The preparation method of tellurium diethyldithiocarbamate
A technology of diethyldithiocarbamic acid and diethylamine, which is applied in the field of rubber vulcanization accelerator preparation, can solve problems such as inconvenient operation, difficult environmental management, low product yield, etc., to achieve improved product yield, The effect of reducing production costs and shortening the production cycle
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preparation example Construction
[0013] The preparation method of tellurium diethyldithiocarbamate according to the present invention comprises the steps of: adding diethylamine into a reaction kettle filled with pure water; then adding tellurium oxide, and after the tellurium oxide is dissolved and saturated, adding Carbon disulfide: After the addition of carbon disulfide, continue to stir, and a precipitation reaction occurs. After cooling to room temperature, filter, precipitate, wash and dry to obtain tellurium diethyldithiocarbamate.
[0014] In the preparation method of tellurium diethyldithiocarbamate according to the present invention, preferably, stirring is added during the process of adding diethylamine, and the stirring time is 10-20min, and the total mass of diethylamine and purified water is Calculated, the mass percentage of diethylamine is 10~30%.
[0015] In the preparation method of tellurium diethyldithiocarbamate according to the present invention, preferably, based on the total mass of di...
Embodiment 1
[0022] Add 13.74g of diethylamine into a three-necked flask containing 123.66g of pure water (the mass fraction of diethylamine is 10%) under stirring, and stir for 15min;
[0023] Then add 5g of tellurium oxide powder, after the tellurium oxide is dissolved and saturated, the temperature is controlled at 35°C, and a total of 9.975g of carbon disulfide is added dropwise for 30 minutes, wherein the molar ratio of diethylamine: carbon disulfide: tellurium oxide is =6:4.2:1;
[0024] Continue to stir for 3 hours after the addition of carbon disulfide, and a precipitation reaction occurs. After cooling to room temperature, filter and wash the precipitate, vacuum-dry at 80°C, and then crush and sieve to obtain a sample of 21.7572g; the tellurium content is 17.68%. The initial melting point is 111.4~112.6, and the product yield is 96.2%.
Embodiment 2
[0026] Add 13.74g of diethylamine into a three-necked flask containing 54.96g of pure water under stirring (the mass fraction of diethylamine is 20%), and stir for 10min;
[0027] Then add 5g of tellurium oxide powder, after the tellurium oxide is dissolved and saturated, the temperature is controlled at 20°C, and a total of 9.5g of carbon disulfide is added dropwise for 25 minutes, wherein the molar ratio of diethylamine: carbon disulfide: tellurium oxide is =6:4:1;
[0028] Continue to stir for 2 hours after the carbon disulfide is added dropwise, and a precipitation reaction occurs. After cooling to room temperature, it is filtered, the precipitate is washed, dried in vacuum at 70°C, and then crushed and sieved to obtain a sample of 21.6926g; the tellurium content is 17.75%. The initial melting point is 111.4~112.8, and the product yield is 96.3%.
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