Method for recovering lithium from sodium sulfate as lithium extraction by-product of spodumene sulfuric acid process

A technology for extracting lithium and by-products from a process, which is applied in the field of lithium recovery, can solve problems such as difficulties in recovering lithium, high production costs, and high production capacity, and achieve good economic benefits, energy saving, and low impurity content

Active Publication Date: 2019-02-19
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 sodium sulfate as lithium extraction by-product of 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...

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 lithiu...

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

[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 solution and solid slag. The lithium sulfate solution is returned to the lithium salt production line, and t...

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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 Applications(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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