of easy introduction of impurities, complex methods, collapse of the shell COFs structure, etc., to achieve rich porosity, simple preparation process, and good thermal stability.

Active Publication Date: 2019-09-20
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the many COFs reported so far, few have a hollow structure, and most of them are prepared by using template molecules. Although the synthesized COFs have good controllability in shape and size, but In the process of etching and removing the template, the structure of the shell COFs often collapses. In addition, this method is relatively complicated and easy to introduce impurities.

Method used

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  • Spherical covalent organic framework material, preparation method and application thereof
  • Spherical covalent organic framework material, preparation method and application thereof
  • Spherical covalent organic framework material, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of monomer 4,4',4",4"'-(9,9'-spirobifluorene-2,2',7,7'-tetrasubstituted)tetraphenylamine:

[0038] 2,2',7,7'-tetrabromo-9,9'-spirobifluorene (1264mg, 2.0mmol), 4-aminophenylboronic acid pinacol ester (2191mg, 10.0mmol), tetrabutyl bromide Ammonium (TBAB) (345mg, 10wt%), catalyst tetrakistriphenylphosphinepalladium (Pd(PPh 3 ) 4 ) is placed in the reaction flask, and the device is sealed to remove oxygen; prepare 2M potassium carbonate aqueous solution, and toluene are respectively deoxidized by nitrogen bubbling, and 20 mL of potassium carbonate aqueous solution and 40 mL of toluene after bubbling deoxygenation are injected into the reaction flask; reflux reaction 72 Hour. After the reaction, the crude product was used as a stationary phase with 100-200 mesh basic alumina, and petroleum ether / ethyl acetate (volume ratio 1:4) was used as an eluent for column chromatography separation and purification to obtain off-white powder. Recrystallization from n...

Embodiment 2

[0043] The preparation method is the same as that in Example 1, the only difference being that the reaction time of step (2) is changed, thereby resulting in a change in the morphology and structure. The reaction time is extended to 12 hours, the small particles of 180-240 nanometers in the product gradually decrease, and the large-size spheres with a diameter of 600-900 nanometers gradually increase, the surface of the spheres is rough, and the inner cavity is a solid structure (see figure 2 with image 3 ). The BET specific surface area of ​​the product is 508m 2 g -1 , used as an electrode material for supercapacitors, the specific capacitance value is 64F / g (see Figure 8 ).

Embodiment 3

[0045] The preparation method is the same as that in Example 1, the only difference being that the reaction time of step (2) is changed, thereby resulting in a change in the morphology and structure. The reaction time is extended to 24 hours, the small particles of 200-500 nanometers in the product are further reduced, and the large-size spheres with a diameter of 600-900 nanometers are further increased, the surface of the spheres is rough, and the inner cavity is a solid structure (see image 3 with Figure 4 ). The product has a specific surface area of ​​550m 2 g -1 , used as an electrode material for a supercapacitor with a specific capacitance of 86F / g (see Figure 8 ).

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Abstract

The invention discloses a spherical covalent organic framework material, a preparation method and application thereof. The spherical covalent organic framework material is of a hollow or solid spherical structure with the diameter controllable within the range of 500-1500 nanometers. The preparation method of the spherical covalent organic framework material comprises the step that under the condition of being free of a template agent, a polyamino monomer and a polyaldehyde monomer of 9,9'-spirobifluorene are subjected to a reversible Schiff base reaction to form a spherical structure. The method is free of a template, the preparation process is simple and easy to operate, the product yield is high, and the product has good thermal stability. The preparation method can realize controllable structure, and can obtain the spherical covalent organic framework material with a hollow or solid spherical structure. The spherical covalent organic framework material has a large specific surface area and a rich pore structure, is conveniently functionally compounded with other materials, and has a wide application prospect in the fields of gas storage and separation, catalysis, sensing, energy storage and conversion, drug delivery and the like.

Description

technical field [0001] The invention belongs to the technical field of organic functional materials, in particular to a spherical covalent organic framework material and its preparation method and application. Background technique [0002] Spherical covalent organic frameworks (COFs) are a new class of crystalline porous polymers emerging in the last ten years, and are a research hotspot in the field of polymer science. The biggest feature of this kind of material is that it has rich porosity, regular and ordered pore structure, low skeleton density, and high specific surface area. It has been used in gas storage and separation, catalysis, sensing, energy storage and conversion, pharmaceuticals Transportation and many other fields have shown broad application prospects. [0003] The comprehensive properties of porous materials are not only related to their chemical composition, skeleton structure, and porosity, but also closely related to their nanomorphology. The controll...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/08H01G11/48
CPCC08G12/08H01G11/48Y02E60/13
Inventor 赖文勇刘园园李祥春黄维
Owner NANJING UNIV OF POSTS & TELECOMM
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