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Method for preparing battery-grade iron phosphate

A ferric phosphate, battery-level technology, applied in the field of electrochemistry, can solve the problems of inability to realize continuous large-scale production of ferric phosphate, low electrolysis efficiency of electrolytic method, large amount of wastewater treatment, etc., achieve high synthesis efficiency, low cost, and ensure repeatability The effect of using

Active Publication Date: 2020-08-14
王家祥
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems in the prior art that the production of battery-grade iron phosphate by chemical methods will produce a large number of by-products, the amount of wastewater treatment is large, causing environmental pollution, and the electrolysis efficiency of the electrolytic method is low, and continuous large-scale production of iron phosphate cannot be realized. The present invention Provides a method for preparing battery-grade iron phosphate by electrolysis that is easy to implement industrially

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  • Method for preparing battery-grade iron phosphate
  • Method for preparing battery-grade iron phosphate
  • Method for preparing battery-grade iron phosphate

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Embodiment 1

[0045] In the electrolytic cell, the iron plate is used as the anode, the graphite plate is used as the cathode, the lithium chloride aqueous solution (LiCl content is 20g / L) is used as the electrolyte, the pH value is adjusted to 10 with lithium hydroxide, and the current density at room temperature is 500A / m 2 For the electrolysis of iron plates, special attention should be paid to safety because hydrogen gas is generated at the cathode; after the electrolysis is completed, a large amount of precipitated products appear in the lower part of the electrolytic tank; hot air at 150 ° C is blown into the solution, and it can be found Within 30 minutes, the lower layer precipitated into a brown floc, and then the reaction solution after generating ferric hydroxide was transferred to the storage tank and left to stand for 24 hours. It can be observed that the mixed reaction solution is separated, the lower layer is a brown precipitate, and the upper layer For the clear liquid, the s...

Embodiment 2

[0047] In the electrolytic cell, the iron rod is used as the anode, the iron plate is used as the cathode, the electrolyte is 40g / L LiCl aqueous solution, the pH is adjusted to 12 with lithium hydroxide, and the current density at room temperature is 100A / m 2 , for the electrolysis of iron rods, because hydrogen gas is generated at the negative electrode, special attention should be paid to safety. When the ferrous hydroxide precipitate is formed at the bottom of the electrolytic cell, the reaction solution after the ferrous hydroxide is continuously pumped into the insoluble anode suspension electrolytic cell for oxidative electrolysis to prepare ferric hydroxide; the dissolved iron electrolytic cell is filled into the circulating electrolysis at the same time liquid to achieve tank liquid level balance. The prepared yellow-brown ferric hydroxide precipitation mixture is left to stand, and the supernatant is drawn out and returned to the electrolytic cell for use as a circula...

Embodiment 3

[0049] Such as figure 1 As shown, iron plates are used at the same time in the anode and cathode in the electrolytic cell, the electrolyte is 30g / L LiCl aqueous solution, the pH is adjusted to 9 with lithium hydroxide, and the current density at room temperature is 1000A / m 2 , Carry out the electrolysis of the iron plate, because hydrogen gas is generated at the negative electrode, special attention should be paid to safety. When ferrous hydroxide precipitates at the bottom of the electrolytic cell, the reaction liquid after ferrous hydroxide is intermittently pumped into the bubbling air oxidation tank. Since the liquid phase is an alkaline environment, a large amount of air is blown in at room temperature , ferrous hydroxide is easily oxidized into yellow-brown ferric hydroxide. In order to shorten the reaction time, the ferrous hydroxide was oxidized to ferric hydroxide by blowing hot air at 120°C, and after 30 minutes of air oxidation, the reaction solution after ferric h...

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Abstract

The invention discloses a preparation method of battery-grade iron phosphate, which comprises the following steps: A. performing electrolysis in an electrolytic cell by using a lithium chloride aqueous solution as an electrolyte, metallic iron as an anode and graphite and metallic iron as a cathode under an alkaline condition that the pH value is greater than or equal to 8 to obtain ferrous hydroxide; B, blowing hot air into the electrolytic cell or an oxidation storage tank to oxidize ferrous hydroxide into ferric hydroxide; C, transferring the reaction solution into a storage tank, standing,separating, adding concentrated phosphoric acid into the ferric hydroxide at the lower layer, and heating to react to generate iron phosphate; and D, filtering the turbid liquid after iron phosphateis generated, carrying out deep micro-crystallization treatment, granulation and sorting on solid iron phosphate, and then carrying out deep washing and drying to obtain a microcrystalline secondary spherical iron phosphate finished product. The method is easy to industrially implement, low in cost, fine in primary crystal grain of the product and uniform in secondary spherical grain, is suitablefor being used as a raw material of the lithium ion battery cathode material lithium iron phosphate, does not generate wastewater in the whole production process, and realizes zero discharge of wastewater.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry, and in particular relates to a method for preparing battery-grade iron phosphate, which can be used as an iron source raw material for lithium iron phosphate, a battery cathode material. Background technique [0002] Iron phosphate is the raw material of lithium iron phosphate, the positive electrode material of the battery. The traditional production method is to use ferrous salt as the raw material, convert it into iron salt through oxidation reaction, and then react with phosphoric acid or phosphate to prepare it. In this process, ferrous phosphate and ferrous nitrate are commonly used as ferrous salt raw materials, and commonly used phosphates are different ammonium salts of phosphoric acid. Due to the large amount of by-products involved in the production process, product washing is relatively cumbersome, and the amount of wastewater treatment is large. The preparation of high-purit...

Claims

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Application Information

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IPC IPC(8): C01B25/37C25B1/00C25B15/08
CPCC01B25/375C25B1/00C25B15/08C01P2004/32C01P2004/61Y02E60/10
Inventor 王家祥余自力何毅王寅
Owner 王家祥