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Nano-scale metal fluoride catalyst with domain-limited structure as well as preparation method and application thereof

A nano-scale, fluoride technology, used in catalyst activation/preparation, physical/chemical process catalysts, dehydrohalogenation preparation, etc.

Active Publication Date: 2019-05-21
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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  • Nano-scale metal fluoride catalyst with domain-limited structure as well as preparation method and application thereof
  • Nano-scale metal fluoride catalyst with domain-limited structure as well as preparation method and application thereof
  • Nano-scale metal fluoride catalyst with domain-limited structure as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
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 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. 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 nano-scale metal fluoride catalyst with a domain-limited structure as well as a preparation method and application thereof. The preparation process of the catalyst is as follows: under the presence of a mineralizer, carrying out crystallization reaction on a metal salt and an organic ligand in a solvent to prepare a MOF material, carrying out calcination carbonization treatment on the MOF material under an inert atmosphere to obtain a carbon-doped metal composite material, the , carrying out calcination and decarbonization on the carbon-doped metal composite materialin an oxidizing atmosphere to obtain a nano-scale carbon-doped metal composite material with a limited-domain structure, and carrying out gas-phase fluorination treatment on the composite material ina fluorination atmosphere for so as to obtain the nano-scale metal fluoride catalyst with the limited-domain structure. The metal active components in the catalyst are dispersed in an atomic level inthe carbon-based material, so that the catalyst has strong sintering resistance, and has the characteristics of strong anti-deposition carbon and the like; the unique structural characteristics of thecatalyst show good catalytic activity in the field of fluorine chemical industry.

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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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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