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Method for preparing battery-level ferric phosphate using pyrite cinders

A technology of pyrite slag and iron phosphate, applied in chemical instruments and methods, removal of phosphorus compounds and solid wastes, etc., can solve the problems of low dissolution rate of iron oxide, difficult to effectively control impurities, etc., to reduce production costs, Mild raw material requirements and the effect of resource utilization

Inactive Publication Date: 2012-10-17
LVLING CHEM GRP CO LTD JIANGSU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing battery-grade iron phosphate by using pyrite slag, and effectively solve the problem of low dissolution rate of iron oxide in pyrite slag and problems in the preparation process of battery-grade iron phosphate materials. Impurities are difficult to effectively control and other issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The main components of the used pyrite slag raw material in the present embodiment are: ~ 90% Fe 2 o 3 , ~5% SiO 2 , ~1% CaO, ~1% MgO, ~1% Al 2 o 3 , and ~2% other impurities, the specific process is as follows:

[0032] 1) Configure 500ml of acetic acid and n-octanol mixed solvent of 0.5mol / l;

[0033] 2) adding 100ml of sulfuric acid with a mass fraction of 50% to the mixed solvent to obtain 600ml of composite acidic medium;

[0034] 3) Put the above-mentioned composite acidic medium and 7.5 grams of pyrite slag together into a 1000ml three-hole flask, put the above-mentioned three-hole flask into a magnetically stirred 100°C oil bath, and place a straight-run condenser on it , start the leaching reaction, keep the reaction for 240 minutes, stop the water bath and filter to obtain an iron-containing organic phase and an aqueous solution phase. After measurement, the iron ion concentration in the organic phase is about 3g / L;

[0035] 4) Get 300ml of the above-men...

Embodiment 2

[0039] The main components of the used pyrite slag raw material in the present embodiment are: ~ 90% Fe 2 o 3 , ~5% SiO2 , ~1% CaO, ~1% MgO, ~1% Al 2 o 3 , and ~2% other impurities, the specific process is as follows:

[0040] 1) Configure 500ml of formic acid and tributyl phosphate mixed solvent of 5mol / l;

[0041] 2) Add 100ml of hydrochloric acid with a mass fraction of 10% to the above mixed solvent to obtain 600ml of composite acidic medium;

[0042] 3) Put the above-mentioned composite acidic medium and 75 grams of pyrite slag into a 1000ml three-hole flask, put the above-mentioned three-hole flask into a magnetically stirred 120°C oil bath, and place a straight-run condenser on it , start the leaching reaction, keep the reaction for 240 minutes, stop the water bath and filter to obtain an iron-containing organic phase and an aqueous solution phase. After measurement, the concentration of iron ions in the organic phase is about 20g / L;

[0043] 4) Get 300ml of the ab...

Embodiment 3

[0047] The main components of the used pyrite slag raw material in the present embodiment are: ~ 90% Fe 2 o 3 , ~5% SiO 2 , ~1% CaO, ~1% MgO, ~1% Al 2 o 3 , and ~2% other impurities, the specific process is as follows:

[0048] 1) Configure 2mol / l oxalic acid and benzene mixed solvent 500ml;

[0049] 2) Add 200ml of nitric acid with a mass fraction of 50% to the mixed solvent to obtain 600ml of composite acidic medium;

[0050] 3) Put the above-mentioned composite acidic medium and 50 grams of pyrite slag together into a 1000ml three-hole flask, put the above-mentioned three-hole flask into a magnetically stirred 100°C oil bath, and place a straight-run condenser on it , start the leaching reaction, keep the reaction for 240 minutes, stop the water bath and filter to obtain an iron-containing organic phase and an aqueous solution phase. After measurement, the iron ion concentration in the organic phase is about 18g / L;

[0051] 4) Take 300ml of the above-mentioned organic...

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Abstract

A method for preparing battery-level ferric phosphate using pyrite cinders uses pyrite cinders as raw materials. The dissolution of iron element in the pyrite cinders is improved by using a composite acidic medium, a soluble organic-acid ferric-salt is extracted and separated synchronously and selectively, and a high-purity ferric phosphate is obtained through replacement in situ under a weak-acid condition, so that the pyrite cinders are transformed into a high-additional ferric phosphate product, thereby realizing the resource utilization of bulk industry solid-wastes in a more economical manner. The ferric phosphate materials prepared by using the method have advantages of a controlled iron-phosphorus ratio, a low impurity content and a high reaction activity, thereby being favorable to insert lithium ion in a subsequent sintering process to form a lithium ferric phosphate crystal suitable for a lithium ion battery positive material.

Description

technical field [0001] The invention belongs to the technical fields of resource utilization of industrial solid waste and energy materials, and in particular relates to a method for preparing battery-grade iron phosphate by using iron-containing solid waste as a raw material through mixed acid leaching-co-precipitation. Background technique [0002] Lithium iron phosphate has high theoretical capacity (170mAh / g), high working voltage (voltage platform around 3.5V), appropriate mass density (3.64g / cm 3 ), small self-discharge, Li in LiFePO4 at low current density + Almost 100% intercalation / deintercalation, long cycle life, good cycle performance, no memory effect, low price, good thermal stability, and environmental friendliness, etc., are expected to replace the high-cost LiCoO 2 Become a new generation of lithium-ion battery cathode material. [0003] At present, the solid-state reaction method is the main method for the synthesis of lithium iron phosphate materials. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37B09B3/00
Inventor 包炜军李会泉吴良恒汪宏林杨鹏
Owner LVLING CHEM GRP CO LTD JIANGSU
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