Process for extracting lithium in salt lake brine through phosphate ion liquid to produce lithium carbonate

A technology of ionic liquids and phosphate esters, applied in the direction of lithium carbonate;/acid carbonate, process efficiency improvement, etc., can solve problems such as the difficulty of separating and extracting lithium, and achieve easy industrial production and shorten the stratification time , Improve the extraction efficiency

Inactive Publication Date: 2018-11-23
青海柴达木兴华锂盐有限公司
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  • Application Information

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Problems solved by technology

Lithium resources exist in the form of solid ore and salt lake brine. my country's salt lake lithium resources are rich, especially in the Qaidam Basin in Qinghai, with reserves of 24.47 million tons (LiCl). Due to the high content of associated magnesium, magnesium in brine The / lithium ratio (mass ratio) is as high as 40-1200, making it very difficult to separate and extract lithium

Method used

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  • Process for extracting lithium in salt lake brine through phosphate ion liquid to produce lithium carbonate
  • Process for extracting lithium in salt lake brine through phosphate ion liquid to produce lithium carbonate
  • Process for extracting lithium in salt lake brine through phosphate ion liquid to produce lithium carbonate

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Embodiment 1

[0028] The ionic liquid is dibutyl(2-(trimethyl-amino)ethyl)phosphonic acid hexafluorophosphate, and its structural formula is:

[0029]

[0030] The co-extraction agent is TBP, and the ratio of the two is 1:9; then it is mixed with the diluent hydrogenated kerosene. Add 1 volume of salt lake brine shown in Table 1 into a separatory funnel, add 1 volume of organic phase (compared to O / A=1), wherein the volume ratio of ionic liquid, co-extractant and diluent is 1 : 9: 2, after shaking for 5 minutes, rest and stratify. Determination of Li in the equilibrium aqueous phase + content, the single extraction rate of lithium is calculated to be 75.15%. Add 1 volume of brine to the organic phase, shake for 5 minutes and then separate into layers, and measure the Li in the equilibrium aqueous phase. + content, the calculated extraction rate is 43.99%, continue to repeat, the third yield is 24.67%, the fourth yield is 16.65%, and the fifth yield is 10.08%. After five extractions, ...

Embodiment 2

[0034] The ionic liquid is diethyl(2-(trimethyl-amino)butyl)phosphonic acid hexafluorophosphate, and its structural formula is:

[0035]

[0036] The co-extractant is a mixture of TBP and N503 (N, N'-dimethylheptylacetamide), the volume ratio of which is 1: 10; it is then mixed with diluent hydrogenated kerosene. Add 1 volume of salt lake brine shown in Table 1 into a separatory funnel, add 1 volume of organic phase (compared to O / A=1), wherein the volume ratio of ionic liquid, co-extractant and diluent is 1 : 10: 3, after shaking for 5 minutes, rest and stratify. Determination of Li in the equilibrium aqueous phase + content, the single extraction rate of lithium is calculated to be 73.89%. Add 1 volume of brine to the organic phase, shake for 5 minutes and then separate into layers, and measure the Li in the equilibrium aqueous phase. +content, the calculated extraction rate was 42.80%, and continued to repeat, the third yield was 26.53%, the fourth yield was 17.32%, a...

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Abstract

The invention provides a process for extracting lithium in salt lake brine to produce lithium carbonate. An extraction system comprises an extraction agent, a co-extraction agent and a diluent, wherein the extraction agent is phosphate ionic liquid containing lithium extraction functional groups, and sodium carbonate is added into solution subjected to extraction and oil removal for primary magnesium removal, after filtering, sodium hydroxide is added into the filtrate for secondary deep magnesium removal, the filtrate is concentrated, sodium carbonate is added for lithium precipitation, filtering is carried out to obtain a filter cake, washing with hot water is carried out, then drying is carried out, and the lithium carbonate is obtained. According to the extraction system, the saturation capacity of the extraction agent is increased by 1 time compared with that of an existing extraction agent and reaches 4 g / L, dilute hydrochloric acid can be used for back extraction, an organic phase is only washed with pure water so that the extraction agent can be regenerated, the process route is simplified, and the production cost is greatly reduced; and according to the process, a soap chemical sequence and an iron removal process are eliminated, so that industrial large-scale production is better facilitated.

Description

technical field [0001] The invention relates to a process for extracting lithium from high-magnesium-lithium ratio salt lake brine and producing lithium carbonate by a solvent extraction method. Background technique [0002] As a new strategic energy source, lithium is mainly used in fields such as batteries, nuclear power generation, aerospace, and medicine. Lithium resources exist in the form of solid ore and salt lake brine. my country's salt lake lithium resources are rich, especially in the Qaidam Basin in Qinghai, with reserves of 24.47 million tons (LiCl). Due to the high content of associated magnesium, magnesium in brine The / lithium ratio (mass ratio) is as high as 40-1200, which makes it very difficult to separate and extract lithium. Extraction method is one of the most promising methods for extracting lithium from brine. The system with better effect is tributyl phosphate-ferric chloride-kerosene system. In 1979, Qinghai Salt Lake Research Institute of Chinese A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/12C22B3/40C01D15/08
CPCC01D15/08C22B26/12C22B3/409Y02P10/20
Inventor 孟庆芬王延风赵朋龙张晓梅席田兴娇春鹏薛林
Owner 青海柴达木兴华锂盐有限公司
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