CN114196840A - Method for extracting lithium from high-sodium lithium-containing brine - Google Patents
Method for extracting lithium from high-sodium lithium-containing brine Download PDFInfo
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- CN114196840A CN114196840A CN202111450265.8A CN202111450265A CN114196840A CN 114196840 A CN114196840 A CN 114196840A CN 202111450265 A CN202111450265 A CN 202111450265A CN 114196840 A CN114196840 A CN 114196840A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for extracting lithium from high-sodium lithium-containing brine, in particular to a method for extracting lithium from the high-sodium lithium-containing solution with high yield and reducing the sodium-lithium ratio of desorption solution, which is used for optimizing a leaching process for extracting lithium from brine of an aluminum adsorbent, and comprises the following steps: passing the high-sodium lithium-containing solution through a resin column filled with an aluminum adsorbent; passing the salt solution containing divalent cations through an adsorption-treated resin column; making the leaching water flow through a resin column subjected to pre-washing treatment; enabling the desorbent to flow through the resin column subjected to leaching treatment, and collecting the lithium-rich desorption solution; and (4) enabling the high-salt solution to flow through the resin column subjected to desorption treatment, and collecting the top material effluent. The invention realizes the high-yield extraction of lithium from the high-sodium lithium-containing solution, reduces the sodium-lithium ratio in the desorption solution, provides operational feasibility for further purification and concentration of the desorption solution and reduces energy consumption.
Description
Technical Field
The invention relates to a method for extracting lithium from high-sodium lithium-containing brine, in particular to a method for extracting lithium from the high-sodium lithium-containing solution with high yield and reducing the sodium-lithium ratio of desorption solution, which is used for optimizing a leaching process for extracting lithium from brine of an aluminum adsorbent
Background
Lithium is the lightest alkali metal with the smallest radius in the nature and has active chemical property, and lithium and compounds thereof are widely applied to the fields of aviation, medicine, chemical industry, national defense, new energy and the like and are called as 'important elements for promoting the world to advance'. The lithium yield influences the development of new industries to a certain extent, and restricts the generation of new technologies, so that the lithium product consumption is generally used as an important index for evaluating the national high and new technology industry level internationally.
At present, through detection, the lithium resource of the Qinghai salt lake is programmed into as many as 10 places of the district with abundant mineral reserves, but the main mining districts are a Riping salt lake, a West Ginell salt lake, a Carl sweat area of the Carl sweat lake, a Pilerian beach area, a Dachadan lake and a east Ginell salt lake due to geological environment, climatic environment and the like.
The technological process for extracting lithium from salt lake brine mainly comprises solvent extraction method, adsorption method, calcination leaching method, membrane separation method and the like. The solvent extraction method has high recovery rate, but has long flow, serious equipment corrosion and high cost, and is difficult to realize industrialization. The lithium extraction process by the calcining method is a high energy consumption process, a large amount of hydrogen chloride gas can be generated in the calcining process, equipment can be seriously corroded, the environmental protection pressure is high, the lithium yield is low, a large amount of waste residues can be generated, the development concept of green economy is violated, and the process faces elimination. The lithium extraction technology from brine is applied to both east Ginell and west Ginell in Qinghai salt lake of 2007 and 2011, and later, due to serious equipment corrosion, high cost and the like, a calcining method completely exits the historical stage of the east Ginell salt lake, and the west Ginell salt lake is applied again after 2016 is completely changed. The membrane separation method has the advantages of good separation effect, no discharge of waste residues, waste and wastewater, environmental protection, no dangerous operation in the process and low production cost. The limitation is the high requirements on the quality and performance of the membrane and the quality of the brine. The lithium extracting process with adsorption process has lithium ion adsorbing material as adsorbent, and the operation principle is that the lithium ion in bittern is adsorbed onto the adsorbing material, the lithium ion is eluted from the adsorbing material with eluent, the lithium ion and impurity are separated, and the eluent containing lithium ion is concentrated to obtain convertible lithium resource. The adsorption method is not limited by the grade of brine, has strong applicability, and has the advantages of simple operation, environmental protection, high safety and the like.
In the prior art, the problems of low separation efficiency and low lithium extraction yield exist in the separation process of the adsorption method of the lithium-containing brine with high sodium content.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: when the lithium-containing brine with high sodium content is separated by adopting an aluminum adsorbent through an adsorption method, the sodium-lithium ion separation coefficient in the obtained material is not high and the lithium loss is more after elution separation.
The technical means of the invention is to pre-elute the adsorbent after adsorption by adopting the brine with higher divalent cation content, and the brine is found to be capable of effectively inhibiting the dissolution of lithium ions in the elution process, simultaneously carrying away redundant sodium ions on the surface of the adsorbent, and reducing the sodium/lithium ratio of the eluent when subsequent elution is carried out, so that the lithium yield is improved.
The technical scheme is as follows:
a method for extracting lithium from high-sodium lithium-containing brine comprises the following steps:
step 1, adopting an aluminum adsorbent to adsorb high-sodium lithium-containing brine;
step 2, pre-leaching the adsorbent in the step 1 by using a solution containing a divalent cation salt;
and 3, eluting lithium ions from the adsorbent obtained in the step 2 by using an eluent to obtain an eluent.
In one embodiment, the high-sodium lithium-containing brine is salt lake brine, lithium precipitation mother liquor (mother liquor obtained by performing lithium carbonate precipitation separation on a lithium-containing raw material), oil field or gas high-sodium lithium-containing brine paddy field brine, concentrated seawater or salt making mother liquor.
In one embodiment, the lithium ion and sodium ion concentrations in the high-sodium lithium-containing solution are 0.01-5.0 g/L and 20.0-120.0 g/L, respectively.
In one embodiment, in the step 1, the adsorption flow rate is 1-50 BV/h.
In one embodiment, the aluminum-based adsorbent component comprises mLiCl 2Al (OH)3·nH2O; m and n are the number of molecules.
In one embodiment, in step 2, the divalent cation is selected from Mg2+、Ca2+Or Fe2+(ii) a The concentration of the divalent cations is 15-70 g/L, and the concentration of the divalent cations is more preferably 15-50 g/L.
In one embodiment, in the step 2, the pre-leaching flow rate is 1-10 BV/h.
In one embodiment, the solution containing the divalent cation salt is selected from one or more of a magnesium chloride solution, a calcium chloride solution, a tail solution after lithium extraction from old brine, old brine and a brine nanofiltration concentrated solution.
In one embodiment, the method further comprises a step 4, wherein after the elution in the step 3 is completed, the adsorption resin is back-washed by high-salt water and the discharged material is collected to be used as top material effluent.
In one embodiment, between the step 2 and the step 3, the method further comprises the step of leaching the adsorption resin; the adopted leacheate is selected from one or more of pure water, tap water, industrial fresh water and top material effluent; the flow of the leaching water is 1-10 BV/h.
In one embodiment, the desorbent comprises one or more mixtures of pure water, tap water, industrial fresh water, and top-feed effluent; the desorption flow is 2-30 BV/h.
In one embodiment, the ejection effluent refers to that after the elution in the step 3 is completed, high-salt water is used for carrying out back flushing on the adsorption resin and collecting the discharged material to be used as ejection effluent; the material ejection flow is 0.5-5 BV/h; and the material ejection adopts a mode of downward feeding and upward discharging.
In one embodiment, the high salt water is selected from one or more of the adsorption tail solution obtained in the step 1, old brine, concentrated seawater, raw brine, sodium chloride solution, potassium chloride solution, magnesium chloride solution or calcium chloride solution.
In one embodiment, the mass ratio of sodium to lithium in the eluent obtained in step 3 is 0.1-1.5.
In one embodiment, the operation temperature in the adsorption treatment in step 1, the pre-leaching treatment in step 2, and the elution treatment in step 3 is 0 to 80 ℃.
Advantageous effects
The method has the advantages that the salt solution of divalent cations is used for pre-leaching the resin column for adsorbing lithium ions, so that desorption of the adsorbent can be inhibited in the washing process, monovalent cations remained on the surface and in the adsorbent can be removed, and the loss of lithium in the leaching process is reduced, thereby improving the lithium concentration in desorption solution, reducing the concentration of other monovalent cations and solving the problem of extracting lithium from the high-sodium lithium-containing solution.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a process flow diagram in comparative example 2;
Detailed Description
The invention relates to a method for extracting lithium from a high-sodium lithium-containing solution with high yield and reducing the sodium-lithium ratio of a desorption solution, in particular to a method for optimizing a leaching process of a lithium extraction adsorbent, so that the sodium-lithium ratio in the desorption solution is reduced and the high lithium recovery rate is kept.
Example 1
In the embodiment, certain salt lake brine is adopted as a raw material, and the concentrations of lithium ions and sodium ions in the brine are respectively 4.9g/L and 90.5 g/L. Feeding the salt lake brine into a resin column filled with an aluminum adsorbent at 5 ℃ according to the ratio of 1BV/h for adsorption, and collecting adsorption tail liquid; feeding tail liquid obtained after lithium extraction from old brine into the column for prewashing according to the flow rate of 10BV/h, wherein the concentration of magnesium ions in the tail liquid obtained after lithium extraction from the old brine is 20.5 g/L; leaching the pre-washed resin column by pure water at a rate of 10 BV/h; then desorbing the solution by pure water with the flow of 30BV/h, and collecting the lithium-containing desorption solution; feeding the adsorption tail liquid from the bottom of the resin column at 0.5BV/h, and collecting the top material effluent discharged from the top of the resin column, wherein the top material effluent is used for leaching or desorbing the resin column. The operation process of this embodiment is shown in fig. 1.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Example 2
In the embodiment, a certain lithium precipitation mother liquor is used as a raw material, and the concentrations of lithium ions and sodium ions in brine are 1.2g/L and 76.1g/L respectively. Feeding the lithium precipitation mother liquor into a resin column filled with an aluminum adsorbent at the temperature of 80 ℃ according to the ratio of 5BV/h for adsorption, and collecting adsorption tail liquor; feeding calcium chloride solution with calcium ion concentration of 50g/L into the column according to the flow rate of 1BV/h for prewashing; leaching the pre-washed resin column by using tap water at a rate of 1 BV/h; then desorbing the solution by using tap water with the flow of 2BV/h, and collecting the desorption solution containing lithium; and feeding the adsorption tail liquid from the bottom of the resin column at 5BV/h, and collecting the top material effluent discharged from the top of the resin column, wherein the top material effluent is used for leaching or desorbing the resin column.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Example 3
In the embodiment, certain oil field brine is adopted as a raw material, and the concentrations of lithium ions and sodium ions in the brine are respectively 0.2g/L and 118.5 g/L. Feeding the oil field brine into a resin column filled with an aluminum adsorbent at the temperature of 20 ℃ at a rate of 25BV/h for adsorption, and collecting adsorption tail liquid; feeding the brine nanofiltration concentrated solution into the column for prewashing according to the flow rate of 5BV/h, wherein the calcium ion concentration of the brine nanofiltration concentrated solution is 15.2 g/L; leaching the pre-washed resin column by using industrial fresh water at 6 BV/h; then, desorbing the solution by using industrial fresh water with the flow rate of 15BV/h, and collecting the desorption solution containing lithium; and feeding the adsorption tail liquid from the bottom of the resin column at 3BV/h, and collecting the top material effluent discharged from the top of the resin column, wherein the top material effluent is used for leaching or desorbing the resin column.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Example 4
In the embodiment, certain concentrated seawater is used as a raw material, and the concentrations of lithium ions and sodium ions in the brine are 0.01g/L and 20.5g/L respectively. Feeding the concentrated seawater into a resin column filled with aluminum adsorbent at 25 deg.C at a rate of 50BV/h for adsorption, and collecting adsorption tail liquid; feeding magnesium chloride solution with the magnesium ion concentration of 30g/L into the column for prewashing according to the flow rate of 3 BV/h; leaching the pre-washed resin column by using a mixed solution of pure water and the top material outlet water at a rate of 6 BV/h; then desorbing the solution by pure water with the flow rate of 10BV/h, and collecting the lithium-containing desorption solution; and feeding the adsorption tail liquid from the bottom of the resin column at 2BV/h, and collecting the top material effluent discharged from the top of the resin column, wherein the top material effluent is used for leaching or desorbing the resin column.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Example 5
In the embodiment, a certain salt making mother liquor is used as a raw material, and the concentrations of lithium ions and sodium ions in brine are 1.5g/L and 50.3g/L respectively. Feeding the salt-making mother liquor into a resin column filled with an aluminum adsorbent for adsorption at 15 ℃ according to the ratio of 4.5BV/h, and collecting adsorption tail liquor; feeding the old halogen solution into the column for prewashing according to the flow rate of 2BV/h, wherein the concentration of old halogen magnesium ions is 49.1 g/L; leaching the pre-washed resin column by using industrial fresh water at 3 BV/h; then desorbing by using a mixed solution of pure water and the top material effluent, wherein the flow rate is 15BV/h, and collecting a lithium-containing desorption solution; and feeding the adsorption tail liquid from the bottom of the resin column at 2BV/h, and collecting the top material effluent discharged from the top of the resin column, wherein the top material effluent is used for leaching or desorbing the resin column.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Example 6
This example differs from example 1 in that the amount of pre-wash water is halved. Other conditions were exactly the same as in example 1.
Comparative example 1
This example differs from example 1 in that pure water was fed to the column at a flow rate of 10BV/h for prewashing. Other conditions were exactly the same as in example 1.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
Comparative example 2
This example differs from example 1 in that there is no prewash step. Other conditions were exactly the same as in example 1.
The lithium recovery rate and the partial ion concentration in the lithium-containing desorption solution of this example are shown in Table 1.
The experimental data for each example are summarized in the following table:
TABLE 1
As can be seen from the comparison of example 6 with example 1, the yield of lithium obtained can be kept unchanged after reducing the amount of pre-leaching, but results in a large increase in the sodium/lithium ratio, since sodium cannot be sufficiently eluted and removed while suppressing desorption of lithium; as can be seen from comparison between comparative example 1 and example 1, elution of lithium cannot be effectively inhibited without adding a divalent salt in the pre-leaching process, and although the final sodium-lithium ratio can be maintained at a low level, the lithium yield is greatly reduced; as can be seen from comparison between comparative example 2 and example 1, the yield of lithium was maintained without pre-rinsing, but sodium ions remained on the aluminum adsorbent could not be effectively removed, and the problem of high sodium-lithium ratio after elution still existed.
Claims (10)
1. A method for extracting lithium from high-sodium lithium-containing brine is characterized by comprising the following steps:
step 1, adopting an aluminum adsorbent to adsorb high-sodium lithium-containing brine;
step 2, pre-leaching the adsorbent in the step 1 by using a solution containing a divalent cation salt;
and 3, eluting lithium ions from the adsorbent obtained in the step 2 by using an eluent to obtain an eluent.
2. The method of claim 1, wherein the high-sodium lithium-containing brine is salt lake brine, lithium precipitation mother liquor, oil field or gas high-sodium lithium-containing brine paddy field brine, concentrated seawater or salt making mother liquor.
3. The method of claim 1, wherein the concentrations of lithium ions and sodium ions in the high-sodium lithium-containing brine are 0.01-5.0 g/L and 20.0-120.0 g/L, respectively.
4. The method for extracting lithium from the high-sodium lithium-containing brine according to claim 1, wherein in the step 1, the adsorption flow rate is 1-50 BV/h; the aluminum adsorbent component comprises mLiCl 2Al (OH)3·nH2O; m and n are the number of molecules.
5. The method of claim 1, wherein in step 2, the divalent cations are selected from Mg2+、Ca2+Or Fe2+(ii) a The concentration of the divalent cations is between 15 and 70g/L, and the concentration of the divalent cations is more preferably between 15 and 50 g/L; in the step 2, the pre-leaching flow is 1-10 BV/h.
6. The method of claim 1, wherein the solution containing divalent cation salts is selected from the group consisting of magnesium chloride solution, calcium chloride solution, tail solution after lithium extraction from old brine, old brine and one or more mixtures of brine nanofiltration concentrate.
7. The method of claim 1, further comprising a step 4, wherein after the elution in the step 3 is completed, the adsorption resin is back-washed with high-salt water and the discharged material is collected as top water.
8. The method for extracting lithium from the lithium-rich brine as claimed in claim 7, wherein between the step 2 and the step 3, the method further comprises a step of rinsing the adsorption resin; the adopted leacheate is selected from one or more of pure water, tap water, industrial fresh water and top material effluent; the flow of the leaching water is 1-10 BV/h; the desorbent comprises one or more of pure water, tap water, industrial fresh water and top-material effluent; the desorption flow is 2-30 BV/h; the ejection water outlet means that after the elution in the step 3 is finished, high-salt water is adopted to carry out reverse flushing on the adsorption resin, and the collected material is discharged and is used as ejection water outlet; the material ejection flow is 0.5-5 BV/h; and the material ejection adopts a mode of downward feeding and upward discharging.
9. The method of claim 1, wherein the brine is selected from one or more of the adsorption tail solution, old brine, concentrated seawater, raw brine, sodium chloride solution, potassium chloride solution, magnesium chloride solution, and calcium chloride solution obtained in step 1.
10. The method for extracting lithium from the lithium-rich brine containing high sodium content according to claim 1, wherein the mass ratio of sodium to lithium in the eluent obtained in the step 3 is 0.1-1.5; the operation temperature in the adsorption treatment in the step 1, the pre-leaching treatment in the step 2 and the elution treatment in the step 3 is 0-80 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114702049A (en) * | 2022-04-11 | 2022-07-05 | 西安蓝深新材料科技有限公司 | Equipment and method for recovering lithium from lithium-containing mother liquor in lithium carbonate preparation process |
| CN115124053A (en) * | 2022-07-19 | 2022-09-30 | 浙江新锂想科技有限责任公司 | Method for extracting and preparing lithium product from lepidolite by adopting composite adsorption resin |
| CN116037222A (en) * | 2023-01-13 | 2023-05-02 | 格尔木藏格锂业有限公司 | Method for extracting lithium by efficient continuous ion exchange |
| CN116287780A (en) * | 2023-03-28 | 2023-06-23 | 中国科学院过程工程研究所 | Method for extracting lithium from oil-gas field brine |
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