A kind of simethicone oil modified by multi-element metal organic compound containing cerium and its preparation method and application
A technology of simethicone and organic compounds, which is applied in the field of organosilicon chemistry, can solve problems such as prolongation of the gelation time of simethicone, and achieve the effect of being suitable for large-scale production, simple operating conditions, and good thermal stability
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Embodiment 1
[0038] 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.
[0039] 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 2
[0042]Weigh 100g of simethicone oil treated with ZnO at 150°C for 3h to a 250mL three-necked flask with reflux condenser, mechanical stirring and thermometer, add 0.0548g of nickel dimethylaminodithioformate (Ni atom and silicone oil The mass ratio is 0.000107: 1), 0.3475g of three (tetramethylcyclopentadiene) cerium (the mass ratio of Ce atom to silicone oil is 0.0009667: 1) and 4.0540g of tetrabutyl zirconate (the ratio of Zr atom to silicone oil The mass ratio is 0.00964:1), the stirring was started, the temperature was gradually raised from room temperature to 310°C, and maintained at 310°C for 15h. 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 residual solvents in metal organic com...
Embodiment 3
[0044] Take by weighing 100g of the simethicone oil prepared in Example 1 at 150°C for 3h to a 250mL three-necked flask with a reflux condenser, a mechanical stirrer and a thermometer, and add 0.07g of dibutyldithiocarbamate Nickel (the mass ratio of Ni atom to silicone oil is 0.0000879:1), 0.2129g of cerium acetylacetonate hydrate (the mass ratio of Ce atom to silicone oil is 0.000655:1) and 3.5g of zirconium acetylacetonate (the mass ratio of Zr atom to silicone oil is 0.00655:1), start stirring, gradually raise the temperature from room temperature to 300°C, and maintain 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 residual solvents in metal organic compounds. Aft...
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