Three-dimensional covalent organic framework material, open tubular capillary electrochromatographic column and preparation method

A technology of covalent organic framework and capillary electrochromatography, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., can solve problems such as difficult large-scale production, large solvent usage, harsh reaction conditions, etc., and achieve good separation Effect and reproducibility, shortened time, effect of large porosity

Active Publication Date: 2020-09-01
CAPITAL NORMAL UNIVERSITY
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Problems solved by technology

However, this method needs to be carried out in a closed condition at a higher temperature, and the reaction time is longer (usually it needs to be heated at a high temperature of 80-120°C in a sealed container for 2-9 days), the reaction conditions are harsh, and the amount of solvent used is large, so it is not easy to scale production

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  • Three-dimensional covalent organic framework material, open tubular capillary electrochromatographic column and preparation method
  • Three-dimensional covalent organic framework material, open tubular capillary electrochromatographic column and preparation method
  • Three-dimensional covalent organic framework material, open tubular capillary electrochromatographic column and preparation method

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preparation example Construction

[0044] The present invention also provides a preparation method of a three-dimensional covalent organic framework material, such as figure 1 shown, including the following steps:

[0045] Step 1. Dissolve 1,3,5-trialdehyde phloroglucinol (Tp) in a mixed solution of ethanol / tetrahydrofuran to obtain the first mixed solution; dissolve tetrakis(4-aminophenyl)methane (TAM) in Obtain the second mixed solution in the mixed solution of ethanol / tetrahydrofuran;

[0046] Step 2. After adding trifluoroacetic acid to the first mixed solution, perform ultrasonic dispersion to obtain the first mixture;

[0047] Step 3, adding the second mixed solution to the first mixture dropwise, followed by ultrasonication to obtain the second mixture;

[0048] Step 4, washing the second mixture with ethanol for 3-5 times and then drying to obtain a three-dimensional covalent organic framework material (TpTAM-like three-dimensional covalent organic framework material, ie 3D TpTAM).

[0049] It should...

Embodiment 1

[0073] This embodiment provides a three-dimensional covalent organic framework material, the three-dimensional covalent organic framework material is a TpTAM three-dimensional covalent organic framework material; the ligands used in the three-dimensional covalent organic framework material include 1,3,5-trialdehyde Phloroglucinol (Tp) and tetrakis(4-aminophenyl)methane (TAM). Wherein, the mass ratio of 1,3,5-trialdehyde phloroglucinol (Tp) to tetrakis(4-aminophenyl)methane (TAM) is 3:2.

[0074] The preparation method of the above-mentioned TpTAM-like three-dimensional covalent organic framework material comprises the following steps:

[0075] Step 1. Dissolve 60mg of 1,3,5-trialdehyde phloroglucinol (Tp) in a mixed solution of 10mL ethanol / tetrahydrofuran (the volume ratio of ethanol and tetrahydrofuran is 9:1) to obtain the first mixed solution; 40mg tetrakis(4-aminophenyl)methane (TAM) was dissolved in 10mL ethanol / tetrahydrofuran mixed solution (the volume ratio of ethano...

Embodiment 2

[0081] This embodiment provides an open-tube capillary electrochromatographic column, and the stationary phase of the open-tube capillary electrochromatographic column is the TpTAM-like three-dimensional covalent organic framework material in the above-mentioned embodiment 1.

[0082] The preparation method of the open-tube capillary electrochromatographic column comprises the following steps:

[0083] S1. Dissolve 30 mg of TpTAM-like three-dimensional covalent organic framework material in 10 mL of ethanol / tetrahydrofuran mixed solution (the volume ratio of ethanol and tetrahydrofuran is 9:1) and 100 μL of trifluoroacetic acid mixed solution, and ultrasonically disperse to obtain the first suspension ;

[0084]S2. Add 100 μL of 3-aminopropyltriethoxysilane (APTES) to the first suspension to obtain a third mixed solution;

[0085] S3. Ultrasonic treatment is performed on the third mixed solution. The temperature of ultrasonic dispersion can be kept at room temperature for 20 ...

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Abstract

The invention relates to a three-dimensional covalent organic framework material, an open tubular capillary electrochromatographic column and a preparation method, belongs to the technical field of covalent organic framework materials, and solves the problems of less research on the existing three-dimensional covalent organic framework material and poor separation effect of the capillary electrochromatographic column. Ligands adopted by the three-dimensional covalent organic framework material comprise 1, 3, 5-trialdehyde phloroglucinol and tetra (4-aminophenyl) methane. A stationary phase ofthe open tubular capillary electrochromatographic column comprises a three-dimensional covalent organic framework material. The open tubular capillary electrochromatographic column provided by the invention is good in separation effect and reproducibility.

Description

technical field [0001] The invention belongs to the technical field of covalent organic framework materials, in particular to a three-dimensional covalent organic framework material, an open-tube capillary electrochromatographic column and a preparation method. Background technique [0002] Covalent organic frameworks (COFs) are a class of crystalline porous polymers connected by covalent bonds. Because of their large specific surface area, adjustable pore size, easy modification and good stability, Yaghi After the research group proposed it for the first time, it has attracted widespread attention. With the deepening of research, COFs materials have been initially applied in various fields such as gas storage and separation, adsorption of heavy metal ions, heterogeneous catalysis, and optical materials. In particular, it is a hotspot of research as a stationary phase for chromatographic techniques. [0003] Open-tubular capillary electrochromatography (OT-CEC) is a separa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01D15/08B01J20/30
CPCB01J20/285B01D15/08
Inventor 叶能胜宗蕊
Owner CAPITAL NORMAL UNIVERSITY
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