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Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole

A technology of mercaptobenzothiazole and vulcanization accelerator, applied in organic chemistry and other directions, can solve the problems of large solvent consumption, complex process, low yield and the like, and achieve the effects of high yield, simple process operation and simple process

Inactive Publication Date: 2012-04-11
CHINA PETROCHEMICAL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this patent reduces the amount of waste water, it requires multiple intermittent extraction operations, the process is complicated, the yield is low, and the solvent consumption is large

Method used

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  • Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole
  • Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] as attached figure 1 As shown, through the closed screw feeding device 1, the vulcanization accelerator with a content of about 90% is continuously added from the top of the continuous extraction tower 3 at a rate of 50-100 kg / hour, and at the same time from the extraction agent feeding port 5 at the bottom of the extraction tower 3 Continuously add the extraction agent toluene with a pump at a speed of 80-170kg / hour, the toluene is heated to 50-160°C by the preheater, the extraction pressure is 0.5MPa, and the continuous stirring device 4 of the extraction tower 3 is started to carry out countercurrent extraction operation. The final vulcanization accelerator M relies on gravity to pass through the outlet 6 at the bottom of the extraction tower 3 and enter the centrifuge through the outlet pipe for centrifugal separation and drying. The extraction solvent is continuously added to the solvent from the extraction agent overflow port 2 at the top of the extraction tower 3...

Embodiment 2

[0022] as attached figure 1 As shown, through the closed screw feeding device 1, the vulcanization accelerator M with a content of about 90% is continuously added from the top of the continuous extraction tower 3 at a rate of 50-100 kg / hour, and at the same time, it is fed from the extraction agent feeding port at the bottom of the extraction tower 3 5. Continuously add the extractant xylene with a pump at a rate of 80-170kg / hour. The xylene is heated to 20-180°C by the preheater, and the extraction pressure is 0.55MPa. Start the continuous stirring device 4 of the extraction tower 3 for countercurrent extraction. Operation, the vulcanization accelerator M after extraction relies on gravity to enter the centrifuge through the discharge port 6 at the bottom of the extraction tower 3 through the outlet pipe for centrifugal separation and drying, and the extraction solvent passes through the overflow pipe from the extraction agent overflow port 2 at the top of the extraction towe...

Embodiment 3

[0024] as attached figure 1 As shown, through the closed screw feeding device 1, the vulcanization accelerator M with a content of about 90% is continuously added from the top of the continuous extraction tower 3 at a rate of 50-100 kg / hour, and at the same time, it is fed from the extraction agent feeding port at the bottom of the extraction tower 3 5 Continuously add the extractant ethanol with a pump at a speed of 80-170kg / hour, the ethanol is heated to 20-180°C through the preheater, the extraction pressure is 0.6MPa, and the continuous stirring device 4 of the extraction tower 3 is started to carry out countercurrent extraction operation, The extracted vulcanization accelerator M relies on gravity to pass through the discharge port 6 at the bottom of the extraction tower 3 and enters the centrifuge through the outlet pipe for centrifugal separation and drying. The extraction solvent is continuously added from the extraction agent overflow port 2 at the top of the extracti...

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Abstract

The invention belongs to the technical field of fine chemistry, and relates to a method for purifying a vulcanization accelerator 2-mercaptobenzothiazole (M). In the method, organic arenes, alcohols, carbon disulfide or phenylamine is used as a solvent; and a continuous solvent extraction and solvent distillation recycling device is adopted at an extraction temperature of 20-180 DEG C and an extraction pressure of 0-0.8 MPa to remove tar and byproducts in accelerant M, and the solvent is continuously recycled at the same time. By adopting the method provided by the invention, the consumption of the solvent is reduced, the purifying yield of the accelerant M is improved, and the production of technical waste water is avoided.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a continuous purification method of a vulcanization accelerator 2-mercaptobenzothiazole. Background technique [0002] The vulcanization accelerator 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 the parent material of most sulfenamide accelerators, and an indispensable intermediate for the production of thiazole vulcanization accelerators. [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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
Inventor 付春韦志强孙阿沁高留冕史乐萌
Owner CHINA PETROCHEMICAL CORP
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