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Method for preparing multielement-doped lithium iron phosphate by using waste phosphate slag as main raw material

A technology of phosphating waste slag and lithium iron phosphate, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve problems such as methods for comprehensive utilization of phosphating waste slag that have not been found, and achieve the effect of reducing production costs

Inactive Publication Date: 2014-05-14
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Through consulting a large amount of information and literature, no better solution to the comprehensive utilization of phosphating waste residues has been found

Method used

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  • Method for preparing multielement-doped lithium iron phosphate by using waste phosphate slag as main raw material

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Embodiment 1

[0024] Embodiment 1: take by weighing the phosphating waste residue of 250g water content 90% color partial green, drop 1ml H 2 o 2 , 1ml of 0.01mol / L dilute phosphoric acid, briefly stir until the color is uniform white or yellowish white. Add 50ml of 0.005mol / L dilute hydrochloric acid, adjust the pH value to 3~4 with ammonia water, heat and stir in a water bath at 60°C for 15min, take 5ml of filtrate after filtration, add excess NaOH solution dropwise, if there is no obvious red precipitate, repeat the above acid wash steps. The resulting filter residue was dried in an oven at 180°C for 2 hours. Its composition was measured by XRF, and the relative molar percentages of Fe, P and each doping element were: 48.57%, 50.12%, and 1.31%, respectively. Do thermogravimetric analysis, after drying at 180°C, every 10g of filter residue contains 0.62g of crystal water. Weigh 10g of filter residue and add 2.61g of LiOH.H 2 O, 1.5g polypropylene powder, ball milling (380rpm, 6h). A...

Embodiment 2

[0025] Example 2: Weigh 250g of white or yellow-white phosphating waste residue with a moisture content of 90%, add 50ml of 0.001mol / L dilute phosphoric acid, adjust the pH value to 3~4 with ammonia water, heat and stir in a water bath at 80°C for 10min, and filter Finally, take 5ml of filtrate and add excess NaOH solution dropwise. If there is no obvious red precipitate, repeat the above pickling step. The resulting filter residue was dried in an oven at 100°C for 4 hours. Its composition was measured by XRF, and the relative molar percentages of Fe, P and each doping element were: 47.53%, 50.35%, and 2.12%, respectively. According to thermogravimetric analysis, every 10g of filter residue contains 1.21g of crystal water after drying at 100°C. Weigh 10g of filter residue and add 2.44g of LiOH.H 2 O, 1.5g polypropylene powder, ball milling (450rpm, 4h). After ball milling, the sample was placed in an enamel crucible at 700 °C, N 2 Roasting under protection for 6 hours, and...

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Abstract

The invention discloses a method for preparing multielement-doped lithium iron phosphate by using waste phosphate slag as a main raw material, belonging to the technical field of preparation of an anode material of a lithium battery. According to the method, a mixture which mainly contains iron phosphate and also contains a defined amount of phosphates of Zn, Ca, Cr, Mn, Al, Ni, Mg, Ti and the like is prepared from waste phosphate slag through oxidation and an acid-washing method. The mixture is used as a main raw material, and Li is added into the mixture according to a chemical ratio, and the mixture with Li is sintered under the protection of inert gas such as N2 or Ar to synthesize multielement-doped lithium iron phosphate. Fe, P and all doped elements used in the method for preparing the multielement-doped lithium iron phosphate are from the phosphate slag, so that the difficult technical problem in the traditional process that raw materials used for preparing the multi-doped lithium iron phosphate only depend on a great amount of various battery-grade raw materials is solved. The method is a new method for harmless and high-additional-value utilization of the dangerous solid waste phosphate slag while the preparation cost of the lithium iron phosphate is obviously reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of cathode materials for lithium ion batteries, and in particular relates to a method for preparing multi-component doped lithium iron phosphate by using phosphating waste residue as a main raw material. Background technique [0002] LiFePO with olivine-type structure 4 It can reversibly intercalate and deintercalate lithium ions. Considering its non-toxicity, environmental friendliness, rich source of raw materials, high specific capacity, and good cycle performance, it is considered to be an ideal cathode material for lithium-ion batteries. However, its conductivity is poor, it is not suitable for high-current charging and discharging, and cannot be directly used as an electrode material. At present, the commonly used modification methods include carbon coating and transition metal element doping, or both methods are used simultaneously. Pure carbon coating only enhances the surface conduc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 李辽沙岳海峰李敏红吴照金
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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