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Terbium-organic framework material based on Z-type ligand as well as preparation method and application of terbium-organic framework material

An organic framework and ligand technology, applied in the field of fluorescent materials, can solve the problem that the pretreatment process is not suitable for on-site and real-time analysis.

Active Publication Date: 2020-12-22
XI'AN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Unfortunately, expensive equipment and time-consuming pretreatment processes are not suitable for on-site and real-time analysis

Method used

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  • Terbium-organic framework material based on Z-type ligand as well as preparation method and application of terbium-organic framework material
  • Terbium-organic framework material based on Z-type ligand as well as preparation method and application of terbium-organic framework material
  • Terbium-organic framework material based on Z-type ligand as well as preparation method and application of terbium-organic framework material

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0043] The preparation method of the terbium-organic framework material based on the Z-type ligand, specifically:

[0044] Under sealed conditions, the hydrated terbium nitrate or Tb(NO 3 ) 3 ·6H 2 O and organic ligand H 2 L is 2,2'-bipyridyl-4,4'-dicarboxylic acid, and the regulator reagent o-fluorobenzoic acid is mixed uniformly in the organic solvent N,N-dimethylformamide, and reacted under solvothermal conditions to obtain Tb-MOF material with the above crystal structure.

[0045] Terbium nitrate hexahydrate and organic ligand H 2 The molar ratio of L is 2-4:1, the molar ratio of terbium nitrate hexahydrate to regulator o-fluorobenzoic acid is 1:100-200; the molar ratio of terbium nitrate hexahydrate to N,N-dimethylformamide is 1: 300-500.

[0046] Preferably, terbium nitrate hydrate and organic ligand H 2 L. The molar ratio of regulator o-fluorobenzoic acid is 3:1:120, specifically 59.35mg (0.131mmol) terbium nitrate hexahydrate, 10.62mg (0.0435mmol) organic ligand...

Embodiment 1

[0059] Tb(NO 3 ) 2 ·6H 2 O (0.04mmol), organic ligand H 2 L (0.02mmol) and o-fluorobenzoic acid (6.4mmol) were uniformly mixed and dissolved in 2.0mL of N,N-dimethylformamide, then transferred and sealed into a 25mL vial. The solvothermal reaction was carried out at 120° C. for 96 hours, and then naturally cooled to room temperature to obtain colorless bulk Tb-organic framework crystals.

Embodiment 2

[0061] Tb(NO 3 ) 2 ·6H 2 O (0.06mmol), organic ligand H 2 L (0.02mmol) and o-fluorobenzoic acid (12mmol) were uniformly mixed and dissolved in 2.0mL of N,N-dimethylformamide, then transferred and sealed into a 25mL vial. The solvothermal reaction was carried out at 115°C for 120 hours, and then naturally cooled to room temperature to obtain colorless bulk Tb-organic framework crystals.

[0062] The method for testing the crystal structure of the Tb-MOF obtained in the above examples is the same as the structure, see the following for details:

[0063] Determination of the crystal structure:

[0064] Select a single crystal of Tb-MOF that is transparent and crack-free, and use a Bruker Aper II CCD single crystal X-ray diffractometer from Bruker, Germany at room temperature (about 296K) to perform single crystal structure testing and diffraction data collection, using graphite Monochromator The unit cell parameters corrected by the least squares method were used to anal...

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Abstract

The invention discloses a terbium-organic framework material based on a Z-type ligand, wherein the chemical formula of the terbium-organic framework material is [Tb6O4(OH)4(L)8(H2O)8]n, and H2L is theZ-type organic ligand, namely 2,2'-dipyridyl-4,4'-dicarboxylic acid; the crystal structure of the terbium-organic framework material belongs to a hexagonal system and an I4 / m space group. The invention also discloses a preparation method of the material, wherein the preparation method comprises the specifically steps: uniformly mixing terbium nitrate hexahydrate, 2,2'-dipyridyl-4,4'-dicarboxylicacid and an adjusting reagent o-fluorobenzoic acid in an organic solvent N,N-dimethylformamide under sealed conditions, and reacting under solvothermal conditions to obtain the terbium-organic framework material. The Tb-organic framework material can recognize trace Pb<2+> and Cr2O7<2-> ions in water through fluorescence quenching response, and qualitative, quantitative, rapid and efficient detection is achieved.

Description

technical field [0001] The invention belongs to the technical field of fluorescent materials, and specifically relates to a Z-type ligand-based terbium-organic framework material, a preparation method of the terbium-organic framework material, and an application of the terbium-organic framework material. Background technique [0002] Lead and chromium are widely used in industrial and agricultural fields such as leather, pigments and metallurgy because of their irreplaceable special properties. However, these non-biodegradable and bioaccumulative heavy metal ions can cause fatal diseases, such as cancer, tumors, kidney diseases, and central nervous system disorders, even at very low concentrations. The U.S. Environmental Protection Agency and the World Health Organization have put divalent Pb 2+ and hexavalent Cr(ZI) ions (with Cr 2 o 7 2- Represented) as a serious pollutant category, for Pb in drinking water 2+ and Cr 2 o 7 2- Ion limits are below 0.01 and 0.05 mg / L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06G01N21/6428C09K2211/182Y02B20/00
Inventor 李庆樊增禄张洛红武占省于翔管斌斌
Owner XI'AN POLYTECHNIC UNIVERSITY