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Method for preparing iron oxalate

A technology of ferrous oxalate and ferrous sulfate, applied in carboxylate preparation, organic chemistry, etc., can solve problems such as low purity, difficulty in ensuring uniformity, low conductivity, etc., achieve simple and controllable process routes, improve electrical Effect of high chemical performance and electrical conductivity

Inactive Publication Date: 2012-06-20
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing ferrous oxalate cannot meet the requirements for preparing high-quality ferric phosphate, because it has low purity, uneven particle size distribution, and especially unstable and not single crystal forms, which are orthorhombic, monoclinic and triclinic The mixed crystal form of the crystal system, in the production process of lithium ferrous phosphate, the physical appearance of the raw material has a great influence on the finished product, so the ferrous phosphate material prepared by the existing ferrous oxalate has poor appearance, The tap density of the prepared lithium iron phosphate powder is low, and the current commercially available materials are lower than 1.2g / cm 3 , which is only one-third of its true density, resulting in a battery with low energy density
In addition, lithium iron phosphate also has a disadvantage in that its low electronic conductivity (about 10 -8 S / cm), at present, the impact of low conductivity is alleviated mainly by adding conductive agents (such as carbon black, copper powder, high-temperature pyrolytic coated carbon) for metal ion doping, and synthesizing nano-particles.
However, the method of doping metal ions is mainly to mix some oxides in the mixing stage. Since there are many reacting materials, it is difficult to ensure the uniformity in the mixing process.

Method used

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  • Method for preparing iron oxalate
  • Method for preparing iron oxalate
  • Method for preparing iron oxalate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Example 2. Take 27.9g of industrial grade ferrous sulfate, dissolve it in 200ml of dilute sulfuric acid with a concentration of 50%, slowly add 10g of iron filings to the solution, stir, control the reaction temperature at 50°C, and add to the ferrous sulfate solution after suction filtration 1g of nickel sulfate (chemically pure), stirred and dissolved to obtain ferrous sulfate solution containing nickel sulfate composition. Dissolve 5.55g of oxalic acid and 6.26g of ammonium oxalate in 20ml of distilled water, stir and heat to 60°C, after the oxalic acid and ammonium oxalate are completely dissolved, suction filter to obtain a mixed solution of oxalic acid and ammonium oxalate. Then add the ferrous sulfate solution containing nickel sulfate to the oxalic acid and ammonium oxalate solution at a rate of 0.2 L / min, the reaction temperature is 60 degrees, keep stirring for 60 minutes, and then stand still for 10 to 30 minutes. The mother liquor is separated, washed twice...

Embodiment 2

[0018] Example 3. Take 41.9g of industrial-grade ferrous sulfate, dissolve it in 300ml of dilute sulfuric acid with a concentration of 50%, slowly add 15g of iron filings to the solution, stir, control the reaction temperature at 50°C, and add to the ferrous sulfate solution after suction filtration The cupric sulfate of 0.5g and 0.5g magnesium sulfate (chemically pure), make it dissolve with stirring and make the ferrous sulfate solution that contains copper sulfate and magnesium sulfate. Dissolve 11.1g of oxalic acid in 20ml of distilled water, stir and heat to 65°C, after the oxalic acid is completely dissolved, suction filter to obtain the oxalic acid solution. Then add the ferrous sulfate solution containing copper sulfate and magnesium sulfate into the oxalic acid solution at a rate of 0.2 L / min, the reaction temperature is 50°C, keep stirring for 60 minutes, and then stand still for 10 to 30 minutes. The mother liquor is separated, washed twice with deionized water and...

Embodiment 3

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Abstract

The present invention discloses a method for preparing ferrous oxalate, which belongs to the technical field of powdered material preparation. The aim of the invention is to provide a preparation method of ferrous oxalate which is high in purity, controllable in granularity, even in grain size, and high in conductivity. The method comprises the following steps of locating ferrous sulfate into dilute sulphuric acid, adding scrap iron with stirring, and obtaining a ferrous sulfate solution after suction filtration; dissolving oxalic acid or / and ammonium oxalate in distilled water with stirring and heating, and obtaining a mixed solution of oxalic acid or / and ammonium oxalate through suction filtration after dissolution; and, slowly adding the ferrous sulfate solution into oxalic acid solution, keeping the temperature, stirring, separating ferrous sulfate from the original synthetic solution after keeping stand, and obtaining ferrous oxalate powder through washing and drying. The ferrousoxalate prepared by the preparation method is a powder with a medium grain diameter of between 0.5 and 80 mu m. The granularity is completely controllable. The product purity is greater than 99.0 percent. The conductivity is high. The electrochemical performance of the ferrous phosphate salt composite material is largely improved. The conductivity of lithium iron phosphate is improved by 5 ordersof magnitude.

Description

technical field [0001] The invention relates to a preparation method of ferrous oxalate, belonging to the technical field of powder material preparation. Background technique [0002] As a chemical raw material, ferrous oxalate is widely used in the production of ceramics, glass, and photosensitive materials. In addition, it is especially used to prepare the iron source of lithium iron phosphate, the preferred positive electrode material for power batteries. As a green high-energy battery, lithium-ion batteries have many advantages such as high voltage, high energy density, good cycle performance, small self-discharge, no memory effect and wide working range. They are widely used in mobile phones, notebook computers, digital cameras and other emerging industries. IT products. In addition, in terms of electric vehicles, electric tools, automotive 42V batteries, and large photovoltaic energy storage batteries, traditional lead-acid batteries have also begun to be gradually re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 蒋华锋徐小明
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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