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A method for preparing battery-grade iron phosphate from lithium phosphate waste

A lithium phosphate, iron phosphate technology, applied in chemical instruments and methods, lithium carbonate;/acid carbonate, phosphorus compounds, etc., can solve the problems of low mother liquor concentration, hydrogen chloride gas overflow, poor operating conditions, etc. Achieve the effect of good operating environment, high process controllability and no waste residue discharge

Active Publication Date: 2020-11-03
HUNAN YACHENG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses hydrochloric acid to dissolve lithium phosphate, which consumes a lot of acid, and hydrogen chloride gas will overflow. The operating conditions are harsh, the equipment is severely corroded, and the concentration of the mother liquor is low, which increases the energy consumption of the subsequent concentrated lithium extraction process.
In the process of precipitating phosphorus, a large amount of liquid alkali needs to be consumed, and a large amount of heat is released during the acid-base neutralization process, and some lithium phosphate will be re-precipitated, which will reduce the lithium yield; at the same time, the phosphorus resources in lithium phosphate are not well utilized. It will generate iron phosphate precipitation colloid, which is difficult to filter and wash, and will also entrain a large amount of solution
In addition, the iron phosphate produced by this operation is in an amorphous state and cannot be directly used as a precursor of lithium iron phosphate. If it is not treated, it will still occupy a lot of space

Method used

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  • A method for preparing battery-grade iron phosphate from lithium phosphate waste
  • A method for preparing battery-grade iron phosphate from lithium phosphate waste
  • A method for preparing battery-grade iron phosphate from lithium phosphate waste

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Embodiment 1 of the present invention is: a method for preparing battery-grade iron phosphate from lithium phosphate waste, the operation process of which is as follows figure 1 As shown, it specifically includes the following steps:

[0044](1) Collect the lithium phosphate waste produced in the process of producing lithium compounds in a certain factory, and detect the components in the waste. The results are shown in Table 1 below:

[0045] Table 1 Lithium phosphate waste composition analysis table

[0046]

[0047] (2) Weigh 5000g of the above-mentioned lithium phosphate waste material and add it to 5L of water (control the mass ratio of lithium phosphate waste material to pure water or washing water at 1:(1-3) so as to increase the concentration of soluble lithium salt and increase The particle size of amorphous ferric phosphate is better for filtering and washing. The present invention adopts the most preferred ratio of 1:1), and after stirring evenly, add 382...

Embodiment 2

[0052] Embodiment 2 of the present invention is: a method for preparing battery-grade iron phosphate by using lithium phosphate waste, its operation process is as follows figure 1 As shown, it specifically includes the following steps:

[0053] (1) Weigh 10 kg of lithium phosphate waste from the same batch of the above-mentioned examples, add it to 30 L of water, add 9150 g of sulfuric acid (wt% = 98%) after stirring evenly, and after the lithium phosphate is completely dissolved, add 23.5 kg of hexahydrate evenly within 60 minutes Ferric chloride (wt%=98%), the speed of reaction solution is 600r / min, adding potassium hydroxide solution to adjust the pH value of the solution to 3.0, after 80°C reaction time of 60min, filter to obtain soluble lithium salt solution I and amorphous Iron Phosphate Precipitation II.

[0054] (2) Add the alkaline impurity removal agent ammonia into the soluble lithium salt solution I, control the pH value of the solution to 4.5, and filter to obtai...

Embodiment 3

[0057] Embodiment 3 of the present invention is: a method for preparing battery-grade iron phosphate by using lithium phosphate waste, the operation process of which is as follows figure 1 shown, including the following steps:

[0058] (1) take by weighing 50kg lithium phosphate waste material, add in 100L water, add 11450g sulfuric acid (wt%=98%) after stirring evenly, after treating that lithium phosphate dissolves completely, evenly add 76kg ferric sulfate (wt%=99.5%) in 100min, The rotational speed of the reaction solution was 300r / min, the pH value of the solution was adjusted to 2.2 by adding ammonia water, and after a reaction time of 80 minutes at 60°C, the soluble lithium salt solution I and the amorphous iron phosphate precipitate II were obtained by filtration.

[0059] (2) Add alkaline impurity remover sodium carbonate solution into soluble lithium salt solution I, control the pH value of the solution to 4.0, and filter to obtain refined soluble lithium salt soluti...

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Abstract

The invention discloses a method for preparing cell grade iron phosphate by using lithium phosphate waste. The method for preparing cell grade iron phosphate by using lithium phosphate wastecomprisesthe following steps that S1, lithium phosphate waste isprepared into slurry, sulfuric acid solution is added to prepare a mixed solution; S2, ferric salt and alkali liquor are sequentially addedto themixed solution to react under stirring, and the pH value of a reaction system is controlled to be 1.8 to 3.0 to obtain amorphous iron phosphate precipitate I and soluble lithium salt solution I; S3,an alkaline impurity removing agent is added to the soluble lithium salt solution I to adjust the pH value of the solution to 3.0 to 4.5, a solid phase partis collected to obtain iron-containing filter residue I; S4, the amorphous iron phosphate precipitate I and the iron-containing filter residue I are washed; S5, washed productsare mixed and subjected to slurrying, phosphoric acid is added, andafter the reaction is completed, aging and crystallization are conducted, and the precipitatesare washed and calcined to obtain an anhydrous iron phosphate finished product. According to the scheme,the recovery rates of lithium and phosphorus are high, and the prepared iron phosphate can be directly used as a precursor of a lithium battery material.

Description

technical field [0001] The invention relates to the technical field of resource recycling and lithium ion battery materials, in particular to a method for preparing battery-grade iron phosphate from lithium phosphate waste. Background technique [0002] Lithium phosphate is a white crystalline powder. In the industrial production process, lithium hydroxide monohydrate or lithium carbonate is usually used as raw material to prepare lithium phosphate. The prepared lithium phosphate is mainly used for the production of colored phosphors, special glass, optical disc materials, etc. In the production process of lithium and lithium compounds using lithium resources such as ore lithium and salt lake lithium, a large amount of lithium phosphate waste will be produced. Due to the low purity of this lithium phosphate waste product and the difficulty in separating impurities, it is very difficult to reuse and prepare a fluorescent agent lithium phosphate material with a specific valenc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37C01D15/08
CPCC01B25/375C01D15/08C01P2006/80C01P2006/82
Inventor 刘志成万文治张洲辉王玉龙
Owner HUNAN YACHENG NEW MATERIAL CO LTD
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