离子液中磷酸铝方英石的低温合成及表征.pdfVIP

2010 Chinese Journal of Catalysis Vol. 31 No. 7 文章编号: 0253-9837(2010)07-0776-05 DOI : 10.3724/SP.J.1088.2010.91139 研究论文: 776~780 离子液中磷酸铝方英石的低温合成及表征 徐仁顺, 张维萍, 韩秀文, 包信和 中国科学院大连化学物理研究所催化基础国家重点实验室, 辽宁大连 116023 摘要：在溴化 1-丁基-3- 甲基咪唑离子液体中, 于低温 80 °C 反应 30 min 即可制得结晶完好的磷酸铝方英石. 详细考察了有机胺和 HF 的加入量、反应原料磷铝比和反应时间等对合成固体磷酸盐骨架结构的影响. 粉末 X 射线衍射和高分辨固体核磁共振结果 表明, 合成的方英石晶体为 α 晶相, 磷铝物种大部分位于分子筛骨架上, 并以四配位的形式通过 Al–O–P 键相连. 关键词：离子热合成; 磷酸铝; 方英石; 固体核磁共振; 离子液体 中图分类号：O643 文献标识码：A Low-Temperature Synthesis and Characterization of AlPO-Cristobalite in Ionic Liquid * * XU Renshun, ZHANG Weiping , HAN Xiuwen, BAO Xinhe State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China Abstract: AlPO-cristobalite was prepared at low temperature of 80 °C for 30 min in the [bmim]Br ionic liquid. The effects of reaction con- ditions, such as the amount of organic amine and HF acid, the P/Al ratio, and reaction time, were investigated in detail in the ionothermal synthesis. Powder X-ray diffraction and high-resolution solid-state NMR show that the resultant sample is α-AlPO-cristobalite, and most of the Al and P species are located on the framework and connected by Al–O–P tetrahedron. Key words: ionothermal synthesis; aluminophosphate; cristobalite; solid state nuclear magnetic resonance; ionic liquid 尽管分子筛材料已广泛应用于催化、吸附和分 多新型材料[5~14]. 离等领域, 但新型分子筛材料的合成和应用仍是一 磷酸铝物种种类繁多, 主要包括磷酸铝分子筛 个研究热点[1]. 分子筛通常采用水热和溶剂热两种 (AlPO -n) 和致密相磷酸铝结构 (AlPO )[15,16], 它们