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Preparationofbenzylalcoholandbenzoicacid湛江師范學(xué)院11化本2班專業(yè)英語(yǔ)實(shí)驗(yàn)報(bào)告First,thepurposeoftheexperiment
1.Learningtheprinciplesandmethodsofpreparationofbenzylalcoholandbenzaldehydebenzoicacid.
2.Morefamiliarwiththeuseofamechanicalstirrer.
3.Furtherunderstandtheextraction,washing,distillation,dryingandrecrystallizationbasicoperations.
4.Comprehensivereviewandconsolidatebasicskillsinorganicchemistryexperiment.Second,thebasicprinciple
Noα-Haldehydeoccursintheconcentratedalkalinesolutiononthedisproportionationreaction,thealdehydeisoxidizedtoacarboxylicacidmoleculeandanothermoleculealdehydeswerereducedtothealcohol,thereactioncalledCannizzaroreaction.ThisexperimentCannizzaroreactionofbenzaldehydeoccursinconcentratedsodiumhydroxidesolution,benzylalcoholandbenzoicacidwasprepared,followingreactionformula:Third,themainreagentandinstrument
1.Reagentsbenzaldehyde10mL(0.10mol),sodiumhydroxide8g(0.2mol),concentratedhydrochloricacid,diethylether,asaturatedsodiumhydrogensulfitesolution,10%sodiumcarbonatesolution,driedoveranhydrousmagnesiumsulfate.
2.Instrument100mLroundbottomflask,sphericalcondenser,aseparatoryfunnel,straightcondenser,distillationhead,thermowell,thermometer(250℃),escortsmanifoldpipe,theconicalflask,thehollowplug,graduatedcylinders,beakers,Brinellfunnel,suctionflask,dishsurface,infraredlight,mechanicalstirrer.Fourth,theexperimentalprocedure
1.Mechanicalstirrerandarefluxcondenserinstalledin250mLthree-neckedflask,andtheotherportpluggedinFigure1.
2.8gofsodiumhydroxideand30mLofwaterwasaddedandstirredtodissolve.Coolish,10mLoffreshlydistilledbenzaldehyde.
3.Opentheblender,adjustthespeed,sostirsmoothly.Heatedtorefluxforabout40min.
4.Heatingwasstopped,wasslowlyaddedfromthesphericalcondensercoldcatchy20mL,shakeevenlycooledtoroomtemperature.
5.Afterthereactionwascooledtoroomtemperature,pouredintoaseparatoryfunnel,andextractedthreetimeswithdiethylether,each10mL.Theaqueouslayerreservedforfutureuse.
6.Threeetherextractswerecombined,successivelywashedwith5mLofsaturatedsodiumbisulfite,washedwith10mL10%sodiumcarbonatesolution,washedwith10mLofwater.
7.Etherlayerwasseparated,driedintoaconicalflask,addanhydrousmagnesiumsulfate,payattentiontotheflaskstoppered.
8.Figure2isinstalledinalow-boilingliquiddistillationapparatusandslowlyheatedtodistilloutdiethylether(recovery).
9.Distillationatelevatedtemperatures,whentheairtemperatureisraisedto140℃switchcondenser,collectingfractionsof198℃~204℃,isbenzylalcohol,theamountofvolumerecoveryyieldiscalculated.
10.Step5Theaqueouslayerwasslowlyaddedtothereserved30mLcontaining30mLofconcentratedhydrochloricacidandthemixtureofwater,whilestirringwithaglassrod,awhitesolidprecipitated.
11.Cooling,filtration,togivethecrudeacid.
12.Thecrudeacidwasrecrystallizedusingwaterasasolvent,theneedtoaddactivecarbon.Aftertheproductwasdriedunderaninfraredlampload,recoveredyieldwascalculated.V.Notes
1.Theexperimentneedswithether,andtheetherethereasytousefire,mustnothaveanykindofopenflameinthevicinityofthetime.SteamedethercanbeconnectedwithinalongrubbertubeintubeescortspassintothebranchpipeunderthesinkpipesorleadoutsidetoacceptUsedcoldbathtocool.
2.Purifiedwaterasthecrystallizationsolventcanbere-benzoicacid,benzoicacidsolubilityinwater:80℃,each100mLofwatersolubleacid2.2g.SixQuestions
1.ComparetheCannizzaroreactionaldolreactionwithaldehydestructureonthedifferences.
2.Inthisexperimentthetwoproductsisbasedontheprincipleoftheseparationandpurificationofwhat?Itwaswashedwithsaturatedsodiumhydrogensulfiteand10%sodiumcarbonatesolutionwiththepurposeof?
Firstly,theextractionprinciple:thesolubilityofbenzylalcoholandsodiumbenzoateinetherisdifferentfromtheextractionagentwithether,benzylalcoholwasextractedintoetherlayer,therebyseparatingthetwo.Theetherlayersweretreatedandthentheaqueouslayer,andthedistillationwasrecrystallizedtwomorepureisolatedproduct.
Theequation:C6H5CHO+NaHSO3=C6H5CH(OH)SO3NaSulfiteishappeningwiththecarbonyladditionreaction
Thereactioncanberemovednotbenzaldehyde3.Theremainingaqueoussolutionwasextractedwithdiethylether,acidifiedwithconcentratedhydrochloricacidtoneutralisthemostappropriate?Why?
4.Whyusefreshlydistilledbenzaldehyde?Long-termplacementofbenzaldehydecontainanyimpurities?Ifnotremove
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