Establishment of anhydrous synthesis process using molten salts as reaction media

以熔盐为反应介质的无水合成工艺的建立

• 批准号: 11450327
• 负责人: ITO Yasuhiko
• 金额: $ 9.73万
• 依托单位: KYOTO UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 1999
• 资助国家: 日本
• 起止时间: 1999 至 2001
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-11450327/
• 关键词: Molten salt; anhydrous; material synthesis process; Electrochemistry; dehydration; room temperature molten salt; 材料評価プロセス

The purpose of this project is to establish the anhydrous synthesis process that consists of purification of molten slats and separation/recovery of products. In year 1999, we succeeded in reducing the size of electrolysis cell to one half and the volume of molten salts to one tenth. In year 2000, we constructed a new electrolysis cell in an argon glove box having a gas purification equipment. By using this apparatus, it was found that water contamination level in LiCl-KCl melts could be reduced to one tenth compared to a conventional preparation method. In LiCl-KCl-DyCl_3 melts, a DyNi_2 film having 60 μm thickness was formed by potentiostatic cathodic electrolysis at a Ni electrode for 2 hours at 723 K. In LiCl-KCl-SmCl_3 melts, a SmNi_2 film having 20μm thickness was formed by galvanostatic cathodic electrolysis at a Ni electrode for 1hour at 723 K. In year 2001, we synthesized and/or searched for new room-and middle-temperature molten salts. At middle temperature range (200-300℃), it was found that the melting point of LiBr-KBr-CsBr was around 230℃, which was the lowest value among molten alkali halides. When LiH was added to this melt, it was found that hydride ion was formed. By using the electrode reaction of hydride ions, hydrogen absorption properties were evaluated for Ti electrode. At room temperature range, we succeeded in synthesizing a novel room temperature molten salt, EMIF-2.3HF, that has the highest conductivity among all room temperature molten salts at 25℃. It was found that EMIF-2.3HF had a electrochemical window of about 3.2 V. A high performance capacitor was constructed by using this melt.

该项目的目的是建立无水合成过程，该过程包括熔融板条的纯化和产品的分离/恢复。在1999年，我们成功地将电解电池的大小减少到了一半，熔融盐的体积降至十分之一。在2000年，我们在具有气体净化设备的氩气手套箱中构建了一个新的电解电池。通过使用该设备，发现与常规制备方法相比，LICL-KCL-SMCL_3熔体中的水污染水平可以降低至十分之一。在LICL-KCL-DYCL_3融化中，通过在723 k的Ni电极在Ni电极上通过潜在的阴极电解形成了60μm厚度的Dyni_2膜，在723 K中，在LICL-KCL-SMCL_3融化中，Smni_2 y Y型20μm厚度的Smni_2 y e e ni ate at a ni ini the。 2001年，我们合成和/或寻找新房间和中温熔融盐。在中等温度范围（200-300℃）下，发现Libr-KBR-CSBR的熔点约为230℃，这是熔融碱中最低的值。当将Lih添加到该熔体中时，发现形成了氢化物离子。通过使用氢化离子的电极反应，评估了Ti电极滥用氢的特性。在室温范围内，我们成功地合成了一种新型的室温熔融盐EMIF-2.3HF，在25℃的所有室温熔融盐中的电导率最高。发现EMIF-2.3HF的电化学窗口约为3.2V。使用此熔体构建了高性能电容器。

项目成果

T.Tsuda: "Electrochmeical behavior of lanthanum ion in basic AlCl_3-EMIC melts"Progress in Molten Salt Chemistry. Vol.1. 543-547 (2000)

T.Tsuda：“镧离子在碱性 AlCl_3-EMIC 熔体中的电化学行为”熔盐化学进展。

T.Nishikiori, T.Nohira, Y.Ito: "Kinetic Investigation of the Ti-H System by a Molten Salt Electrochemical Technique"J. Electrochem. Soc.. Vol.148. E127-E132 (2001)

T.Nishikiori、T.Nohira、Y.Ito：“通过熔盐电化学技术对 Ti-H 体系进行动力学研究”J。

R. Hagiwara, T. Hirashige, T. Tsuda, Y. Ito: "A highly conductive room temperature molten fluoride : EMIF-2.3HF"J. Electrochem. Soc.. Vol.149(1). D1-D6 (2002)

R. Hagiwara、T. Hirashige、T. Tsuda、Y. Ito：“高导电性室温熔融氟化物：EMIF-2.3HF”J。

T. Nishikiori, T. Nohira, Y. Ito: "Kinetic Investigation of the Ti-H System by a Molten Salt Electrochemical Technique"J. Electrochem. Soc.. Vol.148(3). E127-E132 (2001)

T. Nishikiori、T. Nohira、Y. Ito：“通过熔盐电化学技术对 Ti-H 体系进行动力学研究”J。

R.Hagiwara: "A highly conductive room temperature molten fluoride : EMIF・2.3HF"J. Electrochem. Soc.. Vol.149. D1-D6 (2002)

R.Hagiwara：“高导电性室温熔融氟化物：EMIF·2.3HF”J.Electrochem.Vol.149。