Process for producing fluorinated propene
A manufacturing method and technology of trifluoropropene, which are applied in the directions of organic chemistry methods, chemical instruments and methods, dehydrohalogenation preparation, etc., can solve the problems of difficulty in improving the selectivity of target products and low yields, etc.
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[0032] The preparation method of the supported catalyst is not particularly limited. In the case of supporting a liquid substance at normal temperature, it can be adsorbed into the carrier by dripping, dipping, spraying, or the like. When a solid substance is supported at normal temperature, it can be dissolved and immersed in a solvent or the like, or it can be adsorbed by spraying or the like. The carrier on which the metal compound is adsorbed is dried by heating, depressurizing, or depressurizing while heating to remove excess solvent, etc., and then activated with hydrogen fluoride, hydrogen chloride, chlorine, chlorinated fluorinated hydrocarbon, etc. under heating, and then used.
[0033] The solvent is not particularly limited as long as it can dissolve the metal compound and does not decompose due to the reaction. Examples include alcohols such as water, methanol, ethanol, and isopropanol; ketones such as methyl ethyl ketone and acetone; and acetic acid. Carboxylic a...
preparation example 1
[0049] Weigh 300 g of activated alumina (NKHD-24 manufactured by Sumitomo Chemical: particle size 2-4 mm, specific surface area 340 m) 2 / g), wash the powder attached to the surface with water. 115 g of hydrogen fluoride was dissolved in 1035 g of water to prepare 10% hydrofluoric acid. The washed activated alumina was slowly added to 10% hydrofluoric acid, stirred and left to stand for 3 hours. Next, it was washed with water and filtered, and then dried in an electric furnace at 200° C. for 2 hours. 400 ml of dried activated alumina was filled into a gas-phase reaction device (made of SUS316L, diameter 3.8 cm, length 42 cm) consisting of a cylindrical reaction tube equipped with an outer jacket connected to a heating medium circulation device, and nitrogen gas was passed through it. The heating medium temperature was set to 200°C. Next, hydrogen fluoride was introduced together with nitrogen gas and the hydrogen fluoride / nitrogen gas molar ratio was set to 1 / 10 to 1 / 5 to p...
preparation example 2
[0051] 300g of special-grade reagent Cr(NO 3 ) 9H 2 O is dissolved in 1 liter of water to prepare an aqueous solution, and 1.8 liters of 4-8 mm in diameter and a specific surface area of 1200 m are immersed in it. 2 / g, granular activated carbon with a pore diameter of 18A (manufactured by Japan Enviro Chemicals.ltd, Granular Egret G2X), and left to stand all day and night. Next, after filtering the activated carbon, it was kept at 100° C. in a hot air circulation dryer, and further dried all day and night. 400 ml of the obtained chromium-supported activated carbon was filled into a gas-phase reaction apparatus (made of SUS316L, diameter 3.8 cm, length 42 cm) consisting of a cylindrical reaction tube equipped with a jacket connected to a heating medium circulation apparatus, and nitrogen gas was introduced into it. The heating medium temperature was raised to 300°C. When the discharge of water was not seen, hydrogen fluoride was introduced together with nitrogen gas and t...
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