介孔二氧化硅KIT-6介观单晶微球的合成  

Synthesis of mesoporous silica KIT-6 microspheres with single⁃crystalline mesostructure

作　　者：洪美花 刘冠锋 宫毓鹏 李立青 陈铁红 HONG Meihua;LIU Guanfeng;GONG Yupeng;LI Liqing;CHEN Tiehong(CenerTech Tianjin Chemical Research&Design Institute Co.,Ltd.,Tianjin 300131,China;School of Materials Science and Engineering,Nankai University)

机构地区：[1]中海油天津化工研究设计院有限公司,天津300131 [2]南开大学材料科学与工程学院

出　　处：《无机盐工业》2022年第7期149-156,共8页Inorganic Chemicals Industry

基　　金：中国海洋石油集团有限公司海油科技项目(CNOOC-KJ135ZDXM32TJY 005-2018)。

摘　　要：以非离子表面活性剂[聚环氧乙烷(PEO)-聚环氧丙烷(PPO)-聚环氧乙烷三嵌段共聚物,P123]和阳离子聚电解质(聚二甲基二烯丙基氯化铵,PAC)形成的复合物胶束为模板,合成了具有球形形貌的介孔二氧化硅KIT-6介观单晶微球。通过扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、氮气物理吸附和热重分析(TGA)等手段对合成材料的形貌及孔结构进行了表征分析。结果表明,以有机复合物胶束为模板合成出的介孔KIT-6二氧化硅材料具有较规整的球形形貌,颗粒直径为2~3µm,具有较大的比表面积和孔体积(747 m^(2)/g和1.3 cm^(3)/g),介孔孔径为8.5 nm,且在整个颗粒内部介孔保持高度的有序排列。由于长链聚电解质PAC与硅源有着较强相互作用,样品可以在较高水热温度下(160℃)合成,有利于提升介观结构的稳定性。该合成方法对于介孔二氧化硅KIT-6单晶微球的合成及其在催化及吸附分离等领域的应用具有一定的启发意义。Single⁃crystalline mesoporous silica KIT-6 microspheres were synthesized using complex micelles formed by nonionic surfactant(polyethylene oxide(PEO)-polypropylene oxide(PPO)-polyethylene oxide,P123)and cationic poly⁃electrolyte(poly dimethyldiallyl ammonium chloride,PAC)as templates.The morphology and pore structure of the synthe⁃sized materials were characterized by scanning electron microscope(SEM),transmission electron microscope(TEM),X-ray diffraction(XRD),nitrogen physical adsorption and thermogravimetric analysis(TGA).The results showed that the mesoporous KIT-6 silica material synthesized with the organic complex micelles as templates had regular spherical mor⁃phology and particle diameter of 2~3µm.It had a large specific surface area and pore volume(747 m^(2)/g and 1.3 cm^(3)/g)and the mesoporous pore size was 8.5 nm.Within the whole KIT-6 particle,the alignment of mesopores exhibited long-range or⁃der.Due to the strong interaction between long⁃chain polyelectrolyte PAC and the silicon source,the samples were synthe⁃sized at a relatively high hydrothermal temperature(160℃),which was helpful to improve the stability of the mesoscopic structure.This synthesis method had some enlightening significance for the synthesis of mesoporous silica KIT-6 single crys⁃tal microspheres and their applications in the fields of catalysis,adsorption and separation.

关 键 词：介孔二氧化硅 KIT-6 有序介孔 非离子表面活性剂 阳离子聚电解质 

分 类 号：TQ127.2[化学工程—无机化工]