高浓度三氯化铁预处理制纳米纤维素及其性能研究  

Preparation and Properties of Nanocellulose Obtained by Pretreatment of High Concentration Ferric Chloride

作　　者：杨伟胜 冯树 苏阳 刘俊豪 梅泽楷 韩景泉 YANG Weisheng;FENG Shu;SU Yang;LIU Junhao;MEI Zekai;HAN Jingquan(College of Materials Science and Engineering,Nanjing Forestry University,Nanjing 210037,China)

机构地区：[1]南京林业大学材料科学与工程学院,江苏南京210037

出　　处：《林产化学与工业》2024年第5期243-248,共6页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(32371803);江苏省农业自主创新项目(CX(23)3059);大学生实践创新训练计划项目(202410298010Z)。

摘　　要：以漂白桉木浆(BEP)为原料,采用质量分数40%的三氯化铁溶液预处理结合高压均质制备纳米纤维素(CNF)。通过环境扫描电子显微镜(ESEM)、原子力显微镜(AFM)、X射线衍射(XRD)仪、傅里叶变换红外光谱(FT-IR)和热重(TG)分析,对制得CNF的微观形态、尺寸、结晶结构、化学结构和热稳定性进行分析。研究结果表明:质量分数40%的三氯化铁溶液具有强酸性,在110℃的处理温度下,木浆纤维的聚合度(D_(P))从1067急剧下降至160,且水解后纤维样品得率可达75.5%。结合高压均质处理便可获得高度25.1~31.8 nm、长度1~2μm的CNF。与BEP相比,高浓度三氯化铁的水解过程对纤维无定形区进行了有效的破除,使得所制备的CNF的结晶度由63.7%增加至68.7%~71.3%。此外,高浓度三氯化铁预处理并未对纤维结构产生过大影响,CNF表现出较高的热稳定性,最大失重速率温度在343~347℃之间。Cellulose nanofiber(CNF)was prepared from bleached hardwood pulp fiber(BEP)with the pretreatment using 40%mass fraction of ferric chloride solution combined with high-pressure homogenization.The morphology,size,crystal structure,chemical structure and thermal stability of CNF were characterized by environmental scanning electron microscope(ESEM),atomic force microscope(AFM),X-ray diffraction(XRD)analyzer,Fourier transform infrared spectroscopy(FT-IR)and thermogravimetry(TG)analysis.The results showed that a ferric chloride solution with mass fraction of 40%was highly acidic.The polymerization degree of wood pulp fibers reduced drastically from 1067 to approximately 160 at a treatment temperature of 110℃,and the yield of fiber could rate up to 75.5%after hydrolysis.Combined with high-pressure homogenization treatment,CNF with a height of 25.1-31.8 nm and a length of 1-2μm could be obtained.Compared with BEP,the hydrolysis process of high concentration ferric chloride effectively broke the amorphous region of the fiber,so that the crystallinity of the prepared CNF increased from 63.7%to 68.7%-71.3%.In addition,the pretreatment with high-concentration ferric chloride had no significant effect on fiber structure.CNF showed high thermal stability,and the maximum weight loss rate temperature of the obtained CNF ranged from 343 to 347℃.

关 键 词：纳米纤维素 高浓度三氯化铁 水解 性能 

分 类 号：TQ35[化学工程]