Prepn of high-purity acephate powder (2)
A technology of acephate raw powder and acephate, which is applied in the field of producing high-purity acephate raw powder, can solve the problems of high yield and large amount of organic extractant, and achieve low cost and no waste Liquid discharge, pollution reduction effect
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Embodiment 1
[0023] Be 94% O at 920kg content, add 55.2kg dimethyl sulfate in the crude oil of O-dimethyl phosphorothioate and carry out isomerization, then add the acetic anhydride that 682.6kg concentration is 98% (mass), at 55 ℃ React at low temperature for 3 hours to obtain acephate crude oil with a content of 56.4%; add 3107kg of solvent to the crude oil, then neutralize with ammonia gas to a pH value of 6.5-7.0 under normal pressure, filter and neutralize the ammonium acetate crystals produced, Obtain 4330kg content and be the liquid of 21.6%; This liquid is put into the crystallization kettle with agitation after vacuum precipitating and is cooled to-5-0 ℃ and carries out primary crystallization, separates and obtains 742.6kg crude crystal and 978.4kg mother liquor; put into a crystallization kettle with stirring and cool down to -20°C--10°C for secondary crystallization, and 310.3kg of crude crystals and 282.8kg of secondary mother liquor with a content of 28.1% were separated; the ...
Embodiment 2
[0025] In 880kg of 75% O, S-dimethylphosphoramide crude oil, adding 616kg of 98% acetic anhydride and 8.8kg of 98% sulfuric acid reacted at 55°C for 3 hours to obtain 1504.8kg Acephate crude oil with a content of 55-57%; add 3107kg of solvent to the crude oil, then neutralize it with ammonia gas to a pH value of 6.5-7.0, filter and neutralize the ammonium acetate crystals, and obtain 3959.8kg with a content of 21.2% of liquid. After vacuum precipitating, put it into a stirring crystallization kettle and cool it down to -5°C-0°C for primary crystallization, and separate 657.5kg of crude crystals and 853.6kg of mother liquor. Precipitate the mother liquor and put it into a stirring crystallization kettle to cool down Carry out secondary crystallization at -20°C--10°C, and separate 281.6 kg of crude crystals and 245.2 kg of secondary crystallization mother liquor with a content of 30.5%; kg of organic solvent, gradually cool down to the end temperature of -15°C-10°C in 0.5-30 ho...
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