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Method for preparing battery-level ferrous oxalate

A ferrous oxalate, battery-grade technology is applied in the field of energy storage materials to achieve the effects of eliminating pollution, high purity and reducing raw material costs

Active Publication Date: 2013-04-10
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the performance of ferrous oxalate in the current technology in terms of purity and particle size needs to be further improved

Method used

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  • Method for preparing battery-level ferrous oxalate
  • Method for preparing battery-level ferrous oxalate
  • Method for preparing battery-level ferrous oxalate

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Dissolve 2 kg of titanium dioxide by-product ferrous sulfate in 4 liters of deionized water, add 20 grams of reduced iron powder at a stirring rate of 600 rpm, heat at 50°C for 3 hours, and then filter to obtain the purified ferrous sulfate transparent filtrate , adjust this solution pH=3, heating system and keeping temperature are 30 ℃, adding concentration is 1200 grams of the polyethylene glycol 20000 solution of 1.5wt% in the ferrous sulfate filtrate, stir rapidly after 10 minutes under the stirring rate of 600rpm 1100 g of oxalic acid solution with a concentration of 50 wt % was added, and after the addition was completed, it was incubated at 30° C. for 30 minutes to form a pale yellow ferrous oxalate crystal precipitate. The precipitated product is filtered, washed and dried to obtain battery grade ferrous oxalate. The battery-grade ferrous oxalate has a purity of 99.5% and an average particle size of 4.2 micrometers as tested by an X-ray fluorescence spectrometer...

Embodiment 2

[0026] Dissolve 1 kg of titanium dioxide by-product ferrous sulfate in 3 liters of deionized water, add 10 grams of reduced iron powder at a stirring rate of 500 rpm, heat at 50°C for 3 hours, and then filter to obtain the purified ferrous sulfate transparent filtrate , adjust the pH of this solution=1, heat the system and keep the temperature at 60°C, add 200 grams of polyethylene glycol 10000 solution with a concentration of 3wt% in the ferrous sulfate filtrate, stir at a stirring rate of 500rpm for 10 minutes and then add Concentration is 970 grams of 50% ammonium oxalate solution, heat preservation for 2 hours after feeding is completed, light yellow ferrous oxalate crystals are generated, then the product is filtered and washed, dried to obtain battery grade ferrous oxalate, and tested by X-ray fluorescence spectrometer and laser particle size analyzer The battery-grade ferrous oxalate has a purity of 99.6% and an average particle size of 4.8 microns.

Embodiment 3

[0028]Dissolve 2 kg of titanium dioxide by-product ferrous sulfate in 4 liters of deionized water, add 20 grams of reduced iron powder at a stirring rate of 800 rpm, heat at 50°C for 3 hours, and then filter to obtain the purified ferrous sulfate transparent filtrate , adjust this solution pH=2, keep system temperature be 10 ℃, add the polyacrylamide 10000000 solution 1000 grams that concentration is 0.5wt% in ferrous sulfate filtrate, add concentration rapidly after stirring 10 minutes under the stirring rate of 800rpm 1500 grams of 50% sodium oxalate solution. After the addition, the system was kept at 10°C for 2.5 hours to form light yellow ferrous oxalate crystals. Then the product was filtered, washed, and dried to obtain battery-grade ferrous oxalate. X-ray fluorescence The battery-grade ferrous oxalate has a purity of 99.5% and an average particle size of 3.4 microns as measured by a spectrometer and a laser particle size analyzer.

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Abstract

The invention provides a method for preparing battery-level ferrous oxalate, which is characterized in that high molecular weight water soluble polymer is added to a precursor for preparing the ferrous oxalate to form a complex compound structure or other structures with the precursor in order to prepare the battery-level ferrous oxalate by reacting with a precipitator. The preparation method of the precursor ferrisulphas comprises the following steps: ferrisulphas, the by-product of titanium dioxide is dissolved; then reduced iron powder is added to the dissolved ferrisulphas; and finally, the mixture is filtrated. In the invention, the high molecular weight water soluble polymer is introduced in the reaction process to suppress grain diameter of the ferrous oxalate; as a result, superfine ferrous oxalate with a uniform grain diameter is obtained. In addition, the method of the invention has the characteristics of sufficient raw materials, simple technical process, good and stable product quality, low cost and the like, and provides a new means of recycling the waste of the ferrisulphas.

Description

technical field [0001] The invention relates to the technical field of energy storage materials, in particular to a method for assisting the preparation of battery-grade ferrous oxalate by utilizing high-molecular-weight water-soluble polymers. Background technique [0002] With the increasing shortage of chemical fuel resources worldwide, people are forced to look for new alternative clean energy sources. Lithium-ion batteries have the characteristics of high energy density, large output power, high average output voltage, small self-discharge, no memory effect, fast charge and discharge, excellent cycle performance and no environmental pollution. Preferred object, considered to be the most promising chemical power source. In lithium-ion batteries, the positive electrode material occupies the most important position, and the performance of the positive electrode material directly determines the various performance indicators of the final lithium battery product. Tradition...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 刘兆平姚霞银袁国霞周旭峰张建刚唐长林
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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