DOCSLIB.ORG

United States Patent (19) 11 Patent Number: 5,993,767 Willmann Et Al

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
United States Patent (19) 11 Patent Number: 5,993,767 Willmann Et Al USOO5993767A United States Patent (19) 11 Patent Number: 5,993,767 Willmann et al. (45) Date of Patent: Nov.30, 1999 54). SOLVATE OF LITHIUM 5,378,445 1/1995 Salmon et al. .......................... 423/301 HEXAFLUOROPHOSPHATE AND PYRIDINE, 5,616,636 4/1997 Avar et al. ................................ 546/22 ITS PREPARATION AND PREPARATION FOREIGN PATENT DOCUMENTS PROCESS FOR LITHIUM HEXAFLUOROPHOSPHATE USING SAD 20 26 110 12/1970 Germany. SOLVATE OTHER PUBLICATIONS 75 Inventors: Patrick Willmann, Montgiscard; Chemical Abstracts, vol. 100, No. 21, 21 Mai 1984, Colum Régine Naejus, Tours; Robert bus, Ohio, US; abstract no 174608c, Mohamed, K. er at..: Coudert, Notre Dame D'Oe; Daniel “pyridinium poly (hydrogen fluoride)—a reagent for the Lemordant, Orsay, all of France preparation of hexafluorophosphates' XP002024671. 73 Assignee: Centre National D’Etudes Spatiales, Primary Examiner Wayne Langel France Attorney, Agent, or Firm-Burns, Doane, Swecker & Mathis, L.L.P. 21 Appl. No.: 09/000,232 57 ABSTRACT 22 PCT Filed: Jun. 18, 1997 The invention relates to a lithium hexafluorophosphate Sol 86 PCT No.: PCT/FR97/01097 Vate usable for the preparation of high purity lithium S371 Date: Jan. 23, 1998 hexafluorophosphate. S 102(e) Date: Jan. 23, 1998 This solvate of lithium hexafluorophosphate and pyridine 87 PCT Pub. No.: WO97/48709 complies with the formula: PCT Pub. Date: Dec. 24, 1997 30 Foreign Application Priority Data and is prepared by a proceSS comprising the following Stages: Jun. 19, 1996 FR France ................................... 96 O7623 a) preparation of pyridinium hexafluorophosphate of for 511 Int. Cl.CI. ......................... C01B 25/105/10; CO7D 213/20; mula CH-NHPF by the neutralization of hexafluoro CO7F 9/28 phosphoric acid HPF with pyridine and 52 U.S. Cl. ............................. 423/301; 546/22; 546/347 b) conversion of the pyridinium hexafluorophosphate into 58 Field of Search ............................... 423/301; 546/22, Solvate LiPF, CHN by exchange with a lithium 546/347 compound chosen from among lithium hydroxide, lithium alkoxides and alkyl-lithiums. 56) References Cited The LiPF can be regenerated from the Solvate by vacuum U.S. PATENT DOCUMENTS decomposition. 3,654,330 4/1972 Wiesboeck. 4,996,320 2/1991 Omemoto et al. ........................ 546/22 14 Claims, 7 Drawing Sheets % TRANSMISSION A 4.0 1633 U.S. Patent Nov.30, 1999 Sheet 1 of 7 5,993,767 U.S. Patent Nov.30, 1999 Sheet 2 of 7 5,993,767 % TRANSMSSION 25 15 10 5 673.09 557.71 O (cm1) 2OOO 16OO 1200 8OO 400 U.S. Patent Nov.30, 1999 Sheet 3 of 7 5,993,767 000€ 009Z 000Z 000|| 009 G/|0 09||'0 OGO’0 000’0 U.S. Patent Nov.30, 1999 Sheet 4 of 7 5,993,767 9 SN U.S. Patent Nov.30, 1999 Sheet 5 of 7 5,993,767 9 SN U.S. Patent Nov.30, 1999 Sheet 6 of 7 5,993,767 area 8 C w 007 99°888 008 OOZ| OOOZ G’S 0"| U.S. Patent Nov.30, 1999 Sheet 7 of 7 5,993,767 als - S O Ye' 007 89°199 009 86°188 Z| 0|| 5,993,767 1 2 SOLVATE OF LITHIUM Thus, none of the presently known processes makes it HEXAFLUOROPHOSPHATE AND PYRIDINE, possible to prepare high purity lithium hexafluorophosphate ITS PREPARATION AND PREPARATION LiPF under easily implementable conditions and without PROCESS FOR LITHIUM using onerous reagents. HEXAFLUOROPHOSPHATE USING SAD DESCRIPTION OF THE INVENTION SOLVATE The present invention relates to the preparation of high DESCRIPTION purity LiPF by a simple, uncomplicated process using inexpensive, commercial products, with as the intermediate 1. Technical Field a Solvate of lithium hexafluorophosphate and pyridine. It The invention relates to a novel compound constituted by also relates to the Solvate and its preparation process. a Solvate of lithium hexafluorophosphate and pyridine uSable for the preparation of lithium hexafluorophosphate. The Solvate complies with the formula: It more particularly applies to the preparation of lithium Li(CHN)PF hexafluorophosphate used as an electrolyte in lithium 15 and has the advantage of being much easier to handle than carbon batteries. LiPF, because it is stable in air at ambient temperature, At present lithium batteries are being extensively devel whereas LiPF decomposes into PFs and LiF and must be oped for various applications, particularly in electric manipulated in a glove box. It also makes it possible to vehicles, portable equipments Such as portable telephones generate LiPF with a high purity level of 99.8% using and cameScopes, as well as in Space. These batteries use an Simple processes. electrolyte constituted by one or more organic Solvents According to the invention, this Solvate can be prepared containing in Solution a lithium Salt. Among the uSable by a process comprising the following Stages: lithium salts, lithium hexafluorophosphate (LiPF) is at a) preparation of pyridinium hexafluorophosphate of for present the most widely used, due to its high Solubility in mula CH-NHPF by neutralization of hexafluorophos organic Solvents, its conductivity and its Safety. 25 phoric acid HPF with pyridine using the stoichiomet 2. Prior Art ric quantity permitting the neutralization of only the The conventional method for the preparation of LiPF HPF and not the other acid impurities present in the consists of reacting PFs with LiF in anhydrous hydrofluoric Starting acid and acid, but the purity of LiPF prepared in this way is only 90 b) conversion of pyridinium hexafluorophosphate into to 95%, whereas purities of at least 99% are required for use Solvate LiPF, CHN by exchange with a lithium in a lithium battery in order to satisfy the LiPF storage compound chosen from among lithium hydroxide, Stability and Solubility requirements. lithium alkoxides and alkyl-lithiums. In this process, the first stage a) is easy to perform, In order to overcome this difficulty, it is still possible to because it can be carried out in an aqueous medium at obtain LiPF of higher purity by the process described in 35 ambient temperature from an inexpensive, commercial prod U.S. Pat. No. 3,654,330. According to this process, lithium uct (HPF in aqueous Solution). Moreover, through using the fluoride, anhydrous hydrofluoric acid and phosphorus pen precise Stoichiometric quantity corresponding to the neu tafluoride PFs are reacted to obtain impure LiPF, which is tralization of HPF and excluding other acid impurities then purified by reaction with acetonitrile. Thus, tetraaceto present in the Starting product, it is possible to obtain high nitrilolithium hexafluorophosphate Li(CHCN), PF is 40 purity pyridinium hexafluorophosphate, which will then lead produced, which then regenerates lithium hexafluorophoS to a high purity solvate Li(CHN)PF. phate by heating in a partial vacuum. It is also possible to This Stoichiometric quantity can be easily determined by directly produce Li(CHCN), PF by reacting PF in a carrying out before hand a neutralization test on the com Suspension of LiF in acetonitrile. mercial acid HPF used as the Starting product and moni This process makes it possible to obtain high purity 45 toring the neutralization by conductometry. lithium hexafluorophosphate, but it suffers from the disad It has in fact been found that HPF is stronger than the vantage of requiring the use of PF which is a very difficult other acids present as impurities in commercial Solutions product. and is neutralized first giving rise to a rapid conductivity Another way for obtaining alkali metal hexafluorophoS drop of the solution. The end of this drop corresponds to the phates has been investigated by Syed Mohamed et al in J. 50 complete neutralization of HPF and it is thus possible to Fluorine Chem., 23, 1983, pp 509-514. According to this determine the basic Stoichiometric quantity necessary for document, the Starting product is pyridinium hexafluoro this neutralization. phosphate CH-NHPF, which is then treated with an This method for preparing CH-NHPF is much easier to ammonium or alkali metal hydroxide in an aqueous implement than that described by Syed Mohamed in J. medium, but this process has not made it possible to isolate 55 Fluorine Chem., 23, 1983, pp 509-514, where said pyri solid LiPF from said medium. Moreover, the preparation of dinium hexafluorophosphate is obtained by a two-stage the starting product CH-NHPF involves a low temperature reaction, firstly preparing a poly(hydrogen fluoride)- reaction (-80 C.) between the pyridine and the anhydrous pyridinium reagent at a temperature of -80 C., followed by hydrofluoric acid, followed by the reaction of the product the reaction of Said reagent with dropwise added phosphoryl obtained with phosphoryl chloride. This involves difficult 60 chloride. performance using expensive reagents (POCL), which is The first stage of the proceSS according to the invention is difficult to carry out on an industrial Scale. easier to perform, because it is carried out in an aqueous Lange et al in BER. 63B, 1058–70, 1930 describe the Solution at ambient temperature. It also makes use of uncom preparation of CH3NHPF by reacting pyridine in acetic plicated reagents, which are commercially available, Such as acid with ammonium hexafluorophosphate. However, they 65 HPF solutions in water. did not envisage using this pyridinium hexafluorophosphate In the Second stage b) of the process according to the for preparing lithium hexafluorophosphate. invention, the pyridinium hexafluorophosphate is converted 5,993,767 3 4 into Solvate Li(C5H5N)PF by exchange with a lithium illustrative and non-limitative manner, with reference to the compound. This Solvate has the major advantage of being, attached drawings. unlike LiPF, Stable at ambient temperature, permitting easier handling and Storage. BRIEF DESCRIPTION OF THE DRAWINGS According to a first embodiment of Said Stage, the lithium compound used is hydrated or unhydrated lithium FIG. 1 is a graph illustrating the conductometric dosage hydroxide, in an alcoholic medium, e.g.
Load more

Recommended publications
  • Direct Preparation of Some Organolithium Compounds from Lithium and RX Compounds Katashi Oita Iowa State College
    Iowa State University Capstones, Theses and Retrospective Theses and Dissertations Dissertations 1955 Direct preparation of some organolithium compounds from lithium and RX compounds Katashi Oita Iowa State College Follow this and additional works at: https://lib.dr.iastate.edu/rtd Part of the Organic Chemistry Commons Recommended Citation Oita, Katashi, "Direct preparation of some organolithium compounds from lithium and RX compounds " (1955). Retrospective Theses and Dissertations. 14262. https://lib.dr.iastate.edu/rtd/14262 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Retrospective Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. INFORMATION TO USERS This manuscript has been reproduced from the microfilm master. UMI films the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, while others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send UMI a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. Oversize materials (e.g., maps, drawings, charts) are reproduced by sectioning the original, beginning at the upper left-hand comer and continuing from left to right in equal sections with small overiaps.
    [Show full text]
  • Dilithium Sequestrene As Ananticoagulant
    J Clin Pathol: first published as 10.1136/jcp.12.3.254 on 1 May 1959. Downloaded from J. clin. Path. (1959), 12, 254. DILITHIUM SEQUESTRENE AS AN ANTICOAGULANT BY L. S. SACKER,* K. E. SAUNDERS,t BERYL PAGE, AND MARGARET GOODFELLOW From the Departments of Pathology, Dulwich and Lewisham Hospitals, London (RECEIVED FOR PUBLICATION SEPTEMBER 20, 1958) The variety of different anticoagulants used for Ethylene diamine tetra-acetic acid (E.D.T.A.), 29.2 blood samples has increased, but there is still need g., and 7.4 g. of lithium carbonate were intimately for a suitable anticoagulant for the routine mixed. Then 200 ml. of water was added and solution estimation of sodium and potassium by flame took place with vigorous evolution of carbon dioxide. photometry. So far the only satisfactory substance for this purpose has been the expensive calcium Method 2 heparin (King and Wootton, 1956). Disodium sequestrene (Proescher, 1951 ; Hadley E.D.T.A., 29.2 g., was dissolved in 200 ml. of normal and Larson, 1953) and dipotassium sequestrene lithium hydroxide solution (41.96 g. LiOH.H20 per are the most valuable of litre). (Hadley and Weiss, 1955) In both cases the resulting solution contained the the recently introduced anticoagulants for routine dilithium salt. haematological procedures because they preserve Dilithium sequestrene was obtained from these morphology of leucocytes for short periods the solutions after filtration to remove a small quantity copyright. better than the ammonium and potassium oxalate of amorphous debris, by precipitation on the addition mixture or heparin, and they prevent platelets of an equal volume of absolute methyl alcohol and clumping and preserve them.
    [Show full text]
  • Electrolyte Stability and Discharge Products of an Ionic-Liquid-Based Li-O2 Battery Revealed by Soft X-Ray Emission Spectroscopy
    Lawrence Berkeley National Laboratory Recent Work Title Electrolyte Stability and Discharge Products of an Ionic-Liquid-Based Li-O2 Battery Revealed by Soft X-Ray Emission Spectroscopy Permalink https://escholarship.org/uc/item/6gd3f1x1 Journal Journal of Physical Chemistry C, 123(51) ISSN 1932-7447 Authors León, A Fiedler, A Blum, M et al. Publication Date 2019-12-26 DOI 10.1021/acs.jpcc.9b08777 Peer reviewed eScholarship.org Powered by the California Digital Library University of California Electrolyte Stability and Discharge Products of an Ionic- Liquid-based Li-O2 Battery Revealed by Soft X-Ray Emission Spectroscopy Aline Léon*1, Andy Fiedler2, Monika Blum3,4, Wanli Yang4, Marcus Bär5,6,7, Frieder Scheiba2, Helmut Ehrenberg2, Clemens Heske1,3,8, and Lothar Weinhardt1,3,8 1) Institute for Photon Science and Synchrotron Radiation (IPS), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany 2) Institute for Applied Materials (IAM), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany 3) Department of Chemistry and Biochemistry, University of Nevada, Las Vegas (UNLV), NV 89154-4003, USA 4) Advanced Light Source (ALS), Lawrence Berkeley National Laboratory, Berkeley, California 94720, United States 5) Department of Interface Design, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH (HZB), Albert-Einstein-Str. 15, 12489 Berlin, Germany 6) Helmholtz-Institute Erlangen-Nürnberg for Renewable Energy (HI ERN), Albert-Einstein-Str. 15, 12489 Berlin, Germany 1 7) Department of Chemistry and Pharmacy, Friedrich-Alexander- Universität Erlangen-Nürnberg, Egerlandstr. 3, 91058 Erlangen, Erlangen, Germany 8) Institute for Chemical Technology and Polymer Chemistry (ITCP), Karlsruhe Institute of Technology (KIT), Engesserstr.
    [Show full text]
  • Common Name: LITHIUM ALUMINUM HYDRIDE HAZARD
    Common Name: LITHIUM ALUMINUM HYDRIDE CAS Number: 16853-85-3 RTK Substance number: 1121 DOT Number: UN 1410 Date: April 1986 Revision: November 1999 ----------------------------------------------------------------------- ----------------------------------------------------------------------- HAZARD SUMMARY * Lithium Aluminum Hydride can affect you when * Exposure to hazardous substances should be routinely breathed in. evaluated. This may include collecting personal and area * Contact can cause severe skin and eye irritation and burns. air samples. You can obtain copies of sampling results * Breathing Lithium Aluminum Hydride can irritate the from your employer. You have a legal right to this nose and throat. information under OSHA 1910.1020. * Breathing Lithium Aluminum Hydride can irritate the * If you think you are experiencing any work-related health lungs causing coughing and/or shortness of breath. Higher problems, see a doctor trained to recognize occupational exposures can cause a build-up of fluid in the lungs diseases. Take this Fact Sheet with you. (pulmonary edema), a medical emergency, with severe shortness of breath. WORKPLACE EXPOSURE LIMITS * Exposure can cause loss of appetite, nausea, vomiting, The following exposure limits are for Aluminum pyro powders diarrhea and abdominal pain. (measured as Aluminum): * Lithium Aluminum Hydride can cause headache, muscle weakness, loss of coordination, confusion, seizures and NIOSH: The recommended airborne exposure limit is coma. 5 mg/m3 averaged over a 10-hour workshift. * High exposure can affect the thyroid gland function resulting in an enlarged thyroid (goiter). ACGIH: The recommended airborne exposure limit is * Lithium Aluminum Hydride may damage the kidneys. 5 mg/m3 averaged over an 8-hour workshift. * Lithium Aluminum Hydride is a REACTIVE CHEMICAL and an EXPLOSION HAZARD.
    [Show full text]
  • Lithium Aluminum Hydride
    Lithium aluminum hydride sc-215254 Material Safety Data Sheet Hazard Alert Code EXTREME HIGH MODERATE LOW Key: Section 1 - CHEMICAL PRODUCT AND COMPANY IDENTIFICATION PRODUCT NAME Lithium aluminum hydride STATEMENT OF HAZARDOUS NATURE CONSIDERED A HAZARDOUS SUBSTANCE ACCORDING TO OSHA 29 CFR 1910.1200. NFPA FLAMMABILITY4 HEALTH3 HAZARD INSTABILITY2 W SUPPLIER Santa Cruz Biotechnology, Inc. 2145 Delaware Avenue Santa Cruz, California 95060 800.457.3801 or 831.457.3800 EMERGENCY ChemWatch Within the US & Canada: 877-715-9305 Outside the US & Canada: +800 2436 2255 (1-800-CHEMCALL) or call +613 9573 3112 SYNONYMS Li-Al-H4, Al-H4-Li, "lithium aluminum hydride", "lithium aluminum tetrahydride", "lithium aluminium tetrahydride", "lithium tetrahydroaluminate", "aluminate, tetrahydro-, lithium", "lithium aluminohydride", "aluminum lithium hydride", "lithium alanate", LAH Section 2 - HAZARDS IDENTIFICATION CHEMWATCH HAZARD RATINGS Min Max Flammability 4 Toxicity 2 Body Contact 4 Min/Nil=0 Low=1 Reactivity 2 Moderate=2 High=3 Chronic 2 Extreme=4 CANADIAN WHMIS SYMBOLS 1 of 10 CANADIAN WHMIS CLASSIFICATION CAS 16853-85-3Lithium tetrahydroaluminate E-Corrosive Material EMERGENCY OVERVIEW RISK Causes severe burns. Risk of serious damage to eyes. Reacts violently with water liberating extremely flammable gases. Extremely flammable. POTENTIAL HEALTH EFFECTS ACUTE HEALTH EFFECTS SWALLOWED ■ The material can produce severe chemical burns within the oral cavity and gastrointestinal tract following ingestion. ■ Ingestion of alkaline corrosives may produce burns around the mouth, ulcerations and swellings of the mucous membranes, profuse saliva production, with an inability to speak or swallow. Both the oesophagus and stomach may experience burning pain; vomiting and diarrhoea may follow. ■ Accidental ingestion of the material may be damaging to the health of the individual.
    [Show full text]
  • Chemical List
    1 EXHIBIT 1 2 CHEMICAL CLASSIFICATION LIST 3 4 1. Pyrophoric Chemicals 5 1.1. Aluminum alkyls: R3Al, R2AlCl, RAlCl2 6 Examples: Et3Al, Et2AlCl, EtAlCl2, Me3Al, Diethylethoxyaluminium 7 1.2. Grignard Reagents: RMgX (R=alkyl, aryl, vinyl X=halogen) 8 1.3. Lithium Reagents: RLi (R = alkyls, aryls, vinyls) 9 Examples: Butyllithium, Isobutyllithium, sec-Butyllithium, tert-Butyllithium, 10 Ethyllithium, Isopropyllithium, Methyllithium, (Trimethylsilyl)methyllithium, 11 Phenyllithium, 2-Thienyllithium, Vinyllithium, Lithium acetylide ethylenediamine 12 complex, Lithium (trimethylsilyl)acetylide, Lithium phenylacetylide 13 1.4. Zinc Alkyl Reagents: RZnX, R2Zn 14 Examples: Et2Zn 15 1.5. Metal carbonyls: Lithium carbonyl, Nickel tetracarbonyl, Dicobalt octacarbonyl 16 1.6. Metal powders (finely divided): Bismuth, Calcium, Cobalt, Hafnium, Iron, 17 Magnesium, Titanium, Uranium, Zinc, Zirconium 18 1.7. Low Valent Metals: Titanium dichloride 19 1.8. Metal hydrides: Potassium Hydride, Sodium hydride, Lithium Aluminum Hydride, 20 Diethylaluminium hydride, Diisobutylaluminum hydride 21 1.9. Nonmetal hydrides: Arsine, Boranes, Diethylarsine, diethylphosphine, Germane, 22 Phosphine, phenylphosphine, Silane, Methanetellurol (CH3TeH) 23 1.10. Non-metal alkyls: R3B, R3P, R3As; Tributylphosphine, Dichloro(methyl)silane 24 1.11. Used hydrogenation catalysts: Raney nickel, Palladium, Platinum 25 1.12. Activated Copper fuel cell catalysts, e.g. Cu/ZnO/Al2O3 26 1.13. Finely Divided Sulfides: Iron Sulfides (FeS, FeS2, Fe3S4), and Potassium Sulfide 27 (K2S) 28 REFERRAL
    [Show full text]
  • Synthesis of Lithium Peroxide from Hydrogen Peroxide and Lithium Hydroxide in Aqueous-Organic Medium: Wasteless Technology
    MATEC Web of Conferences 96, 00004 (2017) DOI: 10.1051/ matecconf/20179600004 REE-2016 Synthesis of Lithium Peroxide from Hydrogen Peroxide and Lithium Hydroxide in Aqueous-Organic Medium: Wasteless Technology Roman Nefedov* and Yury Ferapontov Tambov State Technical University, Tambov, Russia Abstract. Lithium is a rare element, and widely used in manufacturing, electronics, medicine, and etc. One of the important lithium compounds is lithium peroxide. It is a component of regenerating products to protect the human respiratory system from damaging factors of chemical and biological nature. This paper describes the methods of obtaining the lithium peroxide. All industrial techniques for the synthesis of lithium peroxide are presented. A critical assessment of these techniques is given. A new wasteless synthesis technology of lithium peroxide from Hydrogen Peroxide and Lithium Hydroxide in Aqueous-Organic Medium is presented. This technology allows obtaining the pure product containing Li2O2 up to 94 %. The possibility of the solvent regeneration by the anhydrous lithium hydroxide has been shown. The yield of the lithium – 98 % and a significant reduction in solvent consumption per unit of finished product has been obtained. 1 Introduction The use of ethanol is not a prerequisite for obtaining lithium peroxide, although it is beneficial in terms of that The inorganic peroxide compounds based on rare, lithium peroxide contained in it unlike other organic radioactive, and especially alkali metals have a wide substances practically insoluble (dissolved in methanol range of industrial applications (e.g., energy storage and about 3.5 g/L Li2O2. Ethanol can be replaced by other oxygen source, etc.) [1, 2]. organic solvents (methanol, pyridine, propanol, kenotic An identifying characteristic of inorganic peroxide and others [12, 14]).
    [Show full text]
  • Expansion of Domestic Production of Lithium Carbonate and Lithium Hydroxide to Supply US Battery Industry
    Expansion of Domestic Production of Lithium Carbonate and Lithium Hydroxide to Supply US Battery Industry Austin Devaney Jeff Davis Chemetall Foote Corp May 16, 2012 Project ID# ARRAVT010 This presentation does not contain any proprietary, confidential, or otherwise restricted information Overview Expand Lithium Raw Material Base in US Timeline Barriers Start Date: April 14, 2010 Geothermal Resource Strength and Viability of End Date: December, 2013 Geothermal resource Partners Budget Engineering: BE&K (a KBR DOE Share - $28.4 million company) Rockwood Share - $46.0 Environmental Assessment: million Nevada Bureau Land Mgmt Relevance: Domestic Source of Strategic Materials • Objectives – Expand domestic lithium carbonate and lithium hydroxide production to supply the US electric drive automotive market. – Deliver high quality lithium products to battery component manufacturers to produce high quality lithium ion batteries. – Create construction jobs over three years in the US and permanent jobs for production of lithium raw materials. – Stimulate the US economy with worthwhile long term benefits that will support the conversion to electric drive mobility. Relevance: Domestic Source of Strategic Materials • Milestones – Deliver battery grade lithium products to the DOE and component manufacturers in 2012 from this project. – Maintain the long term viability of domestic production of lithium raw materials by lowering operating cost and at the same time reducing fossil fuel based energy consumption. – Job Creation throughout 2010-2013 for
    [Show full text]
  • United States Patent Office Patented Jan
    3,711,407 United States Patent Office Patented Jan. 16, 1973 2 in the finished grease or during the neutralization step in 3,711,407 the Soap-making stage of grease manufacture. INCORPORATENG LITHIUM SALCYLATE OR THE The aliphatic alcohol whose ester is used in this inven LKE ENTO A GREASE tion will preferably be one whose boiling point is not so Richard J. Plumstead, Mississauga, Ontario, Canada, as high as to prevent its being driven off during the reaction, signor to Esso Research and Engineering Company, 5 Linden, N.Y. unless it is desired to have all or a portion of the alcohol No Drawing. Filed Nov. 18, 1970, Ser. No. 90,878 remain in the composition. Reaction temperatures can Int, C. C10m 5/14 range from about 150 F. to about 550 F., more usually U.S. C. 252-4 6 Claims from about 180° F. to about 380 F. In the case of greases, residual alcohol in the grease may be objection 10 able in that it may exert excessive softening characteris ABSTRACT OF THE DISCLOSURE tics. On the other hand, some softening action may actu An alkali metal salt and particularly a lithium salt ally be desirable where it is necessary to have a high of Salicylic acid or related hydroxy benzoic acid is in thickener content and cost is a secondary consideration. corporated into a lubricating oil or grease as an antioxi Generally the esters will be of C1 to about Caliphatic 15 alcohols, but preferably they will be about C to Cs dant by Saponifying an aliphatic alcohol ester of the hy aliphatic alcohols, including methanol, ethanol, propanol, droxy benzoic acid and then removing the water and isopropanol, secondary butanol, 2-methylbutanol, 2,2-di alcohol formed in the reaction.
    [Show full text]
  • Reintroduction of Lithium Into Recycled Electrode
    (19) TZZ Z_T (11) EP 2 248 220 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: H01M 10/052 (2010.01) H01M 10/42 (2006.01) 04.11.2015 Bulletin 2015/45 H01M 10/54 (2006.01) H01M 4/485 (2010.01) H01M 4/505 (2010.01) H01M 4/525 (2010.01) (2010.01) (21) Application number: 09713108.0 H01M 4/58 (22) Date of filing: 20.02.2009 (86) International application number: PCT/US2009/034779 (87) International publication number: WO 2009/105713 (27.08.2009 Gazette 2009/35) (54) REINTRODUCTION OF LITHIUM INTO RECYCLED ELECTRODE MATERIALS FOR BATTERY WIEDEREINFÜGUNG VON LITHIUM IN VERWERTETE ELEKTRODENMATERIALIEN FÜR BATTERIEN RÉINTRODUCTION DE LITHIUM DANS DES MATÉRIAUX D’ÉLECTRODES RECYCLÉS POUR BATTERIES (84) Designated Contracting States: (56) References cited: AT BE BG CH CY CZ DE DK EE ES FI FR GB GR EP-A1- 1 009 058 CN-A- 1 585 187 HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL JP-A- 11 054 159 US-A- 5 628 973 PT RO SE SI SK TR US-A- 5 679 477 US-A- 6 150 050 US-A1- 2003 180 604 US-A1- 2004 175 618 (30) Priority: 22.02.2008 US 30916 US-A1- 2005 003 276 US-A1- 2005 175 877 US-A1- 2005 244 704 US-A1- 2007 134 546 (43) Date of publication of application: US-A1- 2007 224 508 US-B1- 6 261 712 10.11.2010 Bulletin 2010/45 US-B2- 6 844 103 (73) Proprietor: Sloop, Steven E.
    [Show full text]
  • Lithium and Cobalt Same Purpose, Different Paths
    Energy and Commodities Lithium and cobalt Same purpose, different paths Adrian Casillas / Marcial Nava The commodities of a new energy era Lithium and cobalt are the latest vogue in commodity markets, as evidenced by the significant growth in their prices since 2016. On the London Metal Exchange (LME), the average spot price of cobalt went from $22,813 per metric ton in 1Q16 to $87,352 in 2Q18, a 282% increase. The weighted average stock price of the largest public cobalt mining companies went up 85% in the same period.1 Similarly, Asian and South American lithium-carbonate prices went up by 93% and 120%, respectively, and the weighted average stock price of the five largest lithium firms increased by 84%.2 Chart 1. Lithium Prices ($’000 per metric ton) Chart 2. LME Cobalt Spot ($’000 per metric ton) 25 100 90 20 80 70 15 60 10 50 40 5 30 0 20 2015 2016 2017 2018 10 Asia Lithium Carbonate 0 South America Lithium Carbonate 2015 2016 2017 2018 Source: BBVA Research and Bloomberg Source: BBVA Research and Bloomberg Lithium and cobalt are basic components of the lithium-ion batteries that power cell phones, computers, and electric vehicles (EVs).3 Although both metals have been in high demand for a while due to their use in consumer electronics, the recent spike in prices is largely the result of positive expectations generated by the rapid growth of electric vehicle sales. The share of demand for lithium used in the production of electric vehicles went from 20% in 2014 to 49% in 2018.
    [Show full text]
  • The Use of Lithium to Prevent Or Mitigate Alkali-Silica Reaction in Concrete Pavements and Structures
    The Use of Lithium to Prevent or Mitigate Alkali-Silica Reaction in Concrete Pavements and Structures PUBLIcatION NO. FHWA-HRT-06-133 MARCH 2007 Research, Development, and Technology Turner-Fairbank Highway Research Center 6300 Georgetown Pike McLean, VA 22101-2296 Foreword Progress is being made in efforts to combat alkali-silica reaction in portland cement concrete structures—both new and existing. This facts book provides a brief overview of laboratory and field research performed that focuses on the use of lithium compounds as either an admixture in new concrete or as a treatment of existing structures. This document is intended to provide practitioners with the necessary information and guidance to test, specify, and use lithium compounds in new concrete construction, as well as in repair and service life extension applications. This report will be of interest to engineers, contractors, and others involved in the design and specification of new concrete, as well as those involved in mitigation of the damaging effects of alkali-silica reaction in existing concrete structures. Gary L. Henderson, P.E. Director, Office of Infrastructure Research and Development Notice This document is disseminated under the sponsorship of the U.S. Department of Transportation in the interest of information exchange. The U.S. Government assumes no liability for its contents or use thereof. This report does not constitute a standard, specification, or regulation. The U.S. Government does not endorse products or manufacturers. Trade or manufacturers’ names appear herein only because they are considered essential to the objective of this manual. Quality Assurance Statement The Federal Highway Administration (FHWA) provides high-quality information to serve Government, industry, and the public in a manner that promotes public understanding.
    [Show full text]