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Preparation method and application method of benzothiadiazole-based large-aperture MOF material

A benzothiadiazole and MOF technology, which is applied in the field of preparation and application of chemical materials, can solve the problems of long time consumption and high energy consumption, and achieve the effects of simple preparation process, suitable for mass production and low cost

Inactive Publication Date: 2021-03-26
南京艾姆材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of preparation and application method of the large-aperture MOF material based on benzothiadiazole, to solve the time-consuming and high defects of the method for detecting amine in the prior art

Method used

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  • Preparation method and application method of benzothiadiazole-based large-aperture MOF material
  • Preparation method and application method of benzothiadiazole-based large-aperture MOF material
  • Preparation method and application method of benzothiadiazole-based large-aperture MOF material

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preparation example Construction

[0035] A kind of preparation method of the large aperture MOF material based on benzothiadiazole, described method comprises the steps:

[0036] Step 1: Dissolve a certain amount of metal salt and ligand in a solvent to obtain solution A and solution B;

[0037] Weigh 0.2-2.0mmol metal salt, dissolve it in N,N-dimethylformamide to obtain solution A;

[0038] Weigh 0.1-2.0 mmol of the ligand and dissolve it in N,N-dimethylformamide to obtain solution B;

[0039] Among them: the molar ratio of metal salt and ligand is listed as 2 to 3:1;

[0040] Metal salts are active metals of periods 4, 5, and 6 in the periodic table and metal elements of the main group II to VIA, preferably Sn, Zn, Ga, Ge, In, Sb, Tl, Pb, Bi, Po, Ti, Al, Salts prepared by one or more of Ba, Rh, Ru, Ni, Cu, Fe, Cr, Co, Pd, Mn, V, Sc, Cd, Ag, Tc, Mo, Nb, Zr, Y;

[0041] Metal salts are nitrates, chlorides and acetates of transition metals and nitrates and chlorides of rare earth metals;

[0042] Metal salt...

Embodiment 1

[0063] Weigh 0.2mmol of nickel nitrate hexahydrate and dissolve in 10mL of DMF solution, solution A;

[0064] Weigh 0.1mmol of H 2 L and dissolved in 20mL of DMF solution, solution B;

[0065] Mix solution A and solution B, and ultrasonic 20min, then pack in the liner of tetrafluoroethylene, be placed in the reactor, finally reactor is placed in the vacuum oven;

[0066] Start heating in the drying oven, heat to 120°C within 3 minutes, and keep it for 24 hours;

[0067] After reaching the holding time, cool down to room temperature at a rate of 0.08°C / min, and take out the material;

[0068] Dry the taken-out material at a temperature of 50°C for 12 hours. After drying, a new type of MOF material is obtained;

Embodiment 2

[0070] Weigh 3mmol of zinc nitrate nonahydrate and dissolve in 10mL of DMF solution, solution A;

[0071] Weigh 1mmol of H 2 L and dissolved in 20mL of DMF solution, solution B;

[0072] Mix solution A and solution B, and ultrasonic 40min, then pack in the liner of tetrafluoroethylene, be placed in the reactor, finally reactor is placed in the vacuum oven;

[0073] Start heating in the drying oven, heat to 130°C within 3 minutes, and keep it for 48 hours;

[0074] After reaching the holding time, cool down to room temperature at a rate of 0.9°C / min, and take out the material;

[0075] Dry the taken-out material at a temperature of 60°C for 18 hours. After drying, a new type of MOF material is obtained;

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Abstract

The invention discloses a preparation method and application method of a benzothiadiazole-based large-aperture MOF material. The method comprises the following steps: respectively dissolving a certainamount of metal salts and ligands in a solvent to obtain a solution A and a solution B; fully mixing the solution B and the solution A, heating and keeping the temperature until the reaction is finished, and cooling to room temperature to obtain a crystal; and washing the crystal with eluent and drying to obtain an MOF material. The method comprises the steps of material proportioning and mixing,grinding, cooling, purifying and the like. The preparation method mainly comprises the steps: respectively dissolving zirconium salt, zinc salt, aluminum salt and other metal salts and ligands in N,N-dimethylformamide, uniformly mixing, heating to 120 DEG C in vacuum, keeping the temperature for about 24-72 hours, finally cooling to room temperature at a certain cooling rate, centrifuging, filtering, washing and drying to obtain the crystal. The preparation method disclosed by the invention has the advantages of low cost, simple preparation process, suitability for batch production and the like.

Description

technical field [0001] The present invention relates to the field of preparation and application of chemical materials, in particular to a preparation and application method of a large-aperture MOF material based on benzothiadiazole. Background technique: [0002] Amines and their derivatives play an important role in food, dyes and medicines. In recent years, incidents of unqualified amine content in food, textiles and other fields have frequently attracted attention. Therefore, how to quickly, sensitively and efficiently detect amines has become the research direction of many scientists. However, the current detection methods for amines are mainly liquid chromatography, electrochemical detection, etc., but these detection methods have the disadvantages of long time consumption and high energy consumption, so it is necessary to develop a detection method with fast reaction speed, high sensitivity and low detection limit . Metal-organic frameworks (MOFs) are crystalline ma...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06G01N21/6428C09K2211/185
Inventor 彭雨新赵艳如刘华奇
Owner 南京艾姆材料科技有限公司
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