Jeffamine聚醚胺改性合成介孔及超微孔氧化硅微球  

Modified Jeffamine Molecular Tools for Ordered Mesoporous and Super-Micorporous Silica Microsphere Particles

作　　者：刘春艳[1,2] 龚彩云[1] 周冬雪[1] 王菁[1] 刘家硕 刘照斌[1] 

机构地区：[1]辽宁师范大学化学化工学院,大连116029 [2]大连理工大学精细化工国家重点实验室,大连116024 [3]大连理工大学附属高中,大连116024

出　　处：《无机化学学报》2015年第5期954-960,共7页Chinese Journal of Inorganic Chemistry

基　　金：大连理工大学精细化工国家重点实验室开放课题基金(No.KF1309)资助项目

摘　　要：通过对Jeffamine ED2003进行硬脂酸接枝,获得了一种在水溶液中能够进行自组装的新型聚醚酰胺高分子表面活性剂,命名为ED2003-fa-18。以ED2003-fa-18聚醚酰胺高分子表面活性剂为模板,以正硅酸乙酯（TEOS）为无机硅源,在酸性条件下水热合成了介孔及超微孔氧化硅微球。利用粉末X射线衍射（XRD）、N2物理吸附、红外光谱（IR）、核磁共振波谱（1H NMR）、扫描电镜（SEM）和透射电镜（TEM）等方法对合成样品进行了表征。研究结果表明,通过改变合成体系中表面活性剂的浓度,可控合成出了有序的介孔及超微孔氧化硅材料。当ED2003-fa-18的浓度为1wt%时,合成的材料为介孔氧化硅,样品的最可几孔径约为2.2nm。当ED2003-fa-18的浓度从3wt%增加到7wt%时,样品的最可几孔径从1.98 nm减小到1.94 nm,得到的样品为超微孔氧化硅材料。样品的比表面积在500 m^2·g^-1左右,孔体积在0.3 cm^3·g^-1左右。由SEM照片可知,所合成的介孔及超微孔氧化硅材料均为由20-30 nm的球形纳米颗粒进一步团聚形成的2-4μm的紧密堆积的实心微球。A low toxicity and biodegradable polymetic temlplating route to ordered mesoporous and supermicorporous silica materials is reported. By grafting stearic acid on Jeffamine ED2003（H2N-（PO）l（EO）m（PO）n-NH2,l＋n =6, m =39）, a polyether amide polymeric surfactant was obtained, which has the ability of self-assembly in aqueous solution, named ED2003-fa-18. Using ED2003-fa-18 as a template, tetraethyl orthosilicate（TEOS） as inorganic silicon source, the ordered mesoporous and super-microporous silica microspheres were hydrothermally synthesized under acidic conditions at mild temperature. The resulting materials were characterized by powder X-ray diffraction（XRD）, nitrogen sorption, infrared spectroscopy（IR）,1H NMR, scanning electron microscopy（SEM）and transmission electron microscopy（TEM）. The influence of the templating concentration on the pore size and morphologies of the resulting materials has been investigated. The results show that the well-ordered mesoporous and super-microporous silica materials have been successfully synthesized. As the templating concentration（from1wt% to 7wt%） increased, the pore diameter decreased obviously from mesoporous range to supermicroporous range. SEM photographs show that the as-synthesized silica materials were spherical nanoparticles of 20-30 nm,and these nanoparticles further agglomerated and formed a densely packed microspheres of 2-4 μm. In addition,ordered pore structures can be observed by the transmission electron microscopy（TEM）.

关 键 词：Jeffamine聚醚胺 改性 介孔氧化硅 超微孔氧化硅 微球 

分 类 号：O613.72[理学—无机化学] O643.43[理学—化学]