采用液相法室温制备A型沸石,利用X射线衍射、扫描电子显微镜、红外光谱等考察晶化时间和凝胶中n(Al2O3)/n(Si O2)比对沸石的成核与晶体生长过程的影响。结果表明:晶化120 h时,反应体系以成核作用为主;120~156 h是A型沸石晶体的快速生长期;晶化时间为168 h时,合成产物具有较好结晶度。与常规95℃制备A型沸石相比,室温合成抑制了杂相的形成,延长晶化时间没有诱发羟基方钠石生成。同时,室温合成制备的样品,粒度明显减小,出现明显的附聚现象。n(Al2O3)/n(Si O2)在0.35~0.80时,样品均为单相的A型沸石,提高n(Al2O3)/n(Si O2)导致晶粒细化。n(Al2O3)/n(Si O2)为0.35、0.45、0.60和0.80时,样品的平均粒径分别为385、329、260和192 nm。
Zeolite A was prepared by a room-temperature liquid synthesis route. The influences of crystallization time and molar ratio of Al2O3/SiO2 on the nucleation and crystal growth were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier infrared spectroscopy (FTIR), respectively. The results show that the reaction is mainly dominated by nucleation at the crystallization time of 120 h, the rapid growth of zeolite A occurs at 120-156 h, and the well-crystallized samples are obtained after 168 h. Compared to zeolite A obtained in conventional autoclave treatment at 95 ℃, the room-temperature crystallization hinders the formation of impurity crystals, and no hydroxylsodalite forms for longer crystallization time. Besides, the room-temperature crystallization decreases the crystal size and results in the aggregation. The zeolite A sample obtained at room temperature is a pure phase when the Al2O3/SiO2 ratio ranges in 0.35~0.80. The increase of Al2O3/SiO2 ratio leads to the decrease of size of zeolite A. The samples obtained at molar ratio Al2O3/SiO2 of 0.35, 0.45, 0.60 and 0.80 have the mean particle sizes of 385, 329, 260 and 192 nm, respectively.