Preparation method of sulfur-containing silane coupling agent containing long-chain alkoxy group
A sulfur silane coupling agent, alkoxy-containing technology, applied in the field of fine chemicals, can solve the problems of reducing the safety of rubber mixing, affecting the performance of rubber, etc., to save industrial production costs, excellent wear resistance, high efficiency Effect
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Embodiment 1
[0030] In a 3000ml four-necked flask, install a mechanical stirrer, a distillation receiving device, a thermometer and a heating device, then add 474g (1mol) of bis-[3-(triethoxysilyl)propyl] disulfide, 340g of disulfide Methyl sulfoxide, 4.5g of stannous chloride, heat the material in the flask to 60-65°C and stir for 0.5h in the stirring state, and the material becomes transparent; then continue to stir and heat, when the temperature of the material reaches 122°C 2060 g (4.05 mol) of isomeric tridecyl alcohol polyoxyethylene ether (TO1307) was added dropwise into the reactor; while stirring while adding dropwise, the ethanol produced by the reaction was recovered by condensation at the same time, and the polyether was added dropwise for 5-6 hours.
[0031] After the material is added dropwise, control the reaction temperature at 122-125°C and continue to stir the reaction for 3-4h; then lower the temperature to 65°C, pump negative pressure and gradually increase the temperatu...
Embodiment 2
[0034] In the four-necked flask of 3000ml, install mechanical stirring, distillation receiving device, thermometer and heating device, then add 539g (1mol) of bis-[3-(triethoxysilane)-propyl]-tetrasulfide, 280g dimethyl sulfoxide, 4.5g of stannous chloride, heat the material in the flask to 60-65°C and stir for 0.5h in the stirring state, and the material becomes transparent; then continue stirring and heating, when the temperature of the material reaches 122°C Then add 2060g (4.05mol) of isomeric tridecyl alcohol polyoxyethylene ether (TO1307) dropwise into the reactor; stir while adding dropwise, and recover the ethanol produced by the reaction at the same time, the polyether dropwise adding time is 5-6h .
[0035] After the material is added dropwise, control the reaction temperature at 122-125°C and continue to stir the reaction for 3-4h; then lower the temperature to 65-75°C, pump negative pressure and gradually increase the temperature to distill and recover ethanol and ...
Embodiment 3
[0038] In a 3000ml four-necked flask, install a mechanical stirrer, a distillation receiving device, a thermometer and a heating device, and then add 364g (1mol) of 3-(octanoylthio)propyltriethoxysilane 300g of dimethyl sulfoxide , 1.2g of stannous chloride, heat the material in the flask to 60-65°C and stir for 0.5h in the stirring state, and the material becomes transparent; then continue to stir and heat, and drop it into the reactor when the temperature of the material reaches 122°C Add 1016g (2mol) of isomeric tridecyl alcohol polyoxyethylene ether (TO1307); stir while adding dropwise, and recover the ethanol produced by the reaction through condensation at the same time. The time for adding polyether is 5-5.5h.
[0039] After the material is added dropwise, control the reaction temperature at 122-125°C and continue to stir the reaction for 3-4h; then lower the temperature to 60-65°C, pump negative pressure and gradually increase the temperature to distill and recover ethano...
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