高比表面积聚丙烯腈基炭微球的制备与正交实验分析  

Optimization of the preparation conditions of KOH-activated,PAN-based carbon ellipsoids by orthogonal experimental analysis

作　　者：刘沅明 秦显营 张少琼 张哲旭 康飞宇 李宝华 LIU Yuan-ming;QIN Xian-ying;ZHANG Shao-qiong;ZHANG Zhe-xu;KANG Fei-yu;LI Bao-hua(Engineering Laboratory for Next Generation Power and Energy Storage Batteries,Engineering Laboratory for Functionalized Carbon Materials,Shenzhen International Graduate School,Tsinghua University,Shenzhen 518055,China;School of Materials Science and Engineering,Tsinghua University,Beijing 100084,China;Shenzhen Geim Graphene Center,Shenzhen 518055,China)

机构地区：[1]清华大学深圳国际研究生院下一代动力与储能电池工程实验室,炭功能材料工程实验室,广东深圳518055 [2]清华大学材料学院,先进材料教育部重点实验室,北京100084 [3]深圳盖姆石墨烯中心,广东深圳518055

出　　处：《新型炭材料》2020年第2期131-139,共9页New Carbon Materials

基　　金：国家重点基础研究发展计划(2014CB932400);国家自然基金联合基金(U1401243);国家自然科学基金(51232005);深圳科技计划(JCYJ20150529164918735,KQJSCX20160226191136,JCYJ20170412170911187);广东省科技计划(2015TX01N011).

摘　　要：本研究优化了制备高比表面积聚丙烯腈基多孔炭微球的KOH化学活化工艺,并系统讨论了活化条件对炭微球的孔体积和平均孔径的影响。活化条件的优化原理基于9个正交实验,主要讨论了活化温度、恒温时间以及碱碳质量比3个因素对比表面积的影响与显著性。极差分析和方差分析表明,3个因素对比表面积均具有高度显著的影响,且三者的影响程度有如下关系:活化温度>恒温时间>碱碳比。最佳活化工艺为:活化温度800℃,恒温时间4 h,碱碳比4∶1。由最佳活化工艺制备的聚丙烯腈基多孔炭微球的比表面积可由活化前的463 m^2g^-1显著提高至2517 m^2g^-1。The optimal preparation conditions for activated carbons from polyacrolynitrile ellipsoid powder by KOH activation were investigated by orthogonal experimental analysis.Results indicate that the activation temperature,holding time,KOH/carbon mass ratio all have a significant impact on the specific surface area,but a small impact on the total pore volume and mean pore size.The importance of factors determining(a)specific surface area are activation temperature>activation time>KOH/carbon mass ratio,(b)total pore volume are activation temperature>KOH/carbon mass ratio>activation time,and(c)the mean pore size are activation time>KOH/carbon mass ratio>activation temperature.The optimal combination of conditions(activation temperature of 800℃,holding time of 4 h and KOH/carbon mass ratio of 4∶1)from orthogonal experimental analysis was validated experimentally.Under these conditions the specific surface area,total pore volume and mean pore size of the PAN-based porous carbon reached 2517 m^2g^-1,1.07 cm^3 g^-1 and 1.70 nm,respectively.

关 键 词：多孔炭 KOH活化 比表面积 正交实验 

分 类 号：TQ127.11[化学工程—无机化工]