本文以玉米秸秆为原料,通过氢氧化钠预处理、TEMPO/NaBr/NaClO氧化体系氧化及高压均质制备纳米纤维素。利用光学显微镜、透射电镜、傅立叶红外光谱、X-射线衍射和热失重分析对玉米秸秆纳米纤维素的形态结构、化学结构、结晶性能和热稳定性进行表征和分析。结果表明,制备的玉米秸秆纳米纤维素直径大约为4~7nm,长度大约为200~500nm,结晶度为61.97%。玉米秸秆经碱预处理及TEMPO氧化后,半纤维素和木质素的脱除效果显著,而纤维素晶形没有发生变化。 In this paper, corn stalks as raw materials, sodium hydroxide pretreatment, TEMPO / NaBr / NaClO oxidation system and high pressure homogenization of nano-cellulose. The morphology, chemical structure, crystallinity and thermal stability of corn stalk nanocellulose were characterized and characterized by optical microscope, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction and thermogravimetric analysis. The results showed that the diameter of cornstarch nanocellulose was about 4 ~ 7nm, the length was about 200 ~ 500nm and the crystallinity was 61.97%. Corn stalks pretreated by alkali and TEMPO oxidation, hemicellulose and lignin removal effect was significant, while the cellulose crystal form did not change.