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Clean synthesis process for synthesizing vulcanization accelerators CBBS by using 2-mercaptobenzothiazole and cyclohexane as raw materials

A technology of vulcanization accelerator and benzothiazole, which is applied in the field of vulcanization accelerator synthesis, can solve the problems of waste of raw materials, high cost of raw materials, and difficulty in treating process wastewater, and achieves the effects of cost reduction, easy treatment, and easy industrialization and promotion.

Inactive Publication Date: 2018-11-02
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this route has successfully obtained the target product CBBS, the reaction route uses CBS and acid anhydride as raw materials, and the cost of raw materials is relatively high
At the same time, according to industry common sense, the raw material accelerator CBS in this synthesis route is synthesized using 2-mercaptobenzothiazole and cyclohexylamine as raw materials. According to the examples of the patent CN 106699686 A, it can be seen that the maximum yield of the product calculated by CBS is only 94.3%. Under comprehensive conversion, the overall yield of the route for synthesizing CBBS with 2-mercaptobenzothiazole and cyclohexylamine is about 85%. The waste of raw materials is serious, and the production cost of CBBS is extremely high; in addition, during the process, a large amount of process wastewater that is difficult to treat will be generated, which is very easy to pollute the environment during the industrialization process, and also affects the large-scale industry of this product. promotion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] A kind of clean synthesis technique that takes 2-thiol benzothiazole and cyclohexylamine as raw material synthesis vulcanization accelerator CBBS, the steps that comprise have:

[0061] (1) Generation of intermediate products:

[0062] Mix cyclohexylamine and 30% industrial hydrochloric acid, add hydrogen peroxide dropwise while stirring, after the dropwise addition is completed, let it stand still, when the reaction is completed, the upper layer is the intermediate product, the lower layer is water, and the water is separated to obtain the intermediate product;

[0063] The mol ratio of cyclohexylamine and hydrochloric acid is controlled at 1:2.5;

[0064] The molar ratio of cyclohexylamine to hydrogen peroxide is controlled at 1:2.8;

[0065] The reaction temperature is controlled at 50°C;

[0066] The hydrogen peroxide dripping time is controlled at 1.5h;

[0067] After the dropwise addition, the standing time was controlled at 1h.

[0068] (2) Generation of M-Na s...

Embodiment 2

[0080] A kind of clean synthesis technique that takes 2-thiol benzothiazole and cyclohexylamine as raw material synthesis vulcanization accelerator CBBS, the steps that comprise have:

[0081] (1) Generation of intermediate products:

[0082] Mix cyclohexylamine and 30% industrial hydrochloric acid, add hydrogen peroxide dropwise while stirring, after the dropwise addition is completed, let it stand still, when the reaction is completed, the upper layer is the intermediate product, the lower layer is water, and the water is separated to obtain the intermediate product;

[0083] The mol ratio of cyclohexylamine and hydrochloric acid is controlled at 1:4;

[0084] The molar ratio of cyclohexylamine to hydrogen peroxide is controlled at 1:4;

[0085] The reaction temperature is controlled at 80°C;

[0086] The hydrogen peroxide dripping time is controlled within 3 hours;

[0087] The standing time after the dropwise addition is completed is controlled at 2h;

[0088] (2) Gene...

Embodiment 3

[0100] A kind of clean synthesis technique that takes 2-thiol benzothiazole and cyclohexylamine as raw material synthesis vulcanization accelerator CBBS, the steps that comprise have:

[0101] (1) Generation of intermediate products:

[0102] Mix cyclohexylamine and 30% industrial hydrochloric acid, add hydrogen peroxide dropwise while stirring, after the dropwise addition is completed, let it stand still, when the reaction is completed, the upper layer is the intermediate product, the lower layer is water, and the water is separated to obtain the intermediate product;

[0103] The mol ratio of cyclohexylamine and hydrochloric acid is controlled at 1:2;

[0104] The molar ratio of cyclohexylamine to hydrogen peroxide is controlled at 1:2;

[0105] The reaction temperature is controlled at 30°C;

[0106] The hydrogen peroxide dripping time is controlled at 0.5h;

[0107] After the dropwise addition, the standing time is controlled at 0.5h;

[0108] (2) Generation of M-Na sa...

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PUM

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Abstract

The invention relates to a clean synthesis process for synthesizing vulcanization accelerators CBBS by using 2-mercaptobenzothiazole and cyclohexane as raw materials. The process comprises the following steps of (1) generating intermediate products; (2) generating an M-Na salt solution; (3) synthesizing CBBS. Compared with the synthesis process in the prior art, the clean synthesis process for synthesizing vulcanization accelerators CBBS by using 2-mercaptobenzothiazole and cyclohexane as raw materials has the advantages that the cost is reduced; the whole yield is as high as 90 percent or higher; the purity of the product CBBS can reach 96 percent through HPLC test; less waste water is generated in the synthesis; the waste water can be easily treated; in the industrialization process, theinfluence on the environment is small; the large-scale industrialized popularization is easy.

Description

technical field [0001] The invention relates to the field of synthesis of vulcanization accelerators, in particular to a clean synthesis process for synthesizing vulcanization accelerator CBBS by using 2-mercaptobenzothiazole and cyclohexylamine as raw materials. Background technique [0002] In modern society, rubber has been widely used, such as tires of automobiles and airplanes, various wires and cable outer sheaths in daily life, rubber shoe soles, rubber tubes, etc. must use natural rubber or synthetic rubber. In order to increase the processing performance and weather resistance of rubber products, it is necessary to add appropriate rubber additives, such as rubber vulcanizing agents, vulcanization accelerators, rubber antioxidants, etc. [0003] Common varieties of vulcanization accelerators include NOBS, DCBS and CBS. However, in use, NOBS and DCBS can produce serious carcinogen nitrosamines after being heated, so their use has been banned in European and American ...

Claims

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Application Information

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IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 孟庆森
Owner KEMAI CHEM
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