Investigations on the mobility of novel sol–gel processed inorganic–organic hybrid materials
作者:Ekkehard Lindner、Stefan Brugger、Stefan Steinbrecher、Erich Plies、Hermann A. Mayer
DOI:10.1039/b010009i
日期:——
Novel co-condensing agents of the type Râ²Si(OMe)2(CH2)3R2Si(CH2)3Si(OMe)2Râ² 3[Me2Si(C3D0)2]
(3a), R = Me, Râ²Â = Me; 3[Me2Si(C3T0)2]
(3b), R = Me, Râ²Â = OMe; 4[Et2Si(C3D0)2]
(4a), R = Et, Râ²Â = Me; 4[Et2Si(C3T0)2]
(4b),
R = Et, Râ²Â = OMe} were synthesised by hydrosilylation of the corresponding diallyldialkylsilanes 1, 2 with dichloro(methyl)silane and trichlorosilane, respectively, followed by treatment with trimethyl orthoformate. These precursors were solâgel processed with or without PhSi(OMe)3
[Ph(T0)] to give the xerogels X3aâd, X4aâd. The polysiloxane matrices, the degree of condensation and the integrity of the hydrocarbon backbone were investigated by means of solid state NMR spectroscopy (13C, 29Si). To study the polymer dynamics in the dry state 29Si
CP/MAS NMR measurements of relaxation times (T1ÏH) and cross-polarisation parameters (TSiH) were carried out. 1H HR/MAS NMR experiments and T1ÏH measurements in different solvents were undertaken to get information on the mobility of the polymers in suspension. Scanning electron microscopy (SEM) images show the morphology of the polymers and energy dispersive X-ray spectroscopy (EDX) suggests that the distribution of the elements agrees with the applied stoichiometry.
R−Si(OMe)2(CH2)3R2Si(CH2)3Si(OMe)2R−3[Me2Si(C3D0)2] 型新型共缩合剂
(3a), R = Me, R = Me; 3[Me2Si(C3T0)2]
(3b), R = Me, R = OMe; 4[Et2Si(C3D0)2]
(4a), R = Et, R = Me; 4[Et2Si(C3T0)2]
(4b),
R = Et, R = OMe} 通过相应的二烯丙基二烷基硅烷 1、2 分别与二氯(甲基)硅烷和三氯硅烷进行氢化硅烷化,然后用原甲酸三甲酯处理来合成。这些前体经过溶胶凝胶处理,有或没有 PhSi(OMe)3
[Ph(T0)] 得到干凝胶 X3a–d、X4a–d。通过固态核磁共振波谱 (13C, 29Si) 研究了聚硅氧烷基质、缩合度和烃主链的完整性。研究干燥状态下的聚合物动力学 29Si
对弛豫时间 (T1-H) 和交叉极化参数 (TSiH) 进行 CP/MAS NMR 测量。在不同溶剂中进行 1H HR/MAS NMR 实验和 T1ÏH 测量,以获得有关悬浮液中聚合物流动性的信息。扫描电子显微镜 (SEM) 图像显示了聚合物的形态,能量色散 X 射线光谱 (EDX) 表明元素的分布与所应用的化学计量一致。