Polyhedral oligomeric silsesquioxane containing multiple functional groups as well as synthetic method and application of polyhedral oligomeric silsesquioxane
A polysilsesquioxane and synthesis method technology, which is applied in the direction of silicon organic compounds, can solve the problems of limited application range, and achieve the effects of high synthesis efficiency, mild reaction conditions, and wide application range
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Embodiment 1
[0031] Example 1: Preparation of polyhedral oligomeric silsesquioxane containing phenyl, methyl, hydroxyl and hydrogen
[0032] At -10°C, 10 ml of 1,4-dioxane solution containing 3 g of methyldichlorosilane was slowly added dropwise to the incompletely condensed polyhedral oligomeric sesquihedron containing 3 g of phenyl side groups. Siloxane, 3 g of diethylamine and 10 ml of 1,4-dioxane were placed in a 50 ml three-neck flask, then stirred and reacted for 30 minutes, the organic layer was washed with water until neutral, dried by adding anhydrous sodium sulfate, vacuum The solvent was removed by drying to obtain a white solid with a yield of 78%.
[0033] Matrix-assisted time-of-flight mass spectrometry of polyhedral oligomeric silsesquioxanes containing phenyl, methyl, hydroxyl, and hydrogen such as figure 1 As shown, the H NMR spectrum of polyhedral oligomeric silsesquioxane containing phenyl, methyl, hydroxyl and hydrogen is shown as figure 2 shown.
Embodiment 2
[0034] Example 2: Preparation of polyhedral oligomeric silsesquioxane containing hydrogen, methyl, vinyl and hydroxyl
[0035] At 60°C, slowly dropwise add 20 ml of tetrahydrofuran solution containing 2 g of methyl vinyl dichlorosilane to 200 g of incompletely condensed polyhedral oligosilsesquioxane with side groups hydrogen, 2 g of tris Ethylamine and 300 ml of tetrahydrofuran in a 500 ml three-necked flask, then stirred for 8 hours, after the reaction solution dropped to room temperature, added 300 ml of n-hexane, washed the organic layer with water until neutral, added anhydrous sodium sulfate to dry, vacuum The solvent was removed by drying to obtain a white solid with a yield of 65%.
Embodiment 3
[0036] Example 3: Preparation of polyhedral oligomeric silsesquioxane containing epoxy, methyl, vinyl, ethyl acrylate, allyl and hydrogen
[0037] At -20°C, slowly add 20 ml of methyl isobutyl ketone solution containing 16 g of methylvinyl dichlorosilane dropwise to 100 g of incompletely condensed polyhedral oligomerization times with epoxy groups as side groups. In a 500 ml three-neck flask containing semisiloxane, 0.2 g of tetramethylammonium hydroxide and 200 ml of methyl isobutyl ketone, the reaction was stirred for 3 hours, and the reaction solution was slowly raised to 90° C. A solution of 10 ml of methyl isobutyl ketone in ester allyl iodosilane was slowly added dropwise to the reaction liquid, then stirred for 18 hours, and after cooling down to room temperature, the organic layer was washed with water until neutral, and dried by adding anhydrous sodium sulfate Finally, the solvent was removed by vacuum drying to obtain a white solid with a yield of 80%.
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