低共熔溶剂预处理棕榈壳微波热解制备碳纳米管  

Preparation of carbon nanotubes by microwave pyrolysis of palm kernel shell pretreated with deep eutectic solvents

作　　者：翟庆春 柳懿轩 朱志伟 应家琪 刘康 杜兴云 窦金孝[1] ZHAI Qingchun;LIU Yixuan;ZHU Zhiwei;YING Jiaqi;LIU Kang;DU Xingyun;DOU Jinxiao(Key Laboratory for Advanced Coal and Coking Technology of Liaoning Province,University of Science and Technology Liaoning,Anshan Liaoning 114051,China)

机构地区：[1]辽宁科技大学辽宁省先进煤焦化重点实验室,辽宁鞍山114051

出　　处：《化工矿物与加工》2025年第4期51-58,共8页Industrial Minerals & Processing

基　　金：国家自然科学基金项目(22378180);辽宁省教育厅面上项目(JYTMS20230960);辽宁科技大学大学生创新创业训练计划项目(S202410146006)。

摘　　要：木质纤维素生物质是地球上最丰富的可再生生物质,实现其分级转化和高效高值利用,有助于我国“双碳”目标的实现。棕榈壳是一种常见的废弃物,其富含纤维素和木质素等物质。本文以棕榈壳(palm kernel shell,PKS)为原料,使用低共熔溶剂(deep eutectic solvents,DESs)对其进行预处理得到纤维素组分,并利用微波热解装置直接制备碳纳米管。通过BBD(box-behnken design)响应面法优化棕榈壳预处理工艺参数,通过扫描电镜(SEM)、高分辨率透射电镜(HRTEM)、X射线衍射仪(XRD)、拉曼光谱(Raman)、热重分析仪(TGA)等手段对热解产物进行分析。结果表明:在预处理温度为120℃、预处理时间为3 h、氢键受供体摩尔比为1∶5时,木质素的脱除率最高,纤维素收率最高;工艺参数优化结果显示,两两交互影响因素作用对预处理棕榈壳木质素脱除率的影响显著性排序为预处理温度>氢键受供体摩尔比>预处理时间;棕榈壳纤维素通过微波热解可以一步制得结构完整的碳纳米管。As a rich renewable energy source,the graded conversion and efficient high-value utilization of wood cellulose biomass contribute to the achievement of China’s"dual carbon"goals.Palm shells are a common waste material,which is rich in cellulose,lignin and other substances.In this paper,the palm kernel shell(PKS)as the raw material was pretreated with deep eutectic solvents(DESs)to obtain cellulose components,and carbon nanotubes were directly prepared using the microwave pyrolysis device.The pretreatment process parameters of palm shell were optimized by BBD(box Behnken design)response surface methodology,and the pyrolysis products were analyzed by scanning electron microscopy(SEM),high-resolution transmission electron microscopy(HRTEM),X-ray diffraction(XRD),Raman spectroscopy(Raman),thermogravimetric analysis(TGA)and other methods.The results show that when the pretreatment temperature is 120℃,the pretreatment time is 3 h,and the hydrogen bond donor molar ratio was 1∶5,the removal rate of lignin is the highest and the yield of cellulose is the highest.The optimization results of process parameters show that the degree of influence of pairwise interactive influencing factors on the remo-val rate of lignin from pretreated palm shell is ranked as follows:pretreatment temperature>hydrogen bond donor molar ratio>pretreatment time.Palm shell cellulose can be thermally decomposed by microwave to produce struc-turally intact carbon nanotubes in one step.

关 键 词：棕榈壳 碳纳米管 微波热解 低共熔溶剂 木质素 纤维素 预处理 

分 类 号：TB383.1[一般工业技术—材料科学与工程] O613.71[理学—无机化学]