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A nanoscale metal fluoride catalyst with confined structure and its preparation method and application

A nano-scale, fluoride technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, dehydrohalogenation preparation, etc. See reports and other issues

Active Publication Date: 2021-12-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, due to the easy generation of carbon deposition and sintering in the catalytic reaction, the catalyst is deactivated and affects the life of the catalyst.
Small-sized nanoparticles can inhibit carbon deposition but are easy to sinter, so it is urgent to develop a nanoscale metal fluoride catalyst with a confined structure that can both inhibit carbon deposition and prevent deactivation caused by sintering and grain size growth. question
[0004] At present, carbon-doped metal composites are not common, and the preparation of nanoscale metal fluorides with confined structure has not been reported.

Method used

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  • A nanoscale metal fluoride catalyst with confined structure and its preparation method and application
  • A nanoscale metal fluoride catalyst with confined structure and its preparation method and application
  • A nanoscale metal fluoride catalyst with confined structure and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 3.33g terephthalic acid (C 8 h 6 o 4 ) and 8g chromium nitrate nonahydrate (Cr(NO 3 ) 3 9H 2 O) be dissolved in 160mL deionized water, then add 0.92mL hydrofluoric acid (concentration 40%), magnetically stir for 10min to obtain the solution, place the above solution in a stainless steel autoclave lined with 250mL polytetrafluoroethylene, and The crystallization reaction was carried out in a drying oven at 220° C. for 8 hours. After the reaction, the stainless steel autoclave was taken out, and after it was naturally cooled to room temperature, the reaction product mixture in the stainless steel autoclave was removed. The reaction product mixture was centrifuged to obtain crude MIL-101. Then the crude MIL-101 was washed with 500mL deionized water at 70°C for 6h, and then centrifuged. The obtained sample was washed with 500mL DMF at 70°C for 12h, and then centrifuged. The obtained sample was washed with 300mL absolute ethanol at 70°C. Wash for 6h and twice, then cen...

Embodiment 2

[0035] 3.33g terephthalic acid (C 8 h 6 o 4 ) and 8g chromium nitrate nonahydrate (Cr(NO 3 ) 3 9H 2 O) be dissolved in 160mL deionized water, then add 0.92mL hydrofluoric acid (concentration 40%), magnetically stir for 10min to obtain the solution, place the above solution in a stainless steel autoclave lined with 250mL polytetrafluoroethylene, and The crystallization reaction was carried out at 220° C. in a drying oven for 8 hours. After the reaction, the stainless steel autoclave was taken out, and after it was naturally cooled to room temperature, the reaction product mixture in the stainless steel autoclave was removed. The reaction product mixture was centrifuged to obtain crude MIL-101. Then the crude MIL-101 was washed with 500mL deionized water at 70°C for 6h, and then centrifuged. The obtained sample was washed with 500mL DMF at 70°C for 12h, and then centrifuged. Wash with ethanol for 6 h and twice, then centrifuge the obtained sample at 70°C with 500 mL NH 4 ...

Embodiment 3

[0041] 3.02g triethyl benzene tricarboxylate (C 15 h 18 o 6 ) and 6.67g aluminum nitrate nonahydrate (Al(NO 3 ) 3 9H 2 O) Dissolve in 50mL deionized water, then add 10mL HNO 3 Aqueous solution (4mol / L), magnetically stirred for 10min to obtain the solution, the above solution was placed in a 250mL polytetrafluoroethylene-lined stainless steel autoclave, and crystallized in a blast drying oven at 210°C for 72h. After the reaction, The stainless steel autoclave was taken out, and after it was naturally cooled to room temperature, the reaction product mixture in the stainless steel autoclave was removed. The reaction product mixture was centrifuged, and the resulting solid was washed with deionized water and dried overnight at 80°C to obtain a yellow powder, which was the precursor MIL-110.

[0042] Place the resulting precursor MIL-101 in N 2 Calcined at 400°C for 3h under atmosphere, N 2 The flow rate is 30mL / min, and the N 2 Switch to mixed gas (N 2 / O 2 =1 / 99, volu...

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Abstract

The invention discloses a nanoscale metal fluoride catalyst with a confined structure, a preparation method and application thereof. The preparation process of the catalyst is as follows: in the presence of a mineralizer, the metal salt and the organic ligand undergo a crystallization reaction in a solvent to obtain a MOF material, and the MOF material is placed in an inert atmosphere for calcination and carbonization treatment to obtain a carbon-doped metal Composite material, the carbon-doped metal composite material is placed in an oxidative atmosphere for calcination and carbon removal treatment to obtain a nano-scale carbon-doped metal composite material with a confined structure, and the composite material is placed in a fluorinated atmosphere for gas-phase fluorination treatment , that is, the nanoscale metal fluoride catalyst with the confined structure is obtained. The metal active component in the catalyst of the present invention is dispersed at the atomic level in the carbon-based material, so it has the characteristics of strong resistance to sintering and carbon deposition, and exhibits good catalytic activity in the field of fluorine chemical industry due to its unique structural characteristics.

Description

technical field [0001] The invention belongs to a method for preparing a carbon-based material doped with metal, and in particular relates to a nanoscale metal fluoride catalyst with a confined structure and its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs for short) are a new type of zeolite-like porous materials with a periodic network structure formed by self-assembly of metal ions and organic ligands through complexation. The structure and pore size are adjustable, and the height of metal ions is uniformly dispersed in the framework, making it a precursor for the preparation of various multifunctional hybrid materials such as carbon, metal oxides, metal sulfides, metal phosphides, and metal carbides. , which has received widespread attention. [0003] The fluoride of chromium, magnesium and aluminum is a common solid acid material. In the field of fluorine chemical industry, due to its good corrosion resistance, it can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/132B01J37/02B01J37/08B01J37/26C07C17/25C07C21/18B82Y40/00
Inventor 韩文锋刘兵李西良唐浩东李瑛刘化章
Owner ZHEJIANG UNIV OF TECH
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