石墨基炭材料的制备及其性能  

Preparation and Properties of Graphite-Based Carbon Materials

作　　者：李翔宇[1] 李学琴[2,3] 李阿良 段喜鑫[1] 雷廷宙[3,4] 时君友[1] Li Xiangyu;Li Xueqin;Li Aliang;Duan Xixin;Lei Tingzhou;Shi Junyou(Jilin Province Key Laboratory of Wooden Material Science and Engineering,Beihua University,Jilin 132013,China;Energy Research Institute Co.Ltd.of Henan Academy of Sciences,Zhengzhou 450008,China;Key Biomass Energy Lab of Henan Province,Zhengzhou 450008,China;Henan Academy of Science,Zhengzhou 450008,China)

机构地区：[1]吉林省木质材料科学与工程重点实验室(北华大学),吉林吉林132013 [2]河南省科学院能源研究所有限公司,河南郑州450008 [3]河南省生物质能源重点实验室,河南郑州450008 [4]河南省科学院,河南郑州450008

出　　处：《北华大学学报（自然科学版）》2019年第5期572-579,共8页Journal of Beihua University（Natural Science）

基　　金：吉林省科技厅重大招标项目(20170203001SF);吉林省科技发展计划自然科学基金项目(20190201277JC);吉林市科技创新发展计划校城融合科技创新项目(201830811);河南省科技攻关计划项目(172102410030);河南省科学院基本科研经费项目

摘　　要：以天然鳞片石墨为原料,高锰酸钾(KMnO4)、浓硫酸(H2SO4)、过氧化氢(H2O2)、乙酸(CH3COOH)为氧化插层体系,采用化学氧化法制备石墨基炭材料.采用7因素3水平正交试验L18(3^7)研究不同氧化插层体系配比对石墨基炭材料膨胀体积的影响;通过拉曼光谱(RSM)、扫描电镜(SEM)、比表面积及孔径测定仪(BET)表征石墨基炭材料的性能.结果表明:当氧化插层体系配比为m(KMnO4(g))∶V(H2SO4(mL))∶V(H2O2(mL))∶V(CH3COOH(mL))=1∶10∶2∶2时,在40℃恒温水浴下搅拌60min,80℃下干燥4h制备得到可膨胀石墨;然后,在700℃下高温膨胀得到石墨基炭材料.在该条件下得到的石墨基炭材料的最大膨胀体积为230mL/g.经氧化处理过的石墨高温膨胀后石墨层结构发生了明显变化,无序度增加,结晶度减小;石墨基炭材料的外观蓬松,呈卷曲状,层间孔隙大小明显;最大吸附量可达到75.9cm^2/g,具有较好的吸附性能;最大孔隙结构直径为369.10nm,具有发达的孔隙结构.本研究成果可为石墨基炭材料的制备提供方法和应用依据.Graphite-based carbon was prepared by chemical oxidation with natural flake graphite as raw material,KMnO 4,H2SO4,H2O2,CH3COOH as oxidation intercalation system.The effects of different ratios of oxidation intercalation system on the expansion volume of graphite-based carbon materials were optimized by orthogonal experiment L18(3^7)with 7 factors and 3 levels.The properties of graphite-based carbon materials were characterized by Raman spectroscopy(RSM),scanning electron microscopy(SEM),specific surface area and pore size measurement(BET).The results showed that:when the ratio of oxidation intercalation system was m(KMnO 4(g))∶V(H2SO4(mL))∶V(H2O2(mL))∶V(CH3COOH(mL))for 1∶10∶2∶2,stir 60 min under 40℃constant temperature,dry 4 h under 80℃preparation for expandable graphite;and then to obtain graphite-based carbon material under 700℃high temperature expansion.Under this condition,the maximum expansion volume of graphite-based carbon material was 230mL/g.The structure of the graphite layer after the oxidation treatment of the graphite was obviously changed,the disorder degree increased and the crystallinity reduced;the appearance of the graphite-based carbon material is curled and the pore size of the interlayer is obvious;the maximum adsorption capacity can reach 75.9 cm^2/g and has a good adsorption performance;the largest pore structure diameter is 369.10 nm and has a developed pore structure.This study can provide method and application basis for the preparation of the graphite-based carbon material.

关 键 词：石墨 化学氧化法 不同氧化插层体系 石墨基炭材料 

分 类 号：TQ127.1[化学工程—无机化工]