Rapid preparation method of low-defect manganese-based Prussian blue under solid-liquid dynamic equilibrium

By controlling the temperature and the amount of chelating agent under solid-liquid dynamic equilibrium, the defects and low conductivity of Prussian blue-based cathode materials were solved, enabling the rapid preparation of high-performance manganese-based Prussian blue and improving the crystal integrity and electrochemical performance of the material.

CN121470513AActive Publication Date: 2026-02-06WENZHOU UNIV CARBON NEUTRALITY TECH INNOVATION RES INST
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Patent Information

Application Number
CN202610027042.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-01-09
Publication Date
2026-02-06
Estimated Expiration
2046-01-09

AI Technical Summary

Technical Problem

Existing technologies for preparing Prussian blue-based cathode materials suffer from problems such as numerous vacancies and crystallization defects, difficulty in precisely controlling lattice water content, low electronic conductivity, long synthesis time, high cost, and low resource utilization.

Method used

By controlling the solubility of sodium ferrocyanide and the nucleation rate of manganese-based Prussian blue under solid-liquid dynamic equilibrium, the chelation component ratio is optimized to achieve dynamic equilibrium in crystal growth, reduce the amount of chelating agent, and rapidly prepare low-defect manganese-based Prussian blue.

Benefits of technology

It achieves high crystal integrity and excellent electrochemical performance, shortens synthesis time, reduces costs, improves resource utilization, and enhances electronic conductivity and discharge capacity.

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Abstract

The invention discloses a rapid preparation method of low-defect manganese-based Prussian blue under solid-liquid dynamic equilibrium, which comprises the following steps: S1, dissolving sodium citrate in deionized water, and then adding manganese acetate and ascorbic acid to form a solution A containing a manganese complex; wherein the molar ratio of the sodium citrate to the manganese acetate to the ascorbic acid is (4.5-5.5): 1: (0.3-0.4); s2, adding sodium ferrocyanide into deionized water, and stirring at a set temperature to form a supersaturated turbid liquid B containing an undissolved sodium ferrocyanide solid; wherein the addition amount of the sodium ferrocyanide far exceeds the saturation solubility of the sodium ferrocyanide at the temperature, so that the system is kept in a solid-liquid two-phase equilibrium state; benefited from the whole-process dynamic saturation environment, compared with a comparison file, the manganese-based Prussian blue prepared by the method has more obvious monoclinic phase characteristics (corresponding to obvious XRD double peaks, obvious strength and good signal-to-noise ratio), the lattice vacancy and coordinated water content are obviously lower than those of a comparison file scheme, and the electronic conductivity is increased by nearly 50%.
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