Method for preparing high-purity lithium chloride, high-purity lithium formate and high-purity lithium carbonate

A lithium chloride, high-purity technology, applied in the direction of lithium carbonate;/acid carbonate, lithium halide, carboxylate preparation, etc., can solve the problems of production capacity bottleneck, high raw material quality requirements, long process, etc. Achieve the effect of small project investment, low equipment requirements, and industrialization

Active Publication Date: 2019-05-28
SHENZHEN MAXCHEMTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process from crude lithium chloride to high-purity battery-grade lithium carbonate has various shortcomings such as long process, large investment in new refining equipment, and difficulty in rapidly increasing refining capacity in a short period of time.
[0004] In the carbonate-type lithium-containing salt lake represented by Zabuye Salt Lake in Tibet, the technical route of refining and producing lithium hydroxide and lithium carbonate after the solar pond was used to precipitate lithium carbonate ore in the early stage also has capacity bottlenecks and the purity of lithium carbonate products. ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] One, the preparation of crude lithium chloride raw material in step S1

[0049] Taking crude lithium chloride obtained by extracting lithium from a salt lake with a purity (dry basis) of 85wt% to 99.5wt% as a raw material as an example, the preparation of crude lithium chloride includes the following steps:

[0050] A. Enrich lithium ions from the old salt lake brine to obtain an eluent with higher lithium content. For example, it can be specifically: for carbonate-type or sulfate-type lithium-rich brine, a slight excess of calcium chloride (more than 0% and less than or equal to 5%) can be added according to the total amount of carbonate or sulfate. After the powder is fully stirred and evenly reacted, the precipitates such as calcium carbonate or calcium sulfate produced by the reaction are filtered out by filtration, and after being converted into chloride-type brine, lithium ions are enriched from the old salt lake brine by ion sieve or extraction method , obtain t...

Embodiment 2

[0062] One, the preparation of crude lithium chloride raw material in step S1 '

[0063] Taking crude lithium chloride obtained by extracting lithium from a salt lake with a purity (dry basis) of 85wt% to 99.5wt% as a raw material as an example, the preparation of crude lithium chloride includes the following steps:

[0064] A'. Lithium ions are enriched from the old salt lake brine to obtain an eluent with higher lithium content. For example, it can be specifically: for carbonate-type or sulfate-type lithium-rich brine, a slight excess of calcium chloride (more than 0% and less than or equal to 5%) can be added according to the total amount of carbonate or sulfate. After the powder is fully stirred and evenly reacted, the precipitates such as calcium carbonate or calcium sulfate produced by the reaction are filtered out by filtration, and after being converted into chloride-type brine, lithium ions are enriched from the old salt lake brine by ion sieve or extraction method ,...

Embodiment 3

[0074] Embodiment 3: the preparation of high-purity lithium carbonate (purity (dry basis) >=99.5%)

[0075] 1. Preparation of a mixture of lithium bicarbonate and lithium carbonate

[0076] Can adopt following two kinds of schemes, scheme one: according to the amount of lithium chloride or lithium formate, the methyl alcohol of the refined lithium formate (embodiment 2) obtained in above-mentioned step S3 or the refined lithium formate (embodiment 2) that S3 ' obtains In the solution, a saturated aqueous solution of ammonium bicarbonate in equimolar ratio is added dropwise to undergo metathesis reaction to obtain lithium bicarbonate and lithium carbonate; Scheme 2: at low temperature (0°C to -30°C), the refined chloride obtained in the above step S3 Lithium (Example 1) or the methanol solution of refined lithium formate (Example 2) obtained by S33 is passed into carbon dioxide, fully stirred so that the carbon dioxide is fully absorbed by the solution, after the absorption is ...

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Abstract

The invention discloses a method for preparing high-purity lithium chloride, high-purity lithium formate and high-purity lithium carbonate. The method for preparing high-purity lithium chloride comprises: S1, mixing crude lithium chloride and an organic solvent, heating until boiling, removing water in reflux liquid, refluxing the organic solvent until the water content in the reflux liquid and that in the mixed liquid are detected to be both lower than or equal to 0.5 percent by weight, stopping heating and cooling to room temperature to obtain turbid liquid; S2, while stirring, introducing ammonia gas into the turbid liquid, and maintaining stirring for a period of time, so that lithium chloride suspended in the organic solvent is all dissolved, and insoluble matter impurities are filtered to obtain filtrate; S3, adding pure water into the filtrate, uniformly stirring, then dropwise adding refined and decontaminated pre-prepared liquid, thoroughly stirring, filtering, adding at leastone of oxalic acid, oxalate or oxalate ester into the filtrate, stirring, lowering the temperature to -5 DEG C or below, and keep cold to filter insoluble matters in a solution to obtain an organic solution of refined lithium chloride, wherein the purity (dry basis) of lithium chloride is greater than or equal to 99.9 percent by weight.

Description

technical field [0001] The invention relates to a lithium chloride purification process and a method for preparing high-purity downstream products using high-purity lithium chloride, in particular to a method for preparing high-purity lithium chloride, high-purity lithium formate and high-purity lithium carbonate. Background technique [0002] The purity requirement of battery grade lithium carbonate is greater than 99.5wt%; the purity requirement of reagent grade lithium carbonate is greater than 99.9wt%. The existing production technology routes at home and abroad are mainly through the refining and purification of industrial grade lithium carbonate (purity is 98% ~ 99%), or lithium hydroxide is used as raw material to react with carbon dioxide to produce lithium carbonate (such as Chinese patent: ZL201010600802.8) . Because the impurities in these upstream raw materials are very complex and difficult to remove, resulting in high refining costs, this is why the supply of ...

Claims

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Application Information

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IPC IPC(8): C01D15/04C01D15/08C07C51/41C07C51/43C07C53/06
Inventor 谈宇清任琪宫磊钟泉红
Owner SHENZHEN MAXCHEMTECH
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