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Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application of luminescent metal organic framework material

A metal-organic framework, ion detection technology, applied in the direction of luminescent materials, material analysis by optical means, analysis of materials, etc., to achieve high yield, simple operation, and strong selectivity.

Active Publication Date: 2018-09-28
SHAANXI UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are few reports on the detection of thiocyanate ion by metal-organic framework materials

Method used

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  • Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application of luminescent metal organic framework material
  • Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application of luminescent metal organic framework material
  • Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application of luminescent metal organic framework material

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preparation example Construction

[0036] A method for preparing a luminescent metal-organic framework material for detecting thiocyanate ions in water, comprising the following steps:

[0037] Add organic ligands 2,5-thiophenedicarboxylic acid and 1,3-bis(4-pyridyl)propane to the mixed solvent in sequence, and stir at room temperature;

[0038] Add alkali to adjust the pH of the mixed system to 6.0-8.0, then add the metal zinc salt into the mixed solution, and stir until a light white precipitate appears;

[0039] The mixed solution was subjected to solvothermal reaction at 90-120°C, reacted under autogenous pressure for 48-96h, and naturally cooled to room temperature to obtain colorless blocky crystals;

[0040] Washing with ether, filtering, and drying naturally to obtain a luminescent metal-organic framework material;

[0041] The molar ratio of the organic ligand 2,5-thiophenedicarboxylic acid to 1,3-bis(4-pyridyl)propane is (1-1.5):1;

[0042] The molar ratio of the metal zinc salt to the organic ligan...

Embodiment 1

[0048] A luminescent metal organic framework material, the preparation method comprising the following steps:

[0049] 1) Add 0.5mmol 2,5-thiophenedicarboxylic acid and 0.5mmol 1,3-bis(4-pyridyl)propane to water and N,N-dimethylformamide at a molar ratio of 1:1 In the mixed solvent, the volume ratio of water and N,N-dimethylformamide is 1:1, and the molar ratio of 2,5-thiophene dicarboxylic acid and N,N-dimethylformamide is 1:500, Stir at room temperature for 30 minutes;

[0050] 2) Add triethylamine dropwise to the mixed solution of 1), adjust its pH to 6.5, continue to stir and react for 30 minutes, and the organic ligand is completely dissolved;

[0051] 3) Add 1mmol of Zn(NO 3 ) 2 ·6H 2 O was added to the solution obtained in step 2), Zn(NO 3 ) 2 4H 2 The molar ratio of O, 2,5-thiophenedicarboxylic acid and 1,3-bis(4-pyridyl)propane is 2:1:1, and light white precipitate appears after stirring for 30min;

[0052] 4) Seal the mixed solution described in 3) in a 20ml gl...

Embodiment 2

[0055] A luminescent metal organic framework material, the preparation method comprising the following steps:

[0056] 1) Add 0.75mmol 2,5-thiophenedicarboxylic acid and 0.5mmol 1,3-bis(4-pyridyl)propane to a mixture of water and N,N-dimethylformamide at a molar ratio of 1.5:1 In the mixed solvent, the volume ratio of water and N,N-dimethylformamide is 2:1, and the molar ratio of 2,5-thiophenedicarboxylic acid and 1,3-di(4-pyridyl)propane is 1:500 , stir for 30min;

[0057] 2) Add 0.5 mmol sodium hydroxide dropwise to the mixed solution of 1), adjust its pH to 7, the molar ratio of sodium hydroxide to 2,5-thiophene dicarboxylic acid is 1:1, continue stirring for 60 minutes, the solution completely dissolved;

[0058] 3) Add 1.25mmol of Zn(NO 3 ) 2 ·6H 2 O was added to the solution obtained in step 2), Zn(NO 3 ) 2 ·6H 2 The molar ratio of O and 2,5-thiophenedicarboxylic acid was 2.5:1, and a light white precipitate appeared after stirring for 10 minutes;

[0059] 4) Se...

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Abstract

The invention relates to a luminescent metal organic framework material for detecting thiocyanate ions in water and a preparation method and application of the luminescent metal organic framework material. The chemical formula of the metal organic framework material is {Zn2(tdc)(bpp)2}n, wherein tdc is polyacid ligand 2,5 thiophene dicarboxylic acid with a V-shaped framework, and bpp is linear nitrogen-containing auxiliary ligand 1,3-di(4-pyridyl)propane. The novel luminescent metal organic framework material which is a compound has the advantages that the compound is prepared by a solvothermal method and has a three-dimensional two-fold penetration structure; the prepared compound is good in thermal stability, high in fluorescence intensity and capable of emitting clear pure-blue light; the fluorescence intensity of the compound gradually weakens along with the increasing of the concentration of the thiocyanate ions, and accordingly the compound can be used as the fluorescent probe for fast and selectively detecting the thiocyanate ions. The preparation method is simple in process, easy to implement and high in crystal purity and yield. A detection method using the compound is simple and high in selectivity.

Description

technical field [0001] The invention belongs to the technical field of preparation of new materials, and in particular relates to a luminescent metal organic framework material for detecting thiocyanate ions in water, a preparation method and application thereof. Background technique [0002] Free thiocyanate is a negatively charged polyatomic ion. In environmental monitoring, thiocyanate is potentially harmful to aquatic organisms and humans. In the wastewater environment, thiocyanate is easily chlorinated into volatile and highly toxic hydrogen chloride, and it can also generate chloride under the action of ultraviolet rays in the environment. Therefore, the detection and removal of thiocyanate ion is of great significance. At present, there are many methods for the determination of thiocyanate, such as electrode method, chromatography, photometry, polarography, voltammetry and so on. Although these methods are more sensitive, the operation is more cumbersome, some are s...

Claims

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Application Information

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IPC IPC(8): C09K11/06C08G83/00G01N21/64
CPCC08G83/008C09K11/06C09K2211/188G01N21/643G01N2021/6432
Inventor 张亚男张娇娇成晶李欣吕皓天翁翊凯
Owner SHAANXI UNIV OF SCI & TECH
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