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2-mercaptobenzothiazole refining method

A technology of mercaptobenzothiazole and purification method, applied in the direction of organic chemistry and the like, can solve the problems of low purity of 2-mercaptobenzothiazole, large amount of organic solvent, large amount of waste water, etc., and achieves easy industrial production, low environmental pollution, small effect

Inactive Publication Date: 2015-11-18
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of large amount of organic solvent, large amount of waste water, serious environmental pollution and low purity of 2-mercaptobenzothiazole in the refining process of prior art accelerator 2-mercaptobenzothiazole, the invention provides 2-mercaptobenzothiazole Refining method of thiazole

Method used

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  • 2-mercaptobenzothiazole refining method

Examples

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Effect test

Embodiment 1

[0029] Weigh 9g of crude 2-mercaptobenzothiazole, crush it, and put it into a 250ml three-neck flask. Put the three-necked flask into a 70°C constant temperature oil bath, and install a reflux device. Weigh 42g of toluene and 21g of acetone, pour them into a three-necked flask, start stirring, the stirring rate is 120r / min, and the stirring time is 10min. The crude 2-mercaptobenzothiazole is completely dissolved in the mixed solvent of toluene and acetone, and is filtered by hot suction. Suction filtered solution and ash. Dry the ash, transfer the filtered solution to a small beaker, and then transfer it to a three-neck flask, install a distillation device, raise the temperature to 85°C, and continue stirring at a stirring rate of 120r / min. When the distillate volume reaches 1 / 6 of the composite solvent volume , the distilled solution is turbid, stop the distillation, pour out the distilled solution, stir and cool the solution to room temperature, 2-mercaptobenzothiazole is p...

Embodiment 2

[0031]Weigh 9g of crude 2-mercaptobenzothiazole, crush it, and put it into a 250ml three-neck flask. Put the three-necked flask into a 50°C constant temperature oil bath, and install a reflux device. Take by weighing 54g toluene, 27g isopropanol, pour into a three-necked flask, start heating and reflux, the stirring rate is 80r / min, and the stirring time is 10min, the thick 2-mercaptobenzothiazole is completely dissolved in the mixed solvent of toluene and acetone, heat Suction filtration to obtain suction filtration solution and ash. Dry the ash, transfer the filtered solution to a small beaker, and then transfer it to a three-necked flask, install a distillation device, raise the temperature to 60°C, and continue stirring at a stirring rate of 170r / min. When the distillate volume reaches 1 / 6 of the composite solvent volume , the distilled solution is turbid, stop the distillation, pour out the distilled solution, stir and cool the solution to room temperature, 2-mercaptoben...

Embodiment 3

[0033] Weigh 90g of crude M, crush it, and put it into a 1000ml three-neck flask. Put the three-necked flask into a 90°C constant temperature oil bath, and install a reflux device. Weigh 270g of toluene and 90g of isopropanol, pour them into a three-necked flask, start heating and reflux, the stirring rate is 170r / min, and the stirring time is 100min. Filter solution and ash. Dry the ash, transfer the filtered solution to a small beaker, and then transfer it to a three-necked flask, install a distillation device, raise the temperature to 100°C, and continue stirring at a stirring rate of 80r / min. When the distillate volume reaches 1 / 6 of the composite solvent volume , the distilled solution is turbid, stop the distillation, pour out the distilled solution, stir and cool the solution to room temperature, 2-mercaptobenzothiazole is precipitated, and the filter cake and filtrate are obtained by suction filtration, and the color of the filter cake is yellow. Move the filter cake...

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Abstract

The invention belongs to the field of organic chemistry refining and discloses a 2-mercaptobenzothiazole refining method. The 2-mercaptobenzothiazole refining method comprises that under action of a composite solvent comprising toluene and isopropanol or comprising toluene and acetone, 2-mercaptobenzothiazole is subjected to recrystallization purification so that a 2-mercaptobenzothiazole refined product is obtained. The 2-mercaptobenzothiazole refining method has the advantages of simple and convenient processes, small organic solvent use amount, small environmental pollution and industrialization easiness.

Description

technical field [0001] The invention relates to the field of organic chemical purification, in particular to a method for refining 2-mercaptobenzothiazole. Background technique [0002] 2-Mercaptobenzothiazole is also known as rubber vulcanization accelerator M, and its molecular formula is C 7 h 5 NS 2 , the main purpose is to be used as a rubber vulcanization accelerator, analytical reagent and pharmaceutical intermediate, and can also be used to prepare pesticide fungicides, nitrogen fertilizer synergists, etc. In the next few years, with the rapid development of the global rubber industry, the demand for rubber vulcanization accelerator M and downstream products will increase year by year in both international and domestic markets, so the rubber additive product M will have broad market prospects in the future. [0003] At present, the synthetic techniques of rubber vulcanization accelerator M include aniline method, nitrobenzene method, ortho-nitrochlorobenzene metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
CPCC07D277/72
Inventor 张恒李素香岳保泰殷树梅
Owner QINGDAO UNIV OF SCI & TECH
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