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The preparation method of tetraethylthiuram disulfide

A technology of tetraethylthiuram disulfide and carbon disulfide, applied in the field of rubber additives, can solve the problems of environmental pollution, complicated process, low yield and the like, and achieve the effects of reducing production cost, simple and convenient process operation, and uniform composition

Active Publication Date: 2020-01-24
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of preparation method of tetraethylthiuram disulfide, to alleviate the complicated process when producing tetraethylthiuram disulfide in the prior art, energy consumption is big, three wastes are high, serious environmental pollution and Technical problem with low yield

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  • The preparation method of tetraethylthiuram disulfide
  • The preparation method of tetraethylthiuram disulfide
  • The preparation method of tetraethylthiuram disulfide

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preparation example Construction

[0049] In one embodiment of the present invention, the preparation method comprises the following steps:

[0050] Step a): Adding carbon disulfide to a solution containing a bimetallic catalyst and diethylamine by means of dropwise addition to react carbon disulfide and diethylamine to obtain a first solution;

[0051] Step b): adding hydrogen peroxide dropwise to the obtained first solution for reaction, and obtaining the tetraethylthiuram disulfide after the reaction is completed.

[0052] The separate operation of the dropwise addition of carbon disulfide and hydrogen peroxide can promote the reaction to proceed more fully, better control the temperature during the operation, further improve the reaction efficiency, and increase the product conversion rate.

[0053] In one embodiment of the present invention, in step a), the reaction temperature is 15-25°C, the carbon disulfide addition time is 1.0-1.5h, and the reaction is continued for 0.5-1.0h after the addition;

[005...

Embodiment 1

[0072] The present embodiment is a kind of preparation method of tetraethylthiuram disulfide, comprising the following steps:

[0073] Under normal pressure conditions, 270g n-butanol and 0.09g Pd-Mn-Al 2 o 3 Add it into a 1000ml four-necked bottle for stirring and mixing, then add 60g of diethylamine, control the temperature at 12°C, and start to add 60g of carbon disulfide dropwise. During the dropping process, the temperature is controlled at 12°C, and the dropping time is 40min; React at 12°C for 20 minutes; raise the temperature to 22°C, start adding 48g of hydrogen peroxide dropwise, control the dropping rate so that the reaction temperature is 22°C, and the dropping time is 1.5h; then keep warm for 20 minutes; after the keep warm, start filtering, washing and drying Dried and packaged.

Embodiment 2

[0075] The present embodiment is a kind of preparation method of tetraethylthiuram disulfide, comprising the following steps:

[0076] Under normal pressure conditions, 480g n-butanol and 0.36g Pd-Mn-Al 2 o 3 Add it into a 1000ml four-necked bottle for stirring and mixing, then add 60g of diethylamine, control the temperature at 28°C, and start to add 78g of carbon disulfide dropwise. During the dropping process, the temperature is controlled at 28°C, and the dropping time is 40min; React at 28°C for 20 minutes; raise the temperature to 35°C, start adding 75g of hydrogen peroxide dropwise, control the dropping speed so that the reaction temperature is 35°C, and the dropping time is 1.5h; then keep warm for 20 minutes; after the keep warm, start filtering, washing and drying Dried and packaged.

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Abstract

The present invention relates to the field of rubber additives, specifically, it provides a preparation method of tetraethylthiuram disulfide, the reaction raw materials diethylamine, carbon disulfide and hydrogen peroxide are reacted under the action of a bimetallic catalyst to obtain the Tetraethylthiuram disulfide. The above method uses a bimetallic catalyst to promote efficient and continuous reaction, increase the conversion rate of raw materials, make condensation reaction and oxidation reaction easier to carry out, thereby increasing the yield of products. The method is simple and convenient to operate, can greatly increase the yield of products, reduce production costs, there is no "three wastes" discharge during the preparation process, the mother liquor can be reused, and there is no pollution to the environment. At the same time, the prepared products have stable quality and high purity. , the composition is uniform, and this method can be applied in large-scale production practice.

Description

technical field [0001] The invention relates to the field of rubber additives, in particular to a preparation method of tetraethylthiuram disulfide. Background technique [0002] my country's rubber industry has entered the fast track, and the synthetic rubber industry has formed a relatively complete industrial system. The synthetic rubber industry will enter a period of faster development, and the amount of rubber vulcanization accelerators will also increase sharply. [0003] Vulcanization accelerators, which can be referred to as accelerators, are used to speed up the vulcanization speed, shorten the vulcanization time, reduce the vulcanization temperature, reduce the amount of vulcanization agent during rubber vulcanization, and at the same time improve the physical and mechanical properties of vulcanized rubber. Tetraethylthiuram disulfide (TETD) is a super accelerator and vulcanizing agent for natural rubber, styrene-butadiene rubber, nitrile rubber, butyl rubber, but...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/32
CPCC07C333/32
Inventor 张振飞倪京华徐治松郭同新马胜峰王志强宋风朝王飞李宏喜
Owner WILLING NEW MATERIALS TECH CO LTD
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