Preparation method of rubber vulcanization accelerator tetra(isobutyl)thioperoxydicarbamic acid (TiBTD)
A technology of diisobutyl disulfide, rubber vulcanization, applied in organic chemistry and other directions, can solve the problems of non-compliance with national environmental protection policy production requirements, difficult to clean "green" production, difficult to meet high-end requirements, etc., to achieve excellent vulcanization performance , The effect of short curing time and long scorch time
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Embodiment 1
[0025] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.26:0.49:0.015;
[0026] The process is as follows: into the 2000L enamel reaction kettle, add the specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate in sequence under stirring; turn on the cooling water, cool down to 42°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 6 hours. After the dropwise addition, the pH value of the reaction solution was measured to be 8. After the pH value was stabilized, the temperature was controlled at 58° C., and hydrogen peroxide was started to be added dropwise, and the oxidation reaction was carried out for 5 hours. After the oxidation is finished, heat the reaction for another 1 hour, carry out solid...
Embodiment 2
[0028] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.27:0.51:0.017;
[0029] The process is as follows: add a specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate to the 2000L enamel reaction kettle in a stirring state; turn on the cooling water, cool down to 44°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 6.5 hours. After the dropwise addition, the pH value of the reaction solution was measured to 8.5. After the pH value was stabilized, the temperature was controlled at 60° C., and hydrogen peroxide was added dropwise, and the oxidation reaction was carried out for 5.5 hours. After the oxidation is finished, heat the reaction for another 1 hour, carry out solid-liquid separation, dis...
Embodiment 3
[0031] In this embodiment, the raw materials used are respectively diisobutylamine, carbon disulfide, hydrogen peroxide and sodium dodecylsulfonate, and the stoichiometric molar ratio is: diisobutylamine: carbon disulfide: hydrogen peroxide: dodecyl Sodium sulfonate=1:1.28:0.53:0.019;
[0032] The process is as follows: add a specified amount of diisobutylamine, alcohols or water, and sodium dodecylsulfonate to the 2000L enamel reaction kettle in a stirring state; turn on the cooling water, cool down to 46°C, and start adding dropwise Accurately metered carbon disulfide liquid, the control time is 7 hours. After the dropwise addition, the pH value of the reaction solution was measured to be 9. After the pH value was stabilized, the temperature was controlled at 62° C., and hydrogen peroxide was added dropwise, and the oxidation reaction was carried out for 6 hours. After the oxidation is completed, heat the reaction for 1 hour, separate the solid and liquid, discard the liqui...
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