DNBP生产废水的精馏处理研究杨宗政

DNBP112311.3004572.3004513.30027146-DNBPH2SO4DNBP.104℃pH=7R=12.6g/L.COD60mg/L《》DB12/356-2008.DNBPTQ047.9X783.1A1671－024X201103－0051－04StudyonDNBPwastewatertreatmentbydistillationYANGZong-zheng1ZHANGQiang1CHENXiao-ying2，LIYan-ling3，WANGHong-tai11.CollegeofMaterialScienceandChemicalEngineeringTianjinUniversityofScienceandTechnologyTianjin300457China2.TianjinXinyuEnvironmentalProtectionTechnologyCoLtdTianjin300451China3.ChemicalFactorySINOPECTianjinBranchTianjin300271ChinaAbstractInordertosolvethewastewaterpollutionin2-sec-butyl-46-dinitrophenolproductionprocessdistillationwasusedtoisolatetheorganicmatterinwastewaterforthedifferentboilingpointandrecyclethesulfuricacidH2SO4andDNBPfromreactorraffinate.Thebestdistillationexperimentalconditionsareobtainedoverheadtemperatureinnormalpressuredistillationbeing104℃theeffluentbeingadjustedtopH=7refluxratioinsecondnormalpressuredistillationiscontrolledas1alkalicontentbeing2.6g/L.TheCODofeffluentisbelow60mg/LwhichreachesthesecondarydischargestandardsofIntegratedWastewaterDischargeStandardDB12/356-2008ofTianjin.KeywordsDNBPwastewaternormalpressuredistillationazeotrope2010-09-1909ZCKFSH025001974—[e-mail]30320116JOURNALOFTIANJINPOLYTECHNICUNIVERSITYVol.30No.3June201146-DNBP..DNBP、、COD.DNBPDNBP[1].[2]、[3]、[4]、[5-6]、[7]COD.300~500/t..[8].COD、DNBPH2SO4.11.1DNBP.COD20000mg/L≥10000pH≤1.1.30－HP6890/5973..DB-5ms30mm×0.25mm0.25μm50℃2min8℃/min180℃10min.1.0mL/min15∶1EI70eV.332.1.211200mm50mmФ3mmθ1000mm.1.31500mLDNBP.30min30min.1/3.COD.22.12.1.1DNBP1500mL22.220min104℃.1.01%.pH11/3.338℃DNBP332℃H2SO446%H2SO420%2.3DNBPDNBPDNBP..CODpH3.3COD10000mg/L50%pH.2.1.2pH3NaOHpH6.0、6.5、7.0.pHCOD1DNBPTab.1BoilingpointofmaincomponentsinDNBPwastewater/℃DNBP332338862DNBPTab.2MaincomponentsfromDNBPproductionwastewater/min/%17.6082.4922--11.9752.6834--2,5--1,4-17.0241.1144,6--2-35.72164.121Fig.1Schematicdiagramofdistillationapparatus2Fig.2Relationshipbetweenoverheadtemperatureinnormalpressuredistillationanddistillationtime0100200300400105100959085/minT/℃52——33.3CODCOD.180℃COD192mg/LCOD160mg/L.pH.2.22.2.1NaOHpH74.42COD2COD.COD60mg/L.pH400kgNaOH2000/t800/tpH.2.2.2pHpH4、5、6、7、8、92.COD4.4CODCOD689mg/LHNO3NaOHCOD60mg/L.2.2.3.COD5.5COD60mg/LDB12/356-20081COD.2.6kg200/tDNBP12454035302520COD/mg·L-14CODFig.4EffectofdifferentrefluxratiosonCODofsecondarydistillationeffluent33Tab.3Dataanalysisontopproductsinnormalpressuredistillation/minpHCOD/mg·L-1102.311018202.2510638302.259877402.3510356502.4994100.20.60.81.025002000150010005000COD/mg·L-133pHFig.3EffectofrefluxratiosondistillationresultinthreepHcondition0.4pH=6.0pH=6.5pH=7.0，：DNBP4pHTab.4ResultofeffluentondifferentpHconditionspH456789COD/mg·L-15264291168942514853——30.2.3pH1..H2SO4DNBP2.H2SO4.100mLNaOHH2SO4c=d×w×1000/MH2SO4w.dg/mLMg/mol.5.5H2SO41.346%..3DNBP104℃pH=712.6g/L.COD99%.DNBPDNBP.DNBP.[1]．DNBP[J].2008319129-131．[2]．[J].2008284365-369．[3]．[J].2008281265-69.[4]．Fenton[J].200926334-36．[5]．[J].200844229-31．[6]．[J].200622393-100．[7]．/Fenton[J].2009252388-91．[8]．[J].200323444-46.[9]．·[M]．3.20068．5H2SO4Tab.5ComparisononcontentofH2SO4betweenrawwaterandstillageliquidH2SO4/%20460.01.52.02.53.0353025201510COD/mg·L-15CODFig.5CODofeffluentondifferentrefluxratios1.00.554——