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Low-water and low-defect potassium ferrocyanide manganese Prussian blue cubic crystal and preparation method thereof

A technology of potassium ferrocyanide manganese and Prussian blue, applied in cyanic acid/isocyanic acid and other directions, can solve the problems of increased material preparation cost, can not be reduced, energy consumption and other problems, achieve good economic and application value, easy to operate, reduce The effect of nucleation speed

Active Publication Date: 2022-05-03
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the subsequent treatment under inert gas or high vacuum conditions can make the water of crystallization come out, these post-treatments will consume a lot of energy, cause unnecessary waste, and greatly increase the cost of material preparation; in addition, the physical method of water removal cannot Reduce the high [Fe(CN) in the original material 6 ] 4- Defect rate, and after leaving the crystal water, it is easy to absorb water again when placed in the air, and return to the original state of high water and high defect

Method used

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  • Low-water and low-defect potassium ferrocyanide manganese Prussian blue cubic crystal and preparation method thereof
  • Low-water and low-defect potassium ferrocyanide manganese Prussian blue cubic crystal and preparation method thereof
  • Low-water and low-defect potassium ferrocyanide manganese Prussian blue cubic crystal and preparation method thereof

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preparation example Construction

[0049] The present invention also provides a method for preparing the above-mentioned low-water and low-defect potassium manganese ferrocyanide Prussian blue cubic crystal, which comprises the following steps:

[0050] A. Dissolving potassium ferrocyanide and complexing agent in deionized water to obtain solution A; the molar ratio of potassium ferrocyanide and complexing agent in solution A is 1:20-100;

[0051] B, dissolving the soluble manganese salt in deionized water to obtain solution B;

[0052] C. Drop solution B into solution A, keep warm for reaction, and after the reaction, cool, separate solid and liquid, wash and dry to obtain potassium ferrocyanide Prussian blue cubic crystals.

[0053] The present invention adopts high-concentration complexing agent to improve the combination of complexing agent and Mn ions, thereby realizing the slow release of Mn ions from the complex during the precipitation process and slowing down the precipitation reaction speed; in additi...

Embodiment 1

[0061] Embodiment 1: high temperature+high complexing agent concentration

[0062] A. Dissolve 0.003mol potassium ferrocyanide trihydrate, 0.1mol sodium citrate dihydrate and 0.1mol potassium citrate monohydrate in 100mL deionized water to obtain solution A, and keep the temperature of solution A at 70°C; wherein, The molar ratio of potassium ferrocyanide and citrate complexing agent is 1:67;

[0063] B. Dissolve 0.006mol of manganese nitrate tetrahydrate in 50mL of deionized water to obtain solution B, and keep the temperature of solution B at 70°C;

[0064] C. Drop solution B into solution A at a rate of 0.5mL / min, keep it warm at 70°C for 12 hours, after the reaction, cool, wash and centrifuge the precipitate several times, and finally dry it in an ordinary oven at 80°C Dry for 12 hours to obtain potassium ferrocyanide Prussian blue cubic crystals.

[0065] figure 1 It is the X-ray diffraction pattern of the material obtained in this embodiment, figure 2 and image 3 ...

Embodiment 2

[0066] Embodiment 2: high temperature+high complexing agent concentration

[0067] A, 0.003mol potassium ferrocyanide trihydrate, 0.03mol sodium oxalate and 0.03mol potassium oxalate are dissolved in 50mL deionized water to obtain solution A, keep the temperature of solution A at 95°C; the potassium ferrocyanide and The molar ratio of oxalate complexing agent is 1:20;

[0068] B. Dissolve 0.0045mol of manganese sulfate monohydrate in 100mL of deionized water to obtain solution B, and keep the temperature of solution B at 95°C;

[0069] C. Drop solution B into solution A at a rate of 1mL / min, keep warm at 95°C for 2 hours, after the reaction, cool, wash and centrifuge the precipitate several times, and finally dry it in an ordinary oven at 80°C After 12 hours, potassium ferrocyanide manganese Prussian blue cubic crystals were obtained.

[0070] Figure 6 It is the X-ray diffraction pattern of the material obtained in this embodiment, Figure 7 and Figure 8 A scanning elec...

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Abstract

The invention discloses a low-water and low-defect Prussian blue-like cubic crystal of potassium ferrocyanide manganese and a preparation method thereof, belonging to the technical field of material synthesis. The invention aims to solve the problem of [Fe(CN) 6 ] 4‑ The technical problem of defects and high crystal water provides a low-water and low-defect Prussian blue-like cubic crystal of potassium ferrocyanide manganese, whose general chemical formula is K x Mn[Fe(CN) 6 ] 1‑y □ y ·zH 2 O, 1.9≤x≤2.1, 0≤y≤0.03, 0≤z≤0.2, and the mass content of crystal water is less than 1%. The invention adopts soluble manganese salt and potassium ferrocyanide as raw materials, and by optimizing complexing agent and reaction temperature, the excessively fast precipitation reaction speed is effectively reduced, and the crystal growth time is prolonged, thereby reducing defects and defects in Prussian blue crystals. The purpose of crystal water. Thereby, high-quality near-stoichiometric Prussian blue cubic crystals are obtained.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a low-water and low-defect potassium manganese ferrocyanide Prussian blue cubic crystal and a preparation method thereof. Background technique [0002] Prussian Blue (PB for short), that is, ferric ferrocyanide, chemical formula Fe 4 [Fe(CN) 6 ] 3 , was originally synthesized by the German Diesbach in the early eighteenth century. As the name suggests, Prussian blue was first used as a bright dye and was used in industrial dyeing, pigment ink and other color-related fields. If other transition metals are used to replace part of Fe in Prussian blue, and an appropriate amount of alkali metal or alkaline earth metal elements are introduced, many materials with similar structures can be obtained, which are called Prussian blue analogues (PBA for short). , whose general formula is A x m y [Fe(CN) 6 ] 1-y □ y ·zH 2 O, A stands for alkali metal or alkali...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C3/14
CPCC01C3/14C01P2004/61C01P2002/72C01P2004/03C01P2002/80
Inventor 周爱军要旭许泽民
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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