Fluorating catalyst and preparation method
A fluorination catalyst, catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. Reduce the surface area and other problems to achieve the effect of prolonging life and increasing the number of regenerations
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Embodiment 1
[0031] Dissolve chromium nitrate in water, react with precipitant ammonia water at 60°C, adjust the pH value of the reaction solution in the range of 7.5 to 8.5, make it fully precipitate under stirring conditions, filter the formed slurry, and use deionized Wash with water until neutral, then dry at 200°C for 12 hours to obtain Cr(OH) 3 .
[0032] The obtained Cr(OH) 3 with a specific surface area of 300m 2 The pigment / g was uniformly mixed with channel black at a mass ratio of 70:30, and pressed into tablets to obtain a catalyst precursor. In a tubular reactor, roast in a nitrogen atmosphere at 350°C for 6 hours, then feed a mixture of nitrogen and hydrogen fluoride at a ratio of 4:1, fluoride at 200°C for 4 hours, and then raise the temperature to 350°C at a heating rate of 1°C / min. The fluorination was continued for 8 hours to obtain a fluorination catalyst.
[0033] The specific surface area of the catalyst was measured by BET low temperature nitrogen adsorption m...
Embodiment 2
[0038] The preparation technology of catalyst is substantially the same as embodiment 1, and difference is that Cr(OH) 3 The mass ratio of the tank black to the pigment is 50:50.
[0039] The specific surface area of the catalyst was measured by BET low temperature nitrogen adsorption method to be 54.8m 2 g -1 , the pore volume is 0.19ml·g -1 , and the proportion of micropores is 34%.
[0040] In a nickel tube fixed bed tubular reactor with an internal diameter of 38 mm, 30 ml of the above-mentioned prepared fluorination catalyst are loaded into it, and HF and trichloroethylene are introduced to react, and the mol ratio of HF / trichloroethylene is controlled to be 8: 1. The contact time is 3 seconds, the reaction temperature is 250°C, and after 40 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, and the conversion rate of trichlorethylene is 100% according to gas chromatography analysis. HCFC-133a and HFC-134a The overall selec...
Embodiment 3
[0043] The preparation technology of catalyst is substantially the same as embodiment 1, and difference is that Cr(OH) 3 The mass ratio of the tank black to the pigment is 90:10.
[0044] The specific surface area of the catalyst was measured by BET low temperature nitrogen adsorption method to be 45.8m 2 g -1 , the pore volume is 0.18ml·g -1 , and the proportion of micropores is 30%.
[0045] The catalyst is subjected to forced coking deactivation and regeneration again. After the first regeneration, the specific surface area of the fluorination catalyst is 45.6m 2 g -1 , the pore volume is 0.19ml·g -1 , and the proportion of micropores is 29%. After the second regeneration, the specific surface area of the fluorination catalyst is 43.0m 2 g -1 , the pore volume is 0.16ml·g -1 , and the proportion of micropores is 26%.
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Abstract
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