Amphoteric ligand-based lead metal-organic framework material as well as preparation method and application thereof in fluorescence detection

An organic framework and amphoteric ligand technology, applied in analytical materials, luminescent materials, fluorescence/phosphorescence, etc., can solve the problem of metal-organic framework materials being unstable, and achieve easy mass production and popular use, high yield, and high reliability. Highly reproducible effect

Active Publication Date: 2020-06-05
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, there are certain limitations in the wide application of luminescent metal-organic framework materials as fluorescent detection agents, that is, metal-organic framework materials cannot exist stably in water environments.

Method used

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  • Amphoteric ligand-based lead metal-organic framework material as well as preparation method and application thereof in fluorescence detection
  • Amphoteric ligand-based lead metal-organic framework material as well as preparation method and application thereof in fluorescence detection
  • Amphoteric ligand-based lead metal-organic framework material as well as preparation method and application thereof in fluorescence detection

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Experimental program
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Embodiment 1

[0027] The metal-organic framework of embodiment 1 lead [Pb (cbdcp)] · 0.5H 2 O·0.5CH 3 The preparation method of OH

[0028] Weigh 34mg (0.1mmol) amphoteric organic ligand 4-carboxy-1-(3,4-dicarboxy-benzyl)-pyridine chloride (4-carboxy-1-(3,4-dicarboxy-benzyl)- pyridinium chloride, abbreviated as H 3 cbdcpCl) and 33mg (0.1mmol) lead nitrate Pb (NO 3 ) 2 In the polytetrafluoroethylene liner, add 5mL of deionized water, 1mL of acetonitrile and 1mL of methanol to the mixture, and mix well by ultrasonication for 10-20 minutes, then place the polytetrafluoroethylene liner in a stainless steel reactor jacket and tighten it. Put it in a constant temperature oven at 120°C to react for 4 days, take it out and let it cool down to room temperature naturally, open the polytetrafluoroethylene liner to obtain a yellow rhombic transparent crystal. Rinse the crystals with distilled water, collect the crystals by filtration, and dry at room temperature to obtain the metal-organic framewo...

Embodiment 2

[0029] The metal-organic framework of embodiment 2 lead [Pb (cbdcp)] · 0.5H 2 O·0.5CH 3 Structural characterization of OH

[0030] The crystal structure of the target material was obtained by analyzing the X-ray single crystal diffraction data, and the sample purity and air stability were characterized by X-ray powder diffraction ( figure 1 ). Single crystal test results show that the target material crystallizes in the orthorhombic system, Pca2 1space group. There is a positive divalent lead ion Pb in the asymmetric unit of the structure 2+ , a negative divalent deprotonated organic ligand cbdcp 2- , half a water molecule and half a methanol molecule at the center of symmetry. Central metal Pb 2+ Presents an eight-coordinated geometry, coordinating with eight oxygen atoms from five carboxyl groups ( figure 2 a). The bond length of the Pb-O bond is In the range. adjacent Pb 2+ The ions coordinate with the carboxyl groups of the ligands to form a one-dimensional...

Embodiment 3

[0031] The metal-organic framework of embodiment 3 lead [Pb (cbdcp)] · 0.5H 2 O·0.5CH 3 Characterization of OH Water Stability

[0032] The stability characterization of the target material in the water environment is to soak the material in an aqueous solution containing the target detection substance for 7 days, perform X-ray powder diffraction characterization on it, and judge whether its structure has changed. like image 3 As shown, the target material contains Cr 2 o 7 2- ,CrO 4 2- and Fe 3+ The aqueous solution of ions can maintain its original crystal structure, which proves the stability of the material in the aqueous environment.

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Abstract

The invention discloses an amphoteric ligand-based lead metal-organic framework material and a preparation method thereof. The preparation method comprises the following steps: adding H3cbdcpCl and Pb(NO3)2 into a mixed solution composed of deionized water, acetonitrile and methanol, uniformly mixing, and heating in a reaction kettle to react for a period of time, thereby obtaining yellow rhombictransparent crystals, namely the metal-organic framework material of lead. The metal-organic framework material of lead is a novel three-dimensional metal-organic framework which is constructed by amphoteric ligands and has a three-dimensional SrAl2 topological structure, has good water stability, can be used in a water environment, has stable properties and can be stored in air for a long time. The synthesis method disclosed by the invention is simple and rapid, low in cost, high in yield, high in repeatability and easy for mass production, popularization and use. The lead metal-organic framework material has strong fluorescence emission in an ultraviolet light-visible light region, is suitable for fluorescence detection in the field of water pollution, and can selectively detect Cr2O7<2->, CrO4<2-> and Fe<3+> ions in sewage through the change of fluorescence intensity.

Description

technical field [0001] The invention relates to a metal-organic framework material, and relates to a lead-based metal-organic framework material based on an amphoteric ligand, a preparation method thereof, and an application in fluorescence detection. Background technique [0002] In recent years, luminescent metal-organic framework materials have attracted extensive attention from researchers at home and abroad because of their wide application prospects in fluorescence detection and other aspects. Compared with traditional detection methods such as chromatography, inductively coupled plasma mass spectrometry, and atomic absorption spectrometry, fluorescence detection has the characteristics of simple operation, short detection time, and low detection cost. With the concerted efforts of scholars at home and abroad, some luminescent metal-organic framework materials for environmental pollutants have emerged. These materials are widely used in the detection of heavy metal io...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/188G01N21/6428G01N21/643G01N2021/6432
Inventor 盖艳丽熊克才孟庆华石余雯张慧
Owner XUZHOU NORMAL UNIVERSITY
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