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One-step preparation method of pyrimidine group-containing COFs (covalent organic frameworks) and application of pyrimidine group-containing COFs in mercury (II) detection

A pyrimidine-based, fluorescent detection technology, applied in the field of material preparation technology and analytical chemistry, can solve the problems of poor water solubility, time-consuming, and complicated preparation steps of COFs, and achieve the effects of saving time, accurate and reliable methods, and reducing reagent loss

Pending Publication Date: 2022-06-24
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of synthesis first and then modification has the following disadvantages: 1) Unmodified COFs have poor water solubility, making it difficult to detect the target in aqueous solvents; 2) The preparation steps are complex and time-consuming, and the multi-step reaction also reduces the comprehensive yield of COFs

Method used

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  • One-step preparation method of pyrimidine group-containing COFs (covalent organic frameworks) and application of pyrimidine group-containing COFs in mercury (II) detection
  • One-step preparation method of pyrimidine group-containing COFs (covalent organic frameworks) and application of pyrimidine group-containing COFs in mercury (II) detection
  • One-step preparation method of pyrimidine group-containing COFs (covalent organic frameworks) and application of pyrimidine group-containing COFs in mercury (II) detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Synthesis of Py-U-COF-1:

[0043] The preparation method of Py-U-COF-1 includes the following steps: adding 30.94mg 1,3,6,8-tetrakis(4-formaldehyde phenyl)pyrene, 25.50mg 1,3, 6,8-Tetrakis(4-aminophenyl)-pyrene, 2.54 mg 5-aminouracil, 1.0 mL o-dichlorobenzene, and 1.0 mL n-butanol. After dispersing in a sonicator for 20 minutes, 0.2 mL of 6 mol / L acetic acid was added to the glass tube as a catalyst and then sonicated for 15 minutes. The reaction solvent was quickly frozen in liquid nitrogen, the glass tube was sealed with a hydrogen flame under vacuum conditions, and then placed at 120° C. for constant temperature reaction for 3 days. After the reaction, the unreacted monomers were eluted with N,N-dimethylformamide, tetrahydrofuran and dichloromethane, filtered and dried in an oven at 60 °C for 12 h to obtain Py-U-COF-1.

Embodiment 2

[0045] Synthesis of Py-U-COF-2:

[0046] The preparation method of Py-U-COF-2 includes the following steps: adding 30.94mg 1,3,6,8-tetrakis(4-formaldehyde phenyl)pyrene, 19.84mg 1,3, 6,8-Tetrakis(4-aminophenyl)pyrene, 7.63 mg 5-aminouracil, 1.0 mL o-dichlorobenzene and 1.0 mL n-butanol. After dispersing in a sonicator for 20 minutes, 0.2 mL of 6 mol / L acetic acid was added to the glass tube as a catalyst and then sonicated for 15 minutes. The reaction solvent was quickly frozen in liquid nitrogen, the glass tube was sealed with a hydrogen flame under vacuum conditions, and then placed at 120° C. for constant temperature reaction for 3 days. After the reaction, the unreacted monomers were eluted with N,N-dimethylformamide, tetrahydrofuran and dichloromethane, filtered and dried in an oven at 60 °C for 12 h to obtain Py-U-COF-2.

Embodiment 3

[0048] Synthesis of Py-U-COF-3:

[0049] The preparation method of Py-U-COF-3 includes the following steps: adding 30.94mg 1,3,6,8-tetrakis(4-formaldehyde phenyl)pyrene, 14.17mg 1,3, 6,8-Tetrakis(4-aminophenyl)pyrene, 12.71 mg 5-aminouracil, 1.0 mL o-dichlorobenzene, and 1.0 mL n-butanol. After dispersing in a sonicator for 20 minutes, 0.2 mL of 6 mol / L acetic acid was added to the glass tube as a catalyst and then sonicated for 15 minutes. The reaction solvent was quickly frozen in liquid nitrogen, the glass tube was sealed with a hydrogen flame under vacuum conditions, and then placed at 120° C. for constant temperature reaction for 3 days. After the reaction, use N,N-dimethylformamide, tetrahydrofuran and dichloromethane to elute the unreacted monomer, filter and dry in a 60°C oven for 12h to obtain Py-U-COF-3.

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Abstract

The invention discloses a one-step preparation method of pyrimidine group-containing COFs (covalent organic frameworks) and application of the pyrimidine group-containing COFs in mercury (II) detection. The pyrimidine group-containing COFs are synthesized by taking 1, 3, 6, 8-tetra (4-formaldehyde phenyl) pyrene, 1, 3, 6, 8-tetra (4-aminophenyl) pyrene and 5-amino uracil as raw materials and acetic acid as a catalyst and adding an organic solvent through a solvothermal method, and the product is marked as Py-U-COF. According to the method, synthesis and functional modification of the COF can be completed at the same time through one-step reaction, so that the defects of complicated steps, low yield and time consumption of a post-modification method are overcome. Meanwhile, the Py-U-COF has strong fluorescence, uracil on a framework of the Py-U-COF has strong coordination capability with mercury (II), and the Py-U-COF can be used as a fluorescent indicator of mercury (II). Common metal ions in an environmental water sample do not interfere with detection of mercury (II) ions, and the method is high in accuracy and has high practical application value.

Description

technical field [0001] The invention relates to the field of material preparation technology and analytical chemistry, in particular to a one-step preparation method of pyrimidine group-containing COFs and its application in mercury (II) detection. Background technique [0002] Mercury is a bioaccumulative and highly toxic heavy metal that can cause some serious human health problems such as environmental pollution and Minamata disease. The expanding mercury cycle is posing increasing challenges to the global environment. In this context, mercury detection in the environment is crucial for protecting human health and the ecological environment. Currently, conventional detection methods for mercury(II), such as inductively coupled plasma mass spectrometry and atomic absorption spectrometry, must rely on inconveniently large instruments, limiting applications. In contrast, fluorescence measurement is considered a promising method for mercury(II) detection due to its high sen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/08C08G12/40G01N21/64
CPCC08G12/08C08G12/40G01N21/6428G01N2021/6432
Inventor 张立邓希锐胡阿威邱建丁梁汝萍
Owner NANCHANG UNIV
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