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Covalent organic framework material as well as synthesis method and application thereof

A technology of covalent organic framework and synthesis method, which is applied in the fields of analysis materials, luminescent materials, material excitation analysis, etc., to achieve the effect of sensitive fluorescence response behavior

Inactive Publication Date: 2020-07-03
LINYI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no good detection method or method for heavy metal ion pollution, which is a bottleneck that humans need to break through

Method used

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  • Covalent organic framework material as well as synthesis method and application thereof
  • Covalent organic framework material as well as synthesis method and application thereof
  • Covalent organic framework material as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Synthesis of covalent organic framework material LYU-12

[0023]

[0024] Add 7.0mg of 2,4,6-trihydroxy-1,3,5-trithenaldehyde and 16.9mg of 2,5-dibutoxy-1,4-phthalhydrazide to a 10mL ampoule . Then add 1mL of 1,4-dioxane, 1mL of mesitylene and 1mL of ethanol, shake well and add 0.3mL of 9M acetic acid solution. Place the ampoule in liquid nitrogen, pump the air to 0mbar after the solution solidifies, and then seal the ampoule. It was placed in an oven and reacted at 80° C. for five days. After the reaction, a solid was produced at the bottom of the ampoule, and the solid was transferred to a centrifuge tube, washed with acetone and tetrahydrofuran for 3 times, respectively. The solid was dried at 100° C. to obtain 18.1 mg of brown yellow solid powder LYU-12 with a yield of 82%.

[0025] figure 1 (-Butoxy) is the X-ray diffraction pattern of LYU-12 in Example 1. It can be seen from the comparison of spectra that the powder X-ray diffraction of this ty...

Embodiment 2

[0029] Example 2: Synthesis of covalent organic framework material LYU-12

[0030] Add 7.0mg of 2,4,6-trihydroxy-1,3,5-trithenaldehyde and 11.3mg of 2,5-dibutoxy-1,4-phthalic hydrazide to a 10mL ampoule middle. Then add 1mL of mesitylene and 2mL of ethanol, shake well and add 0.3mL of 9M acetic acid solution. Place the ampoule in liquid nitrogen, pump the air to 0mbar after the solution solidifies, and then seal the ampoule. It was placed in an oven and reacted at 150° C. for seven days. After the reaction, a solid was produced at the bottom of the ampoule, and the solid was transferred to a centrifuge tube, washed with acetone and tetrahydrofuran for 3 times, respectively. The solid was dried at 100°C to obtain 12.1 mg of LYU-1212 as a brown yellow solid powder with a yield of 71%.

Embodiment 3

[0031] Example 3: Synthesis of covalent organic framework material LYU-12

[0032] Add 7.0mg of 2,4,6-trihydroxy-1,3,5-trithenaldehyde and 22.5mg of 2,5-dibutoxy-1,4-phthalhydrazide to a 10mL ampoule . Then add 1mL n-butanol, 1mL o-dichlorobenzene and 1mL ethanol, shake well and add 0.3mL 9M acetic acid solution. Place the ampoule in liquid nitrogen, pump the air to 0mbar after the solution solidifies, and then seal the ampoule. Put it in an oven and react at 90°C for one day. After the reaction, a solid was produced at the bottom of the ampoule, and the solid was transferred to a centrifuge tube, washed with acetone and tetrahydrofuran for 3 times, respectively. The solid was dried at 100° C. to obtain 19.2 mg of brown yellow solid powder LYU-12 with a yield of 69%.

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Abstract

The invention discloses a synthesis method of a covalent organic framework material. The preparation method comprises the following steps: uniformly mixing 2,4,6-trihydroxy-1,3,5-s-tribenzaldehyde and2,5-dialkoxy-1,4-phthaloyl hydrazine in an organic solvent, and reacting under the catalysis of acetic acid to obtain the covalent organic framework material, and alkoxyl is methoxy, ethoxyl, propoxyl, butoxyl or pentoxyl. The covalent organic framework material is applied to fluorescence detection of Cu<2+>, Co<2+>, Cr<3+> and Pb<2+>. The covalent organic framework material synthesized by the method has a long-range ordered two-dimensional hexagonal structure and regular pore passages; the material can be used as a fluorescent probe, can be recognized by heavy metal ions Cu<2+>, Co<2+>, Cr<3+> and Pb<2+> to quench fluorescence, and has sensitive fluorescence response behaviors.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and functional materials, and in particular relates to a class of covalent organic framework materials and their synthesis methods and applications. Background technique [0002] The pollution of heavy metal ions in water is one of the serious problems facing human beings, which will affect the healthy life of human beings. There is no good detection method or method for heavy metal ion pollution, which is a bottleneck that human beings need to break through. [0003] Covalent organic framework materials are a class of new materials that have attracted a lot of attention. At present, they have been initially applied in the fields of gas adsorption / separation / storage, optoelectronics (devices), and catalysis. The conjugated structure of the covalent organic framework material has good light absorption, and some functional units are introduced through a certain structural design to obtain...

Claims

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Application Information

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IPC IPC(8): C08G73/00C09K11/06G01N21/64
CPCC08G73/00C09K11/06G01N21/6428C09K2211/1425G01N2021/6432
Inventor 魏丕峰闻振浩唐李洁韩晓莹王亚琦
Owner LINYI UNIVERSITY
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