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Method for preparing cell-grade lithium iron phosphate from pyrite slag

A technology of pyrite slag and lithium iron phosphate, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve problems such as difficult to effectively control impurities, high energy consumption, and ineffective leaching of iron elements, etc., and achieve reduction Low energy consumption, low water heating temperature and low price

Active Publication Date: 2014-04-23
LINGBAO CITY JINYUAN MINING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing battery-grade lithium iron phosphate by using pyrite slag, which effectively solves the problem of high energy consumption and ineffective iron elements during the preparation of battery-grade iron phosphate materials using pyrite slag as raw material. The problems of ground leaching and impurity are difficult to be effectively controlled

Method used

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  • Method for preparing cell-grade lithium iron phosphate from pyrite slag
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  • Method for preparing cell-grade lithium iron phosphate from pyrite slag

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Embodiment 1

[0029] A method for preparing battery-grade lithium iron phosphate by utilizing pyrite slag, comprising the following steps:

[0030] (1) Import pyrite slag just out of the furnace at about 850°C into the rotary furnace, 2 / N 2 Reduction roasting under a mixed gas reducing atmosphere for 10 hours, H 2 / N 2 The flow rate of the mixed gas is controlled at 8 m 3 / hour, H 2 / N 2 H in the mixture 2 The volume fraction is 5%;

[0031] (2) Add 20% (mass concentration, the same below) sulfuric acid to the pyrite slag, the acid excess coefficient is 1.4 (based on the theoretical stoichiometric ratio of iron / sulfuric acid 1:1, the same below), and the temperature is 60°C , after stirring for 200 minutes, filter to obtain iron-containing leachate;

[0032] (3) Add enough iron nuggets to the leaching solution to consume excess sulfuric acid, and filter at a temperature of 50°C for 120 minutes; add 20% (mass, the same below) concentrated ammonia water to the further obtained leachi...

Embodiment 2

[0037] A method for preparing battery-grade lithium iron phosphate by utilizing pyrite slag, comprising the following steps:

[0038] (1) Import pyrite slag just out of the furnace at about 850°C into the rotary furnace, and add graphite accounting for 20wt% of the mass of pyrite slag as a reducing agent at the same time. 2 (N 2 The flow rate is controlled at 8 m 3 / hour) reduced roasting under the atmosphere for 30 minutes;

[0039] (2) Add 50% sulfuric acid to the pyrite slag, the acid excess coefficient is 1.3, the temperature is 70°C, stir for 100 minutes and then filter to obtain the iron-containing leachate;

[0040] (3) Add enough iron nuggets to the leaching solution to consume excess sulfuric acid, and filter at a temperature of 80°C for 60 minutes; add 25% concentrated ammonia water to the further obtained leaching solution to adjust the pH value to 3, and add ‰ anionic polyacrylamide for flocculation and precipitation (purchased from France Eisen Company), and t...

Embodiment 3

[0045] A method for preparing battery-grade lithium iron phosphate by utilizing pyrite slag, comprising the following steps:

[0046] (1) Import pyrite slag just out of the furnace at about 850°C into the rotary furnace, and add glucose accounting for 10% of the mass of pyrite slag as a reducing agent at the same time. 2 (N 2 The flow rate is controlled at 8 m 3 / hour) reduced roasting under the atmosphere for 60 minutes;

[0047] (2) Add 80% sulfuric acid to the pyrite slag, the acid excess coefficient is 1.2, the temperature is 80°C, and after stirring for 10 minutes, filter to obtain the iron-containing leachate;

[0048] (3) Add enough iron nuggets to the leaching solution to consume excess sulfuric acid at a temperature of 90°C, react for 30 minutes and then filter; in the further obtained leaching solution, add concentrated ammonia water with a concentration of 28% to adjust the pH value to 4, and add 20‰ of anionic polyacrylamide for flocculation and precipitation (...

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Abstract

The invention belongs to the technical fields of comprehensive utilization of industrial solid wastes and energy materials, and especially relates to a method for preparing cell-grade lithium iron phosphate from pyrite slag. The pyrite slag is orderly subjected to the following steps: reduction calcination, acid soaking in sulfuric acid, impurity removing, and hydrothermal synthesis so as to obtain the lithium iron phosphate. The method converts pyrite slag into a lithium cell positive pole material lithium iron phosphate with a high additional value, and economically achieves comprehensive utilization of staple industrial solid wastes. The method has the advantages of simpleness, practicability, safety, reliability, low production cost, high yield, and little environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of industrial solid waste resources and energy materials, and in particular relates to a method for preparing battery-grade lithium iron phosphate by utilizing pyrite slag. Background technique [0002] Lithium-ion battery is a new generation of green high-energy battery and a high-tech product of great significance in the 21st century. It has excellent advantages such as high voltage, small self-discharge, high energy density, good cycle performance, no memory effect, and wide operating temperature range. It is widely used in mobile phone batteries, digital cameras, notebook computers and other electronic products, especially in electric vehicles and The application of energy storage has a good application prospect. The cathode material of lithium-ion batteries is an important part of lithium-ion batteries, and it is also an important direction for the current development of li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCC01B25/45H01M4/5825Y02E60/10
Inventor 张五星杨青时刘树林杜建廷
Owner LINGBAO CITY JINYUAN MINING
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