Preparation method of butyl ammonium black drug

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Synthesis of first-butyl dithiophosphate acid (Ding Hei drug), and then generate ammonia butylammonium aerofloat effect.
Synthesis of dibutyl dithiophosphoric acid Put n-butanol into the reactor, add phosphorus pentasulfide at 70-80 ° C under stirring, the ratio of butanol to phosphorus pentasulfide is 4:1, and the vulcanization released during the reaction. The hydrogen is absorbed by sodium hydroxide, and after the raw material is added, it is kept at 80 to 85 hours, cooled, and left to be filtered to obtain dibutyl dithiophosphoric acid (butyl black medicine). The reaction formula is as follows:
S
70-80 ° C CH 3 CH 2 CH 2 CH 2 O /
4CH 3 CH 2 CH 2 CH 2 OH+P 2 S 5 —————→ P—SH+H 2 S
CH 3 CH 2 CH 2 CH 2 O /
Synthesis of dibutyl dithiophosphate; dissolving dibutyl dithiophosphoric acid in light gasoline or hexane, the ratio of light gasoline to black medicine is about 3:1, maintaining a certain temperature under stirring, and introducing ammonia Gas neutralization, white crystals are formed after neutralization, and filtered under reduced pressure to obtain butyl ammonium black drug. The reaction formula is as follows:
S S
CH 3 CH 2 CH 2 CH 2 O / CH 3 CH 2 CH 2 CH 2 O /
P-SH+NH 3 —→ P—SNH 4
CH 3 CH 2 CH 2 CH 2 O / CH 3 CH 2 CH 2 CH 2 O /
Ding black medicine
The method for producing the butyl ammonium black medicine is unsafe. The pharmaceutical factory does not use the light gasoline solvent, but uses water as a solvent to form an aqueous solution of the butyl ammonium black medicine. After drying, the solid butyl ammonium black medicine is obtained. In order to save ammonia, sodium sulphate can also be made by using sodium hydroxide instead of ammonia.

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