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. סינתזה של Titanate ננו-גלוטמט (nMST) <ol style=";text-align:right;direction:rtl"><li style=";text-align:right;direction:rtl"> הכן 10 מ&quot;ל של תמיסת # 1 על ידי הוספת 0.58 מ&quot;ל של תמיסת 25% WT נתרן methoxide כדי 7.62 מ&quot;ל של isopropanol ואחריו 1.8 מ&quot;ל של isopropoxide טיטניום. </li><li style=";text-align:right;direction:rtl"> הכן 10 מ&quot;ל של תמיסת # 2 על ידי הוספת...

<ol>
	<li>O'Regan, B., Gr&#228;tzel, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+low-cost,+high-efficiency+solar+cell+based+on+dye-sensitized+colloidal+TiO2+films.">A low-cost, high-efficiency solar cell based on dye-sensitized colloidal TiO2 films.</a> Nature. 353, 737-740 (1991).</li><li>Frank, A. J., Kopidakis, N., van de Lagemaat, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrons+in+nanostructured+TiO2+solar+cells:+transport,+recombination+and+photovoltaic+properties.">Electrons in nanostructured TiO2 solar cells: transport, recombination and photovoltaic properties.</a> Coord. Chem. Rev. 248 (13-14), 1165-1179 (2004).</li><li>Mor, G. K., Varghese, O. K., Paulose, M., Shankar, K., Grimes, C. 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+review+on+highly+ordered,+vertically+oriented+TiO2+nanotube+arrays:+fabrication,+material+properties,+and+solar+energy+applications.">A review on highly ordered, vertically oriented TiO2 nanotube arrays: fabrication, material properties, and solar energy applications.</a> Sol. Energy Mater. Sol. Cells. 90 (14), 2011-2075 (2006).</li><li>Dosch, R. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Use of titanates in decontamination of defense waste. Report RS-8232-2/50318. , (1978).</li><li>Sylvester, P., Clearfield, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+removal+of+strontium+from+simulated+Hanford+tank+wastes+containing+complexants.">The removal of strontium from simulated Hanford tank wastes containing complexants.</a> Sep. Sci. Technol. 34 (13), 2539-2551 (1999).</li><li>Manna, B., Dasgupta, M., Ghosh, U. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crystalline+hydrous+titanium(IV)+oxide+(CHTO):+an+arsenic(III)+scavenger+from+natural+water.">Crystalline hydrous titanium(IV) oxide (CHTO): an arsenic(III) scavenger from natural water.</a> J. Water Supply Res. T. 53, 483-495 (2004).</li><li>Elvington, M. C., Click, D. R., Hobbs, D. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sorption+behavior+of+monosodium+titanate+and+amorphous+peroxotitanate+materials+under+weakly+acidic+conditions.">Sorption behavior of monosodium titanate and amorphous peroxotitanate materials under weakly acidic conditions.</a> Sep. Sci. Technol. 45 (1), 66-72 (2010).</li><li>Wataha, J. C., 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=Titanates+deliver+metal+ions+to+human+monocytes.">Titanates deliver metal ions to human monocytes.</a> J. Mater. Sci.: Mater. Med. 21 (4), 1289-1295 (2010).</li><li>Chung, W. O., 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=Peroxotitanate-+and+monosodium+metal-titanate+compounds+as+inhibitors+of+bacterial+growth.">Peroxotitanate- and monosodium metal-titanate compounds as inhibitors of bacterial growth.</a> J. Biomed. Mater. Res., Part A. 97 (3), 348-354 (2011).</li><li>Hobbs, D. T., 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=Strontium+and+actinide+separations+from+high+level+nuclear+waste+solutions+using+monosodium+titanate+1.+Simulant+testing.">Strontium and actinide separations from high level nuclear waste solutions using monosodium titanate 1. Simulant testing.</a> Sep. Sci. Technol. 40 (15), 3093-3111 (2005).</li><li>Ramirez-Salgdo, J., Djrado, E., Fabry, P. <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+sodium+titanate+composites+by+sol-gel+method+for+use+in+gas+potentiometric+sensors.">Synthesis of sodium titanate composites by sol-gel method for use in gas potentiometric sensors.</a> J. Eur. Ceram. Soc. 24 (8), 2477-2483 (2004).</li><li>Yang, J., 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=Study+on+composition,+structure+and+formation+process+of+nanotube+Na2Ti2O4(OH)2.">Study on composition, structure and formation process of nanotube Na2Ti2O4(OH)2.</a> Dalton Trans. 2003 (20), 3898-3901 (2003).</li><li>Chen, W., Guo, X., Zhang, S., Jin, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=TEM+study+on+the+formation+mechanism+of+sodium+titanate+nanotubes.">TEM study on the formation mechanism of sodium titanate nanotubes.</a> J. Nanopart. Res. 9 (6), 1173-1180 (2007).</li><li>Meng, X., Wang, D., Liu, J., Zhang, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+characterization+of+sodium+titanate+nanowires+from+brookite+nanocrystallites.">Preparation and characterization of sodium titanate nanowires from brookite nanocrystallites.</a> Mater. Res. Bull. 39 (14-15), 2163-2170 (2004).</li><li>Yada, M., Goto, Y., Uota, M., Torikai, T., Watari, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Layered+sodium+titanate+nanofiber+and+microsphere+synthesized+from+peroxotitanic+acid+solution.">Layered sodium titanate nanofiber and microsphere synthesized from peroxotitanic acid solution.</a> J. Eur. Ceram. Soc. 26 (4-5), 673-678 (2006).</li><li>Stewart, T. A., Nyman, M., deBoer, M. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Delaminated+titanate+and+peroxotitanate+photocatalysts.">Delaminated titanate and peroxotitanate photocatalysts.</a> Appl. Catal. B. 105 (1-2), 69-76 (2011).</li><li>Rejman, J., Oberle, V., Zuhorn, I. S., Hoekstra, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size-dependent+internalization+of+particles+via+the+pathways+of+clathrin-+and+caveolae-mediated+endocytosis.">Size-dependent internalization of particles via the pathways of clathrin- and caveolae-mediated endocytosis.</a> Biochem. J. 377 (1), 159-169 (2004).</li><li>Hobbs, D. T., Taylor-Pashow, K. M. L., Elvington, M. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Formation+of+nanosized+metal+particles+on+a+titanate+carrier.">Formation of nanosized metal particles on a titanate carrier.</a> US patent application. , (2015).</li><li>Elvington, M. C., Tosten, M., Taylor-Pashow, K. M. L., Hobbs, D. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+nanosize+sodium+titanates.">Synthesis and characterization of nanosize sodium titanates.</a> J. Nanopart. Res. 14, 1114 (2012).</li><li>Duff, M. C., Hunter, D. B., Hobbs, D. T., Fink, S. D., Dai, Z., Bradley, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanisms+of+strontium+and+uranium+removal+from+high-level+radioactive+waste+simulant+solutions+by+the+sorbent+monosodium+titanate.">Mechanisms of strontium and uranium removal from high-level radioactive waste simulant solutions by the sorbent monosodium titanate.</a> Environ. Sci. Technol. 38 (19), 5201-5207 (2004).</li><li>Puangpetch, T., Sreethawong, T., Chavadej, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+production+over+metal-loaded+mesoporous-assembled+SrTiO3+nanocrystal+photocatalysts:+effects+of+metal+type+and+loading.">Hydrogen production over metal-loaded mesoporous-assembled SrTiO3 nanocrystal photocatalysts: effects of metal type and loading.</a> Int. J. Hydrogen Energy. 35 (13), 6531-6540 (2010).</li><li>Fan, X., 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=Facile+method+to+synthesize+mesoporous+multimetal+oxides+(ATiO3,+A+=+Sr,+Ba)+with+large+specific+surface+areas+and+crystalline+pore+walls.">Facile method to synthesize mesoporous multimetal oxides (ATiO3, A = Sr, Ba) with large specific surface areas and crystalline pore walls.</a> Chem. Mater. 22 (4), 1276-1278 (2010).</li><li>Rossmanith, R., 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=Porous+anatase+nanoparticles+with+high+specific+area+prepared+by+miniemulsion+technique.">Porous anatase nanoparticles with high specific area prepared by miniemulsion technique.</a> Chem. Mater. 20 (18), 5768-5780 (2008).</li><li>Wu, Y., Zhang, Y., Xu, J., Chen, M., Wu, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-step+preparation+of+PS/TiO2+nanocomposite+particles+via+miniemulsion+polymerization.">One-step preparation of PS/TiO2 nanocomposite particles via miniemulsion polymerization.</a> J. Colloid Interface Sci. 343 (1), 18-24 (2010).</li><li>Jiang, C., Ichihara, M., Honmaa, I., Zhou, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+particle+dispersion+on+high+rate+performance+of+nano-sized+Li4Ti5O12+anode.">Effect of particle dispersion on high rate performance of nano-sized Li4Ti5O12 anode.</a> Electrochim. Acta. 52 (23), 6470-6475 (2007).</li><li>Bouras, P., Stathatos, E., Lianos, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pure+versus+metal-ion-doped+nanocrystalline+titania+for+photocatalysis.">Pure versus metal-ion-doped nanocrystalline titania for photocatalysis.</a> Appl. Catal. B. 73 (1-2), 51-59 (2007).</li><li>Bonino, R., 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=Ti-Peroxo+species+in+the+TS-1/H2O2/H2O+system.">Ti-Peroxo species in the TS-1/H2O2/H2O system.</a> J. Phys. Chem. B. 108 (11), 3573-3583 (2004).</li><li>Bordiga, S., 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=Resonance+Raman+effects+in+TS-1:+the+structure+of+Ti(IV)+species+and+reactivity+towards+H2O,+NH3+and+H2O2:+an+in+situ+study.">Resonance Raman effects in TS-1: the structure of Ti(IV) species and reactivity towards H2O, NH3 and H2O2: an in situ study.</a> Phys. Chem. Chem. Phys. 2003 (5), 4390-4393 (2003).</li><li>Vacque, V., Sombret, B., Huvenne, J. P., Legrand, P., Suc, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+the+O-O+peroxide+band+by+vibrational+spectroscopy.">Characterization of the O-O peroxide band by vibrational spectroscopy.</a> Spectrochim. Acta Part A. 53 (1), 55-66 (1997).</li></ol>

הנוכחות של מים זרים, למשל מ ריאגנטים טמאים, יכולה לשנות את התוצאה של התגובה, מה שמוביל חלקיקי polydisperse גדולים או יותר. לכן, יש לנקוט זהירות כדי להבטיח מגיבים יבשים משמשים. טיטניום isopropoxide ונתרן methoxide צריך להיות מאוחסן בתוך תא ייבוש כאשר אינו בשימוש. isopropanol הטוהר הגבוה צריך...

Titanates תחמוצת טיטניום מתכת אלקלית נמצא בשימוש נרחב במגוון הרחב של יישומים כגון פיגמנטים של צבעים וחומרי טיפוח עור וכתוצאת photocatalysts בגיור וניצול אנרגיה. 1-3 titanates נתרן הוכח להיות חומרים יעילים להסרת מגוון של קטיונים על פני טווח רחב של מצבי pH באמצעות תגובות קטיוני. 4-7 בנוסף היישומים פשוט תאר, מיקרון בגודל titanates נתרן peroxotitanates נתרן לאחרונה הוכח גם לשמש פלטפורמת משלוח המתכת טיפולית. ביישום זה, יונים של מתכות טיפוליות כגון Au (III), Au (I), ו Pt (II) הם החליפו עבור יוני נתרן של titanate גלוטמט (MST). בדיקות במבחנה עם titanates מתכת-החליפו אצילי מצביעים דיכוי הצמיחה של תאים סרטניים או חיידקים ידי המנגנון ידוע. 8,9 מבחינה היסטורית, titanates נתרן יש להיותen מיוצר באמצעות טכניקות סינטטיות סול ג&#39;ל הידרותרמיות הן וכתוצאה מכך אבקות בסדר עם גדלים של חלקיקים הנעים בין כמה לכמה מאה מיקרונים. 4,5,10,11 לאחרונה, שיטות סינטטיות דווחו שייצרה תחמוצת טיטניום nanosize, חלקי מתכת תחמוצות טיטניום מסוממים, וכן מגוון של titanates מתכת האחרת. דוגמאות כולל צינורות תחמוצת טיטניום נתרן (NaTONT) או nanowires מתגובה של תחמוצת טיטניום ב סודיום הידרוקסיד עודף בטמפרטורה ולחץ גבוהים, 12-14 nanofibers titanate נתרן מתגובה של חומצת peroxotitanic עם סודיום הידרוקסיד עודף בטמפרטורה ולחץ גבוהים, 15 ונתרן ו nanofibers titanate צזיום ידי delamination של titanates חומצה החליפו מיקרון בגודל. 16 הסינתזה של titanates נתרן nanosize ונתרן peroxotitanates הוא עניין לשפר קינטיקה חילוף יונים, אשר נשלטים בדרך כלל על ידי דיפוזיה הסרט או diffu intraparticleשיאון. מנגנונים אלה נשלטים במידה רבה על ידי גודל החלקיקים של מחליפי יונים. בנוסף, כפלטפורמת משלוח המתכת טיפולית, גודל חלקיקים של חומר titanate יהיה צפוי להשפיע על אופי משמעותי של האינטראקציה בין titanate-החליף מתכת סרטן תאים חיידקיים. לדוגמא, תאים חיידקיים, שהן בדרך כלל בסדר גודל של 0.5 - 2 מיקרומטר, עלולים להביא אינטראקציות שונות עם חלקיקים בגודל מיקרון לעומת חלקיקי nanosized. בנוסף, תאי איקריוטיים הלא phagocytic הוכחו להפנים חלקיקים רק עם גודל של פחות מ 1 מיקרון. 17 לפיכך, הסינתזה של titanates נתרן nanosize היא גם עניין להקל משלוח מתכת ספיגה הסלולר מפלטפורמת משלוח titanate. הקטנת נתרן titanates ו peroxotitanates יהיה גם להגדיל את הקיבולת היעילה פרדות מתכת יונים לשפר תכונות פוטו של חומר. 16,18 &lt;/ sup&gt; מאמר זה מתאר פרוטוקול שפותח לסנתז titanate גלוטמט nanosize (nMST) בתנאים סול-ג&#39;ל עדין 19 הכנת מי המקביל שונה nMST.; יחד עם תגובת יון-חילופי לטעון את nMST עם Au (III) מתוארים גם.

<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

מאמר זה מתאר את הסינתיזה-שינוי חמצן של titanate גלוטמט nanosize (nMST), יחד עם תגובת יון-חילופי לטעון את החומר עם Au יונים (III). שיטת הסינתזה נגזרה תהליך סול ג&#39;ל המשמש לייצור titanate גלוטמט מיקרון בגודל (MST), עם כמה שינויים מרכזיים, ובם שינוי ריכוזים מגיבים, השמטת צעד זרע חלקיקים, החדרה פעילה שטח בלתי יוני כדי להקל את השליטה היווצרות וצמיחת חלקיקים. חומר nMST כתוצאת מפגין מורפולוגיה חלקיקים כדורית בצורה עם חלוקת monodisperse בקטרי חלקיקים נעו בין 100 ל 150 ננומטר. חומר nMST נמצא שטח פן Brunauer-אמט-טלר (BET) של 285 מ &#39;2 g -1, וזה יותר ממה בסדר גודל גבוה יותר מאשר MST בגודל מיקרון. הנקודה איזואלקטרית של nMST נמדד 3.34 יחידות pH, שהיא יחידה pH נמוך מזה שנמדד עבור בגודל מיקרון MST. Tהוא nMST החומר נמצא לשמש מחליף יונים יעיל בתנאים חומצי חלש עבור הכנת nanotitanate Au (III) -exchange. בנוסף, היווצרות של peroxotitanate המקביל הודגם על ידי תגובה של nMST עם מי חמצן.

MST הוא מסונתז באמצעות שיטת סול ג &#39;שבו tetraisopropoxytitanium (IV) (TIPT), נתרן methoxide, ומים משולבים והגיב ב isopropanol כדי ליצור חלקיקים זרע MST. 4 חלקיקים מיקרון בגודל אז מגדלים נשלט תוספת של נוספים כמויות של חומרים כימיים. החלקיקים כתוצאה כוללים ליבת אמורפי אזור סיבי חיצוני שיש ממד?...

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.

כימית סינתזת תגובה של nanosize מונוסודיום Titanate

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.

Research

Education

JoVE Core

JoVE Journal

Analytical Chemistry

Chemistry

Unit 1

Chemical Equilibria

SCIENTISTS IN ACTION

Preparation and Use of Samarium Diiodide (SmI2) in Organic Synthesis: The Mechanistic Role of HMPA and Ni(II) Salts in the Samarium Barbier Reaction

Preparation and Use of Samarium Diiodide SmI2 in Organic Synthesis: The Mechanistic Role of HMPA and NiII Salts in the Samarium Barbier Reaction

הכנה ושימוש של סמריום Diiodide (SMI<sub&gt; 2</sub&gt;) בסינתזה אורגנית: התפקיד מכניסטית של HMPA ומלחי ניקל (השני) בתגובת Barbier סמריום

Although initially considered an esoteric reagent, SmI2 has become a common tool for synthetic organic chemists. SmI2 is generated through the addition of ...

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

תגובה אמידה צימוד לסינתזה של ligands מבוסס Bispyridine וcomplexation לפלטינה כסוכנים נגד סרטן Dinuclear

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

Synthesis and Characterization of Functionalized Metal-organic Frameworks

מסגרות סינתזה ואפיון של פונקציונליות מתכת אורגנית

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Highly Stereoselective Synthesis of 1,6-Ketoesters Mediated by Ionic Liquids: A Three-component Reaction Enabling Rapid Access to a New Class of Low Molecular Weight Gelators

סינתזה מאוד Stereoselective של 1,6-Ketoesters מתווכת על ידי נוזלים יוניים: תגובת שלושה רכיבי הפעלה מהירה גישה לסוג חדש של נמוך Gelators משקל המולקולרי

In organic chemistry ionic liquids (ILs) have emerged as safe and recyclable reaction solvents. In the presence of a base ILs can be deprotonated to form ...

Synthesis of Programmable Main-chain Liquid-crystalline Elastomers Using a Two-stage Thiol-acrylate Reaction

סינתזה של אלסטומרים נוזליים-גבישים לתכנות ראשי-שרשרת באמצעות תגובת תיאול-acrylate שני שלבים

This study presents a novel two-stage thiol-acrylate Michael addition-photopolymerization (TAMAP) reaction to prepare main-chain liquid-crystalline ...

Synthesis and Characterization of Supramolecular Colloids

סינתזה ואפיון של קולואידים מולקולריים

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

סינתזה של חלבון Bioconjugates<em&gt; דרך</em&gt; כימיה ציסטאין-maleimide

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

הצמיחה epitaxial של perovskite סטרונציום Titanate על גרמניום באמצעות הפקדת אטומית Layer

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

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

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

זרימה רציפה כימיה: התגובה של Diphenyldiazomethane עם חומצה - Nitrobenzoic p

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

Synthesis and Mass Spectrometry Analysis of Oligo-peptoids

סינתזה וניתוח ספקטרומטר מסה של Oligo-peptoids

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have ...