Patent Application
20140286841
The present disclosure relates to improvements in the field of chemistry applied to the synthesis and/or separation of iron-bearing products and/or aluminum-bearing products. For example, such methods are useful for separating iron ions and aluminum ions contained in a same composition. For example, the methods can also be useful for treating an acidic composition comprising aluminum ions and iron ions.
Iron ions can be difficult to remove from certain ores. For example, extracting aluminum ions from certain material (such as red mud) or certain ores (such as aluminum-bearing ores comprising iron ions) has been a considerable challenge since iron ions are contained in these ores and it can be difficult to separate them from aluminum ions in a simple and cost effective manner.
There is thus a need for providing an alternative method for separating iron ions from aluminum ions. There is thus also a need for treating compositions comprising iron ions and aluminum ions. There is also a need for providing a method that would overcome at least one drawback from the prior art methods.
According to one aspect, there is provided a method for separating iron ions from aluminum ions contained in an acidic composition, the method comprising:
According to another aspect, there is provided a method for separating iron ions from aluminum ions contained in an acidic composition, the method comprising:
According to another aspect, there is provided a method for treating an acidic composition comprising iron ions and aluminum ions, the method comprising:
According to another aspect, there is provided a method for treating an acidic composition comprising iron ions and aluminum ions, the method comprising:
According to another aspect, there is provided a method for separating iron ions from aluminum ions contained in a composition, the method comprising:
According to another aspect, there is provided a method for separating iron ions from aluminum ions contained in a composition, the method comprising:
According to another aspect, there is provided a method for treating a composition comprising iron ions and aluminum ions, the method comprising:
According to another aspect, there is provided a method for treating a composition comprising iron ions and aluminum ions, the method comprising:
In the following drawings, which represent by way of example only, various embodiments of the disclosure:
Further features and advantages will become more readily apparent from the following description of various embodiments as illustrated by way of examples only and in a non-limitative manner.
The expression “at least substantially preventing precipitation of the aluminum ions” as used herein refers to the fact that less than about 20%, less than about 10%, less than about 5%, less than about 3%, less than about 2% or less than about 1% of the aluminum ions are precipitated.
The term “hematite” as used herein refers, for example, to a compound comprising α-Fe2O3, γ-Fe2O3, β-FeO.OH or mixtures thereof.
The expression “iron ions” as used herein refers, for example to ions comprising to at least one type of iron ion chosen from all possible forms of Fe ions. For example, the at least one type of iron ion can be Fe2+, Fe3+, or a mixture thereof.
The expression “aluminum ions” as used herein refers, for example to ions comprising to at least one type of aluminum ion chosen from all possible forms of Al ions. For example, the at least one type of aluminum ion can be Al3+.
Terms of degree such as “about” and “approximately” as used herein mean a reasonable amount of deviation of the modified term such that the end result is not significantly changed. These terms of degree should be construed as including a deviation of at least ±5% or at least ±10% of the modified term if this deviation would not negate the meaning of the word it modifies.
The expression “is maintained” as used herein when referring to a value of a pH or a pH range of the precipitation composition refers to maintaining the value of the pH or the pH range at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the acidic composition and the basic aqueous composition or the reaction between the acidic composition and the base.
The expression “maintaining the precipitation composition at” as used herein when referring to a value of a pH or a pH range, refers to maintaining the value of the pH or the pH range of the precipitation composition at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the acidic composition and the basic aqueous composition or the reaction between the acidic composition and the base.
The expression “is maintained” as used herein when referring to a value of a temperature or a temperature range of the precipitation composition refers to maintaining the value of the temperature or the temperature range at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the acidic composition and the basic aqueous composition or the reaction between the acidic composition and the base.
The expression “is maintained” as used herein when referring to a value of a pH or a pH range of the precipitation composition refers to maintaining the value of the pH or the pH range at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the composition and the basic aqueous composition or the reaction between the composition and the base.
The expression “maintaining the precipitation composition at” as used herein when referring to a value of a pH or a pH range, refers to maintaining the value of the pH or the pH range of the precipitation composition at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the composition and the basic aqueous composition or the reaction between the composition and the base.
The expression “is maintained” as used herein when referring to a value of a temperature or a temperature range of the precipitation composition refers to maintaining the value of the temperature or the temperature range at least 75, 80, 85, 90, 95, 96, 97, 98 or 99% of the time during the reaction between the composition and the basic aqueous composition or the reaction between the composition and the base.
For example, the method can comprise:
obtaining the acidic composition comprising the aluminum ions and the iron ions;
adding the acidic composition into the basic aqueous composition having a pH of at least 10.5 so as to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion; and
separating the liquid portion from the solid portion.
For example, the method can comprise:
For example, the method can comprise:
For example, reacting the acidic composition with the basic aqueous composition is carried out by adding the acidic composition into the basic composition while maintaining the pH of the basic aqueous composition above 10.5 by adding a further amount of base while adding the acidic composition into the basic aqueous composition.
For example, reacting the acidic composition with the base is carried out by adding the acidic composition into the base while maintaining the pH of the precipitation composition above 10.5 by adding a further amount of base while adding the acidic composition.
For example, the acidic composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
For example, the acidic composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
For example, the acidic composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the precipitation composition.
For example, the acidic composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the basic aqueous composition.
For example, the acidic composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the precipitation composition.
For example, the acidic composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the base.
For example, maintaining the pH of the basic aqueous composition above 10.5 can be carried out by adding a further amount of base while adding the acidic composition into the reactor.
For example, maintaining the pH of the precipitation composition above 10.5 is carried out by adding a further amount of base while adding the acidic composition into the reactor.
For example, the acidic composition can be an acidic leaching composition.
For example, the acidic leaching composition can be obtained by leaching an aluminum-bearing ore that comprises iron with at least one acid so as to obtain a leachate and a solid residue and by substantially isolating the leachate. For example, a filtration, decantation, centrifugation etc. can be done.
For example, the method can comprise:
obtaining the composition comprising the aluminum ions and the iron ions;
adding the composition into the basic aqueous composition having a pH of at least 10.5 so as to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion; and
separating the liquid portion from the solid portion.
For example, the method can comprise:
For example, the method can comprise:
For example, reacting the composition with the basic aqueous composition is carried out by adding the composition into the basic composition while maintaining the pH of the basic aqueous composition above 10.5 by adding a further amount of base while adding the composition into the basic aqueous composition.
For example, reacting the composition with the base is carried out by adding the composition into the base while maintaining the pH of the precipitation composition above 10.5 by adding a further amount of base while adding the composition.
For example, the composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
For example, the composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
For example, the composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the precipitation composition.
For example, the composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the basic aqueous composition.
For example, the composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the precipitation composition.
For example, the composition and the base can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition, the reactor having previously been provided with a quantity of the base.
For example, maintaining the pH of the basic aqueous composition above 10.5 can be carried out by adding a further amount of base while adding the composition into the reactor.
For example, maintaining the pH of the precipitation composition above 10.5 is carried out by adding a further amount of base while adding the composition into the reactor.
For example, the composition can be an acidic leaching composition.
For example, the acidic leaching composition can be obtained by leaching an aluminum-bearing ore that comprises iron with at least one acid so as to obtain a leachate and a solid residue and by substantially isolating the leachate. For example, a filtration, decantation, centrifugation etc. can be done.
The acid used for leaching can be HCl, H2SO4, HNO3 or mixtures thereof. For example, HCl can be used. More than one acid can be used as a mixture or separately. Solutions made with these acids can be used at various concentration. For example, concentrated solutions can be used. For example, 6 M or 12 M HCl can be used. For example, up to 100% wt H2SO4 can be used.
The leaching can be carried out under pressure. For example, the pressure can be about 10 to about 300 psig, about 25 to about 250 psig, about 50 to about 200 psig or about 50 to about 150 psig. The leaching can be carried out for about 30 minutes to about 5 hours. It can be carried out at a temperature of about 60 to about 300° C., about 75 to about 275° C. or about 100 to about 250° C.
For example, the precipitation composition can be maintained at a pH of at least about 11.0, at least about 11.5, at least about 12.0, about 10.5 to about 14.5, about 10.5 to about 11.0, about 11.0 to about 14.0, about 11.0 to about 13.0, or about 11.0 to about 12.0.
For example, the precipitation composition can be maintained at a pH of about 10.8 to about 11.8, about 11 to about 12, about 11.5 to about 12.5, about 11.0 to about 11.6, about 11.2 to about 11.5, about 10.5 to about 12, about 11.5 to about 12.5, or about 11.8 to about 12.2, about 11.0, about 11.1, about 11.2, about 11.3, about 11.4, about 11.5, about 11.6, about 11.7, about 11.8, about 11.9, or about 12.0.
For example, the precipitation composition can be maintained at a pH comprised between 10.5 and 14.0; 10.5 and 13.0; 10.5 and 12.0; 10.5 and 11.5; or 10.5 and 11.
For example, addition of the acidic composition into the basic aqueous composition can be carried out by maintaining the pH of the basic composition above 10.5 by adding a further amount of base while adding the acidic composition into the basic aqueous composition.
For example, addition of the composition into the basic aqueous composition can be carried out by maintaining the pH of the basic composition above 10.5 by adding a further amount of base while adding the composition into the basic aqueous composition.
For example, the base can comprise KOH, NaOH, Ca(OH)2, CaO, MgO, Mg(OH)2, CaCO3, Na2CO3, NaHCO3, or mixtures thereof.
For example, the base can comprise KOH, NaOH, or a mixture thereof.
For example, the basic aqueous composition can comprise KOH, NaOH, Ca(OH)2, CaO, MgO, Mg(OH)2, CaCO3, Na2CO3, NaHCO3, or mixtures thereof.
For example, the basic aqueous composition can comprise KOH, NaOH, or a mixture thereof.
For example, the acidic composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
For example, the composition and the basic aqueous composition can be added simultaneously into a reactor so as to be reacted together and to obtain the precipitation composition while maintaining the pH of the precipitation composition above 10.5 so as to cause precipitation of the iron ions, at least substantially preventing precipitation of the aluminum ions, and to obtain a mixture comprising a liquid portion and a solid portion.
The basic aqueous composition can comprise KOH, NaOH, Ca(OH)2, CaO, MgO, Mg(OH)2, CaCO3, Na2CO3, NaHCO3, or mixtures thereof.
For example, the basic aqueous composition can comprise KOH, NaOH or a mixture thereof.
For example, the basic aqueous composition and the acidic composition can be added in a volume:volume proportion of about 1:2 to about 1:6, about 1:3 to about 1:5, or about 1:3 to about 1:4.
For example, the basic aqueous composition and the composition can be added in a volume:volume proportion of about 1:2 to about 1:6, about 1:3 to about 1:5, or about 1:3 to about 1:4.
For example, the acidic composition, prior to be reacted with the basic aqueous composition, can have a pH of about 1 to about 3, about 1.5 to about 2.5, or about 1.8 to about 2.2.
For example, the acidic composition, prior to be reacted with the base, can have a pH of about 1 to about 3, about 1.5 to about 2.5, or about 1.8 to about 2.2.
The basic aqueous composition, prior to be reacted with the acidic composition, can have a pH of about 11 to about 15, about 12 to about 14, or about 13 to about 14. The basic aqueous composition can have a concentration of about 10 to about 25 M, about 15 to about 20 M or about 19 to about 20 M.
The basic aqueous composition, prior to be reacted with the composition, can have a pH of about 11 to about 15, about 12 to about 14, or about 13 to about 14. The basic aqueous composition can have a concentration of about 10 to about 25 M, about 15 to about 20 M or about 19 to about 20 M.
For example, the precipitated iron ions can be recovered.
For example, the precipitated iron ions can be chosen from Fe3+, Fe2+, and a mixture thereof.
For example, the precipitated iron ions can be under the form of Fe(OH)2, Fe(OH)3), or a mixture thereof.
For example, the precipitated iron ions can be under the form of hematite.
For example, the predetermined quantity of hematite can be added to the mixture comprising the liquid portion and the solid portion. For example, this can be made over a predetermined period of time and optionally under agitation.
For example, the predetermined quantity of hematite can be added at a molar ratio hematite/iron ions of about 0.005 to about 0.5 or about 0.01 to about 0.1.
For example, the precipitation composition can be maintained at a temperature of about 50° C. to about 110° C., about 60° C. to about 90° C., about 65° C. to about 85° C., about 70° C. to about 75° C., about 75° C. to about 110° C., about 80° C. to about 100° C., about 85° C. to about 95° C. or about 87° C. to about 93° C.
The aluminum-bearing material that comprises iron can be an aluminium-bearing ore that comprises iron. For example, clays, argillite, mudstone, beryl, cryolite, garnet, spinel, bauxite, or mixtures thereof can be used as starting material. For example, the aluminum-bearing ore can be argillite. The aluminum-containing material can also be a recycled industrial aluminum-bearing material such as slag. The aluminum-bearing material can also be red mud or fly ashes.
For example, iron ions can be precipitated. When precipitating iron ions, the iron ions can be precipitated by means of an ionic precipitation and they can precipitate in the form of various salts, hydroxides or hydrates thereof. For example, the iron ions can be precipitated as Fe(OH)3, Fe(OH)2, hematite, geotite, jarosite or hydrates thereof.
The leaching can be carried out at a pH of about 0.5 to about 2.5., about 0.5 to about 1.5, or about 1; then iron can be precipitated at a pH of at least about 10.5, 11, 11.5, 12.0; then aluminum can be precipitated at a pH of about 7 to about 11, about 7.5 to about 10.5, or about 8 to about 9.
The leaching can be carried out under pressure into an autoclave. For example, it can be carried out at a pressure of 5 KPa to about 850 KPa, 50 KPa to about 800 KPa, 100 KPa to about 750 KPa, 150 KPa to about 700 KPa, 200 KPa to about 600 KPa, or 250 KPa to about 500 KPa. The leaching can be carried out at a temperature of at least 80° C., at least 90° C., or about 100° C. to about 110° C. In certain cases it can be done at higher temperatures so as to increase extraction yields in certain ores.
For example, the aluminum ions can be recovered.
For example, aluminum ions (from the liquid portion) can be precipitated. When precipitating aluminum ions, the aluminum ions can be precipitated by means of an ionic precipitation and they can precipitate in the form of various salts, (such as chlorides, sulfates, hydroxides, or hydrates thereof). For example, the aluminum ions can be precipitated as Al(OH)3, AlCl3, Al2(SO4)3, or hydrates thereof.
For example, the methods can further comprise precipitating the aluminum ions from the liquid portion by adjusting the pH at a value of about 7 to about 11, about 8 to about 10.5, about 8.5 to about 10, about 9 to about 10, or about 9.2 to about 9.8.
The methods can further comprise adding a precipitating agent effective for facilitating precipitation of the aluminum ions. For example, the precipitating agent can be a polymer. For example, the precipitating agent can be an acrylamide polymer.
For example, precipitated aluminium ions can be converted into alumina by means of a calcination. Such a step can be carried out by calcination. Al(OH)3 can then be converted into Al2O3. Such a conversion of Al(OH)3 into Al2O3 can be carried out at a temperature of about 800° C. to about 1200° C. For example, it can be carried out as indicated in WO 2008141423 that is hereby integrated by reference in its entirety. Thus, the person skilled in the art would clearly understand how to convert Al(OH)3 into Al2O3.
For example, the methods can further comprise converting alumina (Al2O3) into aluminum. Conversion of alumina into aluminum can be carried out, for example, by using the Hall-Héroult process. References is made to such a well known process in various patents and patent applications such as US 20100065435; US 20020056650; U.S. Pat. No. 5,876,584; U.S. Pat. No. 6,565,733. Conversion can also be carried out by means of other methods such as those described in U.S. Pat. No. 7,867,373; U.S. Pat. No. 4,265,716; U.S. Pat. No. 6,565,733 (converting alumina into aluminum sulfide followed by the conversion of aluminum sulfide into aluminum.) These documents are also hereby integrated by reference in their entirety. Thus, the person skilled in the art would clearly understand how to convert Al2O3 into aluminum.
For example, Al(OH)3 can be converted into AlCl3. This can be done, for example, by reacting Al(OH)3 with HCl.
As it can be seen from
In the methods of
In the methods of
As discussed in the present disclosure, the iron precipitate shown in
It should also be noted that according to other examples of the present disclosure, methods represented in
In
The aluminum-bearing ore (for example argillite) can be activated mechanically by grinding. Mineral activation leads to a positive influence on the leaching reaction kinetics. For example, a ball mill can be used in air atmosphere for about 2 to 4 hours. Argillite can be also calcinated. This stage of pretreatment can be accomplished at a calcinating temperature between about 400 to about 700° C. for a period about 1 to about 2 hours. These two operations, for example, increase the quantity of extracted aluminum by about 25 to 40%.
Acid leaching can be made by mixing activated argillite with an acid solution (for example HCl) at elevated temperature and under pressure during a given period of time. For example, the argillite/acid ratio can be of about of 1:3 (weight/volume), the concentration of about 6M, the pressure can be of about 70 to about 80 psi, the temperature can be of about 150 to about 170° C., and the reaction time can be about 1 hour to about 7 hours. Under these conditions, over 90% of aluminum and 100% of the iron can be extracted besides the impurities.
At the end of extraction, the solid (non-dissolved portion) can be separated from the liquid rich aluminum and iron by decantation or by filtration, after which is washed. This solid represent about 50 to about 60% of the initial mass of argillite. It can be valorized and be used as constituent alloy.
Separating Aluminum Ions from Iron Ions (Removal of Iron)
The iron contained in the solution can be removed by selectively precipitating it at certain pH values. For example, iron removal can be carried out by precipitation in a basic medium at a pH greater than about 11.0 or 11.2. This stage can be made by reacting the acidic composition (pH of about 2) containing aluminum and iron ions in a basic aqueous composition (see
Hematite can also be added (can be called seeding hematite) to the precipitation reaction. Hematite seed addition can enhance hematite precipitation reaction (for example transformation of Fe(OH)2 and/or Fe(OH)3) into hematite). For example, hematite can be added in a proportion of 10 g for 1L of precipitation composition optionally under agitation. The reaction temperature can be of about 70° C. to about 90° C. (for example, the precipitation composition can be at such a temperature), and the reaction time can be of about 3 hours to about 72 hours. Under such conditions, about 98% to about 100% of iron can be precipitated and about 70% to 100% of this iron can be precipitated as hematite. Optionally, it is possible to recover iron by using a refining step by liquid-liquid extraction for example, through a hollow fiber membrane.
It is possible 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 1M to 2M). At the end of this step, the solid can be washed with water.
This step can also be carried in various ways. Aluminum ions can be precipitated under the form of aluminum hydroxide. For example, an hydrated form of Al(OH)3 can be obtained (by addition of an acid) at a pH of about 7 to about 10.5 or about 7.5 to about 10 or about 9. The temperature can be of about 50° C. to about 80° C., and the reaction time can be of about 3 hours to about 24 hours. This step can be made by adding a solution of HCl, for example at a concentration of 6M. Other acids can also be used. From the previous step, for example 90 to 100% aluminum hydroxide can be precipitated.
Alternatively, aluminum ions can be precipitated by addition of an acidic gas. For example, an hydrated form of Al(OH)3 sprayed by CO2, at a pH of about 7 to about 10.5, the temperature can be of 50° C. to 80° C., and the reaction time can be of about 3 hours to about 24 hours. From the previous step, for example 90 to 100% aluminum hydroxide can be precipitated.
Another way of precipitating aluminum ions can be carried out by addition of a flocculating agent. Various flocculating agents can help to the formation of voluminous flakes which settles by sedimentation. For example, an acrylamide polymer can be used, at a concentration of about 0.1% to about 0.3%. The ratio flocculating agent/solution of hydroxide aluminum can be about 1:300 (volume/volume). The temperature can be below 30° C. and the reaction time can be of about 5 minutes to about 20 minutes. Under such conditions, more than about 97% of the aluminum can be precipitated.
The argillite was ground up in the wet phase in a ball grinder. The mixture of water and roughly crushed argillite coming from the mine was fed into the grinder, where the mineral is reduced to less than 100 microns. The mud went down by gravity into a mixer outfitted with two impellers, which ensures a good homogeneity. When the mixture reaches the desired density, the contents of the mixer are pumped to an accumulation bunker, which will serve to feed the mud to an autoclave.
The acid fed to the leaching came from two sources. The major portion was recycled spent acid. This recycled acid contained about 20 to about 22 wt. % of hydrochloric acid (HCl) and about 10 to about 11% of AlCl3. For example, if excess acid is required, a small quantity of fresh 36% acid can be used.
The mud of argillite and acid were fed to the autoclave of 32 m3 in stoichiometric proportion. The autoclave was then hermetically sealed, mixed well and heated by indirect contact with the steam-fed jacket. As the temperature was rising, the steam pressure increased such that the reaction reached a temperature of about 175° C. and a pressure of about 7.5 barg. At the end of the leaching cycle, the metals contained in the argillite were converted into chlorides. The mixture was then cooled by indirect contact with the cooling water in the reactor jacket. When the mixture was at about 70 to about 80° C., the leached mud was transferred by air pressure to two buffer reservoirs maintained in communicating vessels for further treatment and disposal and the leachate was thus ready for further treatments.
The mother liquor from leaching (leachate) was pumped at constant rate across cartridge filters to the first iron precipitation reactor. This reservoir was well mixed and the temperature was controlled to about 65 to 70° C. by means of a heating coil. The pH was continuously metered and the solution was maintained at a pH of about 12 by addition of 50 wt % caustic soda with the help of a dispensing pump (see
The purpose of the gravity decanter was to produce a thickened mud of the largest crystals of hematite. These crystals served for the seeding in the first precipitation reactor. It was observed that such a technique was useful to promote the creation of precipitates (hematite) that are larger and more easy to filter. A quantity of about 1.5 to about 5.5 g of hematite per liter of the solution was used for seeding. The concentration of Fe in the solution was about 2.5 to about 3.0 g/L.
The filtration of the hematite was carried out with the help of two automated filter presses. The mother liquor was then sent to a buffer reservoir to be pumped to the aluminum precipitation reactor.
The washed hematite was sent to a blade mixer where the pH of the solid is metered. A pH less than about 8 was maintained by the addition of hydrochloric acid (HCl) with the help of a dispensing pump.
For the precipitation of the aluminum, the pH of the mother liquor was adjusted to about 9.5 by reacting it with HCl. Since the mother liquor has been purified of all other metals, the obtained precipitate was white and with purity of at least 98.5%.
The mother liquor was pumped at constant rate across guard filters to the first main reactor for precipitation of aluminum hydroxide. This reservoir was maintained in suspension by an impeller and the temperature was controlled at 65° C. with the help of a heating coil. The pH was metered continuously and the solution was maintained at pH of about 9.5 by addition of HCl using a dispensing pump. The precipitation reaction was effective for converting the aluminum chloride into aluminum hydroxide, which resulted in a gradual precipitation and agglomeration of solid crystals. The liquor was then sent consecutively to two other precipitation reactors where the pH was also controlled by the adding of acid and the temperature maintained by a coil. At the exit from the last reactor, the liquor is fed to a gravity decanter.
A gravity decanter was also used to produce a thickened Al(OH)3 mud of the largest crystals. These crystals were pumped from the bottom of the decanter to the first precipitation reactor to seed the crystallization.
The rest of the Al(OH)3 mud and the supernatant fluid of the decanter were sent to a repulping tank from which the mixture was pumped to a centrifuge type separator/washer. After the treatment with the separator, the Al(OH)3 was then dried.
The Applicant hereby submits that the person skilled in the art would clearly understand that the various embodiments presented in paragraphs [013] to [00124], when applicable, can be combined in all possible manners and be applied to the methods recited in paragraphs [005] to [012]. The embodiments of paragraphs [013] to [00124] of the present disclosure are presented in such a manner in the present disclosure so as to demonstrate that every combinations of embodiments, when applicable can be made. These embodiments have thus been presented in a manner equivalent to making dependent claims for all the embodiments that depend upon any of the preceding claims (covering the previously presented embodiments), thereby demonstrating that they can be combined together.
It was found that the methods of the present application allowed for efficiently separate aluminum ions from iron ions. For example, it was observed that such a drastic pH change for the composition (for example acidic composition) allows for causing precipitation of iron ions by substantially preventing precipitation of aluminum ions. In fact, when for example, adding the acidic composition into a reactor containing the basic composition while simultaneously adding some more base to the basic composition, it was observed that a rapid precipitations of the iron ions occurred without however generating a substantial precipitation of the aluminum ions. In fact, this allows for substantially preventing precipitation of the aluminum ions.
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.
The present application claims priority on U.S. 61/508,950 filed on Jul. 18, 2011, that is hereby incorporated by reference in its entirety.
| Filing Document | Filing Date | Country | Kind | 371c Date |
|---|---|---|---|---|
| PCT/CA2012/000687 | 7/18/2012 | WO | 00 | 4/4/2014 |
| Number | Date | Country | |
|---|---|---|---|
| 61508950 | Jul 2011 | US |
