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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[0033] Example 1
[0034] (1) Add DMF (1.25g), carbon tetrachloride (45.21g), and ethylene (15.43g) used in the telomerization reaction to a stainless steel container with a volume of 120ml and equipped with a valve. Mixed raw materials; (2) In a reactor with a length of 15 inches and a diameter of 1 / 8 inch PFE pipes, the inside is filled with composite metal fillers of iron, chromium, and nickel, and heated to 120°C in an electric furnace; (3) metering The pump pumps the mixed raw materials into the reactor at a flow rate of 0.2 ml / min. The reaction pressure is 0.6Mpa. (4) After 10 minutes of reaction, the reaction product is collected in a cold trap and the product composition is determined by GC. The TCP selectivity is 96.5%. Based on carbon tetrachloride, the yield of TCP was 68.2%, and the purity of TCP after purification under reduced pressure was 99%. (5) Add TCP to a 2L high-pressure reactor with a stirring device, and add chlorine to the high-pressure reactor through a ...
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[0036] Example 2
[0037] (1) Add 1.25 g of DMF, 45.21 g of carbon tetrachloride, and 15.43 g of ethylene to a stainless steel container with a volume of 120ml and a valve, and shake it evenly, as the mixed raw material; (2) 15 inches in length and 1 in diameter A reactor with / 8 inch PFE pipes is filled with composite metal fillers of iron, chromium and nickel, and heated to 120°C in an electric furnace; (3) The mixed raw materials are fed into the reactor at a flow rate of 0.2 ml / min with a metering pump In the reactor, the reaction pressure is 0.8MPa. (4) After 30 minutes of reaction, the reaction products are collected in a cold trap, and the product composition is determined by GC. The TCP selectivity is 97.6%, and the TCP yield is 72.4 based on carbon tetrachloride. %; the reacted mixture is distilled to recover unreacted raw materials and co-catalysts, and vacuum distillation is used to obtain TCP with 99% purity. (5) Add TCP to a 2L autoclave with a stirring device, and ...
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