用多核固体核磁共振研究CsH2PO4 和CsH5(PO4)2的制备

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

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 HAN^1,2*,Sang Geul LEE¹

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 CsH₂PO₄and CsH₅(PO₄₎₂ Investigated with Multinuclear Solid-State NMR Spectroscopy

Seen Ae CHAE¹, Young Eun LEE¹, Oc Hee HAN^1,2*,Sang Geul LEE¹

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/Abstract

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

中图分类号:

O482.53

Seen Ae CHAE, Young Eun LEE, Oc Hee HAN, Sang Geul LEE. 用多核固体核磁共振研究CsH₂PO₄ 和CsH₅(PO₄)₂的制备[J]. 波谱学杂志, 2010, 27(3): 436-444.

Seen Ae CHAE, Young Eun LEE, Oc Hee HAN, Sang Geul LEE. Preparation of CsH₂PO₄and CsH₅(PO₄₎₂ Investigated with Multinuclear Solid-State NMR Spectroscopy[J]. Chinese Journal of Magnetic Resonance, 2010, 27(3): 436-444.

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用多核固体核磁共振研究CsH₂PO₄ 和CsH₅(PO₄)₂的制备

Preparation of CsH₂PO₄and CsH₅(PO₄₎₂ Investigated with Multinuclear Solid-State NMR Spectroscopy

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