Green synthesis technology of O,O-diethyl thiophosphoryl chloride
A technology of ethyl thiophosphoryl and diethyl dithiophosphoric acid ester, which is applied in the field of green synthesis technology of O,O-diethyl thiophosphoryl chloride, can solve the problem of affecting the surrounding environment, serious environmental pollution, production It can prevent air pollution, easily obtain raw materials, and reduce processing costs.
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Embodiment 1
[0030] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:
[0031] S1. Put 800kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after adding phosphorus pentasulfide, add the remaining 1000kg of absolute ethanol and 3kg of the mixed solution of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3318kg of O,O-diethyl phosphorodithioate.
[0032] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 35°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.6kg / min. When the molar ratio of chlorine gas to O, O-diethyl phosphorodithioate reaches 1:1.2, stop the chlorine flow.
[0033] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirrin...
Embodiment 2
[0037] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:
[0038] S1. Put 750kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after the phosphorus pentasulfide is put in, add the remaining 1000kg of absolute ethanol and 3kg of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3312kg of O,O-diethyl phosphorodithioate.
[0039] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 40°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.6kg / min. When the molar ratio of chlorine gas to O,O-diethyl phosphorodithioate reaches 1:1.3, stop the chlorine flow.
[0040] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirring, add 2kg of co...
Embodiment 3
[0044] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:
[0045] S1. Put 700kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after the addition of phosphorus pentasulfide, add the remaining 1000kg of absolute ethanol and 3kg of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3306kg of O,O-diethyl phosphorodithioate.
[0046] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 45°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.8kg / min. When the molar ratio of chlorine gas to O, O-diethyl phosphorodithioate reaches 1:1.2, stop the chlorine flow.
[0047] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirring, add 2kg of...
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