Dehydrofluorination catalyst
A dehydrofluorination and catalyst technology, applied in the field of dehydrofluorination catalysts, can solve the problem of low selectivity of active Z-type fluoroolefins, and achieve the effect of high selectivity and good activity
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Embodiment 1
[0024] Dissolve chromium nitrate in water, add precipitant ammonia water at 60°C, control the pH of the solution between 7.5-8.5, and make it fully precipitate under stirring conditions, filter the formed slurry, and wash with deionized water to neutral , And then dried at 150℃ for 12 hours to obtain Cr(OH) 3 .
[0025] The obtained Cr(OH) 3 It is mixed with ammonium hexafluorotitanate into 70% and 30% by mass, and then compressed into tablets to obtain a catalyst precursor. The catalyst precursor is roasted in a muffle furnace at 400°C for 10 hours, and then loaded into a tubular reactor , The temperature is raised to 300 DEG C, and hydrogen fluoride gas is introduced to activate it for 2 hours, then the temperature is raised to 350 DEG C at a heating rate of 1 DEG C / min, and the activation is continued for 10 hours to prepare a dehydrofluorination catalyst.
[0026] The specific surface area of the catalyst measured by the BET low-temperature nitrogen adsorption method is 56.1m...
Embodiment 2
[0029] The preparation process of the catalyst is basically the same as that of Example 1, except for Cr(OH) 3 The mass of ammonium hexafluorotitanate is divided into 80% and 20%.
[0030] The specific surface area of the catalyst determined by the BET low-temperature nitrogen adsorption method is 53.5m 2 ·G -1 , The pore volume is 0.18ml·g -1 , And the proportion of pores with a pore diameter of less than 2nm is 33%.
[0031] A nickel tube fixed bed reactor with an inner diameter of 38mm is filled with 30ml of the dehydrofluorination catalyst prepared above, the reaction temperature is 350℃, and the HFC-236ea space velocity is 100h -1 After 100 hours of reaction, the samples were washed with water, alkali washed and dried, and analyzed by GC-MS. The conversion rate of HFC-236ea was 98% and the selectivity of Z-HFO-1225ye was 96%.
Embodiment 3
[0033] The preparation process of the catalyst is basically the same as that of Example 1, except for Cr(OH) 3 The mass percentage of ammonium hexafluorotitanate becomes 60% and 40%.
[0034] The specific surface area of the catalyst measured by the BET low-temperature nitrogen adsorption method is 46.3m 2 ·G -1 , The pore volume is 0.19ml·g -1 , And the proportion of pores with a pore diameter of less than 2nm is 32%.
[0035] A nickel tube fixed bed reactor with an inner diameter of 38mm is filled with 30ml of the dehydrofluorination catalyst prepared above, the reaction temperature is 350℃, and the HFC-245eb space velocity is 50h -1 After 100 hours of reaction, the samples were washed with water, alkali washed and dried, and analyzed by GC-MS. The conversion rate of HFC-245eb was 95% and the selectivity of Z-HFO-1234ze was 90%.
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