Name: synthesis and testing of supported pt-cu solid solution nanoparticle catalysts for propane dehydrogenation
Uploaded: 2017-07-18T15:00:00
Description: Watch this Scientific Journal Video about Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation at JoVE.com

Dette arbejde blev støttet af School of Chemical Engineering, Purdue University. Brug af Advanced Photon Source blev understøttet af US Department of Energy, Office of Basic Energy Sciences, under kontrakt nr. DE-AC02-06CH11357. MRCAT operationer, beamline 10-BM understøttes af Department of Energy og MRCAT medlemsinstitutionerne. Forfatterne anerkender også brugen af ​​strålelinie 11-ID-C. Vi takker Evan Wegener for eksperimentel assistance med XAS.

1. Syntese af understøttede 2 nm Pt-Cu bimetalliske nanopartiklekatalysatorer <ol><li> Fremstilling af metalprecursoropløsning <ol><li> Opløs 0,125 g kobbernitrat trihydrat (Cu (NO3) 2 · 3H 2 O) i 1 ml vand for at opnå en himmel blå opløsning. Forsigtig: Brug beskyttelseshandsker ved håndtering af kemikalier. </li><li> Tilsæt ammoniak dråbevis til kobbernitratopløsningen, der danner mørkeblå bundfældninger af kobberhydroxid. Forsigtighed: Br...

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Pt-Cu-katalysatorerne fremstillet i dette værk indeholder ensartede nanopartikler ca. 2 nm, svarende til heterogene katalysatorer, der er kvalificeret til industriel anvendelse. Alle Pt- og Cu-forstadierne danner bimetalliske strukturer i modsætning til separate monometalliske partikler. Denne bimetalliske interaktion og små partikelstørrelser realiseres ved omhyggelig kontrol over synteseprocedurerne. Imprægneringsprocessen gør brug af den stærke elektrostatiske adsorption (SEA) mellem metalioner og overfladen a...

Propan dehydrogenering (PDH) er et nøglebehandlingstrin i produktionen af ​​propylen, idet man udnytter skifergas, den hurtigst voksende gaskilde i landet 1 . Denne reaktion bryder to CH-bindinger i et propanmolekyle for at danne et propylen og molekylært hydrogen. Ædelmetalkatalysatorer, herunder Pd-nanopartikler, udviser dårlig selektivitet for PDH, bryder CC-bindingen for at frembringe methan med højt udbytte, med den samtidige produktion af cola, hvilket fører til katalysatordeaktivering. Nylige rapporter viste, at selektive PDH-katalysatorer kunne opnås ved tilsætning af promotorer som Zn eller In til Pd 2 , 3 , 4 . De promoterede katalysatorer er næsten 100% selektive til PDH, i modsætning til mindre end 50% for monometalliske Pd nanopartikler af samme størrelse. Den store forbedring i selektivitet blev tilskrevet dannelsen af ​​PdZn eller PdIn intermetallisk forbindelse(IMC) strukturer på katalysatoroverfladen. Den ordnede rækkevidde af to forskellige typer af atomer i IMC&#39;erne geometrisk isolerede de Pd-aktive steder med ikke-katalytiske Zn- eller In-atomer, som slukede sidereaktionerne katalyseret af et ensemble (gruppe) af nabostillede Pd-aktive steder. Platin har den højeste egentlige selektivitet blandt ædelmetaller til propandehydrogenering, men det er stadig ikke tilfredsstillende til kommerciel brug 1 . Typisk sættes Sn, Zn, In eller Ga som promotor for Pt 5 , 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 . Baseret på ideen om, at geometrisk aktivitetsisolering bidrager til høj selektivitet, vil ethvert ikke-katalytisk element, der danner en legering sStrukturen med Pt, såsom Cu, bør også potentielt fremme katalysatorpræstationen 14 . Flere tidligere undersøgelser antydede, at tilsætningen af ​​Cu faktisk forbedrede PDH-selektiviteten af ​​Pt-katalysatorer 15 , 16 , 17 , 18 . Ikke desto mindre er der ikke rapporteret direkte beviser for at afgøre, om Pt og Cu danner bimetalliske nanopartikler eller bestilte strukturer, hvilket er afgørende for forståelsen af ​​den salgsfremmende effekt af Cu. I bin-fase-diagrammet af Pt-Cu er to forskellige strukturtyper mulige over et bredt sammensætningsområde 16 , 18 : intermetallisk forbindelse, hvori Pt og Cu hver besætter specifikke krystalsteder og en fast opløsning, hvor Cu tilfældigt erstatter i Pt gitter. IMC&#39;er danner ved lav temperatur og omdannes til fast opløsning ved ca. 600-800 ° C for bulkmaterialer dvs. 550 ° C). Derfor er det vigtigt at undersøge atomorden af ​​Pt-Cu under reaktionsbetingelser. For understøttede nanopartikler med små partikelstørrelser er det meget udfordrende at opnå meningsfuld strukturel information ved hjælp af laboratorieinstrumenter 19 . Den begrænsede gentagelse af enhedsceller fører til meget brede diffraktionstoppe med meget lave intensiteter. På grund af den høje andel af overfladeatomer i nanopartikler, der er 1 til 3 nm i størrelse, som oxideres i luft, skal diffraktion opsamles in situ ved anvendelse af højflux-røntgenstråler, der typisk er tilgængelige med synkrotronteknikker. De tidligere rapporterede Pt-Cu PDH katalysatorer var alle større end 5 nm i størrelse 15 , 16 , 17 , 18. For ædelmetal nanopartiklekatalysatorer er der imidlertid altid et stærkt ønske om at maksimere katalytisk aktivitet pr. Enhedsomkostning ved at syntetisere katalysatorer med høje dispersioner (typisk omkring eller mindre end 2 nm i størrelse) 19 . Selvom fremstillingen af ​​bimetalliske nanopartikler af denne størrelse er mulig ved standard imprægneringsmetoder, er rationel kontrol over procedurerne nødvendig. Metalprecursorerne, pH-værdien af ​​imprægneringsopløsningen og understøttelsestype skal styres for at optimere forankringen af ​​metalarten på overflader med højt overfladeareal. De efterfølgende kalcinerings- og reduktionsvarmebehandlinger bør også kontrolleres omhyggeligt for at undertrykke væksten af ​​metalliske nanopartikler. Denne artikel dækker protokollen til syntese af understøttede 2 nm Pt-Cu bimetalliske nanopartiklekatalysatorer og til test af deres propan dehydrogeneringspræstation. Strukturen af ​​katalysatorerne undersøges ved Scanning TResonanselektronmikroskopi (STEM), in situ synkrotron røntgenabsorptionsspektroskopi (XAS) og in situ synkrotron røntgendiffraktion (XRD), som hjælper med at belyse den forbedrede katalysator ydeevne ved indførelsen af ​​Cu.

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synthesis and testing of supported pt-cu solid solution nanoparticle catalysts for propane dehydrogenation

En praktisk fremgangsmåde til syntesen af ​​bimetalliske Pt-Cu-katalysatorer og præstationsprøver til propandehydrogenering og karakterisering er demonstreret her. Katalysatoren danner en substitutionel fast opløsningsstruktur med en lille og ensartet partikelstørrelse omkring 2 nm. Dette realiseres ved omhyggelig kontrol over imprægnering, kalcinering og reduktionstrin under katalysatorfremstilling og identificeres ved avancerede in situ- synkrotronteknikker. Katalysatorpropanddehydrogeneringsydelsen forbedres løbende med stigende Cu: Pt atomforhold.

Propylenselektiviteten versus tid for Pt- og Pt-Cu-katalysatorer målt ved en initialpropankonvertering på ca. 20% er vist i figur 1A . Pt-katalysatoren har en initial selektivitet på 61%, som stiger til ca. 82% med tiden on-stream, da katalysatoren deaktiveres i 1 time. Pt-0,7Cu katalysatoren viser en bedre initial propylenselektivitet på 72%. For Pt-2,3Cu og Pt-7,3Cu katalysatorer når deres oprindelige selektivitet henholdsvis 90% og 96% og opretholdes...

Watch this Scientific Journal Video about Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation at JoVE.com

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

En bekvem fremgangsmåde til syntese af 2 nm understøttede bimetalliske nanopartikel Pt-Cu katalysatorer til propan dehydrogenering er her beskrevet. In situ- synkrotron-røntgenteknikker tillader bestemmelse af katalysatorstrukturen, hvilket typisk ikke er muligt ved hjælp af laboratorieinstrumenter.

Syntese og test af understøttet Pt-Cu fast opløsning Nanopartiklekatalysatorer til propan dehydrogenering

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

Research

JoVE Journal

Chemistry

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or IV)

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

Kombinere Solid-state og løsning-baserede teknikker: Syntese og reaktivitet af Chalcogenidoplumbates (II eller IV)

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica ...

Measurement of Particle Size Distribution in Turbid Solutions by Dynamic Light Scattering Microscopy

Måling af Particle Size Distribution i uklare Solutions af Dynamic Light Scattering Microscopy

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a ...

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism

Protokol til fastfasesyntese af oligomerer af RNA indeholdende en 2&#39;-<em&gt; O</em&gt; -thiophenylmethyl-modifikation og karakterisering via cirkulær dikroisme

Solid-phase synthesis has been used to obtain canonical and modified polymers of nucleic acids, specifically of DNA or RNA, which has made it a popular ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Væske-celle transmissions elektronmikroskopi til sporing samlesæt af nanopartikler

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Kemisk udfældning metode til syntese af Nb2O5 ændret Bulk nikkel katalysatorer med høje specifikke overfladeareal

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

Hurtig Nanoprobe Signal forstærkning af In Situ guld nanopartikel syntese

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

En hurtig syntese metode til Au, Pd og Pt aerogeler Via direkte løsning-baseret reduktion

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

Fast-fase syntese af [4.4] Spirocyclic Oximes

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

Imine-meta afhandling af silica-støttede katalysatorer ved hjælp af metodologien for overflade Organometallisk kemi

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

Tuning surhedsgraden af PT/CNTs katalysatorer for Hydrodeoxygenering af diphenyl ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...