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化学学报
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化学学报 ›› 2001, Vol. 59 ›› Issue (10): 1592-1598. 上一篇    下一篇

研究论文

有机官能团对硅基MSU-X织构性能的影响

巩雁军;李志宏;吴东;孙予罕;邓风;罗晴;岳勇   

  1. 中国科学院山西煤炭化学研究所.太原(030001);中国科学院煤转化国家重点实 验室;中国科学院武汉物理与数学研究所;中国科学院波谱与原子分子物理国家重 点实验室.武汉(430071)
  • 发布日期:2001-10-15

Effect of organic group on modified MSU-X silicate

Gong Yanjun;Li Zhihong;Wu Dong;Sun Yuhan;Deng Feng;Luo Qing;Yue Yong   

  1. Shanxi Inst Coal Chem., CAS.Taiyuan(030001);.Wuhan(430071)
  • Published:2001-10-15

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623

被引次数

9 | 2

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TO64EOS的摩尔比为0.1:0.9时合成R10-MSU-1分子筛，通过现化分析技术证明BA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数有机硅氧烷存在下，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而层存在，并求得界面层的平均厚度。实验证明有机基团的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。

关键词: 分子筛, 硅氧烷, 水解, 缩聚, 官能团, 织构

Organo-functionalized MSU-X[R-MSU-S,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, 13^C, 29^Si CP MAS NMR, HRTEM, SEM, TG, N2physisorption techniques, bulk element analysis and small angle X-ray scattering (SAXS). The surface morphology and textural porperties 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.

Key words: MOLECULAR SIEVE, SILOXANE, HYDROLYSIS, POLYCONDENSATION, FUNCTIONAL GROUP, TEXTURE

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