A kind of method for synthesizing O,O-dimethyl phosphorodithioate
A technology of dimethyl phosphorodithioate and methyl sulfide, which is applied in the field of synthesis of O,O-dimethyl phosphorodithioate, can solve the problem of low product yield, and achieve the goal of increasing content and yield efficiency, improve the low content of synthetic products, and promote the effect of positive progress
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Embodiment 1
[0020] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:
[0021] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;
[0022] (2) Mix 0.5kg DMAP and 0.5kg pyridine as a catalyst, add to 580kg methanol and mix to obtain reaction feed liquid B;
[0023] (3) control the pressure condition of the reactor to be 30mmHg vacuum degree, and raise the temperature of the reaction feed liquid A in the reactor to 25° C., and start to drop the reaction feed liquid B in the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 50° C. for heat preservation reaction for 1 hour. During the reaction, the hydrogen sulfide g...
Embodiment 2
[0026] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:
[0027] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;
[0028] (2) Get 1.5kg DMAP and 1kg of pyridine to mix as catalyst, add to 584kg methanol and mix well to obtain reaction feed liquid B;
[0029] (3) Control the pressure condition of the reactor to be 30mmHg vacuum degree, and raise the temperature of the reaction feed liquid A in the reactor to 30° C., and start to drop the reaction feed liquid B in the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 55° C. for a heat preservation reaction for 1 hour. During the reaction, the hydro...
Embodiment 3
[0032] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:
[0033] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;
[0034] (2) Take 0.8kg DMAP and 1kg of pyridine and mix it as a catalyst, add to 581kg methanol and mix well to obtain reaction feed liquid B;
[0035] (3) Control the pressure condition of the reactor to be 40mmHg vacuum, and raise the temperature of the reaction feed liquid A in the reactor to 35° C., and start to add the reaction feed liquid B dropwise to the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 55° C. for a heat preservation reaction for 1 hour. During the reaction, t...
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