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Method and device for extracting and preparing battery-grade lithium carbonate from P507 raffinate

A technology of extraction device and raffinate, which is applied in the field of non-ferrous metal hydrometallurgy, can solve the problems of increasing the difficulty of recycling and environmental protection treatment, low purity of lithium products, and failing to reach battery-grade lithium salts, so as to reduce the difficulty of wastewater treatment. , The effect of improving product purity and improving recovery rate

Pending Publication Date: 2021-06-22
HUNAN JIN YUAN NEW MATERIALS LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The prepared lithium product has low purity and cannot reach the standard of battery-grade lithium salt
After precipitation, the concentration of lithium ions in the liquid is still about 200mg / L, and subsequent treatment needs to be continued, which increases the difficulty of recovery and environmental protection treatment

Method used

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  • Method and device for extracting and preparing battery-grade lithium carbonate from P507 raffinate
  • Method and device for extracting and preparing battery-grade lithium carbonate from P507 raffinate
  • Method and device for extracting and preparing battery-grade lithium carbonate from P507 raffinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0028] Implementation mode 1: if figure 1 , a method for extracting and preparing battery-grade lithium carbonate from P507 raffinate, comprising the following steps: blending, extraction, purification, stripping, alkalization, crystallization, separation, and drying. The special features are:

[0029] The blending: first adjust the pH value of the P507 raffinate to 8.5-10.5 with lithium hydroxide or alkali, filter, and keep the filtrate for later use.

[0030] The above-mentioned adjustment of pH value with lithium hydroxide or alkali can be adjusted to 9-10, 8.5-9, 9-9.5, 9.5-10.

[0031] This step can effectively precipitate and remove impurity cations such as nickel, and the experimental data are shown in Table 1.

[0032] Table 1: The effect of pH value on the removal of impurity cations such as nickel by precipitation

[0033]

[0034] The extraction: In the extraction device, mix the saponified P507 with the filtered liquid in the mixing step, and then stand still ...

Embodiment approach 2

[0064] Implementation mode 2: if figure 1 A method for extracting and preparing battery-grade lithium carbonate from P507 raffinate, which is special in that it comprises the following steps:

[0065] a. Blending: first adjust the pH value of the P507 raffinate to 8.5-10.5 with lithium hydroxide or alkali, preferably 9-10, 9.5, filter, and keep the filtrate for later use. It can precipitate and remove impurity cations such as nickel.

[0066] b. Extraction: In the extraction device, mix the saponified P507 with the liquid filtered in the previous step, let stand to separate the phases after mixing, keep the P507 organic phase (loaded organic phase) for use, and detect lithium in the water phase (raffinate) If the ion concentration is less than 1mg / L, it can be sent to wastewater treatment. This step can extract the lithium in the filtrate into the organic phase, reduce the concentration of lithium ions in the raffinate, and reduce the difficulty of wastewater treatment.

[...

Embodiment approach 3

[0074] Implementation mode 3: if Figure 2-4 , an extraction device for extracting and preparing battery-grade lithium carbonate from P507 raffinate, equipped with a stirring chamber 5, which is connected with a clarification chamber 7 through a transition tank 6, and is provided with a stirrer in the stirring chamber 5, and its special feature is that : the stirring chamber 5 is a cube, the clarification chamber 7 is a cuboid, the aspect ratio of the clarification chamber 7 is 4-5:1, the volume ratio of the stirring chamber 5 and the clarification chamber 7 is 1:4.5-5.5, and the mixer consists of a main mixer 1 Composed of auxiliary mixer 2, the main mixer 1 is equipped with stirring blade 4, which is made into a double-layer cross shape, and the stirring body of the auxiliary mixer 2 is made into a cylindrical stirring body 3, which is evenly distributed on the wall of the cylindrical stirring body 3 There is a circular small hole with a diameter of 5-10 mm, and the stirring...

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Abstract

The invention discloses a method and device for extracting and preparing battery-grade lithium carbonate from P507 raffinate, belongs to the technical field of non-ferrous metal wet metallurgy, and particularly relates to a lithium ion extraction purification and concentration crystallization technology. The method comprises the steps of impurity adjustment, extraction, purification, back extraction, alkalization, crystallization, separation, drying and the like; in the step of impurity adjustment, the PH value of P507 raffinate is adjusted to 8.5-10.5 through lithium hydroxide or alkali, filtration is conducted, and filtrate is reserved for use; the alkalization comprises the following steps of heating a lithium solution to 85-95 DEG C, adding lithium hydroxide or alkali to adjust the pH value to 9.0-13.0, keeping the temperature at 85-95 DEG C, standing for 2-8 hours, and filtering to obtain filtrate for later use; and in the crystallization step, compressed air is introduced into the alkalized filtrate, the pressure of the compressed air is 0.2-0.8 MPa, the air flow of the compressed air is 8-30 m < 3 > / h, meanwhile, evaporation and concentration are carried out, and when fine crystals exist in the concentrated solution, discharging and cooling are carried out. The lithium content in the raffinate is less than 1mg / L, so that the wastewater treatment difficulty is reduced; the lithium solution is deeply purified through the processes of impurity adjustment, extraction, purification, back extraction and the like; and the yield of lithium carbonate obtained after alkalization, crystallization, separation and drying is 99% or above, and the product purity completely meets the battery grade requirement.

Description

technical field [0001] The invention relates to the technical field of nonferrous metal hydrometallurgy, in particular to a lithium ion extraction purification and concentration crystallization technology. Background technique [0002] When the positive electrode material of lithium ion battery is recovered by wet method, when P507 extractant is used for extraction, the raffinate contains more than 1g / L lithium. The recovery of lithium in the raffinate is generally prepared by precipitation of trisodium phosphate or carbonate to prepare lithium phosphate or lithium carbonate. The overall yield of lithium phosphate or lithium carbonate prepared by this method is generally 70-90%. The prepared lithium product has low purity and cannot meet the standard of battery-grade lithium salt. After precipitation, the concentration of lithium ions in the solution is still about 200mg / L, and subsequent treatment is required, which increases the difficulty of recovery and environmental p...

Claims

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Application Information

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IPC IPC(8): C01D15/08B01D11/04
CPCC01D15/08B01D11/0457B01D11/0488B01D11/0492C01P2006/80Y02P10/20C22B26/12C22B3/22C22B3/34C01D7/22C01D7/24
Inventor 刘训兵彭灿刘振张超文周群成王子董雄武赵湘平吴山木
Owner HUNAN JIN YUAN NEW MATERIALS LTD
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