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Process for preparing NS by oxidizing M tert-butyl ammonium salt with hydrogen peroxide

A technology of hydrogen peroxide and butylammonium salt, applied in organic chemistry and other directions, can solve the problems of difficult treatment of salt-containing organic wastewater, human and environmental hazards, difficult operation, etc. mild effect

Active Publication Date: 2020-06-19
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the operation is difficult, the chlorine gas process is seriously harmful to the human body and the environment, and the treatment of the salty organic wastewater produced is difficult
These methods either cause a lot of pollution or have too much equipment investment or immature technology. These production processes do not meet the requirements of green chemical industry and clean production.

Method used

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  • Process for preparing NS by oxidizing M tert-butyl ammonium salt with hydrogen peroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 167.25g of accelerator M to 109.71g of tert-butylamine and 20g of water for beating, raise the temperature to 30°C and stir to make all M and tert-butylamine combine to form a salt. After TLC detects that there is no free M, add 0.2g of KI, heat to 30°C, and add 156.4g dropwise Concentration of 27.5% hydrogen peroxide. Hydrogen peroxide was added dropwise for 10 min, and the reaction was incubated until no M tert-butylammonium salt remained in TLC detection. Cool down, centrifuge, wash, recover tert-butylamine, and dry the filter cake to obtain NS finished product. Initial melting point: 107.4°C, purity 98.6%, yield: 98.1%, product appearance is white particles.

Embodiment 2

[0035] Add 167.25g of accelerator M to 182.85g of tert-butylamine and 5g of water for beating, raise the temperature to 20°C and stir to make all M and tert-butylamine combine to form a salt. After TLC detects that there is no free M, add 0.01g of I 2 , the temperature was raised to 25° C., and then 156.4 g of hydrogen peroxide with a concentration of 27.5% was added, and the hydrogen peroxide was added dropwise for 10 min, and the temperature was kept until no M tert-butylammonium salt was left in TLC detection. Cool down, centrifuge, wash, recover tert-butylamine, and dry the filter cake to obtain NS finished product. Initial melting point: 107.2°C, purity 99.5%, yield: 98.2%, product appearance is white particles.

Embodiment 3

[0037] Add 167.25g of accelerator M to 167.1g of tert-butylamine and 10g of water for beating, raise the temperature to 30°C and stir to make all M and tert-butylamine combine to form a salt, and add 0.8g of KIO after TLC detects free M 3 , continue to maintain 30 ° C, and dropwise add 172.1 g of hydrogen peroxide with a concentration of 25.1%. Hydrogen peroxide was added dropwise for 30 minutes, and the reaction was incubated until no M tert-butylammonium salt remained in TLC detection. Cool down, centrifuge, wash, recover tert-butylamine, and dry the filter cake to obtain NS finished product. Initial melting point: 107.6°C, purity 99.2%, yield: 98.6%, product appearance is white particles.

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Abstract

The invention discloses a process for preparing NS by oxidizing M tert-butylammonium salt with hydrogen peroxide, relates to a new synthesis process, in particular to a new NS synthesis process, and belongs to the technical field of chemical synthesis. The method is characterized by comprising the following steps: mixing and pulping a raw material M and tert-butylamine, adding a small amount of iodized salt (KI, NaI, KIO3, I2 and the like), dropwise adding an oxidant hydrogen peroxide under the condition of stirring and heating, and performing oxidation synthesis to obtain the product NS. Themethod provided by the invention not only overcomes the problem that a large amount of waste salt, waste gas and wastewater are generated in the preparation of NS by a traditional process, but also overcomes the problem that a hydrogen peroxide process is unstable, green, environment-friendly and clean production is realized, and the product has the advantages of high initial melting point, high purity and high yield.

Description

technical field [0001] The invention relates to a new synthesis process, in particular to a new synthesis process of NS. It belongs to the technical field of chemical synthesis. Background technique [0002] NS, that is, N-tert-butyl-2-benzothiazole sulfenamide (accelerator NS or TBBS) is one of the important varieties of sulfenamide vulcanization accelerators, and is a rubber vulcanization accelerator with excellent performance. Two major advantages of anti-scorch and fast vulcanization speed. Widely used in natural rubber, styrene-butadiene rubber, cis-butadiene rubber, and isoprene rubber. It is a highly active post-effect accelerator among various accelerators at present, with high processing safety, and vulcanized rubber has good Excellent physical properties, mechanical properties and aging resistance, short vulcanization time. It is mainly used to manufacture industrial rubber products such as tires, rubber hoses, rubber shoes, cables, etc. The radial tire industry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 刘启奎付永丰岳涛夏雪强徐婷冯维春
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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