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Preparation method for prepared 2-thiol benzothiazole

A benzothiazole and thiol-based technology, applied in the field of vulcanization accelerator 2-thiol-based benzothiazole and its preparation, can solve the problems of no economical practical value, no industrialization value, harsh equipment requirements, etc., to avoid decomposition and coking, the reduction of reaction temperature and pressure, and the reduction of process equipment requirements

Inactive Publication Date: 2015-05-20
BAOYUE TIANJIN ENVIRONMENTAL PROTECTION ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method completely uses aniline as raw material, and the amount of catalyst is as high as 5%. It also has the defect of high reaction pressure, has no economic and practical value, has strict requirements on equipment, and has no industrial value.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 500kg of aniline, 80kg of nitrobenzene, 520kg of carbon disulfide and 120kg of sulfur into the autoclave, start stirring, and after mixing for 10 minutes, add 100 grams of tin tetrachloride, and then keep stirring for 10 minutes, replace the air in the kettle with nitrogen, and stir Heat the material to 150°C, keep it at this temperature for 1 hour, then quickly raise the temperature to 200°C within 20 minutes, turn off the heating device, and use the heat of the reaction to naturally raise the temperature of the reactant to 220°C. At this time, the pressure of the reaction is 4.5MPa, after maintaining at this temperature and pressure for 3 hours, lower the temperature to 180°C, remove hydrogen sulfide, discharge, sample analysis, the content of crude M is 93.5%, and the yield is 95%.

Embodiment 2

[0034] Operating conditions are the same as in Example 1, but using 100 grams of ferric chloride instead of tin tetrachloride, the content of crude product M is 92.6%, and the yield is 93.5%.

Embodiment 3

[0036] The operating conditions are the same as in Example 1, but using 100 grams of copper oxide instead of tin tetrachloride, the content of the crude product M is 94.6%, and the yield is 94.5%.

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PUM

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Abstract

The invention discloses 2-thiol benzothiazole which is prepared from the following components in parts by mass: 4 to 6 parts of aniline, 0.8 to 1.2 parts of nitrobenzene, 4 to 7 parts of sulphur, 0.8 to 3 parts of carbon disulfide and 0.00004 to 0.006 part of catalyst. The invention further discloses a preparation method of the 2-thiol benzothiazole. According to the method, the partial nitrobenzene is taken as a reaction raw material instead of the aniline; sulfuretted hydrogen as a byproduct in a reaction process is fully utilized, so that the nitrobenzene is reduced into the aniline and the sulphur to continuously participate into the reaction. Thus, the pressure of a reaction system and the consumption of the aniline and the sulphur as raw materials are decreased. Due to the adoption of the efficient catalyst, the reaction speed is accelerated while the reaction temperature is decreased at the same time. Thus, the 2-thiol benzothiazole is prevented from being decomposed and coked at a high temperature. Therefore, the yield and the quality of the 2-thiol benzothiazole are improved. The reaction temperature and the reaction pressure are decreased, so that the requirement to process equipment is lowered. As a result, the equipment investment is reduced.

Description

technical field [0001] The invention relates to the field of fine chemicals, and relates to a low-cost, energy-saving and high-efficiency vulcanization accelerator 2-mercaptobenzothiazole and a preparation method thereof. Background technique [0002] 2-Mercaptobenzothiazole (hereinafter referred to as Accelerator M) is a general-purpose rubber vulcanization accelerator and a semi-overspeed accelerator, which can be used alone or in combination. It is not only an important vulcanization accelerator in the rubber industry, but also an indispensable intermediate for the production of thiazole vulcanization accelerators and drugs. [0003] At present, the synthesis process of accelerator M is mature. The production mainly adopts the high-pressure method of reacting aniline with carbon disulfide and sulfur. The crude product M is first produced, and then refined by solvent or acid and alkali to obtain a purity of 97%, and a melting point above 170°C. The product. Due to the la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/72
Inventor 邢维宝兰荣民洪学斌李兵兵
Owner BAOYUE TIANJIN ENVIRONMENTAL PROTECTION ENG