(MCM-41)-(偶氮胂-Ⅲ)纳米复合材料的制备与表征

Preparation and Characterization of (MCM-41)-(Arsenano-Ⅲ) Nanocomposite Materials

以纳米MCM-41分子筛为主体,以偶氮胂-Ⅲ(ASA-Ⅲ)为客体,通过液相移植法制备出(纳米MCM-41)-(偶氮胂-Ⅲ)主-客体纳米复合材料。利用系列表征技术化学分析、粉末XRD、傅里叶变换红外光谱、低温N2吸附-解吸附技术、扫描电镜、固体扩散漫反射吸收光谱和发光研究对所制备的材料进行了表征。化学分析证明偶氮胂-Ⅲ存在于制备的纳米复合材料中;粉末XRD结果表明,所制备的(纳米MCM-41)-(偶氮胂-Ⅲ)仍然保持二维的六方结构;红外光谱表明所制备的主-客体纳米复合材料的分子筛骨架完好;低温N2吸附-解吸附结果表明组装后的纳米复合材料分子筛的比表面积和孔体积较未组装的主体分子筛有所降低,表明客体已经部分占据了分子筛孔道;扫描电镜显示(纳米MCM-41)-(偶氮胂-Ⅲ)的粒子形状为球形,尺寸为110±5nm;固体扩散漫反射吸收光谱表明,所制备的纳米复合材料中客体的吸收较相应体相吸收有明显的蓝移,说明客体处于纳米MCM-41分子筛主体孔道内并呈现出分子筛孔道的立体限域效应。所制备的纳米复合材料呈现发光。

（Nanometer MCM-41）-（arsenano-Ⅲ） host-guest nanocomposite materials were prepared by liquid-phase grafting method using nanometer MCM-41 molecular sieve as host and the arsenano-Ⅲ （ASA-Ⅲ） as guest. The prepared nanocomposite materials were characterized by a series of characterization techniques including chemical analysis, powder X-ray diffraction, Fourier transform infrared spectroscopy（FTIR）, low temperature nitrogen adsorption-desorption, scanning electron microscopy（SEM） and solid diffuse refletance absorption spectra. Chemical analysis confirmed that the ASA-Ⅲ existed in the nanocomposite materials. The powder X-ray diffraction indicated the structure of the （nanometer MCM-41）- （ASA-Ⅲ） still remained two-dimensional hexagonal mesostructrure. The infrared spectroscopy suggested that the framework of the molecular sieve was kept intact. The low temperature nitrogen adsorbtion-desorption results showed that the ASA-Ⅲ was present on the inner surface and partially occupied the channels of the molecular sieve. Scanning electron microscopic images showed that the shape of the （nanometer MCM-41）-（ASA -Ⅲ ） was ball and the size of the （nanometer-MCM-41）- （ASA-Ⅲ） particles was 110~5 nm. The UV-Vis solid state diffuse reflectance absorption spectra of the prepared composite materials have obvious blue shift, showing that the guest was in the channels of the nanometer MCM-41 host and the steroconfinmment effect of the molecular sieve emerged. The prepared composite materials presented luminescence.