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以毛竹为原料，高压均质法制备纳米纤丝化纤维素（NFC），再采用溶胶―凝胶法制备NFC/二氧化硅（SiO2）气凝胶。采用傅里叶变换红外光谱（FTIR）、X射线衍射（XRD）、扫描电子显微镜（SEM）、能谱（EDS）等对其进行表征，通过改变正硅酸乙酯/无水乙醇的体积比获得样品微观形貌较佳的反应工艺条件，并采用十八烷基三氯硅烷的正己烷溶液对NFC/SiO2气凝胶进行疏水改性，用接触角测量仪测试改性NFC/SiO2气凝胶的疏水性能。研究结果表明NFC/SiO2气凝胶在正硅酸乙酯/无水乙醇体积比为1.25%时，二氧化硅复合效率高，且所获得的气凝胶形貌较好，二氧化硅以颗粒的形式附着在纳米纤丝化纤维素表面。改性NFC/SiO2气凝胶接触角为132°，达到疏水状态。“,”Nanofibrillated cellulose (NFC) was prepared by high pressure homogenization methodwith Phyllostachys heterocycla cv. Pubescens as raw material. NFC/SiO2 aerogel was prepared by sol-gel method. NFC/SiO2 aerogel was respectively characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy spectrum (EDS). Reaction process condition of better micromorphology of sample was obtained by changing the volume ratio of tetraethoxysilane /anhydrous ethanol. NFC/SiO2 composite aerogel was hydrophobic modified with hexane solution of octadecyl trichlorosilane, and its hydrophobic property was measured by contact angel measuring instrument. The results showed that better micromorphology of NFC/SiO2aerogel was obtained when tetraethoxysilane/anhydrous ethanol volume ratio was 1.25%, and SiO2could composite by higher efficiency and in the form of particles attached on the surface of cellulose nanofibrils. Contact angel of modified NFC/SiO2 aerogels was 132o, and its hydrophobic state was reached.