Non-catalytic efficient preparation method of two-dimensional fluorine-containing covalent organic framework compound

A covalent organic framework and compound technology, which is applied in the field of non-catalytic and efficient preparation of two-dimensional fluorine-containing covalent organic framework compounds, can solve the problems of long reaction time, difficulty in synthesizing crystalline products, and the need for catalysts, etc., and achieve a simple reaction process , high yield, enhanced electrophilicity

Active Publication Date: 2019-04-05
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that the existing reaction time is long, a catalyst is needed, and it is difficult to synthesize a product with good crystallinity

Method used

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  • Non-catalytic efficient preparation method of two-dimensional fluorine-containing covalent organic framework compound
  • Non-catalytic efficient preparation method of two-dimensional fluorine-containing covalent organic framework compound
  • Non-catalytic efficient preparation method of two-dimensional fluorine-containing covalent organic framework compound

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A non-catalytic and efficient preparation method of a two-dimensional fluorine-containing covalent organic framework compound, comprising the following steps:

[0035] 1) Weigh 2,3,5,6-tetrafluoroterephthalaldehyde (82.4mg) and 2,4,6-tris(4-aminophenyl)-1,3,5 with a molar ratio of 1:1.5 - Triazine (94.4mg) in a 2mL heat-resistant glass tube, add 1mL dioxane / mesitylene (v / v=1:1) solvent;

[0036] 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 a 120°C oven for 5 minutes, and obtain the crude product;

[0037] 3) The crude product was taken out and filtered, washed with tetrahydrofuran solution, drained, wrapped with clean filter paper, put into a Soxhlet extractor, and washed with tetrahydrofuran solution at 100°C for 12 hours under reflux;

[0038] 4) Take out the product after reflux washing, and put it into the separat...

Embodiment 2

[0040] A non-catalytic and efficient preparation method of a two-dimensional fluorine-containing covalent organic framework compound, comprising the following steps:

[0041] 1) Weigh 2,3,5,6-tetrafluoroterephthalaldehyde (82.4mg) and 2,4,6-tris(4-aminophenyl)-1,3,5 with a molar ratio of 1:1.5 - Triazine (94.4mg) in a 2mL heat-resistant glass tube, add 1mL dioxane / mesitylene (v / v=1:1) solvent;

[0042] 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, and put it in a 120°C oven for 24 hours to obtain the crude product;

[0043] 3) The crude product was taken out and filtered, washed with tetrahydrofuran solution, drained, wrapped with clean filter paper, put into a Soxhlet extractor, and washed with tetrahydrofuran solution at 100°C for 12 hours under reflux;

[0044] 4) Take out the product after reflux washing, and put it into the separation...

Embodiment 3

[0053] A non-catalytic and efficient preparation method of a two-dimensional fluorine-containing covalent organic framework compound, comprising the following steps:

[0054] 1) Weigh 2,3,5,6-tetrafluoroterephthalaldehyde (82.4mg) and 2,4,6-tris(4-aminophenyl)-benzene (93.6mg) with a molar ratio of 1:1.5 In a 2mL heat-resistant glass tube, add 1mL of dioxane / mesitylene (v / v=1:1) 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. The glass tube was sonicated for 20 minutes, and placed in an oven at 180° C. for 1 minute to obtain a crude product.

[0056] 3) The crude product was taken out and filtered, washed with tetrahydrofuran solution, drained, wrapped with clean filter paper, put into a Soxhlet extractor, and washed with tetrahydrofuran solution at 100°C for 12 hours under reflux;

[0057] 4) Take out the product after reflux washing, and dry it (put it in an ov...

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Abstract

The invention discloses a non-catalytic efficient preparation method of a two-dimensional fluorine-containing covalent organic framework compound. The method comprises dispersing monomer materials into organic solvent, and performing liquid nitrogen freezing-vacuumizing-degassing treatment, sealed ultrasonic treatment and temperature-controlled reaction to obtain a crude product; filtering, washing and drying the crude product to obtain the two-dimensional fluorine-containing covalent organic framework compound. The non-catalytic efficient preparation method of the two-dimensional fluorine-containing covalent organic framework compound saves catalysts and can produce products high in performance through 5-minute reaction; the prepared two-dimensional fluorine-containing covalent organic framework compound is high in specific surface area and has an orderly mesoporous structure containing a large number of fluorine atoms, thereby having a potential application prospect in aspects of gasadsorption and storage, ion adsorption and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a non-catalytic and efficient preparation method of a two-dimensional fluorine-containing covalent organic framework (COFs) compound. Background technique [0002] Covalent organic frameworks (COFs) are a new class of organic porous materials composed of light atoms such as C, H, O, N, and B, which are connected by covalent bonds. In 2005, the Omar.Yaghi group of the University of California, Berkeley Reported (A.P. Cote, Science. 310 (2005) 1166-1170.). The outstanding properties of COFs, such as good material stability, low density, large specific surface area, rich pore structure, strong designability, and various monomers, make them ideal for gas storage, adsorption, catalysis, photoelectricity, energy storage, and biological drug loading. All aspects have a wide range of applications. [0003] At present, the most commonly used method for preparing co...

Claims

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Application Information

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