Purification process for vulcanization accelerator 2-mercaptobenzothiazole

A technology of mercaptobenzothiazole and vulcanization accelerator, which is applied in the direction of organic chemistry to achieve the effect of shortening the process flow, good effect and ensuring safety

Active Publication Date: 2010-04-14
山东戴瑞克新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The principle of this process is a solid-liquid extraction reaction. The disadvantage is that the crude M particles used in the extraction are obtained through cooling and crushing processes. In addition, only the organic matter and other impurities on the surface of the crude M are separated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Pass nitrogen into the extraction kettle of 1500L to replace the air in the kettle, and then add 800Kg of toluene.

[0026] (2) Pass 400kg of crude vulcanization accelerator M melt into the extraction kettle in 20-40 minutes, and at the same time open the valve of the extraction heat preservation medium on the extraction kettle to keep the temperature of the kettle at 45-48°C. Turn on the stirring, the speed is 110-130r / min.

[0027] (3) Immediately after 1.5 hours of extraction, the mixture in the extraction tank was filtered, and the filter cake obtained after filtration was dried at 70° C. under a pressure of -0.05 MPa for 2 hours to obtain 345 Kg with a purity of 98.1%. Accelerator 2- Mercaptobenzothiazole has a melting point of 172°C. Distill the filtrate to recover toluene. During the extraction process, the volatilized toluene is condensed and refluxed, and the non-condensable gas is recycled by activated carbon adsorption.

Embodiment 2

[0029] (1) Pass nitrogen into the extraction kettle of 1500L to replace the air in the kettle, and then add 800Kg of toluene.

[0030] (2) Pass 160kg of crude vulcanization accelerator M melt into the extraction kettle in 10-15 minutes, and at the same time open the valve of the extraction heat preservation medium to keep the temperature of the kettle at 40-45°C. Turn on the stirring, the speed is about 100-120r / min.

[0031] (3) After 1.5 hours of extraction, the mixture in the extraction tank was filtered. The filter cake obtained after filtration was dried at 70°C for 2 hours under a pressure of -0.05MPa to obtain 137Kg of accelerator 2-mercaptobenzothiazole with a purity of 98.4% and a melting point of 172.5°C. Distill the filtrate to recover toluene. During the extraction process, the volatilized toluene is condensed and refluxed, and the non-condensable gas is recycled by activated carbon adsorption.

Embodiment 3

[0033] (1) Pass nitrogen into the extraction kettle of 1500L to replace the air in the kettle, and then add 800Kg of toluene.

[0034] (2) Pass 100kg of crude vulcanization accelerator M melt into the extraction kettle in 8-10 minutes, and at the same time open the valve of the extraction heat preservation medium to keep the temperature of the kettle at 35-40°C. Turn on the stirring, the speed is about 120-130r / min.

[0035] (3) After 1.5 hours of extraction, the mixture in the extraction tank was filtered. The filter cake obtained after filtration was dried at 70° C. for 2 hours under a pressure of −0.05 MPa to obtain 85 kg of accelerator 2-mercaptobenzothiazole with a purity of 98.5% and a melting point of 172.5° C. Distill the filtrate to recover toluene. During the extraction process, the volatilized toluene is condensed and refluxed, and the non-condensable gas is recycled by activated carbon adsorption.

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Abstract

The invention relates to a purification process for vulcanization accelerator 2-mercaptobenzothiazole, which includes that crude 2-mercaptobenzothiazole molten pulp prepared through high-temperature high-pressure condensation is directly led into an extraction kettle filled with organic solvents after complete replacement with nitrogen in advance; impurities are removed by conducting liquid-liquid extraction reaction; the temperature of the extraction kettle is kept no more than 50 DEG C in the process of extraction; mass ratio of the organic solvents to the crude 2-mercaptobenzothiazole molten pulp is (2-10) : 1; after extraction is finished, mixture inside the extraction kettle is filtered; obtained filter cakes are dried so as to obtain the vulcanization accelerator 2-mercaptobenzothiazole; the organic solvents recycled by distilling obtained filter liquor can be reused; and organic solvents evaporated in the extraction process condensate and flow back, and non-condensable gas is recycled by using active carbon to absorb the non-condensable gas. The purification process has safe extraction, shortens process flow, saves labor, material resources and energy sources, and can obtain high-purity vulcanization accelerator 2-mercaptobenzothiazole.

Description

technical field [0001] The invention relates to a purification process of a vulcanization accelerator 2-mercaptobenzothiazole, which belongs to the field of fine chemicals. Background technique [0002] 2-Mercaptobenzothiazole, trade name Accelerator M, referred to as M, is an important vulcanization accelerator in rubber production, and most of them are synthesized by aniline method at present. The preparation process of the aniline method vulcanization accelerator M is formed by condensation of aniline, sulfur and carbon disulfide under high temperature and high pressure, but the crude product M synthesized by high temperature and high compression contains many impurities, which cannot meet the requirements for use and must undergo subsequent purification. processing can be used. There are currently two purification methods, one is the acid-base method, and the other is the solvent extraction method. [0003] Chinese patent document CN1123277A (95112059.X) discloses a ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72C08K5/47
Inventor 杜孟成王文博魏成磊马德龙许思俊孙庆刚
Owner 山东戴瑞克新材料有限公司
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