WO2013152260A1 - Élimination du plomb présent dans des matières solides - Google Patents

Élimination du plomb présent dans des matières solides Download PDF

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Publication number
WO2013152260A1
WO2013152260A1 PCT/US2013/035379 US2013035379W WO2013152260A1 WO 2013152260 A1 WO2013152260 A1 WO 2013152260A1 US 2013035379 W US2013035379 W US 2013035379W WO 2013152260 A1 WO2013152260 A1 WO 2013152260A1
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WO
WIPO (PCT)
Prior art keywords
acid
ammonium
sodium
triazole
potassium
Prior art date
Application number
PCT/US2013/035379
Other languages
English (en)
Inventor
Michael B. Korzenski
Tianniu Chen
Ping Jiang
Original Assignee
Advanced Technology Materials, 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 Advanced Technology Materials, Inc. filed Critical Advanced Technology Materials, Inc.
Priority to CA 2869431 priority Critical patent/CA2869431A1/fr
Priority to US14/389,142 priority patent/US20150050199A1/en
Publication of WO2013152260A1 publication Critical patent/WO2013152260A1/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
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/52—Recovery of material from discharge tubes or lamps
    • 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
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/60—Glass recycling
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]

Definitions

  • the present invention relates generally to a composition that substantially removes lead from solid materials, and a method of using said composition.
  • CRTs cathode ray tubes
  • the safe disposal of CRTs present a serious environmental challenge since they contain leaded glass (primarily in the funnel, neck and frit) which may be readily leached from a landfill by acidic water.
  • the lead content in the glass of a CRT can be as high as 20%, which means that a single 34" television might contain more than 1 kg of lead.
  • Lead is toxic and is known to damage the body's nervous and reproductive systems and kidneys. It can also cause high blood pressure and anemia. Lead is especially harmful to the developing brains of fetuses and young children and to pregnant women. As a result, lead has been banned from fuel, paint, pipes and all new electronics.
  • Recycling glass is manually intensive and expensive. This is so because one vendor of glass may use different concentrations of lead or other metals in their glass products than another glass vendor. Waste disposal facilities receive glass waste that is not separated, and the waste disposal facilities have no effective techniques for automatically separating different glass wastes from one another. Because of the expense and time consuming nature associated with recycling glass waste, many waste disposal facilities have resorted to the illegal disposal of glass waste.
  • the present invention generally relates to a composition that substantially removes lead from solid materials, and a method of using said composition.
  • the concentration of lead in the solid materials following processing is low enough that the solid materials can be reused and/or disposed of at minimal cost to the processor.
  • the solid materials comprise glass, such as cathode ray tube glass.
  • a method of leaching lead or other heavy metals from solid materials comprising: pulverizing the solid materials to size in a range from about 10 microns to about 3 mm; introducing the pulverized solid materials into a chemical processing vessel comprising a leaching composition to form a slurry; agitating the slurry to leach the lead or other heavy metals from the solid material into the leaching composition, wherein the leaching composition comprises at least one oxidant, at least one solvent, optionally at least one metal chelator, optionally at least one accelerator/NO x (nitrogen oxide) suppressor, and optionally at least one etchant.
  • a leaching composition comprising at least one oxidant, at least one solvent, optionally at least one metal chelator, optionally at least one accelerator/NO x (nitrogen oxide) suppressor, and optionally at least one etchant.
  • the present invention generally relates to a composition that substantially removes lead from solid materials, and a method of using said composition to remediate lead from said solid materials.
  • the concentration of lead in the solid materials following processing is low enough that the solid materials can be reused and/or disposed of at minimal cost to the processor.
  • the solid materials comprise glass, such as cathode ray tube glass. It is also contemplated that the compositions described herein can be used to remove lead from soil, electronic equipment, solder sludge, and paint chips.
  • substantially devoid corresponds to less than about 2 wt. %, more preferably less than 1 wt. %, and most preferably less than 0.1 wt. % of the composition, based on the total weight of said composition.
  • substantially removed is defined herein to mean that more than 95 wt. % of the heavy metal originally present is dissolved or otherwise solubilized, preferably more than 98 wt. %, more preferably more than 99 wt. %, and most preferably more than 99.9 wt. %.
  • the term "leaches” corresponds to the complete removal or extraction of the lead or other metals from the material into the leaching composition or the partial removal or extraction of the lead or other metals from the material into the leaching composition.
  • the lead or other metals is dissolved or otherwise solubilized in the leaching composition, preferably dissolved.
  • the "material” corresponds to any solid that requires lead or other metal remediation including, but not limited to, CRT glass waste, soil, paint chips, electronic waste, and solder sludge.
  • glass waste particularly glass waste associated with CRT monitors or televisions, includes unacceptable levels of lead, or other heavy metals (e.g., cadmium, mercury, selenium, arsenic, and the like), that need to be removed or decreased to acceptable levels before the glass waste can be disposed of in a landfill.
  • lead, or other heavy metals e.g., cadmium, mercury, selenium, arsenic, and the like
  • glass waste can economically and safely be disposed of well within the current EPA standards by safely and efficiently removing lead and other heavy metals from the glass waste.
  • the glass can safely be recycled for reuse as glass or for incorporation into other products such as concrete or asphalt.
  • the material such as CRT glass waste, soil, paint chips, electronic waste, and solder sludge
  • CRT glass waste can be fed to a grinding device such as a high-speed hammer mill, grinder, or any other size reduction means.
  • the material is pulverized to size in a range from about 10 microns to about 3 mm.
  • a separation device classifies the material particles by size.
  • the separation device can be configured to classify the material particles into sizes between less than 3 mm and sizes greater than approximately 10 microns.
  • Material particles have a desired diameter size between about 10 microns and about 3 mm or less, although it should be appreciated that diameters less than 10 microns and greater than 3 mm can be processed as well using the composition and method described herein.
  • the pulverized material particles are then introduced into a chemical processing vessel comprising a leaching composition, which will be described below.
  • the chemical processing vessel can be a drum set-up, a tumbler system, a mixing apparatus, or an equivalent thereof.
  • the leaching composition in combination with the pulverized material particles results in the formation of a slurry, which can be agitated by stirring, mixing, tumbling, shaking, etc., in the presence or absence of added heat.
  • the temperature of the slurry during agitation is about 30°C to about 150°C, preferably about 30°C to about 70°C.
  • the slurry can alternatively be circulated using a pumping system.
  • a feed-and-bleed system is contemplated whereby some amount of the leaching composition is removed for processing and fresh or recycled leaching composition added to the chemical processing vessel.
  • the slurry can be agitated for time in a range from about 5 min to 6 hr, depending on the volume of leaching composition and the amount of pulverized material particles added.
  • the leaching composition is removed from the vessel and/or the material particles are filtered from the leaching composition.
  • the material particles are preferably rinsed with water to remove residual leaching composition from the material particles. Thereafter, the material particles can be filtered again.
  • the leaching composition can be reused for another cycle of material particle treatment or treated for disposal.
  • the leaching composition can be reused until the leaching composition is saturated with lead and other metals and no longer efficiently solubilizes lead into the leaching composition.
  • Ion-exchange resins selective to lead can be used in combination with the leaching composition to further extend the life of the bath.
  • the leaching composition can be recycled using diffusion dialysis and reused. With regards to disposal procedures, when no longer viable, the leaching composition can be rendered essentially non-toxic by electrowinning or precipitating the Pb and neutralizing the excess acidity.
  • particles consisting of glass are substantially devoid of lead and other heavy metals on their surface due to the mixing cycles with the leaching composition. Moreover, any lead or heavy metal remaining within the filtered glass particles cannot be extracted from the filtered glass particles because of the size of the glass particle and the fact that the remaining heavy metals are sequestered in the core. Products, such as road materials and others, can include the filtered glass particles with assurance that lead or other heavy metals (e.g., cadmium, mercury, arsenic, selenium, and others) will not be released. Therefore, the particles consisting of glass can be used for other products such as foundations for roads, mixtures for concrete, etc.
  • lead or other heavy metals e.g., cadmium, mercury, arsenic, selenium, and others
  • the leaching composition can penetrate the entire material and the lead can be substantially removed from the material.
  • the material comprises glass, only the lead on the surface of the glass is removed. This is advantageous because the lead in the core of the particle is sequestered and not easily removed if disposed of in a landfill. That said, it is theorized that if the leaching composition can solubilize the glass particle then substantial removal of the lead can be effectuated and substantially lead-free glass re -precipitated and sold for reuse.
  • substantially lead-free corresponds to a concentration of lead in the material less than about 5 wt%, preferably less than about 2 wt%, and even more preferably less than 1 wt%, based on the total weight of the solid glass.
  • the leaching composition is formulated to oxidize and sequester the lead thereby removing same from the material.
  • the leaching composition comprises, consists of, or consists essentially of at least one oxidant, at least one solvent, optionally at least one metal chelator, optionally at least one accelerator/NO x (nitrogen oxide) suppressor, optionally at least one etchant.
  • the leaching composition comprises, consists of, or consists essentially of at least two oxidants, at least one solvent, and at least one accelerator/NO x (nitrogen oxide) suppressor.
  • the leaching composition comprises, consists of, or consists essentially of at least one oxidant, at least one solvent, at least one metal chelator, and at least one accelerator/NO x (nitrogen oxide) suppressor.
  • the components of the leaching composition comprising, consisting of, or consisting essentially of at least two oxidants, at least one solvent, and at least one accelerator/NO x (nitrogen oxide) suppressor can be present in the following amounts, based on the total weight of the leaching composition:
  • the components of the leaching composition comprising, consisting of, or consisting essentially of at least one oxidant, at least one solvent, at least one metal chelator, and at least one accelerator/NO x (nitrogen oxide) suppressor can be present in the following amounts, based on the total weight of the leaching composition:
  • Oxidizing agents are included in the leaching composition to oxidize the metals to be removed into an ionic form and accumulate highly soluble salts of dissolved metals.
  • Oxidizing agents contemplated herein include, but are not limited to, ozone, nitric acid (HN0 3 ), bubbled air, cyclohexylaminosulfonic acid, , hydrogen peroxide (H 2 0 2 ), oxone (potassium peroxymonosulfate, 2KHSO 5 KHSO 4 K 2 SO 4 ), ammonium polyatomic salts (e.g., ammonium peroxomonosulfate, ammonium chlorite (NH 4 C10 2 ), ammonium chlorate (NH 4 CIO 3 ), ammonium iodate (NH 4 IO 3 ), ammonium perborate (NH 4 BO 3 ), ammonium perchlorate (NH 4 CIO 4 ), ammonium periodate (NH 4 IO 3 ), ammonium
  • oxidizing agents further include alkanesulfonic acids (e.g., methanesulfonic acid (MSA), ethanesulfonic acid, 2 -hydroxy ethanesulfonic acid, n-propanesulfonic acid, isopropanesulfonic acid, isobutenesulfonic acid, n-butanesulfonic acid, and n-octanesulfonic acid).
  • the oxidizing agents can include a combination of the any of the species defined herein as oxidizing agent.
  • the oxidizing agent may be introduced to the first composition at the manufacturer, prior to introduction of the leaching composition to the particles, or alternatively in situ.
  • the oxidizing agent comprises methanesulfonic acid, nitric acid, or a combination of methanesulfonic acid and nitric acid.
  • the oxidizing agent in the leaching composition preferably comprises an alkane sulfonic acid (e.g., MSA) and nitric acid, wherein the alkane sulfonic acid is present in an amount ranging from 0.1 to 85 wt%, more preferably from 5 to 45 wt%, and the nitric acid is present in an amount of about 0.1 to 80 wt%, preferably from about 1 to 40 wt%.
  • an alkane sulfonic acid e.g., MSA
  • nitric acid is present in an amount ranging from 0.1 to 85 wt%, more preferably from 5 to 45 wt%
  • the nitric acid is present in an amount of about 0.1 to 80 wt%, preferably from about 1 to 40 wt%.
  • Metal chelators are included to complex the metal ions generated by the oxidizing agent.
  • Metal chelators contemplated herein include, but are not limited to: ⁇ -diketonate compounds such as acetylacetonate, l,l ,l-trifluoro-2,4-pentanedione, and l,l,l,5,5,5-hexafluoro-2,4-pentanedione; carboxylates such as formate and acetate and other long chain carboxylates; and amides (and amines), such as bis(trimethylsilylamide) tetramer.
  • Additional chelating agents include amines and amino acids (i.e.
  • glycine serine, proline, leucine, alanine, asparagine, aspartic acid, glutamine, valine, and lysine
  • citric acid acetic acid, maleic acid, oxalic acid, malonic acid, succinic acid, phosphonic acid, phosphonic acid derivatives such as hydro xyethylidene diphosphonic acid (HEDP), 1 -hydroxyethane- 1,1-diphosphonic acid, nitrilo-tris(methylenephosphonic acid), nitrilotriacetic acid, iminodiacetic acid, etidronic acid, ethyl enediamine, ethyl enediaminetetraacetic acid (EDTA), and (1,2- cyclohexylenedinitrilo)tetraacetic acid (CDTA), uric acid, tetraglyme, pentamethyldiethylenetriamine (PMDETA), l,3,5-triazine-2,
  • the metal chelator comprises ammonium chloride, sodium chloride, lithium chloride, potassium chloride, ammonium sulfate, hydrochloric acid, sulfuric acid, and combinations thereof, most preferably sodium chloride, sulfuric acid, or a combination of sodium chloride and sulfuric acid.
  • NO x suppressors are preferably included when the leaching composition includes nitric acid. Surprisingly, however, the NO x suppressors are also accelerators of the metal etch rates so they can be added even if the leaching composition does not include nitric acid.
  • NO x suppressors/accelerators contemplated include, but are not limited to, ascorbic acid, adenosine, L(+)- ascorbic acid, isoascorbic acid, ascorbic acid derivatives, citric acid, ethylenediamine, gallic acid, oxalic acid, tannic acid, ethyl enediaminetetraacetic acid (EDTA), uric acid, 1,2,4-triazole (TAZ), triazole derivatives (e.g., benzotriazole (BTA), tolyltriazole, 5-phenyl-benzotriazole, 5-nitro- benzotriazole, 3-amino-5-mercapto-l,2,4-triazole, l-amino-l,2,4-triazole, hydroxybenzotriazole, 2-(5- amino-pentyl)-benzotriazole, 1 -amino-1 ,2,3 -triazole, l-amino-5-
  • Solvents contemplated herein include water, preferably deionized water, as well as organic solvent such as alcohols, glycol ethers, glycols, and carbonates, including, but not limited to, methanol, ethanol, isopropanol, butanol, and higher alcohols (including diols, triols, etc.), ethylene glycol, propylene glycol, butylene carbonate, ethylene carbonate, propylene carbonate, dipropylene glycol, diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, diethylene glycol monoethyl ether, triethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether (i.e., butyl carbitol), triethylene glycol monobutyl ether, ethylene glycol monohexyl ether, diethylene glycol monohexyl ether, ethylene glycol phen
  • the at least one etchant can include at least one carbonate species, at least one hydroxide species and/or at least one fluoride species.
  • Carbonates include, but are not limited to, sodium carbonate, potassium carbonate, sodium hydrogen carbonate, and combinations thereof.
  • Hydroxides contemplated include, but are not limited to, alkali hydroxides, alkaline earth metal hydroxides, metal ion-free hydroxides, and combinations thereof such as LiOH, NaOH, KOH, RbOH, CsOH, Mg(OH) 2 , Ca(OH) 2 , Sr(OH) 2 , Ba(OH) 2 , NR 4 OH, wherein R can be the same as or different from one another and include H, C C 6 alkyl (e.g., methyl, ethyl, propyl, butyl, pentyl, hexyl) or C 6 - Cio aryl (e.g., benzyl), and combinations thereof.
  • alkali hydroxides e.g., alkaline earth metal hydroxides, metal ion-free hydroxides, and combinations thereof
  • the at least one fluoride species may comprise a species selected from the group consisting of xenon difluoride; HF; pentamethyldiethylenetriammonium trifluoride; ammonium bifluoride; triethylaminogallate trihydrofluoride; alkyl hydrogen fluoride (NRH 3 F), wherein each R is independently selected from hydrogen and C 1 -C4 alkyl (e.g., methyl, ethyl, propyl, butyl); dialkylammonium hydrogen fluoride (NR 2 H 2 F), wherein each R is independently selected from hydrogen and C C 4 alkyl; trialkylammonium hydrogen fluoride (NR 3 HF), wherein each R is independently selected from hydrogen and C 1 -C4 alkyl; trialkylammonium trihydrogen fluoride (NR 3 :3HF), wherein each R is independently selected from hydrogen and C 1 -C4 alkyl; ammonium fluorides of the formula R 4 NF, wherein each
  • the fluoride source comprises HF, ammonium fluoride, or combinations thereof.
  • the amount of etchant is preferably in a range from about 0.01 wt% to about 10 wt%, based on the total weight of the composition.
  • an easily recyclable leaching composition can be employed in a closed- loop process generating minimal waste.
  • the leaching composition includes MSA
  • the MSA is easily recycled using diffusion dialysis.
  • the leaching composition comprises, consists or consists essentially of MSA, nitric acid, and ATAZ.
  • the leaching composition comprises, consists of, or consists essentially of MSA, sulfuric acid, ATAZ, and NaCl.
  • the leaching composition and the pulverized CRT glass can be placed into a high pressure autoclave for the leaching process.
  • Water is known to have very strong oxidizing properties at hydrothermal (>100°C and >100 psi) conditions and near critical conditions (>300°C and >3000 psi). Accordingly, at these hydrothermal conditions, water alone may be strong enough to oxidize the lead so that the chelator can extract the lead.
  • Suitable chelators include chloride, iodide, hydroxide, or sulfate salts (e.g., as described herein), wherein hydroxide or sulfate are preferred because they will not corrode steel vessels required for high pressure applications and they will readily precipitate from solution upon cooling and depressurizing of the vessel.
  • the resulting lead-free glass may be remelted for reuse (e.g., bricks, tiles, foam), mixed into, for example, asphalt or cement as a filler, or sent to a landfill for safe disposal.
  • Lead can be removed from the solution in the form of an oxide or salt and may be resold. The system is closed so that no vapors escapes and all of the chemistry and the rinse water are recycled for reuse in the process. Small amounts of rinse water are discharged, but it is first neutralized and has less than part-per- million trace metals and no organics.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne une composition de lixiviation qui élimine pratiquement le plomb présent dans des matières solides, ainsi qu'un procédé d'utilisation de ladite composition. De préférence, selon l'invention, la concentration en plomb dans les matières solides à la suite du traitement est suffisamment faible pour que les matières solides puissent être réutilisées et/ou éliminées à un coût minimal pour le traiteur. De préférence, les matières solides comprennent du verre, tel que du verre issu de tubes cathodiques.
PCT/US2013/035379 2012-04-06 2013-04-05 Élimination du plomb présent dans des matières solides WO2013152260A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CA 2869431 CA2869431A1 (fr) 2012-04-06 2013-04-05 Elimination du plomb present dans des matieres solides
US14/389,142 US20150050199A1 (en) 2012-04-06 2013-04-05 Removal of lead from solid materials

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201261621073P 2012-04-06 2012-04-06
US61/621,073 2012-04-06

Publications (1)

Publication Number Publication Date
WO2013152260A1 true WO2013152260A1 (fr) 2013-10-10

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US (1) US20150050199A1 (fr)
CA (1) CA2869431A1 (fr)
WO (1) WO2013152260A1 (fr)

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WO2016081030A1 (fr) * 2014-11-18 2016-05-26 Aqua Metals Inc. Dispositifs et procédé améliorés pour le recyclage sans fonderie d'accumulateurs au plomb
US10316420B2 (en) 2015-12-02 2019-06-11 Aqua Metals Inc. Systems and methods for continuous alkaline lead acid battery recycling
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