AU2012204028B2 - Processes for extracting aluminum and iron from aluminous ores - Google Patents
Processes for extracting aluminum and iron from aluminous ores Download PDFInfo
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- AU2012204028B2 AU2012204028B2 AU2012204028A AU2012204028A AU2012204028B2 AU 2012204028 B2 AU2012204028 B2 AU 2012204028B2 AU 2012204028 A AU2012204028 A AU 2012204028A AU 2012204028 A AU2012204028 A AU 2012204028A AU 2012204028 B2 AU2012204028 B2 AU 2012204028B2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 114
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 77
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- -1 aluminum ions Chemical class 0.000 claims abstract description 148
- 239000000203 mixture Substances 0.000 claims abstract description 95
- 239000007787 solid Substances 0.000 claims abstract description 35
- 150000002500 ions Chemical class 0.000 claims abstract description 33
- 238000002386 leaching Methods 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000000622 liquid--liquid extraction Methods 0.000 claims abstract description 4
- 238000000638 solvent extraction Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 30
- 230000001376 precipitating effect Effects 0.000 claims description 22
- 239000012528 membrane Substances 0.000 claims description 21
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 20
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 18
- 239000012510 hollow fiber Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000000536 complexating effect Effects 0.000 claims description 3
- 238000009877 rendering Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 15
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 239000002184 metal Substances 0.000 abstract description 11
- 150000002739 metals Chemical class 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 9
- 229910052708 sodium Inorganic materials 0.000 abstract description 7
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 abstract description 6
- 229910052700 potassium Inorganic materials 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 239000012141 concentrate Substances 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 229910052787 antimony Inorganic materials 0.000 abstract description 2
- 229910052785 arsenic Inorganic materials 0.000 abstract description 2
- 229910052788 barium Inorganic materials 0.000 abstract description 2
- 229910052790 beryllium Inorganic materials 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract description 2
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 229910052745 lead Inorganic materials 0.000 abstract description 2
- 229910052748 manganese Inorganic materials 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 238000010979 pH adjustment Methods 0.000 abstract description 2
- 229910052718 tin Inorganic materials 0.000 abstract description 2
- 229910052720 vanadium Inorganic materials 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 238000004821 distillation Methods 0.000 abstract 2
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 abstract 1
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- 239000012074 organic phase Substances 0.000 description 36
- 239000008346 aqueous phase Substances 0.000 description 35
- 239000003960 organic solvent Substances 0.000 description 19
- 239000002585 base Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- 230000002378 acidificating effect Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 239000003637 basic solution Substances 0.000 description 4
- 238000010908 decantation Methods 0.000 description 4
- 125000002524 organometallic group Chemical group 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- ZDFBXXSHBTVQMB-UHFFFAOYSA-N 2-ethylhexoxy(2-ethylhexyl)phosphinic acid Chemical compound CCCCC(CC)COP(O)(=O)CC(CC)CCCC ZDFBXXSHBTVQMB-UHFFFAOYSA-N 0.000 description 1
- 238000004131 Bayer process Methods 0.000 description 1
- XBEDEUGIOGUZSN-UHFFFAOYSA-N CCCCC(CC)COP(O)=O Chemical compound CCCCC(CC)COP(O)=O XBEDEUGIOGUZSN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CCPHAMSKHBDMDS-UHFFFAOYSA-N Chetoseminudin B Natural products C=1NC2=CC=CC=C2C=1CC1(SC)NC(=O)C(CO)(SC)N(C)C1=O CCPHAMSKHBDMDS-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HLQQMPGKASWZPH-UHFFFAOYSA-N diethyl hexyl phosphate Chemical compound CCCCCCOP(=O)(OCC)OCC HLQQMPGKASWZPH-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052664 nepheline Inorganic materials 0.000 description 1
- 239000010434 nepheline Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
There are provided processes for extracting aluminum ions from aluminous ores. Such processes can be used with various types of aluminous ores such as aluminous ores comprising various types of metals such as Fe, K, Mg, Na, Ca, Mn, Ba, Zn, Li, Sr, V, Ni, Cr, Pb, Cu, Co, Sb, As, B, Sn, Be, Mo, or mixtures thereof. WO 2008/141423 PCT/CA2008/000877 RAW ARGILITE Option I Leaching at room temperature Preparation Crushing ------- + HC1 (12 M) of argilite Roasting ----------------- Hot leaching Enrichment of HCJ recovered with HCl (6 M) gaseous HCI gazeux or UCI (12 M) Partial distillation t p. HCI recovered SeparationAcdeahn seiatin Concentrated leachate Acid leaching + washing water Argilite impoverished Volume reduction with in metals (resin) more than 90 % by distillation Option 3 'V y Precipitation of Fe Refining by liquid-liquid _..-. Iron removal at pH > 10 extraction tOption 2 p Fe3t ion rich Separation - Fe rich solid concentrate Al rich liquid pH adjustment at 3-4 Aluminum recovery Refining by liquid-liquid extraction Formation Al 3 ions rich pure Formation of A12 0 by concentrate of AI(OH)3 roasting Fig, 1
Description
AUSTRALIA Patents Act 1990 SPECIFICATION Name of Applicant: ORBITE ALUMINAE INC. Actual Inventors: BOUDREAULT, Richard BIASOTTO, Fabienne ALEX, Serge Address for Service: Baldwins Intellectual Property 16 Chisholm Street North Ryde Sydney Invention Title: PROCESSES FOR EXTRACTING ALUMINUM AND IRON FROM ALUMINOUS ORES The following statement is a full description of this invention, including the best method of performing it known to us: KAESO9454ALTPR PROCESSES FOR EXTRACTING ALUMINUM FROM ALUMINOUS ORES TECHNICAL FIELD [0001] The present invention relates to improvements in the field of chemistry applied to extraction of aluminum from aluminous ores. For example, such processes are useful for extracting aluminum from aluminous ores comprising various types of metals such as Fe, K, Mg, Na, Ca, Mn, Ba, Zn, Li, Sr, V, Ni, Cr, Pb, Cu, Co, Sb, As, B, Sn, Be, Mo, or mixtures thereof, BACKGROUND OF THE INVENTION [0002] More than 96 % of the alumina which is produced worldwide is obtained from bauxite, which is a mineral that is particularly rich in alumina (40 - 60 %) and whose main suppliers are from Jamaica, Australia, Brazil, Africa and Russia. In certain areas of the world there are large quantities of aluminous ores, which are aluminosilicates (for example argillite, nepheline, etc.) that are relatively rich in alumina (20 - 28 %). However such areas have received little attention up to now because the production costs for extracting aluminum from such ores remained too high. In these aluminous materials, and contrary to bauxite, aluminum oxide is associated with silicated or sulfated phases, Thus, the Bayer process cannot be used, which means that alternative treatments for the production of alumina must be used or developed. Various processes have been proposed so far in order to extract aluminum from such aluminous ores comprising aluminosilicates but there is still room for improvement or for alternative routes. It is an object of the present invention to provide a process for preparing alumina and/or a process for extracting aluminum ions from an aluminosilicate ore and/or a process for extracting aluminum ions from an ore and/or a process from producing alumina and/or a process for producing aluminum. It is an alternative object of the invention to least provide the public with a useful choice. 1 SUMMARY OF THE INVENTION (0003] According to one aspect, there is provided a process for extracting aluminum ions from a mixture comprising iron ions and the aluminum ions, The process comprises recovering the aluminum ions from a composition comprising the aluminum ions, the iron ions, an organic solvent and an extracting agent adapted to form an organometallic complex substantially 1A WO 2008/141423 PCT/CA2008/000877 selectively with the iron ions or with the aluminum ions which is soluble in the organic solvent. [0004] According to one embodiment, the composition can comprise an acidic aqueous phase comprising aluminum ions and an organic phase comprising iron ions complexed with the extracting agent and wherein the aluminum ions are recovered by separating the aqueous phase from the organic phase. The aqueous phase can have a pH of about 1 to about 2.5 or of about 2. The extracting agent can be chosen from phosphoric acids and derivatives thereof, and phosphinic acids and derivatives thereof. For example, the extracting agent can be chosen from di-2-ethylhexyl phosphoric acid (HDEHP). bis(2,4,4-trimethylpentyl) phosphinic acid and 2-ethyihexyl phosphonic acid mono-2-ethylhexyl ester. The extracting agent can have a concentration of about 0.5 M to about 1.5 M in the organic phase or of about 1 M in the organic phase. The composition can have a volumic ratio organic phase : aqueous phase of about 1:1. After extraction (passing the composition through the membrane), the aqueous phase can be separated from the organic phase, and the aluminum ions can recovered in the aqueous phase and the aqueous phase can be treated with a base (for example NaOH, KOH, or a mixture thereof). The aqueous phase can be treated with the base so as to obtain a pH of at least about 4. The process can further comprise treating the organic phase with HCI and isolating the iron ions in the form of Fet [0005] According to another embodiment, the composition can comprise an acidic aqueous phase comprising iron ions and an organic phase comprising aluminum ions complexed with the extracting agent, and wherein the aluminum ions are recovered by separating the aqueous phase from the organic phase. The aqueous phase can have a pH of about 2.5 to about 3.5. The extracting agent can be a phosphinic acid or a derivative thereof. For example, the extracting agent can be bis(2,4,4-trimethylpentyl) phosphinic acid. The extracting agent can have a concentration of about 10 % to about 25 % v/v with respect to the organic solvent or of about 20 % v/v with respect to the organic solvent. The composition can have a volumic ratio aqueous phase : organic phase of about 1:1 to about 1:3. During the process, the 2 WO 2008/141423 PCT/CA2008/000877 composition can be at a temperature of about 30 "C to about 50 "C or at a temperature of about 35 "C to about 45 "C. After extraction through the membrane, the aqueous phase can be separated from the organic phase. The complexed aluminum ions can be recovered in the organic phase. The organic phase can then be treated with HCl so as to obtain an aqueous composition comprising the aluminum ions. [0006] For example, the organic solvent can be chosen from hydrocarbons. For example, the organic solvent can be chosen from CS-C, 2 alkanes and mixtures thereof. The organic solvent can also be hexane or heptane. The organic phase and the aqueous phase can be separated by means of a filtration membrane, for example a hollow fiber membrane. Such membrane can comprise polypropylene, polyvinylidene difluoride, or a mixture thereof. The aqueous phase can be treated with the base so as to obtain a pH of at least about 4. The process can also further comprise a separation by filtration so as to obtain AI(OH) 3 . The process can also comprise washing the
AI(OH)
3 . The process can also comprise converting AI(OH)3 into A1 2 0 3 , Conversion of AI(OH)a into A1 2 0 3 can be carried out at a temperature of about 800 "C to about 1200 "C. [0001 According to another aspect there is provided a composition comprising aluminum ions, iron ions, an organic solvent and an extracting agent adapted to form an organometallic complex substantially selectively with the iron ions or with the aluminum ions which is soluble in the organic solvent. [0008] According to another aspect, there is provided a composition comprising an acidic aqueous phase comprising aluminum ions and an organic phase comprising iron ions complexed with an extracting agent. [0009] According to another aspect, there is provided a composition comprising an acidic aqueous phase comprising iron ions and an organic phase comprising aluminum ions complexed with an extracting agent. 3 WO 2008/141423 PCT/CA2008/000877 (0010] The various parameters, embodiments and examples previously described concerning the processes can also be applied, when possible, to these compositions, [0011] According to another aspect, there is provided a process for at least partially separating aluminum ions from iron ions comprised in a composition, the process comprising substantially selectively precipitating at least a portion of the iron ions in basic conditions in which the pH is of at least 10. The iron ions can be precipitated from a basic aqueous composition comprising NaOH or KOH. For example, the base can be reacted with the composition so as to obtain a mixture in which the pH is of at least 10, and then, the at least portion of precipitated iron ions can be separated from the rest of the mixture. For example, the precipitated iron ions can be separated from the rest of the mixture by carrying out a filtration, a decantation, a centrifugation, or combinations thereof. The process can further comprise rinsing the obtained precipitated iron ions with a basic solution. The basic solution can have a concentration of about 0.01 M to about 0.02 M. The pH can be at least 11, at least 12, about 10.8 to about 11.2, or about 11.5 to about 12.5. The process can further comprise purifying the precipitated iron ions by means of a hollow fiber membrane. [0012] According to another aspect, there is provided a process for extracting aluminum from an aluminum ore, the process comprising: - leaching the aluminum ore with an acid so as to obtain a leachate and a solid residue; - removing at least a portion of iron ions contained in the leachate by: (i) substantially selectively precipitating the at least portion of the iron ions in basic conditions in which the pH is of at least 10, so as to obtain an aluminum enriched composition; or 4 WO 2008/141423 LPCT/CA2008/000877 (ii) substantially selectively completing the at least portion of the iron ions with an extracting agent adapted to form an organometallic complex substantially selectively with the iron ions so as to obtain an aluminum enriched composition. [0013] For example, the acid can be HCI. The aluminum ore can leached with HCI at a temperature of at least 80 "C, at least 90 *C, or about 100 "C to about 110 *C. HCI can have a concentration of about 6 M. The alunimum ore I acid ratio can be about 1110 in weight by volume. [0014] For example, the removal of the at least portion of iron ions can be carried out by precipitating the iron ions from a basic aqueous composition. The composition can comprise comprising NaOH or KOH. [0015] For example, the removal of the at least portion of iron ions can be carried out by reacting the leachate with a base in order to obtain a pH of at least 10 and precipitating the iron ions. [0016) For example, the precipitated iron ions can be separated from the rest of the leachate by carrying out a filtration, a decantation, a centrifugation, or mixtures thereof. [0017] The process can further comprise rinsing the obtained precipitated iron ions with a basic solution. The basic solution can have a concentration of about 0.01 M to about 0.02 M. The pH can be at least 11, at least 12, about 10.8 to about 11.2, or about 11.5 to about 12.5. The process can further comprise purifying the precipitated iron ions by means of a hollow fiber membrane. [0018] The removal of the at least portion of iron ions can be carried out by reacting the leachate, under acidic conditions, with the extracting agent and an organic solvent in order to obtain a composition comprising an acidic aqueous phase comprising aluminum ions and an organic phase comprising iron ions complexed with the extracting agent. The aluminum enriched composition can be obtained by separating the aqueous phase from the 5 WO 2008/141423 PCT/CA200S/600877 organic phase. The aqueous phase can have a pH of about 1 to about 2.5, or about 2. The extracting agent can be chosen from di-2-ethylhexyl phosphoric acid (HIDEHP), bis(2,4,4-trimethylpentyl) phosphinic acid and 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester). The extracting agent can have a concentration of about 0.5 M to about 1.5 M in the organic phase or about 1 M in the organic phase. [0019] For example, the organic solvent can be chosen from Cr5-C12 alkanes and mixtures thereof. The organic solvent can be heptane. The composition can have a volumic ratio organic phase: aqueous phase of about 1:1. The organic phase and the aqueous phase can be separated by means of a filtration membrane. The membrane can be a hollow fiber membrane. The membrane can comprise polypropylene, polyvinylidene difluoride, or a mixture thereof. [0020] After passing the composition through the membrane, the aqueous phase can separated from the organic phase. The aluminum ions can be recovered in the aqueous phase and the aqueous phase is treated with a base (such as NaOH or KOH), The aqueous phase can be treated with the base so as to obtain a pH of at least about 4. The process can further comprise a separation by filtration to obtain AI(OH) 3 , which can be eventually washed. [0021] For example, the aluminum ore can be crushed and roasted before being leached. (0022 For example, before removal of the iron ions, the leachate is treated with a base. [0023] For example, before removal of the iron ions, the leachate can be distilled so as to reduce its volume. [0024] For example, the process can further comprise at least partially recovering the aluminum ions present in the aluminum enriched composition. 6 [0025] For example, the aluminum enriched composition can be treated with an extracting agent adapted to form an organometallic complex substantially selectively with the aluminum ions in the presence of an organic solvent and an acid solution in order to form a composition comprising an acidic aqueous phase comprising impurities and an organic phase comprising aluminum ions complexed with the extracting agent. The aluminum ions can be recovered by separating the aqueous phase from the organic phase. For example, the aqueous phase can have a pH of about 2,5 to about 3.5. The extracting agent can be a phosphinic acid or a derivative thereof. The extracting agent can be bis(2,4,4-trimethylpentyl) phosphinic acid, The extracting agent can have a concentration of about 10 % to about 25 % v/v or about 20 % v/v with respect to the organic solvent. The organic solvent can be chosen from Cr 1 C alkanes and mixtures thereof. The organic solvent can be heptane. The composition can have a volumic ratio aqueous phase : organic phase of about 1:1 to about 1:3. The organic phase and the aqueous phase can be separated by means of a membrane (for example a hollow fiber membrane) The membrane can comprise polypropylene, polyvinylidene difluoride, or a mixture thereof. The composition can be at a temperature of about 30 'C to about 50 '*C, or about 35 *C to about 45 0 C. After passing the composition through the membrane, the aqueous phase can be separated from the organic phase. The complexed aluminum ions can be recovered in the organic phase, The organic phase can then be treated with HCI so as to obtain an aqueous composition comprising the aluminum ions. The aluminum ions can be converted into AI(OH)3 by contacting it with a base. AI(OH) 3 can then be converted into A1 2 0 3 . Such a conversion of AI(OH)a into A1 2 0 3 can be carried out at a temperature of about 800 *C to about 1200 "C. [0025A] According to another aspect, there is provided a process for preparing alumina comprising: leaching an aluminosilicate ore with an acid to obtain a leachate and a solid residue, and separating said leachate from said solid residue; 7 removing at least a portion of iron ions contained in said leachate by reacting said leachate with a base to obtain a pH of at least 10 and selectively precipitating said at least a portion of iron ions, and separating said precipitated at least a portion of iron ions from said leachate to obtain an Akrich composition; purifying said Al-rich composition; and converting said purified Al-rich composition into alumina. [0025B] According to another aspect, there is provided a process for preparing alumina comprising : leaching an aluminosilicate ore with an acid to obtain a leachate and a solid residue, and separating said leachate from said solid residue; at least partially removing iron ions from said leachate by substantially selectively precipitating said iron ions at a pH greater than 10 by reacting said leachate with a base and at least partially removing said precipitated iron ions from said leachate, thereby obtaining an Al-rich composition comprising Al 3 " ions; purifying said A ions; and converting said A13 ions into alumina. [0025C] According to another aspect, there is provided a process for extracting aluminum ions from an aluminosilicate ore, said process comprising: leaching said aluminosilicate ore with an acid to obtain a composition comprising aluminum ions and iron ions; 7A 0 4TS S at least partially removing said iron ions from said composition by substantially selectively precipitating said iron ions at a pH of at least 10 by reacting said composition with a base and at least partially removing said precipitated iron ions, thereby obtaining an Al-rich composition comprising Al^' ions; and purifying said Al ions. [0025D] According to another aspect, there is provided a process for extracting aluminum ions from an aluminosilicate ore, said process comprising: leaching said aluminosilicate ore with HCI to obtain a composition comprising a leachate and a solid residue; separating said leachate and said solid residue from one another; at least partially removing iron from said leachate by substantially selectively precipitating iron ions by reacting said leachate with a base and removing a so-formed precipitate, to obtain an Al-rich composition comprising Al 3 ions; and purifying said Al 3 , ions. [0025E] According to another aspect, there is provided a process preparing alumina, said process comprising : leaching argillite with HCI to obtain a composition comprising a leachate and a solid residue; separating said leachate and said solid residue from one another; 7B 0 94A A UP at least partially removing iron from said leachate by substantially selectively precipitating iron ions by reacting said leachate with a base and removing a so-formed precipitate, to obtain an Al-rich composition comprising
AI
3 ' ions; purifying said A1 3 + ion; and converting said Al 3 tions into alumina. [0025F] According to another aspect, there is provided a process for extracting aluminum ions from an aluminosilicate ore, said process comprising: leaching said aluminosilicate ore with HCI so as to obtain a composition comprising a leachate and a solid residue, wherein said leachate comprises aluminum ions and iron ions; separating said leachate and said solid residue from one another; rendering insoluble at least a portion of said iron ions or said aluminum ions into said leachate so as to at least partially separate said iron ions from said aluminum ions; and purifying said iron ions and/or said aluminum ions. [0025G] According to another aspect, there is provided a process for extracting aluminum ions from an ore, said process comprising : leaching said ore with HCI and obtaining a composition comprising said aluminum ions and iron ions; '7 C at least partially removing said iron ions from said composition by substantially selectively precipitating said iron ions and at least partially removing said precipitated iron ions or by substantially complexing said iron ions with an extracting agent and at least partially removing said complexed iron ions, thereby obtaining an Alrich composition; and, thereby obtaining an Al-rich composition; and optionally purifying A1 3 * ions from said Al-rich composition, [0025H] According to another aspect, there is provided a process for producing alumina comprising obtaining aluminum ions by means of a process as defined above; and converting said aluminum ions into alumina. [00251] According to another aspect, there is provided a process for producing aluminum comprising obtaining alumina by means of a process as defined above; and converting said alumina into aluminum. BRIEF DESCRIPTION OF DRAWINGS [0026] In the following drawings, which represent by way of example only, various embodiments of the invention: [0027] Fig. 1 shows a bloc diagram of a process according to one embodiment of a process for extracting aluminum from an aluminous or '7D WO 2008/141423 PCT/CA2008/000877 DETAILED DESCRIPTION OF VARIOUS EMBODIMENTS (0028] Further features and advantages will become more readily apparent from the following description of various embodiments as illustrated by way of examples only in the appended drawings wherein: [0029] As it can be seen from Fig. 1, such a process can comprise various steps, and each of these steps can eventually be individually considered has being a process Preparation of argillite sample [0030] Argillite can be finely crushed in order to help along during the following steps. For example, micronization can shorten the reaction time by few hours (about 2 to 3 hours). In order to remove most of the iron, a leaching step at room temperature is optionally carried out between the crushing step and the roasting step (see option 1). This operation is, for example, carried out with hydrochloric acid HCI (12 M) and an argillite I acid ratio (weight / volume) of 1:5 is used. Depending on experimental conditions (sizes of the particles, time of treatment, agitation system), about 65 % to about 93 % of the iron can then be removed. However, this leaching step can also bring in a certain percentage of the aluminum (0 - 5 %). The last step of the preparation of argillite comprises roasting the pretreated argillite. This can be accomplished at a temperature greater than 550 *C for a period of about I to 2 hours. For example, a heat treatment makes it possible to increase the quantity of extracted aluminum by about 30 % to about 40 % for the same period of time. In others words, the quantity of extracted aluminum is doubled. When leaching at room temperature is carried out, a phase separation before roasting can be made in order to recover the acid and reduce heating costs. Acid leaching 10031] Acid leaching comprises reacting the crushed and roasted argillite with a hydrochloric acid solution at elevated temperature during a given period of time. For example, the argillite / acid ratio can be of about of
B
WO 20081141423 PCT/CA2008/000877 1:10 (weight I volume), the HCI concentration can be of about 6 M, the temperature can be of about 100 C to about 110 "C, and the reaction lime can be of about 5 to about 7 hours. Under such conditions, more than about 90 % of the aluminum and about 100 % of the iron can be extracted in addition to impurities. [00321 During the second half of such a treatment (for example the last 2 or 3 hours), a portion of the acid can be recovered by condensation. Once the extraction is terminated, the solid (argillite impoverished in metals) can be separated from the liquid by decantation or by filtration, after which it is washed. The residual leachate and the washing water may be completely evaporated. The corresponding residue can thereafter be washed many times with water so as to decrease acidity and to lower the quantities of sodium hydroxide (NaOH) that are required to adjust the pH during iron removal. Final volume accounts for 10 % to 20 % of initial volume. The acid recovered will can be re-utilized after having adjusted its titer either by adding gaseous HCI, or by adding concentrated HCI (12 M). After the reaction, the titer of the acid can vary from about 4 M to about 6 M depending on experimental conditions. With respect to the solid, it represents about 65 % to about 75 % of the initial mass of argillite, it can be valorized and be used again either as an ion exchange resin, or as an adsorbent. Removal of iron [0033] Removal of iron can be carried out by precipitation of the latter in basic medium for example at a pH of at least 10 or at a pH of about 11.5 to about 12.5. Such a step can be made by adding NaOH, for example at a concentration of 10 M. Other bases such as KOH can also be used. Then, all that is required is to separate the solid portion from the liquid portion by filtration, decantation or centrifugation and to rinse the solid by means of a diluted base, such as a solution of NaOH (for example NaOH at a concentration of 0.01 M to 0.02 M). Then, the solid is washed with distilled water. The liquid portion comprises aluminum and alkaline-earths A substantially complete removal of the iron and of nearly all the impurities 9 WO 2008/141423 PCT/CA2008/000877 (other metals) can thus be achieved. Optionally, it is possible to recover iron by using a refining step by liquid-liquid extraction through a hollow fiber membrane (see option 2). [0034] Alternatively (see option 3), removal of iron can be carried out by using an extracting agent and a hollow fiber membrane. Various extracting agents that could substantially selectively complex iron ions over aluminum ions (or aluminum ions over iron ions) could be used in such a step depending an Al / Fe ratio. For example, extraction can be carried out by using HDEHP (diethylhexylphosphoric acid) as an extracting agent adapted to complex iron ions. A concentration of about 1 M of HDEHP can be used in an organic solvent, such as heptane or any hydrocarbon solvent. Such an extraction can require relatively short contact times (few minutes). For example, the pH of the order of 2 can be used and aqueous phase / organic phase ratio can be of about 1:1. It was observed that is possible to extract from 86 % to 98 % iron under such conditions. It will be understood that in the present case, iron is trapped in the organic phase. To recover iron in an aqueous phase, a reverse extraction with hydrochloric acid (2 M or 6 M) and organic phase / acidic phase ratio of about 1:0.5 can then be carried out. In such a case, the resulting aqueous phase is rich in Fe" ions. Aluminum recovery [0035] The solution obtained from the previous step using either the precipitation or the extraction technique is relatively clean and mainly contains aluminum for example about 90 % to 95 % (without the alkaline-earths in the case of precipitation). Recovery of the latter can be carried out by liquid-liquid extraction for example by using a same hollow fiber membrane and an extracting agent that is adapted to complex at least substantially selectively aluminum over other metals or residues. For example, bis(2,4,4 trimethylpentyl) phosphinic acid (such as the one sold under the name Cyanex T M 272) can be used as an extracting agent specific to aluminum. For example, this extracting agent can be used at a concentration of about 20 % vlv in an organic solvent such as heptane. The ratios between the aqueous 10 WO 2008/141423 PCT/CA2OOS/000877 phase and the organic phase can be of about 1:1 to about 1:3. For example, the extraction temperatures can be of about 40 "C and the pH can be maintained at about 2.5 to about 3.5. It was observed that such a technique makes it possible to extract more than 70 - 90 % of the aluminum. After the aluminum has been trapped in the organic phase, it can berecovered in the form of a concentrate of Al ions by using a back extraction. For example, the reverse extraction can be carried out at a temperature of about 40 *C with hydrochloric acid (for example at a concentration of 6 M). Under this condition, more than 90 % of aluminum can be recovered. Then, Al 3 " can be converted into aluminum hydroxide AI(OH) 3 by addition of NaOH. Finally,
AI(OH)
3 can be converted into alumina (alumina A1 2 0 3 ) by roasting AI(OH) 3 for example at a temperature of about 800 "C tol 200 *C, [0036] The following non-limiting examples further illustrate the invention. Examples Example I Preparation of argillite sample [0037] Crushing of mudstone : The resulting micronization average employed for the tests ranges between 10 and 50 microns. [0035] Roasting : Crushed mudstone was roasted at least during 1 hour at a temperature of 600 *C. Its average composition was: A1 2 0 3 21,0 % Fe 2 0 3 8,0 %
K
2 0 1,5 % Na 2 O 0,9 % TiO 2 0,9 % CaO 0,08 % ZnO 0,06 % SiO 2 51,0 % 11 WO 2008/141423 PCT/CA2008/000877 Acid leaching [0039] 500 g of argillite crushed and roasted were added to S liters of hydrochloric acid 6 M. The mixture was then heated at 100 "C - 110 *C during 7 hours. [0040] After reaction, the liquid part was separated from the solid part by filtration. The solid was washed with distilled water which was added to the liquid portion. This washing makes it possible to recover part of the aluminum trapped in the solid. This solid had a dry mass of 345 ±- 5 g, which corresponds to a loss of about 30 % - 32 %. [0041] The remaining liquid part, containing aluminum, iron and a great part of the impurities initially present in mudstone, was reduced by evaporation at a temperature of 100 *C to 90 % of its initial volume. Residual volume was then 50 mL. The liquid compositions before and after evaporation were: Leaching solution Evaporated leaching solution Composition (%) Composition (%) [concentration (mg/L)] [concentration (mgL)] 47.63 47.86 Aluminum [9 2501 [59 500] 31.54 31.07 Iron [6 125] [38 625] Alkaline-earths 19.30 19.53 (Na, Mg, K, Ca) [3 749] [24 2771 1.53 1.54 Other metals [297.3] [1 920] All the ions species seem to remain soluble. 12 WO 2008/141423 PCT/CA2008/000877 Removal of iron [0042] The residual volume was slightly diluted (+ 25 %) and concentrated hydroxide sodium (10 M) was added until a pH higher than 11.5 was reached. The formed precipitate was separated from the solution by standard filtration and was washed several times with NaOH dilued and hot ultra-pure water. The precipitate contained all the iron and the majority of the metal impurities. The filtrate contained in addition to ions Al" mainly alkaline-earths and some following impurities: Major filtrate impurities (%) Iron 0.14 Sodium 94.13 Alkaline-earths 5.71 (Mg, K, Ca) Other metals 0,02 Na+ came from soda and was also the AI(OH) 4 - counter-ion, Aluminum recovery [0043] The filtrate is adjusted at a pH of 2.5 to 3.5 by addition of HCI 6 M. The resulting solution is extracted by means of the complexing agent, Cyanex 272, at a concentration of 20 % volume / volume in an organic solvent with a volumetric ratio of 1:1. The extraction is carried out at a temperature of 40 "C in a membrane contactor with hollow fibers. In less than about 30 to 60 min, more than 85 % of aluminum is extracted. The pH adjustment is performed by a regulation loop controling the NaOH (10 M) addition. Complexed AI* in Cyanex are then recovered by carrying out a back extraction with HCI (6 M) at 40 "C and an organic phase / acid phase volumetric ratio of 1:0.5. After the back extraction, the composition of the recovered acid phase is: 13 Composition (%) Aluminum 92.81 Iron 0 Alkaline-earths 7.14 (Na, Mg, K, Ca) Other metals 0,05 [0044] To increase the percentage of purity, the Al * ions are precipitated in the form of A(OH)t hydroxide, then washed several times with ultra-pure water. The composition of the hydroxide becomes: Composition (%) Aluminum 99.09 Iron 0 Alkaline-earthsI 0,88 (Na, Mg, K, Ca) Other metals 0,03 [0045] Further purification can be performed by recrystallization [0046] While a description was made with particular reference to the specific embodiments, it will be understood that numerous modifications thereto will appear to those skilled in the art. Accordingly, the above description and accompanying drawings should be taken as specific examples and not in a limiting sense. [0047] Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like, are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense, that is to say, in the sense of "including, but not limited to". [0048] The reference to any prior art in the specification is not, and should not be taken as, an acknowledgement or any form of suggestion that the prior art forms part of the common general knowledge in Australia. 14
Claims (20)
1. A process for preparing alumina comprising: leaching an aluminosilicate ore with an acid to obtain a leachate and a solid residue, and separating said leachate from said solid residue; removing at least a portion of iron ions contained in said leachate by reacting said leachate with a base to obtain a pH of at least 10 and selectively precipitating said at least a portion of iron ions, and separating said precipitated at least a portion of iron ions from said leachate to obtain an Al-rich composition; purifying said Al-rich composition; and converting said purified Al-rich composition into alumina.
2. The process of claim 1, wherein said acid is HC.
3. The process of claim 2, wherein said aluminosilicate ore is leached with HCI at a temperature of at least 100 *C
4, The process of claim 3, wherein aluminum ions in the form of AI(OH) 3 are converted into alumina.
5 The process of claim 1, wherein said pH is at least 11.
6. A process for preparing alumina comprising : leaching an aluminosilicate ore with an acid to obtain a leachate and a solid residue, and separating said leachate from said solid residue; at least partially removing iron ions from said leachate by substantially selectively precipitating said iron ions at a pH greater than 10 by reacting said leachate with a base and at least partially removing said precipitated iron ions from said leachate, thereby obtaining an Al-rich composition comprising Al 3 ions; 15 purifying said A3 ions; and converting said A3 ions into alumina.
7. The process of claim 6, wherein purifying said A1* ions is carried out by selectively precipitating said At* ions.
8. A process for extracting aluminum ions from an aluminosilicate ore, said process comprising : leaching said aluminosilicate ore with an acid to obtain a composition comprising aluminum ions and iron ions; at least partially removing said iron ions from said composition by substantially selectively precipitating said iron ions at a pH of at least 10 by reacting said composition with a base and at least partially removing said precipitated iron ions, thereby obtaining an A-rich composition comprising A3 ions: and purifying said A1* ions.
9. A process for extracting aluminum ions from an aluminosilicate ore, said process comprising : leaching said aluminosilicate ore with HCI to obtain a composition comprising a leachate and a solid residue; separating said leachate and said solid residue from one another; at least partially removing iron from said leachate by substantially selectively precipitating iron ions by reacting said leachate with a base and removing a so-formed precipitate, to obtain an Al-rich composition comprising A1* ions; and purifying said AP* ions.
10. A process preparing alumina, said process comprising: 1 g3 leaching argillite with HCl to obtain a composition comprising a leachate and a solid residue; separating said leachate and said solid residue from one another; at least partially removing iron from said leachate by substantially selectively precipitating iron ions by reacting said leachate with a base and removing a so-formed precipitate, to obtain an Al-rich composition comprising Al 3 ions; purifying said Al 3 ion; and converting said All+ ions into alumina.
11. The process of claim 10, wherein said Al 3 + ions are purified by substantially selectively precipitating them.
12. A process for extracting aluminum ions from an aluminosilicate ore, said process comprising leaching said aluminosilicate ore with HCI so as to obtain a composition comprising a leachate and a solid residue, wherein said leachate comprises aluminum ions and iron ions; separating said leachate and said solid residue from one another; rendering insoluble at least a portion of said iron ions or said aluminum ions into said leachate so as to at least partially separate said iron ions from said aluminum ions; and purifying said iron ions and/or said aluminum ions.
13. A process for extracting aluminum ions from an ore, said process comprising : leaching said ore with HCI and obtaining a composition comprising said aluminum ions and iron ions; at least partially removing said iron ions from said composition by substantially selectively precipitating said iron ions and at least partially removing said precipitated iron ions or by substantially complexing said iron ions with an extracting agent and at least partially removing said complexed iron ions, thereby obtaining an Al-rich composition; and, thereby obtaining an Al-rich composition; and optionally purifying Al ions from said Al-rich composition.
14. The process of claim 13, wherein said process comprises: leaching said ore with HCI so as to obtain a leachate comprising said aluminum ions and said iron ions, and a solid residue; separating said leachate from said solid residue; at least partially removing said iron ions from said leachate by substantially selectively precipitating said iron ions by reacting said base with said leachate and removing a so-formed precipitate, so as to obtain said Al-rich aqueous composition; and purifying said Al-rich aqueous composition by substantially selectively precipitating said Al 34 ions and recovering said precipitated aluminum ions.
15. The process of claim 13, wherein said process comprises: leaching said ore with HCI so as to obtain a leachate comprising said aluminum ions and said iron ions, and a solid residue; separating said leachate from said solid residue; at least partially removing said iron ions from said leachate by substantially selectively precipitating said iron ions by reacting said base with said leachate and removing a so-formed precipitate, so as to obtain said Al-rich aqueous composition; and i-s purifying said Al-rich aqueous composition by means of a hollow fiber membrane, or by a liquid-liquid extraction.
16 The process of claims 13 or 15, wherein said Akrich aqueous composition is purified by complexing said A13 ions with an extracting agent so as to obtain a complex, separating said complex form said composition and precipitating said aluminum ions.
17. A process for producing alumina comprising obtaining aluminum ions by means of a process as defined in any one of claims 8 to 9 and 12 to 16; and converting said aluminum ions into alumina.
18. A process for producing aluminum comprising obtaining alumina by means of a process as defined in any one of claims to 7, 10, 11 and 17; and converting said alumina into aluminum.
19. Alumina or Aluminum prepared by the process of any one of claims 1, 6,8, 9, 10, 12, 13, 17 or 18,
20. A process as claimed in any one of claims 1, 6, 8, 9, 10, 12, 13, 17 or 18 substantially as hereinbefore described with particular reference to any of or the Examples and/or Figures, 19
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| US5868935A (en) * | 1995-03-15 | 1999-02-09 | New Jersey Institute Of Technology | Method and apparatus for extraction and recovery of ions from solutions |
| US6468483B2 (en) * | 2000-02-04 | 2002-10-22 | Goldendale Aluminum Company | Process for treating alumina-bearing ores to recover metal values therefrom |
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| US5868935A (en) * | 1995-03-15 | 1999-02-09 | New Jersey Institute Of Technology | Method and apparatus for extraction and recovery of ions from solutions |
| US6468483B2 (en) * | 2000-02-04 | 2002-10-22 | Goldendale Aluminum Company | Process for treating alumina-bearing ores to recover metal values therefrom |
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