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Method of synthesizing iron lithium phosphate by vacuum carbon heating reduction

A technology of lithium iron phosphate and reduction method, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of ammonia gas generation, unfavorable environmental protection, etc., achieve low synthesis temperature, excellent electrochemical performance and physical performance , the effect of low reaction temperature

Active Publication Date: 2007-04-18
HUNAN RESHINE NEW MATERIAL
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a vacuum carbothermal reduction method for synthesizing lithium iron phosphate, a positive electrode material for lithium ion batteries, in view of the above-mentioned problems in the prior art, so as to avoid the generation of ammonia gas by the traditional process, which is not conducive to environmental protection and The problem of too long reaction time, the method of the present invention has short reaction time, low reaction temperature, saves inert gas, reduces cost, and the prepared lithium iron phosphate has good physical properties, especially high tap density, excellent electrochemical performance, and simple process Easy to operate, suitable for industrial production

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  • Method of synthesizing iron lithium phosphate by vacuum carbon heating reduction
  • Method of synthesizing iron lithium phosphate by vacuum carbon heating reduction
  • Method of synthesizing iron lithium phosphate by vacuum carbon heating reduction

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preparation example Construction

[0026] 1) Preparation of lithium dihydrogen phosphate containing doping elements.

[0027] Lithium hydroxide monohydrate or lithium carbonate or lithium acetate and a compound of doping elements are placed in a ball mill, and then an appropriate amount of water is added for ball milling to make a lithium salt slurry with a solid-to-liquid ratio of 1:1-1:5 (mass Ratio), and then control the flow rate to put the slurry and the phosphoric acid solution with a concentration of 0.1-5.0mol / L into a self-made reaction tank, stir while reacting, and the overflowed solution is concentrated and crystallized to obtain the mixed Heterolithic lithium dihydrogen phosphate. Wherein the molar ratio of raw materials used is: the molar ratio of monohydrate lithium hydroxide or lithium acetate or lithium carbonate and phosphoric acid and the compound of doping element is 0.95-1.05 (monohydrate lithium hydroxide or lithium acetate) or 0.475-0.525 (carbonic acid Lithium): 1.0: 0.1-0.01.

[0028]...

Embodiment 1

[0030] Example 1: Will contain LiOH·H 2 O 4.11 g (or Li 2 CO 3 3.69 g or lithium acetate 6.59 g) and Mg(OH) 2 0.0583 grams (or magnesium acetate 0.142 grams or magnesium carbonate 0.084 grams or MgC 2 o 4 2H 2 (0.148 grams) of 10 grams of slurry injection containing 32.67 grams of phosphoric acid solution (containing 9.8 grams of phosphoric acid, concentration 30%) in the reaction tank, concentrated crystallization after the reaction 1-10h made containing Mg 2+ Lithium dihydrogen phosphate crystals.

Embodiment 2

[0031] Example 2: will contain LiOH·H 2 O 4.11 g (or Li2 CO 3 3.69 g or lithium acetate 6.59 g) and Al(OH) 3 0.0781 grams of 10 grams of slurry are injected into a reaction tank containing 32.67 grams of phosphoric acid solution (containing 9.8 grams of phosphoric acid, concentration 30%), concentrated and crystallized after 1-10 hours of reaction to obtain Al 3+ Lithium dihydrogen phosphate crystals.

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Abstract

The present invention relates to a method for synthesizing lithium ion battery positive electrode material lithium iron phosphate by utilizing vacuum carbonthermic reduction process. Said method includes the following steps; uniformly mixing self-made lithium dihydrogen orthophosphate containing doped element, tri-iron tetroxide or ferric oxide and electric conducting agent or precursor of said electric conducting agent, placing the mixture into a vacuum smelting furnace, vacuum-pumping, heating to make reaction for a period of time, finally cooling to room temperature so as to obtain the invented lithium ion battery positive electrode material lithium iron phosphate.

Description

technical field [0001] The invention relates to a battery material, in particular to a method for synthesizing lithium iron phosphate by a vacuum carbothermal reduction method. Background technique [0002] LiFePO with olivine structure 4 It has wide sources of raw materials, low price, and excellent high-temperature performance as a lithium-ion battery positive electrode material, so it is considered to be a relatively ideal lithium-ion secondary power battery positive electrode material. However, lithium iron phosphate also has disadvantages such as poor conductivity and low tap density, so improving its conductivity and tap density is a problem that must be solved for the industrialization of lithium iron phosphate. [0003] Currently synthesized LiFePO 4 The methods mainly include high-temperature solid-phase method, hydrothermal method, sol-gel method, liquid-phase redox method, and solid-phase microwave method. [0004] At present, the high-temperature solid-phase m...

Claims

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Application Information

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IPC IPC(8): C01B25/45
Inventor 胡国荣
Owner HUNAN RESHINE NEW MATERIAL
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