WO2024259327A2 - Procédés d'isolement de précurseurs cimentaires - Google Patents

Procédés d'isolement de précurseurs cimentaires Download PDF

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Publication number
WO2024259327A2
WO2024259327A2 PCT/US2024/034134 US2024034134W WO2024259327A2 WO 2024259327 A2 WO2024259327 A2 WO 2024259327A2 US 2024034134 W US2024034134 W US 2024034134W WO 2024259327 A2 WO2024259327 A2 WO 2024259327A2
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WIPO (PCT)
Prior art keywords
solution
calcium
leaching agent
isolate
slag
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Ceased
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PCT/US2024/034134
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English (en)
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WO2024259327A3 (fr
Inventor
Rouzbeh SAVARY
Sanan EMINOV
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C-Crete Technologies LLC
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C-Crete Technologies LLC
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Publication of WO2024259327A2 publication Critical patent/WO2024259327A2/fr
Publication of WO2024259327A3 publication Critical patent/WO2024259327A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/02—Portland cement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • 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
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/402—Alkaline earth metal or magnesium compounds of magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/602—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/604—Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/608—Sulfates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00017—Aspects relating to the protection of the environment
    • C04B2111/00019—Carbon dioxide sequestration
    • 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

  • the techniques described herein relate to a method of separating materials, including: providing an input material including one or more metals, contacting the input material with a leaching agent to yield a solid residue and a solution, and performing one or more separations on the solution to isolate the one or more metal compounds.
  • the techniques described herein relate to a method, wherein the input material includes basalt, apatite, gabbro, wollastonite, skarns, anorthosite, feldspar, anorthite, pyroxene, margarite, electric arc furnace slag (EAF), reducing steel slag, oxidizing steel slag, converter steel slag, basic oxygen furnace slag, ladle slag, slow or fast cooled steel slag, blast furnace slag, granulated blast furnace slag, ground granulated blast furnace slag (GGBFS), air- cooled slag, copper slag, Solvay slag, phosphorous slag, bauxite residue/slag, zinc slag, lead slag, fly ash, bottom ash, municipal solid waste incinerated ash, recycled concrete, or combinations thereof.
  • EAF electric arc furnace slag
  • reducing steel slag oxidizing steel slag
  • the techniques described herein relate to a method, wherein the one or more metal compounds include calcium, aluminum, iron, magnesium, or combinations thereof. [0006] In some aspects, the techniques described herein relate to a method, further including sizing the input material by grinding, milling, sieving, or combinations thereof. Attorney Docket No.: 440773-000402 [0007] In some aspects, the techniques described herein relate to a method, further including sizing the input material by milling by one or more of a ball mill, tower mill, pebble mill, high pressure grinding rolls, autogenous mill, rod mill, or combinations thereof.
  • the techniques described herein relate to a method, wherein the leaching agent includes an ammonium salt or a strong acid.
  • the techniques described herein relate to a method, wherein the ammonium salt includes NH4Cl, (NH4)3PO4, (NH4)2SO4, NH4NO3, or combinations thereof.
  • the techniques described herein relate to a method, wherein the strong acid includes HCl, HBr, HI, HNO3, H3PO4, H2SO4, HClO4, or combinations thereof.
  • the techniques described herein relate to a method, wherein the input material and the leaching agent are present in a ratio of about 1:1 to about 1:15 by mass.
  • the techniques described herein relate to a method, wherein contacting the input material with the leaching agent includes heating the input material and the leaching agent together. [0013] In some aspects, the techniques described herein relate to a method, wherein contacting the input material with the leaching agent includes heating the input material and the leaching agent to a temperature of about 200 °C to about 450 °C. [0014] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include adjusting the pH of the solution, heating the solution, or combinations thereof.
  • the techniques described herein relate to a method, wherein the one or more separations include adjusting the pH of the solution to between about 4.0 and about 10.5 to isolate the one or more metal compounds. [0016] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include adjusting the pH of the solution to between about 4.0 and about 5.5 to isolate the one or more metal compounds. [0017] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include adjusting the pH of the solution to between about 5.5 to about 7.5 to isolate the one or more metal compounds.
  • the techniques described herein relate to a method, wherein the one or more separations include adjusting the pH of the solution to between about 8.0 to about 10.5 to isolate the one or more metal compounds. [0019] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include heating the solution to about 100 °C to about 200 °C to isolate the one or more metal compounds. [0020] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include heating the solution to about 100 °C to about 150 °C to isolate the one or more metal compounds.
  • the techniques described herein relate to a method, wherein the one or more separations include heating the solution to about 150 °C to about 200 °C to isolate the one or more metal compounds. [0022] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include a first separation to isolate a first metal compound. [0023] In some aspects, the techniques described herein relate to a method, wherein the one or more separations include a first separation to isolate a first metal and a second separation to isolate a second metal compound.
  • the techniques described herein relate to a method, wherein the one or more separations include a first separation to isolate a first metal, a second separation to isolate a second metal, and a third separation to isolate a third metal compound. [0025] In some aspects, the techniques described herein relate to a method, further including utilizing the one or more metal compounds in ordinary Portland cement production. [0026] In some aspects, the techniques described herein relate to a method, further including utilizing the one or more metal compounds in carbon dioxide capture. [0027] In some aspects, the techniques described herein relate to a method, further including recovering the leaching agent from the solution.
  • the techniques described herein relate to a method, wherein recovering the leaching agent from the solution includes applying an electric current to the solution, Attorney Docket No.: 440773-000402 adjusting the temperature of the solution, contacting the solution with CO2, contacting the solution with ammonia, or combinations thereof.
  • the techniques described herein relate to a method, wherein recovering the leaching agent from the solution includes contacting the solution with CO2 and ammonia to produce the leaching agent and calcium carbonate.
  • the techniques described herein relate to a method, wherein recovering the leaching agent does not require heat, electricity, or a combination thereof.
  • the techniques described herein relate to a method, wherein the one or more metal compounds includes calcium carbonate, and wherein the method further includes using the calcium carbonate to produce ordinary Portland cement.
  • the techniques described herein relate to a method, further including producing CO 2 and using the CO2 to recover the leaching agent, produce ordinary Portland cement, or a combination thereof.
  • the techniques described herein relate to a method, wherein the solid residue includes silica.
  • the techniques described herein relate to a method, further including utilizing the solid residue in ordinary Portland cement production.
  • the techniques described herein relate to a method, further including utilizing the solid residue in carbon dioxide capture.
  • the techniques described herein relate to a method, further including combining the solid residue with one or more alkali activators to produce a cementitious material. [0037] In some aspects, the techniques described herein relate to a method, wherein the input material includes calcium. [0038] In some aspects, the techniques described herein relate to a method, further including a final separation to isolate a calcium species including calcium chloride, calcium carbonate, calcium bicarbonate, calcium hydroxide, calcium oxide, or combinations thereof. Attorney Docket No.: 440773-000402 [0039] In some aspects, the techniques described herein relate to a method, further including utilizing the calcium species in ordinary Portland cement production.
  • the techniques described herein relate to a method, further including utilizing the calcium species in carbon dioxide capture. [0041] In some aspects, the techniques described herein relate to a method, further including combining the calcium species with the solid residue to produce a cementitious material. [0042] In some aspects, the techniques described herein relate to a method, further including combining the calcium species with one or more alkali activators to produce a cementitious material. [0043] In some aspects, the techniques described herein relate to a method, further including combining the calcium species with one or more alkali activators and the solid residue to produce a cementitious material.
  • FIGURE is an illustrative flow diagram of a method of separating materials, according to embodiments of the present disclosure.
  • DETAILED DESCRIPTION [0045] Provided herein are methods of separating materials.
  • the methods disclosed herein include isolating cementitious precursors.
  • An exemplary method may include the extraction of metal compounds from calcium-containing compounds and/or industrial by-products wherein the metal compounds can be used as precursors for cementitious materials.
  • a method of separating materials which includes providing an input material which includes one or more metal compounds or metals; contacting the input material with a leaching agent to yield a solid residue and a solution; and performing one or more separations on the solution to isolate one or more metal compounds.
  • the method may be repeated and/or performed continuously, which may include recovering one or more of the leaching agent or other components produced during the steps of the present method.
  • Attorney Docket No.: 440773-000402 [0047]
  • the FIGURE is an illustrative flow diagram of a method of separating materials, according to embodiments of the present disclosure.
  • the method can include providing an input material 102, contacting the input material with a leaching agent 104 to yield a solid residue 106 and a solution 108.
  • performing the one or more separations can include performing a first separation 110 on the solution 108 to isolate a first metal compound 120.
  • the method further includes a second separation 112 to isolate a second metal compound 122, a third separation 114 to isolate a third metal compound 124, and a fourth separation 116 to isolate a calcium species 126.
  • the method may include the separation 110 to isolate the first metal compound 120 and the separation 116 to isolate the calcium species 126.
  • the input material 102 includes basalt, apatite, gabbro, wollastonite, skarns, anorthosite, feldspar, anorthite, pyroxene, margarite, electric arc furnace slag (EAF), reducing steel slag, oxidizing steel slag, converter steel slag, basic oxygen furnace slag, ladle slag, slow or fast cooled steel slag, ground granulated blast furnace slag (GGBFS), air-cooled slag, copper slag, Solvay slag, phosphorous slag, bauxite residue/slag, zinc slag, lead slag, fly ash, bottom ash, municipal solid incinerated ash, recycled concrete, or combinations thereof and any other calcium-containing mineral.
  • EAF electric arc furnace slag
  • GGBFS ground granulated blast furnace slag
  • the input material 102 may include any industrial byproducts or wastes which may contain calcium and other metals.
  • the one or more metal compounds include calcium, aluminum, iron, magnesium, or combinations thereof.
  • the one or more metal compounds are in the form of metal oxides, metal hydroxides, metal carbonates, metal chlorides, elemental metal, or combinations thereof.
  • the input material 102 does not include carbonated material. Without wishing to be bound by theory, using such an input material may avoid CO2 production during the leaching process.
  • Examples of such input materials include but are not limited to basalts, gabbro, wollastonite, skarns, anorthosite, feldspar, apatite, anorthite, pyroxene, margarite, electric arc furnace slag (EAF), reducing steel slag, oxidizing steel slag, converter steel slag, basic oxygen furnace slag, ladle slag, slow or fast cooled steel slag, blast furnace slag, granulated blast furnace skag, ground granulated blast furnace slag (GGBFS), air-cooled slag, copper slag, Solvay slag, phosphorous slag, bauxite residue/slag, zinc slag, lead slag, fly ash, bottom ash, municipal solid waste incinerated ash, recycled cement, recycled concrete, or a combination of thereof and any other calcium-containing mineral or waste material.
  • EAF electric arc furnace slag
  • the input material 102 includes at least about 5 wt. % calcium, such as about 5 wt. % calcium, about 10 wt. % calcium, about 15 wt. % calcium, about 20 wt. %, about 25 wt. % calcium, about 30 wt. % calcium, about 35 wt. % calcium, about 40 wt. % calcium, about 45 wt. % calcium, about 50 wt. % calcium, about 55 wt. % calcium, about 60 wt. % calcium, about 65 wt. % calcium, about 70 wt.
  • 5 wt. % calcium such as about 5 wt. % calcium, about 10 wt. % calcium, about 15 wt. % calcium, about 20 wt. %, about 25 wt. % calcium, about 30 wt. % calcium, about 35 wt. % calcium, about 40 wt. % calcium, about 45 wt. %
  • the method may further include sizing the input material 102 by grinding, milling, sieving, or combinations thereof. In some embodiments, the method further includes sizing the input material by milling by one or more of a ball mill, tower mill, vertical mill, pebble mill, high pressure grinding rolls, autogenous mill, rod mill, or combinations thereof. In some embodiments, the input material is milled for a time is between about 0 minutes to about 30 minutes. In some embodiments, the milling time is about 1 hour. In some embodiments, the milling time is about 2 hours. In some embodiments, the milling time is about 3 hours.
  • the milling time is about 6 hours. In some embodiments, the milling time is about 8 hours. In some embodiments, the input material is milled for a time of about 0 minutes (such that the input material is not milled) to about 8 hours, or any range or value contained therein.
  • the method may include sizing the input material 102 to a mean particle size of about 1 ⁇ m to about 10 ⁇ m, about 1 ⁇ m to about 20 ⁇ m, about 1 ⁇ m to about 50 ⁇ m, about 1 ⁇ m to about 100 ⁇ m, about 1 ⁇ m to about 150 ⁇ m, about 1 ⁇ m to about 200 ⁇ m, about 1 ⁇ m to about 500 ⁇ m, about 1 ⁇ m to about 1000 ⁇ m, or any range or value contained therein.
  • the leaching agent 104 includes an ammonium salt or a strong acid.
  • the ammonium salt includes NH4Cl, (NH4)3PO4, (NH4)2SO4, NH4NO3, or combinations thereof.
  • the strong acid includes HCl, HBr, HI, HNO 3 , H 3 PO 4 , H 2 SO 4 , HClO 4 , or combinations thereof.
  • the input material 102 and the leaching agent 104 are present in a mass ratio of about 1:1 to about 1:15 by mass.
  • the ratio of the input material to the leaching agent may be about 1:1, about 1:2, about 1:3, about 1:4, about 1:5, about 1:6, about 1:7, about 1:8, about 1:9, about 1:10, about 1:11, about 1:12, about 1:13, about 1:14, about 1:15, or any range or value contained therein.
  • Attorney Docket No.: 440773-000402 [0056]
  • the leaching agent 104 includes an aqueous solution, such as aqueous HCl.
  • the concentration of the leaching agent is at least about 10%, such as about 10%, about 15%, about 20%, about 25%, about 30%, about 35%, about 40%, or any range or value contained therein.
  • the concentration of the leaching agent is about 0.1 M to about 10 M, such as about 0.1 M, about 0.5 M, about 1 M, about 1.5 M, about 2 M, about 2.5 M, about 3 M, about 3.5 M, about 4 M, about 4.5 M, about 5 M, about 5.5 M, about 6 M, about 6.5 M, about 7 M, about 7.5 M, about 8 M, about 8.5 M, about 9 M, about 9.5 M, about 10 M, or any range or value contained therein.
  • Contacting the input material 102 with the leaching agent 104 may include heating the input material and the leaching agent together. In some embodiments, the input material is heated together with the leaching agent to initiate a leaching process.
  • the input material and the leaching agent are both solids and are heated to a temperature of at least about 100 °C to at least about 450 °C.
  • the input material and the leaching agent are heated to at least about 100 °C, at least about 150 °C, at least about 200 °C, at least about 250 °C, at least about 300 °C, at least about 350 °C, at least about 400 °C, at least about 450 °C, or any range or value contained therein.
  • contacting the input material 102 with the leaching agent 104 includes contacting the input material (which may be a solid) with an aqueous solution of the leaching agent.
  • the input material is heated together with the aqueous solution of the leaching agent to initiate the leaching process.
  • the input material is heated with the aqueous solution of the leaching agent to a temperature of at least about 30 °C, such as about 30 °C, about 35 °C, about 40 °C, about 45 °C, about 50 °C, about 60 °C, about 70 °C, about 80 °C, about 90 °C, about 100 °C, about 110 °C, about 120 °C, or any range or value contained therein.
  • the input material 102 and the leaching agent 104 are heated for at least about 0.1 hour.
  • the input material and the leaching agent are heated for at least about 1 hour. In some embodiments, the input material and the leaching agent are heated for at least about 2 hours. In some embodiments, the input material and the leaching agent are heated for at least about 3 hours. In some embodiments, the input material and the leaching agent are heated for at least about 4 hours. In some embodiments, the input material and the leaching agent are heated for at least about 8 hours. In some embodiments, the input material and the leaching agent are heated for at least about 16 hours. In some Attorney Docket No.: 440773-000402 embodiments, the input material and the leaching agent are heated for at least about 24 hours.
  • the input material and the leaching agent may be heated for at least about 1 hour to at least about 24 hours or any range or value contained therein.
  • contacting the input material 102 with the leaching agent 104 includes stirring.
  • the input material may be stirred with the leaching agent at about 100 RPM, about 200 RPM, about 300 RPM, about 400 RPM, about 500 RPM, about 600 RPM, about 700 RPM, about 800 RPM, about 900 RPM, or any range or value contained therein.
  • the input material 102 and the leaching agent 104 are combined with water after heating. In some embodiments, heating the input material with the leaching agent produces ammonia gas, which may be captured and dissolved in water.
  • the ammonia gas captured during the heating is used to precipitate one or more metal compounds from the solution and regenerate the leaching agent.
  • the input material 102 and the leaching agent 104 are both solids.
  • the solid input material and leaching agent may be combined as described herein to provide a solid mixture.
  • the solid mixture may be mixed with water after heating to leach out the one or more metal compounds, which may be soluble in water.
  • the water to solid mixture ratio is about 5:1, about 10:1, about 100:1, about 1000:1, or any range or value contained therein.
  • the input material 102 is a solid and the leaching agent 104 is a liquid.
  • the ratio of solid (input material) to liquid (leaching agent) is about 5%/95%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 10%/90%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 20%/85%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 25%/75%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 30%/70%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 40%/60%. In some embodiments, the ratio of solid (input material) to liquid (leaching agent) is about 50%/50%.
  • contacting the input material 102 with the leaching agent 104 as described herein yields a solid residue 106 and a solution 108.
  • the solid residue 106 may include silica.
  • the solution 108 may include the one or more metal compounds. Separating the solid residue from the solution may be accomplished by any method known to those of ordinary Attorney Docket No.: 440773-000402 skill in the art, such as filtration including vacuum filtration, filter press, centrifuge, and the like.
  • the composition of the solution 108 is related to the composition of the input material 102.
  • the solution will similarly contain calcium- containing compounds.
  • the input material includes calcium, aluminum, iron, or magnesium compounds, or combinations thereof
  • the solution will similarly include calcium, aluminum, iron, or magnesium compounds, or combinations thereof, without wishing to be bound by theory.
  • the one or more separations include adjusting the pH of the solution, heating the solution, or combinations thereof.
  • the one or more separations include adjusting the pH of the solution to between about 4.0 and about 13.5 to isolate the one or more metal compounds, such as adjusting the pH of the solution to about 4.0, about 4.1, about 4.2, about 4.3, about 4.4, about 4.5, about 4.6, about 4.7, about 4.8, about 4.9, about 5.0, about 5.1, about 5.2, about 5.3, about 5.4, about 5.5, about 5.6, about 5.7, about 5.8, about 5.9, about 6.0, about 6.1, about 6.2, about 6.3, about 6.4, about 6.5, about 6.6, about 6.7, about 6.8, about 6.9, about 7.0, about 7.1, about 7.2, about 7.3, about 7.4, about 7.5, about 7.6, about 7.7, about 7.8, about 7.9, about 8.0, about 8.1, about 8.2, about 8.3, about 8.4, about 8.5, about 8.6, about 8.7, about 8.8, about 8.9, about 9.0, about 9.1, about 9.2, about 9.3, about 9.4, about 8.5, about 8.
  • the one or more separations include adjusting the pH of the solution to between about 4.0 and about 5.5. In some embodiments, the one or more separations include adjusting the pH of the solution to between about 5.0 and about 7.5. In some embodiments, the one or more separations include adjusting the pH of the solution to between about 8.0 and about 10.5. In some embodiments, the one or more separations include adjusting the pH of the solution to between about 12.0 and about 13.5.
  • the one or more separations include heating the solution to about 100 °C to about 200 °C to isolate the one or more metal compounds, such as heating the solution to about 100 °C, about 105 °C, about 115 °C, about 125 °C, about 135 °C, about 145 °C, about 150 °C, about 155 °C, about 165 °C, about 175 °C, about 185 °C, about 195 °C, about 200 °C, or any range or value contained therein.
  • the one or more separations include heating the solution to about 100 °C to about 150 °C to isolate the one or more metal compounds. In some embodiments, the one or more separations include heating the solution to about 150 °C to about 200 °C to isolate the one or more metal compounds. [0070] In some embodiments, the one or more separations include a first separation to isolate a first metal compound. In some embodiments, the one or more separations include a first separation to isolate a first metal compound and a second separation to isolate a second metal compound. In some embodiments, the one or more separations include a first separation to isolate a first metal compound, a second separation to isolate a second metal compound, and a third separation to isolate a third metal compound.
  • the method further includes a final separation to isolate a calcium species.
  • the method includes performing a first separation 110 on the solution 108 to isolate a first metal compound 120.
  • the first separation 110 may include adjusting the pH of the solution, heating the solution, or combinations thereof.
  • performing the first separation results in the first metal compound precipitating from the solution.
  • the first metal compound may be removed from the solution by any method, including but not limited to filtration.
  • the method includes only the first separation, and does not include a second separation.
  • the method includes only the first separation and a second separation and does not include a third separation.
  • Adjusting the pH may allow multiple metal compounds to be isolated from the solution 108 one by one, such that a first metal compound may be isolated, then a second metal compound, then a third metal compound, and so forth.
  • the pH may be adjusted by any method familiar to those of ordinary skill in the art.
  • the ammonia gas that is produced from heating the input material and the leaching agent may be used to adjust the pH.
  • Attorney Docket No.: 440773-000402 [0073]
  • a first alkali solution is used to adjust the pH to isolate the first metal compound 120 from the solution 108.
  • the concentration of the first alkali solution used to adjust pH is at least about 0.1 M, at least about 1 M, at least about 5 M, at least about 10 M, or any range or value contained therein.
  • the method further includes recovery of the first alkali.
  • Recovery of the first alkali may include evaporation, that is, evaporation of the first alkali solution to recover the first alkali.
  • 100% of the first alkali is recovered.
  • less than 100% of the first alkali is recovered, such as about 95%, 90%, 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, or any range or value contained therein.
  • the method further includes performing a second separation 112 on the solution 108 to isolate a second metal compound 122.
  • the second separation may be performed after the first separation and after removal of the first metal compound from the solution.
  • the second separation may include adjusting the pH of the solution, heating the solution, or combinations thereof.
  • performing the second separation results in the second metal compound precipitating from the solution.
  • the second metal may be removed from the solution by any method, including but not limited to filtration.
  • a second alkali solution is used to adjust the pH to isolate the second metal compound 122 from the solution 108.
  • the concentration of the second alkali solution used to adjust pH is at least about 0.1 M, at least about 1 M, at least about 5 M, at least about 10 M, or any range or value contained therein.
  • the method further includes recovery of the second alkali.
  • the recovery of the second alkali is performed via electrolysis.
  • about 90% of the second alkali is recovered.
  • less than about 90% of the second alkali is recovered, such as 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, or any range or value contained therein.
  • the method includes performing a third separation 114 on the solution 108 to isolate a third metal compound 124.
  • the third separation may be performed Attorney Docket No.: 440773-000402 after the first separation and the second separation, and after removal of the first metal compound and the second metal compound from the solution.
  • the third separation may include adjusting the pH of the solution, heating the solution, or combinations thereof.
  • performing the third separation results in the third metal compound precipitating from the solution.
  • the third metal compound may be removed from the solution by any method, including but not limited to filtration.
  • the ammonia gas that is produced while heating the input material and the leaching agent is used in the one or more separations, such as any of the first separation 110, second separation 112, third separation 114, or combinations thereof.
  • the ammonia gas may be dissolved in water to form an ammonia solution which may be used to adjust the pH.
  • the concentration of the ammonia solution is at least about 0.1 M. In some embodiments, the concentration of the ammonia solution is at least about 0.5 M. In some embodiments, the concentration of the ammonia solution is at least about 1 M. In some embodiments, the concentration of the ammonia solution is at least about 5 M.
  • the concentration of the ammonia solution is at least about 10 M.
  • the method further includes utilizing the one or more metal compounds, such as the first metal compound 120, the second metal compound 122, and the third metal compound 124 in the production of ordinary Portland cement (OPC).
  • OPC may contain iron, magnesium, aluminum, or combinations thereof, and thus such materials (which may be isolated from the input material as described herein) may be useful in OPC production.
  • one or more of the first metal compound, the second metal compound, and the third metal compound can be used to capture CO2, for example from point sources or direct air capture.
  • one or more of the first metal compound, the second metal compound, and the third metal compound can be used to capture CO2 from OPC production, which decreases the CO 2 emission of OPC production, without wishing to be bound by theory.
  • one or more of the first metal compound, the second metal compound, and the third metal compound can be used in the production of a cementitious material.
  • the one or more metal compound includes magnesium.
  • the magnesium may, in some embodiments, be combined with magnesium-bearing materials including but not limited to basalt, brucite, forsterite, sellaite, gabbro, olivine, wagnerite, Attorney Docket No.: 440773-000402 lizardite, caminite, talc, spinel, skarns, electric arc furnace slag (EAF), reducing steel slag, oxidizing steel slag, converter steel slag, basic oxygen furnace slag, ladle slag, slow or fast cooled steel slag, blast furnace slag, granulated blast furnace slag, ground granulated blast furnace slag (GGBFS), air-cooled slag, slag, fly ash, bottom ash, or combinations thereof to produce a cementitious material.
  • EAF electric arc furnace slag
  • GGBFS ground granulated blast furnace slag
  • the FIGURE shows (via dashed lines) the various way that one or more of the first metal compound, the second metal compound, and the third metal compound may be used.
  • the one or more metal compounds such as the first metal compound, the second metal compound, and the third metal compound can be used in other industries in any manner familiar to those skilled in the art.
  • the one or more metal compounds contained within the input material 102 may include magnesium.
  • isolating magnesium by the methods described herein may provide magnesium in the form of Mg(OH) 2 , which can capture CO 2 from any source, without wishing to be bound by theory.
  • the thermal CO2 produced from OPC production can be sequestered with Mg(OH)2 to reduce thermal CO2 emissions.
  • the method includes recovering the leaching agent 104 from the solution 108.
  • recovering the leaching agent from the solution includes applying an electric current to the solution, adjusting the temperature of the solution, contacting the solution with CO2, contacting the solution with ammonia, or combinations thereof. Recovering the leaching agent may occur at any point in the method after contacting the input material with the leaching agent.
  • the leaching agent includes HCl
  • the leaching agent may be recovered by adjusting the temperature of the solution which may include performing a heat treatment on the solution (from which the one or more metal compounds have been removed as described herein).
  • the solution contains ammonium chloride.
  • performing a heat treatment on the solution which contains ammonium chloride may result in the formation of aqueous HCl and ammonia.
  • recovering the leaching agent 104 includes contacting the solution 108 with an ammonia solution, which may, in some embodiments, be produced during previous steps of the method.
  • the gaseous ammonia that may be produced in previous steps of the method may be dissolved in water and used as described Attorney Docket No.: 440773-000402 herein to recover the leaching agent.
  • recovering the leaching agent includes contacting the leaching agent with the ammonia solution and CO2, thereby capturing CO2 and producing calcium carbonate and ammonium chloride, without wishing to be bound by theory.
  • the calcium carbonate may be further used as described herein and the ammonium chloride may be collected for use as a leaching agent.
  • recovering the leaching agent 104 from the solution 108 includes applying an electric current to the solution, that is, electrolysis.
  • applying the electric current includes the use of renewable energy sources, which may offset the energy cost of the electrolysis.
  • Cl 2 and H 2 gases produced from the electrolysis are combined to recover the leaching agent.
  • the H 2 gas produced from the electrolysis is used to compensate the energy consumption of the electrolysis process, and Cl2 gas is heated with water under UV light to recover the leaching agent.
  • electrolysis is not utilized.
  • recovering the leaching agent from the solution includes contacting the solution with CO2 and ammonia to produce the leaching agent and calcium carbonate. In some embodiments, recovering the leaching agent does not require heat, electricity, or a combination thereof.
  • about 100% of the leaching agent 104 is recovered. In some embodiments, less than about 100% of the leaching agent is recovered, and additional leaching agent may be added to repeat the method as disclosed herein.
  • the input material 102 includes calcium.
  • the input material includes calcium and one or more of iron, magnesium, and aluminum.
  • the input material includes calcium and does not include one or more of iron, magnesium, and aluminum.
  • the solution may include calcium.
  • isolating and removing one or more of the first metal compound, the second metal compound, and the third metal compound from the solution provides a calcium-containing solution.
  • the method further includes performing a final separation 116 on the solution 108 to isolate a calcium species 126, wherein the calcium species may include calcium chloride, calcium carbonate, calcium bicarbonate, calcium hydroxide, calcium oxide, or combinations thereof.
  • the calcium species may be used for CO 2 capture, in some embodiments.
  • the final separation 116 includes isolating the calcium species 126.
  • the final separation 116 may include adjusting the pH of the solution 108.
  • at least about 20% of the calcium species 126 is recovered, relative to the total amount of calcium contained within the input material. For example, about 20%, about 25%, about 30%, about 35%, about 40%, about 45%, about 50%, about 55%, about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 100%, or any range or value contained therein, of the calcium species may be recovered.
  • the method further includes utilizing the calcium species 126 in Portland cement production.
  • the method further includes utilizing the calcium species in carbon dioxide capture. In some embodiments, the method further includes combining the calcium species with the solid residue to produce a cementitious material. In some embodiments, the method further includes combining the calcium species with one or more alkali activators to produce a cementitious material. In some embodiments, the method includes combining the calcium species with one or more alkali activators and the solid residue to produce a cementitious material. [0095] In some embodiments, the calcium species 126 is recovered in the form of calcium carbonate (CaCO3), which can be used in the production of OPC.
  • CaCO3 calcium carbonate
  • the chemical CO2 which is produced during OPC production can be captured as described herein, which, without wishing to be bound by theory, may make the OPC production process CO2 neutral.
  • the total CO2 emission from OPC production can be low CO2, CO2 neutral, or CO2 negative, depending on the magnesium content of the input material.
  • OPC production may result in the chemical and thermal formation of CO2, as would be familiar to those skilled in the art.
  • the chemical CO2 Attorney Docket No.: 440773-000402 may be captured with the calcium species and the thermal CO2 may be captured with a magnesium species, as described herein.
  • the method may include utilizing the calcium species 126 for CO2 capture, which may result in the formation of calcium carbonate (CaCO3).
  • the calcium carbonate formed from CO2 capture may be combined (mixed and/or milled) with the solid residue, which in some embodiments includes silica, and alkali activators to produce a CO 2 sequestered cementitious material.
  • the one or more alkali activators can include one or more of alkali hydroxides, alkali earth hydroxides, alkali carbonate, alkali metal oxides, alkali earth metal oxides, alkali bicarbonates such as one or more of sodium carbonate, sodium bicarbonate, sodium hydroxide, sodium oxide, sodium silicates, sodium sulfate, sodium phosphate, sodium nitrate, potassium carbonate, potassium bicarbonate, potassium hydroxide, potassium oxide, potassium silicates, potassium sulfate, potassium phosphate, potassium nitrate, calcium hydroxide, calcium oxide, calcium sulfate, calcium nitrate, calcium silicates, calcium aluminum silicates, calcium silicate hydrates, calcium aluminum silicate, ordinary Portland cement (OPC), recycled high alkalinity concrete, or combinations thereof.
  • alkali hydroxides alkali earth hydroxides, alkali carbonate, alkali metal oxides, alkali earth metal oxides, alkali bicarbonates
  • sodium carbonate
  • the calcium species 126 may be recovered as calcium hydroxide.
  • the calcium hydroxide is directly used in OPC production which can, without wishing to be bound by theory, eliminate the chemical CO2 produced from the calcination of limestone in traditional OPC production. This may make the OPC production process chemically CO2 neutral.
  • the one or more metal compounds isolated from the solution may contain Mg(OH)2, which can capture CO2.
  • the thermal CO 2 produced from the OPC production during the heating in the kiln can be sequestered with Mg(OH) 2 , which will reduce CO 2 from the thermal process of OPC production.
  • the calcium species 126 is used to produce a cementitious material. When mixed with water, the cementitious material hardens. [0100] In some embodiments, the calcium species 126 is combined (mixed and/or milled) with the solid residue to produce a cementitious material. When mixed with water, this cementitious material hardens. Any of the calcium species produced by the present method and disclosed herein may be used in such an embodiment. Attorney Docket No.: 440773-000402 [0101] In some embodiments, the calcium species 126 is combined (mixed and/or milled) with the solid residue to produce a CO2 sequestered cementitious material.
  • the one or more metal compounds includes calcium carbonate, and the method further includes using the calcium carbonate to produce ordinary Portland cement. In some embodiments, the method further includes producing CO 2 and using the CO 2 to recover the leaching agent, produce ordinary Portland cement, or a combination thereof.
  • the calcium species 126 can be used as a carbon negative filler such as sand and gravel.
  • the solid residue 106 contains silica, aluminosilicate gel, or combinations thereof, and can be used as a supplementary cementitious material.
  • the solid residue contains silica and other metal compounds, and can be used as a supplementary cementitious material if the metal content is within the threshold of OPC metal compound requirements, as would be familiar to one of ordinary skill in the art.
  • the solid residue can be used in carbon dioxide capture, such as to sequester the CO 2 produced from OPC production.
  • the solid residue 106 is used to produce a cementitious material. When mixed with water, the cementitious material hardens.
  • the solid residue 106 is combined with one or more alkali activators to produce a cementitious material.
  • Alkali activators can include one or more of alkali hydroxides, alkali earth hydroxides, alkali carbonate, alkali metal oxides, alkali earth metal oxides, alkali bicarbonates such as one or more of sodium carbonate, sodium bicarbonate, sodium hydroxide, sodium oxide, sodium silicates, sodium sulfate, sodium phosphate, sodium nitrate, potassium carbonate, potassium bicarbonate, potassium hydroxide, potassium oxide, potassium silicates, potassium sulfate, potassium phosphate, potassium nitrate, calcium hydroxide, calcium oxide, calcium sulfate, calcium nitrate, calcium silicates, calcium aluminum silicates, calcium silicate hydrates, calcium aluminum silicate, ordinary Portland cement (OPC), recycled high alkalinity concrete, or combinations thereof.
  • OPC ordinary Portland cement
  • the input material may include iron, aluminum, magnesium, and calcium.
  • a first separation including adjusting the pH of the solution may be used to separate the aluminum compound, followed by a second separation including adjusting the pH of the solution to separate the iron compound, followed by a third separation including adjusting the pH of the solution to separate magnesium compound, thus leaving behind a solution which contains calcium.
  • Such a representative example may further include treating the solution that contains calcium with ammonia (such as the ammonia gas which is produced by the method of the present disclosure) and further isolating the calcium from the solution by, for example, utilizing the solution that contains calcium for CO 2 capture and thus producing calcium carbonate and ammonium chloride, which is in some embodiments used as the leaching agent.
  • ammonia such as the ammonia gas which is produced by the method of the present disclosure
  • Such a representative example may further include treating the solution that contains calcium with ammonia (such as the ammonia gas which is produced by the method of the present disclosure) and further isolating the calcium from the solution by, for example, utilizing the solution that contains calcium for CO 2 capture and thus producing calcium carbonate and ammonium chloride, which is in some embodiments used as the leaching agent.
  • the term “comprising” means “including, but not limited to.”
  • the term “about” means plus or minus 10% of the numerical value of the number with which it is being used. For example, “about 50%” means in the range of 45- 55%.
  • the numerical values used in this disclosure are to be construed as being characterized by the above described “about”, are also intended to include the exact numerical values disclosed herein. The ranges disclosed here includes the upper and lower limits.
  • compositions, methods, and devices are described in terms of “comprising” various components or steps (interpreted as meaning “including, but not limited to”), the compositions, methods, and devices can also “consist essentially of” or “consist of” the various components and steps, and such terminology should be interpreted as defining essentially closed-member groups. It will be further understood by those within the art that if a specific number of an introduced claim recitation is intended, such an intent will be explicitly recited in the claim, and in the absence of such recitation no such intent is present. [0114] For example, as an aid to understanding, the following appended claims may contain usage of the introductory phrases "at least one" and "one or more” to introduce claim recitations.

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Abstract

La présente invention concerne un procédé de séparation de matériaux qui consiste à fournir un matériau d'entrée comprenant un ou plusieurs composés métalliques, mettre en contact le matériau d'entrée avec un agent de lixiviation pour produire un résidu solide et une solution, et réaliser une ou plusieurs séparations sur la solution pour isoler le ou les composés métalliques. Les composants séparés obtenus peuvent être utilisés pour la capture de dioxyde de carbone, en tant que précurseurs pour des matériaux cimentaires ou du ciment Portland ordinaire, ou pour des combinaisons de ceux-ci.
PCT/US2024/034134 2023-06-16 2024-06-14 Procédés d'isolement de précurseurs cimentaires Ceased WO2024259327A2 (fr)

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