Phosphate extraction agent and method for extracting and separating lithium-manganese leaching solution by using phosphate extraction agent

The technology of extracting agent and phosphate ester is applied in the field of extracting agent of phosphate ester and its extraction and separation of lithium manganese leaching solution, which can solve the problems such as the adverse effect of separation and recovery of lithium salt product purity, incomplete separation of lithium manganese and low current efficiency, etc. The effect of eliminating saponification waste liquid, efficient green extraction, and improving lithium recovery rate

Pending Publication Date: 2022-03-01
CENT SOUTH UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Although the chemical precipitation method (neutralization, hydrolysis precipitation and sulfuration precipitation) can quickly precipitate manganese, it is easy to introduce new impurity ions, which not only adversely affects the subsequent separation and recovery of lithium and the purity of lithium salt products, but also produces sodium sulfate and ammonium sulfate. , calcium sulfate and other waste
Electrochemical deposition technology can recover manganese dioxide powder, but it also has the disadvantages of low current efficiency, high power consumption, and incomplete separation of lithium and manganese

Method used

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  • Phosphate extraction agent and method for extracting and separating lithium-manganese leaching solution by using phosphate extraction agent
  • Phosphate extraction agent and method for extracting and separating lithium-manganese leaching solution by using phosphate extraction agent
  • Phosphate extraction agent and method for extracting and separating lithium-manganese leaching solution by using phosphate extraction agent

Examples

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Embodiment 1

[0042] The initial pH value of the lithium-manganese leaching solution is 3, and the contents of valuable metals are Li 20g / L and Mn 40g / L. Follow the steps below for clean and efficient extraction and separation of lithium and manganese in a mixed-settler tank:

[0043] (1) Prepare and extract the organic phase: select dialkyl phosphate (II) as the extractant, n-butanol as the modifier, and sulfonated kerosene as the diluent, according to "40% extractant + 10% modifier + dilution The volume ratio of agent 50%" is configured to extract the organic phase.

[0044] (2) Manganese extraction: using the extracted organic phase configured in step (1), under the process conditions that the O / A ratio is 1:2, the extraction temperature is 40°C, and the extraction time is 10min, the lithium-containing manganese leachate is extracted. 8-stage extraction of manganese to obtain manganese-loaded organic phase and lithium-containing raffinate. Through detection and calculation, the extract...

Embodiment 2

[0048] The initial pH value of the lithium manganese leach solution is 4, and the contents of valuable metals are Li 18g / L and Mn 8g / L respectively. Follow the steps below for clean and efficient extraction and separation of lithium and manganese in a mixed-settler tank:

[0049] (1) Prepare and extract the organic phase: select monoalkyl phosphate (I) as the extractant, n-butanol as the modifier, and sulfonated kerosene as the diluent, according to "35% extractant + 15% modifier + dilution The volume ratio of agent 50%" is configured to extract the organic phase.

[0050] (2) Manganese extraction: using the extracted organic phase configured in step (1), under the process conditions that the O / A ratio is 1:3, the extraction temperature is 45°C, and the extraction time is 6min, the lithium-containing manganese leachate is extracted. Manganese is extracted in three stages to obtain a manganese-loaded organic phase and a lithium-containing raffinate. Through detection and calc...

Embodiment 3

[0054] The initial pH value of the lithium manganese leach solution is 2, and the contents of valuable metals are Li 10g / L and Mn 30g / L respectively. Follow the steps below for clean and efficient extraction and separation of lithium and manganese in a mixed-settler tank:

[0055] (1) Prepare and extract the organic phase: select "20wt% monoalkyl phosphate (I) + 80wt% dialkyl phosphate (II)" as the extractant, isobutanol as the modifier, and sulfonated kerosene as the diluent According to the volume ratio of "extractant 40% + modifier 15% + diluent 45%", the organic phase is extracted.

[0056] (2) Manganese extraction: using the extracted organic phase configured in step (1), under the process conditions that the O / A ratio is 1:1, the extraction temperature is 40°C, and the extraction time is 10min, the lithium-containing manganese leachate is extracted. Manganese is extracted in 4 stages to obtain a manganese-loaded organic phase and a lithium-containing raffinate. Through...

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Abstract

The invention provides a phosphate extracting agent and a method for extracting and separating a lithium-manganese leaching solution by using the phosphate extracting agent, and belongs to the technical field of hydrometallurgy separation. The method comprises the following steps: mixing a phosphate extracting agent with a modifier and a diluent to obtain an extracted organic phase, and carrying out multi-stage extraction under the conditions of preset O / A phase ratio, temperature and time, so that manganese ions are extracted into the organic phase, and lithium ions are retained in raffinate; and after the manganese-loaded organic phase is subjected to multi-stage washing with pure water, the manganese in the organic phase enters the water phase through multi-stage reverse extraction with sulfuric acid, and a pure manganese sulfate solution is produced. Compared with a chemical precipitation manganese separation process, the method can avoid generation of waste residues such as sodium sulfate, ammonium sulfate and calcium sulfate, eliminates saponification waste liquid generated in a saponification process in a traditional phosphoric acid extraction agent manganese extraction process, and realizes efficient separation and green extraction of lithium and manganese in the solution.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgical separation, in particular to a phosphate extraction agent and a method for extracting and separating lithium manganese leaching liquid. Background technique [0002] Waste lithium-ion batteries are rich in valuable resources such as lithium, nickel, cobalt, manganese, copper, aluminum, and graphite. In order to alleviate the supply pressure of key energy metal resources and eliminate potential environmental risks, the recycling of valuable metals in waste lithium-ion batteries has become a hot spot in the lithium battery industry. Waste lithium battery recycling processes include fire method and wet method. Most domestic lithium battery recycling companies use wet method. Patent CN107181014A discloses a recovery method for waste lithium manganate batteries. In this method, the lithium manganate batteries are firstly disassembled and washed to obtain positive electrode materials. Lithi...

Claims

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Application Information

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IPC IPC(8): C22B3/38C22B26/12C22B47/00
CPCC22B26/12C22B47/00Y02P10/20
Inventor 陈永明常娣杨声海李帅张红亮介亚菲常聪石鹏飞方港
Owner CENT SOUTH UNIV
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