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1、附录二 英文文献与翻译英文文献13D interconnected macroporous carbon monoliths preparedby ultrasonic irradiationNattaporn Tonanon , Adisak Siyasukh , Yunyong Wareenin ,Tawatchai Charinpanitkul , Wiwut Tanthapanichakoon , Hirotomo Nishihara ,Shin R. Mukai , Hajime TamonAbstract：A new method in preparation of 3D inte
2、rconnected macroporous carbon monolith has been introduced. Ultrasonic irradiation(ultrasonic intensity 78 W/cm2) and low catalyst concentration (C/W = 10 mol/m3) of RF solution are used as an interesting and unique preparation method for 3D interconnected macroporous sonogel (gel irradiated by ultr
3、asound at gelation stage) and/or3D interconnected macroporous carbon monolith without using templates.Keywords: Porous carbon; Pyrolysis; Adsorption; Scanning electron microscopy; PorosityMacroporous monolith is an interesting structure that has interconnected skeletons in a single column, and this
4、unique structure allows flow paths (throughpores)through the monolithic columns . Carbon monolith has high potential to be good candidates for applications such as columns for chromatography, catalyst supports, adsorbents and porous electrodes under continuous flow conditions. Macroporous carbon mon
5、oliths are mostly prepared by using carbon precursors and macroscopic shape templates . In general, macroscopic shape templates are interconnected skeleton such as silica template, zeolite, stable emulsions, polymer latex and the interstitial volume of other porous structures. Carbon precursors are
6、polymeric materials or precursor of polymeric materials such as sucrose, some thermoplastics, phenolic resin, copolymerization of resorcinol Fe(II) complex and other thermosettings. There are some reports on macroporous carbon aerogels prepared by using metal catalyst or acid catalyst. In this work,
7、 a new method in preparation of 3D interconnected macroporous carbon monolith has been introduced. In general, ultrasonic irradiation has outstanding effects in many chemical reactions such as increasing reaction rates and yields of products, shortening reaction time, altering the reaction path and
8、making milder reaction conditions possible. An interesting role of ultrasonic irradiation on mesoporous properties 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 first to report on the work of ultrasonic ir
9、radiation (ultrasonic intensity 78W/cm2) together with low catalyst concentration (C/W = 10 mol/m3) of RF solution as an interestingand unique preparation method for 3D interconnected macroporous sonogel (gel irradiated by ultrasound at gelation stage) and/or carbon monoliths without usingtemplates.
10、Macroporous sonogel monolith, precursors for macroporous carbon monolith, were prepared from resorcinol formaldehyde (RF) solutions which were composed of resorcinol (C6H4(OH)2) (R), formaldehyde (HCHO) (F), sodium carbonate (Na2CO3) (C) and distilled water (W). All chemicals were research gradesfro
11、m Wako Pure Chemical Industries. Na2CO3 and distilled water were used as a basic catalyst and a diluent respectively. The ratios of resorcinol to formaldehyde (R/F), resorcinol to water (R/W) and catalyst to water (C/W) were fixed at 0.5 mol/mol, 8100 mol/m3 and 10 mol/m3 respectively. Gelation temp
12、erature was 308 K. Ultrasonic wave was applied into RF solution right from the start by Vibra Cell model VC 130 (frequency 20 kHz) with a titanium alloy transducer at intensity 78 W/cm2. When it was close to the gelation time, the ultrasonic irradiation was stopped and the RF solution was then poure
13、d into the cylindrical glass tube (inner diameter = 3 mm, length = 40 mm) followed by aging for 7 days at 348 K in the oven. Before freeze drying, water in RF sonogel monolith was replaced by solvent exchange with t-butanol for three times. After that, RF sonogels were freeze-dried at 263 K for 3 h
14、toobtain freeze dried macroporous RF sonogel monolith. Macroporous carbon sonogel monoliths were obtained by pyrolyzing macroporous RF sonogel monoliths at 1023 K. Pyrolysis was conducted under a 200 cm3STP/min flow of nitrogen gas. At first, the freezedried sonogels were heated to 523 K at a consta
15、nt heating rate of 523 K/h, and were kept at this temperature for 2 h.Then they were heated to 1023 K at a constant heating rate of 523 K/h and were kept at 1023 K for 4 h.The structures of RF gel and RF sonogel monoliths were observed by scanning electron microscope(SEM). Macropore size distributio
16、n was measured by using mercury porosimeter. Porous properties, BET surface area (SBET), mesopore volume (Vmes) and micropore volume (Vmic), were determined from the N2 adsorption method using an adsorption apparatus.The effect of ultrasonic irradiation at gelation stage can be seen as followed. In
17、gelation process, gelation time is shortened outstandingly with ultrasonic irradiation. Gelation time obviously decreases from 48 h (RF gel monolith) to 8 h (RF sonogel monolith). The shrinkages of 3D interconnected macroporous RF gel monolith and RF sonogel monolith, after freeze drying, are 21% an
18、d 1% respectively. It is obvious that ultrasonic irradiation leads to small shrinkage in RF gel sonogel monolith compared to RF gel monolith. In Fig. 1, the cross section of RF sonogel monolith observed by SEM shows 3D interconnected macroporous structure which is totally different from mesoporous s
19、tructure of RF gel monolith. SBET are 228 (RF gel monolith) and 5 (RF sonogel monolith) m2/g. Vmic and Vmes of RF gel are 0.02 and 0.32 cm3/g respectively. For RF sonogel monolith, Vmic and Vmes cannot be detected.After pyrolysis of RF sonogel monolith, no change in macroporous structure and very lo
20、w shrinkage are observed.After pyrolysis SBET and Vmic of sonogel increases from 5 to 366 m2/g and N/D to 0.11 cm3/g respectively (Vmes cannot be detected). It can be seen from SEM micrograph in Fig. 2 together with porous properties that RF carbon monolith can keep 3D interconnected macroporous str
21、uctures. The macropore size distributions of carbon monolith are narrow, the average macropore size around 13 lm as shown in Fig. 3. In this work, new synthesis method for 3D interconnected macroporous sonogel and/or carbon monolith is proposed with some advantages to other methods such as shorter g
22、elation time of polymer monolith, small shrinkage percentage, no template preparation and template removal. In addition to this preliminary work, the effect of R/C on the structure of 3D interconnected macroporous carbon monolith (microwave drying at 200 W after solventexchange with t-butanol) has b
23、een investigated. In Figs. 4 and 5, R/C = 1200 mol/mol gives 3D interconnected macroporous carbon monolith with smaller pore diameters than R/C = 800 mol/mol. 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
24、 is obviously seen that R/C has effects on the structure of interconnected macroporous carbon monolith. These results suggest that there is a possibility to tailor pore structure of 3D interconnected macroporous sonogel monolith (precursor of 3D interconnected macroporous carbon monolith) directly a
25、nd effectively at gelation stage with suitable reactant ratios of RF solution and ultrasonic intensity.References1 Tanaka N, Kobayashi H, Nakanishi K, Minakuchi H, Ishizuka N. A new type of chromatographic support could lead to higher separation efficiencies. Anal Chem 2001:421A9A.2 Liang C, Dai S,
26、Guiochon G. A graphitized-carbon monolithic column. Anal Chem 2003;75:490412.3 Taguchi A, Smatt JH, Linden M. Carbon monoliths possessing a hierarchical, fully interconnected porosity. Adv Mater 2003;15:120911.4 Shi ZG, Feng YQ, Xu L, Da SL, Zhang M. Synthesis of carbon monolith with trimodal pores.
27、 Carbon 2003;41:265389.5 Bu H, Rong J, Yang Z. Template synthesis of polyacrylonitrilebased ordered macroporous materials and their derivatives. Macromol Rapid Commun 2002;23:4604.6 Kang S, Yu JS, Kruk M, Jaroniec M. Synthesis of an ordered macroporous carbon with 62 nm spherical pores that exhibit
28、unique gas adsorption properties. Chem Commun 2002:16701.7 Peters EC, Svec F, Frechet JMJ. Rigid macroporous polymer monoliths. Adv Mater 1999;11:116981.8 Moreno-Castilla C, Maldonado-Hoda FJ, Rivera-Utrilla J, Rodrguez-Castellon E. Group 6 metal oxidecarbon aerogels. Their synthesis, characterizati
29、on and catalytic activity in the skeletal isomerization of 1-butene. Appl Catal A 1999;183:34556.9 Brandt R, Petricevic R, Probstle H, Fricke J. Acetic acid catalyzed carbon aerogels. J Porous Mater 2003;10:1718.10 Tonanon N, Siyasukh A, Tanthapanichakoon W, Nishihara H, Mukai SR, Tamon H. Improveme
30、nt of mesoporosity of carbon cryogels by ultrasonic irradiation. Carbon 2005;43:52531.11 Suslick KS, Price GJ. Applications of ultrasound to materials chemistry. Annu Rev Mater Sci 1999;29:295326. 翻译1超声波辐照法制备三维贯通多孔碳整体柱Nattaporn Tonanon, Adisak Siyasukh , Yunyong Wareenin ,Tawatchai Charinpanitkul ,
31、Wiwut Tanthapanichakoon , Hirotomo Nishihara ,Shin R. Mukai , Hajime Tamon摘要:介绍一种制备三维贯通多孔碳的新方法。间苯二酚-甲醛溶液在超声波辐照(超声波强度78W/cm2)和低催化剂浓度（C/W=10mol/m3）下制备三维贯通多孔声致凝胶(凝胶在胶化阶段辐射超声波) ，是目前倍受关注的也是唯一的一种不用模板的多孔碳整体柱的制备方法。关键词：多孔碳 热分解 吸附 扫描电镜 孔隙率在一个单独柱体内具有连通骨架的多孔整体柱是一个受关注的结构，并且这种唯一的结构能够贯通整个整体柱。碳整体柱因为具有很高的势能作为整体柱便于应用
32、于色谱分析，催化剂支架,吸附剂和多孔电极具有连续不断的流动条件。多孔碳整体柱大部分都是用碳前驱体和宏观外形的模板制备的。大体上讲，宏观外形的模板都具有连通的骨架像硅模板，沸石，稳定的乳剂，高分子乳胶和具有空隙的其它结构。碳前驱是聚合材料或是聚合材料前驱像蔗糖，一些热塑性材料，酚醛树脂，间苯二酚Fe()络合物的共聚物和其它热固性的材料。有一些关于利用金属催化剂或者酸催化剂制备多孔碳气凝胶的报道。本文介绍了一种制备三维连通多孔碳的新方法。大体上讲，超声波辐射法在许多化学反应像提高反应速率与提高反应产率，缩短反应时间，修改反应途径和使反应条件尽量温和中是比较优异的方法。超声波辐射法一种受关注的在中孔
33、材料性质中催化剂与水的比例或者PH过高的作用也有人报道过。具我所知，这篇文章是第一篇报道关于RF溶液中的超声波辐射(超声波强度78W/cm2)和低催化剂浓度（C/W=10mol/m3）是前一段时间受关注的也是唯一的一种制备无模板整体柱三维连通多孔声致凝胶的一种方法(凝胶在胶化阶段照射超声波)。多空声致凝胶整体柱是多孔碳整体柱的前驱，是从由间苯二酚(C6H4(OH)2)(R),甲醛（HCHO）(F)，固体碳酸钠（Na2CO3）(C)和蒸馏水（W）组成的（RF）溶液中制备的。所有的化学用品都是从Wako Pure化学公司研究开发的。Na2CO3和蒸馏水分别被用作基本催化剂和稀释剂。间苯二酚和甲醛的
34、比例（R/F），间苯二酚和蒸馏水的比例(R/W)和催化剂与蒸馏水的比例（C/W）是固定的分别是0.5mol/mol，8100mol/m3和10mol/m3。胶化温度为308K。超声波被应用到RF溶液中，它正好是由78 W/cm2强度的钛合金传感器组成的震动电池模型VC130（频率为20KHz）发挥作作用的。当它接近凝胶时间时，超声波就会停止，RF溶液然后被倒入圆柱形的玻璃试管（该试管内部直径是3mm, 长40mm）,在348K的烘箱内烘烤7天。在低温干燥之前，在RF声致凝胶整体柱内的水应与叔丁醇进行3次溶剂交换。在这之后，RF声致凝胶低温干燥在263K下干燥3小时获得低温干燥的多孔RF声致凝胶
35、整体柱。多孔碳声致凝胶整体柱是由多孔RF声致凝胶整体柱在1023K下高温分解而得的。热分解在200cm3STP/min的氮气保护下进行的。首先，低温干燥声致凝胶在523K/h的速度下加热到523K，并保温2h。再以523K/h的速度加热到1023K保温4h。RF凝胶和RF声致凝胶整体柱的结构是利用扫描电镜（SEM）进行观测的。多孔的尺寸和分布是利用汞孔隙率计测量的。多孔的性质，比表面积（SBET），孔隙体积（Vmes）和小孔体积（Vmic），是利用吸附仪器测N2的吸附量的方法测定的。在胶凝阶段超声波的作用可以在下面看出。在胶凝过程中，超声波使胶凝时间显著缩短。胶凝时间明显的从48h（RF凝胶整
36、体柱）减少到8h（RF凝胶整体柱）。在低温干燥后，三维连通多孔RF凝胶整体柱和RF声致凝胶整体柱的收缩率分别为21和1。由超声波导致RF声致凝胶整体柱的收缩比RF凝胶整体柱要小。如图1，通过扫描电镜观测到的RF声致凝胶整体柱的三维连通多孔结构与RF凝胶的中孔结构完全不同。SBET分别为228m2/g（RF凝胶整体柱）和5 m2/g（RF声致凝胶整体柱）。RF凝胶的Vmes 和Vmic分别为0.02 cm3/g和0.32cm3/g。RF声致凝胶整体柱的Vmes 和Vmic测不出。 图1:RF凝胶和RF声致凝胶整体柱 图2：RF碳整体柱的SEM的SEM显微照片（横截面在1000） 显微照片（横截面
37、在1000）声致凝胶整体柱热解后，观测到的多孔结构和比较低的收缩率没有发生变化。热解后的声致凝胶的SBET从5 m2/g变到366 m2/g，Vmic变到0.11cm3/g（Vmes 测不出）从图2的SEM的显微照片可以看出具有多孔性质的RF碳整体柱能保持三维连通多孔结构。碳整体柱的尺寸分布比较小，从图3可以看出平均孔径大概是13m。这篇文章，合成三维连通多孔声致凝胶和碳整体柱的新方法优于其它方法主要在于缩短了高分子整体柱的胶凝时间，具有较小的收缩百分比，无模板制备和样板移动。 图3：RF碳整体柱的多孔尺寸分布 图5：RF碳整体柱的多孔尺寸分布 （C/W=10 mol/m3，微波干燥）图4：R
38、F碳整体柱的SEM显微照片（C/W=10 mol/m3，微波干燥）在前期工作的基础上，我们研究一下R/C对三维连通多孔碳整体柱（微波干燥是在200W的条件下进行与叔丁醇的溶剂交换）的结构的影响。从图4和图5可以看出R/C=1200mol/mol时得到的三维连通多孔碳整体柱的孔直径要小于R/C=800mol/mol时得到的三维连通多孔碳整体柱。从图5可以看出R/C800mol/mol和R/C=1200mol/mol的三维连通多孔碳整体柱都具有较小的孔尺寸分布。可以看出R/C对连通多孔碳整体柱的结构有着明显的作用。这些结构证明我们可以直接有效的在胶化阶段配以合适的RF溶液与超声波的比例来控制三维连
39、通多孔声致整体柱（的三维连通多孔碳整体柱的前驱）的孔结构。参考文献：1 Tanaka N, Kobayashi H, Nakanishi K, Minakuchi H, Ishizuka N. A new type of chromatographic support could lead to higher separation efficiencies. Anal Chem 2001:421A9A.2 Liang C, Dai S, Guiochon G. A graphitized-carbon monolithic column. Anal Chem 2003;75:490412.3
40、Taguchi A, Smatt JH, Linden M. Carbon monoliths possessing a hierarchical, fully interconnected porosity. Adv Mater 2003;15:120911.4 Shi ZG, Feng YQ, Xu L, Da SL, Zhang M. Synthesis of carbon monolith with trimodal pores. Carbon 2003;41:265389.5 Bu H, Rong J, Yang Z. Template synthesis of polyacrylo
41、nitrilebased ordered macroporous materials and their derivatives. Macromol Rapid Commun 2002;23:4604.6 Kang S, Yu JS, Kruk M, Jaroniec M. Synthesis of an ordered macroporous carbon with 62 nm spherical pores that exhibit unique gas adsorption properties. Chem Commun 2002:16701.7 Peters EC, Svec F, F
42、rechet JMJ. Rigid macroporous polymer monoliths. Adv Mater 1999;11:116981.8 Moreno-Castilla C, Maldonado-Hoda FJ, Rivera-Utrilla J, Rodrguez-Castellon E. Group 6 metal oxidecarbon aerogels. Their synthesis, characterization and catalytic activity in the skeletal isomerization of 1-butene. Appl Catal
43、 A 1999;183:34556.9 Brandt R, Petricevic R, Probstle H, Fricke J. Acetic acid catalyzed carbon aerogels. J Porous Mater 2003;10:1718.10 Tonanon N, Siyasukh A, Tanthapanichakoon W, Nishihara H, Mukai SR, Tamon H. Improvement of mesoporosity of carbon cryogels by ultrasonic irradiation. Carbon 2005;43
44、:52531.11 Suslick KS, Price GJ. Applications of ultrasound to materials chemistry. Annu Rev Mater Sci 1999;29:295326.英文文献2A new methodto estimate pore volume of porousstyrenedivinylbenzene copolymersMuhammadArif Malik , Munir Ahmed, Muhammad IkramAbstract：A new method to estimate the pore volume of
45、porous styrenedivinylbenzene copolymer beads is proposed.The estimatedpore volume（PVe）is basedon the solubility parameters （i） andthe corresponding weight fractions（fi） of styrene, divinylbenzenes and diluents in the polymerization mixture. The equation used is: PVe=1.136（i fi）231.193i fi98.825. Reg
46、ression analysis results show that an ideally close match of the predicted pore volume andthe pore volume determined by mercury porosimeter is achievedwith R2=0.99, when non-polar and moderately polar liquids are employed as diluents. In the case of strongly polar (H-bonding) liquids as diluents, th
47、e method should be used only to predict a trend towards an increase or decrease in pore volume, which occurs as a result of variation in the composition of polymerization mixture.Keywords: Styrene-divinylbenzene; Pore volume estimation; Solubility parameters; Macroporous resins; Polymeric adsorbents
48、1. IntroductionPorous styrenedivinylbenzene (S-DVB) copolymer beads are produced on an industrial scale as well as in laboratories throughout the worldby o/w suspension polymerization andthen convertedto ionexchangers,chelating resins, supports for catalysts and enzymes, etc. . The monomers are diluted with some inert organic liquidthat introduces porosity in the copolymer . The porosity is determined by amount andsolvating property of th
