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Two-dimensional bromine-containing covalent organic framework compound and preparation method thereof

A technology of covalent organic frameworks and compounds, applied in the field of two-dimensional bromine-containing covalent organic framework compounds and their preparation, can solve problems such as research and reports on two-dimensional COFs materials that have not yet been seen, and achieve rich pores, rich structures, and speed up. The effect of reaction rate

Active Publication Date: 2020-01-14
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The exploration of new structures of covalent organic frameworks (COFs) materials plays an important role in expanding the richness of materials. The introduction of specific functional groups in the structure is conducive to the application of COFs materials in various aspects. At present, no two-dimensional COFs containing bromine has been seen. Materials Research and Reporting

Method used

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  • Two-dimensional bromine-containing covalent organic framework compound and preparation method thereof
  • Two-dimensional bromine-containing covalent organic framework compound and preparation method thereof
  • Two-dimensional bromine-containing covalent organic framework compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0041] A method for preparing a two-dimensional bromine-containing covalent organic framework compound, comprising the steps of:

[0042] 1) Weigh 2,5-dibromobenzene-1,4-dicarbaldehyde (232.94 mg) and 2,4,6-tris(4-aminophenyl)-1,3,5 with a molar ratio of 1:0.7 - Triazine (188.8mg) in a 5mL heat-resistant glass tube, add 2mL of dioxane / mesitylene (v / v=1:1) solvent, without catalyst;

[0043] 2) Freeze the glass tube with liquid nitrogen, evacuate to 0 mbar for three minutes, degas, repeat three times, and seal the vacuum glass tube; ultrasonicate the glass tube for 20 minutes, put it in an oven at 120°C for three days, and obtain the crude product;

[0044] 3) Take out the crude product and filter it, wash it with tetrahydrofuran, drain it, wrap it with clean filter paper and put it into a Soxhlet extractor, and wash it under reflux with THF solution at 110°C for 12 hours;

[0045] 4) Take out the product after reflux washing, and put it into the separation kettle of the super...

Embodiment 2

[0053] A method for preparing a two-dimensional bromine-containing covalent organic framework compound, comprising the steps of:

[0054] 1) Weigh 2,5-dibromobenzene-1,4-dicarbaldehyde (291.9 mg) and 2,4,6-tris(4-aminophenyl)-1,3,5 with a molar ratio of 1:0.1 - Triazine (35.4 mg), 0.1 ml of 6M acetic acid, in a 5 mL heat-resistant glass tube, add 1 mL of dimethyl sulfoxide solvent;

[0055]2) Freeze the glass tube with liquid nitrogen, evacuate to 0 mbar for three minutes, degas, repeat three times, and seal the vacuum glass tube. Sonicate the glass tube for 20 minutes, put it in a 90°C oven for seven days, and obtain the crude product;

[0056] 3) Take out the crude product and filter it, wash it with ethanol, drain it, wrap it with clean filter paper and put it into a Soxhlet extractor, and wash it under reflux with ethanol at 100°C for 72 hours;

[0057] 4) Take out the product after reflux washing, put it into a vacuum oven and dry it at 120° C. for 12 hours. That is, a...

Embodiment 3

[0059] A method for preparing a two-dimensional bromine-containing covalent organic framework compound, comprising the steps of:

[0060] 1) Weigh 2,5-dibromobenzene-1,4-dicarbaldehyde (43.8mg) and 1,3,5-tris(4-aminophenyl)-benzene (158.6mg) with a molar ratio of 1:3 Put 5.0 mg of scandium trifluoromethanesulfonate in a 5 mL heat-resistant glass tube, add 1 mL m-cresol / dimethylformamide (v / v=3:5) solvent;

[0061] 2) Freeze the glass tube with liquid nitrogen, evacuate to 0 mbar for three minutes, degas, repeat three times, and seal the vacuum glass tube. The glass tube was sonicated for 20 minutes, and placed in an oven at 180° C. for 1 minute to obtain a crude product.

[0062] 3) Take out the crude product and filter it, wash it with methanol, drain it, wrap it with clean filter paper and put it into a Soxhlet extractor, and wash it under reflux with methanol at 100°C for 1 hour;

[0063] 4) Take out the product after reflux washing and put it into the separation kettle o...

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Abstract

The invention discloses a two-dimensional bromine-containing covalent organic framework compound and a preparation method thereof. The two-dimensional bromine-containing covalent organic framework compound is prepared by assembling an aldehyde compound 2, 5-dibromobenzene-1, 4-dicarboxaldehyde containing bromine atoms and an amine compound containing three aminophenyl through Schiff base amine-aldehyde condensation reaction. The preparation method comprises the following steps: dispersing a monomer material in an organic solvent, and carrying out liquid nitrogen freezing-vacuumizing-degassingtreatment, sealing and carrying out ultrasonic treatment, and reacting at a controlled temperature to obtain a crude product; and filtering and washing the crude product, and drying to obtain the bromine-containing covalent organic framework compound. The invention discloses the novel functionalized two-dimensional covalent organic framework material which is simple and easy to obtain and can be synthesized through catalytic method and non-catalytic method, and the product has a high specific surface area and a regular and ordered mesoporous structure, contains a large number of bromine atomsand has potential application prospects in the aspects of material post-modification, gas adsorption and storage, biological delivery and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a two-dimensional bromine-containing covalent organic framework (COFs) compound and a preparation method thereof. Background technique [0002] Covalent organic frameworks (COFs) were first reported by the Omar.Yaghi group of the University of California, Berkeley in 2005 (A.P.Cote, Science.310 (2005) 1166-1170.), light by C, H, O, N, B, etc. A new class of organic porous materials composed of atomic atoms linked by covalent bonds. The organic building units are connected together by reversible covalent bonds to form a regular and orderly porous crystalline material. At present, the most common bonding method is imine bond connection, which has high reactivity and can form relatively stable products. It has outstanding physicochemical properties. Properties such as low density, large specific surface area, rich pore structure, strong designability, and vari...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008Y02P20/54
Inventor 袭锴柯灿廖峭波黄新
Owner NANJING UNIV