Mercapto silane
A technology of mercaptosilane and group, applied in the field of mercaptosilane, can solve the problems of impossible to omit mercaptosilane, short mixing time, etc.
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Embodiment 1
[0517] Weigh 59.63 g (0.25 mol) of 3-mercaptopropyltriethoxysilane (VP Si 263 from Degussa AG), 212.92 g (0.50 mol) of ethoxylated alcohol R 1 H, where R 5 is CH 2 -CH 2 , R 6 is an unsubstituted monovalent alkyl group containing 13 carbon atoms with an average m of 5 (Lutensol TO5, available from BASF AG), and 30 μl of titanium tetrabutoxide, and placed in a 500 ml four-necked flask at room temperature under a nitrogen atmosphere , equipped with distillation bridge, KPG stirrer and thermometer. The mixture was heated to 140°C. The ethanol formed is distilled off continuously. After 35 minutes, the reduced pressure was adjusted to 640 mbar and decreased to 50 mbar over the course of 3 hours. The reaction was terminated after 3 hours and 35 minutes. 245.37 g (98.6%) of a cloudy and slightly yellowish product were obtained. pass 1 H-NMR spectroscopy gave an average degree of transesterification of 2.0. Depend on 13 C-NMR can determine the distribution of long-chain br...
Embodiment 2
[0518] Embodiment 2 (comparative example)
[0519] 2,925.3 g of 3-mercaptopropyltriethoxysilane, 4,753.4 g of an alcohol mixture containing 72% dodecanol and 28% myristyl alcohol, and 30 μl of titanium tetrabutoxide were weighed and placed at room temperature under a nitrogen atmosphere. into a 4 l four-neck flask equipped with a distillation bridge, a KPG stirrer and a thermometer. The mixture was heated to 110°C. The ethanol formed is distilled off continuously. After 2 hours, the reduced pressure was continuously reduced to 50 mbar over the course of 3 hours. The reaction was terminated when 1,140 ml of ethanol was removed from the reaction mixture. 6.47 kg (98.6%) of a pale yellow liquid were obtained. pass 1 H-NMR spectroscopy gave an average degree of transesterification of 2.0.
Embodiment 3
[0520] Embodiment 3 (comparative example)
[0521] Weigh 150.02 g (0.63 mol) of 3-mercaptopropyltriethoxysilane, 151.2 g (1.26 mol) of diethylene glycol monomethyl ether and 75 μl of titanium tetrabutoxide, and place them at room temperature under a nitrogen atmosphere In a 500ml three-necked flask, it is equipped with an enhanced condenser, a stirrer and a thermometer. The mixture was heated to 80°C. The ethanol formed was removed under reduced pressure of 3 mbar.
[0522] The reaction was terminated after 8 hours. 237.84 g (97.6%) of a clear and slightly yellowish product were obtained. pass 1 H-NMR spectroscopy gave an average degree of transesterification of 2.0.
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