改性木薯淀粉的制备及其对焦化废水絮凝效果研究官挺

(),29,4,24-28,200912JournalofBaojiUniversityofArtsandSciences(NaturalScience),Vol.29,No.4,pp.24-28,Dec.2009＊官　挺,董国文,王仁章,蓝华远(,365004)　:　合成可生物降解的炼焦废水絮凝剂-羧甲基淀粉(CMS),并对其絮凝效果进行研究。　用ClCH2COOH对木薯淀粉(St)进行改性,采用乙醇作为溶剂,分两步合成CMS。　实验结果表明,改性木薯淀粉较佳制备条件:nSt(M=162)∶nClCH2COOH=1∶1,nNaOH∶n(ClCH2COOH)=2.5∶1,碱化温度35℃,醚化温度50℃。获得改性木薯淀粉处理焦化废水工艺条件,在淀粉取代度为0.37,投入量为50g/L废水,反应温度为40℃,搅拌时间为10min,静置时间为30min时,处理效果最好,对焦化废水浊度去除率高达79.5%以上。　改性木薯淀粉对焦化废水浊度有明显降低效果,但用量大(50kg/m3废水)和对于废水中的CODCr去除率低依然需要深入研究。:羧甲基淀粉;取代度;木薯;絮凝效果:O636.12;O631.32　　:A　　:1007-1261(2009)04-0024-05StudyonthepreparationofmodifiedcassavastarchanditsflocculationeffectoncokingwastewaterGUANTing,DONGGuo-wen,WANGRen-zhang,LANHua-yuan(DepartmentofChemicalandBiologicalEngineering,SanmingCollege,Sanming365004,Fujian,China)Abstract:Aim　Toprepareanon-toxicandbiodegradableflocculant-carboxymethylstarch(CMS)-totreatthecokingwastewaterandanalyzeitsflocculationeffect.Methods　Chloroaceticacidisusedtomodifycassavastarch(St),thencarboxymethylstarch(CMS)issynthesizedintwostepsbyusingethanolassolvent.Results　TheexperimentalresultsshowedthattheoptimumconditionsofCMSsynthesisareasfollows:nSt∶nClCH2COOH=1∶1,nNaOH:nClCH2COOH=2.5∶1,alkalizationtempera-ture35℃,etherificationtemperature50℃,thedegreeofsubstitutionofmodifiedcassavastarchwas0.37.Theprocessofcokingwastewatertreatmentwasalsoinvestigated,thebestresultsofover79.5%turbidityremovalratewasobtainedwiththemodifiedcassavastarch(50g/Lwastewater)atreactiontemperature40℃,stirringtime10minandthenstandingtime30min.Conclusion　AlthoughmodifiedcassavastarchhastheobservablepropertiesofreducingtheturbidityandCODCrofthecokingwastewater,itslargeconsumption(50kg/m3wastewater)andlessremovalrateofCODCrwillrequirefurtherstudy.Keywords:carboxymethylstarch;degreeofsubstitution(DS);cassavastarch;flocculation　　(CMS),。(CMC),CMSCMC,CMSCMC,[1,2]。CMS,,,,＊:2009-08-07,:2009-09-08.:2008(ZL0810/CS);(B0706/Q):(1981-),,,,,:.E-mail:[e-mail]:10.13467/j.cnki.jbuns.2009.04.009,,、[3～8]。,,,、pH,,、[9～12]。,CMS,,,,。,CMS,、、。CMS、,“”,。1　1.1　实验材料与仪器:(,),(“”),NaOH(AR,),ClCH2COOH(AR,),(AR,),(AR,),(AR,),(AR),(AR),(CR,),(AR),。:(AVATAR360FITR,Nicolet),SGZ-(),ZH-1B(),JB90-D(),SZCL-Z()。1.2　制备原理α-1,4α-1,6,C-2、C-3、C-6。,C-3,,C-2C-6,1。CH2ClCOOH,2,(degreeofsub-stitution,DS)。DS,[13～18]。1　Fig.1　EtherificationreactionCMS:∶Starch—OH+NaOH※Starch—ONa+H2O:Starch—ONa+ClCH2COONaNaOHStarch—OCH2COONa+NaCl,[19]:CH2ClCOOH+2NaOHHOCH2COONa+NaCl+H2O1.3　CMS的合成:、NaOH、,,(T1)。:,(T2),,ClCH2COOH,ClCH2COOH,45min,1h。CMS:pH6.5～7.0,,95%,,CMS。1.4　产品测试DS:DS,(AGU)。[20,21]DS。:AVATAR360FITR。2　2.1　木薯羧甲基淀粉的红外光谱分析AVATAR360FITR。23。225　4　　3424.15cm-1—OH,1157.63～1081.42cm-1,929.16、860.42、765.51cm-1。31611.72、1421.93、1367.46cm-1—COO,,。2　Fig.2　Infraredspectraofcassavastarch3　CMSFig.3　InfraredspectraofcassavaCMS2.2　反应条件对DS的影响2.2.1　碱用量对DS的影响,,ClCH2COOH。nClCHCOOH=0.10mol,:nSt=0.10mol,35℃,50℃。4。4,nNaOH∶nSt=2.5∶1,DS,,,,,。,,,ClCH2COOH,DS,。4　DSFig.4　InfluenceofNaOHontheproductDS2.2.2　氯乙酸用量对产品DS的影响,ClCH2COOH,,,DS。nClCH2COOH∶nSt:0.75～1.10,:30℃,50℃,5。5　ClCH2COOHDSFig.5　InfluenceofchloroacetateontheproductDS5,DSnClCH2COOH∶nSt。,,,,NaOH,DS。2.2.3　反应温度对DS的影响,,,,ClCH2COOH,CMS。,DSCMS,。,。62～84℃[22],30～60℃。(1)DS,26()2009　。,,,,。6　DSFig.6InfluenceofalkalizationtemperatureontheproductDS6,nClCH2COOH∶nSt=1∶1,35℃,CMS。,、DS。(2)DS,CH2ClCOOHNaOH。CMS,。7　DSFig.7　InfluenceofetherificationtemperatureontheproductDS7,,DS,、。,50℃。2.3　絮凝实验及其结果2.3.1　絮凝实验100.0mL“”(130NTU),1L。20.0mL,,(T)10min30min,,COD,。2.3.2　絮凝实验结果1)DS0.10gDS100.00mL,25℃10min,30min8。8　DSFig.8　InfluenceoftheproductDSontheflocculatingeffect8,DS,,COD。CODDS0.37,,,DSCOD。2)DS0.370.050g,0.070g,0.090g,0.110g,0.130g,0.150g100.00mL,25℃10min,30min,CODCr,9。9　Fig.9　Influenceoftheamountofstarchontheflocculatingeffect9,,COD,100mg,,,,。3)0.10gDS0.37100.0mL,10min,30min,CODCr,10。10,DS,27　4　　,,COD,30℃。10　Fig.10　Influenceoftemperatureontheflocculatingeffect3　(1),NaOH,,,DS0.50,CMS。CMS:nSt(M=162)∶nClCH2COOH=1∶1,nNaOH∶nClCH2COOH=2.5∶1,35℃,50℃。(2)“”,,79.5%,DS0.37,0.10g(2mL),40℃,10min,30min;CODCr,CODCr24.4%。(3),(50kg/m3)CODCr。:[1]　.[J].,2002,5(2):21-24.[2]　XULi-hong,ZHANGBen-shan,YANGLian-sheng.etal.Crystallinestructurechangesoftapiocastarchgranulebyalcoholic-alkalinetreatment[J].NatProdResDev,2007,19:25-28.[3]　,,.[J].,2008,16(17):23-26.[4]　,,,.[J].,2005(1):180-181.[5]　KasineeHemvichain,PhiriyatornSuwanmala,Ma-nitSonsuk.Preparationofcross-linkedcarboxym-ethylcassavastarchfortheadsorptionofheavymetalions[A].31stCongressonScienceandTechnologyofThailandatSuranareeUniversityofTechnology,18-20October2005.[6]　OrnanongSKittipongpatana,SiripornBurapadaja,NisitKittipongpatana.Carboxymethylmungbeanstarchasanewpharmaceuticalgellingagentfortopi-calpreparation[J].DrugDevelopmentandIndustrialPharmacy,2009,35(1):34-42.[7]　YAOJie,CHENWen-ren,RobbertMManurung,etal.Exploratorystudiesonthecarboxymethylationofcassavastarchinwater-miscibleorganicmedia[J].Starch,2004,56:100-107.[8]　MohammadRezaSaboktakin,AbelMaharramov,Mo-hammadAliRamazanov,etal.Modificationofcarboxy-methylstarchasnanocarriersfororaldrugdelivery[J].NatureandScience,2007,5(3):30-36.[