王丽珍,李晓天,王俊跃.TEMPO氧化结合高压均质制备向日葵秸皮纤维素纳米纤维[J].中国造纸学报,2025,(2):26-33 本文二维码信息
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TEMPO氧化结合高压均质制备向日葵秸皮纤维素纳米纤维
Preparation of Sunflower Straw Rind Cellulose Nanofibers by TEMPO Oxidation Combined with High-pressure Homogenization
投稿时间:2024-07-13  修订日期:2024-08-06
DOI:10.11981/j.issn.1000-6842.2025.02.26
中文关键词:  向日葵秸皮  纤维素纳米纤维  TEMPO氧化  高压均质
Key Words:sunflower stalk rind  cellulose nanofibrils  TEMPO oxidation  high pressure homogenization
基金项目:自治区直属高校基本科研业务费(JY20250079);内蒙古工业大学科研启动金(BS2025024);自治区自然科学基金(2025MS05090)。
作者单位邮编
王丽珍* 内蒙古工业大学轻工与纺织学院内蒙古呼和浩特010080
南京林业大学江苏南京210037 
210037
李晓天 内蒙古工业大学轻工与纺织学院内蒙古呼和浩特010080 010080
王俊跃* 内蒙古工业大学工程训练教学部 内蒙古呼和浩特010080 010080
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中文摘要:
      以向日葵秸皮为原料,采用TEMPO/NaBr/NaClO氧化体系制备TEMPO氧化纤维素纤维(TOCF),并进一步结合高压均质法获得羧基含量高、粒径尺度小且分散稳定性良好的TEMPO氧化纤维素纳米纤维(TOCNF)。使用透射电子显微镜(TEM)、傅里叶变换红外光谱仪(FT-IR)、X射线衍射仪(XRD)和热重分析仪(TGA)对其进行表征。结果表明,当NaClO用量为10 mmol/g时,TOCF的羧基含量达1.42 mmol/g;经8次高压均质后,TOCNF的长度和粒径显著减小,分布范围分别为100~250 nm和3~7 nm。TOCF的FT-IR谱图表现出明显的—COOH特征吸收峰,而TOCNF未出现新的特征峰,表明高压均质未改变其官能团。TOCF和TOCNF均保留了纤维素I型结晶结构,但与向日葵秸皮综纤维素相比,TOCF、TOCNF的结晶度与热稳定性均有所下降。
Abstract:
      Using sunflower stalk rind as raw material, TEMPO/NaBr/NaClO oxidation system was used to prepare TEMPO oxidized cellulose fibers (TOCF), and further combined with high-pressure homogenization method to obtain TEMPO oxidized cellulose nanofibrils (TOCNF), which featured with high carboxyl content, small particle size and good dispersion stability. The products was characterized using Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), and Thermogravimetric Analysis (TGA). The results showed that when the dosage of NaClO was 10 mmol/g, the carboxyl content of TOCF reached 1.42 mmol/g. After 8 times of high-pressure homogenization, the length and particle size of TOCNF significantly decreased, with distribution ranges of 100~250 nm and 3~7 nm, respectively. The FT-IR spectrum of TOCF showed a clear —COOH characteristic absorption peak, while TOCNF did not show any new characteristic peaks, indicating that high-pressure homogenization did not change its functional groups. Both TOCF and TOCNF retained the type I crystalline structure of cellulose, but compared with sunflower stalk rind holocellulose, the crystallinity and thermal stability of TOCF and TOCNF had decreased.
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