A kind of preparation method of 1,1,1,3,3-pentachloropropane
A technology for pentachloropropane and vinyl chloride, which is applied in the field of preparation of 1,1,1,3,3-pentachloropropane, can solve the problems of unstable properties, deposition of iron powder, affecting rectification operation and product yield, etc. , to achieve the effect of shortening the reaction time, increasing the reaction speed, and shortening the residence time
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[0024] The invention is a preparation method of 1,1,1,3,3-pentachloropropane, which uses carbon tetrachloride and vinyl chloride as raw materials, and then mixes corresponding catalysts and co-catalysts in a tubular reactor for adjustment. Polymerization reaction, thereby obtain 1,1,1,3,3-pentachloropropane, its concrete preparation steps are as follows:
[0025] (1) Carbon tetrachloride, vinyl chloride and cocatalyst are fully mixed to form a mixture, fully stirred to ensure that carbon tetrachloride and vinyl chloride are fully mixed, the mixture is placed in a preheater, and the mixture is preheated by the preheater Heat to 100-140°C, preferably preheating to 100-120°C; wherein the molar ratio of carbon tetrachloride to vinyl chloride is (1-10):1, wherein the preferred molar ratio of carbon tetrachloride to vinyl chloride The ratio is (1.5-5): 1. When retrieving the materials, the weight of each reclaimed material is generally converted into molar mass, so as to control the...
Embodiment 1
[0034] First, fully mix 432.4g carbon tetrachloride, 69.4g vinyl chloride and 7.4g trimethyl phosphate to form a mixture. The calculated molar ratio of carbon tetrachloride to vinyl chloride is 2:1, and the cocatalyst trimethyl phosphate accounts for The mass percentage of raw materials is 1.45%. Fully stir the mixture, put the mixture in the preheater, and use the preheater to preheat the mixture to 120°C; then take the telomerization reactor, the diameter of the telomerization reactor is Ф20×2.5mm, and the length is 1m externally heated tubular glass reactor. In the externally heated tubular glass reactor, the composite metal catalyst is loaded, and the filling amount of the composite metal catalyst is 80% of the reactor volume, wherein the content of each component in the composite metal catalyst is: iron is 90%, nickel is 4.5%, chromium is 5.5%. Next, the preheated mixture was introduced into an externally heated tubular glass reactor, and the telomerization reaction was...
Embodiment 2
[0043] First, fully mix 426.7g carbon tetrachloride, 40.1g vinyl chloride and 12.5g triethyl phosphate to form a mixture. The calculated molar ratio of carbon tetrachloride to vinyl chloride is 4.32:1, and the cocatalyst triethyl phosphate accounts for The mass percentage of raw materials is 2.61%. Fully stir the mixture, put the mixture in the preheater, and use the preheater to preheat the mixture to 120°C; then take the telomerization reactor, the diameter of the telomerization reactor is Ф20×2.5mm, and the length is 1m externally heated tubular glass reactor. In the externally heated tubular glass reactor, the composite metal catalyst is loaded, and the filling amount of the composite metal catalyst is 90% of the reactor volume, wherein the content of each component in the composite metal catalyst is: iron is 90%, nickel is 4.5%, and chromium is 90%. 5.5%. Next, the preheated mixture was introduced into an externally heated tubular glass reactor, and the telomerization r...
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