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Catalyst for fluoridizing chlorinated olefin and preparation method thereof

A technology for preparing and fluorinating chlorinated olefins, which is applied in the field of fluorination catalysts and its preparation, can solve the problems of small specific surface area, unfavorable industrialization, high price of ammonium hexafluoroaluminate or ammonium tetrafluoroaluminate, etc. problem, to achieve the effect of high specific surface area, lower temperature of carbon removal, and high thermal stability

Inactive Publication Date: 2012-08-08
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The specific surface area prepared by this method is small, and the price of the carrier ammonium hexafluoroaluminate or ammonium tetrafluoroaluminate is relatively expensive, which is not conducive to industrialization.

Method used

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  • Catalyst for fluoridizing chlorinated olefin and preparation method thereof
  • Catalyst for fluoridizing chlorinated olefin and preparation method thereof
  • Catalyst for fluoridizing chlorinated olefin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 10g specific surface area is 350m 2 g -1 γ-Al 2 o 3 , vacuum-dried at 120°C for 4 hours, impregnated 7.5ml of 0.9235mol / L chromium nitrate nonahydrate solution into the dried γ-Al 2 o 3, impregnated for 10 hours, dried in an oven at 120°C for 10 hours, and then calcined in a muffle furnace at 500°C for 4 hours to obtain Cr 2 o 3 The Cr content is 5% of the mass of the carrier 2 o 3 -γ-Al 2 o 3 Composite oxides, secondly, add 11ml of 50% sucrose aqueous solution to the precursor, soak for 5 hours, dry at 500°C 2 Roasting under the atmosphere for 4 hours, the Cr 2 o 3 -γ-Al 2 o 3 Immerse again in sucrose aqueous solution, dry, and calcinate, and repeat this process three times to obtain the carbon-filled Cr 2 o 3 -γ-Al 2 o 3 , put it into a fixed bed reactor and feed HF and N 2 A mixture of gas for fluorination, where HF and N 2 The molar ratio is 1:4, the fluorination temperature is 400°C, and the fluorination time is 10 hours. Finally, the fluor...

Embodiment 2

[0033] Weigh 10g specific surface area is 350m 2 g -1 Aluminum oxide was dried in vacuum at 120°C for 4 hours, and 7.5ml of 0.1772mol / L chromium nitrate nonahydrate solution was impregnated into the dried γ-Al 2 o 3 , impregnated for 10 hours, dried in an oven at 120°C for 10 hours, and then calcined in a muffle furnace at 550°C for 4 hours to obtain Cr 2 o 3 The Cr content is 1% of the mass of the carrier 2 o 3 -γ-Al 2 o 3 Composite oxides, secondly, add 11ml of 50% sucrose aqueous solution to the precursor, soak for 5 hours, dry at 500°C 2 Roasting under the atmosphere for 4 hours, the Cr 2 o 3 -γ-Al 2 o 3 Impregnated again, dried, and calcined, and repeated this process three times to obtain the carbon-containing Cr 2 o 3 -γ-Al 2 o 3 , put it into a fixed bed reactor and feed HF and N 2 A mixture of gas for fluorination, where HF and N 2 The molar ratio is 1:4, the fluorination temperature is 400°C, and the fluorination time is 10 hours. Finally, the fluori...

Embodiment 3

[0038] Weigh 10g specific surface area is 350m 2 g -1 Aluminum oxide was dried in vacuum at 120°C for 4 hours, and 7.5ml of 0.9235mol / L chromium nitrate nonahydrate solution was impregnated into the dried γ-Al 2 o 3 , impregnated for 10 hours, dried in an oven at 120°C for 10 hours, and then calcined in a muffle furnace at 500°C for 4 hours to obtain Cr 2 o 3 The Cr content is 5% of the mass of the carrier 2 o 3 -γ-Al 2 o 3 Composite oxides, secondly, add 11ml of 15% sucrose aqueous solution to the precursor, soak for 5 hours, and dry at 500°C N 2 Roasting under the atmosphere for 4 hours, the Cr 2 o 3 -γ-Al 2 o 3 Impregnated again, dried, and calcined, and repeated this process three times to obtain the carbon-containing Cr 2 o 3 -γ-Al 2 o 3 , put it into a fixed bed reactor and feed HF and N 2 A mixture of gas for fluorination, where HF and N 2 The molar ratio is 1:4, the fluorination temperature is 400°C, and the fluorination time is 10 hours. Finally, the ...

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Abstract

The invention discloses a catalyst for fluoridizing chlorinated olefin. Alpha-AlF3 is used as a carrier, Cr2O3 is used as an active component, the Cr2O3 is loaded on the alpha-AlF3 carrier, the mass of the Cr2O3 is 0.6-13 percent of that of the alpha-AlF3, and the specific surface area of the catalyst is 90-125m<2>g<-1>. The catalyst is prepared by adopting the steps of: dipping a chromic solublesalt solution on aluminum oxide by adopting a dipping method, drying and calcining to prepare a Cr2O3-gamma-AlO3 composite oxide; dipping a cane sugar water solution to the Cr2O3-gamma-AlO3 compositeoxide, converting cane sugar into carbon through carbonization in the presence of N2 to obtain a carbon-containing Cr2O3-gamma-AlO3 composite oxide, fluoridizing the carbon-containing Cr2O3-gamma-AlO3 composite oxide by using an HF and N2 mixed gas to ensure that the carbon-containing Cr2O3-gamma-AlO3 composite oxide is converted into a carbon-containing Cr2O3-alpha-AlO3 composite; and finally, removing carbon through a combustion method.

Description

technical field [0001] The invention relates to a fluorination catalyst and a preparation method thereof, in particular to a catalyst for fluorinating chloroalkenes and a preparation method thereof. Background technique [0002] The large-scale industrial production of chlorofluorocarbons and hydrofluorocarbons usually adopts the method of gas-phase fluorinated chloroalkenes, which has the advantages of simple equipment, easy continuous large-scale production, safety, and environmental protection. The fluorination catalyst plays a central role in the gas-phase fluorination of chloroalkenes. At present, chromium-based catalysts and aluminum fluoride-based catalysts are commonly used fluorination catalysts in the prior art, and are also the technical core of fluorinated hydrocarbon production. It has been proved that The specific surface area of ​​the carrier and catalyst is closely related to the catalytic activity. The larger the specific surface area, the higher the catalyt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/132B01J35/10C07C17/087C07C17/20
Inventor 罗孟飞于洪波彭小波贾文志谢冠群王月娟
Owner ZHEJIANG NORMAL UNIVERSITY
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