Preparation method for chlorotrifluoropropylene
A technology of monochlorotrifluoropropene and trifluorodichloropropane, which is applied in the field of preparation of monochlorotrifluoropropene, can solve the problems of high energy consumption, unsuitability for industrial scale-up production, and impossibility of obtaining it, and achieve low reaction temperature, The effect of meeting the requirements of industrial scale-up production
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Embodiment 1
[0019] 10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride, 200 grams of dimethylformamide and 500 grams of sulfolane, add 6160 grams of carbon tetrachloride, and feed into the stainless steel autoclave jacket Steam heating, start the stirring of autoclave, when autoclave material system temperature rises to 80 ℃, stop passing steam, press into 1250 grams of vinyl chloride. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 100° C., control the temperature of the reaction system to maintain at 100-105° C., and keep the reaction system in this temperature range for 13 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 4317 grams.
[0020] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the ref...
Embodiment 2
[0024] 10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride and 600 grams of sulfolane, add 6160 grams of carbon tetrachloride, steam into the stainless steel autoclave jacket, start the stirring of the autoclave , when the temperature of the autoclave material system rose to 80°C, the steam was stopped, and 1500 grams of vinyl chloride were pressed. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 120° C., control the temperature of the reaction system to maintain at 110 to 125° C., and keep the reaction system in this temperature range for 11 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 5034 grams.
[0025] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the reflux ratio are installe...
Embodiment 3
[0029]10L stainless steel autoclave with jacket and cooling water coil, add 200 grams of cuprous chloride, 200 grams of dimethylformamide and 500 grams of sulfolane, add 6160 grams of carbon tetrachloride, and feed into the stainless steel autoclave jacket Steam heating, start the stirring of autoclave, when autoclave material system temperature rises to 80 ℃, stop passing steam, press into 1750 grams of vinyl chloride. After stirring for 2 hours, continue to open the jacket steam valve. After the temperature of the reaction system reaches 130° C., control the temperature of the reaction system to maintain at 125 to 130° C., and keep the reaction system in this temperature range for 9 hours. Cool down to 60 DEG C then, open the discharge bottom valve of autoclave, obtain crude pentachloropropane 6002 grams.
[0030] The 5L four-necked glass flask has a Φ40×2000 glass column, which is filled with a 1900 mm high glass ring packing, and a condenser and a cock for adjusting the re...
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