刘天赐,杨倩,宋佳慧,孙海东,石海强.预水解协同低共熔溶剂制备芦苇纤维素纳米纤丝的研究[J].中国造纸学报,2023,38(2):43-51 |
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预水解协同低共熔溶剂制备芦苇纤维素纳米纤丝的研究 |
Study on Preparation of Reed CNF by DES Cooperating Pre-hydrolysis |
投稿时间:2022-06-03 |
DOI:10.11981/j.issn.1000-6842.2023.02.43 |
中文关键词: 纤维素纳米纤丝 芦苇 低共熔溶剂 预水解 |
Key Words:cellulose nanofibril reed deep eutectic solvents pre-hydrolysis |
基金项目:国家自然科学基金资助项目(31971608);辽宁省自然科学基金资助项目(2019-ZD-0125);辽宁省“百千万人才工程”A类项目资助;辽宁省高等学校创新人才计划资助项目。 |
作者 | 单位 | 邮编 | 刘天赐* | 大连工业大学轻工与化学工程学院,辽宁省生物质化学与材料重点实验室,辽宁大连,116034 | 116034 | 杨倩 | 大连工业大学轻工与化学工程学院,辽宁省生物质化学与材料重点实验室,辽宁大连,116034 | 116034 | 宋佳慧 | 大连工业大学轻工与化学工程学院,辽宁省生物质化学与材料重点实验室,辽宁大连,116034 | 116034 | 孙海东 | 辽宁盘锦振兴纸业有限公司,辽宁盘锦,124112 | 124112 | 石海强 | 大连工业大学轻工与化学工程学院,辽宁省生物质化学与材料重点实验室,辽宁大连,116034 | 116034 |
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中文摘要: |
采用预水解协同低共熔溶剂法(F-DES)制备芦苇纤维素纳米纤丝(CNF),通过对预水解芦苇得率、化学组分等的分析,探讨较佳预水解工艺,采用红外光谱、扫描电子显微镜、粒径分析、X射线衍射仪分析和热重分析等对预水解处理的芦苇以及芦苇CNF进行了表征。研究结果表明,芦苇预水解的较佳条件为:液比1∶6,预水解温度165 ℃,保温时间50 min。预水解芦苇得率为80.31%,α-纤维素含量为49.62%,预水解处理芦苇纤维素晶型结构未发生变化,保持纤维素Ⅰ型结构。F-DES体系处理预水解芦苇制备CNF的较优工艺条件为:FeCl3·6H2O用量为0.2 mmol/g DES,草酸二水合物/氯化胆碱(Oxd/ChCl)质量比为4∶1,反应时间6 h,温度80 ℃。制备的CNF粒径为200~800 nm,总体呈现均匀的纳米纤丝状,优化条件下制备的CNF中有90%的粒径分布在300~400 nm之间。 |
Abstract: |
Reed cellulose nanofibril (CNF) was prepared by using deep eutectic solvent (F-DES) combined with pre-hydrolysis. The optimum pre-hydrolysis technology was determined by analyzing the yield, extractive, and chemical components of pre-hydrolyzed reed. The pre-hydrolyzed reed and reed CNF were characterized by infrared spectrum, scanning electron microscope, particle size analysis, X-Ray diffraction, and thermogravimetric analysis. The results showed that the optimal conditions for pre-hydrolyzing reed were as follows: liquid ratio of 1∶6, pre-hydrolyzing temperature 165 ℃, and insulation time 50 min. The yield of pre-hydrolyzed reed was 80.31% and α-cellulose content was 49.62%. The crystal structure of reed cellulose did not change after pre-hydrolysis treatment, i.e., the type Ⅰ structure was maintained. The feasible process conditions for preparing CNF from pre-hydrolyzed reed treated by F-DES system were as follows: FeCl3·6H2O dosage of 0.2 mmol/g DES, mass ratio of Oxd/ChCl 4∶1, reaction time 6 h, and temperature 80 ℃. The as-prepared CNF had homogeneous morphology and particle size ranging from 200 to 800 nm, with 90% of them distributed between 300 and 400 nm. |
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