Aluminum base catalyst for preparing vinyl fluoride from 1,1-difluoroethane, and preparation method and application thereof
A difluoroethane and catalyst technology, applied in the field of aluminum-based catalysts and its preparation, can solve the problems of complex catalyst preparation methods and unfavorable industrial scale-up
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Embodiment 1
[0028] According to the molar ratio of Al to Y is 1:0.05, weigh 20.39g of γ-Al 2 o 3 and 7.66g of Y(NO 3 ) 3 ·6H 2 O, first set Y(NO 3 ) 3 ·6H 2 Dissolve O in a certain amount of water to make it fully dissolved, and then add γ-Al 2 o 3 , let it stand for 10 hours to fully impregnate it, then dry it at 105°C for 24 hours, and finally roast it at 600°C for 3 hours to obtain the catalyst precursor Y 2 o 3 / γ-Al 2 o 3 . The catalyst precursor was dried in situ with nitrogen at 200 °C for 6 h, and then passed through HF:N 2 It is a mixed gas of 1:10, fluorinated at 180°C for 4 hours, then heated up to 340°C at a rate of 1°C / min, and gradually increased the concentration of hydrogen fluoride, until the later stage was fed with pure hydrogen fluoride for 8 hours to obtain an aluminum-based catalyst.
[0029] The prepared aluminum-based catalyst is used in the gas-phase dehydrofluorination reaction of 1,1-difluoroethane, and the reaction temperature is controlled at 250-...
Embodiment 2
[0034] According to the molar ratio of Al:Y:Ni is 1:0.04:0.01, weigh 20.39g of γ-Al 2 o 3 , 6.13g of Y (NO 3 ) 3 ·6H 2 O, 1.16g of Ni(NO 3 ) 2 ·6H 2 O, first set Y(NO 3 ) 3 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 Dissolve O in a certain amount of water to fully dissolve the two, and then add γ-Al 2 o 3 , let it stand for 12 hours to make it fully impregnated, then dried at 110°C for 12 hours, and finally calcined at 800°C for 2 hours to obtain the catalyst precursor NiO-Y 2 o 3 / γ-Al 2 o 3 . The catalyst precursor was dried in situ with nitrogen at 300 °C for 4 h, and then passed through HF:N 2 It is a mixed gas of 1:10, fluorinated at 180°C for 4 hours, then heated up to 340°C at a rate of 1°C / min, and gradually increased the concentration of hydrogen fluoride, until the later stage was fed with pure hydrogen fluoride for 8 hours to obtain an aluminum-based catalyst.
[0035] The prepared aluminum-based catalyst was used in the gas-phase dehydrofluorination reaction of ...
Embodiment 3
[0039] According to the molar ratio of Al:Y:Ni:Co of 1:0.03:0.01:0.01, weigh 20.39g of γ-Al 2 o 3 , 4.60g of Y (NO 3 ) 3 ·6H 2 O, 1.16g of Ni(NO 3 ) 2 ·6H 2 O, 1.43g of Co(NO 3 ) 2 ·6H 2 O, first set Y(NO 3 ) 3 ·6H 2 O, Ni(NO 3 ) 2 ·6H 2 O, Co(NO 3 ) 2 ·6H 2 Dissolve O in a certain amount of water to fully dissolve the three, and then add γ-Al 2 o 3 , let stand for 6h to fully impregnate, then dry at 150°C for 10h, and finally roast at 500°C for 6h to obtain the catalyst precursor Co 3 o 4 -NiO-Y 2 o 3 / γ-Al 2 o 3 . The catalyst precursor was dried in situ with nitrogen at 400 °C for 2 h, and then passed through HF:N 2 It is a mixed gas of 1:10, fluorinated at 180°C for 4 hours, then heated up to 340°C at a rate of 1°C / min, and gradually increased the concentration of hydrogen fluoride, until the later stage was fed with pure hydrogen fluoride for 8 hours to obtain an aluminum-based catalyst.
[0040] The prepared aluminum-based catalyst was used in ...
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