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Preparation method for battery grade ferrous sulfate heptahydrate crystal

A technology of ferrous sulfate and ferrous sulfate solution, which is applied in the direction of ferric sulfate, can solve the problem of insufficient purity of battery-grade ferrous sulfate heptahydrate crystals, avoid ferrous oxidation and the consumption of a large amount of steam, and avoid the concentration and evaporation process , the effect of reducing emissions

Active Publication Date: 2016-02-03
HUBEI WANRUN NEW ENERGY TECH DEV
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  • Application Information

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Problems solved by technology

[0009] The present invention is in order to solve the problem that the purity of battery-grade ferrous sulfate heptahydrate crystals is not high enough by using titanium dioxide to produce by-product ferrous sulfate, and provides a kind of preparation method of battery-grade ferrous sulfate heptahydrate crystals, which can obtain The product has high purity and can be conveniently stored for a long time. The content of impurities and ferric iron is low, while the cost is low and the process is simple.

Method used

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preparation example Construction

[0031]The preparation method of the battery-grade ferrous sulfate heptahydrate crystal of the present invention is to use titanium dioxide production by-product ferrous sulfate as raw material, adopt the operation of impurity removal-filter-crystallization-drying, utilize the solubility of ferrous sulfate to change with temperature difference to prepare ferrous sulfate heptahydrate. The impurity removal process is to use a reducing agent to reduce the ferric iron in the by-product ferrous sulfate of titanium dioxide production to ferrous iron, and at the same time add ferrous sulfide to remove heavy metals such as cobalt, nickel, zinc, copper, lead, and cadmium Ions, using fluoride to remove calcium and magnesium ions, so as to purify the ferrous sulfate solution; then obtain pure ferrous sulfate solution through flocculation and filtration, and obtain ferrous sulfate crystals through crystallization, and can control the particle size by adding seeds After solid-liquid separat...

Embodiment 1

[0050] Utilize titanium dioxide to produce by-product ferrous sulfate to prepare battery grade ferrous sulfate heptahydrate crystal, adopt the following steps:

[0051] (1) Reduction and impurity removal, adding ferrous sulfate, a by-product of titanium dioxide production, into deionized water to prepare a concentration of ferrous sulfate of 415g / l, then raising the temperature to 60°C, adding a reducing agent, and maintaining the temperature of the process at 60°C, after 2 hours of reaction, raise the pH of the ferrous sulfate solution to 4.2, then add ferrous sulfide powder, react at 55°C for 2 hours, then add fluoride, and react at 86°C for 4 hours;

[0052] (2) Flocculation and filtration, cool down the solution after the reaction to a temperature of 60°C, add flocculants and filter aids, the amount of flocculants added to each cubic ferrous sulfate solution is 0.3g, and the amount of diatomaceous earth added 2kg, clarified for 30 minutes after flocculation and stirring fo...

Embodiment 2

[0063] Utilize titanium dioxide to produce by-product ferrous sulfate to prepare battery grade ferrous sulfate heptahydrate crystal, adopt the following steps:

[0064] (1) Reduction and impurity removal, adding ferrous sulfate, a by-product of titanium dioxide production, into deionized water to make the concentration of ferrous sulfate 430g / l, then raising the temperature to 70°C, adding a reducing agent, and maintaining the temperature of the process at 70°C, after 2 hours of reaction, raise the pH of the ferrous sulfate solution to 5, then add ferrous sulfide powder, react at 70°C for 2 hours, then add fluoride, and react at 91°C for 5 hours;

[0065] (2) Flocculation and filtration, cool down the solution after the reaction to a temperature of 65°C, add flocculants and filter aids, the amount of flocculants added to each cubic ferrous sulfate solution is 0.8g, and the amount of diatomaceous earth added 3kg, clarified for 50 minutes after flocculation and stirring for 60 m...

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Abstract

The preparation method for battery grade ferrous sulfate heptahydrate crystal of the present invention includes using ferrous sulphate which is the by-product in the titanium dioxide production as raw material, using the operation of purification, filtration, crystallization and dryness, and preparing ferrous sulfate heptahydrate by using the difference of the solubility of ferrous sulphate changing with the temperature. The operation of purification includes performing reduction of ferric iron in ferrous sulphate which is the by-product in the titanium dioxide production to ferrous iron by using a reducing agent, adding ferrous sulfide to remove the heavy metal ions such as cobalt, nickel, zinc, copper, plumbum and cadmium, and using fluoride to remove calcium and magnesium ions. The preparation method uses vacuum drying and packaging, and the main content of ferrous sulfate heptahydrate in the dried material is more than 99.7%. The preparation method has simple technology and low cost, can recycle fluorinion by precipitation conversion, and can reduce the discharge of hazardous waste. Moreover, the prepared product has high purity, low impurity and ferric iron contents, and can be long-term storage. The recovery rate of ferrous sulphate is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of energy material preparation and relates to battery materials, in particular to a method for preparing battery-grade ferrous sulfate heptahydrate crystals. Background technique [0002] The preparation of ferrous sulfate heptahydrate crystal comprises the following methods at present: [0003] One is to add sulfuric acid to dissolve the iron powder or iron sheet, then adjust the pH of the solution to about 1-4, filter, and obtain the ferrous sulfate heptahydrate crystal after the obtained ferrous sulfate solution is cooled, crystallized and dried. The iron powder or iron sheet used requires purity High, less impurities, this process is short, but the problem is that due to the high purity requirements of iron powder or iron sheet, so the cost of raw materials is high, energy consumption is large, a large amount of gas containing acid mist needs to be processed, and the reaction time is long; [0004] The ...

Claims

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Application Information

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IPC IPC(8): C01G49/14
CPCC01G49/14C01P2004/60C01P2006/80
Inventor 刘世琦
Owner HUBEI WANRUN NEW ENERGY TECH DEV
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