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Preparation method of high-purity sodium chromite

A sodium chromite, high-purity technology, applied in separation methods, chemical instruments and methods, chromium compounds, etc., can solve the influence of sodium chromite on electrochemical performance, low purity of sodium chromite samples, long reaction time, etc. problem, to achieve the effect of fine particle size, good crystal integrity, and complete reaction

Active Publication Date: 2022-03-18
四川省绵阳市华意达化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cr(Ⅵ) reduction to prepare sodium chromite has incomplete Cr(Ⅵ) reduction, resulting in lower purity of sodium chromite sample and longer reaction time
[0004] When sodium chromite is used as the positive electrode material, the presence of impurity phases has a great impact on the electrochemical performance of sodium chromite, which will cause a certain degree of capacity loss

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0027] A kind of preparation method of high-purity sodium chromite of the present invention comprises the following steps:

[0028] Step 1. Mix chromium oxide and 20% nitric acid solution according to the solid-to-liquid mass ratio of 1:10, stir at room temperature for 2 hours, filter, wash chromium oxide with high-purity water until the washing water is neutral, and dry at 60°C for 4 hours; mix sodium carbonate with high-purity water Mix according to the mass ratio of 2:1, heat to 60°C, stir and add 2mL ferric chloride solution with a concentration of 1mg / mL, keep the temperature at 60°C and let it stand for 10h, filter out the precipitate impurities, and continue to heat the filtrate at 60°C until the filtrate Concentrate, cool and crystallize, centrifuge and dehydrate, detect that the chloride ion content is less than 0.001%, heat to melt and dry at 110°C for 6 hours;

[0029] Step 2. Mix the pretreated chromium oxide and sodium carbonate in a molar ratio of 1:1.2, pulveriz...

Embodiment 2

[0033] A kind of preparation method of high-purity sodium chromite of the present invention comprises the following steps:

[0034] Step 1. Mix chromium oxide and 20% nitric acid solution according to the solid-to-liquid mass ratio of 1:10, stir at room temperature for 2 hours, filter, wash chromium oxide with high-purity water until the washing water is neutral, and dry at 60°C for 4 hours; mix sodium carbonate with high-purity water Mix according to the mass ratio of 2:1, heat to 60°C, stir and add 2mL ferric chloride solution with a concentration of 1mg / mL, keep the temperature at 60°C and let it stand for 10h, filter out the precipitate impurities, and continue to heat the filtrate at 60°C until the filtrate Concentrate, cool and crystallize, centrifuge and dehydrate, detect that the chloride ion content is less than 0.001%, heat to melt and dry at 110°C for 6 hours;

[0035] Step 2, mixing the pretreated chromium oxide and sodium carbonate in a molar ratio of 1:1.1, pulve...

Embodiment 3

[0039] A kind of preparation method of high-purity sodium chromite of the present invention comprises the following steps:

[0040] Step 1. Mix chromium oxide and 20% nitric acid solution according to the solid-to-liquid mass ratio of 1:10, stir at room temperature for 2 hours, filter, wash chromium oxide with high-purity water until the washing water is neutral, and dry at 60°C for 4 hours; mix sodium carbonate with high-purity water Mix according to the mass ratio of 2:1, heat to 60°C, stir and add 2mL ferric chloride solution with a concentration of 1mg / mL, keep the temperature at 60°C and let it stand for 10h, filter out the precipitate impurities, and continue to heat the filtrate at 60°C until the filtrate Concentrate, cool and crystallize, centrifuge and dehydrate, detect that the chloride ion content is less than 0.001%, heat to melt and dry at 110°C for 6 hours;

[0041]Step 2. Mix the pretreated chromium oxide and sodium carbonate in a molar ratio of 1:1, pulverize t...

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Abstract

The invention discloses a preparation method of high-purity sodium chromite. The method comprises the following steps: firstly, carrying out nitric acid-high-pressure closed digestion pretreatment on chromic oxide, and carrying out ultrasonic vibration recrystallization purification pretreatment on sodium carbonate; mixing the pretreated chromic oxide and sodium carbonate according to a certain proportion, carrying out ultralow-temperature liquid nitrogen ball-milling, crushing and mixing, and then carrying out compression molding; then carrying out high-temperature solid-phase reaction in an inert atmosphere; and finally, washing the cooled reactant with a polar solvent, filtering, and carrying out vacuum drying to obtain the high-purity sodium chromite. The chromium oxide and the sodium carbonate are pretreated before the high-temperature solid-phase reaction of the chromium oxide and the sodium carbonate, so that the purity of the prepared sodium chromite is improved; through ultralow-temperature liquid nitrogen ball milling and mixing treatment, the particle sizes of chromic oxide and sodium carbonate are reduced, the reaction specific surface area is increased, reactants are mixed more uniformly, and the reaction is more thorough. The sodium chromite material prepared by the method is high in purity, uniform in particle size distribution and good in crystal integrity.

Description

technical field [0001] The invention belongs to the technical field of sodium ion batteries, and in particular relates to a preparation method of high-purity sodium chromite. Background technique [0002] As a promising electrochemical energy storage system, sodium-ion batteries have the characteristics of wide sources of sodium and abundant resources, and have become one of the research hotspots in the field of electrochemical energy storage in recent years. Cathode materials are an important part of battery systems, and layered oxide materials are considered ideal cathode materials for sodium-ion batteries due to their stable crystal structure and high reversible capacity. The sodium chromite with a layered structure is applied to the positive electrode material of the sodium ion battery, and the obtained sodium ion battery has high reversible capacity, high electrochemical activity and excellent cycle stability. [0003] The methods for preparing sodium chromite mainly i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G37/00B01D9/00B01J19/18H01M4/58H01M10/054
CPCC01G37/00B01D9/00B01J19/18H01M4/5825H01M10/054C01P2006/80Y02E60/10
Inventor 肖棱尹春林颜欣杨丽婷樊诗贤袁小超
Owner 四川省绵阳市华意达化工有限公司
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