Perfluoroether-based polysiloxane and its preparation method and application

Abstract

The invention relates to perfluoroether-based polysiloxane as well as a preparation method and application thereof. The perfluoroether-based polysiloxane has a structure characteristic as shown in a formula (I). The perfluoroether-based polysiloxane can have excellent performance of a low-temperature-resistance property, a viscosity-temperature property, stability, corrosion resistance and anti-wear capacity, further, is little in evaporation loss, and can be applicable to the fields, with severe environments, of aerospace, special industry and the like.

Description

technical field

[0001] The invention relates to the field of polymer materials, in particular to a perfluoroether-based polysiloxane and its preparation method and application. Background technique

[0002] Silicone oil has good heat resistance, low temperature resistance and oxidation resistance, strong shear resistance, little change in viscosity with temperature, and has the basic characteristics required by lubricating oil. However, the lubricating properties of silicone oil vary greatly depending on the organic groups attached to the silicon atoms. For example, methyl silicone oil with a methyl group attached to the silicon atom has poor lubricity, and fluorine atoms are introduced into the silicone oil molecule. , not only can increase the lubricity but also can improve its heat resistance.

[0003] The fluorine-containing polysiloxane (fluorosilicone oil) obtained by introducing fluorine atoms into the silicone oil molecule has a main chain structure of a soft silico...

Examples

Embodiment 1

[0044] Add 500 mL of m-xylene hexafluoride and 0.25 mol of triethylamine into a four-neck flask, stir and mix evenly, heat to 60°C, and add 0.1 mol of perfluoroether-based dichlorosilane and 150 mL of m-xylene hexafluoride dropwise at the same time and the mixed solution of 0.105mol of disiloxanediol and 150mL of methyl ethyl ketone, after 80 minutes of dripping, the reaction mixture was stirred for 30 minutes; the reactant was washed with water to remove the by-product hydrochloride, separated The organic layer was distilled under reduced pressure to obtain perfluoroether cyclotrisiloxane.

[0045]Under the protection of an inert gas, mix 0.3mol octamethylcyclotetrasiloxane, 0.1mol decamethyltetrasiloxane, and 0.0003mol potassium hydroxide, raise the temperature to 140°C, and add 0.1mol perfluoroether cyclotrisiloxane dropwise. Siloxane, after 2 hours of dripping, continue to react for 1 hour, neutralize with 0.00012mol phosphoric acid after the reaction, and then vacuum remo...

Embodiment 2

[0049] Add 500 mL of m-xylene hexafluoride and 0.22 mol of dimethylaniline into a four-neck flask, stir and mix evenly, heat to 80°C, and at the same time add 0.1 mol of perfluoroether dichlorosilane and m-xylene hexafluoride dropwise 150 mL of the mixed solution, and the mixed solution of 0.105 mol of disiloxanediol and 150 mL of methyl ethyl ketone, dripped for 60 minutes, and after the dropping, stirred the reaction mixture for 30 minutes; The organic layer was taken out and subjected to vacuum distillation to obtain perfluoroether-based cyclotrisiloxane.

[0050] Under the protection of an inert gas, mix 0.2mol DMC, 0.05mol dodecamethylpentasiloxane, and 0.0015mol potassium hydroxide, raise the temperature to 120°C, add 0.2mol perfluoroether cyclotrisiloxane dropwise, drop for 4 hours After completion, the reaction was continued for 3 hours. After the reaction, it was neutralized with 0.0015mol hydrochloric acid, and then vacuum removed at -0.099Mpa at 200°C for 1 hour to ...

Embodiment 3

[0053] Add 500 mL of m-xylene hexafluoride and 0.3 mol of pyridine into a four-neck flask, stir and mix evenly, heat to 30°C, and simultaneously add 0.1 mol of perfluoroether-based dichlorosilane and 150 mL of m-xylene hexafluoride dropwise. solution, and a mixed solution of 0.1 mol of disiloxanediol and 150 mL of methyl ethyl ketone, dripped over 150 minutes, and stirred the reaction mixture for 30 minutes after dripping; washed the reactant with water to remove by-product hydrochloride, and separated the organic layer Distill under reduced pressure to obtain perfluoroether-based cyclotrisiloxane.

[0054] Under the protection of inert gas, mix 0.2mol octamethylcyclotetrasiloxane, 0.001mol decamethyltetrasiloxane, and 0.00025mol tetramethylammonium hydroxide, raise the temperature to 90°C, and add 0.1mol perfluoroether dropwise Cyclotrisiloxane, after 3 hours of dripping, continue to react for 2 hours, after the reaction, heat to 160°C for 0.5h, decompose the catalyst, and th...

technical field

[0001] The invention relates to the field of polymer materials, in particular to a perfluoroether-based polysiloxane and its preparation method and application. Background technique

[0002] Silicone oil has good heat resistance, low temperature resistance and oxidation resistance, strong shear resistance, little change in viscosity with temperature, and has the basic characteristics required by lubricating oil. However, the lubricating properties of silicone oil vary greatly depending on the organic groups attached to the silicon atoms. For example, methyl silicone oil with a methyl group attached to the silicon atom has poor lubricity, and fluorine atoms are introduced into the silicone oil molecule. , not only can increase the lubricity but also can improve its heat resistance.

[0003] The fluorine-containing polysiloxane (fluorosilicone oil) obtained by introducing fluorine atoms into the silicone oil molecule has a main chain structure of a soft silico...

Examples

Embodiment 1

[0044] Add 500 mL of m-xylene hexafluoride and 0.25 mol of triethylamine into a four-neck flask, stir and mix evenly, heat to 60°C, and add 0.1 mol of perfluoroether-based dichlorosilane and 150 mL of m-xylene hexafluoride dropwise at the same time and the mixed solution of 0.105mol of disiloxanediol and 150mL of methyl ethyl ketone, after 80 minutes of dripping, the reaction mixture was stirred for 30 minutes; the reactant was washed with water to remove the by-product hydrochloride, separated The organic layer was distilled under reduced pressure to obtain perfluoroether cyclotrisiloxane.

[0045]Under the protection of an inert gas, mix 0.3mol octamethylcyclotetrasiloxane, 0.1mol decamethyltetrasiloxane, and 0.0003mol potassium hydroxide, raise the temperature to 140°C, and add 0.1mol perfluoroether cyclotrisiloxane dropwise. Siloxane, after 2 hours of dripping, continue to react for 1 hour, neutralize with 0.00012mol phosphoric acid after the reaction, and then vacuum remo...

Embodiment 2

[0049] Add 500 mL of m-xylene hexafluoride and 0.22 mol of dimethylaniline into a four-neck flask, stir and mix evenly, heat to 80°C, and at the same time add 0.1 mol of perfluoroether dichlorosilane and m-xylene hexafluoride dropwise 150 mL of the mixed solution, and the mixed solution of 0.105 mol of disiloxanediol and 150 mL of methyl ethyl ketone, dripped for 60 minutes, and after the dropping, stirred the reaction mixture for 30 minutes; The organic layer was taken out and subjected to vacuum distillation to obtain perfluoroether-based cyclotrisiloxane.

[0050] Under the protection of an inert gas, mix 0.2mol DMC, 0.05mol dodecamethylpentasiloxane, and 0.0015mol potassium hydroxide, raise the temperature to 120°C, add 0.2mol perfluoroether cyclotrisiloxane dropwise, drop for 4 hours After completion, the reaction was continued for 3 hours. After the reaction, it was neutralized with 0.0015mol hydrochloric acid, and then vacuum removed at -0.099Mpa at 200°C for 1 hour to ...

Embodiment 3

[0053] Add 500 mL of m-xylene hexafluoride and 0.3 mol of pyridine into a four-neck flask, stir and mix evenly, heat to 30°C, and simultaneously add 0.1 mol of perfluoroether-based dichlorosilane and 150 mL of m-xylene hexafluoride dropwise. solution, and a mixed solution of 0.1 mol of disiloxanediol and 150 mL of methyl ethyl ketone, dripped over 150 minutes, and stirred the reaction mixture for 30 minutes after dripping; washed the reactant with water to remove by-product hydrochloride, and separated the organic layer Distill under reduced pressure to obtain perfluoroether-based cyclotrisiloxane.

[0054] Under the protection of inert gas, mix 0.2mol octamethylcyclotetrasiloxane, 0.001mol decamethyltetrasiloxane, and 0.00025mol tetramethylammonium hydroxide, raise the temperature to 90°C, and add 0.1mol perfluoroether dropwise Cyclotrisiloxane, after 3 hours of dripping, continue to react for 2 hours, after the reaction, heat to 160°C for 0.5h, decompose the catalyst, and th...

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