Technology Optimization Of N-Tert-Butyl-2-Benzothiazolyl Sulfonamide

A new method to synthesize vulcanization accelerator N-tert-buthylbenzothiazole-2-sulfenamide(NS)was studied in this article.NS was synthesized by the reaction of2-mercaptobenzothiazole(M)and tert-buthylamine with the catalyst palladium chloride.For almost no ‘three wastes',this route was a green production technology.In this route,a large amount of water resources were saved and the production costs were reduced at the same time,which met the requirements of the national development of green chemistry and had broad application prospect.This subject first established the range of explosion limit parameters of tert-butylamine,oxygen and ammonia.Effects of the catalyst type and content,the reaction temperature,the reaction time,the reaction pressure,the reaction mole ratio,the stirring speed,the water content,the ammonia content and the mother liquor recycling times on NS yield and purity were systemically explored.The parameters were as follows:the largest oxygen content was 34.5%,the catalyst type was palladium chloride and the content was 0.6%,the reaction temperature was 60 ?,the reaction time was 8 h,the reaction pressure was 0.6 Mpa,the mole ratio of accelerator M and tert-butylamine was1:5.7,the stirring speed was 600 r/min,the water content was 45%,the ammonia content was 8% and the mother liquor recycling times was 9.The establishment of these parameters were of great significance for industrial safety.The analyses of NS sample by HPLE and melting point showed that it has a high purity which exceeded 98.5% and had great properties.The samples all satisfied the CN GB/T 21840-2008.