Wafer-like ferric phosphate, preparation method and application thereof

A technology of iron phosphate and iron phosphate powder, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of irregular particle shape, uneven size, high impurities, etc., achieve short reaction time and easy process , the effect of high product purity

Active Publication Date: 2010-05-19
GUANGXI RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The proportion of iron phosphate produced by these traditional methods is difficult to control, the impurities are high, the particle shape is irregular, and the size is not uniform
Lithium iron phosphate synthesized from iron phosphate prepared by these traditional methods has two disadvantages. One is low electrical conductivity, resulting in poor high-rate charge and discharge performance; the other is low tap density, resulting in low volume specific capacity.

Method used

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  • Wafer-like ferric phosphate, preparation method and application thereof
  • Wafer-like ferric phosphate, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 1 liter of deionized water adjusted to pH=1 with nitric acid in advance into the stirred reactor, then add 40.4g (0.1mol) Fe(NO 3 ) 3 9H 2 O, to be Fe(NO 3 ) 3 9H 2 After O is dissolved, add 14.2g (0.1mol) Na 2 HPO 4 , 9g (0.15mol) urea, 3g nonylphenol polyoxyethylene (10) ether, and adjust the pH of the solution to 1-1.5 with nitric acid. Heat the reactor solution to 80°C and react at this temperature for 3 hours to obtain a white suspension, cool, filter, wash the filter cake with deionized water three times, and dry the filter cake in an oven at 100-120°C for 6 hours , and iron phosphate powder can be obtained. The product has good whiteness, disc shape, average particle size 0.3-0.5 microns, tap density ≥ 0.95g / cm 3 .

[0017] The FePO prepared in this embodiment 4 with LiOH·H 2 O, sucrose is mixed with the ratio of 1: 1: 1.15 (ratio of the amount of substance), ball milled 4h, puts into the program temperature control tube furnace in high-purity N 2...

Embodiment 2

[0021] Add 1 liter of deionized water adjusted to pH=1 with nitric acid in advance into the reactor with stirring, then add 202g (0.5mol) Fe(NO 3 )3 9H 2 O, to be Fe(NO 3 ) 3 9H 2 After O is dissolved, add 87g (0.5mol) K 2 HPO 4 , 36g (0.6mol) urea, 3g octylphenol polyoxyethylene (10) ether, adjust the pH=1 of the solution with nitric acid. Heat the reactor solution to 80°C and react at this temperature for 3 hours to obtain a white suspension, cool, filter, wash the filter cake with deionized water three times, and dry the filter cake in an oven at 100-120°C for 5 hours , and iron phosphate powder can be obtained. The product has good whiteness, disc shape, average particle size 0.3-0.5 micron, tap density ≥ 0.95g / cm 3 . The lithium iron phosphate synthesized from this iron phosphate has a discharge capacity of 142mAh / g at 0.5C.

Embodiment 3

[0023] Add 1 liter of deionized water adjusted to pH=1 with nitric acid in advance into the reactor with stirring, then add 404g (1.0mol) Fe(NO 3 ) 3 9H 2 O, to be Fe(NO 3 ) 3 9H 2 After O is dissolved, add 66g (0.5mol) (NH 4 ) 2 HPO 4 , 71g (0.5mol) Na 2 HPO 4 , 72g (1.2mol) urea, 5g cetyltrimethylammonium bromide, adjust the pH of the solution to 1-1.5 with nitric acid, heat the reactor solution to 90°C and react at this temperature for 2 hours to obtain a white suspension The turbid liquid is cooled, filtered, the filter cake is washed three times with deionized water, and the filter cake is baked in an oven at 100-120° C. for 4 hours to obtain iron phosphate powder. The product has good whiteness, disc shape, average particle size 0.3-0.5 microns, tap density ≥ 0.95g / cm 3 . The lithium iron phosphate synthesized from this iron phosphate has a discharge capacity of 142mA·h / g at 0.5C.

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Abstract

The invention discloses a method for preparing wafer-like ferric phosphate, which comprises the following steps of: adding deionized water of which the pH value is pre-adjusted to 1 by nitric acid into a reactor with stirring, then adding an iron source into the reactor, completely dissolving the iron source with the stirring, then adding a certain amount of phosphoric acid or phosphate, urea and surfactant into the reactor respectively, adjusting the pH value of reaction solution by using the nitric acid or sodium hydroxide, heating the solution in the reactor to be between 80 and 100 DEG C, performing reaction for 1.5 to 3 hours within the temperature range to obtain a white suspension, cooling and filtering the suspension, washing a filter cake by using the deionized water, and drying the filter cake for 3 to 6 hours in a baking oven at the temperature of between 102 and 120 DEG C to obtain ferric phosphate powder. The product has good whiteness, is of wafer shapes and has more uniform particle sizes; the average particle size is between 0.3 and 0.5 microns; and the tap density is more than or equal to 0.95g / cm3. The discharge capacity of lithium ferric phosphate, which is further synthesized by using the ferric phosphate prepared by the method as a raw material and is taken as an anode material of a lithium ion battery, can reach more than 140mAh / g under the condition of 0.5C. The method has the advantages of short reaction time, simple process, high product purity, and more regular morphology, and is easy to realize industrialization.

Description

Technical field: [0001] The invention relates to an inorganic salt and a preparation method thereof, in particular to a preparation method of disc-shaped iron phosphate powder, which can be used to prepare lithium iron phosphate, a cathode material of a lithium ion battery. Background technique: [0002] Ferric phosphate is a widely used chemical raw material. It can be used as a food thickener and iron supplement, and can also be used in pigments, catalysts for organic synthesis, and glazes for ceramic and metal glazes. In recent years, iron phosphate has been used as a high-quality raw material for the production of lithium iron phosphate, a cathode material for lithium-ion batteries, and has important application value. In Chinese patent (publication number CN1255888, a preparation method of lithium iron phosphate, a positive electrode material for lithium ion batteries), Chinese patent (publication number CN100389062, a method of preparing carbon-coated lithium iron phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37H01M4/58H01M4/1397
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 阮恒龚福忠易君辉
Owner GUANGXI RES INST OF CHEM IND CO LTD
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