Preparation method of covalence organic framework material for detecting trace water in organic solvent

A covalent organic framework, organic solvent technology, applied in material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of cumbersome and time-consuming operation, in the initial stage, lack of materials, etc., to achieve stable fluorescence performance, high crystallinity, high The effect of sensitivity

Inactive Publication Date: 2017-06-23
NANKAI UNIV
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  • Description
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  • Application Information

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Problems solved by technology

Although the research on covalent organic frameworks has developed rapidly in the past decade, such materials are still relatively scarce, especially high crystallinity covalent organic frameworks.
[0003] At present, covalent organic framework materials have shown good application prospects in many fields such as gas storage, catalysis, sensing and separation, but the application research on covalent organic framework materials is still in its infancy, so expanding the application field of this material Has far-reaching implications for the development of covalent organic framework materials
The detection of water in organic solvents is of great significance to many chemical products, because water can affect the selectivity and yield of many chemical reactions. Although the traditional water detection method can accurately detect trace water at the ppm level, its There are still some deficiencies such as the high toxicity of the reagents used, cumbersome and time-consuming operation, etc. Therefore, it is particularly important to develop a fast and simple trace water detection method

Method used

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  • Preparation method of covalence organic framework material for detecting trace water in organic solvent
  • Preparation method of covalence organic framework material for detecting trace water in organic solvent
  • Preparation method of covalence organic framework material for detecting trace water in organic solvent

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Effect test

Embodiment 1

[0016] A method for preparing a covalent organic framework material for detecting trace amounts of water in an organic solvent is prepared by a solvothermal method, and the steps are as follows:

[0017] 1) Mix 21.6mg 1,4-dihydroxyterephthalaldehyde, 31.9mg 2,4,6-tris(4-aminophenyl)-1,3,5-triazine, 0.2mL 6M acetic acid, 1.8mL o Dichlorobenzene and 0.2mL N,N-diethylacetamide were mixed in a Schlenk tube, and ultrasonicated for 5 minutes to obtain a uniform reaction solution;

[0018] 2) React the above-mentioned reaction tube containing the reaction solution at 120°C for 3 days, centrifuge at 10,000rpm to collect the final red solid, wash the separated solid with tetrahydrofuran and dichloromethane alternately for 3 times, and then wash with dichloromethane Soak for 1d, and finally dry at 100°C and -0.1MPa vacuum for 24h to prepare a covalent organic framework material with a yield of 88%.

[0019] figure 1 The powder X-ray diffraction patterns of the prepared covalent organi...

Embodiment 2

[0024] A method for preparing a covalent organic framework material for detecting trace amounts of water in an organic solvent, prepared by a solvothermal method, the steps and method are basically the same as in Example 1, except that the ratio of the reaction solvent in Step 1 is 1.4 mL o-dichlorobenzene and 0.6mL N,N-diethylacetamide, the characterization results of the prepared nanomaterials are similar to those in Example 1. The yield of TzDa obtained was 75%.

Embodiment 3

[0026] A method for preparing a covalent organic framework material for detecting trace amounts of water in an organic solvent, prepared by a solvothermal method, the steps and method are basically the same as in Example 1, except that the proportion of the reaction solvent in Step 1 is 1 mL o-dichlorobenzene and 1 mL N,N-diethylacetamide, the characterization results of the prepared nanomaterials are similar to those in Example 1, and the yield of TzDa obtained is 60%.

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Abstract

The invention relates to a preparation method of a covalence organic framework material for detecting trace water in an organic solvent. The preparation method adopts a solvothermal method. The preparation method comprises the following steps: mixing 1,4-dihydroxy terephthalaldehyde, 2,4,6-tri(4-amino phenyl)-1,3,5-triazine, acetic acid, o-dichlorobenzene or mesitylene, and N,N-diethylacetamide, and ultrasonically uniformly dispersing; transferring a tube with a reaction solution to an environment with the temperature of 120 DEG C to react for 3d; and centrifugally separating obtained red solids, and alternately cleaning the separated solids by using tetrahydrofuran and dichloromethane, and then drying to obtain the needed covalence organic framework material. The preparation method has the advantages that the covalence organic framework material prepared by the method is high in crystallization degree, good in heat stability and chemical stability, stable in fluorescence performance, high in sensitivity to the trace water in the organic solvent, and can be reused for multiple times, so that an effective way is provided for detecting the trace water.

Description

technical field [0001] The invention relates to a covalent organic framework preparation technology and a trace water detection technology in an organic solvent, in particular to a preparation method of a covalent organic framework material for detecting trace water in an organic solvent. Background technique [0002] Covalent organic frameworks are a class of highly ordered porous crystalline polymers composed of organic monomers composed of light elements through covalent bonds. Due to their structural rigidity (2D or 3D), low density, thermal stability and The excellent properties such as good chemical stability, large specific surface area and highly ordered pores have attracted widespread attention of scientists. Although the research on covalent organic frameworks has developed rapidly in the past decade, such materials are still lacking, especially high crystallinity covalent organic frameworks. [0003] At present, covalent organic framework materials have shown goo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/30G01N21/64
CPCC08G12/30G01N21/64
Inventor 严秀平钱海龙杨成雄
Owner NANKAI UNIV
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