Method for synthesizing rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) through two-step method by taking hydrogen peroxide as oxidant
A technology of vulcanization accelerator and synthetic rubber, which is applied in the direction of organic chemistry, can solve the problem of low yield of accelerator NS, and achieve the effect of eliminating the recycling process, simple process, and easy industrialization
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[0008] Example 1:
[0009] The first step takes by weighing 98% sulfuric acid 80g, is configured into 20% sulfuric acid, joins in the reactor of existing 60 grams of tert-butylamine, at 40 DEG C, rotating speed are under the condition of 600 rev / min, make sulfuric acid fully react with tert-butylamine , and then drip the density of 1.5g / ml M-Na salt 105ml to generate M-tert-butylamine salt.
[0010] In the second step, 360ml of oxidant hydrogen peroxide with a mass content of 12.0% was added at a flow rate of 3ml / min, and the dropping time was 2.0 hours. After the reaction was completed, suction filtration, washing, filtration and drying were performed to obtain the rubber accelerator NS product, the purity of the accelerator NS It reaches more than 99%, and the yield reaches 97.1%.
Example Embodiment
[0011] Example 2:
[0012] The first step takes by weighing 98% sulfuric acid 80g, is configured into 20% sulfuric acid, joins in the reactor of existing 60 grams of tert-butylamine, at 40 DEG C, rotating speed are under the condition of 600 rev / min, make sulfuric acid fully react with tert-butylamine , and then drip the density of 1.5g / ml M-Na salt 105ml to generate M-tert-butylamine salt.
[0013] The second step was to add 360ml of oxidant hydrogen peroxide with a mass content of 15.0% at a flow rate of 3ml / min, and the dropping time was 2.0 hours. After the reaction was completed, suction filtration, washing, filtration, and drying were used to obtain the rubber accelerator NS product. The purity is over 99%, and the yield is 97.4%.
Example Embodiment
[0014] Example 3:
[0015] The first step takes by weighing 98% sulfuric acid 80g, is configured into 20% sulfuric acid, joins in the reactor of existing 60 grams of tert-butylamine, at 40 DEG C, rotating speed are under the condition of 600 rev / min, make sulfuric acid fully react with tert-butylamine , and then drip the density of 1.5g / ml M-Na salt 105ml to generate M-tert-butylamine salt.
[0016] In the second step, 360ml of oxidant hydrogen peroxide with a mass content of 18.0% was added at a flow rate of 3ml / min, and the dropping time was 2.0 hours. After the reaction was completed, suction filtration, washing, filtration and drying were performed to obtain the rubber accelerator NS product, the purity of the accelerator NS It reaches more than 99%, and the yield reaches 97.5%.
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