WO2017005113A1 - Procédé d'extraction de lithium dans de la saumure de lac salé - Google Patents

Procédé d'extraction de lithium dans de la saumure de lac salé Download PDF

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Publication number
WO2017005113A1
WO2017005113A1 PCT/CN2016/087443 CN2016087443W WO2017005113A1 WO 2017005113 A1 WO2017005113 A1 WO 2017005113A1 CN 2016087443 W CN2016087443 W CN 2016087443W WO 2017005113 A1 WO2017005113 A1 WO 2017005113A1
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lithium
magnesium
liquid
low
water
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PCT/CN2016/087443
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English (en)
Chinese (zh)
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杨发平
刘炳生
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青海恒信融锂业科技有限公司
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates

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  • the present disclosure relates to the field of membrane separation technology, and more particularly to a method of extracting lithium from salt lake water in combination with a chemical precipitation method and a membrane separation method.
  • Lithium-ion batteries are widely used in mobile communication equipment and various digital products because of their outstanding specific capacity, wide operating temperature range, low self-discharge rate, long cycle life and good safety performance. It is an ideal power source for electric vehicles. Therefore, even if the global economic growth slows down in recent years, the performance of the lithium industry is particularly prominent. Lithium products are one of the few industrial products with rising prices. Therefore, the acquisition of lithium resources has become a hot spot in the world.
  • Embodiments of the present invention provide a method for separating and extracting lithium from brine, comprising:
  • At least one of the high magnesium low lithium product water of the above step 3 and the light liquid of the step 4 may be returned to the second clear liquid of the step 2.
  • step 2 of the pretreatment comprises steps 2A and 2B
  • step 2A comprises: adjusting the pH of the first supernatant of step 1 to 7-9, SO 4 in the brine
  • a part of 2- and Mg 2+ is precipitated in the form of calcium sulfate and magnesium hydroxide.
  • step 2B includes: returning the supernatant with the subsequent step.
  • step 3 of lithium magnesium separation comprises step 3A and step 3B
  • step 3A comprises: adding acid to the supernatant obtained in step 2, adjusting the pH to 7-8.5, using lithium magnesium separation Membrane separation clear liquid obtains high magnesium and low lithium water production 3A and high lithium low magnesium water production 3A, wherein high magnesium and low lithium water production 3A is returned to the salt field for concentration and enrichment, and then combined with raw material brine, high lithium and low magnesium water production 3A Go to step 3B to continue the process or proceed to step 4 to continue the process;
  • step 3B includes: adding a complexing agent to the high-lithium and low-magnesium water-producing water 3A, and separating the high-lithium and low-magnesium water-producing water 3A by using the lithium-magnesium separation membrane to obtain high-magnesium and low-lithium water-producing water.
  • step 3B high-lithium and low-magnesium produced water 3B, wherein the high-magnesium-low-lithium product water 3B returns to the supernatant of step 2A, and the high-lithium low-magnesium produced water 3B proceeds to step 4 to continue the treatment.
  • step 4 of lithium concentration includes step 4A, step 4B, and step 4C, and step 4A includes: concentrating the high-lithium and low-magnesium produced water of step 3 with a lithium concentration membrane to obtain a concentration.
  • step 4B includes: using the lithium concentrated membrane for the concentrated liquid of step 4A 4A is concentrated to obtain a concentrate 4B and a light liquid 4B, wherein the light liquid 4B is returned to be combined with the clear liquid of the step 2A, the concentrated liquid 4B is further advanced to the step 4C or the processing proceeds to the step 5;
  • step 4C includes: using the lithium concentrated film
  • the concentrate 4B of the step 4B is concentrated to obtain a concentrate 4C and a light liquid 4C, wherein the light liquid 4C is returned to the supernatant of the step 2A, and the concentrate 4C is advanced to the step 5 to continue the treatment.
  • the acid removal of the step 1 of the above step comprises: adding acid to adjust the pH of the salt lake brine to 2-4 to precipitate crystals of boric acid, solid-liquid separation to obtain a clear liquid and crude boric acid.
  • the above step 2B comprises: adding a filter aid to the supernatant 2A, and combining the remaining supernatants of the subsequent steps, the remaining SO 4 2- and Mg 2+ in the brine A part of the mixture was continuously precipitated in the form of calcium sulfate and magnesium hydroxide, and the CaSO 4 and Mg(OH) 2 flocs were separated by a polytetrafluoroethylene microfiltration membrane to obtain a clear liquid 2B, and the treatment was continued in step 3.
  • the above-mentioned high magnesium and low lithium water production 3A lithium ion concentration
  • the degree is less than 150ppm
  • the lithium ion concentration in the high lithium and low magnesium water production 3A is more than 300ppm
  • the lithium ion concentration in the high lithium and low magnesium water production 3B is more than 300ppm
  • the lithium to magnesium mass ratio is greater than 1.
  • the concentration of lithium ions in the concentrated liquid 4A is greater than 1000 ppm and the mass ratio of lithium to magnesium is greater than 1; the concentration of lithium ions in the concentrated solution 4B is greater than 2000 ppm and the mass ratio of lithium to magnesium is greater than 1; The medium lithium ion concentration is greater than 16000 ppm and the lithium to magnesium mass ratio is greater than 1.
  • the manner of adjusting the pH of the first supernatant of step 1 comprises adding NaOH, NH 4 OH, KOH or Ca(OH) 2 .
  • the filter aid is perlite, diatomaceous earth or cellulose, and the filter aid is added in an amount of 30-50 ppm.
  • the acid added to the supernatant obtained in step 2 includes one of hydrochloric acid, sulfuric acid, nitric acid, or a combination thereof.
  • the complexing agent added in the high lithium low magnesium product water 3A is a compound EDTA sodium salt, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid. Salt, aminotrimethylenephosphonic acid, diethylenetriaminepentamethylenephosphonic acid, hydroxyethylidene diphosphonic acid or sodium hexametaphosphate, at a concentration of 3-6 ppm.
  • the method for obtaining the clear liquid in the step 5 is: adding sodium hydroxide to the concentrated liquid of the step 4 to obtain a slurry, and a part of the Mg 2+ in the slurry is Mg ( Precipitation in the form of OH) 2 , solid-liquid separation of the above slurry to obtain magnesium hydroxide precipitate and a leachate, magnesium hydroxide precipitation and more than one leaching with water or filtrate, solid-liquid separation to obtain magnesium hydroxide precipitate and filtrate, This filtrate was used to configure sodium hydroxide to continue to be reused, and a leachate was filtered to obtain a clear solution.
  • the method of solid-liquid separation includes high speed centrifugation, plate and frame solid-liquid separation, polytetrafluoroethylene microfiltration membrane separation and/or filtration.
  • FIG. 1 is a flow chart of a method for separating and extracting lithium from brine in accordance with an embodiment of the present invention
  • FIG. 2 is a flow chart of a method for separating and extracting lithium from brine in accordance with still another embodiment of the present invention.
  • FIG. 3 is a flow chart of a method for separating and extracting lithium from brine according to a third embodiment of the present invention.
  • FIG. 4 is a flow chart of a method for separating and extracting lithium from brine in accordance with a fourth embodiment of the present invention.
  • ppm is a mass ratio
  • Chinese has the same meaning as chemical formula, such as magnesium ion and Mg 2+ , sulfate ion and SiO 4 2- .
  • lithium brine resources accounted for 61%, ore lithium resources accounted for 34%, and oil and geothermal water lithium resources accounted for 5%.
  • lithium extraction from salt lake brines is superior to ore extraction in terms of cost and scale.
  • 70% of the world's lithium products come from salt lake brines.
  • China's salt lake brine lithium accounted for more than 80% of the total reserves, however, lithium extracted from salt lake brines only accounted for 8% of the total extraction, for a variety of reasons. The main reason is that China's salt lake brine is mostly high-magnesium-lithium brine.
  • the direct extraction of lithium, the current methods for extracting lithium from high magnesium lithium than brine include organic solvent extraction, ion exchange, electrodialysis, nanofiltration membrane and the like.
  • the organic solvent extraction method has high production cost and serious corrosion to equipment, and is still in the experimental stage; the adsorbent used in the ion exchange method has high price, low productivity, and is easily contaminated, and cannot be mass-produced; the electrodialysis method requires a large amount of consumption. Electrical energy, and a large amount of toxic chlorine gas is produced in the production process; the nanofiltration membrane method has great advantages over the above methods.
  • the nanofiltration membrane is a pressure-driven membrane with a charged group on the membrane, which produces a Donnan effect through electrostatic interaction, and has different selective permeability to ions of different valence states. Separation of different valence ions.
  • the nanofiltration membrane has a rejection rate of monovalent ions of 10% to 80%, and has a relatively high permeability, while the retention rates of both divalent and polyvalent salts are above 90%, thereby realizing monovalent lithium ions and Separation of divalent magnesium ions.
  • domestic companies have used this technology to extract lithium from salt lake brines, but there are still some problems that lead to low production efficiency and high cost.
  • embodiments of the present invention provide a comprehensive lithium ion (Li + ) extraction method combining a chemical reagent method, a physical impurity removal method, a nanofiltration membrane separation method, a concentrated membrane method, and the like.
  • other impurities such as Mg 2+ , SO 4 2- , B 2+ , etc. existing in the salt lake brine are removed before the membrane separation by a method other than the membrane separation method such as a chemical method or a physical impurity removal method. It creates favorable conditions for membrane separation, greatly improves membrane separation efficiency, and optimizes separation effect; in the membrane separation process and after membrane separation, the above method is also combined to further improve the efficiency and purity of lithium extraction.
  • the extraction of lithium from a salt lake by a membrane separation method can generally only reach the industrial grade, and due to the presence of a large amount of impurity ions, a large amount of precipitation often occurs in the membrane separation process to cause fouling of the membrane, which affects the production progress on the one hand. On the other hand, it also increases production costs.
  • the purity of the battery can be achieved, and a large amount of impurity ions are removed before the membrane separation, and the fouling problem in the membrane separation process is also solved, which greatly prolongs the production cycle. , reducing production costs.
  • the "high magnesium and low lithium water production” in the lithium magnesium separation step does not mean The concentration of magnesium is higher than that of lithium, and “high lithium and low magnesium water production” does not mean that the concentration of lithium is higher than that of magnesium, but in the same step (such as step 3A), “high magnesium and low lithium water production”
  • the lithium to magnesium ratio (mass ratio) is lower than the lithium to magnesium ratio (mass ratio) in "high lithium and low magnesium water production”.
  • the feedstock is a lithium-containing brine from a salt lake or a lithium-containing brine from other sources.
  • the salt lake brine used in the examples of the present invention is a salt lake brine with a high magnesium to lithium ratio, and the magnesium to lithium ratio (Mg 2+ : Li + mass ratio) is generally above 20.
  • Acid is added to the raw material brine to adjust the pH of the brine to 2-4 to precipitate crystals of boric acid, and solid-liquid separation is carried out to obtain a clear liquid and crude boric acid.
  • the crude boric acid can be further processed for sale, and the supernatant is passed to step 2 for pretreatment.
  • the manner of precipitation includes a conventional chemical or physical precipitation method such as adding a lye to precipitate magnesium ions in the form of magnesium hydroxide, adding cerium ions to precipitate sulfate ions, or changing the temperature of the solution so that the solubility of calcium sulfate is changed to precipitate or the like.
  • the lithium magnesium separation membrane is used to separate the lithium liquid from the supernatant of the pretreatment step to obtain high magnesium low lithium water production and high lithium low magnesium water production, wherein high lithium and low magnesium water production proceeds to the next step to continue processing.
  • the lithium ion content in the high lithium and low magnesium produced water is greater than 300 PPM, and the lithium magnesium mass ratio is greater than 1:1.
  • the lithium magnesium separation membrane may employ a nanofiltration membrane that can separate monovalent ions and divalent ions.
  • the nanofiltration membrane is a pressure-driven membrane. Because of the charged groups on the membrane or in the membrane, the Donnan effect is generated by electrostatic interaction, and the ions of different valence states have different selectivity, thereby achieving different prices. Separation of state ions.
  • lithium-magnesium separation membranes have been available in the art, and companies such as Membrane Products, Nitto, and Osmonics have related product lines.
  • the above process provided by the embodiments of the present invention can also utilize a lithium-magnesium separation membrane prepared by itself.
  • the high-lithium and low-magnesium produced water obtained in the previous step is concentrated to obtain a concentrated liquid and a light liquid, and the concentrated liquid is further processed in the next step.
  • the method of concentration can use a lithium concentrated membrane to treat high lithium and low magnesium water.
  • the lithium concentrated membrane is generally a reverse osmosis membrane, and a commercial product such as Dow, KOCH, HYDRANAUTICS, GE, TORAY, and the like can be used.
  • the above process provided by the embodiments of the present invention can also utilize a self-prepared lithium concentrated film.
  • the concentration of lithium in the concentrate obtained by concentration is greater than 16000 PPM, and the mass ratio of lithium to magnesium is greater than 1:1.
  • another embodiment of the present invention provides a method for separating and extracting lithium from brine.
  • the method provided by the embodiment has more subdivided steps, including :
  • the pretreatment step 2 comprises a step 2A and a step 2B, the step 2A comprising: raising the pH of the supernatant of the step 1 to adjust the pH to 7-9 a part of SO 4 2- and Mg 2+ in the brine is precipitated in the form of calcium sulfate and magnesium hydroxide, and after the solid-liquid separation, the supernatant 2A is obtained, and the treatment is continued in step 2B; the step 2B includes: adding the auxiliary in the clear solution 2A A filter (such as a homogenous perlite, added in an amount of 30-50 ppm), a portion of the remaining SO 4 2- and Mg 2+ remaining in the brine continues to precipitate as calcium sulfate and magnesium hydroxide, and a solid solution is obtained to obtain a clear liquid. 2B proceeds to step 3 to continue processing.
  • a filter such as a homogenous perlite, added in an amount of 30-50 ppm
  • step 3 Lithium and magnesium separation, lithium and magnesium separation membrane is used to separate lithium and magnesium to obtain high magnesium low lithium water production and high lithium low magnesium water production;
  • step 3 includes step 3A and step 3B,
  • step 3A includes: clear liquid obtained in step 2B Adding acid, adjusting the pH to 7-8.5, separating the clear liquid by lithium-magnesium separation membrane to obtain high-magnesium low-lithium water production 3A and high-lithium low-magnesium water production 3A, high-lithium low-magnesium production water 3A proceeds to step 3B to continue the treatment;
  • 3B includes: adding a complexing agent to the high-lithium and low-magnesium water-producing water 3A (the complexing agent may be a scale inhibitor commonly used in the field of water treatment, for example, it may be a compound of EDTA sodium salt, ethylenediaminetetraacetic acid, and ethylene.
  • the complexing agent may be a scale inhibitor commonly used in the field of water treatment, for example, it may be a
  • step 4 of the lithium concentration includes the step 4A, the step 4B and Step 4C
  • step 4A comprises: concentrating the high-lithium and low-magnesium produced water of step 3 by using a lithium concentrated membrane to obtain concentrated liquid 4A and light liquid 4A, and the concentrated liquid 4A proceeds to step 4B to continue processing
  • Step 4B includes: concentrating the concentrated liquid 4A of the step 4A with a lithium concentrated membrane to obtain a concentrated liquid 4B and a light liquid 4B, and the concentrated liquid 4B proceeds to the step 4C for further processing
  • the step 4C includes: using the lithium concentrated film for the concentrated liquid of the step 4B 4B is concentrated to obtain a concentrate 4C and a light liquid 4C, and the concentrate 4C is advanced to the step 5 to continue the treatment.
  • Example 2 has more subdivision steps, on the one hand, the lithium-magnesium separation effect is better, and the purity of the final product lithium carbonate is also higher; on the other hand, the removal of the precipitate in the brine is more thorough and reduced.
  • the fouling condition in the membrane separation process makes the continuous operation of the method greatly extended, and the automation degree of the whole process is improved.
  • pretreatment step 2 using two pretreatment steps of 2A and 2B, the sulfate ion and magnesium ion in the brine can be reduced more, the precipitate entering the next step is reduced, and the membrane separation is reduced.
  • the probability of fouling in the process is conducive to the subsequent separation of lithium and magnesium.
  • steps 2, 3, and 4 do not need to be subdivided at the same time, and some steps may be subdivided according to actual needs, and other steps are completed in one step.
  • the lithium carbonate finally obtained in this example has a purity of >99.6%.
  • another embodiment of the present invention provides a method for separating and extracting lithium from brine.
  • the method provided in this embodiment recovers the Li + content produced in each step.
  • the high magnesium and low lithium water produced in step 3A is returned to the salt field for concentration and enrichment, and then combined with the raw material brine, and the high magnesium and low lithium produced water 3B obtained in step 3B is returned to be combined with the clear liquid of step 2A.
  • the light liquid 4A obtained in the step 4A is returned to the clear liquid in the step 2A
  • the light liquid 4B obtained in the step 4B is returned to be combined with the clear liquid in the step 2A
  • the light liquid 4C obtained in the step 4C is returned to be combined with the clear liquid in the step 2A. Since the solution with lower Li + content produced in each step is recycled, the extraction rate of Li + in the brine is improved from 40% to over 80%. It should be noted that the above-mentioned solution with a lower Li + content does not need to be simultaneously recovered, and in actual production, a part of the recycling can be reasonably selected according to the situation, taking into consideration the cost and the lithium ion extraction rate.
  • the purity of lithium carbonate finally obtained in this embodiment is >99.7%, and the recovery rate of lithium in brine is above 80%.
  • step 2A includes raising the pH of the supernatant of step 1 to 7-9, and a part of SO 4 2- and Mg 2+ in the brine is precipitated as calcium sulfate and magnesium hydroxide.
  • the method of raising the pH includes, but is not limited to, adding NaOH, KOH, Ca(OH) 2 or ammonia water to the solution, forming a precipitate and separating by solid-state centrifugation or plate-and-frame solid-liquid separation, and the solid matter can be further treated as a raw material of the magnesium product.
  • An increase in pH promotes the removal of magnesium, which removes 20 to 30% of magnesium.
  • a filter aid was introduced in Pretreatment 2B.
  • a filter aid such as homogenous perlite is added to the clear liquid 2A in an amount of 30-50 ppm, and a part of the remaining SO 4 2- and Mg 2+ in the brine is continuously precipitated in the form of calcium sulfate and magnesium hydroxide.
  • the polytetrafluoroethylene microfiltration membrane separates the CaSO 4 and Mg(OH) 2 flocs to obtain the supernatant 2B, and proceeds to step 3 to continue the treatment.
  • a filter aid is a substance that increases the filtration efficiency of the filtrate.
  • the filter aid may be an insoluble inert material having a different degree of fineness.
  • examples of the above filter aids in the present invention include, but are not limited to, perlite, diatomaceous earth, cellulose, and the like.
  • a complexing agent can be introduced in step 3B.
  • a complexing agent such as compounding EDTA sodium salt, 3-6ppm, separating high-lithium and low-magnesium water-producing water 3A by using a lithium-magnesium separation membrane to obtain high-magnesium-low-lithium water-producing water 3B and high-low lithium
  • Magnesium produced water 3B in which high magnesium and low lithium produced water 3B returns with the clear liquid of step 2A, and high lithium low magnesium produced water 3B proceeds to step 4 to continue processing.
  • the above complexing agent functions to complex with calcium, barium, strontium, etc., and prevents calcium sulfate, calcium carbonate, barium sulfate, barium sulfate and the like from scaling on the surface of the film to cause damage to the film.
  • Examples of the above complexing agent in the present invention include, but are not limited to, a compound of EDTA sodium salt, ethylenediaminetetraacetic acid, ethylenediaminetetraacetate, aminotrimethylenephosphonic acid, diethylenetriaminepentamethylphosphonic acid. , hydroxyethylidene diphosphonic acid or sodium hexametaphosphate.

Abstract

La présente invention concerne un procédé de séparation et d'extraction de lithium d'une saumure qui comprend les étapes suivantes : 1) l'acidification pour retirer le bore : l'ajout d'un acide à la saumure pour précipiter l'acide borique et l'exécution d'une séparation solide-liquide pour obtenir un premier surnageant; 2) le prétraitement : l'élimination d'une partie des ions sulfate et des ions magnésium du premier surnageant par précipitation, pour obtenir un second surnageant; 3) la séparation lithium-magnésium : la séparation du lithium et du magnésium dans le second surnageant en utilisant une membrane de séparation de lithium-magnésium, pour obtenir de l'eau produite à teneur élevée en magnésium et faible en lithium et de l'eau produite à teneur élevée en lithium et faible en magnésium; 4) la concentration du lithium : la concentration, en utilisant une membrane de concentration de lithium, de l'eau produite à teneur élevée en lithium et faible en magnésium obtenue dans l'étape 3) pour obtenir une solution concentrée et une solution diluée; 5) la purification et la précipitation du lithium : l'augmentation d'un pH de la solution concentrée obtenue dans l'étape 4), l'élimination de Mg2+ par précipitation de Mg(OH)2 pour obtenir un troisième surnageant, l'introduction de CO3 2- dans le troisième surnageant pour précipiter Li+ sous la forme de Li2CO3, et la séparation, le rinçage et le séchage d'un précipité pour obtenir un produit carbonate de lithium de qualité batterie.
PCT/CN2016/087443 2015-07-03 2016-06-28 Procédé d'extraction de lithium dans de la saumure de lac salé WO2017005113A1 (fr)

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US11865531B2 (en) 2018-02-28 2024-01-09 Lilac Solutions, Inc. Ion exchange reactor with particle traps for lithium extraction
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