CN110723743A - Method for extracting lithium resource from salt lake brine through electric flocculation - Google Patents
Method for extracting lithium resource from salt lake brine through electric flocculation Download PDFInfo
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Abstract
The invention discloses a method for extracting lithium resources from salt lake brine by electric flocculation, which comprises the following steps: (1) adding salt lake brine into an electric flocculation device, and performing electric flocculation reaction and solid-liquid separation to obtain a precipitate I and a tail liquid I; (2) calcining the precipitate I to obtain a calcined product; (3) carrying out leaching reaction on the calcined product, and carrying out solid-liquid separation to obtain a precipitate II and a leaching solution; (4) adding NaOH into the leaching solution for reaction, and performing solid-liquid separation to obtain a magnesium hydroxide product and a lithium-containing solution; (5) and adding sodium carbonate into the lithium-containing solution for reaction, and performing solid-liquid separation to obtain a lithium carbonate product and a tail solution II. The method realizes the efficient extraction of the lithium resource in the salt lake brine, and the alumina solid product produced in the technical process returns to the electric flocculation process for continuous use, thereby greatly reducing the byproduct generation when the salt lake brine with high magnesium-lithium ratio is treated by the traditional precipitation method, and reducing the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of extraction of salt lake lithium resources, and particularly relates to a method for extracting lithium resources from salt lake brine by electric flocculation.
Background
Lithium is widely present in nature in the form of compounds. Lithium resources that can be developed and utilized currently include granite pegmatite lithium minerals, salt lake brine and seawater. The lithium ore resource is mainly existed in salt lake brine and granite pegmatite deposit. Wherein the salt lake lithium resource accounts for 69% of the global lithium reserve and 87% of the global lithium reserve basis. Among the lithium-containing salt lakes of global importance are the Wuynoni salt lake of Bolivia, the Atacama salt lake of Chilean, the Zabuer salt lake and the Carman salt lake of China, the Yinfeng, the Seersi, the Wenbuliemoneto salt lake of Argentina, and the dead sea of the middle east. Lithium resources in brine in China account for 79 percent of the total amount of the lithium resources, and the lithium resources are 27l ten thousand tons in terms of metallic lithium. The reserve of lithium in the brine of the salt lake in the Qinghai and autonomous region of Tibet is equivalent to the reserve found in other countries in the world, and is a world large country for lithium resource reserve. In recent years, researchers in China continuously explore the extraction of lithium resources from salt lake brine, and although certain progress is made, because the type of the salt lake brine in China is unique, the magnesium-lithium ratio in most salt lakes is high, and because the chemical properties of magnesium-lithium ions are similar, the separation is very difficult, and compared with the foreign salt lakes with low magnesium-lithium ratio, the development difficulty of the lithium extraction process in the salt lakes in China is higher.
At present, the technology for extracting lithium from salt lake brine at home and abroad mainly comprises a precipitation method, an adsorption method, a solvent extraction method, a nanofiltration method and the like. The traditional evaporative crystallization precipitation method can generate a large amount of byproducts, is difficult to treat, is easy to cause environmental pollution, is time-consuming in the evaporation process, has low efficiency and is not suitable for extracting lithium from salt lakes with high magnesium-lithium ratio. Although the adsorption method can effectively separate lithium and magnesium in a salt lake with high magnesium-lithium ratio, the adsorbent has low adsorption capacity and poor regeneration capacity. The solvent extraction method uses a large amount of organic extractant, which easily causes influence on the environment. Although the nanofiltration method is regarded as an environment-friendly method for extracting lithium from salt lakes, the problem of membrane pollution of the nanofiltration membrane is not fully solved at present, and the method has high cost. Therefore, aiming at the salt lake brine with high magnesium-lithium ratio, a process method which is simple in process and environment-friendly is developed, so that the efficient extraction of lithium resources in the salt lake brine with high magnesium-lithium ratio is a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for extracting lithium resources from salt lake brine by electroflocculation, which obtains a lithium carbonate product by the process routes of electroflocculation, calcination, leaching and precipitation, realizes the efficient extraction of the lithium resources from the salt lake brine, returns an alumina solid product generated in the process to the electroflocculation process for continuous use, greatly reduces the generation of byproducts when the traditional precipitation method is used for treating the salt lake brine with high magnesium-lithium ratio, and reduces the pollution to the environment.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a method for extracting lithium resources from salt lake brine by electric flocculation comprises the following steps:
(1) adding salt lake brine into an electric flocculation device, and performing electric flocculation reaction and solid-liquid separation to obtain a precipitate I and a tail liquid I;
(2) calcining the precipitate I obtained in the step (1) to obtain a calcined product;
(3) carrying out leaching reaction on the calcined product obtained in the step (2), and carrying out solid-liquid separation to obtain a precipitate II and a leaching solution;
(4) adding NaOH into the leachate obtained in the step (3) for reaction, and carrying out solid-liquid separation to obtain a magnesium hydroxide product and a lithium-containing solution;
(5) and (4) adding sodium carbonate into the lithium-containing solution obtained in the step (4) for reaction, and carrying out solid-liquid separation to obtain a lithium carbonate product and a tail solution II.
Preferably, in the salt lake brine obtained in the step (1), the concentration of lithium ions is 0.2-2.7 g/L, the concentration of magnesium ions is 12-120 g/L, and the mass ratio of the magnesium ions to the lithium ions is 44-600.
In the preferred scheme, in the electric flocculation device in the step (1), the anode plate is an aluminum plate, and the cathode plate is one of an aluminum plate, an iron plate, a stainless steel plate, a graphite plate, a zinc plate, a copper plate and a titanium plate. The anode plate of the invention adopts an aluminum plate,in the process of extracting lithium by electric flocculation, Al is used as an anode reaction process3++Li++Cl-+OH-→LiCl·Al(OH)3·xH2And O, obtaining a precursor for the subsequent calcination process. The inventors have found that when other plates are used as anodes instead of aluminum plates, Al is not generated during the electroflocculation process3+And thus cannot interact with Li in solution+The action gives LiCl. Al (OH)3·xH2O, extraction of lithium was not performed.
Preferably, in the step (1), the electric flocculation reaction is carried out, and the current density is constant and is 30-150 mA/cm2The distance between the polar plates is 1-2 cm, the stirring intensity is 500-1000 r/min, and the reaction time is 90-240 min.
In a preferable scheme, in the step (2), the calcination reaction is carried out at the calcination temperature of 350-500 ℃ for 20-60 min.
In the preferable scheme, in the leaching reaction in the step (3), the leaching temperature is 30-90 ℃, and the liquid-solid ratio is 3: 1-10: 1, the leaching time is 20-100 min.
Preferably, the precipitate II in the step (3) is returned to the step (1) for continuous use.
After the leaching reaction in the step (3), the obtained precipitate II is mainly alumina, the alumina can return to the electrocoagulation process to participate in the reaction, and the process comprises the following steps: al (Al)3++Al2O3+OH-→Al(OH)3，Al(OH)3+LiCl+H2O→LiCl·Al(OH)3·xH2O。
In the invention, the precipitate I is obtained through the electrocoagulation reaction in the step (1), then the precipitate I is calcined in the step (2) to obtain a calcined product, and the Mg in the leachate can be finally controlled after the calcined product obtained in the step (3) is subjected to leaching reaction2+The content of (b) is 0.96-3.6 g/L.
Preferably, in the step (4), the NaOH is added in an amount which is 1.5-2 times of the theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the leachate.
Preferably, in the step (5), sodium carbonate is added into the lithium-containing solution, and the mixture is stirred and reacted for 15-30 min at the temperature of 90-100 ℃.
Preferably, in the step (5), the sodium carbonate is added in an amount of 1.2 to 1.4 times of a theoretical amount required for forming lithium carbonate precipitate from all lithium ions in the lithium-containing solution.
Preferably, in the step (5), the purity of the lithium carbonate product is not lower than 98%.
The invention has the beneficial effects that:
(1) the invention takes salt lake brine with high magnesium-lithium ratio as raw material, and adopts the original electric flocculation lithium extraction technology to precipitate most of lithium to obtain precipitate LiCl. Al (OH)3·xH2And O, calcining and leaching to obtain a lithium-containing solution and solid alumina, and removing a small amount of residual magnesium from the lithium-containing solution to obtain a lithium carbonate product, so that the high-efficiency extraction of lithium resources in the salt lake brine with high magnesium-lithium ratio is realized, and the purity of the lithium carbonate product is not lower than 98%. The method can greatly reduce the generation of solid waste and the pollution to the environment, and the leached solid alumina can be recycled, thereby effectively reducing the cost.
(2) Compared with the traditional lithium extraction process by the aluminum salt precipitation method, the electric flocculation technology can greatly improve the reaction efficiency and shorten the reaction time (1.5-3h), while the traditional aluminum salt precipitation method generally needs to act for 6-7 h; the recovery rate of lithium by an aluminum salt precipitation method is about 75 percent generally, the recovery efficiency is lower, and the recovery rate can reach 90 percent; the aluminum salt precipitation method generally acts under the condition of neutral pH, and the pH adaptability of the method is stronger and is not strictly limited.
In a word, the method has the advantages of high extraction rate of lithium, simple process flow, good filtering performance, effective recycling of alumina slag generated in the process, and very green process.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1
(1) Selecting salt lake brine with high magnesium-lithium ratio in Qinghai, and preparing the brineThe lithium content in the water is 0.28g/L, the magnesium content is 12.76g/L, the magnesium-lithium ratio is 45.6, the anode plate and the cathode plate of the electric flocculation device are aluminum plates, and the current density is 80mA/cm2The pH value is 5.6, the distance between polar plates is 1cm, the stirring intensity is 750r/min, and after the electrolytic reaction is carried out for 150min, the tail liquid I and the sediment are obtained through solid-liquid separation.
(2) Calcining the precipitate in the step (1) at 450 ℃ for 30min, wherein the liquid-solid ratio of the calcined product at 40 ℃ is 5: 1, leaching for 30min, filtering and separating to obtain alumina slag and lithium-containing solution.
(3) And (3) detecting that the lithium-containing solution in the step (2) still contains 2.5g/L magnesium impurities, adding NaOH into the lithium-containing solution, wherein the addition amount of the NaOH is 13g/L (the added NaOH is 1.6 times of the required theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the mother liquor), reacting, filtering and separating to obtain crude magnesium hydroxide and a solution I.
(4) And (4) adding sodium carbonate into the solution I from which the magnesium impurities are removed in the step (3), wherein the added sodium carbonate is 1.3 times of the theoretical amount of lithium carbonate formed by all lithium ions in the solution I through precipitation, controlling the temperature to be 95 ℃, and filtering and separating to obtain a lithium carbonate product after stirring and reacting for 20 min. The recovery rate of lithium in the obtained product was 88%, and the purity of the obtained lithium carbonate product was 98.3%.
Example 2
(1) Selecting salt lake brine with high Mg/Li ratio in Xinjiang, wherein the Li content in the brine is 2.1g/L, the Mg content is 113.6g/L, the Mg/Li ratio is 54.1, an anode plate of the electric flocculation device is an aluminum plate, a cathode plate of the electric flocculation device is an iron plate, and the current density is 150mA/cm2The pH value is 6, the distance between polar plates is 1.5cm, the stirring intensity is 800r/min, and after the electrolytic reaction is carried out for 180min, the tail liquid I and the sediment are obtained through solid-liquid separation.
(2) Calcining the precipitate in the step (1) at 400 ℃ for 50min, wherein the liquid-solid ratio of the calcined product at 60 ℃ is 8: 1, leaching for 50min, filtering and separating to obtain alumina slag and a lithium-containing solution.
(3) And (3) detecting that the lithium-containing solution in the step (2) still contains 3.3g/L magnesium impurities, adding 19g/L NaOH (the added NaOH is 1.8 times of the required theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the mother liquor) into the lithium-containing solution, reacting, filtering and separating to obtain crude magnesium hydroxide and a solution I.
(4) And (4) adding sodium carbonate into the solution I from which the magnesium impurities are removed in the step (3), wherein the added sodium carbonate is 1.4 times of the theoretical amount of lithium carbonate formed by all lithium ions in the solution I through precipitation, controlling the temperature to be 90 ℃, and filtering and separating to obtain a lithium carbonate product after stirring and reacting for 25 min. The recovery rate of lithium in the obtained product was 89%, and the purity of the obtained lithium carbonate product was 98.1%.
Example 3
(1) Selecting salt lake brine with high Mg/Li ratio in Tibet, wherein the Li content in the brine is 1.5g/L, Mg content is 60g/L, Mg/Li ratio is 40, anode plate of the electric flocculation device is aluminum plate, cathode plate is graphite plate, and current density is 115mA/cm2The pH value is 7, the distance between polar plates is 1cm, the stirring intensity is 700r/min, and after the electrolytic reaction is carried out for 150min, the tail liquid I and the sediment are obtained through solid-liquid separation.
(2) Calcining the precipitate in the step (1) at 500 ℃ for 40min, wherein the liquid-solid ratio of the calcined product at 50 ℃ is 10: 1, leaching for 30min, filtering and separating to obtain alumina slag and lithium-containing solution.
(3) And (3) detecting that the lithium-containing solution in the step (2) still contains 3g/L magnesium impurities, adding NaOH into the lithium-containing solution, wherein the adding amount of the NaOH is 14g/L (the added NaOH is 1.5 times of the required theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the mother liquor), reacting, filtering and separating to obtain crude magnesium hydroxide and a solution I.
(4) And (4) adding sodium carbonate into the solution I from which the magnesium impurities are removed in the step (3), wherein the added sodium carbonate is 1.2 times of the theoretical amount of lithium carbonate formed by all lithium ions in the solution I through precipitation, controlling the temperature to be 90 ℃, and filtering and separating to obtain a lithium carbonate product after stirring and reacting for 20 min. The recovery rate of lithium in the obtained product is 90%, and the purity of the obtained lithium carbonate product is 98.2%.
Comparative example 1
(1) Selecting salt lake brine with high magnesium-lithium ratio in Qinghai, wherein the lithium content in the brine is 2g/L, the magnesium content is 60g/L, the magnesium-lithium ratio is 30, an anode plate of an electric flocculation device is an aluminum plate, and a cathode plate of the electric flocculation device is an aluminum plateIs a graphite plate with a current density of 20mA/cm2The pH value is 7, the distance between polar plates is 1cm, the stirring intensity is 500r/min, and after the electrolytic reaction is carried out for 60min, the tail liquid I and the sediment are obtained through solid-liquid separation.
(2) Calcining the precipitate in the step (1) at 400 ℃ for 30min, wherein the liquid-solid ratio of the calcined product at 50 ℃ is 8: 1, leaching for 20min, and filtering and separating to obtain alumina slag and a lithium-containing solution.
(3) And (3) detecting that the lithium-containing solution in the step (2) still contains 1.2g/L magnesium impurities, adding NaOH (the added NaOH is 1.6 times of the required theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the mother liquor) into the lithium-containing solution, reacting, filtering and separating to obtain crude magnesium hydroxide and a solution I.
(4) And (4) adding sodium carbonate into the solution I from which the magnesium impurities are removed in the step (3), wherein the added sodium carbonate is 1.25 times of the theoretical amount required by lithium carbonate formed by all lithium ions in the solution I through precipitation, controlling the temperature to be 95 ℃, stirring for reaction for 30min, and filtering and separating to obtain a lithium carbonate product. The recovery rate of lithium in the obtained product was 30%, and the purity of the obtained lithium carbonate product was 98.1%.
Comparative example 2
(1) Selecting salt lake brine with high Mg/Li ratio in Xinjiang, wherein the Li content in the brine is 1g/L, the Mg content is 80g/L, the Mg/Li ratio is 80, an anode plate and a cathode plate of an electric flocculation device are aluminum plates, and the current density is 200mA/cm2The pH value is 6.5, the distance between polar plates is 1.5cm, the stirring intensity is 600r/min, and after 90min of electrolytic reaction, tail liquid I and sediment are obtained through solid-liquid separation.
(2) Calcining the precipitate in the step (1) at 450 ℃ for 30min, wherein the liquid-solid ratio of the calcined product at 60 ℃ is 9: 1, leaching for 30min, filtering and separating to obtain alumina slag and lithium-containing solution.
(3) And (3) detecting that the lithium-containing solution in the step (2) still contains 12g/L of magnesium impurities, adding NaOH (the added NaOH is 1.7 times of the required theoretical amount of magnesium hydroxide precipitate formed by all magnesium ions in the mother liquor) into the lithium-containing solution, reacting, filtering and separating to obtain crude magnesium hydroxide and a solution I.
(4) And (4) adding sodium carbonate into the solution I from which the magnesium impurities are removed in the step (3), wherein the added sodium carbonate is 1.3 times of the theoretical amount of lithium carbonate formed by all lithium ions in the solution I through precipitation, controlling the temperature to be 95 ℃, stirring for reaction for 30min, and filtering and separating to obtain a lithium carbonate product. The recovery rate of lithium in the obtained product was 85%, and the purity of the obtained lithium carbonate product was 98.3%.
Claims (10)
1. A method for extracting lithium resources from salt lake brine through electric flocculation is characterized by comprising the following steps:
(1) adding salt lake brine into an electric flocculation device, and performing electric flocculation reaction and solid-liquid separation to obtain a precipitate I and a tail liquid I;
(2) calcining the precipitate I obtained in the step (1) to obtain a calcined product;
(3) carrying out leaching reaction on the calcined product obtained in the step (2), and carrying out solid-liquid separation to obtain a precipitate II and a leaching solution;
(4) adding NaOH into the leachate obtained in the step (3) for reaction, and carrying out solid-liquid separation to obtain a magnesium hydroxide product and a lithium-containing solution;
(5) and (4) adding sodium carbonate into the lithium-containing solution obtained in the step (4) for reaction, and carrying out solid-liquid separation to obtain a lithium carbonate product and a tail solution II.
2. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: in the salt lake brine obtained in the step (1), the concentration of lithium ions is 0.2-2.7 g/L, the concentration of magnesium ions is 12-120 g/L, and the mass ratio of the magnesium ions to the lithium ions is 44-600.
3. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: in the electric flocculation device in the step (1), the anode plate is an aluminum plate, and the cathode plate is one of an aluminum plate, an iron plate, a stainless steel plate, a graphite plate, a zinc plate, a copper plate and a titanium plate.
4. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: step (ii) of(1) The electric flocculation reaction has constant current density of 30-150 mA/cm2The distance between the polar plates is 1-2 cm, the stirring intensity is 500-1000 r/min, and the reaction time is 90-240 min.
5. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: and (3) carrying out the calcination reaction in the step (2), wherein the calcination temperature is 350-500 ℃, and the calcination time is 20-60 min.
6. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: and (3) carrying out leaching reaction, wherein the leaching temperature is 30-90 ℃, and the liquid-solid ratio is 3: 1-10: 1, the leaching time is 20-100 min.
7. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: and (4) returning the precipitate II in the step (3) to the step (1) for continuous use.
8. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: in the step (4), the NaOH is added according to 1.5-2 times of the theoretical amount required for forming magnesium hydroxide precipitates by all magnesium ions in the leachate.
9. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: in the step (5), sodium carbonate is added into the lithium-containing solution, and the mixture is stirred and reacted for 15-30 min at the temperature of 90-100 ℃.
10. The method for extracting the lithium resource from the salt lake brine through the electric flocculation, according to claim 1, is characterized in that: in the step (5), the sodium carbonate is added in an amount which is 1.2 to 1.4 times of the theoretical amount required for forming lithium carbonate precipitate by all lithium ions in the lithium-containing solution.
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| CN114854986A (en) * | 2022-05-24 | 2022-08-05 | 四川顺应锂材料科技有限公司 | Method for producing lithium carbonate by leaching spodumene ore with nitric acid |
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2019
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| 施悦等: "《环境氧化还原处理技术原理与应用》", 31 August 2013 * |
| 肖小玲: ""氢氧化铝沉淀法从卤水中提取锂的研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑（电子期刊）》 * |
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| CN114854986A (en) * | 2022-05-24 | 2022-08-05 | 四川顺应锂材料科技有限公司 | Method for producing lithium carbonate by leaching spodumene ore with nitric acid |
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Application publication date: 20200124 |