Method for producing 2,2'-dibenzothiazolyl disulfide by nitric acid one-step method

A technology of dibenzothiazole disulfide and dimercaptobenzothiazole, which is applied in the field of one-step production of dibenzothiazole disulfide with nitric acid, can solve the problems of needing refining, low melting point of DM, and high cost, so as to improve product purity and improve The melting point of the product and the effect of reducing impurities

Inactive Publication Date: 2010-12-29
刘方政
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AI Technical Summary

Problems solved by technology

Its disadvantages are: 1) the obtained DM has a low melting point and cannot be applied to the production of new cephalosporins requiring high purity of DM; 2) DM needs to be refined and the cost is high

Method used

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Embodiment Construction

[0023] A kind of nitric acid one-step method produces the method for dibenzothiazole disulfide, comprises the steps:

[0024] 1) Dissolution: measured softened water 1-1.5M 3 Enter the dissolution tank, start the stirring device, add 75Kg of caustic soda or 230-245Kg of liquid caustic soda to heat, then add 300-400Kg of dimercaptobenzothiazole, 40-60Kg of activated carbon and continue stirring. After stirring for 30 minutes, suction filtration, after suction filtration, pass through PE The filter rod equipment circulates the filter press, and the sampling is qualified and sent to the acidification station; the filter press temperature is 65-90°C.

[0025] 2) Acidification: use 30% nitric acid 200-400kg with 1-2M 3 Demineralized water, prepare 8-12% dilute nitric acid, pour it into the dilute acid metering tank, wait for the dissolving post to pour the material into the acidification kettle, heat up while stirring, start acidification dripping time between 60 minutes and 90 mi...

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Abstract

The invention relates to a thiazole type vulcanization accelerator, in particular to a method for producing 2,2'-dibenzothiazolyl disulfide by the nitric acid one-step method, which sequentially comprises the steps of dissolution of 2-mercaptobenzothiazole, acidification and oxidation, and is characterized in that 1) the dissolution is as follows: dissolving the 2-mercaptobenzothiazole into excess NaOH solution, adding activated carbon, carrying out pressure filtration at 65-90 DEG C and obtaining filtrate; 2) the acidification is as follows: adopting 8-12% of dilute nitric acid to regulate the pH of the filtrate in the step 1) to 6-7, and carrying out centrifugation after the acidification for obtaining sodium 2-mercaptobenzothiazole; and 3) the oxidation is as follows: oxidizing the sodium 2-mercaptobenzothiazole into the 2,2'-dibenzothiazolyl disulfide, wherein an oxidant is mixture of excess hydrogen peroxide and isopropyl alcohol, the oxidation temperature is 25-50 DEG C, and the oxidation time is 90-100min. Compared with the prior art, the method is applicable to large industrial production, and the prepared DM has high melting point (above 180 DEG C) and good purity.

Description

technical field [0001] The invention relates to a thiazole-type vulcanization accelerator, in particular to a method for producing dibenzothiazole disulfide in one step with nitric acid. Background technique [0002] Dibenzothiazole disulfide (hereinafter referred to as "DM") is an excellent rubber vulcanization accelerator, which is used in a large amount in the rubber industry. Essential raw materials, and active esters are intermediates for the production of cephalosporin antibiotics, which are widely used at home and abroad. [0003] The refined DM produced by the traditional process is only suitable for the production of AE active ester, which is used as an intermediate of cephalosporin antibiotics and is a raw material for the production of ceftriaxone, cefotaxime sodium and other pharmaceuticals. With the development of the pharmaceutical industry, a large number of new cephalosporin antibiotics such as ceftazidime and cefdinir have emerged. The production of active...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
Inventor 刘方政刘江涛王宝庆李金生
Owner 刘方政
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