Prepn of aliphatic fluoride
A kind of compound, technology of fluorinated fat, applied in the field of preparation of fluorinated aliphatic compounds
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Embodiment 1
[0048] Synthesis of perfluoro-2-butene
[0049] at 0.3dm 3 A volumetric tubular reactor made of stainless steel equipped with electric heating, thermocouple sheath, and tubes for adding starting components and discharging reaction products was added with about 0.23dm 3 , 35% by weight potassium fluoride promoted silica catalyst. The catalyst was heated in a stream of dry nitrogen, gradually increasing its temperature from 180°C to 350°C over 4 hours. Then, the temperature was allowed to drop to 240° C., and 40 grams of methyl perfluorovalerate were added at a rate of 20 grams / hour. The gas mixture discharged from the reactor was condensed in a trap cooled to -30°C and subjected to cryogenic rectification, whereby 27.4 g of perfluoro-2-butene were obtained. The yield of the target product was 95.1%.
Embodiment 2
[0051] Synthesis of 2-Hydroheptafluoropropane
[0052] In the tubular reactor described in embodiment 1, add about 0.23dm 3 , 30% by weight potassium fluoride promoted activated carbon catalyst. The catalyst was heated in a stream of dry nitrogen, gradually increasing its temperature from 180°C to 350°C over 4 hours. Then, the temperature was allowed to drop to 250°C, and 50 g of methyl perfluoroisobutyrate and 7.5 g of hydrogen fluoride were added within 1 hour. The gas mixture discharged from the reactor was passed through potassium hydroxide solution, collected in a trap cooled to -30°C, and subjected to cryogenic rectification. 36.5 g of the target product are obtained, corresponding to a yield of 98.0%.
Embodiment 3
[0054] Synthesis of 1-Hydropentafluoroethane
[0055] In the tubular reactor described in embodiment 1, add about 0.21dm 3 , 40% by weight cesium fluoride promoted silica catalyst. The catalyst was heated in a stream of dry nitrogen, gradually increasing its temperature from 180°C to 350°C over 4 hours. Then, the temperature was allowed to drop to 260°C, and 20 grams of perfluoropropionyl fluoride and 4 grams of hydrogen fluoride were added over a period of 1 hour. The hydrogen fluoride was added to the middle of the reactor. The gas mixture discharged from the reactor was condensed in a trap cooled to -30°C and subjected to cryogenic rectification. 13 g of the target product indicated in the title of this example were obtained, corresponding to a yield of 89.7%.
[0056] Subsequent syntheses were carried out analogously to Examples 1, 2 (Examples 4-19). The synthesis conditions and results are listed in the table below.
[0057] Thus, a unique method was developed for th...
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