Method for preparing tetraalkyl thiuram disulfide through photocatalytic oxidation

[0046]Example 1

[0047]Add 7.39g of diethylamine, 90mL of absolute ethanol, and 0.052g of hematoxylin into a 250ml beaker with a lid. Turn on the stirring, control the temperature to 20-30°C, slowly add 7.81g of carbon disulfide, about 1min to complete the addition, stir and react for 5min. Turn on the 12W LED blue light source, the light source is located in the center of the liquid surface, 5cm above the liquid surface, open the Sensen ct-201 air pump (with bubble disk) to inject air into the reaction liquid, light the reaction for 2 minutes, stop the ventilation reaction and end. The ethanol was distilled off under reduced pressure and dried to obtain 14.68 g of white tetraethylthiuram disulfide crystals with a yield of 98.99% and a purity of 99.95% by liquid chromatography.

[0048]Example 2

[0049]Add 36.95g of diethylamine, 0.259g of hematoxylin, and 250ml of absolute ethanol into a 500mL beaker with a lid. Turn on the stirring, control the temperature to 20-30°C, slowly add 39.05g of carbon disulfide, about 30 minutes to complete the addition, and stir for 10 minutes. Turn on the 12wLED blue light source, the light source is located in the center of the liquid surface, 5cm above the liquid surface, open the Sensen ct-201 air pump (with bubble disk) to inject air into the reaction solution to illuminate the reaction for 10 minutes, stop the ventilation reaction and end. The mother liquor was filtered and collected, and dried to obtain 63.80 g of white tetraethylthiuram disulfide crystals. The yield was 86.04%, and the purity detected by liquid chromatography was 99.99%.

[0050]Example 3

[0051]36.95 g of diethylamine and the mother liquor collected in Example 2 were added to a 500 mL beaker with a lid. Turn on the stirring, slowly add 39.05g of carbon disulfide at 20-30°C for about 30 minutes, and then stir for 10 minutes. Turn on the 12wLED blue light source, the light source is located in the center of the liquid level, 5cm above the liquid level, open the Sensen ct-201 air pump (with bubble disk) to inject air into the reaction liquid to illuminate the reaction for 10 minutes, stop the ventilation reaction and end. The mother liquor was filtered and collected, and dried to obtain 74.21 g of white tetraethylthiuram disulfide crystals. The yield was 100.07%, and the purity by liquid chromatography was 99.98%.

[0052]After the mother liquor is rectified to recover ethanol, 10.26 g of white crystal tetraethylthiuram disulfide is obtained, and the purity is 99.95% by liquid chromatography. Based on the product quality obtained in Example 2, the yield in Example 2 is 99.87%.