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Method for rapidly preparing metal organic layer material and application

A metal-organic, layered material technology, applied in chemical instruments and methods, catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as low efficiency and long time consumption

Active Publication Date: 2020-10-23
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to overcome the deficiencies of the prior art, especially for the problems of long time consumption and low efficiency in the existing Zr / Hf-MOLs method, and propose a method for rapidly preparing Zr / Hf-MOLs. The method is extremely fast and efficient, and the desired product can be obtained by raising the temperature to 120 degrees Celsius at the fastest without heat preservation, and the obtained product has a very good performance of catalyzing the degradation of organophosphorus poisons, and the degradation half-life is less than 3 minutes. The value of reuse, the degradation half-life of re-use is still only about 5 minutes

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  • Method for rapidly preparing metal organic layer material and application
  • Method for rapidly preparing metal organic layer material and application
  • Method for rapidly preparing metal organic layer material and application

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Embodiment 1

[0039] A method for rapidly preparing metal-organic layer materials of the present invention, comprising the following steps:

[0040]Take 140mg hafnium chloride HfCl 4 (0.438mmol) and 125mg 1,3,5-tricarboxyphenylbenzeneH 3 BTB (0.285mol), add 8.8mL of concentrated hydrochloric acid, 3mL of deionized water and 20mL of DMF, ultrasonically dissolve it fully, transfer it to a 100mL polytetrafluoroethylene-lined polyetheretherketone reactor, put it into a microwave reactor for 5 Heated to 90°C within 1 minute and kept for 1 hour to carry out the reaction. The white precipitated product was centrifuged, washed three times with DMF, absolute ethanol, and water, respectively, and vacuum-dried at 75°C for 24 hours to obtain the final metal-organic layer material. Specifically, it is a hafnium-based metal organic layer material. The resulting sample was designated as Hf-BTB-HCl.

[0041] The product characterization data of this embodiment are as figure 1 , 2 , 3, 4, and 5. figur...

Embodiment 2

[0043] A method for rapidly preparing metal-organic layer materials of the present invention, comprising the following steps:

[0044] Take 116mg hafnium oxychloride HfOCl 2 (0.438mmol) and 125mg three (4-carboxyphenyl) -1,3,5-triazine H 3 TATB (0.285mol), add 8.8mL of formic acid HCOOH, 3mL of deionized water and 20mL of DEF, ultrasonically dissolve it fully, transfer it to a 100mL polytetrafluoroethylene-lined polyetheretherketone reactor, and put it in a microwave reactor for 10 Heated to 120°C within 1 minute and kept for 0min, centrifuged the white precipitated product, washed three times with DEF, absolute ethanol, and water respectively, and dried in vacuum at 75°C for 24 hours to obtain a metal organic layer material, specifically hafnium-based metal organic layer material.

Embodiment 3

[0046] A method for rapidly preparing metal-organic layer materials of the present invention, comprising the following steps:

[0047] Take 100mg zirconium chloride ZrCl 4 (0.438mmol) and 145mg 1,3,5-tris(4-carboxyphenylethynyl)benzeneH 3 BTE (0.285mmol), add 13mL HCOOH, 5mL deionized water and 25mL DMA, sonicate to fully dissolve, then transfer to a 100mL polytetrafluoroethylene-lined polyetheretherketone reactor, put it in a microwave reactor within 10 minutes Heat to 110°C and keep for 10min, centrifuge the white precipitated product, wash three times with DMA, absolute ethanol, and water, and dry in vacuum at 75°C for 24h to obtain a metal-organic layer material, specifically a zirconium-based metal-organic layer material.

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Abstract

The invention discloses a method for rapidly preparing a metal organic layer material and application. The method comprises the following steps: dissolving a metal salt, a tricarboxylic acid ligand and an acidity regulator in a solvent, then carrying out microwave heating to raise the temperature for reaction, and carrying out centrifugal separation, washing and drying on the obtained precipitateproduct to obtain the metal organic layer material. The method is very rapid and efficient, the required product can be obtained by only heating to 120 DEG C at the soonest without a heat preservationreaction process, the obtained product can be applied to catalytic degradation of an organic phosphorus poisoning agent, the performance is very good, the degradation half-life period is less than 3minutes, an excellent recycling value is also achieved, and the degradation half-life period after reuse is still about 5 minutes.

Description

technical field [0001] The invention belongs to the field of preparation of metal-organic coordination materials, and relates to a method and application for rapid preparation of metal-organic layer materials, in particular to a rapid preparation method of zirconium / hafnium-based metal-organic layer materials (Zr / Hf-BTB) and its Application of catalytic degradation of organophosphorus poisons. Background technique [0002] Chemical warfare agents (CWAs) containing phosphonate linkages, known as nerve agents, are among the most toxic chemicals known to man. The development of materials for simple and rapid elimination of these toxic chemicals remains a very important issue. Recently, Zr-based metal-organic framework (MOF) materials, such as UiO-66 and its derivatives UiO-67, MOF-808, NU-1000, have been reported to be effective in decomposing lethal organophosphonate neurotoxins and their analogues. Excellent performance. However, experimental and computational data suggest...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/34A62D3/35A62D101/02A62D101/26
CPCB01J31/1691B01J31/2239B01J37/346A62D3/35B01J2531/49B01J2531/48A62D2101/02A62D2101/26
Inventor 陶呈安陈瑞黄坚李玉姣阳绪衡王芳刘卓靓王建方赵捷张曾慧
Owner NAT UNIV OF DEFENSE TECH
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