以2-氰乙基三乙氧基硅烷(CTES)和正硅酸乙酯(TEOS)为硅源,聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物(P123)为模板剂,采用共缩聚法在酸性条件下合成了氰基功能化的介孔二氧化硅.通过XRD、SEM、氮气吸附-脱附、FT-IR和元素分析等技术对样品的结构、形貌、孔性质和官能团等进行了表征.研究结果表明,硅源的混合方式对氰基的引入量和分布有一定影响,其中以直接混合方式所得样品中基团含量最高,其分布也最均匀.另外,随着氰基引入量的增加,样品的形貌与孔结构略有变化.当CTES加入量超过20mol％时,材料的介孔由圆柱形的直孔道向瓶颈型的孔道结构发生转变.同时随着材料中氰基含量增大,样品的孔容由0.70 cm3/g降到0.22 cm3/g、表面积从666m2/g降到312 m2/g,孔径由4.2 nm减小到2.7 nm.表明氰基分子占据了部分孔道空间.
参考文献
| [1] | Zhu G,Yang Q,Jiang D,et al.Synthesis of bifunctionalized mesoporous organosilica spheres for high-performance liquid chromatography.Chromatogr.A,2006,1103(2):257-264. |
| [2] | Zhu G,Jiang D,Yang Q,et al.trans-(1R,2R)-Diaminocyclohexane-functionalized mesoporous organosilica spheres as chiral stationary phase.Chromatogr.A,2007,1149(2):219-227. |
| [3] | Macquarrie D J.Direct preparation of organically modified MCM-type materials.Preparation and characterisation of aminopropyl-MCM and 2-cyanoethyl-MCM.Chem.Commun.,1996,(16):1961-1962. |
| [4] | Yang C,Wang Y,Zibrowius B,et al.Formation of cyanidefunctionalized SBA-15 and its transformation to carboxylate-functionalized SBA-15.Phys.Chem.Chem.Phys.,2004,6(9):2461-2467. |
| [5] | Fiorilli S,Onida B,Bonelli B,et al.In situ infrared study of SBA-15 functionalized with carboxylic groups incorporated by a co-condensation route.J.Phys.Chem.B,2005,109(35):16725-16729. |
| [6] | Akcakayiran D,Mauder D,Hess C,et al.Carboxylic acid-doped SBA-15 silica as a host for metallo-supramolecular coordination polymers.J.Phys.Chem.B,2008,112(46):14637-14647. |
| [7] | Xu W,Gao Q,Xu Y,et al.Controlled drug release from bifunctionalized mesoporous silica.J.Solid.State.Chem.,2008,181(10):2837-2844. |
| [8] | Yang C,Zibrowius B,Schüth F,A novel synthetic route for negatively charged ordered mesoporons silica SBA-15.Chem.Commun.,2003(14):1772-1773. |
| [9] | Shen S,Chow P S,Kim S,et al.Synthesis of carboxyl-modified rod-like SBA-15 by rapid co-condensation.J.Colloid.Interf.Sci.,2008,321(2):365-372. |
| [10] | Tsai H-H G,Jheng G L,Kao H M.Direct evidence for interactions between acidic functional groups and silanols in cubic mesoporous organosilicas.J.Am.Chem.Soc.,2008,130(35):11566-11567. |
| [11] | Pan Y C,Wu H Y,Lee L P,et al.Cyanide-and carboxylatefunctionalized cubic mesoporous silicas SBA-1:synthesis,characterization and reactivity of organic functional groups.Micropor.Mesopor.Mat.,2009,123(1/2/3):78-90. |
| [12] | Liu N,Assink R A,Brinker C J.Synthesis and characterizetion of highly ordered mesoporous thin films with-COOH terminated pore surfaces.Chem.Commun.,2003(3):370-371. |
| [13] | Tang Q,Xu Y,Wu D,et al.A study of carboxylic-modified.mesoporous silica in controlled delivery for drug famotidine.J.Solid.State.Chem.,2006,179(5):1513-1520. |
| [14] | Elings J A,Ait-Meddour R,Clark J H,et al.Preparation of a silicasupported peroxycarboxylic acid and its use in the epoxidation of alkenes.Chem.Commun,1998(24):2707-2708. |
| [15] | 吴宝虎,张书翠,唐涛,等(WU Bao-Hu,et al).羧基官能化SBA-15型介孔分子筛的小角X射线散射研究.物理化学学报(Acta Phys.Chim.Sin.),2010,26(8):2217-2223. |
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