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Synthesis method of novel ion battery positive pole material iron phosphate

A technology for ion batteries and positive electrode materials, applied in battery electrodes, phosphorus compounds, chemical instruments and methods, etc., can solve the problems of easy attenuation, high raw material prices, and no research on the conductivity of compounds, etc., to achieve easy production, easy preparation, wide range Effect of lithium ion intercalation/extraction range

Inactive Publication Date: 2015-10-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, other materials contain precious elements, and the price of raw materials is higher
These materials are prone to decay during charge and discharge cycles, especially at high temperatures
[0003] Compound (NH 4 )[Fe 2 (OH)(H 2 O)(PO 4 ) 2 ]·1.5H 2 The synthesis, structure and magnetic properties of O have been reported in the literature. For example, Zhou Hong et al. used hydrothermal reaction to synthesize the compound with a three-dimensional porous structure in Solid State Sciences12 (2010) 1816-1821, and discussed it in detail. Its crystal structure and magnetic properties, but did not study the conductivity of the compound, and the intercalation / extraction properties of alkali metal ions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] At room temperature, successively: 0.1476g (NH 4 ) 2 HPO 4 , 0.1506g H 3 BO 3 , 0.1500g C 2 h 4 o 4 2H 2 O, 0.2515g FeSO 4 ·7H 2 O and 0.7275 g NH 3 ·H 2 O was added to 2.9 mL of secondary deionized water, and after mixing, stirred with a magnetic stirrer at 300 rpm for 15 minutes; after mixing evenly, the mixed solution was added to a 50 ml stainless steel reaction kettle and the lid of the reaction kettle was tightened; the above reaction Put the kettle into a constant temperature blast drying oven, heat it at 150°C for 75 hours, and then cool it down to room temperature naturally (the cooling time should exceed 12 hours); finally, wash the reaction product with deionized water several times to obtain blocky green crystals , dried naturally at room temperature, and the yield was about 45%.

Embodiment 2

[0021] At room temperature, sequentially add 0.1476g (NH 4 ) 2 HPO 4 , 0.0960 g H 3 BO 3 , 0.1500g C 2 h 4 o 4 2H 2 O, 0.1635g FeSO 4 ·7H 2 O and 0.7275 g NH 3 ·H 2 O was added to 2.7 mL of secondary deionized water, and after mixing, stirred with a magnetic stirrer at 500 rpm for 10 minutes; after mixing evenly, the mixed solution was added to a 25 ml stainless steel reaction kettle and the lid of the reaction kettle was tightened; the above reaction The kettle was placed in a constant temperature blast drying oven, heated at 180°C for 72 hours, and then naturally cooled to room temperature (cooling time should exceed 12 hours); finally, the reaction product was washed several times with deionized water to obtain blocky green crystals , dried naturally at room temperature, and the yield was about 50%.

Embodiment 3

[0023] At room temperature, sequentially add 0.1476g (NH 4 ) 2 HPO 4 , 0.0680g H 3 BO 3 , 0.1500g C 2 h 4 o 4 2H 2 O, 0.3005g FeSO 4 ·7H 2 O and 0.7275 g NH 3 ·H 2 O was added to 2.5 mL of secondary deionized water, and after mixing, stirred with a magnetic stirrer at 800 rpm for 5 minutes; after mixing evenly, the mixed solution was added to a 25 ml stainless steel reaction kettle and the lid of the reaction kettle was tightened; the above reaction kettle Put it into a constant temperature blast drying oven, heat it at 210°C for 70 hours, then cool it down to room temperature naturally (the cooling time should exceed 12 hours); finally, wash the product with deionized water several times to obtain blocky green crystals. Dry naturally at room temperature, and the yield is about 50%.

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Abstract

The invention relates to a synthesis method of a novel ion battery positive pole material iron phosphate, belonging to the field of chemical synthesis. The synthesis method comprises the following experimental steps: sequentially adding (NH4)2HPO4, H3BO3, C2H4O4.2H2O, FeSO4.7H2O and NH3.H2O into secondary deionized water at room temperature, and mixing; after the mixed solution is uniformly mixed, putting the mixed solution into a reaction kettle, heating to react at 150-210 DEG C, and naturally cooling to room temperature; and washing with deionized water to obtain a massive green crystal, and naturally airing at room temperature, wherein the yield is about 50%. The method performs reaction under hydrothermal conditions, thereby lowering the cost and implementing green production. The raw material charging sequence and stoichiometric proportion, reaction temperature, reaction time and cooling time are regulated and controlled to greatly enhance the yield.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing iron phosphate, a novel ion battery cathode material. Background technique [0002] Inorganic porous materials are widely used in the fields of catalysis, ion exchange and selective adsorption due to their unique pore structure. At present, global resources are increasingly unable to meet the needs of human production activities, and the development of new functional materials has become the primary task of scientific researchers today. At present, the electrode materials of ion batteries mainly include layered LiCoO 2 , spinel-type LiMn 2 o 4 , multi-element metal composite oxide LiNi 1 / 3 co 1 / 3 mn 1 / 3 o 2 . As positive electrode materials for small batteries, the above-mentioned compounds have been commercialized to varying degrees. But for electric vehicles or large batteries with high load levels, the price and effective utiliza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37H01M4/58
CPCY02E60/10
Inventor 任小明刘少贤
Owner NANJING UNIV OF TECH
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