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Cerium-containing multi-metal organic compound modified dimethyl silicone oil, and preparation method and application thereof

A technology of simethicone and organic compounds, which is applied in the field of organosilicon chemistry and can solve problems such as prolonged gelation time of simethicone

Active Publication Date: 2021-09-14
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to solve the problem of improving the high-temperature thermal oxidation stability of simethicone oil in an aerobic environment, the acid value of the modified simethicone oil also meets the national standard. The property of simethicone oil and its preparation method and application, the thermal properties of the prepared simethicone oil in aerobic environment are significantly improved, the gelation time of simethicone oil is significantly prolonged, and the modified dimethyl silicone oil The acid value of silicone oil meets the national standard

Method used

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  • Cerium-containing multi-metal organic compound modified dimethyl silicone oil, and preparation method and application thereof
  • Cerium-containing multi-metal organic compound modified dimethyl silicone oil, and preparation method and application thereof
  • Cerium-containing multi-metal organic compound modified dimethyl silicone oil, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to the field of organosilicon chemistry, and provides a cerium-containing multi-metal organic compound modified dimethyl silicone oil, and a preparation method and application thereof in order to solve the problem that the acid value of the dimethyl silicone oil needs to meet the national standard while the high-temperature thermal oxidation stability of the dimethyl silicone oil in an aerobic environment is improved. The acid value of the prepared modified dimethyl silicone oil is less than 0.05 mgKOH / g, the viscosity is slowly increased in high-temperature and aerobic environments, the gelation time is prolonged, the mass loss at high temperature is less, and the preparation method is simple in operation condition, simple in steps, low in production cost and very suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of organosilicon chemistry, in particular to a modification of dimethyl silicone oil by using metal oxides and cerium-containing multi-element metal organic compounds and its application. [0002] technical background [0003] Polysiloxane is composed of repeating R 1 R 2 Silicone polymer composed of SiO chain members. R 1 and R 2 is a duplicate of R 1 R 2 Organic functional groups directly connected to Si atoms in the SiO chain link, including H, CH 3 、C 2 h 5 、C 6 h 5 、CF 3 CH 2 CH 2 , OCH 3 、OC 2 h 5 Equally saturated organic functional groups and CH 2 = CH and other unsaturated organic functional groups, R 1 with R 2 Can be the same or different. When R 1 When both are methyl with R2, the repeated (CH 3 ) 2 Polysiloxane composed of SiO chain members is also called polydimethylsiloxane (PDMS). Polydimethylsiloxane can be capped with different functional groups. When the capping groups at both...

Claims

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Application Information

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IPC IPC(8): C08G77/398C08G77/38
CPCC08G77/398C08G77/38
Inventor 伍川苏锦华董红肖顺超瞿志荣王旸刘阳蔡亮邱化玉
Owner HANGZHOU NORMAL UNIVERSITY