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簡介：HINDAWIPUBLISHINGCORPORATIONINTERNATIONALJOURNALOFCHEMICALENGINEERINGVOLUME2011,ARTICLEID518592,11PAGESDOI101155/2011/518592RESEARCHARTICLECATALYSTINITIATIONINTHEOSCILLATORYCARBONYLATIONREACTIONKATARINANOVAKOVICANDJULIEPARKERSCHOOLOFCHEMICALENGINEERINGANDADVANCEDMATERIALS,NEWCASTLEUNIVERSITY,NEWCASTLEUPONTYNENE17RU,UKCORRESPONDENCESHOULDBEADDRESSEDTOKATARINANOVAKOVIC,KATARINANOVAKOVICNCLACUKRECEIVED16MARCH2011REVISED21APRIL2011ACCEPTED26APRIL2011ACADEMICEDITORDYUMURZINCOPYRIGHT?2011KNOVAKOVICANDJPARKERTHISISANOPENACCESSARTICLEDISTRIBUTEDUNDERTHECREATIVECOMMONSATTRIBUTIONLICENSE,WHICHPERMITSUNRESTRICTEDUSE,DISTRIBUTION,ANDREPRODUCTIONINANYMEDIUM,PROVIDEDTHEORIGINALWORKISPROPERLYCITEDPALLADIUMIIIODIDEISUSEDASACATALYSTINTHEPHENYLACETYLENEOXIDATIVECARBONYLATIONREACTIONTHATHASDEMONSTRATEDOSCILLATORYBEHAVIOURINBOTHPHANDHEATOFREACTIONINANATTEMPTTOEXTRACTTHEREACTIONNETWORKRESPONSIBLEFORTHEOSCILLATORYNATUREOFTHISREACTION,THESYSTEMWASDIVIDEDINTOSMALLERPARTSANDTHEYWERESTUDIEDTHISPAPERFOCUSESONUNDERSTANDINGTHEREACTIONNETWORKRESPONSIBLEFORTHEINITIALREACTIONSOFPALLADIUMIIIODIDEWITHINTHISOSCILLATORYREACTIONTHESPECIESRESEARCHEDINCLUDEMETHANOL,PALLADIUMIIIODIDE,POTASSIUMIODIDE,ANDCARBONMONOXIDESEVERALCHEMICALREACTIONSWERECONSIDEREDANDAPPLIEDINAMODELLINGSTUDYTHESTUDYREVEALEDTHESIGNIFICANTROLEPLAYEDBYTRACESOFWATERCONTAINEDINTHESTANDARDHPLCGRADEMETHANOLUSED1INTRODUCTIONTHEPALLADIUMCATALYSEDPHENYLACETYLENEOXIDATIVECARBONYLATIONPCPOCREACTIONSTANDSOUTINANUMBEROFRESPECTSITPROVIDESANOVELPHOSCILLATOROPERATINGINASTIRREDBATCHREACTOR1–8FURTHERMORE,WHENOPERATINGTHEPCPOCSYSTEMINANOSCILLATORYREGIMEHIGHLEVELSOFPRODUCTSELECTIVITYAREREPORTEDCOMPAREDTOOPERATINGINANONOSCILLATORYMODE6THEABILITYTOACHIEVESELECTIVEPRODUCTFORMATIONINTHISWAYISANEWANDNOTABLERESULTINTERMSOFREACTIONENGINEERINGTHAT,ONCEUNDERSTOOD,MAYBEIMPOSEDONANDEXPLOITEDININDUSTRIALLYSIGNIFICANTREACTIONSMOREOVER,THEPCPOCREACTIONREPRESENTSTHEFIRSTEXAMPLEOFCOMPLEXMOLECULESSYNTHESISEDFROMRELATIVELYSIMPLEREAGENTSPROCEEDINGINACATALYTICSYSTEMINANOSCILLATORYMODESCIENTIFICALLYTHISISSIGNIFICANTASALLOTHEROSCILLATINGPROCESSES,INCLUDINGTHOSEDRIVENBYHETEROGENEOUSCATALYSIS,INVOLVETHEOXIDATION,HYDROGENATION,ORDESTRUCTIONOFCOMPLEXMOLECULES3INADDITIONTOOSCILLATIONSINPH,THEPCPOCREACTIONHASTHECAPACITYTOPRODUCESIGNIFICANTOSCILLATORYPULSESOFHEATIE,600J/OSCILLATIONOVERLONGPERIODSOFTIMEIE,DAYSTHATMAYBEREGULATEDBYTHEREACTIONCONDITIONS5,6,8FORTHATREASON,THEIMPORTANCEOFTHEPCPOCREACTIONFORPHANDTEMPERATURERESPONSIVE“SMARTMATERIALS”ANDTHEIRFUTUREAPPLICATIONSMAYBEFORESEEN,FOREXAMPLE,INDRUGDELIVERY9THEAFOREMENTIONEDRESULTSIMPLYTHENEEDFORAFUNDAMENTALUNDERSTANDINGOFTHEPCPOCREACTIONINORDERTOMAKEUSEOFTHEOBSERVEDPHENOMENAANDAPPLYTHEKNOWLEDGEGAINEDTOOTHERSYSTEMSTHEKEYTOACHIEVINGTHISISINOBTAININGAREACTIONNETWORKIE,RATEDETERMININGREACTIONSINACHEMICALMECHANISMRESPONSIBLEFORTHEOSCILLATORYNATUREOFTHEPCPOCREACTIONTHEPCPOCREACTIONSYSTEMONINITIATIONCONSISTSOFSEVENSPECIESCH3OH,PDI2,KI,NAOAC,CO,AIR,ANDC8H6CONDUCTINGMECHANISTICMODELLINGSTUDIESISDIFFICULTDUETOTHELARGENUMBEROFSPECIESINTHISWORK,ASTRATEGYTHATREDUCESCOMPLEXITYISAPPLIEDTHEOVERALLSYSTEMISSIMPLIFIEDTOASERIESOFSUBSYSTEMSCONSISTINGOFASLITTLEASTWOSPECIESTHEROLEOFEACHSPECIESINTHESUBSYSTEMANDTHEIRINTERACTIONWITHOTHERSPECIESISINVESTIGATEDEXPERIMENTALLYANDDATAOBTAINEDAREEMPLOYEDINMODELLINGSTUDIESTHEEXPERIMENTALSTUDIESAREPERFORMEDINSTANDARDLABORATORYGLASSWAREWITHAMAGNETICSTIRRER,USINGHELMICRONOTEFORONLINEDATALOGGINGBATCHCADSOFTWAREISUSEDFORKINETICFITTING,MODELLINGANDSIMULATIONSTUDIESANALLAQUEOUSPHMETERSETUPCONSISTINGOFAQUEOUSPHELECTRODEFILLINGSOLUTIONANDAQUEOUSCALIBRATIONBUFFERSISUSEDINALLEXPERIMENTSTHEPHVALUESMEASUREDWITHTHISPROCEDUREAREOFTENCALLEDAPPARENTPHVALUESPHAPP10THEPHMEASUREMENTSAREEMPLOYEDINTHEMODELLINGSTUDYASHYDROGENIONCONCENTRATIONWHENWATERISUSEDASTHESOLVENT,HYDROGENINTERNATIONALJOURNALOFCHEMICALENGINEERING3150010005000TIMEMIN225335445555665PHFIGURE2KI4810?1MOL/DM3PDI2IFALLDISSOLVED26610?3MOL/DM3COFLOW6ML/MIN25MLOFWATERCOPURGINGPDI2ADDITION200150100500TIMEMIN56789PHAPPFIGURE3KI4810?1MOL/DM3PDI2IFALLDISSOLVED26610?3MOL/DM3COFLOW6ML/MIN25MLOFDRYMETHANOL25MLOFDEIONISEDWATER,ANDTHEN24MGOFPDI2WASADDEDAPPROXIMATELY1HAFTERTHEADDITIONOFPALLADIUMIIIODIDE,PURGINGWITHCARBONMONOXIDE6ML/MINBEGANTHECOLOUROFTHESOLUTIONWASINITIALLYBROWN,THENOVERTHECOURSEOFTHEEXPERIMENTITBECAMECOLOURLESSANDABLACKPRECIPITATEWASOBSERVEDTHEPHRESULTSAREPRESENTEDINFIGURE224DRYMETHANOLASSOLVENTTHISEXPERIMENTUSEDDRYMETHANOLASSOLVENTINSTEADOFSTANDARDGRADEMETHANOLWATERWASREMOVEDFROMTHEMETHANOLUSINGMOLECULARSIEVESPORESIZE3?AANDABSORPTION≥15ASTOCKSOLUTIONOFKIINMETHANOLWASMADE8GOFKIAND100MLOFCH3OH,MOLECULARSIEVESWEREADDED4672G,ANDTHEMIXTUREWASSTIRREDFORAPPROXIMATELY20HTHEEXPERIMENTWASPERFORMEDASFOLLOWS1GOFFRESHMOLECULARSIEVESWASPLACEDINTOANEMPTYVIALFOLLOWEDBY25MLOFTHEPREVIOUSLYPREPAREDSTOCKSOLUTIONAND24MGOFPDI2CARBONMONOXIDEADDITION6ML/MINCOMMENCEDAPPROXIMATELY1HAFTERPDI2WASADDEDTHECOLOUROFTHESOLUTIONWASDARKREDBROWN,ANDNOPRECIPITATEWASOBSERVEDTHEPHAPPRESULTSAREPRESENTEDINFIGURE325STANDARDGRADE“WET”METHANOLASSOL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