Method for synthesizing ferric phosphate by utilizing waste phosphate generated by precipitation of trace heavy metal

A waste phosphate and heavy metal technology, which is applied in the direction of phosphorus compounds, non-metallic elements, chemical instruments and methods, etc., can solve the problems of high production cost and small particle size of iron phosphate, and achieve qualified product quality, simple process and good industrial The effect of applying the foreground

Active Publication Date: 2019-05-28
취저우화여우코발트뉴머터리얼컴퍼니리미티드
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Problems solved by technology

Chinese Publication No. CN103887499A introduces a method for preparing iron phosphate by using an aqueous solution of iron acrylate and a soluble phosphate solution. The particle size of iron phosphate prepared by this method is small and uniform, but there is also the problem of high production cost.

Method used

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  • Method for synthesizing ferric phosphate by utilizing waste phosphate generated by precipitation of trace heavy metal
  • Method for synthesizing ferric phosphate by utilizing waste phosphate generated by precipitation of trace heavy metal
  • Method for synthesizing ferric phosphate by utilizing waste phosphate generated by precipitation of trace heavy metal

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Embodiment 1

[0031] In this embodiment, the iron source is ferrous sulfate solution, and the phosphorus source is scrap lithium phosphate slag.

[0032] 1) Prepare 75g / L ferrous sulfate solution, wash the scrap lithium phosphate residue with water 1-2 times at the same time, add sulfuric acid to the filter residue after filtration to dissolve it.

[0033] 2) Add tap water + a small amount of hydrogen peroxide to make a base in the reactor. During the stirring process, add waste phosphate solution, 2.5mol ferrous sulfate solution and hydrogen peroxide into the reactor for synthesis. 1. The amount of hydrogen peroxide used is 1.5-2.0 times the amount of ferrous substances in the iron-containing solution, the feeding temperature is 40°C-50°C, the feeding time is 10min, the stirring speed is 240rpm, and the pH value of the process is 2.3-2.6. After the synthesis, the material is reacting After the kettle was kept warm for 60 minutes, the synthetic material and lithium-containing liquid were ob...

Embodiment 2

[0041] The iron source used in the present embodiment is a white metal leaching solution, and the phosphorus source is scrap lithium phosphate slag, and the main components of the white metal leaching solution are shown in Table 2:

[0042] Table 2 Contents of main elements in white alloy leaching solution (g / L)

[0043] element

co

Cu

Ni

Fe

Al

mn

Ca

Mg

Zn

content

37.71

0.0067

0.016

112.3

0.55

0.35

0.72

0.76

0.65

[0044] 1) Adjust the pH of the white metal leaching solution to 4-5 with cobalt carbonate at room temperature, then add iron powder and stir for 0.5 hours at room temperature, then filter with suction. After the filter, adjust the pH of the filtrate to 2.8 to obtain purified liquid , diluted to 72g / L.

[0045] 2) Wash the scrap lithium phosphate slag with water for 1-2 times, and add sulfuric acid to the filter residue after filtering to dissolve it.

[0046]3) Add tap water + a smal...

Embodiment 3

[0054] In this embodiment, the iron source is ferric chloride solution, and the phosphorus source is scrap lithium phosphate slag.

[0055] 1) Prepare a 75g / L ferric chloride solution, and at the same time wash the scrap lithium phosphate residue with water for 1 to 2 times, and add phosphoric acid to the filter residue after filtration to dissolve it.

[0056] 2) Add tap water into the reaction kettle, and feed the waste phosphate solution and 2.5mol ferric chloride solution into the reaction kettle to synthesize during the stirring process. During the process, keep the molar ratio of iron and phosphorus as 1, and the feeding temperature is 40°C-50°C , the feeding time is 10min, the stirring speed is 240rpm, and the pH value of the process is 2.3-2.6. After the synthesized material is kept warm in the reactor for 60min, the synthesized material and lithium-containing liquid are obtained by suction filtration.

[0057] 3) Wash the synthesized material at a temperature of 40-70...

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Abstract

The invention discloses a method for synthesizing ferric phosphate by utilizing waste phosphate generated by precipitation of trace heavy metal. The method is characterized by utilizing the waste phosphate as a phosphorus source, mixing the phosphorus source with an ferric-containing solution or mixing the phosphorus source with a ferrous solution and hydrogen peroxide after dissolving, synthesizing the ferric phosphate under a low-temperature condition, and filtering, thus obtaining filtrate and filter residue; recycling other valuable metal in the filtrate, adding phosphoric acid after washing and pulpifying the filter residue, converting under the condition that the temperature is 90 DE C, carrying out suction filtration after keeping warm, and drying free water in a suction filtrationmaterial, thus obtaining ferric phosphate dihydrate; calcining, thus preparing an anhydrous ferric phosphate product. The method for synthesizing the ferric phosphate by utilizing the waste phosphategenerated by precipitation of the trace heavy metal, disclosed by the invention, is simple in operation, a prepared ferric phosphate product can meet battery-grade standard requirements, the purpose of recycling phosphorus from the waste phosphate is realized, and the synthesis cost of the ferric phosphate can be obviously reduced; meanwhile, waste residue can be recycled, the additional value ofthe waste residue can be increased, and the problem of environment protection caused by the waste phosphate is also solved.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy, and in particular relates to a method for synthesizing battery-grade iron phosphate from waste phosphate or unqualified phosphate produced by precipitation of trace heavy metals. Background technique [0002] Olivine-type lithium iron phosphate has unique advantages as a cathode material for lithium-ion secondary batteries, not only has a wide source of raw materials, low preparation costs, and is environmentally friendly, but also its stable internal structure shows excellent safety and cycle performance. Through the comparison of different synthesis processes of lithium iron phosphate materials at present, it is found that iron phosphate is used as the precursor of lithium iron phosphate material synthesis, which has many advantages. The precursor iron phosphate and lithium iron phosphate have similar structures. Unique advantages, and iron phosphate provides iron source and phosphorus ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 胡雷田金花丁子君王磊纪婉莹
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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