Name: temperature-programmed deoxygenation of acetic acid on molybdenum carbide catalysts
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Description: Watch this Scientific Journal Video about Temperature-programmed Deoxygenation of Acetic Acid on Molybdenum Carbide Catalysts at JoVE.com

This work was supported by the Department of Energy Bioenergy Technologies Office under Contract no. DE-AC36-08-GO28308. The U.S. Government retains and the publisher, by accepting the article for publication, acknowledges that the U.S. Government retains a nonexclusive, paid up, irrevocable, worldwide license to publish or reproduce the published form of this work, or allow others to do so, for U.S. Government purposes.

FORSIKTIG: Ta kontakt med sikkerhetsdatablad (SDS) for alle kjemikalier som brukes før operasjon. Brannfarlige gasser kan presentere eksplosjonsfare hvis den kombineres med luft eller oksygen og en tennkilde. Hydrogen er en ekstremt brannfarlig gass. Syrer er etsende, og når det gjelder hud eller øyne, er irriterende og kan forårsake forbrenninger. Eddiksyre er en brennbar væske og damp, og dermed kan antenne og / eller eksplodere i nærvær av åpen flamme, gnister og oksidasjonsmidler, i tillegg til potensielt fo...

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T., Bhan, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structure+and+site+evolution+of+molybdenum+carbide+catalysts+upon+exposure+to+oxygen.">Structure and site evolution of molybdenum carbide catalysts upon exposure to oxygen.</a> J Catal. 326, 82-91 (2015).</li><li>Lee, W. S., Kumar, A., Wang, Z. 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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Modern Practice of Gas Chromatography. , 403-460 (2004).</li><li>Guiochon Georges, L., Guillemin Claude, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Journal of Chromatography Library. 42, 563-586 (1988).</li><li>Guiochon Georges, L., Guillemin Claude, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Journal of Chromatography Library. 42, 587-627 (1988).</li><li>Guiochon Georges, L., Guillemin Claude, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Journal of Chromatography Library. 42, 629-659 (1988).</li><li>Guiochon Georges, L., Guillemin Claude, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Journal of Chromatography Library. 42, 661-687 (1988).</li><li>Baddour, F. 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Den TPRxn metode er et kraftig verktøy for screening av katalytiske materialer, som gir informasjon om aktiviteten og selektiviteten av en katalysator som en funksjon av reaksjonstemperaturen. Andre temperaturprogrammerte metoder som TPD, TPO og TPR kan gi informasjon om adsorpsjon styrken av reagenser, antall adsorpsjon nettsteder, og passende katalysator før behandlingsprosedyrer, men gir ikke direkte katalytiske ytelsesdata. Det er viktig å merke seg at TPRxn fremgangsmåten beskrevet i dette arbeidet ikke måler ...

Temperaturen programmert reaksjon (TPRxn) er en av mange temperaturprogrammerte metoder, herunder desorpsjon (TPD), oksydasjon (TPO), og reduksjon (TPR), og forløper via eksponering av en katalysator til en reaktant samtidig med eller etterfulgt av en jevn økning i temperatur. 1, 2, 3 TPRxn er en forbigående teknikk som gir informasjon om katalysatoraktivitet og selektivitet som en funksjon av reaksjonstemperaturen. 4, 5, 6 Det er også en populær teknikk: et søk på søkeord &quot;temperatur programmert reaksjon&quot; i litteraturen gir over 1000 kilder siterer bruken. TPRxn eksperimenter blir typisk utført i en mikroreaktor system, som er utstyrt med et massespektrometer (MS) for sanntids analyse av reaktoravløpet og korrelasjonen av pYtelse med temperaturen. Reaktantgassene kan innføres ved hjelp av massestrøm kontrollere og væsker kan innføres via en sprøytepumpe eller som damp ved å boble inert gass gjennom en væske. Katalysatoren blir ofte forbehandlet in situ for å danne den ønskede katalytiske fase for reaksjonen. Noen systemer er utstyrt med ekstra analyseutstyr, utover den typiske massespektrometer, for å gi kvantitativ eller kvalitativ informasjon om katalysatorens selektivitet, overflatetyper til stede på katalysatoren, eller reaksjonsmekanisme. For eksempel temperatur programmert in situ Fourier Transform Infrared Spectroscopy (FTIR) gir informasjon om utviklingen av overflate arter med varierende reaksjonstemperaturen. 7, 8 TPRxn system demonstrert i dette arbeidet er utstyrt med et gass-kromatogram (GC) i tillegg til de mer vanlige MS. Dette GC, som er utstyrt med fire parallelle søyler, åpner for mer nøyaktig quantifiseringen av reaksjonsproduktene, men er begrenset i frekvens-analyse av den tiden det tar for produktet å eluere gjennom kolonnene. Således kan en kombinasjon av MS og GC være spesielt nyttig for kobling av sanntids identifikasjon med nøyaktig kvantifisering av reaktanter og produkter. Her bruker vi den TPRxn metodikk for å studere deoksygenering av eddiksyre på molybden karbid katalysatorer. Dette er en interessant og viktig reaksjon i katalysatoren forskning, som eddiksyre er en nyttig analogt for de mange karboksyl-syrer som er tilstede i biomassen pyrolysegasser. 9 Det høye oksygeninnhold i biomassepyrolyse damper nødvendiggjør fjerning av oksygen for å produsere hydrokarbon-brennstoffer, 10, 11, 12 og molybdenkarbid katalysatorer har vist lovende resultater deoksygenering for mange biomassepyrolyse dampmodellforbindelser, inkludert furfural, 1-propanol,fenoliske forbindelser og eddiksyre. 9, 13, 14, 15, 16 Imidlertid er aktiviteten og selektiviteten av molybdenkarbid katalysatorer i deoksygenering reaksjoner avhengig av katalysator struktur og sammensetning, de reagerende arter og reaksjonsbetingelsene. Det oppsamlede fra TPRxn eddiksyre data viser at molybden-karbid-katalysatorer som er aktive for deoksygenering reaksjonene ovenfor ca. 300 ° C, og når det kombineres med katalysator karakterisering informasjon gjør det mulig for kvantifisering av katalysatoraktiviteten som en funksjon av temperaturen til ved beregningen av eddiksyre omsetning priser. De TPRxn Resultatene viser at deoxygenation (dvs. CO bond-breaking) produkter favoriseres ved temperaturer under ca. 400 ° C og dekarbonylering (dvs. CC bond-breaking) produkter er favorød ved temperaturer over ca. 400 ° C. I tillegg TPRxn studier illustrerer endringene i aktivitet og selektivitet av molybden karbid katalysatorer fremstilt ved hjelp av forskjellige syntetiske fremgangsmåter (dvs. produksjon av forskjellige molybdenkarbid katalysator struktur og kjemisk sammensetning). Likevel, verdien av denne informasjonen og, mer generelt, den vellykkede anvendelse av TPRxn eksperimentelle data mot katalysator utforming og prosessoptimalisering er en funksjon av kvaliteten av de oppnådde data. Nøye vurdering og kunnskap om potensielle problemer og begrensninger uthevet hele TPRxn prosedyren er det viktigste.

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	<tbody>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">glacial acetic acid</td>
			<td style="width:179px;">Cole-Parmer</td>
			<td style="width:148px;">EW-88401-62</td>
			<td style="width:401px;">alternate supplier acceptable if ACS purity grade. See caution statement in protocol for safety information</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">UHP H&#8322;</td>
			<td style="width:179px;">Airgas</td>
			<td style="width:148px;">HY R300</td>
			<td>alternate supplier acceptable if &#62;99.99% purity</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">UHP He</td>
			<td style="width:179px;">Airgas</td>
			<td style="width:148px;">HE R300SS</td>
			<td>alternate supplier acceptable if &#62;99.99% purity</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">UHP Ar</td>
			<td style="width:179px;">Arigas</td>
			<td style="width:148px;">AR R200</td>
			<td>alternate supplier acceptable if &#62;99.99% purity</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">acetone</td>
			<td style="width:179px;">VWR International</td>
			<td style="width:148px;">BDH1101-4LP</td>
			<td>alternate supplier acceptable if &#62;99.5% purity</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">quartz chips</td>
			<td style="width:179px;">Powder Technology Inc.</td>
			<td style="width:148px;">Crushed Quartz</td>
			<td style="width:401px;">sieved 180-300 &#181;m, calcined in air at 500 &#176;C overnight</td>
		</tr>
		<tr height="56">
			<td height="56" style="height:56px;width:215px;">mass spectrometer - turbo vacuum pump</td>
			<td style="width:179px;">Pfeiffer Vacuum</td>
			<td style="width:148px;">TSU 071</td>
			<td style="width:401px;">mass spectrometer is controlled with LabVIEW 2010 software package (National Instruments)</td>
		</tr>
		<tr height="56">
			<td height="56" style="height:56px;width:215px;">mass spectrometer - turbo vacuum pump</td>
			<td style="width:179px;">Stanford Research Systems</td>
			<td style="width:148px;">RGA100</td>
			<td style="width:401px;"></td>
		</tr>
		<tr height="126">
			<td height="126" style="height:126px;width:215px;">micro gas chromatograph</td>
			<td style="width:179px;">Agilent</td>
			<td style="width:148px;">CP740388</td>
			<td style="width:401px;">490 Micro GC; 4-channel system 
			Channel 1: 494001360 Molseive 10m, heated backflush 
			Channel 2: 494001460 PPU 10m, heated backflush 
			Channel 3: 490040 AL2O3/KCL 10+0.2m, heated backflush SPECIAL 
			Channel 4: 492005750 5CB 15m, heated</td>
		</tr>
		<tr height="56">
			<td height="56" style="height:56px;width:215px;">GC software</td>
			<td style="width:179px;">Aglient</td>
			<td style="width:148px;">OpenLAB CDS EZChrom Edition</td>
			<td style="width:401px;"></td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">clean gas filters</td>
			<td style="width:179px;">Agilent</td>
			<td style="width:148px;">CP17974</td>
			<td>for use on GC carrier gases (He, Ar)</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">quartz &#34;U-tube&#34; reactor</td>
			<td style="width:179px;">n/a</td>
			<td style="width:148px;"></td>
			<td>hand blown glass, custom built to order</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">bubbler</td>
			<td style="width:179px;">n/a</td>
			<td style="width:148px;"></td>
			<td>custom built to order</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">ceramic furnace</td>
			<td style="width:179px;">Watlow</td>
			<td style="width:148px;">discontinued</td>
			<td>Similar furnace part #: VC401J12A-B000R</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">heat tape controller</td>
			<td style="width:179px;">n/a</td>
			<td style="width:148px;"></td>
			<td>custom built with Watlow EZ-zone parts</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">heat tape</td>
			<td style="width:179px;">Omega</td>
			<td style="width:148px;">FGH051-060</td>
			<td style="width:401px;">alternate supplier for extreme temperature heat tape acceptable</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">heat tape insulation</td>
			<td style="width:179px;">JEGS</td>
			<td style="width:148px;">710-80809</td>
			<td>alternate supplier acceptable</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">thermocouple</td>
			<td style="width:179px;">Omega</td>
			<td style="width:148px;">e.g., KMQSS-062U-18</td>
			<td>K-type thermocouples; alternate sizes may be required</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">thermocouple o-ring</td>
			<td style="width:179px;">Swagelok</td>
			<td style="width:148px;">VT-7-OR-001-1/2</td>
			<td>perfluoroelastomer(fluorocarbon FKM) o-ring</td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">2 &#181;m solids filter, VCR gasket</td>
			<td style="width:179px;">Swagelok</td>
			<td style="width:148px;">SS-4-VCR-2-2M</td>
			<td></td>
		</tr>
		<tr height="57">
			<td height="57" style="height:58px;width:215px;">1 &#181;m orifice, VCR gasket</td>
			<td style="width:179px;">Lenox Laser</td>
			<td style="width:148px;">SS-4-VCR-2</td>
			<td>for mass spectrometer orifice</td>
		</tr>
		<tr height="93">
			<td height="93" style="height:94px;width:215px;">316/316L stainless steel tubing and fittings</td>
			<td style="width:179px;">Swagelok</td>
			<td style="width:148px;">Varies</td>
			<td style="width:401px;">See Swagelok &#39;VCR Metal Gasket Face Seal Fittings&#39; and &#39;Stainless Steel Seamless Tubing and Tube Support Systems&#39; catalogs for more information</td>
		</tr>
		<tr height="93">
			<td height="93" style="height:94px;width:215px;">316/316L stainless steel tubing and fittings</td>
			<td style="width:179px;">Swagelok</td>
			<td style="width:148px;">Varies</td>
			<td style="width:401px;">See Swagelok &#39;Integral-Bonnet Needle Valves&#39;, &#39;Bellows-Sealed Valves&#39; and &#39;One-Piece Instrumentation Ball Valves&#39; catalogs for more information</td>
		</tr>
	</tbody>
</table>

temperature-programmed deoxygenation of acetic acid on molybdenum carbide catalysts

Temperatur programmert reaksjon (TPRxn) er et enkelt men kraftig verktøy for screening fast katalysator ytelse til en rekke forhold. Et TPRxn systemet omfatter en reaktor, ovn, gass- og dampkilder, flytkontroll, instrumentering for å kvantifisere reaksjonsprodukter (for eksempel gass kromatograf), og instrumentering for å overvåke reaksjonen i sanntid (f.eks massespektrometer). Her bruker vi den TPRxn metodikk for å studere molybdenkarbid katalysatorer for deoksygenering av eddiksyre, en viktig reaksjon blant mange i oppgradering / stabilisering av biomassepyrolysegasser. TPRxn brukes til å evaluere katalysatoraktivitet og selektivitet, og å teste hypotetiske reaksjonsveiene (f.eks, dekarbonylering, ketonization, og hydrogenering). Resultatene av TPRxn studiet av eddiksyre deoksygenering viser at molybden karbid er en aktiv katalysator for denne reaksjonen ved temperaturer over ca. 300 ° C, og at reaksjons favorisererdeoxygenation (dvs. CO bond-breaking) produkter ved temperaturer under ca. 400 ° C og dekarbonylering (dvs. CC bond-breaking) produkter ved temperaturer over ca. 400 ° C.

Den elektroniske MS gir mulighet til å analysere gass komposisjon ved utløpet av reaktoren i sanntid. Den elektroniske MS er ikke sammen med hvilken som helst enhet for å skille produktene før analyse, og dermed artsbestemmelse er utfordrende når skille mellom forbindelser med overlappende massefragmenteringsmønster. Som vist i tabell 2, er mange av de vanlige produkter fra eddiksyre TPRxn eksperimenter kjennetegnes ved mange vanlige m / z signaler. Dekonvolvering ...

Watch this Scientific Journal Video about Temperature-programmed Deoxygenation of Acetic Acid on Molybdenum Carbide Catalysts at JoVE.com

Temperature-programmed Deoxygenation of Acetic Acid on Molybdenum Carbide Catalysts

Presenteres her er en protokoll for drift av et mikroskala temperatur-programmert reaktor for å evaluere den katalytiske ytelsen av molybdenkarbid i løpet av eddiksyre deoksygenering.

Temperatur-programmert Deoksygenering av Eddiksyre på Molybden Carbide Katalysatorer

Temperature programmed reaction (TPRxn) is a simple yet powerful tool for screening solid catalyst performance at a variety of conditions. A TPRxn system ...

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Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

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Continuous Flow Chemistry: Reaction of Diphenyldiazomethane with p-Nitrobenzoic Acid

Continuous Flow Chemistry: Reaction of Diphenyldiazomethane with p-Nitrobenzoic Acid

Kontinuerlig kjemi: Reaksjon av Diphenyldiazomethane med p- Nitrobenzoic syre

Continuous flow technology has been identified as instrumental for its environmental and economic advantages leveraging superior mixing, heat transfer and ...

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

Kjemisk nedbør metoden for syntese av Nb2O5 endret Bulk nikkel katalysatorer med høy bestemt areal

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 ...

Preparation of Polyoxometalate-based Photo-responsive Membranes for the Photo-activation of Manganese Oxide Catalysts

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This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic ...

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

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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

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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 ...