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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

Active Publication Date: 2016-03-23
广东先导稀贵金属材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process of this process, there are many synthesis steps, inconvenient operation, a large amount of waste water and a large amount of salt that is difficult to directly biochemically treat in the waste water, which brings great difficulties to environmental governance and does not meet the national environmental protection policy and energy-saving production requirements; and Product yield is low, it is difficult to meet the needs of economic benefits

Method used

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Examples

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Effect test

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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Abstract

The present invention provides a tellurium diethyldithiocarbamate preparation method, which comprises: adding diethylamine to a reaction kettle filled with purified water; adding tellurium oxide, and adding carbon disulfide under temperature control after the tellurium oxide is dissolved and achieves a saturated state; and after completing the carbon disulfide addition, continuously stirring, carrying out a precipitation reaction, cooling to a room temperature, filtering, and washing and drying the precipitate to obtain the tellurium diethyldithiocarbamate. According to the present invention, wastewater emission during the product production process is significantly reduced, the wastewater does not contain salt, and the environmental pollution is low; the one-step method is adopted to synthesize the product so as to eliminate the synthesis process of the intermediate and significantly shorten the production cycle; the safety factor of the production process is increased to a certain extent; and the product yield is increased, and the production cost is reduced.

Description

technical field [0001] The invention relates to a method for preparing a rubber vulcanization accelerator, in particular to a method for preparing tellurium diethyldithiocarbamate. Background technique [0002] Adding an accelerator to the rubber can greatly promote the reaction between the rubber and the vulcanizing agent, increase the vulcanization speed, lower the vulcanization temperature, and reduce the amount of vulcanizing agent. Tellurium diethyldithiocarbamate, referred to as TDEC, belongs to dithiocarbamate rapid vulcanization accelerator, is a super-accelerator with particularly high activity, often used in rapid vulcanization and low temperature vulcanization products, and can be directly added to rubber medium without causing scorching. For example, when used in natural rubber, EPDM rubber, butyl rubber and styrene-butadiene rubber, it can not only improve the vulcanization efficiency, reduce energy consumption, but also improve the foaming uniformity and mecha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/16
Inventor 李长龙吕铁铮童培云高远
Owner 广东先导稀贵金属材料有限公司
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