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Eu (III)-metal-organic framework and preparation and application methods thereof

A metal-organic framework, Å technology, applied in the field of fluorescent probes, can solve the problem of less Ln-MOFs, and achieve the effect of low cost, improved fluorescence activity and high purity

Active Publication Date: 2019-01-04
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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  • Eu (III)-metal-organic framework and preparation and application methods thereof
  • Eu (III)-metal-organic framework and preparation and application methods thereof
  • Eu (III)-metal-organic framework and preparation and application methods thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0035] Accurately weigh 0.0243g (0.1mmol) 3-4-(carboxyphenyl)-6-carboxypyridine (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 3-4-(carboxyphenyl)-6-carboxypyridine (H 2 cppc) is a well-known substance in the art, and 3-4-(carboxyphenyl)-6-carboxypyridine (H in the present invention) 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 the crystals were collected by a German Bruker Smart-Apex CCD surface detection X-ray single crystal diffractometer, and the Mo-Kα 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 , 7 ) shows that solvent molecules have a very obvious effect on the luminescence intensity of the complex, and the order of fluorescence ...

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Abstract

The invention relates to the field of fluorescence probes, particularly to an Eu (III)-metal-organic framework and preparation and application methods thereof. The Eu (III)-metal organic framework isapplied to detection of quintozene. The Eu (III)-metal-organic framework has a chemical formula of {[(CH3)2NH2][Eu(cppc)2*2H2O]}n. The Eu (III)-metal-organic framework saves post-synthesis purification and can be directly applied to fluorescence detection of quintozene, thereby having the advantages of simple design, low cost and the like and being applicable to online sensitive and rapid analysis. The Eu (III)-metal-organic framework achieves a quintozene detecting limit of 1.67*10<-6> M and meanwhile is short in response time, and meanwhile, can be thoroughly separated through simple filtering, thereby being high in reutilization rate. Besides, the Eu (III)-metal-organic framework achieves universality in the field of fluorescence sensing and facilitates practical application.

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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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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