可控粒径mTiO_2/mSiO_2及其中空结构mSiO_2微球制备
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摘要
近年来,mTiO_2/mSiO_2复合材料和中空结构介孔二氧化硅在生物催化、药物控释等领域展现出良好的应用前景。在乙醇体系下,以十六胺为模板剂,运用自组装原理制备出介孔氧化钛;并运用晶种法,通过改变TEOS量、模板剂用量、异丙醇和水的用量制备出一种粒径大小在0.80~1.92μm范围内可控的mTiO_2/mSiO_2复合材料;最后在乙醇体系中加入盐酸冷凝回流制备出中空结构介孔二氧化硅微球。通过透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线衍射(XRD)对合成的产物进行表征。
In recent years,the mTiO_2/mSiO_2 microspheres and the hollow-structured mesoporous silica show a good application prospect in biological catalysis,drug release,and other fields.Self-assembly method was used to prepare a mTiO_2 in ethanol system,then a mTiO_2/mSiO_2 composite with particle sizes controllable within the range of0.80 μm to 1.92 μm was synthesized by changing the amount of TEOS,template agent,and isopropyl alcohol/water ratio.Finally the hollow-structured mesoporous silica was prepared in ethanol system by the hydrochloric acid reflux.The samples were characterized by transmission electron microscopy(TEM),scanning electron microscopy(SEM)and X-ray diffraction(XRD).
In recent years,the mTiO_2/mSiO_2 microspheres and the hollow-structured mesoporous silica show a good application prospect in biological catalysis,drug release,and other fields.Self-assembly method was used to prepare a mTiO_2 in ethanol system,then a mTiO_2/mSiO_2 composite with particle sizes controllable within the range of0.80 μm to 1.92 μm was synthesized by changing the amount of TEOS,template agent,and isopropyl alcohol/water ratio.Finally the hollow-structured mesoporous silica was prepared in ethanol system by the hydrochloric acid reflux.The samples were characterized by transmission electron microscopy(TEM),scanning electron microscopy(SEM)and X-ray diffraction(XRD).
引文
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2 Wang P,Yang J,Shi J H,et al.Effect of synthesis conditions of SiO2/TiO2comosite on its capacity to treat cyanide wastewater[J].Nonferrous Metals:Extractive Metallurgy,2014(1):71(in Chinese)王平,杨静,史娟华,等.二氧化硅/二氧化钛复合材料合成条件对其处理含氰废水性能的影响[J].有色金属:冶炼部分,2014(1):71
3 Li Z,Hou B,Xu Y,et al.Hydrothermal synthesis,characterization,and photocatalytic performance of silica-modified titanium dioxide nanoparticles[J].J Colloid Interface Sci,2005,288(1):149
4 Sun X G,Zhang J M,Peng Z.Preparation and properties of silicamodified nano-titania by coating precipitation method[J].J Funct Mater,2008,38(11):1898(in Chinese)孙秀果,张建民,彭政.包覆沉淀法制备氧化硅改性的纳米二氧化钛及其性质[J].功能材料,2008,38(11):1898
5 Deng W,Gong L X,Cheng G Z,et al.Hollow microsphere and their preparation techniques[J].Polym Bull,2011(4):110(in Chinese)邓伟,宫理想,程冠之,等.中空微球及其制备方法[J].高分子通报,2011(4):110
6 McDonald C J,Devon M J.Hollow latex particles:Synthesis and applications[J].Adv Colloid Interface Sci,2002,99(3):181
7 Fei J B,Cui Y,Yan X H,et al.Controlled preparation of MnO2hierarchical hollow nanostructures and their application in water treatment[J].Adv Materials-Deerfield Beach Then Weinheim,2008,20(3):452
8 Ren L X,Wang B.Preparation and characterization of carvedilol solid dispersions using hollow mesoporous silica nanoparticles[J].J China Pharmaceutical University,2014(1):15(in Chinese)任丽霞,王柏.卡维地洛-中空介孔二氧化硅固体分散体的制备与表征[J].中国药科大学学报,2014(1):15
9 Zhu F D,Zhang G W,Liu J N,et al.Research progress of hollow titania microspheres[J].Mater Rev,2010,24(S2):8(in Chinese)朱发德,张高文,刘嘉宁,等.二氧化钛中空微球材料的研究进展[J].材料导报,2010,24(S2):8
10 He K C,Wang M,Zhao B,et al.Recent progress on mesoporous silica composite nanomaterials[J].Mater Rev:Rev,2014,28(7):33(in Chinese)贺旷驰,王蒙,赵斌,等.介孔二氧化硅纳米复合材料的研究进展[J].材料导报:综述篇,2014,28(7):33
11 Huo Q,Margolese D I,Ciesla U,et al.Organization of organic molecules with inorganic molecular species into nanocomposite biphase arrays[J].Chem Mater,1994,6(8):1176
12 Zhu W Y,Cao M J,Cai Q,et al.Synthesis of functional mesoporous silica/poly(N,N/-methylenebisacrylamide)composite materials and application of seepage[J].Mater Rev:Res,2015,29(10):9(in Chinese)朱维耀,曹孟菁,蔡强,等.多功能复合微球的制备及渗流应用[J].材料导报:研究篇,2015,29(10):9
13 Cao M,Jin M,et al.The synthesis of a core-shell hybrid composite micro-sphere with controllable homogenous or heteroge-neous multishell structure by multiple-growth via a combination method[J].Colloids Surf A:Physicochem Eng Aspects,2014,444:289
14 Li W,Li F Y,Shi Z S,et al.Preparation and characterization of strong-lightweight porous silica spheres in millimeter-scale[J].Chem J Chinese Universities,2015(9):1655(in Chinese)李娃,李凤云,史志胜,等.毫米级轻质高强度多孔二氧化硅球的制备与表征[J].高等学校化学学报,2015(9):1655
15 Peng C,Mu M W,Xie S H,et al.Morphological transformation of nesoporous silica using binary cationic-anionic surfactant as template[J].Chem J Chinese Universities,2014,35(9):1864(in Chinese)彭策,牟鸣薇,谢诗航,等.二元阴、阳离子表面活性剂调控合成不同形貌的介孔二氧化硅[J].高等学校化学学报,2014,35(9):1864
16 Zhang X L,Zhu W Y,Cai Q,et al.A size-controllable preparation of monodisperse mesoporous SiO2 microspheres[J].J Funct Mater,2011,42(B11):803(in Chinese)张雪龄,朱维耀,蔡强,等.单分散介孔氧化硅微球的粒径可控制备[J].功能材料,2011,42(B11):803