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Improve method for preparing N-tert-butylbenzothiazolesulfenamide

A technology of thiazole sulfenamide and benzothiazole, applied in the direction of organic chemistry, etc., to achieve the effect of stabilizing methanol insolubles

Inactive Publication Date: 2011-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention aims at the shortcomings of the above synthetic methods, and proposes a synthetic process of TBBS, which can effectively solve the problems existing in the existing synthetic methods, stabilize the product yield above 96%, and have a melting point of 105°C

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250ml four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 80ml of water, 0.1g of nonionic surfactant Nongru 600#, start stirring, and add 17g (0.1mol) of gram promoter in batches at room temperature. Add agent M, stir for half an hour after adding tert-butylamine, then add 12 grams (0.15mol) of tert-butylamine, the addition temperature is controlled at 30-35°C, and the addition time is 20-30 minutes. After adding tert-butylamine, maintain at 30-35°C for 2 hours After completion, add 60 ml of 10% sodium hypochlorite at 35-40°C within 1-4 hours, heat up to 60-65°C for 1 hour after adding sodium hypochlorite, add 2 ml of 5% sodium sulfite solution, stir and cool down to 15- 20°C, filter, wash four times with 40 ml of water, the first washing water and the mother liquor are combined and distilled to recover tert-butylamine, the last washing water is 50°C hot water, apply it as the dilution water of the next batch, filter, 50°C Drying, sa...

Embodiment 2

[0028] The operating conditions were the same as in Example 1, but 0.1 g of ionic surfactant was used instead of Nongru 600# to obtain 23.2 g of finished product with a melting point of 105°C and a TBBS yield of 97.5%. Methanol insoluble matter 0.52%.

Embodiment 3

[0030] The operating conditions were the same as in Example 1, but 0.1 g of polyoxyethylene octadecylamine was used instead of Nongru 600# to obtain 23.1 g of finished product with a melting point of 105.1°C, a TBBS yield of 97%, and methanol insolubles of 0.3%.

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Abstract

The invention belongs to the field of fine chemical engineering, and relates to an improved method for preparing N-tert-butylbenzothiazolesulfenamide. 2-benzothiazolethiol and tertbutylamine are taken as raw materials, and undergo oxidation reaction by using sodium hypochlorite as an oxidant in the presence of an ionic or nonionic surfactant, and after the reaction is finished, a proper amount of reducing agent is added to remove unreacted sodium hypochlorite so as to improve the stability in the process of drying the product. In the method, sulfuric acid and sodium hydroxide are not needed, so that wastewater amount is small, the product yield is over 95 percent, the smelting point is 105DEG C, and the insoluble matter content in methanol is stabilized in a range of 0.28 to 0.68 percent and reaches the national standard. The consumption of main raw materials is low, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for preparing N-tert-butylbenzothiazole sulfenamide by using sodium hypochlorite as an oxidizing agent. Background technique [0002] N-tert-butyl-2-benzothiazole sulfenamide (hereinafter referred to as accelerator TBBS) is one of the important varieties of sulfenamide vulcanization accelerators. It has two advantages of scorch resistance and fast vulcanization speed. In natural rubber, styrene-butadiene rubber, cis-butadiene rubber, and isoprene rubber, it is especially suitable for furnace-process carbon black rubber with high alkalinity, with slight discoloration and pollution, and can replace the carcinogenic NOBS containing secondary amino groups (N-morpholino benzothiazole sulfenamide), Germany legislated in 1994 to replace NOBS used in the tire industry with CBS (CZ) or TBBS. At present, the production and consumption of TBBS abroad account for...

Claims

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Application Information

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IPC IPC(8): C07D277/80
Inventor 付春刘伊文陶建青张云刚
Owner CHINA PETROLEUM & CHEM CORP
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