有机官能团对硅基MSU—X织构性能的影响  

Effect of Organic Group on Modified MSU - X Silicate

作　　者：巩雁军[1] 李志宏[1] 吴东[1] 孙予罕[1] 邓风[2] 罗晴[2] 岳勇[2] 

机构地区：[1]中国科学院山西煤炭化学研究所 [2]中国科学院武汉物理与数学研究所

出　　处：《化学学报》2001年第10期1592-1598,共7页Acta Chimica Sinica

基　　金：国家自然科学基金，国家重点基础研究发展计划(973计划)

摘　　要：采用有机硅氧烷(RTES)与硅氧烷(TEOS)共水解缩聚合成了有机官能化的MSU-1中孔材料(R=甲基,苯基,乙烯基,脲丙基).当前驱体中RTES与TE0S的摩尔比为0.1:0.9时合成R10-MSU-1分子筛,通过现代分析技术证明所选有机官能团均能进入分子筛骨架,而且在相同摩尔数的各种有机硅氧烷存在下,由于其反应速率、空间位阻的不同使其对骨架的缩聚程度、孔道和表面性质有不同的影响.利用SAXS实验技术对所合成R10-MSU-1材料结构表面以及由于有机官能团的存在对无机骨架产生的影响进行了研究.SAXS较强的散射强度分布对Porod定理形成负偏离,表明孔和基体之间有明显的界面层存在,并求得界面层的平均厚度.实验证明有机基团均匀分布于孔道表面而形成有机界面层.SAXS测试还显示上述分子筛呈质量分形特征,其形成过程可能为非平衡非线性的聚集机制.Organo - functionalized MSU - X [R - MSU - X, R = CH3, C6H5, CH2 = CH and NH2CONH(CH2)(3)] silicates were prepared by one - pot synthesis methodology, using an improved procedure developed for synthesizing MSU - X. The incorporated organic groups were characterized by XRD, FT - IR, C-13, Si-29 CP MAS NMR, HRTEM, SEM, TG, N-2 physisorption techniques, bulk element analysis and small angle X ray scattering (SAXS). The surface morphology and textural properties of such materials varied with R groups in organosiloxanes precursor and their content in the pore. The effects of the organic groups on the modified MSU - 1 were investigated carefully. SAXS results show that the organic groups appeared to be uniformly distributed in R - MSU - X and form interfacial layers that led to the scattering of the pore distortion and gave a negative deviation from Porod's law. The average thickness of the interfacial layer was further obtained by analyzing this deviation.

关 键 词：有机硅氧烷 硅氧烷 合成 中孔分子筛 有机官能化 MSU-X 界面特征 SAXS表征 织构 性能 

分 类 号：TQ424.25[化学工程]