CN112226632B - Method for selectively extracting and precipitating lithium in lithium mother liquor by using hydrophobic eutectic solvent - Google Patents
Method for selectively extracting and precipitating lithium in lithium mother liquor by using hydrophobic eutectic solvent Download PDFInfo
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Abstract
The invention discloses a method for selectively extracting and precipitating lithium in lithium precipitation mother liquor by using a hydrophobic eutectic solvent. The hydrophobic eutectic solvent takes tetrabutylammonium chloride, tetrahexylammonium chloride and tetraoctylammonium chloride as at least one hydrogen bond acceptor and oleic acid as hydrogen bond donors, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1: (1-3). The invention also specifically discloses a preparation method of the hydrophobic eutectic solvent, an organic phase composition and an extraction application of the hydrophobic eutectic solvent in lithium-containing aqueous solution and lithium in lithium precipitation mother liquor. The extraction organic phase constructed by the hydrophobic eutectic solvent has the advantages of simple synthesis, convenient operation, short extraction time, easy separation, good selective extraction performance and the like.
Description
Technical Field
The invention relates to a method for selectively extracting and precipitating lithium in lithium precipitation mother liquor by using a hydrophobic eutectic solvent.
Background
Lithium is used as a new energy metal and strategic resource and is widely applied to the fields of ceramics, lithium batteries, nuclear energy, glass and the like. With the continuous development of new energy resources worldwide, the lithium ion battery industry for power and energy storage is rapidly developing, and battery grade lithium carbonate (Li) is used2CO3) Is increasing. Currently, sodium carbonate is generally used as a precipitator for preparing lithium carbonate, but in the process, a large amount of lithium precipitation mother liquor with high sodium-lithium ratio is generated. The composition of the lithium precipitation mother liquor is complex, wherein Li+Has high concentration (1.42g/L) and contains a large amount of Na+(55.62g/L)、CO3 2-、Cl-Or SO4 2-. The lithium precipitation mother liquor is directly discharged back to salt lake brine or a recovery system, which not only causes CO3 2-、Cl-Or SO4 2-Enrichment of impuritiesAnd the quality of the lithium salt product is lowered. Therefore, the high-efficiency lithium ion recovery process of the lithium precipitation mother liquor has very important significance for the whole lithium product industrial development.
The solvent extraction method has the advantages of low energy consumption of continuous extraction, easy industrialization, simple operation, small dosage of an extracting agent and the like. The solvent extraction method is widely applied to the extraction of lithium ions from salt lake brine. Common extractants and extraction systems are beta-diketones, crown ethers, organophosphines and ionic liquids. However, ketone extractants are more severely damaged and costly. Crown ethers are expensive and the oxygen atom on the crown ether ring is prone to form hydrogen bonds with water, thereby causing solution losses. The traditional extraction system usually adopts volatile organic solvent as diluent, which not only affects the cycle life of the extraction system, but also causes environmental pollution. Researchers propose that the traditional organic solvent is replaced by the ionic liquid with low vapor pressure and high thermochemical stability, but the ionic liquid is difficult to purify, complex to synthesize and high in cost, and the practical application is greatly limited.
Eutectic Solvents (DES) are a new class of ionic liquid analogues formed by self-association of two-or three-component eutectic mixtures through hydrogen bonding interactions. DES is considered a green solvent due to its low volatility, low cost, biodegradability and low toxicity, and has a wide application prospect. The eutectic solvent is generally composed of hydrophilic compounds, which easily form hydrogen bonds with water, thereby destroying the hydrogen bonds between the components of the eutectic solvent. Therefore, it is important to expand the scope of application of DES from organic to aqueous phase. The hydrophobic eutectic solvents (HDESs) are constructed for the water-containing system, so that the environmental pollution caused by using volatile organic solvents is avoided, the use cost of expensive ionic liquid as an extracting agent is reduced, and the method has wide application potential in solvent extraction.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for selectively extracting and precipitating lithium in lithium mother liquor based on a hydrophobic eutectic solvent, wherein the extraction system takes tributyl phosphate as an extracting agent, and the hydrophobic eutectic solvent as a co-extracting agent and a diluting agent, and has the advantages of high efficiency, good selectivity, convenient operation, environmental friendliness, no pollution and the like.
The technical purpose is achieved through the following technical scheme.
A method for selectively extracting lithium in lithium precipitation mother liquor based on a hydrophobic eutectic solvent comprises the following steps:
(1) preparation of a hydrophobic eutectic solvent:
mixing the hydrogen bond donor and the hydrogen bond acceptor according to a molar ratio, and stirring for 4-12 hours under a heating condition of 50-80 ℃ to obtain a clear transparent solution; namely a hydrophobic eutectic solvent; the hydrogen bond donor is oleic acid, and the hydrogen bond acceptor is quaternary ammonium salt;
(2) and (3) extraction:
forming an organic phase by the hydrophobic eutectic solvent prepared in the step (1) and an extractant tributyl phosphate, mixing the organic phase with a lithium-containing water phase with the pH value regulated by ammonia water, extracting for a period of time under violent oscillation, and centrifuging and layering to obtain an extraction phase and raffinate;
(3) and (3) elution:
and (3) eluting the extract phase obtained in the step (2) with hydrochloric acid, and centrifuging and layering to obtain a lithium-rich solution.
In the step (1), the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is (1-3): 1.
further, the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is 3: stirring time was 6 hours.
In the step (1), the quaternary ammonium salt is at least one of tetrabutylammonium chloride, tetrahexylammonium chloride and tetraoctylammonium chloride.
In the step (2), the volume fraction of the hydrophobic eutectic solvent in the organic phase is 10-40%.
In the step (2), the concentration of the ammonia water in the lithium-containing aqueous phase is 0.5-2.5 mol/L.
In the step (2), the volume ratio of the organic phase to the lithium-containing aqueous phase is 0.4-1.2.
In the step (2), the oscillating speed of the violent oscillation is 130 rpm-200 rpm.
In the step (3), the concentration of the hydrochloric acid is 0.5-2.5 mol/L, and the elution time is 20-40 minutes.
The invention has the beneficial effects that:
1) the invention firstly provides an extraction system based on a hydrophobic eutectic solvent for selective extraction of lithium in lithium precipitation mother liquor. The eutectic solvent has the advantages of simple synthesis, low price, environmental friendliness and the like, and the extraction system based on the hydrophobic eutectic solvent can selectively extract lithium.
2) The extraction system based on the hydrophobic eutectic solvent has better extraction rate.
3) The extraction system based on the hydrophobic eutectic solvent has the advantages of simple operation, good safety and the like. And the eutectic solvent is easy to separate, can not cause secondary pollution of water, and has better economic and social benefits.
Drawings
Fig. 1 is a flow chart of a method for extracting lithium from a lithium deposition mother liquor according to an embodiment of the present invention.
FIG. 2 is a real image of the two-phase interface of organic phase-aqueous phase containing lithium under the extraction system.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
(1) Preparation of hydrophobic eutectic solvent: tetrabutylammonium chloride and oleic acid are mixed according to a molar ratio of 1: (1-3), and stirring for 4-12 hours under the heating condition of 50-80 ℃ to obtain a clear transparent solution, namely the hydrophobic eutectic solvent.
(2) Preparation of an organic phase: tributyl phosphate is used as an extracting agent, a hydrophobic eutectic solvent is used as a co-extracting agent and a diluting agent, and the volume fraction change of the hydrophobic eutectic solvent is 10-40%.
(3) Preparation of a lithium-containing water phase: preparing a hydrated lithium chloride solution with the concentration of 0.1g/L, and regulating the pH value of a lithium-containing water phase by regulating the concentration of ammonia water (0.5-2.5 mol/L).
(4) And (3) mixing the organic phase in the step (1) with the lithium-containing water phase in the step (2), extracting for a period of time under violent shaking, and centrifuging and layering to obtain an extract phase and raffinate.
(5) And eluting the obtained extract phase with hydrochloric acid, and centrifuging and layering to obtain a lithium-rich solution.
Example 2
The extraction procedure was the same as in example 1, step 4.
Wherein, the volume of the organic phase is the same as that of the aqueous phase containing lithium, and the hydrophobic eutectic solvents with different molar ratios prepared in step 1 of example 1 have extraction effect on lithium ions under the condition of the lithium-containing solution with the volume fraction of the hydrophobic eutectic solvent in the organic phase being 10% and the ammonia water concentration being 1 mol/L. Wherein when the molar ratio of tetrabutylammonium chloride to oleic acid is 1: 1. 1: 2 and 1: at 3, the corresponding extraction rates were 45%, 52.4% and 63.1%, respectively. When the molar ratio of tetrabutylammonium chloride to oleic acid in the hydrophobic eutectic solvent is 1: and 3, the extraction rate of lithium in the lithium-containing solution is the maximum.
Example 3
The extraction procedure was the same as in example 1, step 4.
Wherein the volume of the organic phase is the same as that of the lithium-containing aqueous phase, and the molar ratio of tetrabutylammonium chloride to oleic acid in the hydrophobic eutectic solvent is 1: 3. under the condition that the volume fraction of the hydrophobic eutectic solvent in the organic phase is 10%, the hydrophobic eutectic solvent has an extraction effect on lithium ions in lithium-containing aqueous phases configured with different ammonia water concentrations. When the concentration of the ammonia water is more than 1.5mol/L, the extraction rate of the hydrophobic eutectic solvent to lithium in the lithium-containing solution is more than 70 percent.
Example 4
The extraction procedure was the same as in example 1, step 4.
Wherein the volume of the organic phase is the same as that of the lithium-containing aqueous phase, and the molar ratio of tetrabutylammonium chloride to oleic acid in the hydrophobic eutectic solvent is 1: 3. under the condition of a lithium-containing solution with the ammonia water concentration of 1.5mol/L in the water phase, when the volume fraction of the hydrophobic eutectic solvent is 10-40%, the eutectic solvent has an extraction effect on lithium ions in the lithium-containing solution. When the volume fraction of the eutectic solvent is more than 10%, the extraction rate of the hydrophobic eutectic solvent to lithium in the lithium-containing solution is more than 70%. The distribution coefficient is increased along with the increase of the using amount of the eutectic solvent, and the distribution coefficient is maximized when the using amount of the eutectic solvent is 30 percent. Continued increase in the volume fraction of the eutectic solvent dilutes the tributyl phosphate extractant concentration, which results in a decrease in extraction yield.
Example 5
The extraction procedure was the same as in example 1, step 4.
Wherein the molar ratio of tetrabutylammonium chloride to oleic acid in the hydrophobic eutectic solvent is 1: 3, the volume fraction of the hydrophobic eutectic solvent in the organic phase is 30%. And (3) carrying out extraction experiments by changing the volume ratio (0.4-1.2) of the organic phase to the aqueous phase under the condition of the lithium-containing solution with the ammonia water concentration of 1.5mol/L in the aqueous phase. The extraction rate of lithium increases with increasing ratio of organic phase to aqueous phase. When the ratio is 1, the extraction rate of lithium in the lithium-containing solution by the hydrophobic eutectic solvent is more than 70%. When the ratio is continuously increased, the extraction ratio of lithium is continuously increased, but the distribution ratio thereof is decreased.
Example 6
The extraction procedure was the same as in example 1, step 4.
Wherein the molar ratio of tetrabutylammonium chloride to oleic acid in the hydrophobic eutectic solvent is 1: 3, the volume fraction of the hydrophobic eutectic solvent in the organic phase is 30%. And mixing the organic phase with the lithium precipitation mother liquor with the same volume for extracting lithium in the lithium precipitation mother liquor. Under the condition of the lithium precipitation mother liquor with the sodium-lithium ratio of 11.3, the ammonia water concentration of the lithium precipitation mother liquor is adjusted to be 1.5mol/L and compared with the lithium precipitation mother liquor without ammonia water addition, and relevant extraction data are listed in Table 1.
TABLE 1 extraction of lithium from lithium precipitation mother liquor based on hydrophobic eutectic solvent extraction system
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (7)
1. A method for selectively extracting and precipitating lithium in lithium mother liquor based on hydrophobic eutectic solvent is characterized in that: the method comprises the following steps:
(1) preparation of hydrophobic eutectic solvent:
mixing the hydrogen bond donor and the hydrogen bond acceptor according to a molar ratio, and stirring for 4-12 hours under a heating condition of 50-80 ℃ to obtain a clear transparent solution; namely a hydrophobic eutectic solvent;
the hydrogen bond donor is oleic acid, and the hydrogen bond acceptor is quaternary ammonium salt;
the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is (1-3): 1;
the quaternary ammonium salt is at least one of tetrabutylammonium chloride, tetrahexylammonium chloride and tetraoctylammonium chloride;
(2) extraction:
forming an organic phase by the hydrophobic eutectic solvent prepared in the step (1) and an extractant tributyl phosphate, mixing the organic phase with a lithium-containing water phase with the pH value regulated by ammonia water, extracting for a period of time under violent oscillation, and centrifuging and layering to obtain an extraction phase and raffinate;
(3) and (3) elution:
and (3) eluting the extract phase obtained in the step (2) with hydrochloric acid, and centrifuging and layering to obtain a lithium-rich solution.
2. The method of claim 1, wherein the molar ratio of hydrogen bond donor to hydrogen bond acceptor is 3: stirring time was 6 hours.
3. The method according to claim 1, wherein in the step (2), the volume fraction of the hydrophobic eutectic solvent in the organic phase is 10-40%.
4. The method of claim 1, wherein in the step (2), the concentration of the aqueous ammonia solution containing lithium in the aqueous phase is 0.5 to 2.5 mol/L.
5. The method of claim 1, wherein in step (2), the volume ratio of the organic phase to the aqueous phase containing lithium is 0.4 to 1.2.
6. The method according to claim 1, wherein the oscillating speed of the vigorous oscillation in the step (2) is 130rpm to 200 rpm.
7. The method according to claim 1, wherein in the step (3), the hydrochloric acid concentration is 0.5 to 2.5mol/L, and the elution time is 20 to 40 minutes.
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| CN112981139B (en) * | 2021-02-04 | 2022-08-16 | 西安建筑科技大学 | Hydrophobic eutectic solvent for separating nickel and cobalt ions, preparation method thereof and method for separating nickel and cobalt ions |
| CN114438343B (en) * | 2022-01-24 | 2023-03-17 | 中国科学院过程工程研究所 | Difunctional hydrophobic eutectic solvent for selectively extracting lithium and preparation method and application method thereof |
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| CN114645144B (en) * | 2022-03-17 | 2023-07-04 | 中国科学院青海盐湖研究所 | Method for extracting lithium by using deep eutectic solvent |
| CN115074551B (en) * | 2022-06-29 | 2023-10-17 | 北京工业大学 | Synergistic extraction method for selectively separating lithium and transition metal from waste battery by using hydrophobic eutectic solvent |
| CN115784273B (en) * | 2022-10-18 | 2024-04-02 | 广东台泉科技股份有限公司 | Multistage lithium carbonate extraction process |
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