Co-templating Ionothermal Synthesis and Crystal Structure of a New Layered Aluminophosphate from a Protic Deep Eutectic Solvent

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• 作者：Yuan Li ; Xiangdong Gong ; Lei Liu and Jinxiang Dong
• 关键词：structure-directing agent ; ionothermal synthesis ; deep eutectic solvent ; crystal structure
• 刊名：Chinese Journal of Chemistry
• 出版年：2016
• 出版时间：April, 2016
• 年：2016
• 卷：34
• 期：4
• 页码：419-424
• 全文大小：1190K
• ISSN：1614-7065

文摘

Protic deep eutectic mixtures are usually composed of organic amine hydrochloride salts and hydrogen bond donors in a specific molar ratio. Ionothermal synthesis of aluminophosphate as an example, herein, was reported for the first time from an urea-based protic eutectic mixture, consisting of diethylammonium chloride (DEACl) and 1,3-dimethyl urea (DMU). As a result, a new two dimensional aluminophosphate with 4.8-network, [CH₃NH₃]₂[(C₂H₅)₂NH₂]Al₃(PO₄)₄, has been successfully synthesized by co-templating the DEA and methylamine in situ generated from the decomposition of DMU in the absence of HF. Compared to alkyl quaternary ammonium salts with more alkyl-group connected with N atom, this kind of organic amine salts are more likely as the structure-directing agents to synthesize aluminophosphates in urea-based deep eutectic mixtures. It was also found that HF is crucial to the phase selectivity, a known compound with chain-like structure was obtained with the single methylamine as a structure-directing agent in the presence of HF. These materials were characterized by powder XRD, SEM, TG-DSC, ¹³C CP-MAS NMR and CHN analyses.