Asymmetric hydroxyl-containing double deck and trapezoidal oligomeric silsesquioxane and its synthesis method and application
A technology of polysilsesquioxane and synthesis method, applied in the direction of silicon organic compounds, etc., can solve the problems of random distribution of product functional groups, and achieve the effects of simple and easy product purification process, mild reaction conditions and wide application range.
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Embodiment 1
[0025] Example 1: Preparation of asymmetric hydroxyl-containing double deck oligomeric silsesquioxane containing methyl, phenyl and hydrogen
[0026] At -20°C, 10 ml of 1,4-dioxane solution containing 3 g of 1,3-dimethyl-1,3-dichlorodisiloxane was slowly added dropwise to the side containing 3 g In a 50-ml three-necked flask containing phenyl-based double-deck oligomeric silsesquioxane tetrasilanol, 3 g of diethylamine and 10 ml of 1,4-dioxane, the reaction was stirred for 30 minutes and washed with water. The organic layer was neutralized, dried by adding anhydrous sodium sulfate, and vacuum drying to remove the solvent to obtain a white solid with a yield of 78%.
[0027] The infrared spectrum of asymmetric hydroxyl-containing double deck oligomeric silsesquioxane containing methyl, phenyl and hydrogen is shown in figure 1 As shown, the 1H NMR spectrum of an asymmetric hydroxyl-containing double deck oligomeric silsesquioxane containing methyl, phenyl and hydrogen is shown ...
Embodiment 2
[0028] Example 2: Preparation of asymmetric hydroxyl-containing ladder oligomeric silsesquioxane containing methyl, phenyl and hydrogen
[0029] At 60°C, a solution of 2 g of 1,3-dimethyl-1,3-dichlorodisiloxane in 20 ml of tetrahydrofuran was slowly added dropwise to the trans-ring containing 200 g of phenyl pendant. In a 500 ml three-necked flask containing tetrasiloxane tetrasilanol, 2 g of triethylamine and 300 ml of tetrahydrofuran, the reaction was stirred for 8 hours. After the reaction solution was lowered to room temperature, 300 ml of n-hexane was added, and the organic layer was washed with water to medium After drying by adding anhydrous sodium sulfate, the solvent was removed by vacuum drying to obtain a white solid with a yield of 85%.
[0030] The infrared spectrum of asymmetric hydroxyl-containing ladder oligomeric silsesquioxane containing methyl, phenyl and hydrogen is shown in image 3 shown.
Embodiment 3
[0031] Example 3: Preparation of asymmetric hydroxyl-containing double deck oligomeric silsesquioxane containing vinyl, ethyl acrylate and allyl groups
[0032] At a temperature of 90°C, a solution of 16 g of 1,3-divinyl-1,3-diacrylate ethyl ester-1,3-dichlorodisiloxane in 20 ml of methyl isobutyl ketone was slowly dropped Add to a 500 ml three-neck flask containing 100 g of double deck oligomeric silsesquioxane tetrasilanol with allyl side groups, 0.1 g of tetramethylammonium hydroxide and 200 ml of methyl isobutyl ketone , then stirred and reacted for 16 hours, and after cooling to room temperature, the organic layer was washed with water until neutral, dried by adding anhydrous sodium sulfate, and then dried in a vacuum to remove the solvent to obtain a white solid with a yield of 78%.
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