Preparation method of tetraalkylthiuram monosulfide

[0026] Put 80.0g of water, 50.0g of ethanol, and 36.4g of carbon disulfide into a four-necked flask with a condenser in turn at room temperature, cool down to 10-15°C, and stir at this temperature for 2.5h; control the temperature to 10-15°C and dropwise add 50.0 g dimethylamine (wt40%) aqueous solution, after the completion, the temperature was slowly raised to 15~20℃ and reacted for 1.5h; 63.8g hydrogen peroxide (wt13%) was added dropwise at a controlled temperature of 15~20℃, and stirred for 2.5h after the dropwise addition was completed; Add 37.2g of sodium cyanide (wt27.5%) aqueous solution dropwise at ~20°C, stir for 1.5h after the dropwise addition, control the temperature to 15~20°C and dropwise add 19.9g of triphenylphosphine (wt17.5%) alcohol solution, dropwise After adding, stir for 3.5h; filter, dry and pulverize to obtain 45.7g of tetramethylthiuram monosulfide, the mother liquor is recovered and separated by-products sodium thiocyanate and triphenylphosphine sulfur;

[0028] Put 80.0g of water, 53.0g of methanol, and 53.4g of carbon disulfide into a four-necked flask with a condenser in turn at room temperature, cool down to 10-15°C, and stir at this temperature for 2.5h; control the temperature to 10-15°C and dropwise add 50.0 g diethylamine solution, slowly heat up to 15~20℃ for 1.5h after completion; add 83.5g hydrogen peroxide (wt 15%) dropwise at a controlled temperature of 15~20℃, stir for 2.5h after the dropwise addition; control the temperature at 15~20℃ Add 56.0g sodium cyanide (wt27.5%) aqueous solution, stir for 1.5h after the dropwise addition; control the temperature to 15~20℃ and add dropwise 50.2g triphenylphosphine (wt17.5%) alcohol solution, stir after the dropwise addition 3.5h; filter, dry and pulverize to obtain 87.3g of tetraethylthiuram monosulfide, the mother liquor was recovered and separated by-products sodium thiocyanate and triphenylphosphine sulfur; the yield of tetramethylthiuram monosulfide was 98.6%, Liquid phase

[0030] Put 80.0g of water, 55.0g of isopropanol and 31.1g of carbon disulfide into a four-necked flask with a condenser in turn at room temperature, cool down to 10-15°C, and stir at this temperature for 2.5h; control the temperature to 10-15°C dropwise Add 50.0g of diisobutylamine solution, slowly heat up to 15~20℃ and react for 1.5h after completion; control the temperature to 15~20℃, add 48.1g hydrogen peroxide (wt15%) dropwise, stir for 2.5h after the dropwise addition; control the temperature to 15~20℃ 49.9g sodium cyanide (wt27.5%) aqueous solution was added dropwise at 20°C, stirred for 1.5h after the dropwise addition; 34.1g triphenylphosphine (wt17.5%) alcohol solution was added dropwise at a temperature of 15-20°C After completion, stir for 3.5h; filter, dry and pulverize to obtain 70.5g of tetraisobutylthiuram monosulfide, the mother liquor is recovered and separated by-products sodium thiocyanate, triphenylphosphine sulfur; tetraisobutylthiuram monosulfide The yield w