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1、针对氧化还原法制备石墨烯产品产率低，纯度不好和还原剂污染环境、能量消耗大等问题的综合性考虑，本文首先以100目的片状石墨为原料，以浓硫酸和浓磷酸为氧化剂，采用止交试验设计合成氧化石墨，探究高锚酸钾添加时间、石墨粉添加时间、石墨与高镒酸钾质量比、浓硫酸和浓磷酸体积比对氧化石墨产率的影响，然后采用超声法，以绿色环保原料抗坏血酸为还原剂述原氧化石墨制备石墨烯，利用SEM、FTIR、XRD及Raman光谱对氧化石翠、石翠烯进行了表征。结果表明：氧化石墨合成的最佳工艺条件是100目片状石墨与高镒酸钾质量比为1:4,高猛酸钾添加
2、时间为47min,石墨粉添加时间为30min,浓硫酸与浓磷酸体积比为8.16:1；石墨原样片层的空间排列非常规整，氧化石墨结构无序度增加，氧原了进入到了石墨层间，生成新的晶体结构，石墨已经被氧化；当氧化石墨被还原成为石墨烯时，某些部位化学键断裂，晶体结构的完整性下降，无序度增加，缺陷增多，说明超声波的剥离作用已经使氧化右墨成为单层片状结构，加入抗坏血酸在超声条件下对英进行还原可以将氧化石墨还原为单层的石墨烯。关键词：氧化还原法；正交设计；氧化石墨；石墨烯AbstractForOxidation-reductionme
3、thodofgrapheneproductspreparedbythelowyield,purityisbadandreductantsuchproblemsasenvironmentalpollutionandenergyconsumptionofacomprehensiveconsideration,thisarticlefirstto100purposeflakegraphiteasrawmaterial,growswithaconcentratedsulfuricacidandphosphoricacidas
4、oxidant,syntheticgraphiteoxidebyorthogonalexperimentdesign,explorethepotassiumpermanganateisaddedtime,graphitepowderaddedtime,qualitythangraphitewiththepotassiumpermanganate,sulfuricacidandconcentratedphosphoricacidvolumeratioontheproductionrateofgraphiteoxide.
5、Andthenusingtheultrasonicmethod,withgreenenvironmentalprotectionrawmaterialVcasreductant,reductivegraphiteoxidepreparationofgraphene.UsingSEM,FTIR,XRDandRamanspectrumofgraphiteandgrapheneoxidewerecharacterized.Resultsindicatethattheoptimumprocessconditionsofgra
6、phiteoxidesynthesisis100meshflakegraphite1g,4gpotassiumpermanganate,potassiumpermanganateisaddedtimewas46.75min,graphitepowdertoaddtimefor30min,sulfuricacidandconcentratedphosphoricacidvolumeratiois8.16:1.Graphite,thesamelayerofspacearrangementisveryneat,disord
7、erincreases,thestructureofgraphiteoxideoxygenintothegraphitelayers,generateanewcrystalstructure，graphitehasbeenoxidized.Whenthereductionofgraphiteoxideasgraphene,somepartsofchemicalbondrupture,integrityofcrystalstructure,thedisorderincreases,defects.Explainultr
8、asonicstrippingeffecthasbeenmadeofgraphiteoxidesingleflakestructure,addingascorbicacidundertheconditionofultrasoniconthereductioncanbegraphiteoxideoxidationforsingle-layergr
