Production technology of 2-sulfamide-N,N-dimethylnicotinamide
A technology of dimethylnicotinamide and production process, which is applied in the direction of organic chemistry, can solve the problems of low yield and odor, and achieve the effects of increasing yield, reducing emissions, and avoiding odor and sulfide by-products
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Embodiment 1
[0017] 1. Add 50kg of 2-chloro-N,N-dimethylnicotinamide and 23kg of thiourea into the 500L enamel reaction kettle through the feeding port, and add 200kg of 2wt% HCl from the head tank through the flow meter. Open the steam valve and raise the temperature to 80 o C, stirring the reaction for 1h.
[0018] 2. Put 2.5kg of acetic acid from the acetic acid storage tank into the reaction kettle in step 1 through the metering pump, and put frozen brine into the jacket to cool down to -5 o c. Cl 2 The above reaction materials are blown into the liquid chlorine storage tank through the liquid chlorine vaporizer and gas flow meter, and react for 1 hour. use N 2 Bubble removal of dissolved Cl 2 , and then centrifuged to obtain 2-sulfonyl chloride-N,N-dimethylnicotinamide, and the filtrate was sent to the waste water treatment device.
[0019] 3. Add the 2-sulfonyl chloride-N,N-dimethylnicotinamide obtained in step 2 into a 500L enamel reaction kettle through the feeding port, 200k...
Embodiment 2
[0021] 1. Add 50kg of 2-chloro-N,N-dimethylnicotinamide and 29kg of thiourea into the 500L enamel reaction kettle through the feeding port, and add 300kg of 10wt% HCl from the head tank through the flow meter. Open the steam valve and raise the temperature to 100 o C, stirring the reaction for 2h.
[0022] 2. Put 10kg of acetic acid from the acetic acid storage tank into the reaction kettle in step 1 through the metering pump, and put frozen brine into the jacket to cool down to -10 o c. Cl 2 From the liquid chlorine storage tank, the above reaction materials are blown into the liquid chlorine vaporizer and gas flow meter, and react for 2 hours. use N 2 Bubble removal of dissolved Cl 2 , and then centrifuged to obtain 2-sulfonyl chloride-N,N-dimethylnicotinamide, and the filtrate was sent to the waste water treatment device.
[0023] 3. Add the 2-sulfonyl chloride-N,N-dimethylnicotinamide obtained in step 2 into a 500L enamel reaction kettle through the feeding port, 30...
Embodiment 3
[0025] 1. Add 50kg of 2-chloro-N,N-dimethylnicotinamide and 25kg of thiourea into the 500L enamel reaction kettle through the feeding port, and add 225g of 5wt% HCl from the head tank through the flow meter. Open the steam valve and raise the temperature to 90 o C, stirring the reaction for 1.5h.
[0026] 2. Put 6 kg of acetic acid from the acetic acid storage tank into the reaction kettle in step 1 through the metering pump, and put frozen brine into the jacket to cool down to -15 o c. Cl 2 The above reaction materials are blown into the liquid chlorine storage tank through the liquid chlorine vaporizer and gas flow meter, and react for 1.4 hours. use N 2 Bubble removal of dissolved Cl 2 , and then centrifuged to obtain 2-sulfonyl chloride-N,N-dimethylnicotinamide, and the filtrate was sent to the waste water treatment device.
[0027] 3. Add the 2-sulfonyl chloride-N,N-dimethylnicotinamide obtained in step 2 into a 500L enamel reaction kettle through the feeding port,...
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