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.

ADVARSEL: Se sikkerhedsdatablade (SDS) for alle kemikalier, der anvendes før operation. Brandfarlige gasser kan udgøre eksplosionsfare, hvis de kombineres med luft eller ilt og en antændelseskilde. Hydrogen er en yderst brandfarlig gas. Syrer er ætsende, og i tilfælde af hud- eller øjenkontakt, er irritanter og kan frembringe forbrændinger. Eddikesyre er en brandfarlig væske og damp, og dermed kan antænde og / eller eksplodere ved tilstedeværelse af åbne flammer, gnister og oxidationsmidler, foruden potentiel...

<ol>
	<li>Cvetanovi&#263;, R. J., Amenomiya, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+a+Temperature-Programmed+Desorption+Technique+to+Catalyst+Studies.">Application of a Temperature-Programmed Desorption Technique to Catalyst Studies.</a> Adv. Catal. 17, 103-149 (1967).</li><li>Falconer, J. L., Schwarz, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Temperature-Programmed+Desorption+and+Reaction:+Applications+to+Supported+Catalysts.">Temperature-Programmed Desorption and Reaction: Applications to Supported Catalysts.</a> Catal. Rev. - Sci. Eng. 25 (2), 141-227 (1983).</li><li>Hurst, N. W., Gentry, S. J., Jones, A., McNicol, B. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Temperature+Programmed+Reduction.">Temperature Programmed Reduction.</a> Catal. Rev. - Sci. Eng. 24 (2), 233-309 (1982).</li><li>Sanchez, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=When+Gold+Is+Not+Noble:+Nanoscale+Gold+Catalysts.">When Gold Is Not Noble: Nanoscale Gold Catalysts.</a> J. Phys. Chem. A. 103 (48), 9573-9578 (1999).</li><li>Alayoglu, S., Nilekar, A. U., Mavrikakis, M., Eichhorn, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ru-Pt+core-shell+nanoparticles+for+preferential+oxidation+of+carbon+monoxide+in+hydrogen.">Ru-Pt core-shell nanoparticles for preferential oxidation of carbon monoxide in hydrogen.</a> Nat Mater. 7 (4), 333-338 (2008).</li><li>Wachs, I. E., Madix, R. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+oxidation+of+methanol+on+a+silver+(110)+catalyst.">The oxidation of methanol on a silver (110) catalyst.</a> Surf. Sci. 76 (2), 531-558 (1978).</li><li>Topsoe, N. Y., Topsoe, H., Dumesic, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Vanadia/Titania+Catalysts+for+Selective+Catalytic+Reduction+(SCR)+of+Nitric-Oxide+by+Ammonia.">Vanadia/Titania Catalysts for Selective Catalytic Reduction (SCR) of Nitric-Oxide by Ammonia.</a> J Catal. 151 (1), 226-240 (1995).</li><li>Clarke, D. B., Bell, A. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+Infrared+Study+of+Methanol+Synthesis+from+CO2+on+Clean+and+Potassium-Promoted+Cu/SiO2.">An Infrared Study of Methanol Synthesis from CO2 on Clean and Potassium-Promoted Cu/SiO2.</a> J Catal. 154 (2), 314-328 (1995).</li><li>Schaidle, J. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Experimental+and+Computational+Investigation+of+Acetic+Acid+Deoxygenation+over+Oxophilic+Molybdenum+Carbide:+Surface+Chemistry+and+Active+Site+Identity.">Experimental and Computational Investigation of Acetic Acid Deoxygenation over Oxophilic Molybdenum Carbide: Surface Chemistry and Active Site Identity.</a> ACS Catal. 6 (2), 1181-1197 (2016).</li><li>Ruddy, D. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+advances+in+heterogeneous+catalysts+for+bio-oil+upgrading+via+"ex+situ+catalytic+fast+pyrolysis":+catalyst+development+through+the+study+of+model+compounds.">Recent advances in heterogeneous catalysts for bio-oil upgrading via "ex situ catalytic fast pyrolysis": catalyst development through the study of model compounds.</a> Green Chem. 16 (2), 454-490 (2014).</li><li>Dutta, A., Schaidle, J. A., Humbird, D., Baddour, F. G., Sahir, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Conceptual+Process+Design+and+Techno-Economic+Assessment+of+Ex+Situ+Catalytic+Fast+Pyrolysis+of+Biomass:+A+Fixed+Bed+Reactor+Implementation+Scenario+for+Future+Feasibility.">Conceptual Process Design and Techno-Economic Assessment of Ex Situ Catalytic Fast Pyrolysis of Biomass: A Fixed Bed Reactor Implementation Scenario for Future Feasibility.</a> Top. Catal. 59 (1), 2-18 (2016).</li><li>Venkatakrishnan, V. K., Delgass, W. N., Ribeiro, F. H., Agrawal, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Oxygen+removal+from+intact+biomass+to+produce+liquid+fuel+range+hydrocarbons+via+fast-hydropyrolysis+and+vapor-phase+catalytic+hydrodeoxygenation.">Oxygen removal from intact biomass to produce liquid fuel range hydrocarbons via fast-hydropyrolysis and vapor-phase catalytic hydrodeoxygenation.</a> Green Chem. 17 (1), 178-183 (2015).</li><li>Bej, S. K., Thompson, L. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Acetone+condensation+over+molybdenum+nitride+and+carbide+catalysts.">Acetone condensation over molybdenum nitride and carbide catalysts.</a> Appl. Catal., A. 264 (2), 141-150 (2004).</li><li>Sullivan, M. M., Held, J. 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. S., 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=Chemical+Titration+and+Transient+Kinetic+Studies+of+Site+Requirements+in+Mo2C-Catalyzed+Vapor+Phase+Anisole+Hydrodeoxygenation.">Chemical Titration and Transient Kinetic Studies of Site Requirements in Mo2C-Catalyzed Vapor Phase Anisole Hydrodeoxygenation.</a> ACS Catal. 5 (7), 4104-4114 (2015).</li><li>Ren, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+Hydrodeoxygenation+of+Biomass-Derived+Oxygenates+to+Unsaturated+Hydrocarbons+using+Molybdenum+Carbide+Catalysts.">Selective Hydrodeoxygenation of Biomass-Derived Oxygenates to Unsaturated Hydrocarbons using Molybdenum Carbide Catalysts.</a> Chemsuschem. 6 (5), 798-801 (2013).</li><li>Grob, R. L., Kaiser, M. 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. G., Nash, C. P., Schaidle, J. A., Ruddy, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+&#945;-MoC1-x+Nanoparticles+with+a+Surface-Modified+SBA-15+Hard+Template:+Determination+of+Structure-Function+Relationships+in+Acetic+Acid+Deoxygenation.">Synthesis of &#945;-MoC1-x Nanoparticles with a Surface-Modified SBA-15 Hard Template: Determination of Structure-Function Relationships in Acetic Acid Deoxygenation.</a> Angew. Chem., Int. Ed. n/a-n/a. , (2016).</li><li>Habas, S. E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Facile+Molecular+Precursor+Route+to+Metal+Phosphide+Nanoparticles+and+Their+Evaluation+as+Hydrodeoxygenation+Catalysts.">A Facile Molecular Precursor Route to Metal Phosphide Nanoparticles and Their Evaluation as Hydrodeoxygenation Catalysts.</a> Chem. Mater. 27 (22), 7580-7592 (2015).</li><li>Zhang, Q., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deconvolution+and+quantification+of+hydrocarbon-like+and+oxygenated+organic+aerosols+based+on+aerosol+mass+spectrometry.">Deconvolution and quantification of hydrocarbon-like and oxygenated organic aerosols based on aerosol mass spectrometry.</a> Environ Sci Technol. 39 (13), 4938-4952 (2005).</li><li>Ko, E. I., Benziger, J. B., Madix, R. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+of+Methanol+on+W(100)+and+W(100)-(5+X+1)C+Surfaces.">Reactions of Methanol on W(100) and W(100)-(5 X 1)C Surfaces.</a> J Catal. 62 (2), 264-274 (1980).</li><li>Pestman, R., Koster, R. M., Pieterse, J. A. Z., Ponec, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+of+carboxylic+acids+on+oxides:+1.+Selective+hydrogenation+of+acetic+acid+to+acetaldehyde.">Reactions of carboxylic acids on oxides: 1. Selective hydrogenation of acetic acid to acetaldehyde.</a> J Catal. 168 (2), 255-264 (1997).</li><li>Pestman, R., Koster, R. M., Van Duijne, A., Pieterse, J. A. Z., Ponec, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+of+carboxylic+acids+on+oxides:+2.+Bimolecular+reaction+of+aliphatic+acids+to+ketones.">Reactions of carboxylic acids on oxides: 2. Bimolecular reaction of aliphatic acids to ketones.</a> J Catal. 168 (2), 265-272 (1997).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NIST+Standard+Reference+Database+Number+69.">NIST Standard Reference Database Number 69.</a> NIST Chemistry WebBook. , (2016).</li><li>Ausloos, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+critical+evaluation+of+a+comprehensive+mass+spectral+library.">The critical evaluation of a comprehensive mass spectral library.</a> J. Am. Soc. Mass Spectrom. 10 (4), 287-299 (1999).</li><li>Barwick, V., Langley, J., Mallet, T., Stein, B., Webb, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Best Practice Guide for Generating Mass Spectra. , (2006).</li><li>Lecchi, P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Method+for+Monitoring+and+Controlling+Reproducibility+of+Intensity+Data+in+Complex+Electrospray+Mass+Spectra:+A+Thermometer+Ion-based+Strategy.">A Method for Monitoring and Controlling Reproducibility of Intensity Data in Complex Electrospray Mass Spectra: A Thermometer Ion-based Strategy.</a> J. Am. Soc. Mass Spectrom. 20 (3), 398-410 (2009).</li></ol>

Den TPRxn metoden er et kraftfuldt værktøj til screening af katalytiske materialer, der giver oplysninger om aktivitet og selektivitet af en katalysator som en funktion af reaktionstemperaturen. Andre temperatur-programmerede metoder såsom TPD, TPO og TPR kan give oplysninger om adsorption styrken af ​​reaktanter, antal adsorptionssteder, og passende katalysator procedurer før behandlingen, men giver ikke direkte katalytiske data ydeevne. Det er vigtigt at bemærke, at TPRxn metoden beskrevet i dette arbejde ikk...

Temperatur programmeret reaktion (TPRxn) er en af ​​mange temperatur programmeret metoder, herunder desorption (TPD), oxidation (TPO), og reduktion (TPR), og fortsætter via eksponering af en katalysator til en reaktant samtidig med eller efterfulgt af en støt stigning i temperatur. 1, 2, 3 TPRxn er en forbigående teknik, der giver oplysninger om katalysatoraktivitet og selektivitet som en funktion af reaktionstemperaturen. 4, 5, 6 Det er også en populær teknik: en søgning på søgeordene &#39;temperatur programmeret reaktion &quot;i litteraturen udbytter over 1.000 kilder angivelse af dens brug. TPRxn eksperimenter udføres typisk i et mikroreaktor, som er udstyret med et massespektrometer (MS) for real-time analyse af reaktoren spildevand og korrelation af pPFYLDELSE med temperaturen. Reaktantgasser kan indføres med massestrøm controllere og væsker kan indføres via en sprøjtepumpe eller som dampe ved at boble inert gas gennem en væske. Katalysatoren ofte forbehandles in situ til dannelse af den ønskede katalytiske fase til reaktionen. Nogle systemer er udstyret med ekstra analyseudstyr, ud over den typiske massespektrometer, at give kvantitative eller kvalitative oplysninger om katalysator selektivitet, overflade arter til stede på katalysatoren, eller reaktionsmekanisme. For eksempel, temperatur programmeret in situ Fourier Transform infrarød spektroskopi (FTIR) indeholder oplysninger om udviklingen af overflade arter med varierende reaktion temperatur. 7, 8 TPRxn demonstreret i dette arbejde er udstyret med en gas chromatogram (GC) ud over de mere typiske MS. Denne GC, udstyret med fire parallelle søjler, giver mulighed for mere præcis kvantifikation af reaktionsprodukterne, men er begrænset i analysen frekvens med den tid, det tager produkterne til eluering gennem søjlerne. Således kan kombinationen af ​​MS og GC være særlig nyttige til kobling identifikation realtid med nøjagtig kvantificering af reaktanter og produkter. Her anvender vi den TPRxn metode til at undersøge deoxygenering af eddikesyre på molybdæncarbid katalysatorer. Dette er en interessant og vigtig reaktion i katalysatoren forskning, som eddikesyre er en nyttig analog for de mange carboxylsyrer stede i biomasse pyrolysedampene. 9 Det høje iltindhold i biomasse pyrolysedampene nødvendiggør fjernelse oxygen til frembringelse af carbonhydridbrændstoffer, 10, 11, 12 og molybdæn hårdmetal katalysatorer har vist lovende deoxygenering ydeevne til mange biomasse pyrolyse damp model forbindelser, herunder furfural, 1-propanol,phenoler og eddikesyre. 9, 13, 14, 15, 16 imidlertid aktiviteten og selektiviteten af molybdæncarbid katalysatorer i deoxygenering reaktioner er afhængig af katalysatoren struktur og sammensætning, de reagerende arter og reaktionsbetingelserne. De indsamlede fra TPRxn eddikesyre data viser, at molybdæn carbid katalysatorer er aktive til deoxygenering reaktioner over ca. 300 ° C, og når de kombineres med katalysator karakterisering information muliggør kvantificering af katalysatoraktiviteten som funktion af temperaturen via beregning af eddikesyre omsætningshastigheder. De TPRxn Resultaterne viser, at iltsvind (dvs., CO bond-breaking) produkter er begunstiget ved temperaturer under ca. 400 ° C og decarbonylation (dvs. CC bond-breaking) produkter er favorød ved temperaturer over ca. 400 ° C. Derudover TPRxn undersøgelser illustrerer ændringer i aktiviteten og selektiviteten af molybdæncarbidproduktet katalysatorer fremstillet under anvendelse af forskellige syntetiske procedurer (dvs. produktion af forskellige molybdæncarbid katalysatorstrukturer og sammensætninger). Stadig, at værdien af ​​disse oplysninger og mere generelt den vellykkede anvendelse af TPRxn eksperimentelle data mod katalysator design og procesoptimering er en funktion af kvaliteten af ​​de opnåede data. Omhyggelig overvejelse og viden om de potentielle vanskeligheder og begrænsninger fremhævet hele TPRxn procedure er altafgørende.

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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 programmeret reaktion (TPRxn) er en simpel endnu kraftfulde værktøj til screening fast katalysator ydeevne på en række betingelser. En TPRxn Systemet omfatter en reaktor, ovn, gas og damp kilder, flow control, instrumentering at kvantificere reaktionsprodukter (fx gaskromatograf) og instrumentering til at overvåge reaktionen i realtid (fx massespektrometer). Her anvender vi den TPRxn metode til at studere molybdæncarbid katalysatorer til deoxygenering af eddikesyre, en vigtig reaktion blandt mange i opgradering / stabilisering af biomasse pyrolysedampene. TPRxn anvendes til at evaluere katalysatoraktivitet og selektivitet og afprøve hypotetiske reaktionsveje (f.eks decarbonylation, ketonization, og hydrogenering). Resultaterne af TPRxn undersøgelse af eddikesyre deoxygenering viser, at molybdæncarbidproduktet er en aktiv katalysator til denne reaktion ved temperaturer over ca. 300 ° C, og at reaktionen favorisereriltsvind (dvs. CO bond-breaking) produkter ved temperaturer under ca. 400 ° C og decarbonylation (dvs. CC obligation-breaking) produkter ved temperaturer over ca. 400 ° C.

Online MS giver mulighed for at analysere gassammensætningen ved reaktoren i realtid. Den online MS ikke er koblet med en enhed til at adskille produkter før analyse, og dermed identifikation arter er udfordrende at differentiere mellem forbindelser med overlappende masse fragmenteringsmønstre. Som vist i tabel 2, mange af de fælles produkter fra eddikesyre TPRxn eksperimenter er kendetegnet ved multiple fælles m / z signaler. Udfoldning af MS-data (m / z = 1 - 100 ...

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

Præsenteret her er en protokol til driften af ​​en mikro-skala temperatur-programmeret reaktor til vurdering af den katalytiske ydeevne af molybdæn hårdmetal under eddikesyre iltsvind.

Temperatur-programmeret iltsvind i eddikesyre på Molybdæn 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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Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

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

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

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

Kontinuert Flow kemi: Reaktion af 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

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 ...

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

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 ...