摘要
In the selected experimental conditions, firstly, the branched products with functional groups, N-（2-hydroxylpropylphenylether） （3-aminopropyl） triethoxysilane （APES-PGE, containing one hydroxyl group） and N-[di（2-hydroxylpropylphenylether）]（3-aminopropyl） triethoxysilane （APES-PGE2, containing two hydroxyl groups）, were synthesized by reacting 1 mole of （3-aminopropyl）triethoxysilane （APES） with 2 mole of phenylglycidylether （PGE）. Then the hydrolytic condensation of APES-PGE and APES-PGE2 was performed by dissolving 1 g of the corresponding silane in 1.5 ml tetrahydrofuran （THF）, adding water and eventually a catalyst （molar ratios: [H2O]/Si=3, [NaOH]/Si=0.05）, and heating at 50 ℃ for 24 h, allowing continuous evaporation of volatiles. The final products with branches containing hydroxyl groups were polyhedral oligomeric silsesquioxanes （POSS）. The products from two reactions were characterized by standard spectroscopic techniques, gel partition chromatography （GPC）, Fourier-transformed infrared spectroscopy （FTIR） and matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry （UV-MALDI-TOF MS）. Additionally, a narrow mass distribution of multifunctionalized POSS was shown by UV-MALDI-TOF MS and assignments of the MS peaks.
In the selected experimental conditions, firstly, the branched products with functional groups, N-(2-hydroxylpropylphenylether) (3-aminopropyl) triethoxysilane (APES-PGE, containing one hydroxyl group) and N-[di(2-hydroxylpropylphenylether)](3-aminopropyl) triethoxysilane (APES-PGE_2, containing two hydroxyl groups), were synthesized by reacting 1 mole of (3-aminopropyl)triethoxysilane (APES) with 2 mole of phenylglycidylether (PGE). Then the hydrolytic condensation of APES-PGE and APES-PGE_2 was performed by dissolving 1 g of the corresponding silane in 1.5 ml tetrahydrofuran (THF), adding water and eventually a catalyst (molar ratios: [H_2O]/Si=3, [NaOH]/Si=0.05), and heating at 50 ℃ for 24 h, allowing continuous evaporation of volatiles. The final products with branches containing hydroxyl groups were polyhedral oligomeric silsesquioxanes (POSS). The products from two reactions were characterized by standard spectroscopic techniques, gel partition chromatography (GPC), Fourier-transformed infrared spectroscopy (FTIR) and matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS). Additionally, a narrow mass distribution of multifunctionalized POSS was shown by UV-MALDI-TOF MS and assignments of the MS peaks.
基金
SponsoredbytheFoundationsoftheKeyScience&TechnologyandInternationalCooperationProjectionsofHeilongjiangProvince(GrantNo.GB01A2060andWB02104).
