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Modified fluorine-containing silicone oil and preparation method thereof

A fluorine-containing silicone oil and modification technology, which is applied in the field of organosilicon material preparation and fluorine-containing organosilicon polymers, can solve the problems of poor industrialization of fluorine-containing alkyl chlorosilane monomers, high raw material prices, and difficulty in realization, etc. Achieving the effects of superior surface inertness, product stability and low surface tension

Active Publication Date: 2015-05-13
苏州盛泽科技创业园发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are at least the following three problems in the two methods of appeal: 1. The industrialization degree of fluoroalkyl chlorosilane monomer is poor, and the price of raw materials is high; 2. Only a small amount of cage structure products can be obtained through hydrolysis and condensation of fluoroalkyl silane monomer. The yield is very low; 3. Fluoroalkylated cage silsesquioxane is inert, and it is difficult to achieve it due to poor reactivity when preparing other derivative products from it.

Method used

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  • Modified fluorine-containing silicone oil and preparation method thereof
  • Modified fluorine-containing silicone oil and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1. Synthesis of cage-type silsesquioxanylmethyldichlorosilane

[0038] Add 60g of octavinylsilsesquioxane and 300g of anhydrous toluene into a 500mL three-necked flask, protect with nitrogen, add 10g of methylhydrogen dichlorosilane, 0.01g of chloroplatinic acid catalyst, heat up to 75°C, and react for 5h , stop responding. The toluene and unreacted methylhydrogendichlorosilane were distilled off under reduced pressure under the conditions of a vacuum degree of 2 mmHg and a temperature of 45°C. The product obtained as a white solid was cage-type silsesquioxanylmethyldichlorosilane.

[0039] 2. Synthesis of cage-type silsesquioxane-based modified organopolysiloxane

[0040] Dissolve 20 g of dimethyldichlorosilane, 5 g of trimethylchlorosilane and the white solid prepared above in 200 g of anhydrous tetrahydrofuran, stir well, and set aside. Add 200g of saturated sodium bicarbonate solution into a 2000mL three-neck flask equipped with a thermometer, magnetic stirrer, con...

Embodiment 2

[0050] 1. Synthesis of cage-type silsesquioxanylmethyldichlorosilane

[0051] Add 120g of octavinylsilsesquioxane and 400g of anhydrous xylene into a 5000mL three-necked flask, under nitrogen protection, add 20g of methylhydrogen dichlorosilane, 0.01g of chloroplatinic acid catalyst, heat up to 80°C, and react for 5h After that, stop the reaction. Under the conditions of vacuum degree of 2 mmHg and temperature of 45° C., xylene and unreacted methylhydrogen dichlorosilane were distilled off under reduced pressure. The product was white solid cage silsesquioxanylmethyldichlorosilane.

[0052] 2. Synthesis of cage-type silsesquioxane-based modified organopolysiloxane

[0053] Dissolve 40 g of dimethyldichlorosilane, 10 g of trimethylchlorosilane and the white solid prepared above in 200 g of anhydrous 1,4-dioxane, stir well, and set aside. Add 200g of saturated sodium bicarbonate solution into a 2000mL three-neck flask equipped with a thermometer, magnetic stirrer, condensing ...

Embodiment 3

[0061] 1. Synthesis of cage-type silsesquioxanylmethyldichlorosilane

[0062] Add 80g of octavinylsilsesquioxane and 400g of anhydrous toluene into a 5000mL three-necked flask, under nitrogen protection, add 20g of methylhydrogen dichlorosilane, 0.02g of chloroplatinic acid catalyst, heat up to 82°C, and react for 8h , stop responding. The toluene and unreacted methylhydrogendichlorosilane were distilled off under reduced pressure under the conditions of a vacuum degree of 2 mmHg and a temperature of 50°C. The product was white solid cage silsesquioxanylmethyldichlorosilane.

[0063] 2. Preparation of cage-type silsesquioxane-based modified organopolysiloxane

[0064] Dissolve 50 g of dimethyldichlorosilane, 25 g of trimethylchlorosilane and the white solid prepared above in 300 g of anhydrous ether, stir well, and set aside. Add 200g of saturated sodium bicarbonate solution into a 2000mL three-neck flask equipped with a thermometer, magnetic stirrer, condensing reflux tube...

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Abstract

The invention discloses modified fluorine-containing silicone oil and a preparation method thereof. The preparation method of the modified fluorine-containing silicone oil comprises the following steps: firstly reacting hydrogen-containing dichloromethylsilane which serves as a starting material, chloroplatinic acid which serves as a catalyst and octavinyl polyhedral oligomeric silsesquioxane (POSS) to synthesize a vinyl polyhedral oligomeric silsesquioxane dichloromethylsilane monomer; then carrying out hydrolysis co-balance by the monomer, dimethyldichlorosilance and trimethylchlorosilane to prepare vinyl polyhedral oligomeric silsesquioxane side group silicone oil; and finally carrying out single electron transfer reaction (SET) by vinyl and perfluoroalky iodide in a vinyl polyhedral oligomeric silsesquioxane structure of the side group to prepare the modified fluorine-containing silicone oil. According to the modified fluorine-containing silicone oil, octavinyl polyhedral oligomeric silsesquioxane is added in a side chain of the silicone oil, so that the heat resistance of the silicon oil is improved; by virtue of the fluoroalkylation reaction, the surface tension of the fluorine-containing silicone oil is reduced. The modified fluorine-containing silicone oil is excellent in water and oil repellency and resistance to high temperature; the high-temperature-resistant fluorine-containing silicone oil is mild in reaction conditions, simple and convenient tin preparation process and easily available in raw materials, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a modified fluorine-containing silicone oil and a preparation method, in particular to a cage-type silsesquioxane-containing fluorine-containing silicone oil and a preparation method, belonging to the field of organosilicon material preparation and fluorine-containing organosilicon polymers. Background technique [0002] In recent decades, in terms of material surface treatment, one of the mainstream surface treatment materials is a synthetic polymer material that can adapt to extreme conditions such as high and low temperature and has extreme surface inertness. [0003] Since the surface energy of an object only depends on the interface properties of the solid surface in contact with the outside world, people pay more attention to the study of the interface. To obtain materials with lower surface energy, the most common application at present is to add a fluorine-containing hydrophobic and oleophobic layer on the surface of th...

Claims

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Application Information

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IPC IPC(8): C08G77/385C08G77/22C08G77/10C08G77/06
Inventor 臧雄李战雄蔡露袁艳华戴礼刘安琪
Owner 苏州盛泽科技创业园发展有限公司
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