WO1997003022A1 - High yield precipitation process - Google Patents
High yield precipitation process Download PDFInfo
- Publication number
- WO1997003022A1 WO1997003022A1 PCT/AU1996/000435 AU9600435W WO9703022A1 WO 1997003022 A1 WO1997003022 A1 WO 1997003022A1 AU 9600435 W AU9600435 W AU 9600435W WO 9703022 A1 WO9703022 A1 WO 9703022A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- caustic
- liquor
- slurry
- precipitation
- stage
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/144—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by precipitation due to cooling, e.g. as part of the Bayer process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Definitions
- the present invention relates to an improved precipitation process used in the production of alumina by the Bayer process.
- the Bayer process is widely used to recover alumina from bauxite ores.
- the Bayer process involves contacting bauxite with a caustic liquor at elevated temperature to dissolve the alumina contained therein.
- Insolubles commonly called red mud, are separated from the resulting liquor.
- Dissolved impurities such as silicates and organics, may also be removed from the liquor.
- the dissolved alumina is recovered from the liquor by precipitation.
- the precipitation stage of the Bayer process involved passing a supersaturated Bayer liquor to a series of precipitation tanks, which are generally arranged in agglomeration and growth sections. Seed hydrate is typically added to both sections to promote precipitation of hydrate and produce particles of required size.
- Precipitation trains at alumina refineries include a plurality of stages, usually in the form of separate precipitation tanks, and the liquor is cooled as it moves through each successive tank. At the end ofthe precipitation stage, the precipitated hydrate particles are separated and classified. Smaller particles are generally retained as seed particles whilst particles in the desired size range are recovered and calcined to produce alumina.
- the Bayer process is widely used throughout the world and is well known to those involved in the production of alumina.
- alumina in solution sodium aluminate (NaAlO 2 ) and other dissolved aluminium values being formed as the dissolved species. Throughout this specification, this will be referred to as alumina in solution.
- the precipitation stage results in the precipitation of alumina trihydrate (Al 2 O 3 « 3H 2 O). This will be referred to as hydrate or precipitated hydrate.
- the precipitated hydrate is calcined to remove the water of hydration to form the final product alumina.
- the present invention provides an improved precipitation process that has the potential to increase alumina recovery.
- the present invention provides an improved precipitation process for producing hydrate from a Bayer liquor comprising precipitating hydrate from a Bayer liquor having a high caustic concentration, diluting the Bayer liquor to reduce the caustic concentration and precipitating further hydrate.
- the present invention provides a process for precipitating alumina trihydrate from a pregnant caustic liquor containing dissolved aluminium values, the process comprising the steps of supplying the pregnant caustic liquor to a precipitation stage of a Bayer plant, precipitating alumina trihydrate from the pregnant liquor to form a slurry of precipitated alumina trihydrate in caustic liquor, - adding an aqueous stream to the slurry to thereby dilute the caustic liquor and precipitating further alumina trihydrate.
- the present invention is particularly suitable for the production of smelter grade alumina.
- a Bayer feed liquor having high caustic concentration and a high dissolved alumina concentration is fed to a precipitation train. After precipitation in a high caustic environment, a dilution stream is added to reduce caustic concentration which thereby decreases alumina solubility and promotes further precipitation. This increases yields above currently achievable levels.
- the slurry obtained from precipitation in the high caustic environment is not deslurried before dilution, which means that the dilution stream is added to the slurry of precipitated hydrate in the caustic liquor.
- the dilution stream is preferably water or wash water which has been produced elsewhere in the Bayer process. Wash water may have a low caustic concentration. It will be appreciated that any liquid stream that has a lower caustic concentration than the Bayer liquor will be suitable for use as a dilution stream.
- the ratio of alumina concentration to caustic concentration stays substantially the same, because both the alumina and caustic concentrations are reduced by equal amounts.
- the equilibrium A/C is reduced and thus the supersaturation of the liquor is increased. This promotes further precipitation of hydrate.
- Dilution of the liquor may occur in a single step, for example, by addition of a large amount of dilution stream at a single point in the precipitation train.
- the dilution may occur as a plurality of smaller dilution steps, for example, by adding the dilution stream at two or more stages of the precipitation train.
- the Bayer liquor that is used as a feed stream to the high caustic precipitation has a caustic concentration in the range of 200-350gA£, calculated as Na 2 CO 3 more preferably 240-275g/ .
- the caustic concentration is preferably reduced to from 200-250g/-f .
- the alumina concentration of a Bayer liquor is usually measured by reporting the A/C ratio, which is:
- the A/C at the start ofthe high caustic precipitation is preferably within the range of 0.65-0.80, more preferably within the range of 0.72 to 0.75 at the preferred caustic concentration of 240-275 g/i?.
- the high caustic precipitation preferably proceeds until the A/C ratio in the precipitation liquor falls within the range of 0.40 to 0.60, more preferably 0.45 to 0.50. Addition ofthe dilution liquor does not significantly alter the A/C but it does reduce the caustic concentration.
- the A/C is preferably within the range of 0.25 to 0.35, more preferably 0.30 to 0.33.
- a currently preferred seeding strategy uses a double seeding strategy which is similar to that practiced at many alumina refineries throughout the world. This strategy includes:
- Coarse seed would be charged to give a solids content of 200 - 700g/£ in the last precipitator, more preferably about 400 - 500g/ solids in the last precipitator. This seed is preferably added to the first tank of the growth stage of the precipitative process.
- the temperature profile used in the precipitation train may also be any suitable profile.
- the feed liquor to the precipitation has a temperature of from 65 - 85°C, more preferably 75 - 80°C.
- Precipitators would be progressively cooled to achieve 45 - 55°C in the last of the precipitators. It is preferred that each precipitator is cooled by about 1-3°C relative to the adjacent upstream precipitator, in accordance with the disclosure in our co-pending Australian Patent Application
- the total residence time for the precipitation process may be in the range of about 30 to 50 hours, more preferably about 40 - 45 hours, with the high caustic precipitation suitably having a residence time of about 15 - 20 hours.
- the improved precipitation process of the present invention allows a yield of up to 95 to 120g £ A1 2 0 3 or higher. This is considerably higher than current best practice that obtains hydrate yields of about 85g/f A1 2 0 3 .
- the slurry from the last precipitator is treated to separate the solids from the liquor. After removing suitable quantities of the solids for seeding, the particles of the desired size range are calcined to form the alumina product.
- the liquor recovered from the last precipitator of the precipitation train is conventionally returned to the digestion step in which the liquor is contacted with bauxite to extract alumina into solution.
- this liquor has a lower caustic concentration due to the dilution carried out during the precipitation process.
- this liquor it is likely to be necessary to treat this liquor to increase its caustic concentration prior to re-using the liquor in the extraction step. Preferably, this is achieved by evaporating off some of the water from the liquor equivalent to the dilution added.
- any other process that increases the caustic concentration of the liquor may also be used.
- the process of the present invention adds another degree of freedom to the precipitation phase of the Bayer process.
- Conventional Bayer precipitation processes control the inlet A/C ratio, feed caustic concentration, seeding parameters and temperature profile.
- the process of the present invention also allows for control of the caustic concentration of the liquor during the precipitation process by providing for dilution during precipitation.
- the process of the present invention provides increased production and improved efficiency. Hydrate quality may be improved by reducing soda pick-up. Moreover, stand-alone ancillary processes that are normally uneconomic may be attached to Bayer processes in an economic way, e.g. recovery of soda from DSP in mud. If an evaporation plant is used to concentrate the diluted caustic liquor after precipitation, power generation by high efficiency co-generation power stations becomes possible. Processes which recover soda from DSP in mud usually produce a dilute caustic stream of say 10-50 gpl Na ⁇ O*,. Although this stream contains valuable caustic it also contains water. To reuse (recover) the caustic, the stream must be re-introduced to the Bayer process circuit.
- the stream is introduced as a dilute stream in a Bayer process circuit having a conventional precipitation step there is too much water added to the circuit and as a consequence the evaporation capacity of the refinery has to be increased. This requires capital and increased energy. Such processes do not provide for economic recovery of caustic when the cost of caustic and energy (fuel) are considered.
- the dilute caustic stream can be introduced to the Bayer circuit to give increased precipitation yield. It is still necessary to evaporate the additional water but when the additional alumina production from increased yield is considered the process of caustic recovery may produce favourable economics.
- Bayer refineries require electrical power.
- the power can be purchased from a State authority if the refinery is suitably located but has to be generated by the refinery if located in a remote area. In such a case power is usually generated by steam turbines. In a refinery which has a requirement for low pressure steam, e.g. to run an Evaporation Plant, the power can be generated by operating back pressure or let-down turbines, so producing low pressure steam and power from the feed high pressure steam from the Boilerhouse (co-generation). However, in a refinery that does not use low pressure steam the power is generated by condensing turbines where cooling water is used to condense the steam. The fuel efficiency of the co-generation power station is 70-80% whereas in the power station using condensing turbines it is 25-35%.
- Soda pick-up in hydrate occurs primarily in areas of the process with high alumina supersaturation, i.e. in front-end of the precipitation process.
- the improved process may achieve higher yields by recovering more hydrate from the area where low soda hydrate is produced, i.e. within latter part ofthe process where supersaturations are lower. While the addition of dilution liquor increases the supersaturation to promote precipitation the increase is not sufficient to increase soda pick-up, so the high soda hydrate produced at the front-end gets diluted by the increase of low soda hydrate.
- the present process is also especially useful for modern alumina refineries.
- Such refineries typically utilise very high caustic concentration to digest the bauxite.
- caustic liquors having a high caustic concentration are very aggressive, corrosive liquors that can cause severe corrosion of the process vessels used in digestion, especially at higher temperatures used for boehmite digestion.
- limitations may be put on the digestion process (in terms of either or both of residence time and digestion temperatures).
- the content of dissolved alumina in the pregnant liquors may be high, the supersaturation of those liquors may be low.
- the dilution step or steps included in the present invention act to increase the supersaturation of the liquor and allow recovery of a larger proportion of the dissolved alumina content of the caustic liquor.
- FIGURE 1 is a schematic diagram of the general flowsheet ofthe process of the present invention
- FIGURE 2 is a schematic diagram showing a general flowsheet of a conventional precipitation process used in the Bayer process
- FIGURE 3 shows an expanded flowsheet ofthe conventional precipitation process of FIGURE 2
- FIGURE 4 shows an expanded flowsheet of a precipitation process according to the present invention
- FIGURE 5 shows another expanded flowsheet of a precipitation process according to the present invention.
- feed liquor is supplied to a high caustic precipitation process which includes a double seeding strategy.
- the slurry resulting from the high caustic precipitation is diluted and a low caustic precipitation then occurs to precipitate further hydrate.
- the slurry bearing the low caustic precipitation stages is subsequently sent to classification.
- FIG. 2 shows a schematic diagram of a prior art precipitation process.
- feed liquor is supplied to a high caustic precipitation process which includes a doubled seeding strategy.
- the slurry levering the high caustic precipitation process is then sent to classification.
- Figure 3 is an expanded flowsheet of the conventional precipitation process shown in Figure 2.
- the precipitation train includes two agglomeration precipitators Al and A2 and a growth stage having a multiplicity of growth precipitators Gl, G2,...G Last.
- a Bayer liquor 10 is fed to the first agglomeration precipitator Al.
- Washed tertiary seed 12 is also supplied to agglomeration precipitator Al.
- the slurry of seed and liquor (which will also include some agglomerated or precipitated hydrate) then passes to precipitator A2 and then into the first of the growth precipitators Gl. Deliquored secondary seed 14 is also fed to first growth precipitator Gl .
- the slurry of liquor and hydrate sequentially passes through the growth precipitators and it is slowly cooled. The A/C ratio of the liquor gradually reduces but the caustic concentration remains essentially constant. After leaving the final growth precipitator (G Last), the slurry is classified
- the secondary seed is deliquored at 18 to produce a deliquored secondary seed 14 and spent liquor stream 20.
- the tertiary seed is deliquored and washed at 22 to produce tertiary seed 12 and spent liquor stream 24.
- the product hydrate is washed at 26 which produces a wash water/spent liquor stream 28 and a washed product hydrate 30.
- FIG 4 is an expanded flowsheet showing one embodiment of the precipitation process of the present invention.
- This flowsheet includes agglomeration precipitators Al and A2 and a multiplicity of growth precipitators Gl, G2,...G Last.
- Pregnant liquor 110 and tertiary seed 112 are supplied to agglomeration precipitator Al.
- the slurry passes sequentially through precipitator A2 to precipitator Gl, wherein secondary seed 114 is added.
- the flowsheet of Figure 4 is essentially identical to the flowsheet of Figure 3.
- a dilution stream 115 is added to the slurry. This reduces the caustic concentration without changing the A/C ratio and this increases the yield of hydrate in the overall process.
- the slurry leaving the last precipitator (G Last) is classified into secondary seed, tertiary seed and product hydrate.
- the respective spent liquor streams 120, 124 and 128 are combined and evaporated in an evaporation plant 132.
- Evaporation plant 132 is required in order to remove the dilution water added during the precipitation process to thereby concentrate the spent liquor to a caustic concentration suitable for use in digesting bauxite.
- Figure 5 is another embodiment of the precipitation process of the present invention.
- the flowsheet of Figure 5 is similar to that shown in Figure 4, with the exception that the dilution stream is added as a series of dilution streams 215a, 215b ... 215x to the respective growth precipitators Gl, G2,... G(Last-l).
- the embodiments shown in Figures 4 and 5 respectively show addition of the dilution stream in one step and addition of the dilution stream in a number of steps. It will be appreciated that the dilution stream may be added as a single stream to one precipitator, as two streams to two precipitators or as a number of streams to a number of precipitators. All such additions fall within the scope ofthe present invention.
- the embodiments of Figures 4 and 5 also show seed additions to precipitators Al and Gl. Other seeding strategies may be used that vary the number of seed additions and/or the precipitators to which the seed is added. All such seeding strategies fall within the scope of the present invention.
- Tables 4 and 5 detail the experimental results obtained using the profile 1 in which dilution occurred just before the commencement of the stage at 72°C.
- Table 6 details the results obtained using Profile 2 in which dilution took place just prior to commencement ofthe stage at 72.4°C.
- the liquor was diluted with the aim of obtaining a caustic concentration within the range of 200- 250 g/£ following dilution. This was a calculated value and the actual caustic concentration obtained after dilution is similar to the end liquor caustic concentrations given in Tables 4, 5 and 6.
- Oxalate (g/l as Na ⁇ O n/a (-1) n/a
- Oxalate (g/l as Na ⁇ O n/a ( ⁇ 1) n/a
- Oxalate (g/l as Na ⁇ O ⁇ n/a n/a
- Table 10 tabulates the start and finish caustic soda contents of the liquor and the yield (in g/l as Al 2 O 3 ) obtained from the experiments detailed in Tables 4 to 9.
- the yield is determined by a number of solution and process conditions, chiefly the pregnant liquor A/C, caustic soda concentration, and inlet/outlet temperatures.
- the temperature profile plays an important role in the quality ofthe product, influencing such aspects as soda percentage and strength.
- the liquor conditions determine the equilibrium alumina concentration, and as Bayer liquors are supersaturated, the difference between the actual and equilibrium alumina concentration (the supersaturation) is also dependent on the liquor condition. This difference is generally accepted as the driving force for precipitation, and is the main influence on the yield obtained in any given process configuration.
- the process of the present invention includes a dilution step in which water or a low strength caustic stream is added to the slurry of liquor and hydrate. This decreases the caustic concentration of the liquor, and although the A/C ratio of the liquor remains unchanged, the equilibrium alumina concentration of the liquor is lower at the lower caustic concentration and this increases the supersaturation ofthe liquor. This results in an increase in the driving force for precipitation.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP96922684A EP0839118A4 (en) | 1995-07-11 | 1996-07-11 | High yield precipitation process |
BR9609429-0A BR9609429A (en) | 1995-07-11 | 1996-07-11 | High-yield precipitation process. |
AU63484/96A AU697413B2 (en) | 1995-07-11 | 1996-07-11 | High yield precipitation process |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AUPN4107 | 1995-07-11 | ||
AUPN4107A AUPN410795A0 (en) | 1995-07-11 | 1995-07-11 | High yield precipitation process |
AUPN4785 | 1995-08-14 | ||
AUPN4785A AUPN478595A0 (en) | 1995-08-14 | 1995-08-14 | High yield precipitation process |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1997003022A1 true WO1997003022A1 (en) | 1997-01-30 |
Family
ID=25644991
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/AU1996/000435 WO1997003022A1 (en) | 1995-07-11 | 1996-07-11 | High yield precipitation process |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP0839118A4 (en) |
KR (1) | KR19990028922A (en) |
BR (1) | BR9609429A (en) |
CA (1) | CA2226842A1 (en) |
WO (1) | WO1997003022A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008116260A1 (en) * | 2007-03-27 | 2008-10-02 | Alcoa Of Australia Limited | Method for preparing aluminium oxide |
CN113608506A (en) * | 2021-06-18 | 2021-11-05 | 东北大学 | Intelligent detection device for alumina operation index |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018194397A1 (en) * | 2017-04-19 | 2018-10-25 | 한국지질자원연구원 | Method for smelting ilmenite using red mud |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3486850A (en) * | 1967-02-16 | 1969-12-30 | Kaiser Aluminium Chem Corp | Flash cooling of liquor during the continuous precipitation of alumina hydrate from bayer process liquor |
US4051222A (en) * | 1971-09-21 | 1977-09-27 | Alcan Research And Development Limited | Coarsening of partially calcined alumina dust |
US4305913A (en) * | 1980-08-06 | 1981-12-15 | Kaiser Aluminum & Chemical Corporation | Alumina hydrate production from Bayer liquor by seeding |
AU4373189A (en) * | 1988-10-27 | 1990-05-03 | Gyorgy Banvolgyi | Process for producing alumina from gibbsitic bauxites |
AU7768794A (en) * | 1993-11-09 | 1995-05-18 | Aluminium Pechiney | Process for the treatment of bauxites containing alumina trihydrate and alumina monohydrate |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NO135059C (en) * | 1975-04-16 | 1977-02-02 | Norsk Hydro As | |
FR2591581B1 (en) * | 1985-12-17 | 1990-05-25 | Pechiney Aluminium | PROCESS FOR OBTAINING HIGH PRODUCTIVITY OF ALUMINUM TRIHYDROXIDE, HIGH PURITY AND MEDIAN DIAMETER LESS THAN 4 MICROMETERS, ADJUSTED ON REQUEST. |
-
1996
- 1996-07-11 KR KR1019980700224A patent/KR19990028922A/en not_active Application Discontinuation
- 1996-07-11 WO PCT/AU1996/000435 patent/WO1997003022A1/en not_active Application Discontinuation
- 1996-07-11 BR BR9609429-0A patent/BR9609429A/en not_active Application Discontinuation
- 1996-07-11 CA CA002226842A patent/CA2226842A1/en not_active Abandoned
- 1996-07-11 EP EP96922684A patent/EP0839118A4/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3486850A (en) * | 1967-02-16 | 1969-12-30 | Kaiser Aluminium Chem Corp | Flash cooling of liquor during the continuous precipitation of alumina hydrate from bayer process liquor |
US4051222A (en) * | 1971-09-21 | 1977-09-27 | Alcan Research And Development Limited | Coarsening of partially calcined alumina dust |
US4305913A (en) * | 1980-08-06 | 1981-12-15 | Kaiser Aluminum & Chemical Corporation | Alumina hydrate production from Bayer liquor by seeding |
AU4373189A (en) * | 1988-10-27 | 1990-05-03 | Gyorgy Banvolgyi | Process for producing alumina from gibbsitic bauxites |
AU7768794A (en) * | 1993-11-09 | 1995-05-18 | Aluminium Pechiney | Process for the treatment of bauxites containing alumina trihydrate and alumina monohydrate |
Non-Patent Citations (1)
Title |
---|
See also references of EP0839118A4 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008116260A1 (en) * | 2007-03-27 | 2008-10-02 | Alcoa Of Australia Limited | Method for preparing aluminium oxide |
CN113608506A (en) * | 2021-06-18 | 2021-11-05 | 东北大学 | Intelligent detection device for alumina operation index |
Also Published As
Publication number | Publication date |
---|---|
EP0839118A4 (en) | 1998-12-09 |
EP0839118A1 (en) | 1998-05-06 |
CA2226842A1 (en) | 1997-01-30 |
BR9609429A (en) | 2000-04-25 |
KR19990028922A (en) | 1999-04-15 |
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