中空介孔二氧化硅微球的制备及表征分析  

Preparation and Characterization of Hollow Mesoporous Silica Microspheres

作　　者：黄晓琳 倪佳馨 韩有奇 刘嘉恒 苗媛媛[1] 韩世岩[1] HUANG Xiaolin;NI Jiaxin;HAN Youqi;LIU Jiaheng;MIAO Yuanyuan;HAN Shiyan(Key Laboratory of Bio-Based Material Science and Technology,Ministry of Education, Northeast Forestry University,Harbin 150040,China)

机构地区：[1]东北林业大学生物质材料科学与技术教育部重点实验室,黑龙江哈尔滨150040

出　　处：《林产化学与工业》2022年第1期64-70,共7页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(31700502);中央高校基金科研业务专项基金(2572020BB07);大学生国家级创新项目(202110225167)。

摘　　要：以二氯化-N,N′-二(3-氢化松香酰氧-2-羟丙基)四甲基乙二胺(DHRT)为模板剂,正硅酸乙酯为硅源,采用溶胶-凝胶和水热合成的方法,分别制备了中空介孔二氧化硅微球SiO_(2)-1和SiO_(2)-2。利用SEM、TEM、FT-IR、XRD和氮气吸附-脱附对SiO_(2)-1和SiO_(2)-2进行表征分析,结果表明:两种方法均已成功制备了具有无定形结构的二氧化硅微米球;随着模板剂用量(0.1~1 g)的增加,二氧化硅粒子间团聚现象逐渐消失,SiO_(2)-1主要为带有花纹的松散状微米球,SiO_(2)-2为壁厚80~85 nm的中空微米球。不同模板剂用量(0.3~1 g)制备的SiO_(2)-1的平均粒径分布在0.22~0.33μm,SiO_(2)-2的平均粒径分布在0.34~0.41μm。DHRT用量0.7 g时,两种方法制备的SiO_(2)-1-0.7和SiO_(2)-2-0.7形貌和粒径相对较好,比表面积分别为561.52和463.41 m^(2)/g,累积孔体积分别为0.35和0.42 m^(3)/g,平均孔径分别为2.56和3.66 nm。通过Zeta电位分析表明:SiO_(2)中空介孔结构的形成主要是由正硅酸乙酯水解缩聚得到的低聚物与模板剂之间的协同自组装过程引起的。Hollow mesoporous silica microspheres SiO_(2)-1 and SiO_(2)-2 were prepared by sol-gel and hydrothermal synthesis using dichloride-N,N′-bis(3-hydrorosin loxy-2-hydroxypropyl)tetramethylenediamine(DHRT)as template agent and ethyl orthosilicate as silicon source.SEM,TEM,FT-IR,XRD and nitrogen adsorption-desorption were used to characterize SiO_(2)-1 and SiO_(2)-2.The results showed that silicon dioxide microspheres with amorphous structure were successfully prepared by both methods;the agglomeration phenomenon between silica particles gradually disappeared with the increase of the amount of template agent(0.1-1 g);SiO_(2)-1 was mainly loose microsphere with patterns,and SiO_(2)-2 was hollow microsphere with the wall thickness of 80-85 nm.The average particle size distributions of SiO_(2)-1 and SiO_(2)-2 prepared with different template dosages(0.3-1 g)were 0.22-0.33μm and 0.34-0.41μm,respectively.The morphology and particle size of SiO_(2)-1-0.7 and SiO_(2)-2-0.7 prepared by two methods exhibited good morphology and low particle size,with specific surface area of 561.52 and 463.41 m^(2)/g,cumulative pore volume of 0.35 and 0.42 m^(3)/g,and average pore size of 2.56 and 3.66 nm,respectively.Zeta potential analysis showed that the formation of SiO_(2) hollow mesoporous structure was mainly caused by the cooperative self-assembly process between the oligomer obtained by hydrolyzing polycondensation of ethyl orthosilicate and the template agent.

关 键 词：二氧化硅 微球 介孔 中空 

分 类 号：TQ35[化学工程] TB34[一般工业技术—材料科学与工程]