Name: millifluidics for chemical synthesis and time-resolved mechanistic studies
Uploaded: 2013-11-27T20:00:00
Description: Watch this Scientific Journal Video about Millifluidics for Chemical Synthesis and Time-resolved Mechanistic Studies at JoVE.com

Denne forskning arbejde understøttes som en del af Center for Atomic Level Catalyst Design, en Energy Frontier Research Center finansieret af det amerikanske Department of Energy, Office of Science, Kontoret for Basic Energi Videnskaber under Award Number DE-SC0001058 og støttes også af bestyrelse Regents under tilskud tildeling nummer LEQSF (2009-14)-EFRC-MATCH og LEDSF-EPS (2012)-OPT-IN-15. MRCAT funktioner er understøttet af Institut for Energi og MRCAT medlemsinstitutioner. Brugen af ​​Advanced Foton Kilde ved ANL understøttes af det amerikanske Department of Energy, Office of Science, Kontoret for Basic Energi Sciences, under kontrakt nr. DE-AC02-06CH11357. Finansiel støtte til JTM blev givet som en del af Institut for Atom-effektive kemiske omdannelser (IACT), en Energy Frontier Research Center finansieret af det amerikanske Department of Energy, Office of Science, Kontoret for Basic Energi Sciences.

Millifluidics set-up: Køb et millifluidic chip (lavet af polyesterterephthalat polymer) fra Microplumbers Microsciences LLC, som har Serpentine kanaler med dimensioner 2 mm (B) x 0,15 mm (H) x 220 mm (L). Brug FEP Tubing med dimensionerne 0,25 mm ID, 1/16 i OD, til at forbinde chippen til pumpen. Brug to forskellige pumper til de to forskellige eksperimenter. Brug P-Pumpe til det første eksperiment (kobber nanopartikler) og millifluidic enhed til det andet eksperiment (guld nanopartikler). For at mini...

<ol>
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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Developing+Millifluidic+Platform+for+Synthesis+of+Ultra-small+Nanoclusters+(UNCs):+Ultra-small+Copper+Nanoclusters+(UCNCs)+as+a+Case+Study.">Developing Millifluidic Platform for Synthesis of Ultra-small Nanoclusters (UNCs): Ultra-small Copper Nanoclusters (UCNCs) as a Case Study.</a> Small. 8 (5), 688-698 (2012).</li><li>Li, Y., Sanampudi, A., Reddy, V. R., Biswas, S., Nandakumar, K., Yamane, D. G., Goettert, J. S., Kumar, C. S. S. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size+Evolution+of+Gold+Nanoparticles+in+a+Millifluidic+Reactor.">Size Evolution of Gold Nanoparticles in a Millifluidic Reactor.</a> Phys. Chem. Phys. 13 (1), 177-182 (2012).</li><li>Li, Y., Yamane, D. G., Li, S., Biswas, S., Reddy, R., Goettert, J. S., Nandakumar, K., Kumar, C. 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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Microfluidic Devices in nanotechnology-Fundamental Concepts. , (2010).</li><li>Meille, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Review+on+Methods+to+Deposit+Catalysts+on+Structured+Surfaces.">Review on Methods to Deposit Catalysts on Structured Surfaces.</a> Appl. Catal. A Gen. 315, 1-17 (2006).</li><li>Shin, W. C., McDonald, J. A., Zhao, S., Besser, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Etching+Characteristics+of+a+Micromachined+Chemical+Reactor+Using+Inductively+Coupled+Plasma.">Etching Characteristics of a Micromachined Chemical Reactor Using Inductively Coupled Plasma.</a> , p357 (2002).</li><li>Abahmane, L., K&#246;hler, J. M., Gro&#223;, G. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gold-nanoparticle-catalyzed+synthesis+of+propargylamines:+the+traditional+A3-multicomponent+reaction+performed+as+a+two-step+flow+process.">Gold-nanoparticle-catalyzed synthesis of propargylamines: the traditional A3-multicomponent reaction performed as a two-step flow process.</a> Chem. Eur. J. 17, 3005-3010 (2011).</li><li>Abahmane, L., Knauer, A., Ritter, U., K&#246;hler, J. M., Gro&#223;, G. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Heterogeneous+Catalyzed+Pyridine+Synthesis+using+Montmorillionite+and+Nanoparticle-Impregnated+Alumina+in+a+Continuous+Micro+Flow+System.">Heterogeneous Catalyzed Pyridine Synthesis using Montmorillionite and Nanoparticle-Impregnated Alumina in a Continuous Micro Flow System.</a> Chem. Eng. Technol. 32, 1799-1805 (2009).</li><li>Abahmane, L., Knauer, A., K&#246;hler, J. M., Gro&#223;, G. 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+polypyridine+derivatives+using+alumina+supported+gold+nanoparticles+under+micro+continuous+flow+conditions.">Synthesis of polypyridine derivatives using alumina supported gold nanoparticles under micro continuous flow conditions.</a> Chem. Eng. J. 167, 519-526 (2011).</li><li>Negishi, Y., Tsukuda, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-Pot+Preparation+of+Subnanometer-Sized+Gold+Clusters+via+Reduction+and+Stabilization+by+meso-2,3-Dimercaptosuccinic+Acid.">One-Pot Preparation of Subnanometer-Sized Gold Clusters via Reduction and Stabilization by meso-2,3-Dimercaptosuccinic Acid.</a> J. Am. Chem. Soc. 125, 4046-4047 (2003).</li><li>Abou-Hassan, A., Sandre, O., Cabuil, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidics+in+Inorganic+Chemistry.">Microfluidics in Inorganic Chemistry.</a> Angew. Chem. Int. Ed. 49, 6268-6286 (2010).</li><li>Jiang, D., Walter, M., Dai, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gold+Sulfide+Nanoclusters:+A+Unique+Core-In-Cage+Structure.">Gold Sulfide Nanoclusters: A Unique Core-In-Cage Structure.</a> Chem. Eur. J. 16, 4999-5003 (2010).</li><li>Kuroda, K., Ishida, T., Haruta, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reduction+of+4-nitrophenol+to+4-aminophenol+over+Au+nanoparticles+deposited+on+PMMA.">Reduction of 4-nitrophenol to 4-aminophenol over Au nanoparticles deposited on PMMA.</a> J. Mol. Catal. A Chem. 298, 7-11 (2009).</li><li>Navin, C. V., Krishna, K. S., Theegala, C. S., Kumar, C. S. S. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lab-on-a-chip+devices+for+gold+nanoparticle+synthesis+and+their+role+as+a+catalyst+support+for+continuous+flow+catalysis.">Lab-on-a-chip devices for gold nanoparticle synthesis and their role as a catalyst support for continuous flow catalysis.</a> Nanotech. 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De UCNCs blev dannet ved reduktionsreaktionen kobbernitrat med natriumborhydrid i nærværelse af det polymere endeafslutningsmiddel O-[2 - (3-Mercaptopropionylamino) ethyl]-O&#39;-methylpolyethylenglycol (MW = 5,000) [MPEG]. Reaktionen blev udført inden for den millifluidic chip reaktor ved forskellige strømningshastigheder, såsom 6,8 ml / time, 14,3 ml / time, 32,7 ml / time, og 51,4 ml / time for at studere effekten af ​​strømningshastigheder på UCNCs dannes. De respektive opholdstider for ovennævnte flowha...

Lab-on-a-chip (LOC) enheder til kemisk syntese har vist signifikant fordel i form af øget masse og varmeoverførsel, overlegen reaktion kontrol, high throughput og sikrere drift miljø 1. Disse enheder kan groft inddeles i chip baserede fluidik og nonchip baseret fluidic enheder. Blandt de chip-baserede fluidik er mikrofluidik godt undersøgt, og et emne godt dækket i litteraturen 2-5. Nonchip baseret LOC systemer bruger rørreaktorer 6. Konventionelt mikrofluide systemer anvendes til præcis styring og håndtering af væsker, der er geometrisk begrænsede til submillimeter skala. Vi har for nylig indført begrebet chipbaserede millifluidics, som kan anvendes til manipulation af væsker i kanaler i millimeterskala (enten bredde eller dybde eller begge af kanalerne er mindst en millimeter i størrelse) 7-9. Desuden er relativt let at fremstille whi de millifluidic chipsle tilbyde lignende kontrol over flowhastigheder og manipulation af reagenser. Disse chips kan også betjenes ved højere strømningshastigheder, skaber mindre opholdstider dermed giver mulighed for opskalering af kontrolleret syntese af nanopartikler med snævrere størrelsesfordeling. Som et eksempel har vi for nyligt vist, at syntesen af ultrasmå kobber nanoklynger og karakteriseret dem ved hjælp af in situ-røntgen-absorptionsspektroskopi samt TEM. Evne til at opnå små opholdstider inden millifluidic kanaler i kombination med anvendelsen af MPEG, som er meget effektiv bidentat PEGyleret stabiliserende middel til dannelse af stabile kolloider af kobber nanoklynger 7. Ud over syntesen af ​​kemikalier og nanomaterialer, kunne millifluidics tilbyder, på grund af større volumen og koncentration ved sonden, et syntetisk platform, der er mere generel og effektiv for tidsopløst kinetikstudier og også achieves bedre signal-støj-forhold end mikrofluide systemer 7,10 til. Vi viser anvendelsen af millifluidic chip som et eksempel på tidsopløst analyse af væksten af guld nanostrukturer fra opløsning under anvendelse af in situ XAS med en tidsopløsning så lille som 5 msek 11. Desuden er størstedelen af de mikro-reaktorer, der er udviklet til dato for katalyse applikationer baseret på silicium 12,13. Deres dyre fabrikation i tillæg til små volumener genereres gør dem uegnede til stor skala produktion. De to generelle metoder til at overtrække kanaler med nanocatalysts - kemiske og fysiske, der ofte omtales som silicium belægning procedurer, er i øjeblikket på mode 14,15. Ud over dyre mikro fabrikation, tilstopning af kanalerne gør mikroreaktor katalyse kan være uegnet til fremstilling i stor skala. Selv mikroreaktorer har været brugt til heterogen katalyse i mikro kontinuerlig gennemstrømning processer earliare 16-18, blev evnen til at styre dimensionen, og morfologi af de indlejrede guld nanostrukturerede katalysatorer inden kontinuerlige strømningskanaler udforsket aldrig før. Vi har for nylig udviklet en teknologi til at overtrække millifluidic kanaler med Au-katalysatorer, at det er kontrolleret nano morfologi og dimensioner (figur 5) 11, til udførelse af katalyse af industrielt vigtige kemiske reaktioner. Som et eksempel har vi vist, omdannelse af 4-nitrophenol i 4-aminophenol katalyseret af nanostrukturerede guldbelagt inden millifluidic kanaler. I betragtning af at en enkelt millifluidic reaktor chip kan producere strømningshastigheder på 50-60 ml / time, 7 high-throughput og kontrolleret syntese af kemikalier er muligt enten ved kontinuerligt flow drift eller parallel behandling. For at udnytte de muligheder millifluidics tilbyder, med få beskrevet som ovenfor eksempler vi også vise en brugervenligmillifluidic enhed, der er transportabel og har alle de nødvendige komponenter såsom millifluidic chips, mangfoldigheder, flow controllere, pumper og elektriske forbindelser integreret. En sådan millifluidic enhed, som vist i figur 7, er nu tilgængelig fra firmaet Millifluidica LLC ( <a href="http://www.millifluidica.com" target="_blank">www.millifluidica.com</a> ). Håndskriftet tilvejebringer også protokoller anvender håndholdte millifluidic enhed, som beskrevet nedenfor, til styret syntese af nanomaterialer tidsopløst analyse af reaktionsmekanismer og kontinuerlig strøm katalyse.

<table border="1">
	<tbody>
		<tr>
			<td>Copper (II) nitrate hydrate</td>
			<td>Sigma-Aldrich</td>
			<td>13778-31-9</td>
			<td>99.999% pure</td>
		</tr>
		<tr>
			<td>O-[2-(3-mercaptopropionylamino)ethyl]-O&#8242;-methylpolyethylene glycol</td>
			<td>Sigma-Aldrich</td>
			<td>401916-61-8&#160;</td>
			<td>MW=5,000</td>
		</tr>
		<tr>
			<td>HAuCl4.3H2O (Chloroauric acid)</td>
			<td>Sigma-Aldrich</td>
			<td>27988-77-8&#160;</td>
			<td>99.999% pure</td>
		</tr>
		<tr>
			<td>meso-2,3-dimercaptosuccinic acid (DMSA)</td>
			<td>Sigma-Aldrich</td>
			<td>304-55-2</td>
			<td>~98% pure</td>
		</tr>
		<tr>
			<td>4-Nitrophenol</td>
			<td>Sigma-Aldrich</td>
			<td>100-02-7&#160;</td>
			<td>spectrophotometric grade</td>
		</tr>
		<tr>
			<td>4-Aminophenol</td>
			<td>Sigma-Aldrich</td>
			<td>123-30-8&#160;</td>
			<td>&#62;99% pure (HPLC grade)</td>
		</tr>
		<tr>
			<td>Sodium borohydride</td>
			<td>Sigma-Aldrich</td>
			<td>16940-66-2&#160;</td>
			<td>98% pure</td>
		</tr>
		<tr>
			<td>Sodium hydroxide pellets</td>
			<td>Sigma-Aldrich</td>
			<td>1310-73-2&#160;</td>
			<td>99.99% pure</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>[header]</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>EQUIPMENT</td>
		</tr>
		<tr>
			<td>Millifluidic Chips</td>
			<td>Microplumbers Microsciences LLC</td>
			<td>SDC-01</td>
			<td>Made from polyester terephthalate polymer</td>
		</tr>
		<tr>
			<td>Pressure Pump</td>
			<td>Mitos P-Pump, Dolomite</td>
			<td>3200016</td>
			<td></td>
		</tr>
		<tr>
			<td>Automated Syringe Pump</td>
			<td>Cetoni Automation and Microsystems, GmbH</td>
			<td></td>
			<td>Syringe pump neMESYS</td>
		</tr>
		<tr>
			<td>UV-3600 UV-VIS-NIR Spectrophotometer</td>
			<td>Shimadzu</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Hand-held Millifluidic Device</td>
			<td>Millifluidica</td>
			<td>SCMD-1008</td>
			<td>Figure 7</td>
		</tr>
	</tbody>
</table>

millifluidics for chemical synthesis and time-resolved mechanistic studies

Procedurer, som anvender millifluidic udstyr til kemisk syntese og tidsopløste mekanistiske undersøgelser er beskrevet ved at tage tre eksempler. I den første, er syntese af ultra-små kobber nanoclusters beskrevet. Det andet eksempel giver deres anvendelighed til undersøgelse tid løst kinetik kemiske reaktioner ved at analysere guld nanopartikel dannelse ved hjælp af in situ røntgen absorption spektroskopi. Det sidste eksempel viser kontinuerlig strøm katalyse af reaktioner inde millifluidic kanal overtrukket med nanostrukturerede katalysator.

Godt spredt og ensartede mellemstore kobber nanoclusters med en snæver størrelsesfordeling blev opnået ved hjælp af den millifluidic chip setup (fig. 1a). De forskellige strømningshastigheder, der anvendes til syntese ikke har en væsentlig indvirkning på størrelsen af ​​de klynger. Ikke desto mindre, med stigning i strømningshastighed, der er en observerbar forbedring i indsnævringen af ​​størrelsesfordelingen. UCNCs med en bedste snæver størrelsesfordeling blev opnået ved en strømningshastighed p...

Watch this Scientific Journal Video about Millifluidics for Chemical Synthesis and Time-resolved Mechanistic Studies at JoVE.com

Millifluidics for Chemical Synthesis and Time-resolved Mechanistic Studies

Millifluidic enheder er brugt til styret syntese af nanomaterialer, tidsopløst analyse af reaktionsmekanismer og kontinuerlig strøm katalyse.

Millifluidics til kemisk syntese og tidsopløste mekanistiske undersøgelser

Procedures utilizing millifluidic devices for chemical synthesis and time-resolved mechanistic studies are described by taking three examples. In the ...

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Injectable biomaterials are defined as implantable materials that can be introduced into the body as a liquid and solidify in situ. Such materials offer ...

The Synthesis of RGD-functionalized Hydrogels as a Tool for Therapeutic Applications

Syntesen af ​​RGD-funktionaliserede Hydrogeler som værktøj for terapeutiske applikationer

The use of polymers as biomaterials has provided significant advantages in therapeutic applications. In particular, the possibility to modify and ...

Polydimethylsiloxane-polycarbonate Microfluidic Devices for Cell Migration Studies Under Perpendicular Chemical and Oxygen Gradients

Polydimethylsiloxan-polykarbonat mikrofluidenheder for Cell Migrationsstudier Under Perpendicular Kemiske og Oxygen farveforløb

This paper reports a microfluidic device made of polydimethylsiloxane (PDMS) with an embedded polycarbonate (PC) thin film to study cell migration under ...

Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

Syntese af Hydrogeler med antitilsmudsningsegenskaber som membraner til vandrensning

Hydrogels have been widely utilized to enhance the surface hydrophilicity of membranes for water purification, increasing the antifouling properties and ...

Ammonia Synthesis at Low Pressure

Ammoniak syntese ved lavt tryk

Ammonia can be synthesized at low pressure by the use of an ammonia selective absorbent. The process can be driven with wind energy, available locally in ...