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Lithium salt refining process

A lithium salt and process technology, applied in the direction of lithium carbonate;/acid carbonate, etc., can solve the problems of poor decomposition effect and low recovery rate, so as to improve decomposition yield, reduce process cost and operation process Simplified effect

Inactive Publication Date: 2017-09-22
WENGFU (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is: the present invention provides a lithium salt refining process to solve the shortcomings of low recovery rate and poor decomposition effect in the carbonization decomposition method in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1. The first carbonization reaction process conditions:

[0018] The first carbonization reaction process conditions: add 22 parts of water to 1 part of the crude lithium salt to be purified, and feed CO at a rate of 2 times / min of the amount of water 2 Until the carbonization is complete (about 80 minutes), the stirring rate is 300r / min (adjusted according to the size of the reactor and the efficiency of stirring and ventilation);

[0019] 2. The first thermal decomposition process conditions:

[0020] The first thermal decomposition process: After the carbonization is completed, add ethanol solution to the carbonization solution, add 8 parts of ethanol solution, and then directly raise the temperature from 25°C to 90°C (the heating time is about 60 minutes, during which 4.4-4.5 parts of water are evaporated), Thermally decompose for 30 minutes under the thermal decomposition condition with a stirring rate of 300r / min, suction or pressure filter to obtain a crude carb...

Embodiment 2

[0029] 1. The first carbonization reaction process conditions:

[0030] The first carbonization reaction process conditions: add 23 parts of water to 1 part of the crude lithium salt to be purified, and feed CO at a rate of 2 times / min of the water volume 2 Until the carbonization is complete (about 80 minutes), the stirring rate is 300r / min (adjusted according to the size of the reactor and the efficiency of stirring and ventilation);

[0031] 2. The first thermal decomposition process conditions:

[0032] The first thermal decomposition process: After the carbonization is completed, add ethanol solution to the carbonization solution, add 4 parts of ethanol solution, and then directly raise the temperature from 25°C to 90°C (the heating time is about 60 minutes, during which 4.4-4.5 parts of water are evaporated), Thermally decompose for 30 minutes under the thermal decomposition condition with a stirring rate of 300r / min, suction or pressure filter to obtain a crude carboni...

Embodiment 3

[0040] Embodiment 3 (comparative example)

[0041] With a liquid-solid ratio of 22:1 in a single cycle, 500ml of water is used as the reaction solution to weigh the crude lithium carbonate, and the reaction device is placed in a water bath at 25°C, and CO is introduced at a rate of 1L / min. 2 , After 80 minutes of reaction at a stirring speed of 300r / min, the carbonization reaction ends. The solution after the carbonization reaction is filtered, and the filtrate is heated from a water bath of 25°C to 90°C, and the stirring rate is 300r / min under the thermal decomposition condition for 90 minutes, and the thermal filtration is performed after the thermal decomposition, and the obtained product does not need to be washed.

[0042]Add water to the filtrate after thermal decomposition to 500ml, and add quantitative crude lithium carbonate at the same time to carry out the first cycle. The cycle reaction conditions and operation process are the same as the first reaction. The final...

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Abstract

The invention discloses a lithium salt refining process, which is characterized by comprising the following steps of (1) primary carbonization reaction: adding lithium salt crude products to be purified into water; introducing CO2 at the gas introducing speed of 2 times of the water quantity per minute until the carbonization is complete; (2) primary heat decomposition: after the carbonization completion, adding ethyl alcohol solution; directly raising the temperature from 25 DEG C to 90 DEG C; performing heat decomposition, suction filtration or pressing filtering to obtain a crude carbonization product; performing hot water stirring and washing for three times; drying and refining the carbonization product; putting washing liquid and mother liquid into the next reaction; (3) circulation carbonization reaction: supplementing and adding water to 22 to 23 parts in the mother liquid in the primary heat decomposition mother liquid; adding 0.6 part of lithium salt crude product to be purified; introducing CO2 at the gas introducing speed of 2 times of water quantity per minute until the carbonization is complete; (4) circulation heat decomposition: after the carbonization completion, directly raising the temperature of the carbonization liquid from 25 DEG C to 90 DEG C; under the stirring condition, performing heat decomposition; performing hot water stirring and washing for three times; performing suction filtration or pressing filtration to obtain a crude carbonization product; drying and refining the carbonization product; putting the washing liquid and the mother liquid to the next reaction; (5) final treatment: repeating the steps (3) and (4) for 2 to 5 times; performing final treatment on the washing liquid and the mother liquid.

Description

technical field [0001] The invention relates to a process for purifying lithium salts, in particular to a process for purifying lithium salts by carbonization and decomposition. Background technique [0002] At present, the common lithium carbonate products in the market adopt the lime causticization process. This process is such as lithium concentrate grinding → ore washing → causticization → separation of lithium hydroxide solution and lithium slag → evaporation and concentration → impurity removal → carbon dioxide carbonization → separation Washing → lithium carbonate products. This process needs to consume lime and produce more lithium slag (about 2.8 tons of lithium slag per ton of product output), and the causticizing solution must also be evaporated and concentrated (from Li 2 The mass concentration of O is about 18g / L increased to 50-60g / L), the lithium carbonate produced by this process can only meet the industrial grade lithium carbonate standard, and cannot be di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/08
CPCC01D15/08C01P2006/80
Inventor 陈卓谢田尹晓刚程琥杨锦瑜郭举李鹏武
Owner WENGFU (GRP) CO LTD