Process for preparing 2, 3-dichloropropylene
A preparation process and a technology for dichloropropene, which are applied in the field of pesticide intermediates 2, can solve the problems of high production cost and low product reaction yield, and achieve the effects of reduced production cost, simple process and improved quality
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Embodiment 1
[0015] (1) Use allyl chloride as the starting material to react with chlorine to generate 1,2,3-trichloropropane
[0016] a. Reaction equation
[0017]
[0018] b. Operating procedures
[0019] Put 1000g of allyl chloride into the reaction bottle, stir and freeze the brine, and lower the temperature to about 0°C; open the main chlorine valve, start to feed chlorine gas into the reaction bottle, and control the humidity not to exceed 25°C, and let it pass for about 5 hours. Inject about 946g of chlorine gas, and use gas spectrum to track the raw material <3%, then stop the chlorine gas flow; stir at about 25°C for 1 hour, and then use a slight negative pressure to remove excess chlorine gas. After about 20 minutes, discharge and weigh to obtain about 1900 g of 1,2,3-trichloropropane.
[0020] c. Feeding ratio
[0021] Allyl chloride: chlorine = 1: 1.02 (mol ratio)
[0022] (2) react with 1,2,3-trichloropropane and liquid caustic soda to generate 2,3-dichloropropene
[0...
Embodiment 2
[0030] (1) Put 951g of 1,2,3-trichloropropane (93%) and 25g of TEBA into the reaction flask, start stirring, and raise the temperature to 80°C.
[0031] (2) Add 453g of ethanol to 960g of liquid caustic soda, slowly drop into the reaction kettle after mixing, reflux for about 2 hours after dripping, and remove the water layer; add 400g of water to the reaction bottle, change reflux to distillation, collect The 93-105°C fraction yielded 512 g of 2,3-dichloropropene, with a content of 95.1% and a yield of 72.5%.
Embodiment 3
[0033] (1) drop 1000g allyl chloride into the reaction bottle, start stirring, freeze the brine, and reduce the temperature to about 0°C; open the main chlorine valve, start to feed chlorine into the reaction bottle, and control the humidity to be no more than 25°C, Introduce about 946g of chlorine gas for about 5 hours, and track the raw material to 3% by gas spectrometry, then stop the chlorine gas flow; stir at about 25°C for 1 hour, and then use a slight negative pressure to remove excess chlorine gas. After about 20 minutes, the materials were discharged and weighed to obtain 1908 g of 1,2,3-trichloropropane with a content of 93.5% and a yield of 92.5%.
[0034] (2) Put 951g of 1,2,3-trichloropropane and 25g of TEBA into the reaction bottle, start stirring, and after raising the temperature to 80°C, add 960g of liquid caustic soda dropwise; layer; add 400g water in the reaction bottle, change the reflux to distillation, use the oil-water separator, and the oil enters the ...
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