英文有机化学实验 水蒸汽蒸馏与萃取与洗涤课件

有机化学实验ExperimentalOrganicChemistry英文有机化学实验水蒸汽蒸馏与萃取与洗涤课件Steamdistillation1.Purpose1.1StudytheprincipleandmethodsofSteamDistillationusedforpurifingorganicliquids.1.2Graspthetechniquesofsteamdistillation.2.PrincipleSteamdistillation,oneoftheimmiscible（不溶的）phasesbeingwater,isoneofthemostcommonlyusedmethodsofseparatingandpurifyingliquids.Inthismethodsteamispassedintotheimmiscibleandvolatileliquidinthedistillationflask,andthenthewaterandorganiccompoundco-distill（共沸）,condenseinthecondenser,andarecollectedinthenormalway.Accordingtothelawofpartialpressure,thetotalvaporpressure（蒸气压）abovethemixtureisthesumofthepartialpressuresofthepureindividualcomponents.Steamdistillation1.Purpose1.BpIsthevaporpressureoftheimmiscibleorganiccompound.Inthedistillate（馏出液）,theweightrationoforganiccompoundmBandmH2Ocanbeexpressedasinequation:=BpIsthevaporpressureoftheSteamdistillationisapplicabletothefollowingsituations:Ahighboiling-pointorganiccompoundwhichdecomposeatitsboilingpoint.Amixturecontaininginorganicsaltsorotherorganicsolids,notsuitablefordistillation,filtraionandextraction.Amixturecontainglargeamountsofresin-likenearlyintractablesubstancesornonvolatileimpuritieswhichishardtoisolateorpurifyinanyotherway.SteamdistillationisapplicabInorderforsteamdistillationtobefeasible,thesubstancestobepurifiedshouldhavethesecharacteristics:Insolubleorimmiscibleinwater.Noreactionwithwaterwhenco-boiling.Havingacertainvaporpressureat100℃,>665PaInorderforsteamdistillatio3.ProcedureFigure1TypicalApparatusforsteamdistillation图1水蒸气蒸馏装置3.ProcedureFigure1TypicalApBoingchipsOne–third

BoingchipsOne–thirdNOTESInordertoavoidfillingwithcondensedwaterinthethree-neckflaskduringdistillation,heattheflaskwithasmallflametomaketheon-goingdistillationproceedmorequickly.Beforeendthesteamdistillation,opentheTtubeclampfirst,thenremovetheheatsource,disassembletheapparatus,inturn.Avoidlettingtheliquidformtheflaskbackupintothesteamline.NOTESInordertoavoidfilling0.16(4℃)2.8(75℃)6.6(98℃)2.6Solubility水中溶解度/g/100g258（分解）131.5b.p.沸点/℃0.11531.8vapourpressureat100℃100℃时蒸气压/kPasalicylicacid水杨酸isopentanol异戊醇Organiccompound有机物名称Separateisopentanol(异戊醇)andsalicylicacid(水杨酸)mixtureIsopentanolinsolubleorimmiscibleinwater.Isopentanol(异戊醇)andsalicylicacid(水杨酸)noreactionwithwaterwhencoboiling.Isopentanolinsolublehavingacertainvapourpressureat100℃Theprincipleofisopentanol(异戊醇)andsalicylicacid(水杨酸)mixturecanbeseparatebysteamdistillation:0.16(4℃)2.6Solubility水中溶解度/g/productiontest产品检验:①salicylicacidtest水杨酸的检验10d0.1％FeCl3Observablephenomena!!!10dsolutionproductiontest产品检验:①salicyl②isopentanoltest异戊醇的检验10dsolution10d5％K2Cr2O75d16％H2SO4Observablephenomena!!!②isopentanoltest异戊醇的检验10dsSolventextractionandsolutionwashing1.Purpose1.2Learnhowtochoosesuitablesolvent.2.Principle1.1StudytheprincipleandmethodsofSolventextractionandsolutionwashing.Solventextractionisatechniquefrequentlyusedintheorganicchemistrylaboratorytoseparateorisolateadesiredspeciesfromamixtureofcompoundsorfromimpurities.Substancesforextractionusuallyaresolidorliquid.Solutionwashingisthereverseprocessofsolventextraction.Usuallyitisperformedinthecaseofimpuritiesinasolutionthatcanbeextractedbyanotherimmisciblesolvent,whichhasasmallsolubilitytothedesiredsubstance.SolventextractionandsolutioTheapparatusforextractionandsolutionwashingfromliquidiscalledseparatoryfunnel,anditsuseisoneoftheessentialoperationsfororganicchemistryexperiments.Figure1Separatoryfunnel（分液漏斗）Thereathreekindsofseparatoryfunnel-spherical(球形）,subulate（锥形的）andpear（梨形）forms.Inorganicexperiments,aseparatoryfunnelismainlyappliedtothisareas:Separatetwokindsofliquidwhichareimmiscibleanddonotreactwitheachother.Extractaceratincomponentfromasolutiom.Washaliquidproductorthesolutionofasolidproductwithwater,aqueousalkalineoracidicsolution.Adddropwiseacertainreagent(usedasadrippingfunnle)Separatoryfunnelsareveryexpensiveandborkeneasily.NeverpropThefunnelonitsstem,butsupportitonaring,afunnelsupport,orsomeotherstablesupport.TheapparatusforextractionaFigure2Ventingseparatoryfunnel（分液漏斗的振摇与放气）Figure2Ventingseparatoryfu英文有机化学实验水蒸汽蒸馏与萃取与洗涤课件Theextractionprinciplecanbeillustratedbythefollowingcalculation.Theconcentrationrationofxinsolvent1and2isaconstantatagiventemperature,andtheratioisalsocalledthedistributioncoefficient,expressedasK.TheextractionprinciplecanbFirstextractionSecondextractionMultiple(n)extraction<1Basedontheabovecalculations,itisknownthatthemultipleextracionsaremoreefficicentthanasingleextractionwiththesamevolumeofextracionsolvent.FirstextractionSecondextracAnaqueoussolutioncontaining4gofbutanoicacidin100mlofwaterisexractedat15℃with100mlbenzene.TheKvalue(participationcoefficientofbutanoicacidbetweenbenzeneandwater)is1/3.afteronceextcrationwith100mlofbenzene,theremainedamountofbutanoicacidinwateris:Ifthe100mlofbenzeneisdividedintothreeportions,theremainedamountofbutanoicacidinwaterafterthethirdextrationis:Theextractionefficiency:Theextractionefficiency:Anaqueoussolutioncontaining3ProcedureTheextractionofaceticacid（乙酸）fromanaqueoussolutionbydiethylether（乙醚）.SingleextractionTripleextractioncNaOH=0.2000Mol/L乙酸的密度：1.049g/cm33ProcedureTheextractionof英文有机化学实验水蒸汽蒸馏与萃取与洗涤课件有机化学实验ExperimentalOrganicChemistry英文有机化学实验水蒸汽蒸馏与萃取与洗涤课件Steamdistillation1.Purpose1.1StudytheprincipleandmethodsofSteamDistillationusedforpurifingorganicliquids.1.2Graspthetechniquesofsteamdistillation.2.PrincipleSteamdistillation,oneoftheimmiscible（不溶的）phasesbeingwater,isoneofthemostcommonlyusedmethodsofseparatingandpurifyingliquids.Inthismethodsteamispassedintotheimmiscibleandvolatileliquidinthedistillationflask,andthenthewaterandorganiccompoundco-distill（共沸）,condenseinthecondenser,andarecollectedinthenormalway.Accordingtothelawofpartialpressure,thetotalvaporpressure（蒸气压）abovethemixtureisthesumofthepartialpressuresofthepureindividualcomponents.Steamdistillation1.Purpose1.BpIsthevaporpressureoftheimmiscibleorganiccompound.Inthedistillate（馏出液）,theweightrationoforganiccompoundmBandmH2Ocanbeexpressedasinequation:=BpIsthevaporpressureoftheSteamdistillationisapplicabletothefollowingsituations:Ahighboiling-pointorganiccompoundwhichdecomposeatitsboilingpoint.Amixturecontaininginorganicsaltsorotherorganicsolids,notsuitablefordistillation,filtraionandextraction.Amixturecontainglargeamountsofresin-likenearlyintractablesubstancesornonvolatileimpuritieswhichishardtoisolateorpurifyinanyotherway.SteamdistillationisapplicabInorderforsteamdistillationtobefeasible,thesubstancestobepurifiedshouldhavethesecharacteristics:Insolubleorimmiscibleinwater.Noreactionwithwaterwhenco-boiling.Havingacertainvaporpressureat100℃,>665PaInorderforsteamdistillatio3.ProcedureFigure1TypicalApparatusforsteamdistillation图1水蒸气蒸馏装置3.ProcedureFigure1TypicalApBoingchipsOne–third

BoingchipsOne–thirdNOTESInordertoavoidfillingwithcondensedwaterinthethree-neckflaskduringdistillation,heattheflaskwithasmallflametomaketheon-goingdistillationproceedmorequickly.Beforeendthesteamdistillation,opentheTtubeclampfirst,thenremovetheheatsource,disassembletheapparatus,inturn.Avoidlettingtheliquidformtheflaskbackupintothesteamline.NOTESInordertoavoidfilling0.16(4℃)2.8(75℃)6.6(98℃)2.6Solubility水中溶解度/g/100g258（分解）131.5b.p.沸点/℃0.11531.8vapourpressureat100℃100℃时蒸气压/kPasalicylicacid水杨酸isopentanol异戊醇Organiccompound有机物名称Separateisopentanol(异戊醇)andsalicylicacid(水杨酸)mixtureIsopentanolinsolubleorimmiscibleinwater.Isopentanol(异戊醇)andsalicylicacid(水杨酸)noreactionwithwaterwhencoboiling.Isopentanolinsolublehavingacertainvapourpressureat100℃Theprincipleofisopentanol(异戊醇)andsalicylicacid(水杨酸)mixturecanbeseparatebysteamdistillation:0.16(4℃)2.6Solubility水中溶解度/g/productiontest产品检验:①salicylicacidtest水杨酸的检验10d0.1％FeCl3Observablephenomena!!!10dsolutionproductiontest产品检验:①salicyl②isopentanoltest异戊醇的检验10dsolution10d5％K2Cr2O75d16％H2SO4Observablephenomena!!!②isopentanoltest异戊醇的检验10dsSolventextractionandsolutionwashing1.Purpose1.2Learnhowtochoosesuitablesolvent.2.Principle1.1StudytheprincipleandmethodsofSolventextractionandsolutionwashing.Solventextractionisatechniquefrequentlyusedintheorganicchemistrylaboratorytoseparateorisolateadesiredspeciesfromamixtureofcompoundsorfromimpurities.Substancesforextractionusuallyaresolidorliquid.Solutionwashingisthereverseprocessofsolventextraction.Usuallyitisperformedinthecaseofimpuritiesinasolutionthatcanbeextractedbyanotherimmisciblesolvent,whichhasasmallsolubilitytothedesiredsubstance.SolventextractionandsolutioTheapparatusforextractionandsolutionwashingfromliquidiscalledseparatoryfunnel,anditsuseisoneoftheessentialoperationsfororganicchemistryexperiments.Figure1Separatoryfunnel（分液漏斗）Thereathreekindsofseparatoryfunnel-spherical(球形）,subulate（锥形的）andpear（梨形）forms.Inorganicexperiments,aseparatoryfunnelismainlyappliedtothisareas:Separatetwokindsofliquidwhichareimmiscibleanddonotreactwitheachother.Extractaceratincomponentfromasolutiom.Washaliquidproductorthesolutionofasolidproductwithwater,aqueousalkalineoracidicsolution.Adddropwiseacertainreagent(usedasadrippingfunnle)Separatoryfunnelsareveryexpensiveandborkeneasily.NeverpropThefunnelonitsstem,butsupportitonaring,afunnelsupport,orsomeotherstablesupport.TheapparatusforextractionaFigure2Ventingseparatoryfunnel（分液漏斗的振摇与放气）Figure2Ventingseparatoryfu英文有机化学实验水蒸汽蒸馏与萃取与洗涤课件Theextractionprinciplecanbeillustratedbythe