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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AI-Extracted Technical Summary

Problems solved by technology

[0005] But also because of this, the prepared ferrocyanide generally has poor crystallinity, which leads to the low...
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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.

Application Domain

Iron cyanidesCell electrodes +1

Technology Topic

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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(3)
  • Comparison scheme(2)

Example Embodiment

[0034] Example 1
[0035] Dissolve ammonium ferrocyanide in deionized water, stir evenly to obtain ferrocyanide ion (Fe(CN) 6 4- ) Solution A with a concentration of 0.1mol/L; add MnCl 2 Dissolve in deionized water to obtain Mn 2+ Calculate the concentration of 0.2mol/L solution B (MnCl 2 The molar ratio with ammonium ferrocyanide is 2.5); Mix solution A and solution B, hydrothermally react at 60°C for 2h, filter, wash, and dry to obtain (NH 4 ) x Mn[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 solution C with a concentration of 0.2mol/L (the molar ratio of NaCl and ammonium ferrocyanide is 2.5 ), will (NH 4 ) x Mn[Fe(CN)] y Add to solution C, after ultrasonic dispersion, react for 1.5h at 150°C under nitrogen atmosphere, 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 1.75, the y value is 0.85, the crystal lattice structure is rhombohedral phase, and the particle size is 200-400nm.
[0036] figure 1 The X-ray diffraction spectrum of the cyano complex compound prepared in this embodiment can be attributed to sodium ferromanganese cyanide.
[0037] The cyano complex compound prepared in this example was used as the positive electrode, sodium metal was used as the negative electrode, glass fiber (brand Whatman GF/D) was used as the separator, and NaPF 6 The ethylene carbonate (EC)/diethyl carbonate (DEC) solution is the electrolyte. The battery is assembled in a glove box filled with argon, and the charge and discharge test is performed. The charge and discharge curve is as follows figure 2 Shown. Constant current charge and discharge test (current density 30mA/g, voltage range 2V ~ 4V. From the figure, the capacity can reach 151mAh/g.

Example Embodiment

[0044] Example 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 Dissolve in deionized water to obtain Mn 2+ And Fe 2+ The total concentration of solution B (MnCl 2 With FeSO 4 The ratio of the total number of moles to the number of moles of ammonium ferrocyanide is 3); Mix Solution A and Solution B, hydrothermally react at 60°C for 2h, filter, wash, and dry to obtain (NH 4 ) x Mn 0.5 Fe 0.5 [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 solution C with a concentration of 0.4 mol/L (the molar ratio of NaCl and ammonium ferrocyanide is 3 ), will (NH 4 ) x Mn 0.5 Fe 0.5 [Fe(CN)] y Add to solution C, after ultrasonic dispersion, react at 140℃ for 2h under nitrogen atmosphere, then cool, filter, wash and dry to obtain the cyano complex compound Na x Mn 0.5 Fe 0.5 [Fe(CN)] y , Where x=1.61, y=0.77; the lattice structure is rhombohedral phase, and the particle size is 200-400nm.
[0046] The cyano complex compound prepared in this example was used as the positive electrode, sodium metal was used as the negative electrode, glass fiber (brand Whatman GF/D) was used as the separator, and NaPF 6 The ethylene carbonate (EC)/diethyl carbonate (DEC) solution is the electrolyte, the battery is assembled in a glove box filled with argon, and the charge and discharge test is performed. Constant current charge and discharge test (current density 30mA/g, voltage range 2V ~ 4V, show that the capacity can reach 142mAh/g.

Example Embodiment

[0047] Example 3
[0048] Dissolve ammonium ferrocyanide in deionized water, stir evenly to obtain ferrocyanide ion (Fe(CN) 6 4- ) Solution A with a concentration of 0.1mol/L; add FeCl 2 Dissolve in deionized water to obtain Fe 2+ Calculate the concentration of 0.2mol/L solution B (FeCl 2 The ratio of moles to ammonium ferrocyanide is 3); Mix solution A and solution B, hydrothermally react at 60℃ for 2h, filter, wash, and dry 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 solution C(N) with a concentration of 0.2mol/L a The molar ratio of Cl and ammonium ferrocyanide is 2.5), the (NH 4 ) x Fe[Fe(CN)] y Add to solution C, after ultrasonic dispersion, under nitrogen atmosphere, after reacting at 160℃ for 1 hour, then cooling, filtering, washing and drying, the cyano complex compound Na is obtained x Fe[Fe(CN)] y In the formula, x=1.72, y=0.83; the crystal lattice structure is rhombohedral phase, and the particle size is 200-400nm.
[0049] The ferrocyanide-based positive electrode material prepared in this example was used as the positive electrode, sodium metal was used as the negative electrode, glass fiber (brand Whatman GF/D) was used as the separator, and NaPF 6 The ethylene carbonate (EC)/diethyl carbonate (DEC) solution is the electrolyte, the battery is assembled in a glove box filled with argon, and the charge and discharge test is performed. Constant current charge and discharge test (current density 30mA/g, voltage range 2V ~ 4V, show that the capacity can reach 148mAh/g.
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PUM

PropertyMeasurementUnit
Current density30.0ma/g
Current density30.0a/g
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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