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Cyano complex compounds as well as preparation method and application thereof

A technology of complex compound and cyano group, which is applied in the field of cyano complex compound and its preparation, can solve the problems of poor crystallinity of ferrocyanide, low capacity of sodium ion battery, unsatisfactory cycle stability, etc., and achieve short cycle time, The effect of high capacity and good crystallinity

Active Publication Date: 2017-11-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] But also because of this, the prepared ferrocyanide generally has poor crystallinity, which leads to the low capacity and unsatisfactory cycle stability of the sodium-ion battery assembled as the positive electrode material.

Method used

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  • Cyano complex compounds as well as preparation method and application thereof
  • Cyano complex compounds as well as preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0035] Dissolve ammonium ferrocyanide in deionized water, stir evenly to obtain ferrocyanide ion (Fe(CN) 6 4- ) meter concentration is the solution A of 0.1mol / L; MnCl 2 Dissolved in deionized water to obtain Mn 2+ Solution B (MnCl 2 The molar ratio of ammonium ferrocyanide to ammonium ferrocyanide is 2.5); solution A and solution B were mixed, subjected to hydrothermal reaction at 60°C for 2 hours, filtered, washed and dried to obtain (NH 4 ) x Mn[Fe(CN)] y Precipitation; NaCl is dissolved in the mixed solvent of ethylene glycol and deionized water (the volume ratio of the two is 90:10) to obtain a concentration of 0.2mol / L solution C (the mol ratio of NaCl and ammonium ferrocyanide is 2.5 ), will (NH 4 ) x Mn[Fe(CN)] y Add it into solution C, after ultrasonic dispersion, under nitrogen atmosphere, react at 150°C for 1.5h, then cool, filter, wash and dry to obtain the cyano complex compound Na x Mn[Fe(CN)] y . Through ICP analysis, the x value of the product is 1.7...

Embodiment 2

[0045] Dissolve ammonium ferrocyanide in deionized water, stir evenly to obtain ferrocyanide ion (Fe(CN) 6 4- ) solution A with a concentration of 0.2mol / L; MnCl with a molar ratio of 1:1 2 and FeSO 4 Dissolved in deionized water to obtain Mn 2+ and Fe 2+ Solution B (MnCl 2 with FeSO 4 The ratio of the total moles of ammonium ferrocyanide to the moles of ammonium ferrocyanide is 3); solution A and solution B are mixed, subjected to hydrothermal reaction at 60°C for 2 hours, filtered, washed and dried to obtain (NH 4 ) x mn 0.5 Fe 0.5 [Fe(CN)] y Precipitation; NaCl is dissolved in the mixed solvent of ethylene glycol and deionized water (the volume ratio of the two is 90:10) to obtain a concentration of 0.4mol / L solution C (the mol ratio of NaCl and ammonium ferrocyanide is 3 ), will (NH 4 ) x mn 0.5 Fe 0.5 [Fe(CN)] y Add it into solution C, after ultrasonic dispersion, under nitrogen atmosphere, react at 140°C for 2 hours, then cool, filter, wash and dry to obta...

Embodiment 3

[0048] Dissolve ammonium ferrocyanide in deionized water, stir evenly to obtain ferrocyanide ion (Fe(CN) 6 4- ) meter concentration is solution A of 0.1mol / L; FeCl 2 dissolved in deionized water to obtain Fe 2+ Solution B (FeCl 2 The molar ratio of ammonium ferrocyanide to ammonium ferrocyanide is 3); solution A and solution B are mixed, subjected to hydrothermal reaction at 60°C for 2 hours, filtered, washed and dried to obtain (NH 4 ) x Fe[Fe(CN)] y Precipitation; NaCl is dissolved in a mixed solvent of ethylene glycol and deionized water (the volume ratio of the two is 90:10) to obtain a concentration of 0.2mol / L solution C (N a The mol ratio of Cl and ammonium ferrocyanide is 2.5), with (NH 4 ) x Fe[Fe(CN)] y Add it into solution C, after ultrasonic dispersion, under nitrogen atmosphere, react at 160°C for 1 hour, then cool, filter, wash and dry to obtain the cyano complex compound Na x Fe[Fe(CN)] y , where, x=1.72, y=0.83; the lattice structure is rhombohedral p...

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Abstract

The invention discloses a preparation method of cyano complex compounds. The preparation method comprises specific steps as follows: mixing ammonium ferrocyanide with deionized water to obtain a solution A, mixing soluble salt of bivalent transition metal ions M<2+> with the deionized water to obtain a solution B, and mixing the solution A with the solution B to obtain an intermediate product after a hydrothermal reaction; dissolving sodium salt in an ethylene glycol / deionized water mixed solvent to obtain a solution C, and mixing an intermediate product with the solution C to obtain the cyano complex compounds after an ion exchange reaction. The invention discloses the preparation method of the cyano complex compounds. With adoption of the method, the morphology and the lattice structure of the target product can be regulated; the prepared cyano complex compounds have good crystallinity, and can remarkably improve electrochemical performance of sodium ion batteries after being applied to electrodes of the sodium ion batteries.

Description

technical field [0001] The invention relates to the technical field of novel energy storage batteries, in particular to a cyano complex compound and its preparation method and application. Background technique [0002] Lithium-ion batteries are now widely used in mobile electronic devices, such as smartphones, laptops, etc., and have huge markets in grid energy storage, electric vehicles. However, with the popularization of lithium-ion batteries, especially large-scale use in electric vehicles, the consumption of lithium resources is also huge. However, the reserves of lithium resources are limited, and there is currently no effective and economical technology for the recovery of lithium elements in waste lithium-ion batteries. In contrast, the reserves of sodium on the earth are much higher than that of lithium, and the price is much lower than that of lithium. Therefore, in recent years, sodium-ion batteries have attracted much attention. It is generally believed that s...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M10/054C01C3/12
CPCC01C3/12C01P2002/72C01P2004/62C01P2006/40H01M4/364H01M4/58H01M10/054Y02E60/10
Inventor 谢健沈志龙孙云坡曹高劭赵新兵
Owner ZHEJIANG UNIV
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