在正硅酸乙酯(TEOS)酸碱两步催化的溶胶-凝胶过程中,加入干燥控制化学添加剂(DCCA)N,N-二甲基甲酰胺(DMF)和三甲基氯硅烷(TMCS)的混合溶液,进行原位疏水改性处理,并结合常压干燥工艺制备了高比表面积的疏水SiO2气凝胶.利用N2物理吸附,全自动X射线衍射仪(XRD),傅立叶变换红外光谱仪(FTIR),扫描电子显微镜(SEM)等对样品的形貌结构进行了表征.实验结果表明,原位疏水改性比非原位疏水改性制备的SiO2气凝胶具有更大的比表面积,可达979m2·g^-1,气凝胶表面存在憎水性基团-CH3,有良好的疏水性.500℃热处理后,气凝胶因失去大量的-CH3基团,由憎水性转为亲水性;800℃高温热处理后,疏水SiO2气凝胶仍处于非晶态,具有良好的热稳定性能.
Using an acid-base two-step catalysis for the hydrolysis of tetraethyl orthosilicate (TEOS), hydrophobic silica aerogel with a high specific surface area was prepared by an in-situ sol-gel process and ambient pressure drying utilizing the introduction of drying control chemical additives (DCCA) N,N-dimethylformamide (DMF) and trimethylchlorosilane (TMCS) to allow for the hydrophobic modification of the sol system. The structure and morphology of these samples were characterized by N2 physical adsorption, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrometry, and scanning electron microscopy (SEM). Results showed that the specific surface area of the hydrophobic silica aerogel modified by this in-situ method was larger than that of an aerogel modified by the ex-situ method. The specific surface area of the former aerogel was up to 979 m2·g-1. The aerogel had a good hydrophobic property because of the hydrophobic group (--CH3) that was linked to the aerogel's surface. After heat treatment at 500 ℃, the aerogel became hydrophilic because it lost most of its hydrophobic groups (--CH3). After heat treatment at high temperature 800 ℃ the hydrophobic silica was still in an amorphous state, which indicated good thermal stability for the hydrophobic silica aerogel.