Catalyst used for preparing fluorinated alkene with chloro-fluoro alkane and preparation method thereof
A technology of fluorine-containing olefins and chlorofluoroalkanes, which is applied in the field of refrigerants, can solve the problems of no selective reporting of HFO-1234yf, reduced service life of catalysts, and many separation operations, and achieve low raw material purity requirements, high selectivity, and high yield. high rate effect
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[0061] The above-mentioned preparation method of a catalyst for preparing fluorine-containing olefins from chlorofluoroalkanes, the method comprises the following steps:
[0062] Step 1, preparing an aqueous solution of the soluble salt corresponding to the active component, impregnating the carrier with the aqueous solution of the soluble salt of the active component for more than 6 hours, wherein:
[0063] The active components are composed of alkali metal oxides, rare earth metal oxides and high-valent metal oxides;
[0064] The alkali metal oxide is Li + 、Na + 、K + , Rb + and Cs + one or more of the corresponding oxides;
[0065] Rare earth metal oxides are La 3+ 、Ce 4+ and Y 3+ one or more of the corresponding oxides;
[0066] The high valence metal oxide is Mg 2+ , Cr 3+ , Al 3+ , Fe 3+ , Sn 4+ , Ti 4+ and Zr 4+ one or more of the corresponding oxides;
[0067] Described soluble salt is nitrate, sulfate, chloride or oxalate;
[0068] The carrier adopts ...
Embodiment 1
[0089] This embodiment provides a method for preparing a catalyst for preparing fluorine-containing olefins from chlorofluoroalkanes, the method comprising the following steps:
[0090] (1) Dissolve a mixture of 8.0g sodium nitrate, 15.5g lanthanum chloride and 19.0g zirconium oxychloride in 100mL water to make an active component impregnation solution; mix 45.0g plant-based activated carbon with the above impregnation solution, and Dipping for 12h;
[0091] (2) Dry the impregnated carrier at 80°C for more than 12h, and finally bake it at 400°C for 6h to obtain the catalyst, the mass percentage is: 3.3wt.%Na-13.4wt.%La-14.8wt.%Zr / AC.
[0092] 60mL of the above catalyst (3.3wt.%Na-13.4wt.%La-14.8wt.%Zr / C) was loaded into a nickel tube fixed-bed tubular reactor with an inner diameter of 38mm, the reaction temperature was 450°C, and HCFC-244bb Airspeed 50min -1 , The reaction continued to run for 100h, and the gas product was washed with water, washed with alkali and dried, a...
Embodiment 2
[0094] The difference between the preparation process of the catalyst and Example 1 is only that zirconium oxychloride is changed into ferric chloride, lanthanum chloride is changed into cerium nitrate, the soaking time is changed into 8h, the roasting temperature is changed into 550 ℃, and the roasting time Change it to 3h to obtain a catalyst, the mass percent composition is: 3wt.%Na-10wt.%Ce-8wt.%Fe / AC.
[0095] In a nickel-tube fixed-bed tubular reactor with an inner diameter of 38 mm, 60 mL of the catalyst prepared above (3wt.%Na-10wt.%Ce-8wt.%Fe / AC) was loaded, the reaction temperature was 350°C, and HCFC-243db Airspeed 80min -1 , The reaction continued to run for 100h, and the gas product was washed with water, washed with alkali and dried, and analyzed by gas chromatography. The average conversion rate of HCFC-243db was 97%, and the selectivity of product HCFO-1233xf was 96%.
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