稀碱-球磨协同制备菠萝皮渣纤维素纳米纤丝及其结构表征  

Preparation and characterization of pineapple peel cellulose nanofibrils by dilute alkali-ball milling synergistic method

作　　者：包含笑 胡菽翰 黄越 吕天艺 张宇昊[1,3,4] 余永 陈海 戴宏杰 BAO Hanxiao;HU Shuhan;HUANG Yue;LYU Tianyi;ZHANG Yuhao;YU Yong;CHEN Hai;DAI Hongjie(College of Food Science,Southwest University,Chongqing 400715,China;Chongqing Sericulture Science and Technology Research Institute,Chongqing 400700,China;National Demonstration Center for Experimental Food Science and Technology Education(Southwest University),Chongqing 400715,China;Chongqing Key Laboratory of Speciality Food Co-Built by Sichuan and Chongqing(Southwest University),Chongqing 400715,China)

机构地区：[1]西南大学食品科学学院,重庆400715 [2]重庆市蚕业科学技术研究院,重庆400700 [3]食品科学与工程国家级实验教学示范中心(西南大学),重庆400715 [4]川渝共建特色食品重庆市重点实验室(西南大学),重庆400715

出　　处：《食品与发酵工业》2023年第10期64-70,77,共8页Food and Fermentation Industries

基　　金：国家自然科学基金项目(31901683);西南大学大学生创新创业训练计划项目(S202210635296);中央高校基本科研业务费专项资金资助(SWU-KT22046);重庆市自然科学基金面上项目(cstc2020jcyj-msxm1875)。

摘　　要：以菠萝皮渣为原料,不同质量分数(0%~5%)NaOH溶液为湿磨介质,通过机械球磨法制备菠萝皮渣纤维素纳米纤丝(pineapple peel cellulose nanofibrils,PCNF),利用傅里叶变换红外光谱(Fourier transform infrared spectroscopy,FTIR)、X射线衍射(X-ray diffraction,XRD)、X射线光电子能谱(X-ray photoelectron spectroscopy,XPS)、原子力显微镜(atomic force microscope,AFM)、热重分析仪和流变仪等对PCNF进行结构表征。结果表明,随着NaOH溶液浓度的增加,菠萝皮渣中的非纤维组分(木质素和半纤维素)和纤维素中的无定形区域逐渐被除去,PCNF得率降低,但结晶度和纤维素纯度逐渐增加。相比于单一球磨处理样品(PCNF-0%),稀碱-球磨处理未改变纤维素的晶体结构,但促进了原料解纤和纳米化,改善了PCNF形貌和网络结构,导致PCNF的黏度和模量均有所增加,表现出剪切变稀和弹性凝胶行为。当前研究通过不同NaOH溶液质量分数有效调控球磨制备的PCNF结构,为果蔬加工余渣的直接纳米化提供简易途径。Using pineapple peel as raw material and sodium hydroxide(NaOH)solution with different mass fractions(0%-5%)as wet grinding medium,pineapple peel cellulose nanofibrils(PCNF)were prepared by mechanical ball milling.The obtained PCNF was characterized by Fourier transform infrared spectroscopy(FTIR),X-ray diffraction(XRD),X-ray photoelectron spectroscopy(XPS),atomic force microscope(AFM),thermal gravimeter,and rheometer.Results showed that with the increase of NaOH solution concentration,the non-fibrous components(lignin and hemicellulose)in pineapple peel and the amorphous regions in cellulose were gradually removed,the yield of PCNF decreased,but the crystallinity and cellulose purity of PCNF increased gradually.Compared with the single ball-milled sample(PCNF-0%),the dilute alkali-ball-milling treatment did not change the crystal structure of cellulose but promoted the defibrillation and nanocrystallization process.The morphology and network structure of PCNF were also improved which resulted in the increase of viscosity and moduli,exhibiting a typical shear thinning and elastic gel behavior.The current study proved that the structure of PCNF could be effectively controlled by ball milling with different NaOH solution concentrations,which provided an easy approach for the direct nanocrystallization of fruit and vegetable processing residues.

关 键 词：菠萝皮渣 纳米纤维素 球磨 NAOH 结构 

分 类 号：TS209[轻工技术与工程—食品科学] TQ352.79[轻工技术与工程—食品科学与工程]