Method for synthesizing thiofide NS by oxygen oxidation method
A vulcanization accelerator and a technology for synthesizing rubber, which is applied in the field of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide, can solve the problems of low yield of accelerator NS, and achieve good product quality and low consumption. The effect of small amount and high yield
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[0007] example 1:
[0008] The condensation reaction of aniline, carbon disulfide and sulfur is carried out at 270-280° C. and pressure of 9-10 MPa to generate MBT with a mass content of 92%. After purification, MBT with a mass percentage of 95% is obtained. 50 grams of MBT and 97 grams of ammonia water with a mass percentage of 10% were added to a three-necked flask, and dissolved under the conditions of a temperature of 35° C. and a stirring speed of 30 rpm. When the MBT was completely dissolved, the solution was added to the autoclave. Dissolve 0.04 g of catalyst copper sulfate with 10 g of ammonia water with a mass percentage of 10%, and add it into the autoclave. Under the conditions that the reaction temperature is 40° C. and the stirring speed is 300 rev / min, oxygen is introduced into the autoclave, and the reaction is carried out for 1 hour under the condition that the reaction pressure is 0.2 MPa. 21.3 grams of tert-butylamine with a mass percentage of 97% was added...
Example
[0009] Example 2:
[0010] The condensation reaction of aniline, carbon disulfide and sulfur is carried out at 270-280° C. and pressure of 9-10 MPa to generate MBT with a mass content of 92%. After purification, MBT with a mass percentage of 97% is obtained. 50 grams of MBT and 123 grams of ammonia water with a mass percentage of 20% were added to a three-necked flask, and dissolved under the conditions of a temperature of 40° C. and a stirring speed of 30 rpm. When the MBT was completely dissolved, the solution was added to the autoclave. Dissolve 0.16 grams of catalyst copper sulfate with 15 grams of ammonia water with a mass percentage of 20%, and add it to the autoclave. Under the condition that the reaction temperature is 55° C. and the stirring speed is 600 rev / min, oxygen is introduced into the autoclave, and the reaction is carried out under the condition that the reaction pressure is 0.5 MPa for 3 hours. 53.7 grams of tert-butylamine with a mass percentage of 99% wa...
Example
[0011] Example 3:
[0012] The condensation reaction of aniline, carbon disulfide and sulfur is carried out at 270-280° C. and pressure of 9-10 MPa to generate MBT with a mass content of 92%. After purification, MBT with a mass percentage of 99% is obtained. 50 grams of MBT and 126 grams of ammonia water with a mass percentage of 25% were added to a three-necked flask, and dissolved under the conditions of a temperature of 45° C. and a stirring speed of 30 rpm. When the MBT was completely dissolved, the solution was added to the autoclave. Dissolve 0.28 g of catalyst copper sulfate with 20 g of ammonia water with a mass percentage of 25%, and add it into the autoclave. Under the conditions that the reaction temperature is 70° C. and the stirring speed is 1000 rev / min, oxygen is introduced into the autoclave, and the reaction is carried out for 5 hours under the condition that the reaction pressure is 0.7 MPa. 60.0 grams of tert-butylamine with a mass percentage of 99.5% was ...
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