磁性羧甲基壳聚糖微粒结构及性能表征及其用于造纸废水处理研究

ChinaBiotechnology,2010,30(6):65O69*李艳1龙柱1**江华1李海峰2冯菲1(12141222325011)采用反相悬浮法制备改性壳聚糖磁性微粒絮凝剂,并探讨了该絮凝剂对造纸废水的絮凝作用,着重考察了絮凝剂的投入量体系pH值搅拌速度搅拌时间沉降时间对造纸废水中COD去除率的影响结果表明在最佳条件下该絮凝剂对造纸废水的COD去除率可达56.52%,且具有投入量少pH应用范围广絮凝时间和沉降时间短的优点,说明改性壳聚糖磁性微粒作为絮凝剂对造纸废水的处理切实可行改性壳聚糖磁性微粒制浆造纸废水Q819:2010-04-19:2010-04-22*/0(2007BAE48B01)**,:[e-mail],,Fe3O4,[1],[2],[3](CS),,[4],[5],[6];-OH-NH2[7],,,,,,pHFe3O4,,(W/O)Fe3O4,,,11.1(90%,);NH3#H2O();FeCl2#4H2O(,);(,),(,),FeCl3#6H2O,,,,Tween-80,(,):,黒液,后经酸化法脱出木素后得到的制浆废CODcr23353mg/L,pH3.57,,FALA2000104(Boman),KBr,500~4000nm;EV7(VSM,ADE);CSPM4000(AFM,),;H-7650(TEM,);TGA-SDTA851;ChinaBiotechnologyVo.l30No.620105B-1COD;7211.21.2.1改性Fe3O4纳米粒子的制备Fe3O4[8~9],:Fe2++2Fe3++8OH-yFe3O4+4H2O:FeCl3FeCl2#4H2O60e,,1h,3h,,Fe3O41.2.2羧甲基壳聚糖(CMC)的制备5g,45e1h,30%NaOH,2h,60e3h300ml,10%HClpH,,3,60e,[10]1.2.3磁性羧甲基壳聚糖微粒的制备1500r/min(,)(),,,,,,50e1.2.4絮凝实验及分析测试,pH5,5~6100ml,50ml,,,,,,(GB11914-89)[11]CODcr22.113400cm-1O-HN-H;2924cm-1C-H;1635cm-11385cm-1-COO-[12-13];1084cm-1C-O-C;634cm-1586cm-1Fe-O,,1Fig.1FTIRspectraofmodifiedchitosanmagneticparticle2.2TEM22,5~20nm,,,2,,3AFM3,,50nm2.3VSM,4,Ms33.0emu/g,2.45:CODcr,CODcr,16mg,CODcr,56.5%;662010,30(6):,CODcr:,,COD,CODcr;,[14],CODcr,,1L16mg5Fig.5TheeffectofthedosageontheremovingofCODCrRoomtemperature,120r/min,agitationtime:3min,settlingtimeunderanexternalmagneticfield:10min2.5pH6,pH4~9CODcr,50%,H+,pH2.67,120r/min,,CODcr56.5%;,CODcr,,,,,,CODcr67ChinaBiotechnologyVo.l30No.620102.78,3min,,CODcr56.5%;,CODcr3min,CODcr[15]12h,2.89,,1min8Fig.8TheeffectofagitationtimeontheremovingofCODCr(roomtemperature,120r/min,settlingtimeunderanexternalmagneticfield:10min)Fe3O4,,,,,[16],,,9Fig.9TheeffectofsettlingtimeontheremovingofCODCr(roomtemperature,120r/min,agitationtime:3min)3Fe3O4,,Fe3O4,682010,30(6):5~20nm;,Ms33.0emu#g-1CODcr56.52%,pH[1]ZhangJ,MisraRDK.Magneticdrug-targetingcarrierencapsulatedwiththermosensitivesmartpolymer:Core-shellnanoparticlecarrieranddrugreleaseresponse.ActaBiomaterialia,2007,3(6):838-850.[2]GuptaAK,GuptaM.Synthesisandsurfaceengineeringofironoxidenanoparticlesforbiomedicalapplications.Biomaterials,2005,26(18):3995-4021.[3]ChangYC,ChenDH.Preparationandadsorptionpropertiesofmonodispersechitosan-boundFe3O4magneticnanoparticlesforremovalofCu(II)ions.JournalofColloidandInterfaceScience,2005,283(2):446-451.[4]LiBQ,JiaDC,ZhouY,eta.lInsituhybridizationtochitosan/magnetitenanocompositeinducedbythemagneticfield.JournalofMagnetismandMagneticMaterials,2006,306(2):223-227.[5]WuY,GuoJ,YangWL,eta.lPreparationandcharacterizationofchitosanpoly(acrylicacid)polymermagneticmicrospheres.Polymer,2006,47(15):5287-5294.[6]DenkbaEB,KilicayE,BirliksevenC,eta.lMagneticchitosanmicrospheres:preparationandcharacterization.ReactiveandFunctionalPolymers,2002,50(1),225-232.[7]AgnihotriSA,MalliarjunaNN,AminabhaviTM,eta.lRecentadvancesonchitosan-basedmicroandnanoparticlesindrugdelivery.JournalofControlledRelease,2004,100(1):5-28.[8]MassartR,DuboisE,CabuilV,eta.lPreparationandpropertiesofmonodispersemagneticfluids.JournalofMagnetismandMagneticMaterials,1995,149(1-2):1-5.[9],,,..,2003,17(F9):66-68.QingRH,JiangW,LiuHY,eta.l.MaterialsRebiew,2003,17(F9):66-68.[10],..,2008,29(2):201-203.JiSJ,GaoQ.ScienceandTechnologyofFoodIndustry,2008,29(2):201-203.[11].(),GB11914-89.ThestandardofthePeople.sRepublicofChinanationa.lGB11914-89.[12]WuN,Fu,L,SuM,eta.lInteractionoffattyacidmonolayerswithcobaltnanoparticles.NanoLett,2004,4(2):383-386.[13]HuignardA,BuissetteV,LaurentG,eta.lSynthesisandcharacterizationsofYVO4:Eucolloids.ChemistryofMaterials,2002,14(5):2264-2269.[14],,,..,2008,27(3):29-31.WuZH,LuoC,JiangJQ.PaperScienceandTechnology,2008,27(3):29-31.[15],,..,2007,21(2):148-152.ShiZL,WangCS,YaoSH.JournalofShenyangInstituteofChemicalTechnolgy,2007,21(2):148-152.[16],,,.FPAS.,2009,39(2):56-59.GaoF,LiuWH,LiKL.FineChemicalIntermediates,2009,39(2):56-59.PreparationandApplicationofModifiedChitosanMagneticParticleFlocculantinTreatmentforWastewaterofPulpingandPapermakingLIYan1LONGZhu1JIANGHua1LIHa-ifeng2FENGFei1(1KeyLaboratoryofEco-TextilesJiangnanUniversity,MinistryofEducation,Wuxi214122,China)(2ZhejiangDongfangInstituteofTechnology,Wenzhou325011,China)AbstractAnewtypeofflocculantwhichmodifiedchitosanmagneticmicroscopicparticleswerepreparedbyinversesuspensionmethodinLab.Andbasedonthis,theflocculabilityexperimentonpapermakingwastewaterwascarriedout.Relationsofflocculabilitywiththedosageofflocculan,tpH,agitationspeed,agitationtimeandsettlingtimewerediscussed.TheresultsindicatethattheremovingefficiencyforCODCrare56.52%underthebestconditions.Italsohadsomeadvantagessuchaslittledosage,widepHandshortersettlingtime.Soitisagoodmethodfortreatmentofpulpandpaperwastewaterbymodifiedchitosanmagneticmicroscopicparticles.KeywordsModifiedchitosanMagneticparticlesWastewaterofpulpingandpapermaking69