WO2015171109A1 - Sorbant amélioré pour l'extraction de lithium - Google Patents

Sorbant amélioré pour l'extraction de lithium Download PDF

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Publication number
WO2015171109A1
WO2015171109A1 PCT/US2014/036774 US2014036774W WO2015171109A1 WO 2015171109 A1 WO2015171109 A1 WO 2015171109A1 US 2014036774 W US2014036774 W US 2014036774W WO 2015171109 A1 WO2015171109 A1 WO 2015171109A1
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WO
WIPO (PCT)
Prior art keywords
lithium
polymer
matrix
lai
weight
Prior art date
Application number
PCT/US2014/036774
Other languages
English (en)
Inventor
John L. Burba, Iii
Ray F. Stewart
Brian E. VIANI
Stephen Harrison
Christine Ellen Vogdes
John Galil Salim LAHLOUH
Original Assignee
Simbol, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Simbol, Inc. filed Critical Simbol, Inc.
Priority to PCT/US2014/036774 priority Critical patent/WO2015171109A1/fr
Publication of WO2015171109A1 publication Critical patent/WO2015171109A1/fr

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Classifications

    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3007—Moulding, shaping or extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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

Definitions

  • geothermal brines can include various metal ions, particularly alkali and alkaline earth metals, as well as transition metals such as lead, silver and zinc, in varying concentrations, depending upon the source of the brine.
  • metal ions particularly alkali and alkaline earth metals, as well as transition metals such as lead, silver and zinc
  • recovery of these metals is potentially important to the chemical and pharmaceutical industries.
  • the economic recovery of metals from natural brines which may vary widely in composition, depends not only on the specific concentration of the desired metal, but also upon the concentrations of interfering ions, particularly silica, calcium and magnesium, because the presence of the interfering ions will increase recovery costs as additional steps must be taken to remove the interfering ions.
  • the lithium aluminate intercalate solid is present in an amount of at least 75%o by weight and the polymer is present in an amount of between about 1 % and 25% by weight.
  • the lithium aluminate intercalate solid is present in an amount of at least 80%) by weight and the polymer is present in an amount of between about 1% and 20% by weight.
  • the lithium salt is lithium chloride.
  • the lithium salt can be selected from the group consisting of lithium chloride, lithium bromide, lithium nitrate, or lithium hydroxide.
  • the polymer is a solid or a powder.
  • the alumina is selected from gibbsite, alumina hydrate, bayerite, nordstandite, bauxite, amorphous aluminum trihydroxide, and activated alumina.
  • a composition for the recovery of lithium from a brine includes particulate material that includes a lithium aluminate intercalate and a polymer.
  • the lithium aluminate intercalate is produced by infusing alumina with a lithium salt to produce a LiX/Al(OH)3 solid having a mole fraction of lithium to aluminum of up to 0.33, wherein X is the anion of the lithium salt.
  • the lithium aluminate intercalate solid is present in an amount of at least 70% by weight and the polymer is present in an amount of between about 1% and 30% by weight.
  • the lithium aluminate intercalate solid is present in
  • Figure 1 is an illustration of one embodiment of the present invention.
  • Figure 2 is a graphical representation showing the loading and unloading of a column according to an embodiment of the present invention.
  • lithium salts include lithium nitrates, lithium sulfates, lithium bicarbonate, lithium halides (particularly chlorides and bromides), and acid salts.
  • novel methods for the selective extraction of lithium halides from solutions and brines that include said lithium halides are described herein.
  • the fine particles which still retain a maximum lithium to aluminum ratio, can have an average diameter of less than about 80 ⁇ , alternatively less than about 50 ⁇ , alternatively less than about 25 ⁇ , alternatively less than about 10 ⁇ , alternatively less than about 5 ⁇ .
  • the particulate matter has a diameter of between about 0.1 and 10 ⁇ , alternatively between about 0.5 and 8 ⁇ , alternatively between about 1 and 5 ⁇ .
  • at least about 50% of the particulate matter has a diameter of less than about 2 ⁇ , alternatively at least about 75% of the particulate matter has a diameter of less than about 2 ⁇ , and alternatively at least about 90% of the particulate matter has a diameter of less than about 2 ⁇ .
  • the particulate matter has a bimodal size distribution, wherein the material has a first peak distribution of about 50 ⁇ and a second peak distribution of about 10 ⁇ .
  • Exemplary elements present in the geothermal brines can include sodium, potassium, calcium, magnesium, lithium, strontium, barium, iron, boron, silicon, manganese, zinc, aluminum, antimony, chromium, cobalt, copper, lead, arsenic, mercury, molybdenum, nickel, silver, gold, thallium, radon, cesium, rubidium, vanadium, sulfur, chlorine, and fluorine, although it is understood that other elements and compounds may also be present.
  • Brines can be obtained from natural sources, such as, Chilean brines, Argentinean brines, Venezuelan brines, or Salton Sea brines, geothermal brines, sea water, oilfield brines, mineral brines (e.g., lithium chloride or potassium chloride brines), alkali metal salt brines, and industrial brines, for example, industrial brines recovered from ore leaching, mineral dressing, and the like.
  • the method is equally applicable to artificially prepared brine or salt solutions, as well as waste water streams, assuming that the salinity of the solution is high enough (for example, a minimum concentration of about 14% by weight common salt). It is understood that, in certain embodiments, the exact concentration of salt sufficient to drive to sorption of lithium into the lithium aluminate is dependent on the exact species and their concentrations present in the solution.
  • the fine particulate matter has a diameter of less than about 80 ⁇ , alternatively less than about 50 ⁇ , alternatively less than about 25 ⁇ , alternatively less than about 10 ⁇ .
  • the material has a bimodal size distribution wherein the material has a first peak distribution of about 50 ⁇ and a second peak distribution of about 10 ⁇ .
  • the particulate material has a diameter of between about 0.1 and 8 ⁇ , alternatively between about 0.5 and 5 ⁇ .
  • the polymer is an emulsified water insoluble polymer.
  • the water insoluble polymer is a fluoropolymer.
  • the water insoluble polymer is an acrylic interpolymer.
  • the polymer can be a crosslinked polymer.
  • a pore forming material can be added to the matrix material and then removed after matrix formation.
  • Preferred pore forming materials can include water or alcohol soluble salts, such as calcium carbonate, lithium chloride, sodium chloride, sodium sulfate, sodium benzoate, organic materials such as polyvinyl alcohol, sugars, polyethylene oxide and copolymers, urea, calcium carbonate, and triacetin.
  • a calcined diatomaceous earth and similar material may be added to the matrix to promote fluid flow and prevent compaction of , the. matrix and the resultant loss of permeability. These additives are generally added before, or during the sintering process.
  • the powder mixture in the press frame was placed in a hydraulic press and subjected to approximately 3500 psi pressure for approximately three minutes, released, subjected to approximately 4000 psi of pressure for approximately, released, subjected to approximately 5000 psi of pressure and a temperature of about 360°C for approximately 3 minutes, released, subjected to approximately 10,000 psi of pressure and a temperature of about 360°C for approximately 3 minutes, and released.
  • the assembly was then subjected to approximately 3500 psi of pressure for about 2-3 minutes.
  • the resulting sintered block was then broken into large granulates using a hammer.
  • Example 4 The LAI/PVDF material from Example 2, sieved to approximately 180- 300 ⁇ , was washed with an approximately 26% solution of sodium chloride having a lithium concentration of approximately 200 ppm, loaded into a standard laboratory ion exchange column (co-current up flow, glass wool packed bed, having a bed volume of approximately 9.4 mL). The column was then subjected to 150 load and unload cycles.
  • the resin was heated at a temperature of between about 75 and 80°C to convert the amorphous Al(OH)3 into gibbsite, which served as a seed for subsequent precipitation.
  • the gibbsite-seeded resin was reacted with sodium aluminate solution at a pH of about 13 and titrated with a 37% solution of HC1 to lower the pH to approximately 7 and precipitate Al(OH) 3 on the gibbsite seed.
  • the mixture was washed with w ater to remove excess NaCl and Al(OH) 3 , and then heated to a temperature of between about 75 and 80°C.
  • the gibbsite-loaded resin was reacted with LiOH at a pH of about 12 and a temperature of between about 55 and 60°C to form a 3-layer polytype lithium aluminate (LiAl 2 (OH) 6 OH) within the resin.
  • the resulting lithiated resin was then titrated with a 20% solution of HC1 to a pH of about 7 to convert the hydroxide form of the lithium aluminate to the chloride form. Excess lithium aluminate and LiCl were removed by washing with water.
  • the resulting resin contained between about 2 and 4 mmol of aluminum and between about 1 and 2 mmol of lithium per mL of resin.
  • the paste was manually pressed through a 500 micron square opening screen while hot air was directed over the strands to prevent sticking.
  • the resulting strands were collected and dried for approximately seventy-two hours in an oven maintained at a temperature of about 50°C, followed by curing for about two hours at approximately 120°C.
  • the cured strands were then manually broken into shorter agglomerates on a 600 micron sieve.
  • the broken strands were sieved in a stack of various size screens, having openings ranging from about 106 to 600 ⁇ and various size fractions of agglomerated particles were collected separately and weighed. Agglomerates from the 425- 600 ⁇ fraction were further tested for operating capacity.
  • Example 1 1 Polymer/LAI agglomerates described in Example 1 1 were loaded onto a column having a volume of about 10.6 mL and were loaded with about eight bed volumes (hereinafter, "BV") of a simulated brine prepared as described herein at a rate of about 8 BV/hour.
  • BV bed volumes
  • the column was stripped with approximately 1 .5 BV of a deionized water solution containing about 1000 ppm lithium at a rate of about 2.4 BV/hour. All test solutions were supplied by co-current upflow, and because these tests were accelerated by reducing the loading and stripping solution volumes, lithium saturation in the column effluent during loading was not observed (i.e., the lithium concentration in the column effluent never equaled the lithium concentration in the feed solution).
  • a metering pump was used to titrate for up to about 4 hours to provide a stable pH of between about 6.5 and 7, ensuring that the pH is greater than 6.
  • the water and supernatant are removed and the resulting solid material is dried in an oven.
  • the yield was about 80 kg (90%) providing LAI particles having a bimodal distribution of about 100-125 ⁇ and about 10 ⁇ , as determined with a Microtrac Laser Diffration Type Analyzer.
  • the free flow bulk density was about 0.6 g/mL and the tapped bulk density was about 0.8 g/mL.

Abstract

La présente invention concerne un procédé de préparation d'un solide de matrice d'intercalaire d'aluminate de lithium (LAI) et des procédés pour l'extraction sélective et la récupération de lithium à partir de solutions contenant du lithium, comprenant des saumures. Le procédé de préparation du solide de matrice LAI comprend la réaction d'hydroxyde d'aluminium et d'un sel de lithium pour former l'intercalaire d'aluminate de lithium, qui peut ensuite être mélangé avec jusqu'à environ 25 % en poids d'un polymère pour former la matrice LAI.
PCT/US2014/036774 2014-05-05 2014-05-05 Sorbant amélioré pour l'extraction de lithium WO2015171109A1 (fr)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018170721A1 (fr) * 2017-03-21 2018-09-27 Dow Global Technologies Llc Matrices contenant des aluminates de lithium
WO2019173716A1 (fr) * 2018-03-08 2019-09-12 Ut-Battelle, Llc Composite d'extraction de lithium pour la récupération de lithium à partir de saumures, et procédé d'utilisation de ladite composition
CN111163852A (zh) * 2017-08-02 2020-05-15 锂莱克解决方案公司 使用多孔离子交换珠进行的锂提取
CN112313006A (zh) * 2018-04-23 2021-02-02 株式会社Posco 锂吸附成型体及其制造方法
US11339457B2 (en) 2020-01-09 2022-05-24 Lilac Solutions, Inc. Process for separating undesirable metals
US11358875B2 (en) 2020-06-09 2022-06-14 Lilac Solutions, Inc. Lithium extraction in the presence of scalants
US11377362B2 (en) 2020-11-20 2022-07-05 Lilac Solutions, Inc. Lithium production with volatile acid
US11806641B2 (en) 2016-11-14 2023-11-07 Lilac Solutions, Inc. Lithium extraction with coated ion exchange particles
US11865531B2 (en) 2018-02-28 2024-01-09 Lilac Solutions, Inc. Ion exchange reactor with particle traps for lithium extraction

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4159311A (en) * 1977-07-05 1979-06-26 The Dow Chemical Company Recovery of lithium from brines
US4347327A (en) * 1978-09-05 1982-08-31 The Dow Chemical Company Recovery of lithium from brines
US4727167A (en) * 1984-06-11 1988-02-23 The Dow Chemical Company Intercalations of crystalline lithium aluminates
US6280693B1 (en) * 1993-05-24 2001-08-28 Fmc Corporation Composition for the recovery of lithium values from brine and process of making/using said composition
US20140102946A1 (en) * 2009-12-18 2014-04-17 Simbol Inc. Lithium Extraction Composition and Method of Preparation Thereof
US8753594B1 (en) * 2009-11-13 2014-06-17 Simbol, Inc. Sorbent for lithium extraction

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4159311A (en) * 1977-07-05 1979-06-26 The Dow Chemical Company Recovery of lithium from brines
US4347327A (en) * 1978-09-05 1982-08-31 The Dow Chemical Company Recovery of lithium from brines
US4727167A (en) * 1984-06-11 1988-02-23 The Dow Chemical Company Intercalations of crystalline lithium aluminates
US6280693B1 (en) * 1993-05-24 2001-08-28 Fmc Corporation Composition for the recovery of lithium values from brine and process of making/using said composition
US8753594B1 (en) * 2009-11-13 2014-06-17 Simbol, Inc. Sorbent for lithium extraction
US20140102946A1 (en) * 2009-12-18 2014-04-17 Simbol Inc. Lithium Extraction Composition and Method of Preparation Thereof

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11806641B2 (en) 2016-11-14 2023-11-07 Lilac Solutions, Inc. Lithium extraction with coated ion exchange particles
WO2018170721A1 (fr) * 2017-03-21 2018-09-27 Dow Global Technologies Llc Matrices contenant des aluminates de lithium
CN110573633A (zh) * 2017-03-21 2019-12-13 陶氏环球技术有限责任公司 含有铝酸锂的基体
US11371118B2 (en) 2017-03-21 2022-06-28 Ddp Specialty Electronic Materials Us, Llc Matrices containing lithium aluminates
CN111163852A (zh) * 2017-08-02 2020-05-15 锂莱克解决方案公司 使用多孔离子交换珠进行的锂提取
EP3661619A4 (fr) * 2017-08-02 2021-05-05 Lilac Solutions, Inc. Extraction de lithium avec des billes d'échange ionique poreuses
US11253848B2 (en) 2017-08-02 2022-02-22 Lilac Solutions, Inc. Lithium extraction with porous ion exchange beads
US11794182B2 (en) 2017-08-02 2023-10-24 Lilac Solutions, Inc. Lithium extraction with porous ion exchange beads
US11975317B2 (en) 2018-02-28 2024-05-07 Lilac Solutions, Inc. Ion exchange reactor with particle traps for lithium extraction
US11865531B2 (en) 2018-02-28 2024-01-09 Lilac Solutions, Inc. Ion exchange reactor with particle traps for lithium extraction
WO2019173716A1 (fr) * 2018-03-08 2019-09-12 Ut-Battelle, Llc Composite d'extraction de lithium pour la récupération de lithium à partir de saumures, et procédé d'utilisation de ladite composition
US11253820B2 (en) 2018-03-08 2022-02-22 Ut-Battelle, Llc Lithium extraction composite for recovery of lithium from brines, and process of using said composition
CN112313006B (zh) * 2018-04-23 2023-10-13 浦项股份有限公司 锂吸附成型体及其制造方法
CN112313006A (zh) * 2018-04-23 2021-02-02 株式会社Posco 锂吸附成型体及其制造方法
US11339457B2 (en) 2020-01-09 2022-05-24 Lilac Solutions, Inc. Process for separating undesirable metals
US11358875B2 (en) 2020-06-09 2022-06-14 Lilac Solutions, Inc. Lithium extraction in the presence of scalants
US11964876B2 (en) 2020-06-09 2024-04-23 Lilac Solutions, Inc. Lithium extraction in the presence of scalants
US11377362B2 (en) 2020-11-20 2022-07-05 Lilac Solutions, Inc. Lithium production with volatile acid

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