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Method for recovering lithium from lithium by-product sodium sulfate extracted from spodumene sulfuric acid process

A technology for extracting lithium and by-products

Active Publication Date: 2021-01-22
天齐锂业(射洪)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention provides a method for recovering lithium from sodium sulfate, a by-product of lithium extraction by spodumene sulfuric acid process, which solves the difficulty in recovering lithium from the by-product sodium sulfate produced by spodumene sulfuric acid process and makes lithium sulfate into element The problem of high production capacity and high production cost when making powder

Method used

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  • Method for recovering lithium from lithium by-product sodium sulfate extracted from spodumene sulfuric acid process

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Effect test

Embodiment 1

[0039] Embodiment 1: the method for reclaiming lithium from lithium by-product sodium sulfate from spodumene sulfuric acid process

[0040] Include the following steps in order:

[0041] Step (1), get the sodium sulfate of lithium carbonate workshop, its main composition is as follows: (%)

[0042] Na 2 SO 4

Li 2 SO 4 (with Li 2 O meter)

Fe pH (5% aqueous solution) 99.35 0.035 0.0008 6.5

[0043] Take 2.1Kg of dry coal powder and 10Kg of sodium sulfate, mix them evenly, and react in an oxygen-isolated reactor at 825°C for 55 minutes. After the reaction is completed, cool to obtain a roasted material.

[0044] Step (2), the roasted material is extracted with hot water at 70°C, filtered and separated to obtain filter residue, filtrate and washing water, and the washing water is used for the next extraction;

[0045] In step (3), dilute sulfuric acid is added to the filter residue according to the alkali content to obtain lithium sulfate s...

Embodiment 2

[0050] Embodiment 2: the method for reclaiming lithium from lithium by-product sodium sulfate from spodumene sulfuric acid process

[0051] Include the following steps in order:

[0052] Step (1), get the sodium sulfate of lithium hydroxide workshop, its main composition is as follows: (%)

[0053] Na 2 SO 4

Li 2 SO 4 (with Li 2 O meter)

Fe pH (5% aqueous solution) 98.77 0.27 0.0007 12

[0054] Take 2.9Kg of dry coal powder and 10Kg of sodium sulfate, mix them evenly, and react in an oxygen-isolated reactor at 1075°C for 25 minutes. After the reaction is completed, cool to obtain a roasted material.

[0055] Step (2), the roasted material is extracted with hot water at 40°C, filtered and separated to obtain filter residue, filtrate and washing water, and the washing water is used for the next extraction;

[0056] In step (3), dilute sulfuric acid is added to the filter residue according to the alkali content to obtain lithium sulfate ...

Embodiment 3

[0061] Embodiment 3: the method for reclaiming lithium from lithium by-product sodium sulfate from spodumene sulfuric acid process

[0062] Include the following steps in order:

[0063] Step (1), get the sodium sulfate of lithium carbonate workshop, its main composition is as follows: (%)

[0064] Na 2 SO 4

Li 2 SO 4 (with Li 2 O meter)

Fe pH (5% aqueous solution) 99.22 0.15 0.0006 5.8

[0065] Take 2.5Kg of dry coal powder and 10Kg of sodium sulfate, mix them evenly, and react in an oxygen-isolated reactor at 895°C for 40 minutes. After the reaction is completed, cool to obtain a roasted material.

[0066] Step (2), the roasted material is extracted with hot water at 40°C, filtered and separated to obtain filter residue, filtrate and washing water, and the washing water is used for the next extraction;

[0067] In step (3), dilute sulfuric acid is added to the filter residue according to the alkali content to obtain lithium sulfate ...

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Abstract

A method for recovering lithium from sodium sulfate as a lithium extraction by-product of a spodumene sulfuric acid process is characterized by including: uniformly mixing the lithium-containing sodium sulfate as the lithium extraction by-product with pulverized coal, and roasting in an oxygen-isolated condition to obtain roasted material; extracting the roasted material by water, and filtering toobtain a filter residue and filter liquid; adopting dilute sulfuric acid to extract the lithium in the filter residue, and performing solid-liquid separation to obtain a lithium sulfate solution anda solid residue; subjecting the filter liquid to evaporation, concentration and crystallization, and when a solid is separated out, performing solid-liquid separation to obtain a solid product and a first mother liquid; introducing carbon dioxide into the first mother liquid according to lithium content, and performing solid-liquid separation to obtain secondary mother liquid and lithium carbonate. The method for recovering the lithium from the sodium sulfate as the lithium extraction by-product of the spodumene sulfuric acid process solves the problem that the lithium in the lithium-containing sodium sulfate as the lithium extraction is difficult to recover formerly, and has the advantages that lithium recovering rate can be over 95%, the low-value lithium-containing sodium sulfate as thelithium extraction by-product can be turned into high-value sodium sulfide, iron content in the sodium sulfide is less than 0.0010%, and impurity content in the sodium sulfide is much lower.

Description

technical field [0001] The invention relates to the field of lithium recovery, in particular to a method for recovering lithium from sodium sulfate, a by-product of lithium extraction in a spodumene sulfuric acid process. Background technique [0002] The preparation of lithium sulfate from spodumene by sulfuric acid method will produce sodium sulfate as a by-product, which contains high water and a certain amount of lithium due to its special process. A certain amount of lithium (calculated as lithium oxide, the same below) is entrained in sodium sulfate, and its content is 0.01-0.35% according to different process parameters and equipment. Lithium is currently an important raw material for new energy vehicles, energy storage materials, and lithium-ion batteries for 3C products. It is not only scarce, but also has a high market price, so it should be recycled. [0003] Lithium is the metal element with the highest negative potential (-3.043V) and the highest electrochemica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/06C01D15/08C01B17/26
CPCC01B17/26C01D15/06C01D15/08C01P2006/80
Inventor 邓红云严新星陈格
Owner 天齐锂业(射洪)有限公司
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