WO1997022554A1 - Process for recovery of alumina and silica - Google Patents
Process for recovery of alumina and silica Download PDFInfo
- Publication number
- WO1997022554A1 WO1997022554A1 PCT/IL1996/000179 IL9600179W WO9722554A1 WO 1997022554 A1 WO1997022554 A1 WO 1997022554A1 IL 9600179 W IL9600179 W IL 9600179W WO 9722554 A1 WO9722554 A1 WO 9722554A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- solution
- process according
- cacl
- alumina
- silica
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
-
- 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
- C01F7/22—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids
-
- 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
-
- 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
Definitions
- the present invention relates to a process for the recovery of substantially pure alumina and silica from raw materials containing aluminosilicates, and particularly from waste products resulting from coal combustion.
- coal ash which comprises fly ash - the fine particles collected from the combustion-off gas by electrostatic precipitators - and the ash remaining at the bottom of the combustion vessels.
- the volume of coal ash resulting from coal combustion world-wide is constantly on the rise, resulting in an ever increasing problem of disposing the waste without damaging the environment.
- the availability of the waste products at no cost and their being adjacent to sources of power and transport make them attractive as raw material for the extraction of various chemical products.
- coal ash The chemical composition of coal ash varies as a function of the source and type of the coal. However, A1 2 0 3 and Si0 2 are almost always major components of the ash, usually in the form of aluminosilicates and quartz. It would therefore be advantageous to use coal ash as a source for alumina and silica.
- the major source of pure alumina today is bauxite, with the alumina generally being extracted by the Bayer process.
- bauxite is in ample supply and the alumina can be extracted relatively easily and inexpensively, any alternate method for extracting alumina must be economically competi ⁇ tive with the Bayer process.
- the savings in disposal and disposal site maintenance costs should be taken into account, as well as environmental considerations.
- Direct acid leaching (either single-stage or multi-stage) with HCl, HN0 3 , or H 2 S0 4 usually results in quite low recovery rates of Al (under 50%).
- Lime and lime/soda sinter processes involve sintering coal wastes at 1200-1300°C with powdered limestone (CaC0 3 ) or limestone and soda ash (Na 2 C0 3 ) to form calcium or sodium aluminates. The aluminates are then dissolved by leaching with Na 2 CO 3 .
- a NaCl-Na 2 C0 3 mixture is sintered with fly ash, quenched in a water leach, and then leached in a dilute HN0 3 or H 2 S0 4 solution.
- the Calsinter process (developed at Oak Ridge National Laboratory, Tennessee, U.S.A.) involves the combination of a CaSO 4 -CaCO 3 -fly ash sintering system and an acid leach with H 2 SO 4 .
- alumino ⁇ silicate is reacted with hydrated calcium and/or magnesium chloride, with or without a minor proportion of sodium chloride.
- a leached water- insoluble residue is obtained which is treated, preferably with the application of heat, with a mineral acid such as HCl which forms a water-soluble aluminum salt.
- the salt is then diluted with water to produce an aqueous solution of the aluminum salt and an insoluble residue comprising hydrated silica.
- the aluminum is then recovered from the salt solution.
- U.S. 1,868,499 to Guertler describes a process for the recovery of alumina from silicious materials such as clay, leucite and silicious bauxite.
- the process comprises the steps of heating the silicious material with CaCl 2 at 650-900° C, treating the heated mixture with HCl to dissolve and separate CaCl 2 for reuse and conversion of the aluminum to A1C1 3 , separating the non-gelatinous silicic acid precipitate, and purifying the A1C1 3 solution and decomposing to form alumina.
- substantially pure as used in the present specification with respect to the alumina and silica products preferably relates to a purity of >97%, and most preferably to a purity of >99%.
- the process comprises the following further steps:
- step (v) substantially removing MgCl 2 from the CaCl 2 solution of step (iv);
- step (vi) recycling the CaCl 2 solution for use in step (i).
- the reuse of CaCl 2 contributes to the efficiency of the process.
- Fe is extracted from the A1C1 3 solution of step (ii) by either ion exchange or solvent extraction prior to or after the A1C1 3 crystallization of step (iv).
- novel process of the present invention differs from previously described processes, such as those described in GB 2,205,558 and US-
- the CaCl 2 which is recovered from the process for recycling must also be purified from MgCl 2 , since many sources of aluminosilicates contain small amounts of Mg impurities which dissolve in HCl during the leaching stage.
- the MgCl 2 is removed by precipitation with Ca(OH) 2 .
- Fig. 1 is a flow diagram of the process of the invention.
- the raw materials which can be used in the process of the invention include coal reject, fly ash, collieries, kaolin, shale, clays, and other aluminosilicate containing materials.
- the hydrated CaCl 2 can be in either salt form or brine.
- hydrated CaCl 2 is reacted with a material containing aluminosilicates and at a temperature of between 900-1300°C, and preferably at a temperature of 1000-1100°C. This temperature is lower than the temperatures of previously described processes (1300-1400°C), but higher than the temperature used in the process described in the Guertler patent, supra.
- the CaCl 2 is added to the alumino- silicate-containing material at a weight ratio of 0.5:1 - 3:1 depending on the phase composition of the material and its relative alumina content, as well as on the concentrations of mullite and silica. Most preferably, the weight ratio is in the range of 0.5:1 - 2:1.
- the mixture of alumino ⁇ silicate and CaCl 2 salt is dried at 200-250°C to obtain a solid mixture prior to heating (sintering).
- the aluminosilicate reacts with the CaCl 2 , for example according to the following reaction:
- the evolved HCl can be absorbed in a gas trap and used in the later steps.
- the aluminum and calcium salts are leached from the calcium-alumino-silicate by HCl at a concentration of 2-8N.
- the reaction is as follows: Ca 2 Al 2 SiO 7 + CaAl 2 Si 2 0 8 + Ca 12 Al 14 0 33 + 84HC1 — > I8AICI 3 + 15CaCl 2 + 42H 2 0 + 3Si0 2
- the resulting solution may contain a number of salts in addition to A1C1 3 and CaCl 2 such as FeCl 3 , MgCl 2 and heavy metals.
- the Si0 2 residue can be separated from the salt solution by known methods such as filtration and decantation.
- the Si0 2 will usually be of greater than 97% purity and at a yield of >90%.
- the A1C1 3 is separated from the solution by concentration and crystallization in a strongly acidic environment (HCl). Due to differences in solubility in the presence of a high chloride ion concentration, the A1C1 3 crystallizes before the other salts in the solution.
- the A1C1 3 crystals are filtered out and alumina is recovered by hydrolytic decomposition according to the following reaction:
- the HCl can be recovered for reuse.
- the A1 2 0 3 will usually be recovered at a purity of >99% and a yield of >95%.
- the Fe can also be recovered from the solution by either ion exchange or liquid extraction prior to or after the A1C1 3 crystallization.
- the remaining solution contains a high concentration of CaCl 2 which can be recovered for reuse in the first step of the process after removal of MgCl 2 , for example by precipitation with Ca(OH) 2 .
- Precipitation with Ca(OH) 2 also removes other metal chlorides present in the solution.
- Fig. 1 illustrates the complete process of the invention including the recycling of various components.
- the mixture was heated for 1 hour at 1100°C and then kept at 1100°C for an additional hour during which HCl vapors were released.
- the solid product was thoroughly leached with hot HCl 6N solution. 20 parts by weight of the product were leached for 2 hours with 100 ml of 6N HCl at 103°C.
- A1C1 3 *6H 2 0 was crystallized from the leaching solution by increasing the hydrochloric acid concentration to 30%. The crystals were filtered, washed with HCl and dissolved before being hydrolytically decomposed by heating at 400-600°C to produce pure alumina.
- the mixture was dried for 3 hours at 230°C.
- the dry product was then heated at 1100°C for 1 hour and then kept at 1100°C for an additional hour during which HCl vapors were released.
- the product was thoroughly leached with a hot 6N HCl solution. 20 parts by weight of the product were leached for 2 hours with 100 ml of 6N HCl at 103°C. Silica content in the residue was 98.6% of the dry material. The yield was 95%.
- A1C1 3 *6H 2 0 was crystallized from the leaching solution by increasing the HC1 concentration to 30%. The crystals were filtered and dissolved before hydrolytic decomposition by heating at 400-600°C to produce pure alumina.
- composition of the acidic filtrate from the crystallization step of the AlCl 3 *6H 2 O of Example 2 was: weight %
- Fe ions were extracted from the above solution. 654 parts by weight of the solution were then treated with 7.35 parts by weight of CaC0 3 and subsequently with 20.5 parts by weight of Ca(OH) 2 to precipitate Mg(OH), and the insoluble metal hydroxides and gypsum.
- the composition of the purified solution is: weight % AICI 3 1.6
- A1C1 3 *6H 2 0 was crystallized from the leaching solution by increasing the hydrochloric acid concentration to 30%. The crystals were filtered and dissolved prior to hydrolytic decomposition by heating at 400-600°C to produce pure alumina.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
Claims
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP96940107A EP0866769B1 (en) | 1995-12-15 | 1996-12-12 | Process for recovery of alumina and silica |
US09/091,457 US5993758A (en) | 1995-12-15 | 1996-12-12 | Process for recovery of alumina and silica |
DE69603289T DE69603289T2 (en) | 1995-12-15 | 1996-12-12 | METHOD FOR RECOVERY OF ALUMINUM OXIDE AND SILICON OXIDE |
JP9522639A JP2000505034A (en) | 1995-12-15 | 1996-12-12 | Recovery method of alumina and silica |
AU77079/96A AU713938B2 (en) | 1995-12-15 | 1996-12-12 | Process for recovery of alumina and silica |
KR10-1998-0704457A KR100421596B1 (en) | 1995-12-15 | 1996-12-12 | Process for Recovery of Alumina and Silica |
BR9612010-0A BR9612010A (en) | 1995-12-15 | 1996-12-12 | Process for the simultaneous recovery of substantially pure alumina and silica from an aluminosolicate |
HK99100062A HK1014923A1 (en) | 1995-12-15 | 1999-01-07 | Process for recovery of alumina and silica |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IL116409 | 1995-12-15 | ||
IL11640995A IL116409A (en) | 1995-12-15 | 1995-12-15 | Process for the recovery of alumina and silica |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1997022554A1 true WO1997022554A1 (en) | 1997-06-26 |
Family
ID=11068319
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/IL1996/000179 WO1997022554A1 (en) | 1995-12-15 | 1996-12-12 | Process for recovery of alumina and silica |
Country Status (18)
Country | Link |
---|---|
US (1) | US5993758A (en) |
EP (1) | EP0866769B1 (en) |
JP (1) | JP2000505034A (en) |
KR (1) | KR100421596B1 (en) |
CN (1) | CN1085622C (en) |
AT (1) | ATE182128T1 (en) |
AU (1) | AU713938B2 (en) |
BR (1) | BR9612010A (en) |
CA (1) | CA2240067A1 (en) |
CZ (1) | CZ184998A3 (en) |
DE (1) | DE69603289T2 (en) |
ES (1) | ES2134649T3 (en) |
HK (1) | HK1014923A1 (en) |
HU (1) | HUP0001163A3 (en) |
IL (1) | IL116409A (en) |
RU (1) | RU2176984C2 (en) |
WO (1) | WO1997022554A1 (en) |
ZA (1) | ZA9610486B (en) |
Cited By (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999008959A1 (en) * | 1997-08-14 | 1999-02-25 | Goodanew, Martin, Eric | A process for producing silica acid |
WO2001058807A1 (en) * | 2000-02-10 | 2001-08-16 | Promeks As | A process for the preparation of amorphous silica |
WO2005108290A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous silica from quartz preferably to be used as filler material |
WO2005108293A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous mesoporous silica from quartz |
WO2005108291A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous silica in particular xerogels for beer stabilization and for insulation purposes |
WO2005108292A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous and hydrophobic silica from quartz |
WO2008100123A1 (en) * | 2007-02-14 | 2008-08-21 | Alexandr Kosmukhambetov | Integrated method for processing alumosilicate raw material |
US9023301B2 (en) | 2012-01-10 | 2015-05-05 | Orbite Aluminae Inc. | Processes for treating red mud |
EP2755918A4 (en) * | 2011-09-16 | 2015-07-01 | Orbite Aluminae Inc | Processes for preparing alumina and various other products |
US9150428B2 (en) | 2011-06-03 | 2015-10-06 | Orbite Aluminae Inc. | Methods for separating iron ions from aluminum ions |
US9181603B2 (en) | 2012-03-29 | 2015-11-10 | Orbite Technologies Inc. | Processes for treating fly ashes |
US9260767B2 (en) | 2011-03-18 | 2016-02-16 | Orbite Technologies Inc. | Processes for recovering rare earth elements from aluminum-bearing materials |
US9290828B2 (en) | 2012-07-12 | 2016-03-22 | Orbite Technologies Inc. | Processes for preparing titanium oxide and various other products |
US9353425B2 (en) | 2012-09-26 | 2016-05-31 | Orbite Technologies Inc. | Processes for preparing alumina and magnesium chloride by HCl leaching of various materials |
US9410227B2 (en) | 2011-05-04 | 2016-08-09 | Orbite Technologies Inc. | Processes for recovering rare earth elements from various ores |
US9534274B2 (en) | 2012-11-14 | 2017-01-03 | Orbite Technologies Inc. | Methods for purifying aluminium ions |
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WO2002053500A2 (en) * | 2000-12-31 | 2002-07-11 | Ati-Aluminum Technologies Israel Ltd. | Production of aluminum compounds and silica from ores |
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WO2007116326A2 (en) * | 2006-02-20 | 2007-10-18 | Hyattville Company Ltd. | Production of solar and electronic grade silicon from aluminosilicate containing material |
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CN101759210B (en) * | 2010-01-18 | 2012-12-05 | 马昱昭 | Method for extracting high purity alumina and silica gel from coal ash |
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KR101443836B1 (en) * | 2012-04-17 | 2014-09-30 | 송병옥 | Apparatus of separating alumina and silica from kaolin and the method of the same |
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Citations (1)
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GB2205558A (en) * | 1987-05-18 | 1988-12-14 | Lonhro Plc | Recovery of alumina from aluminosilicates |
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US1868499A (en) * | 1929-06-07 | 1932-07-26 | Electric Smelting & Aluminum C | Process of recovering alumina from silicious materials containing it |
US2413709A (en) * | 1943-03-31 | 1947-01-07 | John D Hoffman | Method of recovering alumina and hydrochloric acid |
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US3427127A (en) * | 1966-05-09 | 1969-02-11 | Louis Stanton Mccollum | Process for recovering aluminum values from heat expandable materials |
US4056363A (en) * | 1974-03-21 | 1977-11-01 | Georg Messner | Apparatus for the fabrication of pure alumina from Al2 O3 and silica containing raw materials by leaching with hydrochloric acid |
DE2555875A1 (en) * | 1975-09-30 | 1977-03-31 | Financial Mining Ind Ship | PROCESS FOR PROCESSING ALUNIT |
US4158042A (en) * | 1977-10-07 | 1979-06-12 | Alcan Research And Development Limited | Recovery of alumina from siliceous minerals |
NO147516C (en) * | 1979-02-13 | 1983-04-27 | Elkem Spigerverket As | PROCEDURE FOR THE DEPOSIT OF A PURE ALUMINUM CHLORIDE FROM SOLUTIONS CONTAINING ALUMINUM AND MAGNESIUM IONS. |
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1995
- 1995-12-15 IL IL11640995A patent/IL116409A/en not_active IP Right Cessation
-
1996
- 1996-12-12 US US09/091,457 patent/US5993758A/en not_active Expired - Fee Related
- 1996-12-12 DE DE69603289T patent/DE69603289T2/en not_active Expired - Fee Related
- 1996-12-12 JP JP9522639A patent/JP2000505034A/en not_active Ceased
- 1996-12-12 RU RU98113521/12A patent/RU2176984C2/en not_active IP Right Cessation
- 1996-12-12 BR BR9612010-0A patent/BR9612010A/en not_active IP Right Cessation
- 1996-12-12 KR KR10-1998-0704457A patent/KR100421596B1/en not_active IP Right Cessation
- 1996-12-12 EP EP96940107A patent/EP0866769B1/en not_active Expired - Lifetime
- 1996-12-12 AT AT96940107T patent/ATE182128T1/en not_active IP Right Cessation
- 1996-12-12 HU HU0001163A patent/HUP0001163A3/en unknown
- 1996-12-12 AU AU77079/96A patent/AU713938B2/en not_active Ceased
- 1996-12-12 ES ES96940107T patent/ES2134649T3/en not_active Expired - Lifetime
- 1996-12-12 CZ CZ981849A patent/CZ184998A3/en unknown
- 1996-12-12 ZA ZA9610486A patent/ZA9610486B/en unknown
- 1996-12-12 CN CN96199671A patent/CN1085622C/en not_active Expired - Fee Related
- 1996-12-12 CA CA002240067A patent/CA2240067A1/en not_active Abandoned
- 1996-12-12 WO PCT/IL1996/000179 patent/WO1997022554A1/en active IP Right Grant
-
1999
- 1999-01-07 HK HK99100062A patent/HK1014923A1/en not_active IP Right Cessation
Patent Citations (1)
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GB2205558A (en) * | 1987-05-18 | 1988-12-14 | Lonhro Plc | Recovery of alumina from aluminosilicates |
Cited By (23)
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---|---|---|---|---|
WO1999008959A1 (en) * | 1997-08-14 | 1999-02-25 | Goodanew, Martin, Eric | A process for producing silica acid |
WO2001058807A1 (en) * | 2000-02-10 | 2001-08-16 | Promeks As | A process for the preparation of amorphous silica |
US6797249B2 (en) | 2000-02-10 | 2004-09-28 | Promeks As | Process for the preparation of amorphous silica |
WO2005108290A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous silica from quartz preferably to be used as filler material |
WO2005108293A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous mesoporous silica from quartz |
WO2005108291A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous silica in particular xerogels for beer stabilization and for insulation purposes |
WO2005108292A1 (en) * | 2004-05-12 | 2005-11-17 | Promeks As | Improved process for production of pure amorphous and hydrophobic silica from quartz |
WO2008100123A1 (en) * | 2007-02-14 | 2008-08-21 | Alexandr Kosmukhambetov | Integrated method for processing alumosilicate raw material |
US9260767B2 (en) | 2011-03-18 | 2016-02-16 | Orbite Technologies Inc. | Processes for recovering rare earth elements from aluminum-bearing materials |
US9945009B2 (en) | 2011-03-18 | 2018-04-17 | Orbite Technologies Inc. | Processes for recovering rare earth elements from aluminum-bearing materials |
US9410227B2 (en) | 2011-05-04 | 2016-08-09 | Orbite Technologies Inc. | Processes for recovering rare earth elements from various ores |
US9150428B2 (en) | 2011-06-03 | 2015-10-06 | Orbite Aluminae Inc. | Methods for separating iron ions from aluminum ions |
US9382600B2 (en) | 2011-09-16 | 2016-07-05 | Orbite Technologies Inc. | Processes for preparing alumina and various other products |
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US10174402B2 (en) | 2011-09-16 | 2019-01-08 | Orbite Technologies Inc. | Processes for preparing alumina and various other products |
AU2013202318B2 (en) * | 2012-01-10 | 2015-11-05 | Aem Technologies Inc. | Processes for treating red mud |
US9556500B2 (en) | 2012-01-10 | 2017-01-31 | Orbite Technologies Inc. | Processes for treating red mud |
US9023301B2 (en) | 2012-01-10 | 2015-05-05 | Orbite Aluminae Inc. | Processes for treating red mud |
US9181603B2 (en) | 2012-03-29 | 2015-11-10 | Orbite Technologies Inc. | Processes for treating fly ashes |
US9290828B2 (en) | 2012-07-12 | 2016-03-22 | Orbite Technologies Inc. | Processes for preparing titanium oxide and various other products |
US9353425B2 (en) | 2012-09-26 | 2016-05-31 | Orbite Technologies Inc. | Processes for preparing alumina and magnesium chloride by HCl leaching of various materials |
US9534274B2 (en) | 2012-11-14 | 2017-01-03 | Orbite Technologies Inc. | Methods for purifying aluminium ions |
WO2023044537A1 (en) * | 2021-09-21 | 2023-03-30 | Tianqi Lithium Kwinana Pty Ltd | A process for producing alumina |
Also Published As
Publication number | Publication date |
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HUP0001163A3 (en) | 2001-07-30 |
IL116409A0 (en) | 1996-03-31 |
CZ184998A3 (en) | 1999-03-17 |
CN1085622C (en) | 2002-05-29 |
KR20000064401A (en) | 2000-11-06 |
RU2176984C2 (en) | 2001-12-20 |
AU713938B2 (en) | 1999-12-16 |
DE69603289T2 (en) | 1999-12-09 |
JP2000505034A (en) | 2000-04-25 |
DE69603289D1 (en) | 1999-08-19 |
AU7707996A (en) | 1997-07-14 |
HK1014923A1 (en) | 1999-10-08 |
IL116409A (en) | 1999-11-30 |
ES2134649T3 (en) | 1999-10-01 |
CA2240067A1 (en) | 1997-06-26 |
BR9612010A (en) | 1999-12-28 |
EP0866769A1 (en) | 1998-09-30 |
ZA9610486B (en) | 1997-06-24 |
KR100421596B1 (en) | 2004-04-17 |
US5993758A (en) | 1999-11-30 |
HUP0001163A2 (en) | 2000-08-28 |
EP0866769B1 (en) | 1999-07-14 |
CN1207719A (en) | 1999-02-10 |
ATE182128T1 (en) | 1999-07-15 |
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