WO2024065007A1 - Procédé de production d'un matériau alumineux - Google Patents

Procédé de production d'un matériau alumineux Download PDF

Info

Publication number
WO2024065007A1
WO2024065007A1 PCT/AU2023/050939 AU2023050939W WO2024065007A1 WO 2024065007 A1 WO2024065007 A1 WO 2024065007A1 AU 2023050939 W AU2023050939 W AU 2023050939W WO 2024065007 A1 WO2024065007 A1 WO 2024065007A1
Authority
WO
WIPO (PCT)
Prior art keywords
aluminium
containing feedstock
hydrochloric acid
chloride hexahydrate
pregnant liquor
Prior art date
Application number
PCT/AU2023/050939
Other languages
English (en)
Inventor
Cameron Johnston
Rachel Pepper
Wayde Martens
Sara Couperthwaite
Original Assignee
Lava Blue Ltd
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
Priority claimed from AU2022902817A external-priority patent/AU2022902817A0/en
Application filed by Lava Blue Ltd filed Critical Lava Blue Ltd
Publication of WO2024065007A1 publication Critical patent/WO2024065007A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/48—Halides, with or without other cations besides aluminium
    • C01F7/56—Chlorides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
    • C01F7/0693—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process from waste-like raw materials, e.g. fly ash or Bayer calcination dust
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C01F7/306—Thermal decomposition of hydrated chlorides, e.g. of aluminium trichloride hexahydrate
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium 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
    • C22B21/00—Obtaining aluminium
    • 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
    • C22B21/00—Obtaining aluminium
    • C22B21/0015—Obtaining aluminium by wet processes
    • C22B21/0023—Obtaining aluminium by wet processes from waste materials
    • 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
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • 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
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates to a method for producing an aluminous material from an aluminium-containing material.
  • the present invention relates to a method for producing an aluminous material from a solid waste obtained from the combustion of coal.
  • Aluminium is a useful material which can be used to provide strong and lightweight metal alloys which are resistant to rusting. Aluminium is traditionally extracted from aluminium- containing ores such as bauxite, or recovered from the recycling of aluminium scrap metal. However, industrial waste materials and solid waste residue from the combustion of coal (such as fly ash, boiler ash, red mud, dross, production line scrap, coal bottom ash, boiler slag, municipal incinerator bottom ash, or the like) may also contain commercially viable levels of aluminium.
  • coal such as fly ash, boiler ash, red mud, dross, production line scrap, coal bottom ash, boiler slag, municipal incinerator bottom ash, or the like
  • Fly ash or flue ash is a waste material generated during the combustion of organic materials, such as coal, and refers to the fine particulate material captured from flue gases.
  • Fly ash typically comprises minerals such as silicon dioxides, aluminium oxides, calcium oxides and iron oxides and may also contain trace amounts of other elements including rare earth elements.
  • Fly ash typically comprises around 5-35% aluminium content, depending on the origin of the material being combusted as well as the power plant mode of operation. However, liberation of aluminium from fly ash is often difficult due to the nature of the aluminium oxides.
  • Embodiments of the present invention provide a method for producing an aluminous material, which may at least partially address one or more of the problems or deficiencies mentioned above or which may provide the public with a useful or commercial choice.
  • alkali fusion is intended to refer to a method of heating an ore or other source of minerals with an alkali or alkaline earth reagent at an elevated temperature to render the mineral amenable to further treatment
  • the present invention in one form, resides broadly in a method for producing an aluminous material including: providing an aluminium-containing feedstock; subjecting the aluminium-containing feedstock to an alkali fusion process to generate an activated aluminium-containing feedstock; contacting the activated aluminium-containing feedstock with a hydrochloric acid to obtain a leachate; separating the leachate to generate a pregnant liquor; subjecting the pregnant liquor to a sodium reduction process, the sodium reduction process including: adjusting a pH of the pregnant liquor to precipitate an aluminium hydroxide; separating the precipitated aluminium hydroxide from a spent liquor; and contacting the precipitated aluminium hydroxide with hydrochloric acid to provide a reduced-sodium pregnant liquor, subjecting the reduced-sodium pregnant liquor to a crystallisation process to form an aluminium chloride hexahydrate crystals slurry, and separating the aluminium chloride hexahydrate crystals slurry to obtain aluminium chloride
  • the method of the present invention enables the production of relatively high purity aluminium chloride hexahydrate from an aluminium-containing waste material comprising high sodium content.
  • relatively high purity aluminium chloride hexahydrate it is envisaged that the aluminium chloride hexahydrate may contain less than 10% w/w of impurities. More preferably, the aluminium chloride hexahydrate may contain less than 5% w/w of impurities. More preferably, the aluminium chloride hexahydrate may contain less than 2.5% w/w impurities. More preferably, the aluminium chloride hexahydrate may contain less than 1% w/w impurities.
  • the aluminium chloride hexahydrate may contain less than 0.1 % w/w impurities.
  • the method of the present invention proceeds at a lower caustic fusion temperature compared to other alkali or alkali metal reagents.
  • the method of the present invention has improved cost efficiencies and reduced complexity compared to traditional aluminium extraction processes as it does not require ion exchange, solvent extraction or magnetic separation unit operations/
  • an aluminium-containing feedstock may be provided.
  • Any suitable type of aluminium-containing feedstock may be used.
  • the aluminium-containing feedstock may be a solid material. Any suitable solid material may be used, such as a waste residue from combustion of coal or other organic material, or an incinerator waste.
  • the aluminium-containing feedstock may be fly ash, boiler ash, boiler slag, bottom ash, or the like.
  • the aluminium-containing feedstock comprises or consists of fly ash.
  • the aluminium-containing feedstock may be an aluminosilicate.
  • the aluminium-containing feedstock may be kaolin, zeolite, feldspar, or the like.
  • the aluminium-containing feedstock may be of any suitable form.
  • the aluminium-containing feedstock may be provided in the form of a solid material.
  • the aluminium-containing feedstock may be provided in granulated or particulate form.
  • the aluminium-containing feedstock may undergo one or more preparation steps prior to subjecting the aluminium-containing feedstock to an alkali fusion process. Any suitable preparation steps may be used. For instance, the aluminium- containing feedstock may undergo a size reduction step. Similarly, the aluminium- containing feedstock may undergo a separation step (such as separation on the basis of
  • the aluminium- containing feedstock may undergo a sieving step to obtain a desired particle size distribution.
  • the aluminium-containing feedstock may be subjected to an alkali fusion process to provide an activated aluminium-containing feedstock.
  • any suitable alkali fusion process may be used.
  • the alkali fusion process may cause the activation of the aluminium-containing feedstock and/or improve aluminium recovery during subsequent process steps (such as, but not limited to, leaching).
  • alkali fusion may cause non-reactive insoluble materials (such as mullite) found in solid waste residue from the combustion of coal or other organic materials to undergo a phase change into a more reactive soluble sodium aluminosilicate.
  • the alkali fusion process comprises contacting the aluminium- containing feedstock with an alkali or alkaline earth reagent at elevated temperatures.
  • any suitable alkali or alkaline earth reagent may be used.
  • the alkali or alkaline earth reagent may comprise sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, calcium oxide, calcium carbonate, sodium carbonate, or the like, or any suitable combination thereof.
  • the alkali or alkaline earth reagent may be sodium hydroxide.
  • the alkali or alkaline earth reagent may be of any suitable form.
  • the alkali or alkaline earth reagent may be provided in solid form (such as in the form of a powder, granules, flakes, pearls, pellets or the like).
  • an alkali or alkaline earth reagent solution may be provided.
  • the alkali or alkaline earth reagent may be in the form of pellets.
  • the alkali or alkaline earth reagent may be applied at any suitable application rate to the aluminium-containing feedstock.
  • the application rate may vary depending on the form and/or concentration of the alkali or alkaline earth reagent and the type of aluminium- containing feedstock.
  • the mass ratio of alkali or alkaline earth reagent to aluminium-containing feedstock may be about 10% w/w. about 20% w/w, about 30% w/w, about 40% w/w, about 50% w/w, about 60% w/w, about 70% w/w, about 80% w/w, about 90%
  • SUBSTITUTE SHEET (RULE 26) ⁇ N/ ⁇ N, about 100% w/w, or about 125% w/w.
  • the mass ratio of alkali or alkaline earth reagent to aluminium- containing feedstock may be about 50% w/w to about 100% w/w.
  • about 50% w/w sodium hydroxide pearls may be applied to fly ash.
  • about 100% w/w sodium hydroxide pearls may be applied to fly ash.
  • the aluminium-containing feedstock may be contacted with an alkali or alkaline earth reagent in any suitable manner. It is envisaged, however, that the method of contacting the aluminium-containing feedstock with the alkali or alkaline earth reagent may be configured to maximise contact between the alkali or alkaline earth reagent and the surface of the aluminium-containing feedstock.
  • the aluminium-containing feedstock may be dispersed within a solution of the alkali or alkaline earth reagent.
  • a solution of the alkali or alkaline earth reagent may be applied to the aluminium-containing feedstock (for instance, by spraying, coating or the like).
  • the aluminium-containing feedstock and alkaline earth reagent may be mixed together to form a mixture.
  • the aluminium-containing feedstock and the alkali or alkaline earth reagent may be mixed together to form a substantially homogenous mixture.
  • the aluminium-containing feedstock may be contacted with an alkali or alkaline earth reagent at any suitable temperature.
  • the alkali fusion process may be conducted at a temperature of between about 400 °C and about 700 °C, between about 425 °C and about 675 °C, between about 450 °C and about 650 °C, between about 500 °C and about 600 °C, between about 525 °C and about 575 °C.
  • the aluminium-containing feedstock may be contacted with an alkali or alkaline earth reagent at a temperature of about 550 °C to provide an activated aluminium- containing feedstock.
  • the alkali fusion process may be carried out using any suitable equipment.
  • the alkali fusion process may be performed in a rotary kiln, fluidised bed, calciner, or the like.
  • the activated aluminium-containing feedstock may undergo a comminution process (or similar size reduction process) before being contacted with hydrochloric acid to obtain a leachate.
  • SUBSTITUTE SHEET (RULE 26)
  • Any suitable size reduction or comminution process may be used, such as crushing, grinding, cutting, vibrating or the like.
  • the process may be configured to reduce the particle size of the activated aluminium-containing feedstock and increase the surface area to be exposed to hydrochloric acid during leaching.
  • the activated aluminium-containing feedstock may be contacted with hydrochloric acid to obtain a leachate.
  • the activated aluminium-containing feedstock may be contacted with the hydrochloric acid in any suitable manner.
  • the method of contacting the activated aluminium-containing feedstock with the hydrochloric acid may be configured to effectively leach aluminium (and, in particular, a relatively high proportion of aluminium) from the activated aluminium-containing feed.
  • the activated aluminium-containing feedstock and the hydrochloric acid may be mixed together to form a slurry.
  • any suitable concentration of hydrochloric acid may be used. Generally, the concentration of hydrochloric acid may be sufficient to solubilise aluminium into solution.
  • a hydrochloric acid solution may be used.
  • the hydrochloric acid solution may have a concentration of between about 5 % and about 35 % hydrochloric acid, between about 10 % and about 30 % hydrochloric acid, between about 15 % and about 25 % hydrochloric acid.
  • the hydrochloric acid solution may have a concentration of about 20 % hydrochloric acid. It will be understood that the volume of hydrochloric acid (or hydrochloric acid solution) required may vary depending on a number of factors, including the particle size and composition of the activated aluminium-containing feedstock and the level of impurities.
  • the addition of the hydrochloric acid to the activated aluminium-containing feedstock may form a mixture of any suitable pulp density.
  • the mixture may be between about 10% m/v and about 25% m/v pulp density.
  • the activated aluminium-containing feedstock-hydrochloric acid mixture may be about 20% m/v pulp density.
  • the activated aluminium-containing feedstock-hydrochloric acid mixture may be held at any suitable temperature. However, it will be understood that the temperature may be elevated in order for the leaching process to be effective. The temperature may vary depending on a number of factors, such as whether the leaching is conducted under
  • SUBSTITUTE SHEET (RULE 26) pressure, the leaching time and concentration of the hydrochloric acid as well as the composition and particle size of the activated aluminium-containing feedstock.
  • the activated aluminium-containing feedstock-hydrochloric acid mixture may be held at a leaching temperature of between about 40 °C and about 110 °C. More preferably, the activated aluminium-containing feedstock-hydrochloric acid mixture may be held at a leaching temperature of between about 70 °C and about 90 °C. In some embodiments, the activated aluminium-containing feedstock-hydrochloric acid mixture may be held at a leaching temperature of about 80 °C.
  • the activated aluminium-containing feedstock-hydrochloric acid mixture may be held at a leaching temperature for any suitable period of time.
  • the leaching time may vary depending on a number of factors such as whether the leaching is conducted under pressure, the leaching temperature and concentration of the hydrochloric acid as well as the composition and particle size of the activated aluminium- containing feedstock.
  • the activated aluminium-containing feedstock may be contacted with a 20 % solution of hydrochloric acid at a temperature of about 80 °C to obtain a leachate.
  • the leachate may be separated to provide a pregnant liquor.
  • the leachate may be separated using any suitable technique.
  • the separation technique may be configured to separate the leachate into a pregnant liquor and a residue (in particular a solid residue).
  • the separation technique may include gravity settling clarifiers, sedimentation, decanting, centrifugation, filtration, or the like.
  • the pregnant liquor may be polished.
  • the pregnant liquor may be polished or clarified using any suitable technique.
  • the polishing step may be configured to remove or reduce suspended solids such as fine precipitate, insoluble material, or the like.
  • the pregnant liquor may be polished or clarified using a filtration process and/or through the addition of one or more flocculants.
  • the pregnant liquor may be subjected to a sodium reduction process.
  • SUBSTITUTE SHEET (RULE 26) pregnant liquor may undergo a sodium reduction process prior to the step of subjecting the pregnant liquor to a crystallisation process.
  • the sodium reduction process may result in the selective precipitation of aluminium hydroxide.
  • the sodium reduction process may include adjusting a pH of the pregnant liquor to precipitate an aluminium hydroxide.
  • the sodium reduction process may further include the step of separating the precipitated aluminium hydroxide from a spent liquor.
  • the sodium reduction process may further include the step of contacting the precipitated aluminium hydroxide with hydrochloric acid to provide a reduced-sodium pregnant liquor.
  • the pH of the pregnant liquor may be adjusted to any suitable value.
  • the pH of the pregnant liquor may be adjusted to provide favourable conditions for the selective precipitation of aluminium hydroxide.
  • the pH of the pregnant liquor may be adjusted to an acidic pH. It is envisaged that, while the pH of the pregnant liquor may be an acidic pH, the pH may be adjusted by increasing the pH of the pregnant liquor.
  • the pH of the pregnant liquor may be adjusted to a pH of between about 6 and about 7.
  • the pH of the pregnant liquor may be adjusted to a pH of about 6.5.
  • the pH of the pregnant liquor may be adjusted using a basic substance, such as, but not limited to, ammonia.
  • concentration of ammonia may be used.
  • concentration of ammonia may be selected so as to adjust the pH of the pregnant liquor to the desired value while minimising the volume of ammonia added.
  • the ammonia may have a concentration of between about 3 M and about 9 M, between about 4 M and about 8 M, or between about 5 M and about 7M. It will be understood that the volume of ammonia may vary depending on a number of factors, including the pH of the pregnant liquor and the composition of the leachate.
  • the pH adjustment step may be conducted at any suitable temperature and pressure.
  • the pH adjustment step may be conducted at ambient temperature.
  • ambient temperature may include any temperature within the range of about 18 °C and about 25 °C.
  • the pH adjustment step may be conducted at atmospheric pressure.
  • the precipitated aluminium hydroxide may be separated from the spent liquor using any suitable technique.
  • the separation technique may be configured to remove the spent liquor (including dissolved sodium) from the precipitated aluminium hydroxide.
  • the separation technique may include gravity settling clarifiers, sedimentation, decanting, centrifugation, filtration, or the like, or any suitable combination thereof.
  • the precipitated aluminium hydroxide may be washed after being separated from the spent liquor.
  • the precipitated aluminium hydroxide may be contacted with hydrochloric acid to generate a reduced-sodium pregnant liquor.
  • hydrochloric acid may be contacted with hydrochloric acid to generate a reduced-sodium pregnant liquor.
  • aluminium hydroxide reacts with the hydrochloric acid to produce aluminium chloride.
  • any suitable concentration of hydrochloric acid may be used.
  • the concentration of hydrochloric acid may be configured to solubilise aluminium into solution as aluminium chloride.
  • the hydrochloric acid may be provided in the form of a hydrochloric acid solution (such as an aqueous solution).
  • the hydrochloric acid solution may have a concentration of between about 20 % and about 40 % hydrochloric acid. More preferably, the hydrochloric acid solution may have a concentration of between about 25 % and about 35 % hydrochloric acid. Most preferably, the hydrochloric acid solution may have a concentration of about 32 % hydrochloric acid. It will be understood that the volume of hydrochloric acid solution used may vary depending on a number of factors, including the particle size and composition of the precipitated aluminium hydroxide and the level of impurities.
  • the addition of the hydrochloric acid (or hydrochloric acid solution) to the precipitated aluminium hydroxide may form a mixture of any suitable pulp density.
  • the mixture may be no more than about 25% m/v pulp density. More preferably, the mixture may be of no more than about 20% m/v pulp density. More preferably, the mixture may be of no more than about 15% m/v pulp density. Most preferably, the mixture may be of no more than about 10% m/v pulp density.
  • the aluminium hydroxide-hydrochloric acid mixture may be about 10% m/v pulp density.
  • aluminium hydroxide-hydrochloric acid mixture may be held at any suitable temperature
  • the aluminium hydroxide-hydrochloric acid mixture may be held at an ambient temperature during leaching.
  • ambient temperature may include any temperature within the range of between about 18 °C and about 25 °C.
  • the leaching process using the aluminium hydroxide-hydrochloric acid mixture may be conducted at substantially atmospheric pressure.
  • the precipitated aluminium hydroxide may be dewatered prior to contacting with the hydrochloric acid.
  • the precipitated aluminium hydroxide may be dewatered using any suitable technique.
  • the precipitated aluminium hydroxide may be dewatered using centrifugal separation, a screw press, a belt press, gravity settling, sedimentation, decanting, or the like, or any suitable combination thereof.
  • the reduced-sodium pregnant liquor may be subjected to a crystallisation process to form an aluminium chloride hexahydrate crystals slurry.
  • any suitable crystallisation process may be used.
  • the crystallisation process may be configured to precipitate the aluminium chloride hexahydrate crystals from the reduced-sodium pregnant liquor and/or to minimise the precipitation of impurities.
  • the crystallisation process may include sparging the reduced- sodium pregnant liquor (such as with gaseous hydrochloric acid) to produce crystallisation, and to form a slurry of aluminium chloride hexahydrate crystals.
  • the crystallisation process may include evaporative crystallisation.
  • the aluminium chloride hexahydrate crystal slurry may be subjected to one or more recrystallisation processes. It is envisaged that a recrystallisation process may be performed on crystals formed from a crystallisation method in order to reduce or remove impurities in the compound produced from crystallisation.
  • aluminium chloride hexahydrate crystal slurry obtained from the crystallisation of the reduced-sodium pregnant liquor may be subjected to one or more recrystallisation steps before the aluminium chloride hexahydrate crystals are separated from the aluminium chloride hexahydrate crystal slurry.
  • the recrystallisation process may comprise separating and washing the precipitated crystals. Further, the recrystallisation process may comprise dissolving the washed precipitated crystals in a solvent (such as ultra-pure water, demineralised water, or the like) to form a feed liquor.
  • a solvent such as ultra-pure water, demineralised water, or the like
  • the feed liquor may undergo a polishing step to remove insoluble contaminants such as silica.
  • the feed liquor may be sparged (such as with gaseous hydrochloric acid) to precipitate aluminium chloride hexahydrate crystals.
  • the aluminium chloride hexahydrate crystals slurry may undergo a separation process to obtain aluminium chloride hexahydrate crystals.
  • the aluminium chloride hexahydrate crystals slurry may be separated from the spent liquor using any suitable technique.
  • the separation technique may be configured to separate the aluminium chloride hexahydrate crystals from a spent liquor.
  • the separation technique may include the use of gravity settling clarifiers, sedimentation, decanting, centrifugation, filtration, or the like, or any suitable combination thereof.
  • the aluminium chloride hexahydrate crystals may undergo one or more further processing steps.
  • the aluminium chloride hexahydrate crystals may undergo a recrystallisation step to increase the purity of the crystals, may be at least partially dried, may undergo a decomposition step to form an intermediate alumina precursor, or the like, or a combination thereof.
  • the method for producing an aluminous material according to the first aspect of the invention may further include washing the activated aluminium- containing feedstock and separating the washed activated aluminium-containing feedstock from the wash liquid.
  • the activated aluminium-containing feedstock may be washed before the step of contacting the activated aluminium-containing feedstock with hydrochloric acid (or a hydrochloric acid solution) to obtain a leachate.
  • hydrochloric acid or a hydrochloric acid solution
  • washing the activated aluminium-containing feedstock may assist in reducing sodium levels prior to the leaching step.
  • the method for producing an aluminous material comprises two sodium reduction processes.
  • the activated aluminium-containing feedstock may be washed with any suitable
  • wash liquid may be configured to solubilise the residual alkali or alkaline metal reagent from the alkali fusion process without leaching aluminium from the activated aluminium-containing feedstock.
  • the wash liquid may be water, ultra-pure water, demineralised water, or the like.
  • the washed activated aluminium-containing feedstock may be dewatered prior to contacting the activated aluminium-containing feedstock with hydrochloric acid.
  • the dewatering process may assist in removing additional contaminated liquor from the process. Any suitable dewatering process may be used, such as centrifugal separation, a screw press, a belt press, gravity settling, sedimentation, decanting, or the like, or any suitable combination thereof.
  • the method for producing an aluminous material further includes calcining the aluminium chloride hexahydrate crystals to obtain alumina.
  • the aluminium chloride hexahydrate crystals may be calcined (for example, by means of a rotary kiln, fluidised bed, calciner, etc.) at a relatively high temperature in order to obtain alumina.
  • the alumina obtained may comprise substantially alpha alumina.
  • the aluminium chloride hexahydrate crystals may be calcined at any suitable temperature.
  • the calcination temperature may be configured to at least partially convert the aluminium chloride hexahydrate crystals to alpha alumina.
  • the calcination temperature may vary depending on a number of factors, including the residence time in the calciner, equipment capability, and sintering temperature.
  • the aluminium chloride hexahydrate crystals may be heated to a calcination temperature of between about 950 °C and about 1 ,300 °C, and more preferably between about 1 ,100 °C and about 1 ,300 °C.
  • the aluminium chloride hexahydrate crystals may be heated to a calcination temperature of between about 1 ,100 °C and about 1 ,300 °C.
  • the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for any suitable period of time.
  • the aluminium chloride hexahydrate crystals may be heated to a
  • SUBSTITUTE SHEET (RULE 26) calcination temperature for a period of at least about 30 minutes. More preferably, the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for a period of at least 60 minutes. More preferably, the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for a period of at least about 90 minutes. More preferably, the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for a period of at least about 2 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for a period of at least about 3 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a calcination temperature for a period of at least about 4 hours.
  • the aluminium chloride hexahydrate crystals may be subjected to a decomposition step before the step of calcining the aluminium chloride hexahydrate crystals to provide alumina.
  • a preliminary decomposition process may produce transition alumina phases and amorphous alumina which during calcination are subsequently converted to alpha alumina.
  • the aluminium chloride hexahydrate crystals may be decomposed at any suitable temperature and using any suitable technique.
  • the decomposition temperature may be configured to remove remaining chlorides.
  • the decomposition temperature may vary depending on a number of factors, including the decomposition time, the heat transfer rate, the particle size of the aluminium chloride hexahydrate crystals, and whether the vessel is agitated.
  • the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature of between about 600 °C and about 1 ,200 °C, more preferably between about 700 °C and about 1 ,100 °C, and more preferably between about 800 °C and about 1 ,000 °C.
  • the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature of about 800 °C.
  • the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for any suitable period of time.
  • the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 30 minutes. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 60 minutes. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period
  • the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 2 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 3 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 4 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 5 hours. More preferably, the aluminium chloride hexahydrate crystals may be heated to a decomposition temperature for a period of at least about 6 hours.
  • splitting the calcination process into a lower temperature decomposition stage and a higher temperature calcination stage may effectively split the process across two pieces of equipment that can each be designed for a more specific range of operating conditions. This may in turn reduce the stress placed on each piece of equipment, reducing maintenance requirements and the chance of potential equipment failure.
  • the step of decomposing the aluminium chloride hexahydrate crystals may comprise controlling the humidity in the vessel.
  • controlling the humidity of the vessel may assist in promoting chloride removal prior to the calcination step.
  • Figure 1 illustrates a method of producing an aluminous material according to an embodiment of the invention.
  • Figure 2 illustrates a method of producing an aluminous material according to an embodiment of the invention.
  • the aluminous material comprises aluminium chloride hexahydrate.
  • an aluminium-containing feedstock may be provided.
  • Any suitable type of aluminium-containing feedstock may be used.
  • the aluminium-containing feedstock may be fly ash, boiler ash, boiler slag, bottom ash, or the like.
  • the aluminium-containing feedstock may be an aluminosilicate such as kaolin, zeolite, feldspar, or the like.
  • the aluminium-containing feedstock may be fly ash.
  • the aluminium-containing feedstock is subjected to an alkali fusion process to provide an activated aluminium-containing feedstock.
  • the alkali fusion process comprises contacting the aluminium- containing feedstock with an alkali or alkaline earth reagent at elevated temperatures.
  • any suitable alkali or alkaline earth reagent may be used.
  • the alkali or alkaline earth reagent may comprise sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, calcium oxide, calcium carbonate, sodium carbonate, or the like.
  • the alkali or alkaline earth reagent may be sodium hydroxide.
  • the aluminium-containing feedstock may be contacted with an alkali or alkaline earth reagent at a temperature of about 550 °C to provide an activated aluminium- containing feedstock.
  • the activated aluminium-containing feedstock may undergo a size reduction or comminution process before being contacted with hydrochloric acid to obtain a leachate.
  • the activated aluminium-containing feedstock is contacted with a hydrochloric acid to obtain a leachate.
  • the activated aluminium-containing feedstock may be contacted with a 20 % solution of hydrochloric acid at a temperature of about 80 °C to obtain a leachate.
  • the activated aluminium-containing feedstock-hydrochloric acid mixture may be about 20 % m/v pulp density.
  • the leachate is separated to provide a pregnant liquor.
  • the pregnant liquor is subjected to a sodium reduction process (steps 18, 20, and 24).
  • a sodium reduction process enables the production of higher purity aluminium chloride hexahydrate crystals during subsequent crystallisation stages with lower levels of mixed aluminium-sodium chlorides.
  • step 18 the pH of the pregnant liquor is adjusted to precipitate an aluminium hydroxide.
  • the pH of the pregnant liquor may be adjusted to a pH of about 6.5.
  • the pH of the pregnant liquor may be adjusted using ammonia.
  • the precipitated aluminium hydroxide is separated from a spent liquor.
  • the precipitated aluminium hydroxide is contacted with hydrochloric acid to provide a reduced-sodium pregnant liquor.
  • the precipitated aluminium hydroxide may be contacted with a 32 % solution of hydrochloric acid.
  • the aluminium hydroxide-hydrochloric acid mixture may be about 10 % m/v pulp density.
  • the aluminium hydroxide-hydrochloric acid mixture may be held at an
  • SUBSTITUTE SHEET (RULE 26) ambient temperature during leaching, that is, at a temperature of between about 18 °C and about 25 °C.
  • the reduced-sodium pregnant liquor is subjected to a crystallisation process to form an aluminium chloride hexahydrate crystals slurry.
  • step 26 the aluminium chloride hexahydrate crystals slurry is separated to obtain aluminium chloride hexahydrate crystals.
  • the aluminous material comprises aluminium chloride hexahydrate.
  • the method as illustrated in Figure 2 and described in the specification is the same as the method illustrated in Figure 1 and described in the specification with the exception that the activated aluminium-containing feedstock is subjected to additional processing steps 28 and 30.
  • Steps 10, 12, 14, 16, 18, 20, 22, 24, and 26 in the method as illustrated in Figure 2 correspond to steps 10, 12, 14, 16, 18, 20, 22, 24, and 26 in the method as illustrated in Figure 1.
  • the activated aluminium-containing feedstock Prior to contacting the activated aluminium-containing feedstock with hydrochloric acid to obtain a leachate at step 14, the activated aluminium-containing feedstock may be subjected to a subjected to a sodium reduction process (steps 28 and 30).
  • washing the activated aluminium-containing feedstock may assist in reducing sodium levels prior to the leaching step.
  • step 28 the activated aluminium-containing feedstock is washed.
  • the washed activated aluminium-containing feedstock is separated from the wash liquid.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne un procédé de production d'un matériau alumineux à partir d'un matériau contenant de l'aluminium, en particulier un déchet solide obtenu à partir de la combustion de charbon. Le procédé consiste à fournir une charge d'alimentation contenant de l'aluminium et à soumettre la charge d'alimentation à un processus de fusion alcaline pour activer la charge d'alimentation. La charge d'alimentation activée est digérée avec de l'acide chlorhydrique pour obtenir un lixiviat. Le lixiviat est séparé pour produire une liqueur résiduaire qui est soumise à un procédé de réduction du sodium. La liqueur résiduaire de sodium réduite est soumise à un procédé de cristallisation pour former des cristaux d'hexahydrate de chlorure d'aluminium.
PCT/AU2023/050939 2022-09-29 2023-09-28 Procédé de production d'un matériau alumineux WO2024065007A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2022902817 2022-09-29
AU2022902817A AU2022902817A0 (en) 2022-09-29 A method for producing an aluminous material

Publications (1)

Publication Number Publication Date
WO2024065007A1 true WO2024065007A1 (fr) 2024-04-04

Family

ID=90475011

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/AU2023/050939 WO2024065007A1 (fr) 2022-09-29 2023-09-28 Procédé de production d'un matériau alumineux

Country Status (1)

Country Link
WO (1) WO2024065007A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013142957A1 (fr) * 2012-03-29 2013-10-03 Orbite Aluminae Inc. Procédés de traitement de cendres volantes
WO2014075173A1 (fr) * 2012-11-14 2014-05-22 Orbite Aluminae Inc. Procédé de purification d'ions aluminium
US20190153562A1 (en) * 2017-11-20 2019-05-23 Purdue Research Foundation Preparation of rare earth metals and other chemicals from industrial waste coal ash
CN110668452A (zh) * 2019-10-28 2020-01-10 北京科技大学 一种由粉煤灰制备SiO2-Al2O3复合气凝胶材料的方法
AU2019250157A1 (en) * 2018-10-16 2020-05-07 Altech Chemicals Australia Pty Ltd A method for the preparation of alumina

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013142957A1 (fr) * 2012-03-29 2013-10-03 Orbite Aluminae Inc. Procédés de traitement de cendres volantes
WO2014075173A1 (fr) * 2012-11-14 2014-05-22 Orbite Aluminae Inc. Procédé de purification d'ions aluminium
US20190153562A1 (en) * 2017-11-20 2019-05-23 Purdue Research Foundation Preparation of rare earth metals and other chemicals from industrial waste coal ash
AU2019250157A1 (en) * 2018-10-16 2020-05-07 Altech Chemicals Australia Pty Ltd A method for the preparation of alumina
CN110668452A (zh) * 2019-10-28 2020-01-10 北京科技大学 一种由粉煤灰制备SiO2-Al2O3复合气凝胶材料的方法

Similar Documents

Publication Publication Date Title
CA2116468C (fr) Recyclage de revetements de cuves uses
AU764739B2 (en) A method for isolation and production of magnesium metal, magnesium chloride, magnesite and magnesium based products
KR102614181B1 (ko) 리튬 슬래그로부터 가치물을 추출하기 위한 방법
US6248302B1 (en) Process for treating red mud to recover metal values therefrom
AU713938B2 (en) Process for recovery of alumina and silica
EA018749B1 (ru) Способ переработки никель-латеритных руд
US3776717A (en) Method for processing of red mud
GB2083450A (en) Reducing Iron Content of Raw Materials
AU2018359800A1 (en) Method for processing bauxite
WO2024084233A1 (fr) Production de produits chimiques de qualité pour batterie
CN109970102B (zh) 一种铝灰制备聚合氯化铝联产五氧化二钒的方法
WO2024065007A1 (fr) Procédé de production d'un matériau alumineux
WO2002010068A1 (fr) Production d'oxydes metalliques
WO1997029992A1 (fr) Traitement des boues rouges
US11753697B2 (en) Method of processing and treatment of alunite ores
CN112813284A (zh) 一种从含铝矿物中提取铝的方法
NO164665B (no) Fremgangsmaate for gjenvinning av aluminium fra avfallsmateriale.
US6528028B2 (en) Process for treating bauxite in which a desilication product and an insoluble residure are separately precipitated
WO2023235913A1 (fr) Méthode de production d'un matériau alumineux
JP2001192207A (ja) ボーキサイトの処理方法
CN117003269A (zh) 一种含铝硅酸盐矿物及次生含铝硅酸盐混合物的高效综合利用方法
CA3231096A1 (fr) Procede de production d'alumine
AU719126B2 (en) Red mud processing
RU2061068C1 (ru) Способ переработки металлургических шлаков
CN113767067A (zh) 铝土矿物理富集残渣的处理方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 23869338

Country of ref document: EP

Kind code of ref document: A1