A kind of dimethyl silicone oil modified by hafnium-containing multi-element metal organic compound and its preparation method and application
A technology of simethicone and organic compounds, which is applied in the field of organosilicon chemistry, can solve the problems of undisclosed simethicone viscosity, no consideration of the change of simethicone acid value, and no study of thermal oxygen stability, etc., to achieve Prolonged gelation time, suitable for large-scale production, and slow viscosity growth
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Embodiment 1
[0037] Add 150g of commercially available simethicone oil with a viscosity (20°C) of 100cP into a 250mL three-necked flask equipped with nitrogen protection, reflux condenser, mechanical stirring and thermometer, and then add 15g of ZnO which has been vacuum-dried at 150°C for 2h. powder, start stirring, and gradually raise the temperature from room temperature to 150° C. under the protection of nitrogen, and maintain at this temperature for 3 hours. After cooling down to room temperature, the mixture in the three-necked flask was filtered under reduced pressure, and the filtrate was collected.
[0038] Transfer the collected filtrate to the device for removing low boilers, blow a small amount of nitrogen gas into it, and when the absolute pressure of the system reaches 1500Pa, gradually raise the temperature from room temperature to 200°C, and maintain at 200°C for 1.5h to remove the filtrate Medium low boilers. After the kettle liquid drops to room temperature, turn off the...
Embodiment 2
[0041] Add 2400g of commercially available simethicone oil with a viscosity (20°C) of 100cP into a 3000mL three-necked flask equipped with nitrogen protection, reflux condenser, mechanical stirring and thermometer, and then add 240g of ZnO which has been vacuum-dried at 150°C for 3h. powder, start stirring, and gradually raise the temperature from room temperature to 150° C. under the protection of nitrogen, and maintain at this temperature for 3 hours. After cooling down to room temperature, the mixture in the three-necked flask was filtered under reduced pressure, and the filtrate was collected.
[0042] Transfer the collected filtrate to a device for removing low boilers, blow a small amount of nitrogen gas into it, and when the absolute pressure of the system reaches 10Pa, gradually raise the temperature from room temperature to 200°C, and maintain it at 200°C for 4 hours to remove the filtrate. of low boilers. After the kettle liquid drops to room temperature, turn off t...
Embodiment 3
[0045]Take by weighing the simethicone oil that the ZnO treatment of 100g embodiment 2 prepares in the 250mL three-necked flask that has reflux condenser, mechanical stirring and thermometer, add the nickel dibutyl dithiocarbamate of 0.07g (Ni atom and Silicone oil mass ratio is 0.0000879: 1), adding 0.0792g mass concentration is 45% n-butanol hafnium hexane solution (the mass ratio of Hf atom and silicone oil is 0.000135: 1) and 3.5g zirconium acetylacetonate (Zr atom and silicone oil The mass ratio is 0.00655:1), the stirring was started, the temperature was gradually raised from room temperature to 300°C, and maintained at 300°C for 12h. After cooling down to room temperature, filter, transfer the filtrate to the low boiling reaction kettle, feed a small amount of nitrogen (purity 99.9%) bubbling, when the absolute pressure of the system reaches 0.1Pa, gradually heat up from room temperature to 205 ° C, and Maintain at 205°C for 2h to remove low boilers in the filtrate and ...
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