波谱学杂志 ›› 2010, Vol. 27 ›› Issue (3): 436-444.

• 液体及固体NMR • 上一篇    下一篇

用多核固体核磁共振研究CsH2PO4 和CsH5(PO4)2的制备

Seen Ae CHAE1, Young Eun LEE1, Oc Hee HAN1,2*, Sang Geul LEE1   

  1. 1.韩国基础科学研究院 大丘中心,大丘  702-701, 韩国; 2. 忠南国立大学 分析科学技术研究生院,大丘  305-764, 韩国
  • 收稿日期:2010-07-16 出版日期:2010-09-05 发布日期:2010-09-05

Preparation of CsH2PO4 and CsH5(PO4)2 Investigated with Multinuclear Solid-State NMR Spectroscopy

Seen Ae CHAE1, Young Eun LEE1, Oc Hee HAN1,2*, Sang Geul LEE1   

  1. 1. Daegu Center, Korea Basic Science Institute, Daegu, 702-701, Republic of Korea; 2. Graduate School of Analytical Science and Technology, Chungnam National University, Daejeon, 305-764, Republic of Korea
  • Received:2010-07-16 Online:2010-09-05 Published:2010-09-05

摘要:

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Cs2HPO4·1.5H2O (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133Cs 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.

关键词: 固体核磁共振, 固体酸电解质,  CsH2PO4, CsH5(PO4)2, 133Cs 魔角旋转NMR, 31P 魔角旋转NMR, 1H 魔角旋转NMR

Abstract:

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.

Key words: solid-state NMR, solid acid electrolyte, CsH2PO4, CsH5(PO4)2, 133Cs MAS NMR,  31P MAS NMR,  1H MAS NMR

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