Synthesis, structural characterization and properties of a cubic octa-n-propylsilsesquioxane inorganic–organic hybrid material

• Published in: Journal of molecular structure 2013-01, Vol.1032 (30), p.29-34
• Main Authors: Liu, Hui, Zhu, Qingzeng, Feng, Lei, Yao, Bingjian, Feng, Shengyu
• Format: Article
• Language: English
• Subjects: acetone; benzene; chloroform; condensation; Crystal structure; Cubic; Diffraction; dimethylformamide; Fourier transform infrared spectroscopy; hexane; isopropyl alcohol; methanol; Methyl alcohol; methylene chloride; n-Propylsilsesquioxane; nitrogen; Nuclear magnetic resonance; nuclear magnetic resonance spectroscopy; pentane; solvents; Sublimate; Synthesis; TGA; Thermogravimetric analysis; thermogravimetry; toluene; Transmission electron microscopy; X-radiation; X-ray diffraction; X-ray single crystal diffraction; X-rays; xylene
• ISSN: 0022-2860; 1872-8014
• DOI: 10.1016/j.molstruc.2012.07.045

► Cubic octa-n-propylsilsesquioxanes was synthesized with a 68.9% yield. ► Soluble in common organic solvents. ► A triclinic system crystal with a P-1 space group. ► Sublimate above 200°C and not to decompose until 524°C under a nitrogen atmosphere. Synthesis, structural characterization and property studies were carried out on cubic octa-n-propylsilsesquioxanes (n-Pr-POSS) in this paper. n-Pr-POSS was synthesized by an acid-catalyzed hydrolytic condensation of n-propyltriethoxysilane with a 68.9% yield. Common organic solvents, such as benzene, chloroform, tetrahydrofuran, diethyl ether, dichloromethane, toluene, cyclohexane, hexane and pentane can be used to dissolve n-Pr-POSS; however, n-Pr-POSS is insoluble or poorly soluble in acetone, dichloroethane, chlorobenzene, dimethylformamide, xylene, methanol, alcohol and isopropanol. The cubic structure and crystal morphology of n-Pr-POSS have been investigated by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), optical microscope, 1H, 13C and 29Si nuclear magnetic resonance (NMR), X-ray single crystal diffraction and X-ray powder diffraction (XRD) methods. Crystalline n-Pr-POSS is a triclinic system crystal with a P-1 space group. Thermogravimetric analysis (TGA) indicates that n-Pr-POSS begins to sublimate above 200°C and does not decompose until 524°C under a nitrogen atmosphere.