A kind of method of producing sulfenamide type rubber vulcanization accelerator
A technology of sulfenamides and rubber vulcanization, applied in the direction of organic chemistry, etc., can solve the problems of high cost and low yield, and achieve the effects of low cost, high yield and reduced environmental pollution
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Embodiment 1
[0019] Add 45.3g (0.25mol), 2-mercaptobenzothiazole (M, content not less than 96%), 90mL deionized water (solvent) into the reactor and mix well, then add 240.0g (2.4mol) Cyclohexylamine, mixed well and evenly, controlled the reaction temperature at 35°C, slowly added 8.4g (0.125mol) of chlorine dioxide aqueous solution with a mass fraction of 15%, and continued the reaction for 2.0h. After the reaction, the solution was cooled to room temperature, and the stirring was stopped. Then put the reaction mixture into a solid-liquid separator for separation, and the separated solid filter cake is washed with water, dehydrated, and dried to obtain the finished product of N-cyclohexyl-2-benzothiazole sulfenamide (CZ). Hexylamine is recovered for use. After testing, the purity of the finished CZ is 99.1%, and the yield is 95.8%.
[0020] Under the conditions that the reaction conditions and the amount of materials added are the same, using three different oxidants of sodium hypochlor...
Embodiment 2
[0024] Add 52.6g (0.30mol) of 2-mercaptobenzothiazole (M, content not less than 96%) and 100mL saturated saline (solvent, can also be replaced by the mother liquor after the last batch reaction) into the reactor and mix evenly, and then Add 27.8g (0.32mol) morpholine into the reactor with stirring, raise the temperature to 85°C, slowly introduce 27.0g (0.40mol) chlorine dioxide gas, react for 1.5h, cool the solution to room temperature, and stop stirring. Then put the reaction mixture into a solid-liquid separator for separation, and the separated solid filter cake is washed with water, dehydrated, and dried to obtain the finished product of N-oxydiethylene-2-benzothiazole sulfenamide (NOBS), and the filtrate is It is used as a circulating material for the mother liquor. After testing, the purity of the finished NOBS is 99.8%, and the yield is 95.5%.
[0025] Under the conditions that the reaction conditions and the amount of materials added are the same, using sodium hypochl...
Embodiment 3
[0029] Add 123.5g (0.71mol) 2-mercaptobenzothiazole (M, content not less than 96%), 100mL deionized water to a four-neck flask equipped with a stirrer, thermometer and dropping funnel and stir well, Then add 73.1g (1.0mol) of tert-butylamine under stirring, mix well, control the temperature at 5°C, slowly add 20% chlorine dioxide aqueous solution with a mass fraction of 45.2g (0.67mol) of chlorine dioxide dropwise, and then continue the reaction 4.5h. After the reaction, the temperature of the solution was controlled to room temperature, and the stirring was stopped. Then the reaction mixture was precipitated and suction filtered, and the separated solid filter cake was washed with water, dehydrated and dried to obtain the finished product of N-tert-butyl-2-benzothiazole sulfenamide (NS), and the tert-butylamine in the filtrate was recovered for use. After testing, the purity of the finished NS is 99.5%, and the yield is 96.8%.
[0030] Under the conditions that reaction con...
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