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Preparation method of thiofide DPTT-6

A DPTT-6, rubber vulcanization technology, applied in the direction of organic chemistry, can solve the problems of high environmental protection pressure, no water, difficult reaction, etc., and achieve the effect of zero pollution emission, high product yield and simple process

Inactive Publication Date: 2018-06-12
WILLING NEW MATERIALS TECH CO LTD
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Problems solved by technology

Reaction is difficult to carry out, can not realize better production state; CN200810183220.7 introduces a kind of preparation method of rubber vulcanization accelerator bispentamethylene thiuram tetrasulfide, wherein said method is solvent with water, used raw material and Its molar ratio is: hexahydropyridine: carbon disulfide: sulfur: hydrogen peroxide = 1: 1-1.3: 1.8-2.5: 0.4-0.7. Add hexahydropyridine and sulfur in sequence to the reaction kettle. After the addition, control the temperature within the range of 20-30°C, then add carbon disulfide liquid dropwise, and control the dropping time for 2-3 hours. After the dropwise addition, measure the pH of the reaction solution value, after the pH value of the reaction solution is stabilized in the range of 6.5-7.5, control the temperature of the reaction solution at 30°C-40°C, and start to add hydrogen peroxide dropwise to carry out the oxidation reaction. The oxidation reaction time is 3-4 hours. After the reaction is over, keep warm for another 1 hour, and then perform solid-liquid separation to obtain the product
However, since the reaction uses water as a solvent, the waste water is difficult to treat, which brings great pressure on environmental protection
[0006] Therefore, research and develop a kind of process simple, product yield height, high purity, simultaneously, reaction solvent does not contain water and recyclable bispentamethylene thiuram hexasulfide (DPTT-6) preparation method, to alleviate existing technology The production process of DPTT-6 in China has high energy consumption and produces a large amount of waste water, which brings great difficulties to environmental protection and becomes very necessary and urgent

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  • Preparation method of thiofide DPTT-6
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preparation example Construction

[0032] According to one aspect of the present invention, a kind of preparation method of rubber vulcanization accelerator DPTT-6, described preparation method comprises the following steps: join sulfur, hexahydropyridine and surfactant in low carbon alcohol solvent and mix, subsequently, Add carbon disulfide and hydrogen peroxide dropwise and react at elevated temperature to obtain rubber vulcanization accelerator DPTT-6.

[0033] The preparation method of the rubber vulcanization accelerator DPTT-6 of the present invention is to add sulfur, hexahydropyridine and surfactant into a low-carbon alcohol solvent and mix evenly, then, add carbon disulfide and hydrogen peroxide dropwise in sequence and react at elevated temperature to prepare the rubber vulcanization accelerator DPTT-6. The above preparation method adopts low-carbon alcohol which is low-toxic, cheap, easy to recycle and apply mechanically as a solvent, and synthesizes dipentamethylenethiuram hexasulfide (DPTT-6) thro...

Embodiment 1

[0059] A kind of preparation method of rubber vulcanization accelerator DPTT-6, described preparation method comprises the following steps:

[0060] First, under normal pressure, add 250ml of ethanol and 14.0g of sulfur into a 1000ml four-neck flask for stirring and mixing for 30 minutes; then add 19.6g of hexahydropyridine and 0.98g of trimethyloctadecylammonium chloride , control the temperature at 18°C, start to add 17.87g of carbon disulfide dropwise, control the temperature at 18°C ​​during the dropping process, and add the time for 1.5h; after the dropwise addition, control the temperature at 18°C ​​for 1.0h;

[0061] Subsequently, the temperature was raised to 22°C, and a mixed solution of 17.07g of hydrogen peroxide and 108.17ml of ethanol was added dropwise, and the rate of addition was controlled so that the reaction temperature was 22°C, and the dropping time was 3.5h; then, the reaction was kept for 0.5h;

[0062] Finally, the temperature of the obtained reaction s...

Embodiment 2

[0068] A kind of preparation method of rubber vulcanization accelerator DPTT-6, described preparation method comprises the following steps:

[0069] First, under normal pressure, add 250ml of ethanol and 14.0g of sulfur into a 1000ml four-neck flask for stirring and mixing for 30 minutes; then add 22.5g of hexahydropyridine and 0.98g of trimethyloctadecylammonium chloride , control the temperature at 18°C, start to add 19.87g of carbon disulfide dropwise, control the temperature at 18°C ​​during the dropping process, and add the time for 1.5h; after the dropwise addition, control the temperature at 18°C ​​for 1.0h;

[0070] Subsequently, the temperature was raised to 22°C, and a mixed solution of 17.07g of hydrogen peroxide and 108.17ml of ethanol was added dropwise, and the rate of addition was controlled so that the reaction temperature was 22°C, and the dropping time was 3.5h; then, the reaction was kept for 0.5h;

[0071] Finally, the temperature of the obtained reaction s...

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Abstract

The invention provides a preparation method of thiofide DPTT-6, and relates to the technical field of thiofide. The preparation method comprises the steps of adding sulphur, hexahydropyridine and a surface active agent into a low-carbon alcohol solvent, mixing uniformly, then sequentially dropwise adding carbon disulfide and hydrogen peroxide, rising temperature for reaction, and preparing to obtain the thiofide DPTT-6. According to the preparation method, low-carbon alcohol low in toxicity, cheap in price and easy to recover and use indiscriminately is adopted as the solvent, and through theoxidation of the oxidizing agent hydrogen peroxide at lower temperature, dipentamethylenethiuram hexasulfide is synthesized. The preparation method has the advantages of simple process, high product yield and high purity; the prepared product has the product yield being larger than or equal to 97.0 percent, the initial melting point being larger than or equal to 115.0 DEG C, and the purity being larger than or equal to 98.0 percent; meanwhile, during the preparation process, no 'three wastes' (waste water, waste gas and waste solid) is discharged, all solvents are recovered and used indiscriminately, no environment pollution is caused, and zero emission of pollution is realized.

Description

technical field [0001] The invention relates to the technical field of rubber vulcanization accelerators, in particular to a preparation method of rubber vulcanization accelerator DPTT-6. Background technique [0002] At present, the contradiction between the pollution caused by my country's industrial development and the limited capacity of the ecological environment has become a major strategic problem that needs to be solved urgently in the development of my country's social economy. In the future, the development of the rubber additives industry must adhere to the concept of low-carbon economy and green economy, and take the continuous development of clean and low-carbon process routes as the main development model. Only in this way can my country's rubber additives industry be truly enlarged and strengthened. Therefore, the development and application of clean and efficient process technologies for some major varieties has become the key to industrial development. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/21
CPCC07D295/21
Inventor 张振飞韩晓飞徐治松马胜峰王志强宋风朝倪京华王飞李宏喜
Owner WILLING NEW MATERIALS TECH CO LTD
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