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1、3D interconnected macroporous carbon monoliths prepared by ultrasonic irradiationNattaporn Tonanon a,*, Adisak Siyasukh a, Yunyong Wareenin a, Tawatchai Charinpanitkul a, Wiwut Tanthapanichakoon b, Hirotomo Nishihara c,
2、Shin R. Mukai c, Hajime Tamon ca Department of Chemical Engineering, Faculty of Engineering, Chulalongkorn University, Bangkok 10330, Thailand b National Nanotechnology Center, 111 Thailand Science Park, Klong Luang, Pat
3、humthani 12120, Thailand c Department of Chemical Engineering, Graduate School of Engineering, Kyoto University, Katsura, Kyoto 615-8510, JapanReceived 4 February 2005; accepted 26 May 2005 Available online 11 July 2005A
4、bstractA new method in preparation of 3D interconnected macroporous carbon monolith has been introduced. Ultrasonic irradiation (ultrasonic intensity 78 W/cm2) and low catalyst concentration (C/W = 10 mol/m3) of RF solut
5、ion are used as an interesting and unique preparation method for 3D interconnected macroporous sonogel (gel irradiated by ultrasound at gelation stage) and/or 3D interconnected macroporous carbon monolith without using t
6、emplates. ? 2005 Elsevier Ltd. All rights reserved.Keywords: Porous carbon; Pyrolysis; Adsorption; Scanning electron microscopy; PorosityMacroporous monolith is an interesting structure that has interconnected skeletons
7、in a single column, and this unique structure allows flow paths (through- pores) through the monolithic columns [1,2]. Carbon monolith has high potential to be good candidates for applications such as columns for chromat
8、ography, cata- lyst supports, adsorbents and porous electrodes under continuous flow conditions. Macroporous carbon monoliths are mostly prepared by using carbon precur- sors and macroscopic shape templates [3–7]. In gen
9、eral, macroscopic shape templates are interconnected skele- ton such as silica template, zeolite, stable emulsions, polymer latex and the interstitial volume of other por- ous structures. Carbon precursors are polymeric
10、materi- als or precursor of polymeric materials such as sucrose,some thermoplastics, phenolic resin, copolymerization of resorcinol Fe(II) complex [2] and other thermoset- tings. There are some reports on macroporous car
11、bon aerogels prepared by using metal catalyst [8] or acid cat- alyst [9]. In this work, a new method in preparation of 3D interconnected macroporous carbon monolith has been introduced. In general, ultrasonic irradiation
12、 has out- standing effects in many chemical reactions such as increasing reaction rates and yields of products, shorten- ing reaction time, altering the reaction path and making milder reaction conditions possible [10,11
13、]. An interest- ing role of ultrasonic irradiation on mesoporous proper- ties of RF carbon gel when the ratio of catalyst to water C/W or pH is high was also reported [10]. To the best of our knowledge, this study is the
14、 first to report on the work of ultrasonic irradiation (ultrasonic intensity 78 W/cm2) together with low catalyst concentration (C/W = 10 mol/m3) of RF solution as an interestingCarbon 43 (2005) 2808–2811www.elsevier.com
15、/locate/carbon0008-6223/$ - see front matter ? 2005 Elsevier Ltd. All rights reserved. doi:10.1016/j.carbon.2005.05.026* Corresponding author. Tel.: +66 2 218 6865; fax: +66 2 218 6877. E-mail address: nattaporn.t@chula.
16、ac.th (N. Tonanon).shrinkage percentage, no template preparation and tem- plate removal. In addition to this preliminary work, the effect of R/C on the structure of 3D interconnected macroporous car- bon monolith (microw
17、ave drying at 200 W after solventexchange with t-butanol) has been investigated. In Figs. 4 and 5, R/C = 1200 mol/mol gives 3D interconnected macroporous carbon monolith with smaller pore dia- meters than R/C = 800 mol/m
18、ol. 3D interconnected macroporous carbon monolith from both R/C = 800 and 1200 mol/mol show narrow pore size distributions as shown in Fig. 5. It is obviously seen that R/C has effects on the structure of interconnected
19、macroporous carbon monolith. These results suggest that there is a possibility to tai- lor pore structure of 3D interconnected macroporous sonogel monolith (precursor of 3D interconnected mac- roporous carbon monolith) d
20、irectly and effectively at gelation stage with suitable reactant ratios of RF solu- tion and ultrasonic intensity.AcknowledgementsThis research was partially supported by the Thai Government (Matching Fund), the Thailand
21、 Research Fund (Senior Researcher Scholarship), Thai-Japan Technology Transfer Project (TJTTP)/Chulalongkorn University, Silver Jubilee Research Fund/Chulalong- korn University, National Metal and Materials Technol- ogy
22、Center (MTEC)/Thailand?s National Science and Technology Development Agency (NSTDA) and the Thailand Graduate Institute of Science and Technology (TGIST)/NSTDA.References[1] Tanaka N, Kobayashi H, Nakanishi K, Minakuchi
23、H, Ishizuka N. A new type of chromatographic support could lead to higher separation efficiencies. Anal Chem 2001:421A–9A.00.10.20.30.40.50.60.01 0.1 10 100Pore Diameter [ m]Incremental Volume [cm3/g]1 µFig. 3. M
24、acropore size distribution of RF carbon monolith.Fig. 4. SEM micrograph (cross section at 5000·) of RF carbon monolith (C/W 10 mol/m3, microwave drying).00.10.20.30.40.50.60.01 0.1 10 100R/C = 800 mol/molR/C = 1200
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