Method for synthesizing 2,3,3,3-tetrafluoropropene
A synthetic method, fluorine and chlorine technology, applied in 2 fields, can solve the problems such as the difficulty of catalyst preparation, achieve the effect of major industrial application prospects, easy to obtain, and less by-products
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Embodiment 1
[0034] (1) The raw material DMF (1.25 grams), carbon tetrachloride (45.21 grams), ethylene (15.43 grams) that the telomerization reaction is used are added successively to volume is 120ml, in the stainless steel container that valve is housed, concussion shakes up, as Mix raw materials; (2) in the reactor of the PFE pipe material of 15 inches in length, 1 / 8 inch in diameter, the composite metal filler of iron, chromium, nickel is filled inside, is heated to 120 ℃ in the electric furnace; (3) uses metering Pump mixes raw material with the flow rate of 0.2 milliliters / minute and squeezes in the reactor, and reaction pressure is 0.6Mpa, (4) after reacting 10min, cold trap collects reaction product, measures product composition with GC, and wherein TCP selectivity is 96.5%, Based on carbon tetrachloride, the yield of TCP is 68.2%, and the purity of TCP is 99% after purification by distillation under reduced pressure. (5) Add TCP in a 2L high-pressure reactor with a stirring device...
Embodiment 2
[0037] (1) Add 1.25 grams of DMF, 45.21 grams of carbon tetrachloride, and 15.43 grams of ethylene in a stainless steel container with a volume of 120 ml, and shake it well as a mixed raw material; (2) 15 inches in length and 1 in diameter / 8-inch PFE pipe reactor, filled with iron, chromium, nickel composite metal filler, heated to 120 ° C in an electric furnace; (3) use a metering pump to drive the mixed raw materials into the In the reactor, the reaction pressure is 0.8MPa, (4) after reacting for 30min, the cold trap collects the reaction product, and measures the product composition with GC, wherein the TCP selectivity is 97.6%, and in terms of carbon tetrachloride, the productive rate of TCP is 72.4% %; The reacted mixture reclaims unreacted raw material and cocatalyst by the method for distillation, and underpressure distillation obtains the TCP that purity is 99%. (5) Add TCP in a 2L autoclave with stirring device, and chlorine gas is added to the autoclave through a po...
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