A kind of eu(Ⅲ)-metal organic framework and its preparation method and application

A metal-organic framework and pentachloronitrobenzene technology, applied in the field of fluorescent probes, can solve the problems of less Ln-MOFs, and achieve the effects of low cost, simple design and high recyclability.

Active Publication Date: 2021-11-30
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are few Ln-MOFs for trace detection of PCNB using fluorescence

Method used

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  • A kind of eu(Ⅲ)-metal organic framework and its preparation method and application
  • A kind of eu(Ⅲ)-metal organic framework and its preparation method and application
  • A kind of eu(Ⅲ)-metal organic framework and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1. Preparation of Eu(Ⅲ)-MOF:

[0035] Accurately weigh 0.0243g (0.1mmol) 5-(4-carboxyphenyl)picolinic acid (H 2 cppc) was dissolved in 6mL DMF, CH 3 CN and H 2 O (V:V:V=3:2:1) mixed solvent, pipette 1mL Eu(NO 3 ) 3 ·6H 2 O (0.1mol / L) aqueous solution in the above mixed solvent, the mixture was magnetically stirred at room temperature for 15min, then 20 microliters of 4M HCl was added dropwise; Reacted for 3 days, and finally cooled to room temperature at 5°C / hour to obtain colorless rod-shaped crystals, which were filtered, washed and collected to obtain a metal organic framework compound.

[0036] The 5-(4-carboxyphenyl)picolinic acid (H 2 cppc) is a well-known substance in the art, and 5-(4-carboxyphenyl) picolinic acid (H 2 cppc) was purchased from Jinan Henghua Chemical Co., Ltd.

Embodiment 2

[0037] Example 2, Eu(Ⅲ)-metal-organic framework crystallographic structure parameters

[0038] The Eu(III)-MOF crystal structure obtained in Example 1 was determined as follows: a single crystal with a suitable size was selected under a microscope for X-ray single crystal structure analysis. The X-ray diffraction data of crystals were collected by German Bruker Smart-Apex CCD surface detection X-ray single crystal diffractometer. target, measured at room temperature. Data reduction and structural elucidation were performed using the SHELXTL-97 program. The main crystallographic data of the organic frameworks are listed in Table 1.

[0039] Table 1. Crystallographic structural parameters of organic frameworks

[0040]

Embodiment 3

[0041] Example 3. Experimental operation of Eu(Ⅲ)-metal-organic framework fluorescence detection in organic solvents:

[0042] Accurately weigh 0.5 mg of Eu(Ⅲ)-MOF sample powder and disperse in 4.00 mL of acetonitrile (CH 3 CN), Methanol (CH 3 OH), dichloromethane (CHCl 2 ), ethanol (C 2 h 5 OH), N,N-dimethylacetamide (DMA), N,N-dimethylformamide (DMF), n-hexane (C 6 h 14 ), formaldehyde (HCHO), H 2 O, n-butanol (C 4 h 9 OH), chloroform (CHCl 3 ), benzene (C 6 h 6 ), tetrahydrofuran (THF), and pentachloronitrobenzene (PCNB) in acetonitrile solution, after ultrasonic vibration for 30 min, dispersions in different solvents were obtained. After the configuration is complete, in λ ex =275nm excitation wavelength, respectively measure the fluorescence spectrum of the corresponding dispersion. From the emission spectrum ( Figure 6 ) shows that solvent molecules have a very obvious effect on the luminescence intensity of the complex, and the order of fluorescence inten...

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Abstract

The invention relates to the field of fluorescent probes, in particular to a Eu(III)-metal-organic framework and its preparation method and application, which are applied to the detection of pentachloronitrobenzene. Eu(Ⅲ)‑MOF, its chemical formula is: {(CH 3 ) 2 NH 2 ][Eu(cppc) 2 2H 2 O]} n . The Eu(III)-MOF described in the present invention does not need to be purified after synthesis, and can directly perform fluorescence detection of pentachloronitrobenzene, has the advantages of simple design, low cost, etc., and is suitable for online sensitive and rapid analysis. The detection limit of Eu(Ⅲ)-MOF of the present invention reaches 1.67×10 to pentachloronitrobenzene ‑6 M, and the response time is short, and can be completely separated after simple filtration, high recycling rate, universal in the field of fluorescence sensing, and helpful for practical applications.

Description

technical field [0001] The invention relates to the field of fluorescent probes, in particular to an Eu(III)-metal-organic framework and a preparation method and application thereof, which are applied to the detection of pentachloronitrobenzene. Background technique [0002] Pesticide is an important means and tool to protect crops and reduce yield loss, and is an effective weapon to control crop diseases, insect pests and weeds. However, pesticides are also a "double-edged sword". Unreasonable use of pesticides will cause problems such as crop injury, human and animal poisoning, environmental pollution, and food safety. Excessive pesticide residues in agricultural products not only affect food quality and safety, but also cause harm to human health and quality of life through the food chain, and even cause "three causes" (carcinogenic, teratogenic, and mutagenic). Therefore, the rapid and selective detection of pesticides has become one of the most pressing issues for huma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00G01N21/64
CPCC08G83/008G01N21/6428G01N2021/6432
Inventor 宋江锋姚瑞超周瑞莎温慧芳张雯
Owner ZHONGBEI UNIV
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