Preparation method of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfonamide (NS)
A technology of benzothiazole sulfenamide and dibenzothiazole disulfide, which is applied in the field of rubber vulcanization accelerator preparation, can solve the problems of large discharge of organic wastewater, low product yield and quality, and large amount of auxiliary raw materials. Achieve the effect of reducing the amount of wastewater treatment, using fewer types of materials, and shortening the vulcanization time
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Embodiment 1
[0035] Add 35ml of ammonia water in a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and put in the reactant dibenzothiazole disulfide 33.25g (0.1mol), copper ammonia catalyst 0.12g and surfactant under strong stirring TW-20 0.005g, control the temperature to 20°C, feed oxygen to make the pressure 0.4MPa, add 16.09g of tert-butylamine within 2.5h, at this time, the temperature in the kettle rises, control the temperature to 40°C, react for 1.5h, absorb oxygen When it is rare, the reaction reaches the end and the stirring is stopped. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is off-white. It is determined that the reaction yield is 96.2%. The product obtained after the reaction has an initial melting point of 106.3° C. and a purity of 98.6%.
Embodiment 2
[0037] Add 42ml of ammonia water to a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and add 33.25g (0.1mol) of the reactant dibenzothiazole disulfide, 0.18g of cuproammonia catalyst and surfactant under strong stirring. TW-20 0.006g, control the temperature to 16°C, feed oxygen to make the pressure 0.6MPa, add 15.36g of tert-butylamine within 2h, at this time, the temperature in the kettle rises, control the temperature to 38°C, react for 1.5h, oxygen absorption is very When it is small, the reaction will reach the end, so stop stirring. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is off-white. It is determined that the reaction yield is 95.8%. The product obtained after the reaction has a melting point of 106.8° C. and a purity of 98.9%.
Embodiment 3
[0039] Add 50ml of ammonia water to a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and add 33.25g (0.1mol) of dibenzothiazole disulfide, 0.20g of cuproammonia catalyst and surfactant under strong stirring. TW-20 0.008g, control the temperature to 10°C, feed oxygen to make the pressure 0.5MPa, add 17.55g of tert-butylamine within 3.0h, at this time, the temperature in the kettle rises, control the temperature to 35°C, react for 2h, oxygen absorption is very When it is small, the reaction will reach the end, so stop stirring. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is white, and the reaction yield is 97.4%. The product obtained after the reaction has a melting point of 107.2° C. and a purity of 99.1%.
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