A kind of preparation method of fluorosilicone oil
A technology of fluorosilicone oil and fluoroalkyl iodide, applied in the field of preparation of fluorosilicone oil, can solve the problems of harsh reaction conditions, high equipment requirements and high cost, and achieve the effects of reducing preparation cost, high yield and low cost
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0043] The invention provides a preparation method of fluorosilicone oil, which is characterized in that it comprises the following steps:
[0044] a) after trimethylchlorosilane, dimethyldichlorosilane and methylvinyldichlorosilane are hydrolyzed in the first non-aqueous solvent and water, the resulting hydrolyzate is polymerized under the action of a catalyst to obtain poly Methyl vinyl siloxane;
[0045] b) under the action of an initiator, perform an addition reaction of the polymethylvinylsiloxane and fluoroalkyl iodide in a second solvent to obtain an adduct;
[0046] The fluoroalkyl iodide is selected from C1-C12 fluorine-containing alkyl iodides;
[0047] c) performing a hydrodeiodination reaction of the adduct and a reducing agent in a third solvent to obtain the fluorosilicone oil shown in formula (1);
[0048]
[0049] Among them, m is an integer from 1 to 10000, n is an integer from 1 to 10000; R F It is a C1-C12 fluorine-containing alkyl group.
[0050] In ...
Embodiment 1
[0080] S1: Add 200mL petroleum ether and 200mL water into the reaction flask, cool in an ice-water bath to 0-5°C, slowly add 0.109g (1mmol) trimethylchlorosilane and 2.58g (20mmol) dimethyldichlorosilane dropwise under stirring and 2.82g (20mmol) of methylvinyldichlorosilane, control the temperature of the reaction system to be less than 10°C, and continue to stir for 5 hours after the dropwise addition; then, stand still, separate the lower liquid, and extract twice with 1000mL petroleum ether , the organic phases were combined, washed with water until neutral, dried over anhydrous sodium sulfate, and filtered to remove the solvent to obtain 4.5 g of a hydrolyzate.
[0081]The above hydrolyzate was added to the reaction flask, 0.1 g of trifluoromethanesulfonic acid was added, stirred at room temperature for 1 hour, and then heated to 90° C. for 10 hours to react. Then, cool to room temperature, separate the trifluoromethanesulfonic acid in the lower layer, add 150mL of petrol...
Embodiment 2
[0086] S1: Add 200mL of n-hexane and 200mL of water into the reaction flask, cool in an ice-water bath to 0-5°C, slowly add 0.109g (1mmol) trimethylchlorosilane and 2.58g (20mmol) dimethyldichlorosilane dropwise under stirring and 2.82g (20mmol) of methylvinyldichlorosilane, control the temperature of the reaction system to be less than 10°C, and continue to stir for 5 hours after the dropwise addition; then, let stand, separate the lower liquid, and extract twice with 1000mL n-hexane , the organic phases were combined, washed with water until neutral, dried over anhydrous sodium sulfate, and filtered to remove the solvent to obtain 4.1 g of a hydrolyzate.
[0087] Add the above hydrolyzate into the reaction flask, add 0.1 g of sulfuric acid, stir at room temperature for 1 hour, and raise the temperature to 90° C. for 10 hours to react. Then, cool to room temperature, separate the lower layer of sulfuric acid, add 150mL n-hexane to dissolve the upper layer liquid, wash to neut...
PUM
| Property | Measurement | Unit |
|---|---|---|
| molecular weight distribution | aaaaa | aaaaa |
| molecular weight distribution | aaaaa | aaaaa |
| molecular weight distribution | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More