Preparation method and application of battery grade manganese sulfate

A manganese sulfate, battery-grade technology, applied in manganese sulfate, battery electrodes, secondary batteries, etc., can solve the problems of weak participation, high cost, and difficult recovery process of precipitated slag ions, so as to reduce costs, ensure purity, Reduce the effect of the extraction process

Active Publication Date: 2020-05-29
GUANGDONG JIANA ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the prior art, some preparation methods do not participate in the reaction due to the same ion effect, so that more manganese sulfide needs to be used to achieve the same precipitation effect, and the cost is high
In some preparation methods, when using copper, cobalt, and zinc ions in the sodium sulfide precipitation solution, the precipitation slag will be mixed with various ions, making the precipitation slag more difficult in the subsequent ion recovery process

Method used

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  • Preparation method and application of battery grade manganese sulfate
  • Preparation method and application of battery grade manganese sulfate

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preparation example Construction

[0051] In a first aspect, in at least one embodiment, a method for preparing battery-grade manganese sulfate is provided, comprising the steps of:

[0052] (A) obtain the first filtrate after the precipitation of copper ions, calcium ions and zinc ions in the copper manganese chloride solution;

[0053] (B) under a protective atmosphere, mix the first filtrate, the manganese precipitation agent and the bottom liquid, carry out the manganese precipitation reaction, and separate the solid and liquid to obtain manganese hydroxide;

[0054] (C) Manganese hydroxide is mixed with concentrated sulfuric acid, neutralized to obtain crude manganese sulfate, and refined to obtain battery-grade manganese sulfate;

[0055] Wherein, in step (B), the manganese precipitation agent comprises ammoniacal liquor;

[0056] The base solution consists of ammonia and soluble hydroxides.

[0057] The preparation method of battery-grade manganese sulfate provided by the present invention makes full u...

Embodiment 1

[0122] The present embodiment provides a kind of preparation method of battery grade manganese sulfate, and its steps are as follows:

[0123] (1) Add solid sodium sulfate to the copper manganese chloride solution at a ratio of 110g / L, adjust the pH of the solution to 2.5, and perform a calcium precipitation reaction. After 2 hours, continue to add sodium carbonate solid, adjust the pH value of the solution to 5.0, carry out copper precipitation reaction and secondary calcium precipitation reaction, and filter after the reaction to obtain copper calcium slag and copper calcium precipitation liquid;

[0124] (2) Heat up the copper-calcium solution to 85°C, add sodium fluoride solids to 8 times the mass of calcium ions in the copper-calcium solution, adjust the pH of the solution to 5.16 with ammonium bicarbonate solid, and keep the reaction for 3 hours After filtration, calcium slag and calcium precipitated liquid are obtained;

[0125] (3) Add a sodium sulfide solution (conce...

Embodiment 2

[0129] The present embodiment provides a kind of preparation method of battery grade manganese sulfate, and its steps are as follows:

[0130] (1) Add ammonium sulfate solid to the copper manganese chloride liquid at a ratio of 80g / L, adjust the pH of the solution to 3.5, and perform a calcium precipitation reaction. After 1 hour, continue to add sodium hydroxide solid, adjust the pH value of the solution to 5.2, carry out copper precipitation reaction and secondary calcium precipitation reaction, and filter after the reaction to obtain copper-calcium slag and copper-calcium precipitation liquid;

[0131] (2) Heat up the copper-calcium solution to 70°C, add potassium fluoride solid at 10 times the mass of calcium ions in the copper-calcium solution, adjust the pH value of the solution to 6 with ammonium bicarbonate solid, and keep the reaction for 2 hours After filtration, calcium slag and calcium precipitated liquid are obtained;

[0132] (3) Add a sodium sulfide solution (c...

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Abstract

The invention belongs to the technical field of hydrometallurgy, and relates to a preparation method and application of battery grade manganese sulfate. The preparation method of the battery grade manganese sulfate comprises the following steps of: (A) precipitating copper ion, calcium ion and zinc ion in a copper chloride manganese solution to obtain first filtrate; (B) in a protective atmosphere, mixing the first filtrate, a precipitating manganese agent and a base solution for manganese precipitation reaction and separation of solid and liquid to obtain manganese hydroxide; (C) mixing themanganese hydroxide with concentrated sulfuric acid for neutral reaction to obtain coarse manganese sulfate, and refining the coarse manganese sulfate to obtain the battery grade manganese sulfate; wherein in step (B), the precipitating manganese agent comprises ammonia water; and the base solution comprises the ammonia water and soluble hydroxide. The preparation method of the battery grade manganese sulfate can not only achieve preparation of the battery grade manganese sulfate, but also benefit recovery of zinc, copper, calcium and the like, thereby maximizing utilization of copper-manganese chloride waste liquor, reducing cost and conforming to a concept of sustainable development.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy, and in particular relates to a preparation method and application of battery-grade manganese sulfate. Background technique [0002] Due to the widespread use of nickel-cobalt lithium manganese oxide cathode materials in lithium-ion batteries, the demand for battery-grade manganese sulfate is also increasing. The existing method for preparing battery-grade manganese sulfate has complex processes, which makes the cost of battery-grade manganese sulfate products relatively high. [0003] During the wet extraction process of cobalt, a waste liquid mainly containing copper and manganese will be produced. This waste liquid is called copper manganese chloride liquid. raw materials. [0004] In the prior art, there are many preparation methods using copper-manganese chloride solution as a raw material for preparing battery-grade manganese sulfate. However, in the prior art, some preparation me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/10H01M4/505H01M4/525H01M10/0525
CPCC01G45/10C01P2006/80H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 张颖汤依伟彭灿黄铁熙
Owner GUANGDONG JIANA ENERGY TECH CO LTD
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