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7 USOO9347111B2 (12) United States Patent (10) Patent No.: US 9,347,111 B2 KOmon et al. (45) Date of Patent: May 24, 2016 (54) MAKING MINERAL SALTS FROM VARIOUS (58) Field of Classification Search SOURCES None See application file for complete search history. (71) Applicant: Lixivia, Inc., Santa Barbara, CA (US) (56) References Cited (72) Inventors: Zachary J. A. Komon, San Diego, CA (US); Michael D. Wyrsta, Santa U.S. PATENT DOCUMENTS Barbara, CA (US) 5,939,034 A 8/1999 Virnig et al. 6.951,960 B2 10/2005 Perraud (73) Assignee: LIXIVIA, INC., Santa Barbara, CA 2004/0228783 A1 11/2004 Harris et al. (US) FOREIGN PATENT DOCUMENTS (*) Notice: Subject to any disclaimer, the term of this EP 1309392 B1 T 2006 patent is extended or adjusted under 35 JP 2005-097072 A 4/2005 U.S.C. 154(b) by 155 days. WO 2012-055750 A1 5, 2012 WO 2012-055750 A4 T 2012 (21) Appl. No.: 14/073,406 OTHER PUBLICATIONS (22) Filed: Nov. 6, 2013 Kodama, Satoshi, et al., “Development of a New Ph-Swing CO2 Mineralization Process with a Recyclable Reaction Solution.” (65) Prior Publication Data Energy 33 (2008) 776-784, 9 pages. US 2014/O127096 A1 May 8, 2014 Primary Examiner — Melissa Swain (74) Attorney, Agent, or Firm — Fish & Tsang, LLP Related U.S. Application Data (57) ABSTRACT Hydrometallurgical systems, methods, and compositions are (60) Provisional application No. 61/796,304, filed on Nov. described in which organic amine-based lixiviants are uti 6, 2012. lized in the selective recovery of alkaline earth elements. The (51) Int. Cl. lixiviant can be regenerated and recycled for use in Subse C22B 3/16 (2006.01) quent iterations of the process. Multiple alkaline earth ele (52) U.S. Cl ments can be recovered from a sample in parallel or in serial CPC ............. c22B 3/1625 (2013 olyop 102.34 applications of the disclosed methods. (2015.11) 23 Claims, 5 Drawing Sheets "y 105 N 2 Hic \ 107 101 N 2 MEA 2 MEAFC 1 103 -b 2 MFAf2C l 2 IC C 1137"A C aCl2 as 107-1 2 MEAF2CI 115 G U.S. Patent May 24, 2016 Sheet 1 of 5 US 9,347,111 B2 "y 105 N2 HC 107 101 2 MEA/CI -D 103 : i -1 111 109 2 MEA"/2CI CaCl2 (aq) 2 MEA"/2CI 115 119 117 Figure 1 U.S. Patent May 24, 2016 Sheet 2 of 5 US 9,347,111 B2 "y 201 2O3 205 Lixiviant 213 Supernatant + Regeneration Sample (e.g., addition of acid) 207 Treated Sample Supernatant Metal 211 Hydroxide Forming Species Figure 2 U.S. Patent May 24, 2016 Sheet 3 of 5 US 9,347,111 B2 300 301 303 Sample First Lixiviant 305 First Lixiviant Supernatant + Regeneration First Depleted (e.g., addition of Sample acid) 317 307 Second First Depleted First Lixiviant Sample Supernatant First Metal 3 11 LiXiviant Second Hydroxide Regeneration Supernatant + Forming (e.g., addition of Second Depleted Species acid) Sample 323 Second Second Depleted Supernatant Sample Second Metal Hydroxide Forming Species Figure 3 U.S. Patent May 24, 2016 Sheet 4 of 5 US 9,347,111 B2 400 401 403 Lixiviant First Supernatant + Sample Lixiviant Regeneration (e.g., addition of acid) First Treated Sample Supernatant First Metal Hydroxide Second Forming Supernatant Species Second Metal Hydroxide Forming Species Figure 4 U.S. Patent May 24, 2016 Sheet 5 of 5 US 9,347,111 B2 501 503 500 & 1. Grind slag or other 2. Mix water and calcium Source to Lixiviant to ~0.1-50% preferably <125 Wt in Water, or used microns recycled solution 3. Combine 1 and 2, in the appropriate vessel and stir until pH rises to ~8-12 4A. Add Sufficient HCI 4B. Allow lixiviant to to regenerate lixiviant,- - - react, until pH rises to but not more than that ~8-12 or stops rising due to extraction limit 513 5. Filter away the solid residue, retain the liquid fraction 6. Use Solution as-is 8A. Partially evaporate Solvent and/or cool With lixiviant as Solution to precipitate acceptable contaminant 7. Evaporate all CaCl hydrates Solvent and optionally lixiviant if possible leave solid CaCl2 hydrates; Solvent and 8B. Filter Off lixiviant can be crystalline product; recycled to Step 3 Supernatant may be further processed to obtain more product or recycled back into proccSS 521 9. Purified CaCl2 hydrates may be further dehydrated or uScd as-is Figure 5 US 9,347,111 B2 1. 2 MAKING MINERAL SALTS FROM VARIOUS cient and selective extraction of the desired metal or metals SOURCES has been a significant technical barrier to their adoption in the isolation of some metals. Similarly, the expense of lixiviant This application claims priority to U.S. Provisional Appli components, and difficulties in adapting Such techniques to cation No. 61/796,304, filed Nov. 6, 2012. These and all other current production plants, has limited their use. referenced extrinsic materials are incorporated herein by ref. Approaches have been devised to address these issues. U.S. erence in their entirety. patent application No. 2004/0228783 (to Harris, Laksh manan, and Sridhar) describes the use of magnesium salts (in FIELD OF THE INVENTION addition to hydrochloric acid) as a component of a highly 10 acidic lixiviant used for recovery of other metals from their The field of the invention is hydrometallurgy, particularly oxides, with recovery of magnesium oxide from the spent as it is related to the extraction or recovery of alkaline earth lixiviant by treatment with peroxide. Such highly acidic and elements. oxidative conditions, however, present numerous production and potential environmental hazards that limit their utility. In BACKGROUND 15 an approach disclosed in U.S. Pat. No. 5,939,034 (to Virnig and Michael), metals are solubilized in an ammoniacal thio The following description includes information that may Sulfate solution and extracted into an immiscible organic be useful in understanding the present invention. It is not an phase containing guanidyl or quaternary amine compounds. admission that any of the information provided herein is prior Metals are then recovered from the organic phase by electro art or relevant to the presently claimed invention, or that any plating. publication specifically or implicitly referenced is prior art. A similar approach is disclosed in U.S. Pat. No. 6,951,960 All publications identified herein are incorporated by ref (to Perraud) in which metals are extracted from an aqueous erence to the same extent as if each individual publication or phase into an organic phase that contains an amine chloride. patent application were specifically and individually indi The organic phase is then contacted with a chloride-free cated to be incorporated by reference. Where a definition or 25 aqueous phase that extracts metal chlorides from the organic use of a term in an incorporated reference is inconsistent or phase. Amines are then regenerated in the organic phase by contrary to the definition of that term provided herein, the exposure to aqueous hydrochloric acid. Application to alka definition of that term provided herein applies and the defi line earth elements (for example, calcium) is not clear, how nition of that term in the reference does not apply. ever, and the disclosed methods necessarily involve the use of There is a long-standing need to efficiently and cost-effec 30 expensive and potentially toxic organic solvents. tively recover commercially valuable metals from low yield In a related approach, European Patent Application No. Sources, such as mine tailings. EP1309392 (to Kocherginsky and Grischenko) discloses a Historically, it has been especially desirable to recover membrane-based method in which copper is initially com alkaline earth elements. Alkaline earth elements, also known plexed with ammonia or organic amines. The copper:ammo as beryllium group elements, include beryllium (Be), mag 35 nia complexes are captured in an organic phase contained nesium (Mg), calcium (Ca), strontium (Sr), barium (Ba) and within the pores of a porous membrane, and the copper is radium, (Ra), which range widely in abundance. Applications transferred to an extracting agent held on the opposing side of of these commercially important metals also vary widely, and the membrane. Such an approach, however, requires the use include uses as dopants in electronic components, structural of complex equipment, and processing capacity is necessarily materials, and in the production foods and pharmaceuticals. 40 limited by the available surface area of the membrane. Methods of isolating of one member of the alkaline earth Methods for capturing CO could be used to recover alka family, calcium, from minerals such as limestone, have been line earth metals, but to date no one has appreciated that Such known since ancient times. In a typical process limestone is could be done. Kodama et al. (Energy 33(2008), 776-784) calcined or otherwise roasted to produce calcium oxide discloses a method for CO capture using a calcium silicate (CaO), or quicklime. This material can be reacted with water 45 (2CaO-SiO) in association with ammonium chloride to produce calcium hydroxide (Ca(OH)), or slaked lime. (NHCl). This reaction forms soluble calcium chloride Calcium hydroxide, in turn, can be suspended in water and (CaCl), which is reacted with carbon dioxide (CO) under reacted with dissolved carbon dioxide (CO) to form calcium alkaline conditions to form insoluble calcium carbonate carbonate (CaCO), which has a variety of uses. Approaches (CaCO) and release chloride ions (C1-). that have been used to isolate other members of this family of 50 Kodama et al. uses clean forms of calcium to capture CO, elements often involve the production of insoluble hydrox but is silent in regard to the use of other alkaline earth ele ides and oxides using elevated temperatures or strong acids.
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