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Method for preparing ferrous oxalate hydrated salt crystal

A technology of ferrous oxalate and oxalate, applied in the direction of organic chemistry, can solve the problems of large particle size and poor reactivity, and achieve the effect of good reactivity

Inactive Publication Date: 2011-04-06
海宁市盐官工业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The object of the present invention is to overcome the defects in the above-mentioned prior art that the particle size is relatively large, needs to be reprocessed and has poor reactivity when used as a synthetic raw material for the positive electrode active material lithium ferrous phosphate of a lithium ion secondary battery, and provides a When used as a raw material for the synthesis of lithium ferrous phosphate, the positive electrode active material of a lithium-ion secondary battery, a method for preparing ferrous oxalate hydrate crystals with smaller particle size, no need for further processing and better reactivity

Method used

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  • Method for preparing ferrous oxalate hydrated salt crystal
  • Method for preparing ferrous oxalate hydrated salt crystal
  • Method for preparing ferrous oxalate hydrated salt crystal

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preparation example Construction

[0019] The preparation method of the ferrous oxalate hydrate salt crystal provided by the present invention comprises the contact reaction of the oxalate aqueous solution and the ferrous salt solution, wherein, the contact reaction of the oxalate solution and the ferrous salt solution is carried out in an organic solvent and In the presence of a mixed solvent of water, the organic solvent is completely miscible with water.

[0020] According to the preparation method provided by the present invention, the contact reaction of the oxalate aqueous solution and the ferrous salt aqueous solution is to add the oxalate aqueous solution and the ferrous salt aqueous solution into a mixed solvent of an organic solvent and water.

[0021] According to the preparation method provided by the present invention, the pH value at the end of the reaction between the oxalate aqueous solution and the ferrous salt aqueous solution is preferably 1-5, more preferably 2-4. The pH value can be control...

Embodiment 1

[0037] 1.0 liter of ethanol (C 2 h 5 OH) is miscible with 0.2 liter of water to make a mixed solvent (temperature 25°C). Dissolve 556 g (2 moles) of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 0), and add a small amount of sulfuric acid to adjust the pH value of the solution to 1.8. In addition, dissolve 368 grams (2 moles) of potassium oxalate monohydrate (K 2 C 2 o 4 ·H 2 O), and add a small amount of potassium hydroxide (KOH) aqueous solution to adjust the pH of the solution to 8.6. With a dropping speed of 50 ml / min, 2000 ml of potassium oxalate solution was dripped to this ethanol mixed solvent with 40 minutes, and at the same rate, 2000 ml of ferrous sulfate solution was dripped to this mixed solvent with 40 minutes. With the dropping of potassium oxalate solution and ferrous sulfate solution, ferrous oxalate precipitates (temperature 25°C, pH 2.8).

[0038] Next, the ferrous oxalate was recovered by filtration, and the recovered ferrous oxalate was washed with 1...

Embodiment 2

[0042] 335 ml ethanol (C 2 h 5 OH) was miscible with 65 ml of water to make a mixed solvent (temperature 25°C). Dissolve 556 grams (2 moles) of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O), and adding a small amount of sulfuric acid to adjust the pH value of the solution to 2.0. In addition, dissolve 368 grams (2 moles) of potassium oxalate monohydrate (K 2 C 2 o 4 ·H 2 O), and add a small amount of potassium hydroxide (KOH) aqueous solution to adjust the pH of the solution to 8.0. With a dropping speed of 100 ml / min, 2000 ml of potassium oxalate solution was dripped to this ethanol mixed solvent in 20 minutes, and at the same rate, 2500 ml of ferrous sulfate solution was dripped to this mixed solvent in 25 minutes. With the dropping of potassium oxalate solution and ferrous sulfate solution, ferrous oxalate precipitates (temperature 25°C, pH 2.5).

[0043] Next, the ferrous oxalate was recovered by filtration, and the recovered ferrous oxalate was washed with 10 lit...

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Abstract

The invention relates to a preparation method for a hydrous salt crystal of ferrous oxalate. The method comprises a contact reaction between water solution of oxalate and water solution of ferrous salt, which is carried out in the presence of mixed solvent of organic solvent and water; the organic solvent and water are totally soluble. The hydrous salt crystal of ferrous oxalate prepared by the method provided by the invention has small average grain size, as small as 1-5 micron, has good reactivity, and is suitable for being as compound raw material of lithium iron phosphate, an active substrate of anode of lithium-ion secondary batteries.

Description

technical field [0001] The invention relates to a method for preparing ferrous oxalate hydrate crystals, in particular, a method for preparing ferrous oxalate hydrate crystals for synthesizing lithium iron phosphate. Background technique [0002] At present, the cathode material commonly used in lithium batteries is lithium cobalt oxide (LiCoO 2 ), lithium nickel cobalt oxide (LiNi x co 1-x o 2 ), lithium nickel cobalt manganese oxide (LiNi x co y mn 1-x-y o 2 ) and lithium manganate (LiMn 2 o 4 ). LiCoO 2 、LiNi x co 1-x o 2 and LiNi x co y mn 1-x-y o 2 It is an oxide of hexagonal layered salt structure. Lithium ions move in the octahedral layer gap composed of O-Co-O, and has high conductivity and reversibility of lithium ion deintercalation. LiMn 2 o 4 It is an oxide with a three-dimensional structure of spinel. Lithium ions move in the octahedral channel formed by O-Mn-O. It also has high electrical conductivity and reversibility of lithium ion deinter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/06
Inventor 白琳曹文玉肖峰
Owner 海宁市盐官工业投资有限公司
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