英语翻译
forHPLCwasusedasreactionmedium(J.T.Baker,99.99%)
andH2O230%w/w(Merck)wasusedfordecompositiontests,
whileanalysesusedpotassiumiodide(Sigma-Aldrich),Hydra-
nal-Composite2(Fluka),drymethanolforKFT(Fluka),acetic
acid(Sigma-Aldrich),sodiumthiosulfatepenta-hydrate(99.5%,
Sigma-Aldrich),starch(Sigma-Aldrich),andpotassiumdichro-
mate(RiedeldeHaen).Catalysthasbeenpreparedasalready¨
14reportedandpre-reducedinsitubeforeuse.Preliminarytests
ofH2O2decompositionwerecarriedouttoascertainthatthe
supportalonedoesnotdecomposeH2O2.Weusedpurecalcined
sulfatedceriaat20°C,1barfor5h.14
ReactorSetupfortheExperiments.Acocurrent,downflow
TBRwasdeveloped.Inadditiontothemotivationsalready
mentioned,theTBRallowsshortliquidresidencetimeif
requiredforselectivity.Itisasteady-statereactor,sothat
chemicalanalysishasnolimitationonthesampledquantityand
doesnotaffectthereactoroperation.
Theexperimentalreactorsetupisshownschematicallyin
Figure1.ThereactorismadeofAISI316stainlesssteel,30
cmlong,1.5cmI.D.,andinternallylinedwithTeflon(1.15cm
finalI.D.)topreventH2O2decompositionduetoaccessibleFe3+
ions.Thereactorcanaccommodateacatalystbedupto20cm
long.Anexternalchiller(GrantLTD6G)allowsforworking
temperaturesbetween-20and60°C.Threemassflow
controllers(MFC;Brooks5850series)areusedtoindependently
feedthegases:N2,CO2/H297.5/2.5%,andO2(AGAgas).MFC
havebeencalibratedonactualmassflow;volumetricflowrates
reportedintheFiguresarecalculatedwithmixturedensities
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