Name: microhoneycomb monoliths prepared by the unidirectional freeze-drying of cellulose nanofiber based sols: method and extensions
Uploaded: 2018-05-24T13:30:00
Description: Watch this Scientific Journal Video about Microhoneycomb Monoliths Prepared by the Unidirectional Freeze-drying of Cellulose Nanofiber Based Sols: Method and Extensions at JoVE.com

Dette arbeidet ble støttet av National grunnleggende forskning Program i Kina (2014CB932400), National Natural Science Foundation i Kina (nr. 51525204 og U1607206) og Shenzhen grunnleggende forskningsprosjekt (nr. JCYJ20150529164918735). Også, vi ønsker å takke Daicel Allnex Ltd og JSR co for vennlig leverer polyuretan og styren butadien gummi, henholdsvis.

1. utarbeidelse av 1 wt % 2,2,6,6-Tetramethylpiperidin-1-oxyl (TEMPO)-mediert oksidert Cellulose Nanofiber (TOCN) Sol
Merk: Sol er definert som en kolloidalt suspensjon av svært små faste partikler i en kontinuerlig flytende medium.
<ol><li>Avbryte 66.7 g Nadelholz bleket Kraft fruktkjøtt (NBKP, som inneholder 12 g cellulose) 700 mL deionisert (DI) vann med en mekanisk agitator på 300 rpm for 20 min.</li>
	<li>Legge til 20 mL av vandig TEMPO løsning (inneholder 0.15 g av TEMPO) og 20 mL...

<ol>
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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+two-step+sintering+on+micro-honeycomb+BaTiO3+ceramics+prepared+by+freeze-casting+process.">Effect of two-step sintering on micro-honeycomb BaTiO3 ceramics prepared by freeze-casting process.</a> J. Eur. Ceram. Soc. 36 (10), 2647-2652 (2016).</li><li>Yoshida, 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=CO2+Separation+in+a+flow+system+by+silica+microhoneycombs+loaded+with+an+ionic+liquid+prepared+by+the+ice-templating+method.">CO2 Separation in a flow system by silica microhoneycombs loaded with an ionic liquid prepared by the ice-templating method.</a> Ind. Eng. Chem. Res. 56 (10), 2834-2839 (2017).</li><li>Mukai, S. R., Nishihara, H., Tamon, H. <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+monolithic+silica+gel+microhoneycombs+(SMHs)+using+pseudosteady+state+growth+of+microstructural+ice+crystals.">Formation of monolithic silica gel microhoneycombs (SMHs) using pseudosteady state growth of microstructural ice crystals.</a> Chem. Commun. (7), 874-875 (2004).</li><li>Gutie&#180;rrez, M. 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=Macroporous+3D+Architectures+of+Self-Assembled+MWCNT+Surface+Decorated+with+Pt+Nanoparticles+as+Anodes+for+a+Direct+Methanol+Fuel+Cell.">Macroporous 3D Architectures of Self-Assembled MWCNT Surface Decorated with Pt Nanoparticles as Anodes for a Direct Methanol Fuel Cell.</a> J. Phys. Chem. C. 111, 5557-5560 (2007).</li><li>Mukai, S. R., Nishihara, H., Tamon, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Morphology+maps+of+ice-templated+silica+gels+derived+from+silica+hydrogels+and+hydrosols.">Morphology maps of ice-templated silica gels derived from silica hydrogels and hydrosols.</a> Micropor. Mesopor. Mat. 116 (1-3), 166-170 (2008).</li><li>Okaji, R., Taki, K., Nagamine, S., Ohshima, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+of+porous+honeycomb+monolith+from+UV-curable+monomer/dioxane+solution+via+unidirectional+freezing+and+UV+irradiation.">Preparation of porous honeycomb monolith from UV-curable monomer/dioxane solution via unidirectional freezing and UV irradiation.</a> J. Appl. Polym. Sci. 125 (4), 2874-2881 (2012).</li><li>Pan, Z. -. Z., 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=Cellulose+nanofiber+as+a+distinct+structure-directing+agent+for+xylem-like+microhoneycomb+monoliths+by+unidirectional+freeze-drying.">Cellulose nanofiber as a distinct structure-directing agent for xylem-like microhoneycomb monoliths by unidirectional freeze-drying.</a> ACS Nano. 10 (12), 10689-10697 (2016).</li><li>Saito, T., Nishiyama, Y., Putaux, J. -. L., Vigon, M., Isogai, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Homogeneous+Suspensions+of+Individualized+Microfibrils+from+TEMPO-Catalyzed+Oxidation+of+Native+Cellulose.">Homogeneous Suspensions of Individualized Microfibrils from TEMPO-Catalyzed Oxidation of Native Cellulose.</a> Biomacromolecules. 7 (6), 1687-1691 (2006).</li><li>Saito, T., Kimura, S., Nishiyama, Y., Isogai, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cellulose+Nanofibers+Prepared+by+TEMPO-Mediated+Oxidation+of+Native+Cellulose.">Cellulose Nanofibers Prepared by TEMPO-Mediated Oxidation of Native Cellulose.</a> Biomacromolecules. 8, 2485-2491 (2007).</li><li>Bekyarova, 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=Multiscale+carbon+nanotube&#8722;+carbon+fiber+reinforcement+for+advanced+epoxy+composites.">Multiscale carbon nanotube&#8722; carbon fiber reinforcement for advanced epoxy composites.</a> Langmuir. 23, 3970-3974 (2007).</li><li>Nishihara, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Study on the simultaneous control of the nanostructure and morphology of the porous materials prepared via the ice-templating method [D]. , (2005).</li><li>Zhang, 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=Three-dimensional+porous+graphene+sponges+assembled+with+the+combination+of+surfactant+and+freeze-drying.">Three-dimensional porous graphene sponges assembled with the combination of surfactant and freeze-drying.</a> Nano Research. 7 (10), 1477-1487 (2014).</li><li>Tao, Y., 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=Towards+ultrahigh+volumetric+capacitance:+graphene+derived+highly+dense+but+porous+carbons+for+supercapacitors.">Towards ultrahigh volumetric capacitance: graphene derived highly dense but porous carbons for supercapacitors.</a> Sci. Rep. 3, 2975 (2013).</li></ol>

Det viktigste trinnet for å oppnå MHMs er enveis frysing skritt, under vann stivner å danne kolonne iskrystaller og presse dispersoid til side til rammen. Enveis frysing prosessen innebærer i utgangspunktet termisk overføring mellom forløper sol og kjølevæsken. I våre oppsett, ble en dipping maskin brukt til å sette inn en PP rør som inneholder en forløper sol i kjølevæsken (flytende nitrogen) med en konstant hastighet. Siden flytende nitrogen holder fordamper hele tiden, genereres en fluctuant temperaturgr...

Som et helt nytt materiale, har microhoneycomb Monolitten (betegnet MHM) nylig tiltrukket stor oppmerksomhet fra tverrfaglig felt1,2,3,4,5, 6 , 7 , 8. den MHM først utarbeidet av S. Mukaiya et al. gjennom en modifisert enveis Frysetørring (UDF) tilnærming som en Monolitten med en rekke rett microchannels med honeycomb-lignende tverrsnitt9. MHM besitter de generelle fordelene Bikakestrukturer, dvs, effektiv flislegging, høy styrke-til-vekt forhold og lav trykkfall. Videre, sammenlignet med den honeycomb Monolitten med større kanal, MHM har et mye større bestemt areal. UDF metoden innebærer enveis veksten av iskrystaller og samtidige fase separasjon på frysing. Etter fjerning av iskrystallene hentes en solid komponent formet av isen krystall. Morfologi dannet på fase separasjon, avhenger av den iboende naturen av forløperen (sol eller gel), og i de fleste tilfeller, lameller10, fiber11fishbone12 strukturer er sannsynlig å danne i stedet for MHMs. Som et resultat, dannelsen av MHMs har blitt rapportert bare i begrenset forløpere, og dette har betydelig hemmet mangfoldet av deres kjemiske egenskaper. Vi har nylig funnet at cellulose nanofibers har en sterk struktur-regi funksjon mot danner MHM strukturen gjennom UDF prosessen13. Ved blanding av cellulose nanofibers med andre vann-dispergerbare komponenter, er det mulig å forberede en rekke MHMs med forskjellige kjemiske egenskaper. Videre er deres ytre former og kanal størrelser fleksibelt og lett kontrollert13. Dermed skal MHMs brukes som filtre, katalysator støtter, -typen elektroder, sensorer og stillaser for biologisk materiale.
I dette papiret forklare vi først tilberedning av grunnleggende teknikken av MHMs fra vandig spredning av cellulose nanofibers gjennom UDF prosessen i detalj. Videre viser vi utarbeidelse av flere forskjellige typer sammensatte MHMs.

<table border="0" cellpadding="0" cellspacing="0" width="572">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Nadelholz Bleached Kraft Pulp</td>
			<td style="width:100px;">Seioko PMC company</td>
			<td style="width:89px;">CSF=600</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">TEMPO</td>
			<td style="width:100px;">Macklin Inc.</td>
			<td style="width:89px;">T819129</td>
			<td style="width:167px;">98%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">NaBr</td>
			<td style="width:100px;">Macklin Inc.</td>
			<td style="width:89px;">S818075</td>
			<td style="width:167px;">AR, 99%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">NaClO</td>
			<td style="width:100px;">Aladin Inc.</td>
			<td style="width:89px;">S101636</td>
			<td style="width:167px;">6-14 wt% active chlorine basis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">SBR colloid</td>
			<td style="width:100px;">JSR corp.</td>
			<td style="width:89px;">TRD102A</td>
			<td style="width:167px;">48.5 wt%</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:216px;">TiO2</td>
			<td style="width:100px;">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td style="width:89px;">A63725402</td>
			<td style="width:167px;">crystalline anatase phase</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">carbon fiber</td>
			<td style="width:100px;">Shenzhen Xian&#8217;gu Ltd.</td>
			<td style="width:89px;">XGCP-300</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Nitric acid</td>
			<td style="width:100px;">Huada Reagent Ltd.</td>
			<td style="width:89px;">7697-37-2</td>
			<td style="width:167px;">65-68 wt%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Mixer</td>
			<td style="width:100px;">Scientific Industries, Inc</td>
			<td style="width:89px;">G-560</td>
			<td style="width:167px;">the mixer&#160;</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">Mechanical blender</td>
			<td style="width:100px;">Waring Lab Ltd.</td>
			<td style="width:89px;">MX1000XTX</td>
			<td style="width:167px;">For disintegrating cellulose bundles into nanofibers.</td>
		</tr>
		<tr height="46">
			<td height="46" style="height:46px;width:216px;">Homogenizer</td>
			<td style="width:100px;">Scientz Ltd.</td>
			<td style="width:89px;">HXF-DY</td>
			<td style="width:167px;">For dispersing TiO2 nanoparticles</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pH meter&#160;</td>
			<td style="width:100px;">Horiba Ltd.</td>
			<td style="width:89px;">F-74BW</td>
			<td></td>
		</tr>
	</tbody>
</table>

microhoneycomb monoliths prepared by the unidirectional freeze-drying of cellulose nanofiber based sols: method and extensions

Monolittisk Bikakestrukturer er attraktiv for tverrfaglig felt på grunn av deres høy styrke-til-vekt forhold. Spesielt forventes microhoneycomb monolitter (MHMs) med mikrometer skala kanaler som effektive plattformer for reaksjoner og separasjoner på grunn av deres store flater. Til nå, har MHMs utarbeidet av en enveis Frysetørring (UDF) metode fra svært begrenset prekursorer. Her, rapportere vi en protokoll som en rekke MHMs som består av ulike komponenter kan oppnås. Nylig fant vi den cellulose nanofibers funksjonen som tydelig struktur-regi agent mot dannelsen av MHMs gjennom UDF prosessen. Ved å blande den cellulose nanofibers med vann løselig stoffer som ikke gir MHMs, kan en rekke sammensatt MHMs tilberedes. Dette betydelig beriker kjemiske grunnlov MHMs mot allsidig søknadene.

Morphologies for forskjellige posisjoner på MHM-TOCN retning enveis frysing er undersøkt og vist i figur 2. Med stillingen blir ytterligere fra den nederste delen av MHM-TOCN, en gradvis morfologi endring ble avslørt (figur 2, diskusjon). Ved å introdusere en andre komponenten i TOCN sol å danne en homogen blanding sol, er det mulig å tilberede ulike typer sammensatte MHMs. For eksempel er sammensatte MHMs ...

Watch this Scientific Journal Video about Microhoneycomb Monoliths Prepared by the Unidirectional Freeze-drying of Cellulose Nanofiber Based Sols: Method and Extensions at JoVE.com

Microhoneycomb Monoliths Prepared by the Unidirectional Freeze-drying of Cellulose Nanofiber Based Sols: Method and Extensions

Her presenterer vi en generell protokoll for å forberede en rekke microhoneycomb monolitter (MHMs) i hvilke væske kan passere gjennom med en ekstremt lav trykkfall. MHMs fått skal brukes som filtre, katalysator støtter,-typen elektroder, sensorer og stillaser for biologisk materiale.

Microhoneycomb Monoliths utarbeidet av den enveis Frysetørring av Cellulose Nanofiber basert Sols: metoden og utvidelser

Monolithic honeycomb structures have been attractive to multidisciplinary fields due to their high strength-to-weight ratio. Particularly, microhoneycomb ...

This method can help answer key questions about achieving functional MHM materials for applications such as filtration, catalyst supporting, flow type batteries, sensors and bio-scaffolds. The main advantage of this technique is that it utilizes the structure directing function of cellulose nanofibers and can realize constitutional control of the targeted MHMs. This method can help answer key questions about achieving functional MHM materials for applications such as filtration, catalyst supporting, flow type batteries, sensors and bio-scaffolds.Demonstrating the procedure with myself and Cong Wang, a grad student from our laboratory. To begin preparing the tempo-mediated oxidized cellulose nanofiber sol, first combine 66.7 grams of softwood bleached kraft pulp with 700 microliters of deionized water. Mechanically agitate the mixture for 20 minutes at 300 rpm.Over the course of one minute, slowly add to the stirring kraft pulp suspension 20 milliliters each of a 7.5 gram per liter aqueous tempo solution and 75 gram per liter aqueous sodium bromide solution. Begin continuously monitoring the pH of the mixture with a pH meter. Adjust the mixture pH to about 10.5 with a three molar sodium hydroxide solution.Then, over the course of several minutes, slowly pipette into the suspension 63.8 grams of aqueous sodium hypochlorite with 6 to 14%active chlorine. After addition is complete, continue adjusting the pH back to 10.5 whenever it drops to about 10. Once the pH decrease slows, time how long it takes for the pH to drop from 10.5 to 10 to determine how often to check on the mixture during the reaction.Allow the tempo mediated oxidation to proceed normally for a bout 2.5 hours from the start of the sodium hypochlorite addition. Afterwards, filtrate the reaction mixture through a filter. And collect the oxidized cellulose nanofiber.Then, agitate the oxidized cellulose fibers in 1.2 liters of deionized water. Rinse the fibers three times in this way. Dry a small portion of the washed fiber paste overnight in an oven at 60 degrees Celsius to determine the solid content of the paste.Calculate the quantity of water needed to make a 1%by weight sol from the paste. Then transfer the washed fiber paste to laboratory grade blender. Add an appropriate amount of DI water to adjust the concentration of the mixture to 2%by weight.Vigorously blend the paste to disintegrate the oxidized cellulose fibers into nanofibers. Begin with low power blending before vigorously blending the paste at high power. Add one fifth of the needed volume of deionized water to the paste, and blend thoroughly.Repeat this process four more times to obtain the 1%by weight tempo mediated oxidized cellulose nanofiber sol. Store the sol at four degrees Celsius. We hear extracting is constant of the resulting TOCN sol.If it is hot enough, the MHM is likely to be obtained through the newly added process. Normally, the viscosity must be greater than 20, 000 millipascal second. Prior to preparing the tempo mediated oxidized cellulose nanofiber surface oxidized carbon fiber mixed sol, reflux 1.7 grams of 300 mesh carbon fiber in 150 milliliters of concentrated nitric acid to obtain the surface oxidized carbon fibers.Then, place in a 20 milliliter glass vial, 01 grams of the prepared surface oxidized carbon fibers, and 10 grams of the 1%by weight tempo mediated oxidized cellulose nanofiber sol. Manually shake the mixture until the surface oxidized carbon fibers are evenly distributed throughout the sol. Sonicate the mixture for five minutes to obtain an evenly dispersed TOCN SOCF mixed sol.Store the sol at four degrees Celsius. To begin preparing a microhoneycomb monolith, fill the bottom five centimeters of the 13 by 150 millimeter or similarly sized polypropylene tube with glass beads as filler material. Slowly load at least 2.7 milliliters of the chosen sol into the tube, ensuring that the sol level is about 22 millimeters or more above the glass beads.Avoid disturbing the sol unnecessarily to minimize the formation of bubbles in the tube. Use a narrow tipped pipette to carefully remove from the sol any bubbles that were introduced during the loading process. Store the sol sample at four degrees Celsius overnight.Then connect the sample tube to a dipping instrument for a unidirectional freezing. Place a Dewar of liquid nitrogen under the tube. Freeze the sol at an emerging speed of either 50 centimeters per hour for the TOCN sol or 20 centimeters per hour for the mixed sols.Keep the sol frozen once unidirectional freezing is complete. We use our cool time to constantly cool the frozen TOCN sol side hook to prevent it from sleep which will lead to the deterioration of the micromorphology of the resulting monolith. Use a saw to cut open the polypropylene tube.Crack the frozen sol into several pieces using pliers. Freeze dry the frozen sol pieces at minus ten degrees Celsius, minus five degrees Celsius, and zero degrees Celsius for one day each sequentially to obtain the microhoneycomb monolith. Unidirectionally freezing 1%by weight TOCN sol at 50 centimeters per hour without glass beads resulted in a gradual change in orientation and channel size along the freezing direction.The microhoneycomb morphology was retained longitudinally throughout the monolith. The bottom centimeter of the monolith was oriented toward the center of the bulk. A well-aligned honeycomb morphology was obtained two centimeters from the bottom.The microhoneycomb channel size increased from 10 micrometers between the second and third centimeters of the monolith and then remained stable. Overall, the unidirectional freezing effect showed no influence on the morphology past three centimeters. The channel size could be tuned by altering the dipping speed and the temperature of the coolant.Tempo oxidized cellulose nanofibers strongly tended to form the microhoneycomb structure via the unidirectional freezing process even in the presence of a second component. A mixed sol with styrene butadiene rubber yielded a composited microhoneycomb monolith with smooth walls. Tempo oxidized cellulose nanofiber microhoneycomb monoliths also supported titanium oxide nanoparticles in a well-ordered microhoneycomb monolith with nanoparticles adhering to the microhoneycomb walls.A mixed sol with SOCF yielded a novel substructure in which the carbon fibers bridged the neighboring microhoneycomb walls. The unidirectional freeze-drying technique is a novel approach through which many regular microstructures can be obtained. We first had the idea for this method will be so well in random microhoneycomb morphology in a wood pattern.It seems the major component of the wood is cellulose. We began to try imbuing up a similar construction with cellulose. Once mastered, this technique can be used to construct many other functional composite MHMs for targeted applications.

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En netto Mold-basert metode skaperverket stillaset-fri tredimensjonale hjerte vev

This protocol describes a novel and easy net mold-based method to create three-dimensional (3-D) cardiac tissues without additional scaffold material. ...

Detection of Endotoxin in Nano-formulations Using Limulus Amoebocyte Lysate (LAL) Assays

Detection of Endotoxin in Nano-formulations Using Limulus Amoebocyte Lysate LAL Assays

Deteksjon av Endotoxin i Nano-formuleringer bruker Limulus Amoebocyte Lysate (LAL) analyser

When present in pharmaceutical products, a Gram-negative bacterial cell wall component endotoxin (often also called lipopolysaccharide) can cause ...

Seeding and Implantation of a Biosynthetic Tissue-engineered Tracheal Graft in a Mouse Model

Såing og implantering av en biosyntetiske vev-konstruert Tracheal pode i en musemodell

Treatment options for congenital or secondary long segment tracheal defects have historically been limited due to an inability to replace functional ...

3D Printed Porous Cellulose Nanocomposite Hydrogel Scaffolds

3D trykt porøse Cellulose Nanocomposite Hydrogel stillaser

This work demonstrates the use of three-dimensional (3D) printing to produce porous cubic scaffolds using cellulose nanocomposite hydrogel ink, with ...