Method for preparing FexPO4 by electrolyzing ferrophosphorus

A technology for electrolysis of ferrophosphorus and electrolysis, which is applied in the electrolysis process, electrolysis components, electrodes, etc., and can solve the problem of the type and content of impurities, the difficulty in controlling the particle size and morphology of the product, the different types and contents of ferrophosphorus impurities, and the influence of the particle size of ferrophosphorus raw materials. Larger problems such as overcoming the difficulty of raw material ratio, reducing the influence of impurity elements, and eliminating the easy corrosion of equipment

Inactive Publication Date: 2013-01-02
SICHUAN UNIV
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  • Application Information

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Problems solved by technology

In our original special implementation process of preparing iron phosphate from iron phosphorus [Chinese patent CN101659406A], relying on iron phosphorus to be oxidized to Fe at high temperature in a dry oxygen-containing atmosphere 2 o 3 and P 2 o 5 Then react again to reduce the impact of impurity elements in ferrophosphorus on the product, and do not directly prepare ferric phosphate with controllable morphology by electrolytic dedoping of ferrophosphorus at room temperature, which is obviously different from the process and technology of this application
In addition, the types and contents of impurities in ferrophosphorus obtained by different processes in different regions are different, making it difficult to fully purify ferrophosphorus
However, these impurities will affect the performance of the product, and it needs to be purified to a certain extent
In addition, when preparing ferric phosphate directly from ferrophosphorus, it needs to be completed in a dry and oxidizing atmosphere at a relatively high temperature. The reaction process is complex and costly, and the requirements for equipment are relatively high. Greater impact
[0005] In order to overcome the current Fe x PO 4 The deficiencies in the production process solve the problem of preparing Fe by ferrophosphorus x PO 4 High temperature dry oxidizing atmosphere, uncertain types and contents of impurities in ferrophosphorus raw materials make it difficult to fully purify impurity elements and Fe x PO 4 The technical problem that the product particle size and shape are difficult to control, simplify the preparation process, reduce energy consumption, and reduce waste discharge, the present invention proposes a new process method completely different from the above invention: electrolysis of ferrophosphorus in aqueous solution to prepare Fe x PO 4 , apply a voltage of 1 to 20V, and a current density of 5 to 1500A m -2 , to obtain Fe by electrolysis x PO 4 solution, adding alkaline oxides, adjusting the pH value of the solution to 1-8, Fe x PO 4 Precipitated, filtered and washed to obtain Fe x PO 4 finished product

Method used

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  • Method for preparing FexPO4 by electrolyzing ferrophosphorus
  • Method for preparing FexPO4 by electrolyzing ferrophosphorus

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Effect test

Embodiment 1

[0028] Preparation of iron phosphate from iron phosphorus by electrolysis, and preparation of FePO by iron phosphorus FeP 4 , the electrolytic device is composed of ferrophosphorus and graphite, ferrophosphorus is used as anode, placed in the anode bag, graphite is used as cathode, tap water is used as electrolyte, 1% phosphoric acid is added to increase conductivity, electrolysis is performed on a DC power supply, and the voltage is 5-7V , the current is 1.5-2A, the electrolysis time is 50-60h, adding ammonia water to the electrolyzed solution to adjust the pH=5-6, after filtering, washing and drying, the finished product of ferric phosphate is obtained.

[0029] In this reaction, ammonia water is added to adjust the pH value, and the remaining solution after filtration is ammonium phosphate, which can be used as chemical fertilizer, realizing green and clean production.

Embodiment 2

[0031] Ferrophosphorus Fe by electrolysis 2 Preparation of iron phosphate by P, preparation of FePO with ferrophosphorus as iron source and part of phosphorus source 4 , the electrolysis device is composed of iron phosphorus and graphite, iron phosphorus is used as anode, graphite is used as cathode, aqueous solution is used as electrolyte, phosphoric acid is used as a supplementary phosphorus source, and the conductivity of the aqueous solution is also improved. Electrolyzed on a DC power supply, the voltage is 4~ 6V, current 1.5-2A, electrolysis time 30-40h, add ammonium carbonate to the electrolyzed solution to adjust pH=4-5, filter, wash and dry to obtain finished iron phosphate.

[0032] In this reaction, ammonium carbonate is added to adjust the pH, and the remaining solution after filtration is ammonium phosphate, which can be used as chemical fertilizer, realizing green and clean production.

Embodiment 3

[0034] Ferrophosphorus Fe by electrolysis 1.5 P prepares ferrous phosphate, and prepares Fe with ferrophosphorus as iron source and part of phosphorus source 3 (PO 4 ) 2 , the electrolytic device is composed of ferrophosphorus and graphite, ferrophosphorus is used as the anode, placed in the anode bag, graphite is used as the cathode, the aqueous solution is used as the electrolyte, and ammonium phosphate is used as the supplementary phosphorus source, which also improves the conductivity of the aqueous solution. On electrolysis, the voltage is 5-7V, the current is 1.8-2A, and the electrolysis time is 40-45h. Ammonium bicarbonate is added to the electrolyzed solution to adjust the pH to 6-7. After filtering, washing and drying, phosphite Iron products.

[0035] In this reaction, ammonia water is added to adjust the pH, and the remaining solution (ammonium phosphate) after filtration can be used as fertilizer. Realized green and clean production.

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Abstract

The invention relates to a method for preparing FexPO4 by electrolyzing ferrophosphorus, which comprises the following steps: by using ferrophosphorus as the anode and providing an oxygen source by using oxygen in water as the product, electrolyzing to obtain a FexPO4 solution, wherein only ferrophosphorus and water are consumed in the reaction process; adding basic oxides to regulate the pH value of the solution so as to settle out FexPO4; and granulating, filtering and washing to obtain the finished FexPO4 product. In the method, cheap ferrophosphorus is converted into high-value FexPO4 by using the electrolytic reaction process; the source of ferrophosphorus is not limited; the influence of impurity elements on the product can be eliminated; the product can be granulated into controlled shape and particle size; the byproduct H2 can be recycled; the treated filtrate can be used cyclically; the obtained finished FexPO4 product has the advantages of high purity, small particle size, easily controlled shape, and low power consumption; the reaction process has low requirements for equipment and is easy to operate; and the preparation method has the advantages of simple technique, high resource utilization rate, low cost, low investment, good benefit, high cleanness and environmental protection, can be easily industrialized, and is suitable for high-value comprehensive utilization of byproducts in chemical industry and large-scale industrial low-cost clean production of high-end phosphates.

Description

technical field [0001] The invention relates to a method for preparing Fe by electrolysis of ferrophosphorus x PO 4 The method uses the reaction process to eliminate the influence of impurities in the raw materials on the product. The product has high purity, fine particle size, easy control of shape, and simple process. It can be applied to the high-value comprehensive utilization of chemical solid waste and the low cost of high-end phosphate materials. Clean manufacturing. Background technique [0002] Fe x PO 4 It is a kind of iron phosphate, which is widely used in energy materials, catalysts, ceramics, food additives and other fields. In the field of energy materials, Fe x PO 4 It can be used as an electrode material (its electrochemical performance is greatly affected by the crystal form of the material and the preparation method, among which amorphous FePO 4 The operating voltage is 3V), and can also be used as a preparation of LiFePO 4 , LiFeP 2 o 7 and Li ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/00C25B11/04
Inventor 闫康平王贵欣刘严
Owner SICHUAN UNIV
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