用多核固体核磁共振研究CsH_2PO_4和CsH_5(PO_4)_2的制备(英文)

Preparation of CsH_2PO_4 and CsH_5(PO_4)_2 Investigated with Multinuclear Solid-State NMR Spectroscopy

探讨可能用作燃料电池固体酸电解质的化合物CsH2PO4(CDP)和CsH5(PO4)2(CPDP)的制备.CDP和CPDP混合物由摩尔比1:4的Cs2CO3:H3PO4水溶液结晶而成,而CDP和Cs2HPO4.1 .5 H2O( H-DCHP)混合物依其摩尔比1:2的水溶液制备.甲醇清洗能最有效地将CDP从其混合物中分离出来.CDP、CPDP以及H-DCHP的33Cs和31P魔角旋转谱以及CPDP和H-DCHP的1H魔角旋转谱均为首次报道,对各化合物的谱峰做了指认.说明,透过确认合成的电解质以及合成过程所产生的副产物,多核固体核磁共振对于控制固体酸电解质合成的品质是一个非常有用的工具.

We attempted to prepare CsH2PO4 （CDP） and CsH5（PO4）2 （CPDP）,compounds known to be promising solid acid electrolytes for fuel cells.The CDP and CPDP mixture was crystallized from an aqueous solution of Cs2CO3：H3PO4,in a molar ratio of 1：4,while the mixture of CDP and Cs2HPO4·1.5H2O （H-DCHP） was obtained from the aqueous solution in a molar ratio of 1：2.Methanol washing was most effective in separating the CDP from the mixture.The 133Cs and 31P MAS NMR spectra of CDP,CPDP,and H-DCHP,and the 1H MAS NMR spectra of CPDP and H-DCHP were reported for the first time and the peaks corresponding to each compound assigned.Herein,we demonstrated multinuclear SS-NMR to be a very useful tool to control the quality of the syntheses of solid acid electrolytes by identification of the electrolytes synthesized and the by-products produced in the process of the syntheses.