Complete method for preparing diethylaminoethanethiol
A complete technology of ethylaminoethane mercaptan, applied in the field of preparing diethylaminoethane mercaptan, can solve the problems of low product purity, environmental pollution, complicated reaction operation and the like
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Embodiment 1
[0035] Use a double-cone vacuum dryer to dry sodium thiocyanate, vacuumize under negative pressure, and under the condition of vacuum degree -0.07 MPa, heat and dry sodium thiocyanate, heat up to 120°C, dry for 1.5 hours, and rotate at a speed of 3-4 r / min, water-cooled to 50°C, slowly fill the system with nitrogen to normal pressure during cooling, and seal it to achieve air isolation and heat preservation.
[0036] For the cyclization reaction of sodium thiocyanate and ethylene carbonate, add 500 kg ethylene carbonate into the cyclization kettle, start stirring at a stirring speed of 60-70 r / min, then add dry sodium thiocyanate, ethylene carbonate and sulfur The molar ratio of sodium cyanate reaction is 1:1.03, continue to fill nitrogen to the micro pressure level of 0-0.3 kpa, slowly raise the temperature to 80°C to start the reaction, stop nitrogen filling, continue to heat up, maintain 105°C, until no liquid flows out of the sight glass At the end of the distillation, the...
Embodiment 2
[0040] Use a double-cone vacuum dryer to dry sodium thiocyanate, negative pressure vacuum, vacuum degree -0.08 MPa, heat and dry sodium thiocyanate, heat up to 130 ° C, drying time 1.5 hours, speed 3-4 r / min, cool down to 48°C, slowly fill the system with nitrogen to normal pressure during cooling, and seal it to achieve air isolation and heat preservation.
[0041] For the cyclization reaction of sodium thiocyanate and ethylene carbonate, add 500 kg ethylene carbonate into the cyclization kettle, start stirring at a stirring speed of 60-70 r / min, then add dry sodium thiocyanate, ethylene carbonate and sulfur The molar ratio of sodium cyanate reaction is 1:1.1, continue to fill nitrogen to the micro pressure level of 0-0.3 kpa, slowly raise the temperature to 80°C to start the reaction, stop nitrogen filling, continue to heat up, maintain 110°C, until no liquid flows out of the sight glass At the end of the distillation, the gas phase generated by the addition reaction is cond...
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