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WO2014174527A1 - Procédé de récupération d'alumine à partir de scories d'aluminium - Google Patents

Procédé de récupération d'alumine à partir de scories d'aluminium Download PDF

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Publication number
WO2014174527A1
WO2014174527A1 PCT/IN2014/000197 IN2014000197W WO2014174527A1 WO 2014174527 A1 WO2014174527 A1 WO 2014174527A1 IN 2014000197 W IN2014000197 W IN 2014000197W WO 2014174527 A1 WO2014174527 A1 WO 2014174527A1
Authority
WO
WIPO (PCT)
Prior art keywords
alumina
aluminium
range
liquid phase
dross
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/IN2014/000197
Other languages
English (en)
Inventor
Amlan Datta
Jitendra Kumar KAR
Rajni BARANGULE
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aditya Birla Science and Technology Co Ltd
Original Assignee
Aditya Birla Science and Technology Co 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
Application filed by Aditya Birla Science and Technology Co Ltd filed Critical Aditya Birla Science and Technology Co Ltd
Publication of WO2014174527A1 publication Critical patent/WO2014174527A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • 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
    • 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
    • C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
    • 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
    • C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
    • C01F7/26—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with sulfuric acids or sulfates
    • 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
    • C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
    • C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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 present disclosure provides a method for recovery of a-alumina from aluminium dross. Particularly, a method of recovery of nano alumina from aluminium dross is disclosed.
  • Aluminium dross is residue from primary and secondary aluminium production and is generated during aluminium smelting process. Aluminium dross is classified into white and black dross, according to its metal content. White dross is of higher metal content and it is produced from primary and secondary aluminium smelters. White dross may contain 15% to 70% recoverable metallic aluminium. Black dross has a lower metal content and is generated during aluminium recycling. Black dross contains recoverable aluminium in a range of 2% to 15%. Black dross is mainly mixture of aluminium oxide and other compounds such as A1N, AI4C3, MgF 2 , NaAlCl 4 , KNaCl 4 , Si0 2 , Fe 2 0 3 and MgO etc.
  • aluminium dross is processed in rotary kilns to recover the aluminium and the resultant salt cake is sent to landfills as waste.
  • Such disposal is increasingly facing environmental problems since salts can leach from the aluminium dross and pass into the soil below.
  • aluminium dross comes in contact with water it emits harmful gases such as NH 3 , CH 4 , PH 3 , H 2 , H 2 S, etc.
  • harmful gases such as NH 3 , CH 4 , PH 3 , H 2 , H 2 S, etc.
  • the dross produced by the aluminium industry although a waste, contain significant amount of valuable element such as aluminium oxide, which can be recovered and reused.
  • US7651676 describes a process for preparing aluminium chloride by leaching aluminium dross residues with hydrochloric acid or sulphuric acid to obtain a mixture comprising a solid and a liquid. Further,the liquid obtained is hydrochlorinated to precipitate aluminium chloride. The process further comprises of converting the aluminium chloride into alumina.
  • the method known in the art either use an additional calcining step 3 ⁇ 4 other multiple steps to obtain alumina. There is therefore a need for a simpler and ecdllomical process for recovery of alumina from aluminium dross.
  • a method for recovery of cc-alumina from aluminium dross comprises of grinding aluminium dross to obtain particles having average particle size in the range of 80-100 micron, leaching aluminium dross with an acid to obtain a leach liquor having precipitated silica, separating the silica from the leach liquor to obtain a liquid phase, treating the liquid phase with an aqueous ammonia at acidic pH to facilitate precipitation of iron hydroxide, separating the iron hydroxide from the liquid phase to obtain an iron free liquid phase, treating the iron free liquid phase with aqueous ammonia at alkaline pH to facilitate precipitation of aluminium hydroxide; separating and calcining the aluminium hydroxide to obtain a-alumina having size in the range of 200-700 nm.
  • Figure 1 illustrates scanning electron micrograph of a-alumina obtained in accordance with the disclosed method.
  • Figure 2 illustrates phase analysis using powder X-ray diffraction of a-alumina obtained by the disclosed method.
  • nano alumina as referred to herein means alumina particles having dimensions of nanoscale (1-lOOOnm).
  • the present disclosure provides a method for recovery of a-alumina from aluminium dross. Particularly, a method of recovery of nano alumina from aluminium dross is disclosed.
  • Nano alumina has better properties including reactivity as compared to a-alumina not having dimensions of nanoscale.
  • the method comprises of grinding of aluminium dross to obtain an average particle size in a range of 80-100 micron.
  • the ground aluminium dross is subjected to leaching at high temperature with an acid to obtain leach liquor having aluminium and iron in a dissolved state and a precipitate of silica.
  • the silica thus obtained is separated from the leach liquor.
  • the liquid phase obtained after separation of silica is treated with aqueous ammonia at an acidic pH to facilitate precipitation of iron as iron hydroxide [Fe(OH) 3 ].
  • the iron hydroxide is separated to obtain iron free liquid phase.
  • iron free liquid phase is treated with aqueous ammonia at an alkaline pH to facilitate precipitation of aluminium hydroxide.
  • the method further comprises of separating and calcining the aluminium hydroxide to obtain a- alumina having size in a range of 200 nm to 700 nm.
  • separation of silica from the leach liquor is carried out by filtration.
  • the acidic pH at which the liquid phase is treated with aqueous ammonia is in a range of 4-6.
  • separation of iron hydroxide from the liquid phase is carried out by filtration.
  • the alkaline pH at which the iron free liquid phase is treated with aqueous ammonia is in a range of 7.5-8.5.
  • separation of aluminium hydroxide is carried out by any known methods such as filtration.
  • the separated aluminium hydroxide is subjected to washing and drying.
  • dried aluminium hydroxide is calcined at a temperature in a range of 1 100°C to 1200°C to obtain a-alumina.
  • the aluminium dross may be a black dross comprising A1 2 0 3 , AIN, Si0 2 and Fe 2 0 3 .
  • the black dross comprises of A1 2 0 3 in a range of 60-80%, AIN in a range of 15-30%, Si0 2 in a range of 0-10% and Fe 2 0 3 in a range of 0-5%.
  • the black dross comprises of 70% of A1 2 0 3> 25% of AIN, 3.5% of Si0 2 and 1.5% of Fe 2 0 3 .
  • the grinding of aluminium dross is earned out to obtain particle size in a range of 7-1540 micron, with average particle size of 80-100 micron, preferably 90 micron.
  • acid utilized for leaching of aluminium ? dross is sulphuric acid having concentration in a range of 30%-50% (v/v).
  • leaching of aluminium dross with sulphuric acid is carried out at a high temperature in a range of 170 °C -230 °C for a time period in a range of 10- 15 hours. Leaching of aluminium dross at such a temperature for prolonged duration of time (i.e. 10-15 hrs) facilitates production of highly pure a-alumina with high percentage yield.
  • aqueous ammonia used for precipitation of iron hydroxide and aluminium hydroxide has a concentration in a ratio of 1 : 1.
  • drying of aluminium hydroxide precipitate prior to calcination is carried out at a temperature in a range of 100 °C to 200 °C.
  • calcination of dried aluminium hydroxide precipitate is carried out for a time period in a range of 15 minutes to 1 hour to obtain a- alumina having size in the range of 200 run to 700 nm.
  • percentage yield of -alumina by the method disclosed herein is >90.
  • the a-alumina obtained by the method disclosed herein is highly crystalline single phase a-alumina (as illustrated in Figure 2) having purity of 99.5%.
  • the raw aluminium dross used in this study contained 80% alumina, (quantitative XRD study using Rietveld analysis (70% A1203 and 20% AIN, i.e 10% A1203). 10 gms batch of the aluminium dross was taken and subjected to leaching, precipitation followed by calcination at 1200°C. White powder obtained after calcination was subjected to powder X-ray diffraction which revealed the single phase nature of the material (presence of highly crystalline alumina). The weight of the powder was found to be 5.6 gms indicating 92% alumina extraction efficiency (yield). Whiteness of the powder sample was found to be 92 when measured using reflectance spectrophotometer.
  • EDTA back titration Purity of synthesised alumina was evaluated using EDTA back titration.
  • a method for recovery of a-alumina from aluminium dross comprising grinding aluminium dross to obtain particles having average particle size in the range of 80-100 micron, leaching aluminium dross with an acid to obtain a leach liquor having precipitated silica, separating the silica from the leach liquor to obtain a liquid phase, treating the liquid phase with an aqueous ammonia at acidic pH to facilitate precipitation of iron hydroxide, separating the iron hydroxide from the liquid phase to obtain an iron free liquid phase, treating the iron free liquid phase with aqueous ammonia at alkaline pH to facilitate precipitation of aluminium hydroxide; and
  • Such method(s), wherein the acidic pH at which the liquid phase is treated with aqueous ammonia is in the range of 4-6.
  • Such method(s), wherein the alkaline pH at which the iron free liquid phase is treated with aqueous ammonia is in the range of 7.5 to 8.5.
  • the method for recovery of a-alumina from aluminium dross described above is easy to perform, economical and utilizes a waste generated during aluminium smelting process as a starting material.
  • the a-alumina obtained from the method described above is highly crystalline single phase ⁇ -alumina having percentage purity of 99.5. Further, a- alumina obtained has a size in the range of 200 nm to 700 nm. Nano alumina even if used in small amounts significantly improves properties of a desired product.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Cette invention concerne un procédé de récupération d'alumine à partir de scories d'aluminium. Le procédé selon l'invention comprend le broyage des scories d'aluminium pour obtenir des particules ayant une taille de particule moyenne dans la plage de 80 à 100 microns, la lixiviation des scories d'aluminium avec un acide pour obtenir une liqueur lixiviante contenant une silice précipitée, la séparation de la silice de la liqueur lixiviante pour obtenir une phase liquide, le traitement de la phase liquide avec de l'ammoniac aqueux à un pH acide pour faciliter la précipitation d'hydroxyde de fer, la séparation de l'hydroxyde de fer de la phase liquide pour obtenir une phase liquide sans fer, le traitement de la phase liquide sans fer avec de l'ammoniac aqueux à un pH alcalin pour faciliter la précipitation d'hydroxyde d'aluminium ; la séparation et la calcination de l'hydroxyde d'aluminium pour obtenir une alumine α ayant une taille dans la plage de 200 à 700 microns.
PCT/IN2014/000197 2013-04-22 2014-03-28 Procédé de récupération d'alumine à partir de scories d'aluminium Ceased WO2014174527A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN1469/MUM/2013 2013-04-22
IN1469MU2013 IN2013MU01469A (fr) 2013-04-22 2014-03-28

Publications (1)

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WO2014174527A1 true WO2014174527A1 (fr) 2014-10-30

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IN (1) IN2013MU01469A (fr)
WO (1) WO2014174527A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3825426A1 (fr) 2019-11-22 2021-05-26 Befesa Aluminio, S.L. Procédé de transformation d'oxyde d'aluminium secondaire en une matière première alternative et ses utilisations
WO2024209483A1 (fr) * 2023-04-04 2024-10-10 Runaya Refining Llp Procédé de production d'alumine à partir d'écume d'aluminium
WO2024257067A1 (fr) * 2024-06-18 2024-12-19 Seyed Alikhani Seyedeh Zahra Procédé d'extraction et de production d'alumine pure à partir de l'industrie des crasses d'aluminium nocives

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030185746A1 (en) * 2002-01-16 2003-10-02 Sumitomo Chemical Company, Limited Calcined alumina, its production method and fine alpha-alumina powder obtained by using the calcined alumina

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030185746A1 (en) * 2002-01-16 2003-10-02 Sumitomo Chemical Company, Limited Calcined alumina, its production method and fine alpha-alumina powder obtained by using the calcined alumina

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"Light Metals 2011", 28 February 2011, JOHN WILEY & SONS, INC., Hoboken, NJ, USA, ISBN: 978-1-11-802935-0, article LIU QINGSHENG ET AL: "High Purity Alumina Powders Extracted from Aluminum Dross by the Calcining-Leaching Process", pages: 197 - 200, XP055135313, DOI: 10.1002/9781118061992.ch34 *
DAS ET AL: "Production of eta-alumina from waste aluminium dross", MINERALS ENGINEERING, PERGAMON PRESS , OXFORD, GB, vol. 20, no. 3, 9 February 2007 (2007-02-09), pages 252 - 258, XP005880787, ISSN: 0892-6875, DOI: 10.1016/J.MINENG.2006.09.002 *
DASH B ET AL: "Acid dissolution of alumina from waste aluminium dross", HYDROMETALLURGY, ELSEVIER SCIENTIFIC PUBLISHING CY. AMSTERDAM, NL, vol. 92, no. 1-2, 1 May 2008 (2008-05-01), pages 48 - 53, XP022603241, ISSN: 0304-386X, [retrieved on 20080126], DOI: 10.1016/J.HYDROMET.2008.01.006 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3825426A1 (fr) 2019-11-22 2021-05-26 Befesa Aluminio, S.L. Procédé de transformation d'oxyde d'aluminium secondaire en une matière première alternative et ses utilisations
WO2024209483A1 (fr) * 2023-04-04 2024-10-10 Runaya Refining Llp Procédé de production d'alumine à partir d'écume d'aluminium
WO2024257067A1 (fr) * 2024-06-18 2024-12-19 Seyed Alikhani Seyedeh Zahra Procédé d'extraction et de production d'alumine pure à partir de l'industrie des crasses d'aluminium nocives

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