Preparation method of anhydrous ferric phosphate in organic system

An anhydrous phosphoric acid, organic system technology, applied in organic chemistry, preparation with chloride, chemical instruments and methods, etc., can solve the problems of long process, long process, large processing capacity, etc., achieve uniform particle size distribution, simple process, Good dispersion effect

An anhydrous phosphoric acid, organic system technology, applied in organic chemistry, preparation with chloride, chemical instruments and methods, etc., can solve the problems of long process, long process, large processing capacity, etc., achieve uniform particle size distribution, simple process, Good dispersion effect

CN110451472AActive Publication Date: 2019-11-15SICHUAN LOMON PHOSPHORUS CHEM
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  • Preparation method of anhydrous ferric phosphate in organic system
  • Preparation method of anhydrous ferric phosphate in organic system
  • Preparation method of anhydrous ferric phosphate in organic system

Examples

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Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of anhydrous iron phosphate in an organic system, which comprises the following steps:

[0044](1) Dry ferric chloride until the water content is lower than 0.05%, then dissolve it in absolute ethanol, stir until completely dissolved to obtain ferric chloride-ethanol solution, transfer it to a sealed reaction kettle, and Add ethanolamine phosphate into the sealed reaction kettle, maintain the reaction temperature during feeding at 35°C, and the feeding time is 80 minutes. After the feeding is completed, continue to react at a temperature of 50°C for 20 minutes to obtain the reaction material;

[0045] (2) After the reaction material is filtered, the filter residue and filtrate are obtained. The filter residue is washed with absolute ethanol to obtain the washing residue and the washing liquid. After the washing residue is vacuum-dried, it is crushed, sieved and iron-removed to obtain battery-grade Anhydrous iron phosphate;

[0046] (3) Filtrate and...

Embodiment 2

[0056] A preparation method of anhydrous iron phosphate in an organic system, which comprises the following steps:

[0057] (1) Dry ferric chloride until the water content is lower than 0.05%, then dissolve it in absolute ethanol, stir until completely dissolved to obtain ferric chloride-ethanol solution, transfer it to a sealed reaction kettle, and Add ethanolamine phosphate into the sealed reaction kettle, keep the reaction temperature at 40°C during the feeding, and the feeding time is 70 minutes. After the feeding is completed, continue to react at the temperature of 55°C for 20 minutes to obtain the reaction material;

[0058] (2) After the reaction material is filtered, the filter residue and filtrate are obtained. The filter residue is washed with absolute ethanol to obtain the washing residue and the washing liquid. After the washing residue is vacuum-dried, it is crushed, sieved and iron-removed to obtain battery-grade Anhydrous iron phosphate;

[0059] (3) Filtrate ...

Embodiment 3

[0068] A preparation method of anhydrous iron phosphate in an organic system, which comprises the following steps:

[0069] (1) Dry ferric chloride until the water content is lower than 0.05%, then dissolve it in absolute ethanol, stir until completely dissolved to obtain ferric chloride-ethanol solution, transfer it to a sealed reaction kettle, and Add ethanolamine phosphate into the sealed reaction kettle, maintain the reaction temperature during feeding at 35°C, and the feeding time is 60 minutes. After the feeding is completed, continue to react at a temperature of 55°C for 30 minutes to obtain the reaction material;

[0070] (2) After the reaction material is filtered, the filter residue and filtrate are obtained. The filter residue is washed with absolute ethanol to obtain the washing residue and the washing liquid. After the washing residue is vacuum-dried, it is crushed, sieved and iron-removed to obtain battery-grade Anhydrous iron phosphate;

[0071] (3) Filtrate an...

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Abstract

The invention discloses a preparation method of anhydrous ferric phosphate in an organic system. The method comprises the steps that ferric chloride is dried till the water content is lower than 0.05%, then dissolved into absolute ethyl alcohol, stirred to be completely dissolved to obtain a ferric chloride-ethyl alcohol solution and transferred into a sealed reaction kettle, under the stirring condition, dihydrogen phosphate ester is added into the sealed reaction kettle, the reaction temperature during feeding is maintained to be 35-40 DEG C, the heating time is 60-90 min, and after feedingis completed, the reaction continues to be performed to obtain a reaction material; after the reaction material is filtered, filter residues and a filtrate are obtained, the filter residues are addedinto absolute ethyl alcohol to be washed, washing residues and a washing solution are obtained through washing, the washing residues are subjected to vacuum drying, and smashing, screening and iron removing are performed to obtain battery grade anhydrous ferric phosphate. The technology is simple, the flow path is short, the one-step method synthesis technology of anhydrous ferric phosphate in theorganic system is realized, the cost is low, no wastewater is generated, the obtained anhydrous ferric phosphate is good in dispersibility, and grain fineness distribution is more uniform.

Description

technical field [0001] The invention relates to a method for preparing anhydrous iron phosphate in an organic system, and belongs to the technical field of new energy lithium battery materials. Background technique [0002] With the depletion of oil resources, the development of electric vehicles is imperative. At present, the most critical technology for electric vehicles is to develop cheap, safe and environment-friendly secondary batteries. Due to the characteristics of high voltage, high specific energy and high power, lithium-ion batteries are recognized as the best candidates for electric vehicle power batteries. For lithium-ion batteries, the cathode material is a key factor that determines its electrochemical performance, safety performance, energy density, and price. In 1997, Goodenough et al first reported the olivine structure LiFePO 4 reversible lithium intercalation-delithiation properties. Due to its good safety performance, long cycle life, wide source of ...

Claims

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Application Information

Patent Timeline
15 Nov 2019
Publication
CN110451472A
IPC
C01B25/37; C01B7/03; C07C209/68; C07C211/15
CPC
C01B7/035; C01B25/375; C01P2004/32; C01P2004/61; C01P2006/11; C01P2006/12; C01P2006/80; C01P2006/82
Inventors
李旭意