Name: synthesis and reaction chemistry of nanosize monosodium titanate
Uploaded: 2016-02-23T14:00:00
Description: Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

The authors thank the Laboratory Directed Research and Development program at the Savannah River National Laboratory (SRNL) for funding. We thank Dr. Fernando Fondeur for collection and interpretation of the FT-IR spectra and Dr. John Seaman of the Savannah River Ecology Laboratory for the use of the DLS instrument for particle size measurements. We also thank the Dr. Daniel Chan of the University of Washington and the National Institute of Health (Grant #1R01DE021373-01), for funding experiments investigating the ion exchange reactions with Au(III). The Savannah River National Laboratory is operated by Savannah River Nuclear Solutions, LLC for the Department of Energy under contract DE-AC09-08SR22470.

1. Sintesi di Nano-monosodico titanato (nMST) <ol><li> Preparare 10 ml di soluzione # 1 aggiungendo 0,58 ml di 25% in peso una soluzione di sodio metilato al 7,62 ml di isopropanolo seguito da 1,8 ml del titanio isopropossido. </li><li> Preparare 10 ml di soluzione # 2 aggiungendo 0,24 ml di acqua ultrapura a 9,76 ml di isopropanolo. </li><li> Aggiungere 280 ml di isopropanolo in un pallone a fondo rotondo a 3 colli da 500 ml, seguito da 0,44 ml di Triton X-100 (media MW: 625 g / mol). Agitare bene la soluzione con un...

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La presenza di acqua estranea, per esempio da reagenti impuri, può alterare il risultato della reazione, portando a particelle più grandi o più polidispersi. Pertanto, occorre prestare attenzione per garantire reagenti secchi vengono utilizzati. Il isopropossido titanio e metossido di sodio devono essere conservati in un essiccatore quando non in uso. Elevata purezza isopropanolo dovrebbe anche essere utilizzato per la sintesi. Temperatura stata trovata a svolgere un ruolo chiave nella co...

Biossido di titanio e metalli alcalini titanati sono ampiamente utilizzati in una varietà di applicazioni come pigmenti di vernice e la cura della pelle e come fotocatalizzatori nella conversione dell&#39;energia e utilizzazione. Hanno dimostrato 1-3 titanati sodio essere materiali efficaci per rimuovere una gamma di cationi su una vasta gamma di condizioni di pH attraverso reazioni di scambio cationico. 4-7 Oltre alle applicazioni appena descritti, micron dimensioni titanati di sodio e sodio peroxotitanates hanno recentemente dimostrato di servire anche come una piattaforma di distribuzione di metallo terapeutico. In questa applicazione, ioni metallici terapeutiche come Au (III), Au (I) e Pt (II) sono scambiati con gli ioni di sodio di monosodico titanato (MST). In vitro con i titanati metallo scambiate nobili indicano soppressione di la crescita del cancro e cellule batteriche mediante un meccanismo sconosciuto. 8,9 Storicamente, titanati sodio hanno essereen prodotta utilizzando sia sol-gel e tecniche di sintesi idrotermali conseguente polveri fini con dimensioni delle particelle variano da pochi a diverse centinaia di micron. 4,5,10,11 Più recentemente, metodi di sintesi sono stati segnalati che produceva nanodimensioni biossido di titanio, metallo- ossidi di titanio drogate, e una varietà di altri titanati metallici. Esempi includono sodio nanotubi di ossido di titanio (NaTONT) o nanofili mediante reazione di biossido di titanio in idrossido di sodio in eccesso, a temperatura e pressione elevate, 12-14 sodio nanofibre titanato di reazione di acido peroxotitanic con idrossido di sodio in eccesso a temperatura elevata e pressione, 15 e sodio e cesio nanofibre di delaminazione di titanati acido scambiati micron di dimensioni titanato. 16 La sintesi di titanati nanodimensioni di sodio e peroxotitanates sodio è di interesse per migliorare la cinetica di scambio ionico, che sono tipicamente controllate per diffusione pellicola o diffu intraparticellaresione. Questi meccanismi sono in gran parte controllate dalla dimensione delle particelle dello scambiatore di ioni. Inoltre, come una piattaforma di distribuzione di metallo terapeutica, la dimensione delle particelle del materiale titanato sarebbe dovrebbe influenzare significativamente la natura dell&#39;interazione tra il titanato metallo scambiate e il cancro e cellule batteriche. Ad esempio, cellule batteriche, che sono tipicamente dell&#39;ordine di 0,5 - 2 ìm, sarebbe probabilmente diverse interazioni con particelle di dimensioni micron contro particelle di dimensioni nanometriche. Inoltre, è stato dimostrato cellule eucariotiche non fagocitiche di internalizzare solo particelle di dimensioni inferiori a 1 micron. 17 Pertanto, la sintesi di titanati sodio nanosize è interessante anche per facilitare l&#39;erogazione metallo e assorbimento cellulare dalla piattaforma consegna titanato. La riduzione delle dimensioni dei titanati sodio e peroxotitanates aumenterà anche la capacità effettiva in separazioni di ioni metallici e migliorare le proprietà fotochimiche del materiale. 16,18 &lt;/ sup&gt; Questo documento descrive un protocollo sviluppato per sintetizzare nanodimensioni monosodico titanato (nMST) in condizioni sol-gel mite 19 La preparazione del corrispondente perossido modificato nMST.; insieme ad una reazione di scambio ionico per caricare il nMST con Au (III) sono descritti anche.

<table border="0" cellpadding="0" cellspacing="0" width="923">
	<tbody>
		<tr>
			<td>Titanium(IV) isopropoxide</td>
			<td>Sigma Aldrich</td>
			<td>377996</td>
			<td>99.999% trace metals basis</td>
		</tr>
		<tr>
			<td>Isopropyl alcholol, 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>650447</td>
			<td>HPLC grade (Chomasolv)</td>
		</tr>
		<tr>
			<td>Sodium methoxide in methanol</td>
			<td>Sigma Aldrich</td>
			<td>156256</td>
			<td>25 wt%</td>
		</tr>
		<tr>
			<td>Triton X-100</td>
			<td>Sigma Aldrich</td>
			<td>T9284</td>
			<td>BioXtra</td>
		</tr>
		<tr>
			<td>hydrogen tetrachloroaurate(III) trihydrate</td>
			<td>Sigma Aldrich</td>
			<td>G4022</td>
			<td>ACS reagent grade</td>
		</tr>
		<tr>
			<td>hydrogen peroxide (30 wt%)</td>
			<td>Fisher</td>
			<td>H325</td>
			<td>Certified ACS</td>
		</tr>
		<tr>
			<td>10-mL syringes</td>
			<td>Fisher</td>
			<td>14-823-16E</td>
			<td></td>
		</tr>
		<tr>
			<td>Dual channel syringe pump</td>
			<td>Cole Parmer</td>
			<td>EW-74900-10</td>
			<td>Or equivalent programmable dual channel syringe pump</td>
		</tr>
		<tr>
			<td>Tygon tubing 1/8 inch ID, 1/4 inch OD</td>
			<td>Cole Parmer</td>
			<td>EW-0640776</td>
			<td></td>
		</tr>
		<tr>
			<td>Tygon tubing 1/16 inch ID, 1/8 inch OD</td>
			<td>Cole Parmer</td>
			<td>EW-0740771</td>
			<td></td>
		</tr>
		<tr>
			<td>0.1-&#181;m Nylon filter</td>
			<td>Fisher</td>
			<td>R01SP04700</td>
			<td></td>
		</tr>
		<tr>
			<td>Labquake shaker rotisserie</td>
			<td>Thermo Scientific</td>
			<td>4002110Q</td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis and reaction chemistry of nanosize monosodium titanate

Questo documento descrive la sintesi e perossido-modifica di nanodimensioni monosodico titanato (nMST), oltre ad una reazione di scambio ionico per caricare il materiale con Au ioni (III). Il metodo di sintesi è stato derivato da un processo sol-gel utilizzato per produrre micron dimensioni monosodico titanato (MST), con diverse modifiche chiave, tra alterando le concentrazioni dei reagenti, omettendo un passo seme particelle, e introducendo un tensioattivo non ionico per facilitare il controllo della la formazione di particelle e la crescita. Il materiale nMST risultante presenta la morfologia delle particelle di forma sferica con una distribuzione monodisperse di diametri delle particelle nell&#39;intervallo da 100 a 150 nm. Il materiale nMST risulta avere una superficie Brunauer-Emmett-Teller (BET) di 285 m 2 g -1, che è più di un ordine di grandezza superiore al micron dimensioni MST. Il punto isoelettrico del nMST misurato 3,34 unità di pH, che è una unità di pH inferiore a quello misurato per il micron-size MST. Tsi nMST materiale è stato trovato per servire come un efficace scambio ionico in condizioni debolmente acide per la preparazione di un Au (III) -scambio nanotitanate. Inoltre, la formazione del peroxotitanate corrispondente è stata dimostrata per reazione del nMST con acqua ossigenata.

MST è sintetizzato utilizzando un metodo sol-gel in cui tetraisopropoxytitanium (IV) (Tipt), metossido di sodio e acqua sono combinati e reagiva in isopropanolo per formare particelle seme di MST. 4 particelle Micron dimensioni vengono quindi coltivate mediante aggiunta controllata di ulteriori quantità dei reagenti. Le particelle risultanti presentano un nucleo amorfo e una regione fibroso esterno avente dimensioni di circa 10 nm di larghezza per 50 nm di lunghezza. 20 <p class="jove_content...

Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

Sintesi e Reazione chimica della nanosize monosodico titanato

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the ...

The overall goal of the following experiment is to prepare nanosized sodium titanate materials including peroxide-modified and gold(III)loaded materials. This is achieved by first performing a surfactant-mediated sol-gel synthesis to prepare nanosized monosodium titanate particles in the range of 100 to 150 nanometers. As a second step, the nanosized monosodium titanate can be treated with hydrogen peroxide which converts a portion of the material to a peroxotitanate form.Next, an ion-exchange reaction can be performed to prepare metal-loaded titanates for various applications. An example is the addition of a solution of gold(III)chloride to the nanotitanate to produce the corresponding gold(III)exchanged titanate. Results are obtained that show spherical particles in the range of 100 to 150 nanometers can be prepared using the method, based on electron microscopy imaging and dynamic light scattering measurements.We first had the idea for this method when we began looking at the application of titanates in the biomedical field where particle size becomes more important. This method can be extended to materials normally synthesized using sol-gel techniques, allowing materials with a range of different particle sizes to be prepared. Nanosized particles, monosodium titanate, provide the opportunity to improve ion exchange performance due to their higher surface area to volume ratio.Use of metal exchange titanates as bactericides can be enhanced with nanosized materials. To begin the synthesis of nano monosodium titanate, or nMST, first add 0.58 milliliters of 25 weight percent sodium methoxide solution to 7.62 milliliters of isopropanol followed by 1.8 milliliters of titanium isopropoxide. Label the solution number one.Next, add 0.24 milliliters of ultra-pure water to 9.76 milliliters of isopropanol to make solution number two. Add 0.44 milliliters of Triton X-100 to 280 milliliters of isopropanol in a three-neck flask and stir well with a magnetic stirrer. Fit the syringe ends with tubing of sufficient length to deliver the solutions below the level of the liquid in the flask and load solutions one and two into two separate syringes.Next, place the syringes into a dual-channel syringe pump and deliver the solutions at a rate of 0.333 milliliters per minute to the flask. After addition, cap the flask and continue stirring for 24 hours at room temperature. Afterwards, uncap the flask and heat the mixture to reflux for 45 to 90 minutes.Purge the flask with nitrogen and add ultra-pure water in portions to replace evaporated isopropanol as heating is continued. After most of the isopropanol has evaporated and the volume of water added has reached approximately 50 milliliters, remove the heat from the flask and allow the mixture to cool. Filter the product through a 0.1 micron nylon filter paper and wash it several times with water.Finally, transfer the slurry from the filter into a pre-weighed bottle and store it at ambient temperature. To determine the yield, weigh an aliquot of the aqueous slurry before and after drying. To perform the exchange with gold(III)ions, first transfer 6.50 grams of the 4.23 weight percent slurry of nMST to a 50 milliliter centrifuge tube.Next, add about one milliliter of water to 0659 grams of hydrogen tetrachloro gold(III)trihydrate in a one dram glass vial. Transfer the solution to the centrifuge tube. Continue by rinsing the glass vial with water and adding it to the tube.Repeat this several times to ensure that all of the gold reagent is transferred. Add water to the tube to bring the total volume up to 11 milliliters. Wrap the tube in foil and then tumble it on a shaker for a minimum of four days.After tumbling the mixture, centrifuge the tube for 15 minutes. Discard the supernatant and re-suspend the solids in distilled water. Centrifuge the sample again and repeat the washing procedure twice more.Finally, re-suspend the solids in water and store in the dark at room temperature. To prepare peroxotitanate, begin by adding five grams of a 9.8 weight percent slurry of nMST to a flask and stir the slurry magnetically. Continue by adding dropwise 0.154 grams of a 30 weight percent hydrogen peroxide solution to the flask, which induces a color change from white to yellow.Continue stirring the mixture at ambient temperature for 24 hours. Next, filter the product through a 0.1 micron nylon filter paper and was the product several times with water to remove any un-reacted hydrogen peroxide. Finally, transfer the slurry from the filter into a pre-weighed bottle and store the aqueous slurry of peroxotitanate at ambient temperature.Shown here is a typical particle size distribution as measured by dynamic light scattering using the established sol-gel method. Note that this synthesis produces a multimodal distribution of particles with the majority around one micrometer. When reaction conditions that aimed to reduce the particle size of the monosodium titanate were employed, which involved removing the seeding step and using more dilute reagents, this resulted in a bimodal distribution of particle sizes centered at 50 to 100 nanometers and 500 nanometers after 24 hours.After 48 hours, a trimodal distribution of particles measuring up to 1000 nanometers was observed, as demonstrated in this graph. Importantly, the addition of Triton X-100 during the synthesis of nMST is critical for producing an almost uniform particle size distribution as measured by dynamic light scattering. Transmission and scanning electron microscopy showed that the Triton X-100 produced nMST particles at a more uniform size and morphology when compared to those of monosodium titanate.The surface modification of nMST particles by hydrogen peroxide was confirmed by the appearance of an absorption band at 883 wave numbers in its Fourier transform infrared spectrum. After its development, this technique paved the way for researchers in the field of biological applications of inorganic materials to explore the use of nanotitanates to deliver therapeutic metals and the metal exchange titanates to service bactericides. After watching this video, you should have good understanding of how to prepare nanoscale particles of monosodium titanate along with the peroxide-modified and metal-loaded forms.Remember that working with flammable solvents and reagents can be extremely hazardous. Precautions should be taken to prevent the buildup of flammable vapors. It is recommended that sol-gel synthesis be carried out in a chemical fume hood.

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