Solvent extraction method and system
The use of discontinuous packing medium in solvent extraction columns for parallel flow addresses inefficiencies in conventional methods, enhancing extraction efficiency and reducing operational costs and time by minimizing emulsion formation and energy use.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-02-23
- Publication Date
- 2026-04-08
Smart Images

Figure 2026510559000001_ABST
Abstract
Description
Technical Field
[0001] Cross - reference to Related Applications This application claims the benefit and priority of U.S. Provisional Application No. 63 / 448,060, filed on February 24, 2023, having the title "SOLVENT EXTRACTION METHOD AND SYSTEM". The content of the above patent application is hereby incorporated by reference into the detailed description of this specification.
[0002] This specification relates to a method for solvent extraction of one or more target species in a first solvent phase into a second solvent phase. Additionally, this specification relates to a system for performing a method for solvent extraction.
Background Art
[0003] Solvent Extraction Solvent extraction ("SX") (100) is a well - established chemical process that involves a liquid - liquid separation process used for the extraction of one or more ions in an initial solution by contacting it with a second solution. By repeating this process multiple times, it is possible to separate even similar elements from each other.
[0004] The feed solution (102) is the first aqueous solution to be subjected to the SX process. In the case of SX for metal extraction, this can be produced by dissolving a solid containing one or more target metals (typically not a chemical concentrate resulting from an upstream process, but usually) in an acidic solution such as hydrochloric acid ("HCl"). The feed solution (102) can also be an existing solution such as a lithium ("Li") brine that already contains the target metal.
[0005] Conventional SX processes for metal extraction typically involve contacting a feed solution (102) with an organic solution ("organic matter" or "organic phase") consisting of an aliphatic diluent (such as kerosene) in which one or more specific extractants ("extractants") are dissolved. The extractants are typically complex organic compounds selected by their ability to selectively bind to the target metal in the solution. Numerous extractants are commercially available for SX.
[0006] The SX (100) operation can be described as a chemical circuit consisting of numerous unit operations. Figure 1 shows a block diagram of a typical SX circuit (100) used for metal separation. Five typical unit operations are as follows: Extraction (104): The target metal ions are transferred from the supply solution (102) to the organic phase (106), leaving the depleted raffinate (108). Scrub (110): Using an aqueous solution (such as HCl), impurities (i.e., non-target metal ions) are removed from the organic phase, and this is called the scrub solution (112), which is typically returned to the extraction (104) and recycled. Strip (114): The target metal ions are transferred from the organic phase to a fresh aqueous solution (such as HCl) to generate a rich strip (116) while the organic phase is being regenerated. Washing (118): The organic phase is washed or cleaned to remove any residual target and non-target ions, and the resulting washing solution (120) is typically returned to the strip and recycled (this step also helps to raise the pH, thereby reducing the amount of sodium hydroxide (NaOH) required in the following pre-neutralization step), and Pre-neutralization (122): Also called pre-filling or saponification, this is an optional unit operation used with a specific feed solution in which a metal such as sodium ("Na") is added to the organic phase through the addition of a solution such as sodium hydroxide ("NaOH"), and subsequently exchanged for a target metal ion in extraction (104).
[0007] The organic phase (106) is systematically moved from one unit operation to the next, and once the subsequent unit operation is complete, it is returned to the extraction (104) and recycled.
[0008] Subsequently, the raffinate (108) and rich strip (116) produced from the SX circuit (100) may, where appropriate, be used as feed solutions for additional separation in subsequent SX circuits, etc., until a final raffinate and rich strip solution is produced containing primarily only the desired target metal ions at an acceptable purity level (typically 99-99.9%), which is then processed using standard unit operations such as precipitation and calcination to produce solid compounds containing the separated metals.
[0009] Any given SX unit (100) operation contains an aqueous solution, also referred to as the aqueous substance or aqueous phase. The objective in extraction (104) and pre-neutralization (122) is to transfer metal ions from the aqueous substance to the organic substance. The objective in scrubbing (110), stripping (114), and washing (118) unit operations is to transfer metal ions from the organic substance to the aqueous substance.
[0010] The contact process used to facilitate this movement or diffusion of metal ions between the aqueous and organic phases is conventionally achieved by actively mixing the two solutions together in a tank ("mixer") and then allowing them to coagulate or settle in a second tank ("setra"). The mixing station uses a rotary agitator to induce contact between the aqueous phase, which may contain the target element (along with other elements), and the lighter organic phase. The two phases are nominally horizontal, and the mixer aims to increase the surface area of the two solutions in contact with each other. This mixing action may create a considerable amount of microbeads from the two phases, which are then sent to the setra, where the setra separates as much as it can. Since the two solutions are immiscible, they separate, with the organic matter floating on top of the aqueous matter (similar to how oil and water naturally separate after being mixed together).
[0011] The equipment conventionally used in this process is called a mixer-setter contactor. Each unit operation utilizes one or more mixer-setter contactors to achieve the objective of a particular unit operation. Each mixer-setter contactor is referred to as a stage (199) within a given unit operation.
[0012] Some mixer-settra contactors have a bleeding option that returns a portion of the respective output aqueous and organic phases to their respective input streams via a recycle valve, as a means of increasing the relative concentration of ions that have moved from one phase to the other during mixing.
[0013] In addition to the above, there are several column-based approaches to solvent extraction that do not use the mixer-cetera contactor described above. These generally fall into two broad categories.
[0014] The first is a non-agitated column extractor that does not have moving internal parts. Examples include spray columns, packed columns, and sieve-tray columns. In each case, the phases are in contact with each other in a counterflow manner. The second is an agitated column extractor, which is similar to a non-agitated extractor but has mechanical assistance to agitate the phases as they pass through the column. Examples include, A pulsed column uses a pump to create pressure waves (typically air) in a phase as it moves through the column. Baffles may be included along the length of the column to facilitate the mixing and dispersion of one phase into another. An example is the Tenova pulsed column. ● Also known as a sieve-tray column, a perforated plate column is a column in which the dispersed phase aggregates in a plate inserted along the length of the column and then moves through perforations. Sometimes, perforated plate columns are combined with the aforementioned pulse mechanism, as well as A rotary agitated column containing a rotating internal mechanism that agitates the phase as it flows through the column with a rotating disk. Typically, it has different mixing and sedimentation zones within the column. The mixing zone typically has a turbine impeller operating between baffles. Examples include Scheibel columns and Oldshue-Rushton columns.
[0015] In each type of agitated column, aqueous substances enter the upper column and organic substances enter from the bottom, creating a countercurrent within the column.
[0016] chemical similarity For a given extractant, each metal typically has a specific profile of effectiveness in binding to or releasing from the extractant as the pH or acidity level changes. A perfect extractant under specific operating conditions is one that binds only to (or releases from) the target metal, while not interacting with other metal ions present.
[0017] In practice, metals from the same group within the periodic table have similar chemical properties, so their profiles often overlap, reducing selectivity.
[0018] As a result, each SX unit operation (100) often requires multiple stages (199) to ultimately achieve acceptable purity levels of the raffinate (108) and rich strip (116) solutions (the two main working products from any SX circuit). One of the most extreme examples of this is the separation of rare earth elements ("REE") from one another, where, within a given conventional SX circuit (100), dozens of stages (199) may be required for each unit operation.
[0019] The distribution coefficient K is a measure of how well a metal can be extracted from an aqueous solution into an organic solution. K affects the process yield and depends on the extractant used, diffusion rate, contact time, and other process parameters. For a given metal, A:
number
[0020] The separation factor S is a measure of the selectivity of extraction. S affects the purity of the resulting solution - essentially, what is extracted and what is not extracted. For a given metal, A and B: [Number]
[0021] A lower separation factor leads to a greater number of stages (199) being required for effective separation in a given unit operation, and in order to achieve the desired yield and purity, the same process must be repeated within the given unit operation using additional stages (199). The specific number and distribution of stages (199) within various unit operations are known as staging.
[0022] Figure 2 shows a representative block diagram of the extraction staging (200) of a conventional SX circuit (100) used to separate REEs in a mixer - settler contactor.
[0023] The two solutions in any given unit operation flow counter - currently to each other. In the example of Figure 2, there are 10 stages (199) (EX1 to EX10), and the organic flows into stage EX1 (2)01), and after completion of mixing and settling, then flows out of EX1 (201) and into EX2 (202), and from there into EX3 (203), etc., while the feed solution and scrub solution flow in the other direction from EX10 (210) to EX9 (209), EX8 (208), etc.
[0024] In the art, there remains a need to improve solvent extraction processes or to provide alternative solvent extraction processes. In particular, there is a need in the art for alternative methods for solvent extraction that can avoid the formation of significant microbeads of the two phases when mixed. In addition, there is a need in the art for processes that can provide high surface area contact (and mass transfer) between phases without requiring vigorous mixing. Furthermore, there is a need in the art for processes that can improve the transport rate of desired elements between two phases (aqueous and organic). Furthermore, there is a need in the art for processes that can address one or more of the following: reducing the operational footprint, reducing inventory in the process such as the volume of organic solvents in the process, enabling faster restart of processing equipment, reducing energy consumption in the process, improving the separation of desired elements, and reducing the volatilization of organic matter into the atmosphere. [Overview of the project]
[0025] In one embodiment, this specification provides a method for separating one or more target species from a first solvent phase, wherein the method is A step of passing a first solvent phase containing one or more target species and a first portion of a second solvent phase through a first set of one or more columns containing a discontinuous packing medium, wherein the first solvent phase and the second solvent phase are immiscible with each other and the flows of the first solvent phase and the second solvent phase are parallel. The present invention relates to a method comprising enabling a first solvent phase and a second solvent phase to come into contact with each other, thereby enabling the extraction of one or more target species from the first solvent phase to the second solvent phase.
[0026] In another embodiment, this specification provides a system for extracting one or more target species from a first solvent phase to a second solvent phase, wherein the system is It comprises a first set of one or more columns containing a discontinuous packing medium, The system relates to a system configured for the parallel flow of a first solvent phase and a second solvent phase, enabling contact between the first solvent phase and the second solvent phase as the solvent flows through a discontinuously packed medium.
[0027] In a third aspect, this specification describes a process for purifying one or more target species, wherein the process is It includes a scrubbing step and an extraction step that is in fluid communication with the scrubbing step, and a stripping step that is in fluid communication with the scrubbing step, The process relates to a method disclosed herein, wherein at least one of the extraction step, scrubbing step, and stripping step includes the method disclosed herein.
[0028] In a fourth aspect, this specification relates to a system for the purification of one or more target species, wherein the system is It includes an extraction stage that is in fluid communication with a scrubbing stage, and a stripping stage that is in fluid communication with a scrubbing stage, The present invention relates to a system in which at least one of an extraction stage, a scrubbing stage, and a stripping stage comprises the system disclosed herein. [Brief explanation of the drawing]
[0029] Here, as an example, we refer to the accompanying drawings illustrating exemplary embodiments of this application.
[0030] [Figure 1] This is a block diagram showing typical unit operation and fluid flow in a conventional SX circuit (100). [Figure 2] This block diagram shows the staging (200) of the extraction unit operation in a typical conventional SX circuit (100) for REE separation using a mixer-settra contactor. [Figure 3]This is a schematic diagram showing a RapidSX® contactor (1) according to one embodiment of the foregoing, showing an inflow manifold (single-port or multi-port depending on the column diameter) for receiving and then distributing input solutions, a single column filled with discontinuous media receiving the solutions, and a setter. [Figure 4] A) a side view and B) a front view of a RapidSX® contactor according to another embodiment disclosed herein, showing an inlet manifold for receiving and subsequently distributing input solutions, four columns filled with discontinuous media receiving the solutions, and a shared setter. [Figure 5] This schematic diagram shows a RapidSX™ contactor according to another embodiment disclosed herein, illustrating an inlet manifold for receiving and subsequently distributing input solutions, a single column filled with discontinuous media that has received the solutions, a setter, and a recycle valve for enabling large-volume bleeding of each output solution back into each input solution entering the top of the stage. [Figure 6] A) a side view and B) a front view of a RapidSX® contactor according to another embodiment disclosed herein, showing an inlet manifold for receiving and subsequently distributing input solutions, four columns filled with discontinuous media that have received the solutions, a shared setter, and a recycle valve for enabling large-volume bleeding of each output solution back into each input solution entering the top of the stage. [Figure 7] This block diagram shows the staging of extraction, scrubbing, stripping, washing, and pre-neutralization unit operations in an SX circuit for REE separation using a RapidSX® contactor, as described in Example 1 below.
[0031] In each of Figures 2-7, solid arrows indicate the flow of the aqueous phase, and dotted arrows indicate the flow of the organic phase.
[0032] Similar reference numbers may be used in different drawings to indicate similar components. [Modes for carrying out the invention]
[0033] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as those generally understood by those skilled in the art to which this disclosure belongs. In addition, any methods and materials similar to or equivalent to those described herein may be used in practice for testing the present invention, but typical materials and methods are described herein. It should also be understood that the terms used herein are for the purpose of describing specific embodiments only and are not intended to limit them. Any patent applications, patents, and publications referenced herein are provided for the purpose of understanding the embodiments described herein. Each of these references is incorporated herein by reference in whole.
[0034] When introducing elements of the disclosure in this specification, the articles “a,” “an,” “the,” and “said” are intended to mean that one or more of the elements may exist.
[0035] Where used herein, the term “comprising” and its derivatives are intended to be open-ended terms specifying the presence of the described features, elements, components, groups, integers, and / or steps, but not excluding the presence of other undescribed features, elements, components, groups, integers, and / or steps. The foregoing also applies to similarly meaning words such as the terms “including,” “having,” and their derivatives. Any embodiment described as “comprising” certain components may also “consist of” or “essentially consist of” those components, and it will be understood that “consist of” has a closed-ended or restrictive meaning, while “essentially consist of” includes the specified components but excludes other components, except for materials present as impurities, unavoidable materials present as a result of processes used to provide the components, and components added for purposes other than achieving the technical effects described herein.
[0036] It will be understood that any component defined herein as being included may be expressly excluded from the claimed invention by any proviso or negative limitation, whether implicitly or expressly defined herein, such as any particular compound or method step.
[0037] In addition, all ranges provided herein include the endpoint of the range, and any intermediate range points, whether or not they are explicitly stated otherwise.
[0038] Finally, as used herein, terms of degree such as “substantially,” “about,” and “approximately” mean a reasonable deviation of the modified term so that the final result does not change significantly. These terms of degree should be interpreted as including a deviation of at least ±5% of the modified term, provided that this deviation does not negate the meaning of the word it modifies.
[0039] The abbreviation "e.g." originates from the Latin "exempli gratia" and is used herein to indicate non-restrictive examples. Therefore, the abbreviation "e.g." is synonymous with the term "for example." The word "or" is intended to include "and" unless otherwise explicitly stated in the context.
[0040] The phrase "at least one of" is understood to mean one or more. The phrase "at least one of...and..." is understood to mean at least one of the listed elements, or any combination thereof, unless explicitly listed. For example, "at least one of A, B, and C" is understood to mean A alone, or B alone, or C alone, or a combination of A and B, or a combination of A and C, or a combination of B and C, or a combination of A, B, and C.
[0041] As described above, in one embodiment, this specification relates to a method for separating one or more target species from a first solvent phase, the method comprising the steps of passing a first solvent phase containing one or more target species and a first portion of a second solvent phase through a first set of one or more columns containing a discontinuous packing medium, wherein the first solvent phase and the second solvent phase are immiscible with respect to each other, the flows of the first solvent phase and the second solvent phase are parallel, and the first solvent phase and the second solvent phase are allowed to come into contact with each other, thereby enabling the extraction of one or more target species from the first solvent phase to the second solvent phase.
[0042] In another embodiment, this specification relates to a system for extracting one or more target species from a first solvent phase to a second solvent phase, the system comprising a first set of one or more columns containing a discontinuous packing medium, the system configured for parallel flow of the first and second solvent phases, and enabling contact between the first and second solvent phases as the solvent flows through the discontinuous packing medium.
[0043] In a third aspect, this specification relates to a process for purifying one or more target species, the process comprising an extraction step having fluid communication with a scrubbing step, and a stripping step having fluid communication with the scrubbing step, wherein at least one of the extraction step, the scrubbing step, and the stripping step comprises a method disclosed herein.
[0044] In a fourth aspect, this specification relates to a system for purifying one or more target species, the system comprising an extraction stage having fluid communication with a scrubbing stage, and a stripping stage having fluid communication with the scrubbing stage, wherein at least one of the extraction stage, the scrubbing stage, and the stripping stage comprises the system disclosed herein.
[0045] As used herein, the term “separation” is not particularly limited and should be understood by those skilled in the art. In the context herein, separation may include the separation of one or more target species from other species present in a medium. For example, separation may include the removal of a target species, which may be, for example, one or more metals of interest, from a first phase to a second phase in order to help separate the target species from other impurities present in the first phase. In this scheme, performing separation can result in an improvement in the purity of one or more target species by the removal of other species. Separation is performed using liquid-liquid extraction according to this specification.
[0046] The term “target species” is not particularly limited and should be understood by those skilled in the art. This term may include any compound, element, complex, or ion that is desirable to be separated from the resulting solution. While this specification has particular utility for the separation of metals from aqueous solutions, it can be applied, as assumed, to any situation in which solvent extraction (SX) is currently used as a separation method.
[0047] As used herein, the term “solvent” is not particularly limited and should be understood by those skilled in the art. A solvent is a substance that contains or dissolves a solute. According to this specification, separation can be performed using two different solvents comprising a first solvent phase and a second solvent phase. The two solvent phases to be selected are immiscible with each other as disclosed herein and are not particularly limited and can be determined by those skilled in the art. In addition, the two solvents can be selected based on design and application requirements. Furthermore, the terms “first solvent phase” and “second solvent phase” are not particularly limited and should be understood by those skilled in the art. The first and second solvent phases may vary depending on the unit operation being performed. In one embodiment, for example, if the unit operation is a stage of the extraction step, the first solvent phase may be an aqueous phase containing one or more target species and the second solvent phase may be an organic phase. In a second embodiment, for example, if the unit operation is a stage of the strip step, the first solvent phase may be an organic phase containing one or more target species and the second solvent phase may be an aqueous phase. Although this specification primarily describes the present invention by reference to the extraction step, it should be noted that the present invention can similarly be carried out in other unit operations, as will be understood by those skilled in the art.
[0048] The step of passing a first solvent phase containing one or more target species and a first portion of a second solvent phase through a first set of one or more columns (4) is not particularly limited and should be understood by those skilled in the art. This step may include a fluid flow of the first solvent phase and the first portion of the second solvent phase through one or more columns (4). Such a fluid flow can be achieved by steps such as pumping, injecting, or spraying the solvent into the hollow columns (4) containing the medium. In addition, a fluid flow into the columns can be achieved by providing a manifold (2).
[0049] The terms “column” or “one or more columns” used to perform SX are not particularly limited and should be understood by those skilled in the art. In one embodiment, for example, but not limited, column (4) is a contactor column. A contactor column is a container in which liquids or gases have a large contact area with each other. The number of columns used is not particularly limited and may vary based on design and application requirements. In one embodiment, for example, but not limited, a process and / or system (1) utilizes two, three, four, five, six, seven, eight, nine, or ten columns. The number of columns described refers to the number of columns in each stage of a unit operation, where different stages have the same or different number of columns. The use of multiple columns potentially makes such a system (1) much easier to set up and more efficient to operate. The contactor column (also referred to herein as the “RapidSX® contactor” or “RapidSX® extractor”) contains a randomly packed discontinuous medium (12), i.e., composed of discrete beads or particles, as opposed to fibers, foams, or porous packing running along the length of the column. The discontinuous medium (12) in the RapidSX® extractor may typically have a higher packing density than in a simple packed column.
[0050] As described herein, in one embodiment, for example, but not limited to, a solvent is introduced to one end of a column through an orifice. The orifice is used to help mix the aqueous fluid and the organic fluid before they enter the packed bed. Its purpose is to help achieve a complete and homogeneous mixture of the solvents, in other words, to increase the Reynolds number, create turbulence in the fluids, and mix them. The size of the orifice selected depends on the volumetric flow rate of the fluid. Lower flows require smaller orifices to help increase the Reynolds number sufficiently to produce a proper mix. As the flow rate increases, the orifice can be increased to avoid having excessive flow limitations that may require larger pumps, higher pressures, and more energy to overcome. It should be noted that the orifice is not required for the function of the present invention, and other mixing means, such as static mixers, can also be used, for example, but not limited to. Static mixers and orifice mixing are easily modifiable and offer better flexibility than static mixers, so these were tried during testing and the orifice was selected.
[0051] In addition, it should be noted that a mixing head is not necessarily required for the technology to function. Unmixed fluid entering the packed bed will mix and remain mixed within the packed bed, provided a sufficient fluid velocity is achieved. In one embodiment, for example, but not limited to, the fluid entering the packed bed has a fluid velocity of approximately 17.8 mm / second or higher. For example, in a 2-inch diameter contactor column without a mixing head, homogeneous mixing has been observed after approximately 400 mm of packed bed. Larger diameter contactor columns with a central entry point may require a longer distance to achieve homogeneous mixing. In further embodiments, for example, but not limited to, the fluid velocity within the packed bed is maintained at approximately 17.8 mm / second or higher to help avoid and minimize fluid separation within the contactor.
[0052] Returning to embodiments utilizing orifices, in one embodiment, for example, the orifice has a specific diameter. In the first embodiment, for example, the orifice has a diameter of 0.2 mm. In the second embodiment, for example, the orifice has a diameter of 0.5 mm. In the third embodiment, for example, the orifice has a diameter of 1 mm. In the fourth embodiment, for example, the orifice has a diameter of 2 mm. In the fifth embodiment, for example, the orifice has a diameter of 3 mm. In the sixth embodiment, for example, the orifice has a diameter of 5 mm. In the seventh embodiment, for example, the orifice has a diameter of 9 mm. There is one orifice for each solvent phase entering the column. Each orifice may have the same diameter. Alternatively, the orifices may be of different sizes. In one embodiment, for example, the orifices are positioned perpendicular to each other to allow contact before the solvent phase continues to pass through the column. In a second embodiment, for example, but not limited to, the orifices are arranged in a face-to-face relationship to allow contact before the solvent phase continues to pass through the column.
[0053] As described herein, in one embodiment, for example, but not limited to, the column contains a randomly packed discontinuous medium that allows a first solvent phase and a second solvent phase to come into contact as the solvent phase flows through the column. Terms such as “randomly packed” and “randomly packed” should be known or understood by those skilled in the art, and are not particularly limited. Random packing can use a random distribution of small packing material to aid in a separation process, helping to increase the surface area for the solvent phases to come into contact with each other, thereby enabling mass transfer and extraction to occur. In contrast, structured packing uses a larger, fixed packing structure used to guide a liquid material into a specific shape. Structured packing may use, for example, a disk or plate that can be attached to a column and may be made of a material such as metal, plastic, or porcelain having an internal structure arranged into different types of shapes, such as a honeycomb, to guide the fluid flow in a specific controlled manner.
[0054] The terms “discontinuous medium” or “discontinuous packed medium” as used herein are not particularly limited and should be known to or understood by those skilled in the art. The discontinuous medium disclosed herein relates to small diameter particles that create small gaps or spaces between particles, allowing the flow of the solvent phase. This creates void spaces (related to porosity) that allow the fluid to flow. In addition, the degree of packing of the discontinuous medium leads to the packing density of the packed medium. In one embodiment, for example, but not limited, a column contains randomly packed discontinuous packed medium. In another embodiment, for example, but not limited, a discontinuous packed medium can be achieved by additive manufacturing of a column and filling the inside of the column, such as by 3D printing of a column and packed medium having similar void spaces as a randomly packed discontinuous packed medium, for example, but not limited. The discontinuous packed medium as used herein creates void spaces, providing spaces to interact with the solvent phase as described herein, and enabling the separation of target species.
[0055] As disclosed herein, randomly packed discontinuous media have a porosity due to gaps or spaces between particles. The porosity provides information about the void space in the column bed and relates to the ratio of the volume of voids in the bed to the total volume of the bed (voids plus solids). In the first embodiment, for example, a randomly packed discontinuous medium has a porosity of 0.30 to 0.44, for example. In the second embodiment, for example, a randomly packed discontinuous medium has a porosity of 0.33 to 0.41, for example. In the third embodiment, for example, a randomly packed discontinuous medium has a porosity of 0.36 to 0.38, for example.
[0056] As disclosed herein, a randomly packed discontinuous medium may have a packing density. The term “packing density” is not particularly limited and should be known or understood by those skilled in the art. The packing density or packing rate of a filler in any space is the ratio of the space filled by the material constituting the filler. In other words, it is the ratio of the volume of the object in the space to the volume of the space itself. It should also be noted that packing density correlates with particle density, and very heavy particles result in a higher packing density. In the first embodiment, for example, a randomly packed discontinuous medium may have a packing density of 0.48–0.63 g / cm³. 3 It has a packing density of 0.52 to 0.60 g / cm³. In the second embodiment, for example, but not limited to, a randomly packed discontinuous medium has a packing density of 0.52 to 0.60 g / cm³. 3 It has a packing density of 0.55 to 0.57 g / cm³. In a third embodiment, for example, but not limited to, a randomly packed discontinuous medium has a packing density of 0.55 to 0.57 g / cm³. 3 It has a packing density of .
[0057] The use of a discontinuous packing medium (12) containing small-diameter particles in the contactor column helps to provide close contact across a large interface region between the first fluid (or solvent) phase and the second fluid (or solvent) phase flowing in parallel through the medium, thereby achieving highly efficient transfer of the target species from the first fluid (solvent) phase to the second fluid (solvent) phase without the need for mechanical stirring. This method helps to maximize extraction efficiency while maintaining the dispersion of the easily separable first and second fluid (solvent) phases. In Figure 3, the discontinuous medium (12) is shown as a gray-colored section in column (4); however, for the sake of discussion, similar discontinuous medium (12) is not shown in all columns in Figures 4–6 (but is present).
[0058] The step of enabling the first solvent phase and the second solvent phase to come into contact with each other is not particularly limited. In one embodiment, the first fluid (solvent) phase and the second fluid (solvent) phase are guided to flow in parallel through the contactor column. In other words, the first solvent phase and the second solvent phase flow in the same direction through the contactor column, rather than flowing in different directions such as opposite directions (countercurrent). None of the fluid phases are arranged to be confined to the packing medium.
[0059] The particles of the packing medium are sized to retain the fluid (solvent) phase in the contactor column (4) for a sufficient time to allow the diffusion of the target species from the first solvent phase to the second solvent phase. If the particle size is too large, the size of the voids between the particles may be too large, and the solvent phase will leave the column without reaching equilibrium in terms of this diffusion. On the other hand, the particle size must not be so small that the fluid flow through the column (4) is obstructed due to capillary or viscosity issues. Therefore, the particle size of the packing medium is selected according to the specific target species and the column dimensions for the specific SX application.
[0060] In one embodiment, for example, but not limited, the particles have a diameter of about 5 mm or less. In another embodiment, for example, but not limited, the particles have a diameter of about 0.5 mm to about 5 mm. In yet another embodiment, for example, but not limited, the particles have a diameter of about 1 mm to about 4 mm. In yet another embodiment, for example, but not limited, the particles have a diameter of about 1.0 mm to about 3.5 mm. In yet another embodiment, for example, but not limited, particles having a diameter in the range of 1.5 to 3 mm are particularly suitable for bringing about effective contact between fluid phases in a parallel flow and achieving highly efficient transfer of target species between them, while helping to reduce or prevent emulsion formation.
[0061] The method disclosed herein affects the juxtaposition of a first and second fluid phase with high interfacial surface area contact, without mixing them or by reducing the amount of mixing, while reducing or preventing emulsion formation. Each fluid phase is in close contact and brought together, but blending or fusing is reduced or avoided, so that there is no significant discontinuous dispersion of one phase into the other phase, and / or a significant portion of one phase is not substantially or completely encapsulated by the other phase. The constituent phases may generally remain separate and may be easily separable. While we do not wish to be bound by any particular theory, as described above, each droplet of the two phases is considered to interact with each other as it drips down the column, but not emulsified. This allows for the extraction of one or more target species from the first solvent phase to the second solvent phase.
[0062] In one embodiment, for example, but not limited to, the particles are substantially spherical or oval-shaped beads. In one embodiment, for example, but not limited to, the particles are polymer beads, for example, polypropylene beads. Polymer beads are relatively lightweight compared to, for example, ceramic beads or metal beads, which offers advantages in terms of mechanics, handling, and logistics. Polypropylene is hydrophobic and therefore repels water and aqueous solutions and attracts oil and organic solutions. In one embodiment, for example, but not limited to, the particles are glass beads. Glass is hydrophilic and therefore attracts water and aqueous solutions and repels oil and organic solutions. The selection of material for the particles in the column can change the function of the column packing and help improve solvent extraction efficiency. In further embodiments, multiple materials are selected for use as particles in the column, and the multiple materials can be divided into zones based on their physical-chemical properties. Therefore, in one embodiment, for example, but not limited to, the contactor column (4) has a first zone (30) containing a first discontinuous medium and a second zone (32) containing a second discontinuous medium, wherein the first discontinuous medium contains hydrophobic particles and the second discontinuous medium contains hydrophilic particles (Figure 6). If multiple zones exist, the first zone (30) and the second zone (32) may be located in a single contactor column (4), or if the stage operation involves multiple columns (4) (as shown in Figure 6), the first zone (30) and the second zone (32) may be located in separate contactor columns (4).
[0063] In one embodiment, as shown in Figures 4 and 6, the two phases enter the stage at the top of each column (4) and thus flow in a parallel manner from top to bottom inside each column (4). In each column (4) of a stage utilizing two or more columns (4), this parallel flow occurs simultaneously and in parallel within each column (4). The same SX unit operation is utilized without changing the aqueous or organic phase used. The entry of the solvent phase into one or more columns (4) can be carried out using a manifold (2), which is attached to one or more columns (4) in fluid communication with the columns (4) and allows the flow of the first solvent phase and / or the second solvent phase to enter one or more columns (4).
[0064] The use of parallel flow of liquids differs from most other column-based methods. Parallel flow is possible because the beads in the column provide a higher flow rate and surface area for contact between two immiscible liquid phases. This allows the first and second solvent phases to come into contact with each other, enabling the extraction of one or more target species from the first solvent phase to the second. Furthermore, the beads do not act on capillary action, which helps ensure that phase flow can be maximized. Since capillary action results in slow fluid flow, this approach can be problematic in applications utilizing fiber-based contactors. Countercurrent flow does not improve this type of mixing and is likely to require assistance from mechanical agitation. In addition, the use of parallel flow can help improve the rate and degree of subsequent separation of the two phases after mixing. Overmixing can result in very long sedimentation times, which can negatively impact the overall throughput of the plant; therefore, phase mixing and demixing can be optimized to reduce sedimentation time. Such advantages can be achieved through the use of beads in column (4). The two (parallel flow and beads) work simultaneously to help provide maximum throughput while also maximizing transport.
[0065] In addition, using beads in contrast to larger saddles or other filling shapes means that there is more physical mobility on the wetted surface of the beads, and therefore, the transport of mass between the wetted and unwetted phases is improved.
[0066] The presence of beads in column (4) causes the phases to droop and interact with each other on the surface of the beads and in the spaces between them. This approach can help increase the specific surface area of the interface between the two phases during contact in each RapidSX™ contactor compared to the specific surface area of the same interface using a conventional mixer in a mixer-cetera contactor. This increased specific surface area can increase the overall rate of mass transfer between the two phases (such as the diffusion of metal ions).
[0067] Simultaneously, phase contact occurs without agitation and without a significant discontinuous dispersion of one phase into the other. This results in a significant reduction in the time required for the two phases to settle or aggregate after contact, and a significant reduction in entrainment (the aforementioned permanent and troublesome dispersion of droplets from one phase into the interior of the other phase).
[0068] The combination of improvements disclosed herein can result in a significant reduction in the overall time it takes to complete the process in each RapidSX® contactor compared to a mixer-settra contactor.
[0069] To further clarify the embodiments disclosed herein, with reference hereto to the figures, Figure 3 shows a schematic diagram of a RapidSX® contactor (1) having one column (4) and one setra (6). The aqueous phase, which may be the first solvent phase in the extraction unit operation and is shown by a solid line, enters the manifold (2). Similarly, the organic phase, which may be the second solvent phase in the extraction unit operation and is shown by a dashed line, enters the manifold (2). The configuration of the manifold (2) is not particularly limited and may vary depending on the design and application requirements. For example, the first and second solvent phases may be mixed before entering the column (4), although this is not limited. Alternatively, the first and second solvent phases may be kept separate in the manifold (2), and mixing of the first and second solvent phases occurs when entering the column (4).
[0070] Next, the first and second solvent phases enter the upper end (14) of the upright column (4), exit the manifold (2), and flow downward through the column while passing through the discontinuous packing medium (12). The vertical positioning of the column (4) allows for gravity flow of the first and second solvent phases from the upper end (14) to the lower end (16) of the column (4). As the solvent phases pass from the upper end (14) to the lower end (16) of the column (4), they flow into the space between the discontinuous packing medium (12), resulting in phase-phase contact and extraction of one or more target species from the first solvent phase to the second solvent phase. The embodiment in the figure relates to an upright column positioned vertically from the ground, but it should be noted that other positions are possible and are included herein, such as when the column is positioned horizontally. In such embodiments, the first and second solvent phases then enter the column from the first end and exit from the second end.
[0071] As the solvent phase exits the discontinuous packing medium (12), it flows into the setra (6), where separation of the first solvent phase and the second solvent phase can occur. In one embodiment, as shown in Figure 3, the column (4) is attached to the setra (6) via a joint (18) that allows fluid communication between the column (4) and the setra (6). The first and second solvent phases flow from the column (4) to the setra (6) through the joint (18). Upon entering the setra (6), the first and second solvent phases are separated. After separation, one of the solvent phases can be removed from the first end (20) of the setra (6), and the other solvent phase can be removed from the second end (22) of the setra (6). In the embodiment shown in Figure 3, the aqueous phase is the first solvent phase and is heavier than the organic (second solvent) phase, so the aqueous (first solvent) phase can be removed from the first end (20) of the cetra (6) and the organic (second solvent) phase can be removed from the second end (22) of the cetra (6). In one embodiment, for example, but not limited to, the cetra (6) is positioned vertically as shown in Figure 3.
[0072] Figure 4 shows another embodiment of system (1) according to this specification. System (1) shown in Figure 4 operates similarly to system (1) shown in Figure 3, with some differences disclosed herein. In Figure 4, the manifold (2) is fluidly attached to a plurality of columns (4). Thus, the first and second solvent phases flow from the manifold (2) into the plurality of columns (4). In the embodiment shown in Figure 4, there are four columns (4), each containing a discontinuous packing medium (12), and separate portions of the first and second solvent phases flow through the columns (4). In addition, the lower ends (16) of the columns (4) open to a single setter (6). Consequently, the system (1) configuration shown in Figure 4 does not require any joints. Furthermore, since the lower end (16) of column (4) opens to a single setra (6), portions of all of the first and second solvent phases flowing through different columns are combined, and then the first and second solvent phases are separated in the setra (6). In one embodiment, for example, but not limited to, as shown in Figure 4, the setra (6) is provided with a weir system (24) that helps guide the separated first and second solvent phases from the setra (6) to separate outlet ports (not shown) (of the first and second solvent phases) from the setra (6). The weir system used is not particularly limited and should be known to those skilled in the art. The weir system can help separate the first and second solvent phases. In one embodiment, for example, but not limited to, the setra (6) disclosed in Figure 4 is positioned horizontally (compared to the setra (6) shown in Figure 3) and has a length greater than its height. Such a setra (6) can help increase the separation rate between the first solvent phase and the second solvent phase.
[0073] Figure 5 shows a further embodiment of system (1) according to this specification. Figure 5 is similar to system (1) shown in Figure 3, except that system (1) in Figure 5 is provided with a first solvent system recycling valve (10, also described as an aqueous recycling valve) and a second solvent system recycling valve (8, also described as an organic recycling valve). The organic solvent system recycling valve (8) enables the recycling of the organic solvent phase, and the aqueous solvent system recycling valve (10) enables the recycling of the aqueous solvent phase. After the separation of the first and second solvent phases in the cetera (6), the recycling valves (8, 10) can reintroduce the first and second solvent phases to the injection system (26). From the injection system (26), the first and second solvent phases reintroduce into the manifold. Various options are available by using recycling valves (8, 10) that include only one of the solvent phases to be recycled and / or a portion of the solvent phases to be recycled. The recycling valves (8, 10) are also characterized in that they allow the solvent phase to be re-introduced into separate containers for further processing.
[0074] In addition to the above, in one embodiment, for example, as shown in the embodiment shown in Figure 5, the processes and systems disclosed herein are provided with a flocculant (28) located downstream of the discontinuous packing medium (12). In a further embodiment, for example, but not limited to, the flocculant (28) is located at the junction (18) connecting the column (4) to the setra (6). In a further embodiment, for example, but not limited to, the flocculant (28) exists as a cartridge. In another embodiment, for example, but not limited to, the process further includes the step of flocculating a first solvent phase and a second solvent phase.
[0075] The type of coagulator used is not particularly limited and should be known to those skilled in the art. In one embodiment, for example, a mechanical coagulator is used. In another embodiment, for example, the coagulator is an electromechanical coagulator.
[0076] The flocculation step used herein is not particularly limited. In one embodiment, for example, this step may include passing the first and second solvent phases through a further packing medium. The further packing medium may be placed in a cartridge and can help act as a flocculant to reduce phase separation time under certain conditions and thereby improve the efficiency of the solvent extraction process. In one embodiment, for example, the packing medium used to flocce the first and second solvent phases is glass wool. In another embodiment, for example, the glass wool used is made of silicon dioxide (SiO2). In a further embodiment, for example, the glass wool may be amorphous or quartz (crystalline). In yet another embodiment, for example, the glass wool is about 0.07 to about 0.1 g of glass wool / cm³. 3 It is filled with a density within that range.
[0077] As used herein, the term "cartridge" is not particularly limited and should be understood by those skilled in the art. A cartridge may be a section of a mixer-setter containing further packing medium, or it may be provided as a separate housing containing further packing medium. In addition, for example, the further packing medium may be replaced with a fibrous medium to increase the surface area. In addition, for example, the further packing medium or fibrous medium may be a hydrophilic medium. Non-limiting examples of hydrophilic media include glass wool or beads.
[0078] Figure 6 shows a further embodiment of system (1) according to this specification. Figure 6 is similar to system (1) shown in Figure 4, but has the added feature of recycle valves (8, 10) as shown and described in Figure 5. In addition, the embodiment shown in Figure 6(A&B) shows a contactor column (4) containing a first zone (30) containing a first discontinuous medium present in the first contactor column (4) of the stage, and a second zone (32) containing a second discontinuous medium present in the second contactor column (4) of the same stage (in Figure 6, the difference between the first and second discontinuous media is shown based on the shade of gray).
[0079] Figure 7 shows an SX operation comprising several unit operations for performing the solvent extraction described herein. The use of the methods and systems disclosed herein is not particularly limited to the extraction step (EX1, EX2, or EX3), but may also be used in other unit operations (such as scrubbing (SC1, SC2), stripping (ST1, ST2), washing (WA1), or pre-neutralization (PN1)) depending on design and process requirements. In embodiments disclosed herein, the system (100) is described with respect to the extraction step, in which a first solvent phase (aqueous phase) containing one or more target species enters EX3 (for example, but not limited to) together with a portion of a second solvent (organic) phase. After flowing through one or more columns (4), the first solvent phase is guided to a second system (EX2), where the solvent phase is separated in a cetera (6) and mixed with a second portion of the second solvent phase for further extraction. This is continued in a third system (EX1), where the first solvent phase exits as aqueous raffinate. As disclosed herein, different portions of the second solvent (organic) phase may undergo further processing in other unit operations of the solvent extraction operation.
[0080] Furthermore, because the two phases can move through the RapidSX® contactor at a much faster speed than a comparable mixer-setra contactor while maintaining separation performance, the overall working volume of the RapidSX® contactor may be significantly lower than that of a mixer-setra contactor. Due to the faster separation time, the size of the setra portion of the unit can be reduced, thereby reducing the working volume. In addition, compared to conventional SX circuits, less organic matter can be used in the overall circuit, and the physical stock of supply solution bound to the circuit can always be reduced.
[0081] This combination also means that the overall size, physical footprint, and capital costs of the associated SX circuits can be significantly reduced.
[0082] As shown in Figure 7, the organic phase (or pre-neutralized organic phase) (106) enters extraction stage 1 (EX1) via the inlet B01 of the extraction unit operation in the solvent extraction system (100). The flow of the organic phase (106) in Figure 7 is disclosed using dashed arrows, and the flow of the aqueous fluid or feed solution (102) is indicated using solid arrows. After extraction is complete in extraction stage 1 (EX1), the organic phase (106) flows into extraction stage 2 (EX2) via a tube or other connection (B02). Extraction stage 2 (EX2) is connected to extraction stage 3 (EX3) via a connection (B03) that allows the flow of the organic phase (106) from extraction stage 2 (EX2) to extraction stage 3 (EX3).
[0083] In the solvent extraction system (100) disclosed in Figure 7, the feed solution (102) enters the system (100) via the inlet port (A01) of the extraction stage 3 (EX3). To control the pH of the phase, sodium hydroxide (NaOH) may also be added to the extraction stage 3 (EX3) via the inlet port (A16). In binding the extractant to the desired metal or other species, pH control can help improve selectivity. In addition, sodium hydroxide (NaOH) can help neutralize any excess hydrochloric acid (HCl) (which may be present in the extraction stage 3 (EX3)) entering from the scrubbing unit operation described herein.
[0084] From extraction stage 3 (EX3), the feed solution (102) flows into extraction stage 2 (EX2) via a connecting tube or other connection (A02). After flowing through extraction stage 2 (EX2), the aqueous solution (102) flows through a connection (A03) that allows fluid flow from extraction stage EX2 to extraction stage 1 (EX1). After sedimentation in extraction stage 1, the aqueous phase is removed as raffinate (108) via an outlet (A04).
[0085] The solvent extraction system (100) has three extraction stages (EX1, EX2, and EX3) in its extraction unit operation. The organic phase (106) flows from EX1 to EX2 to EX3, and the aqueous phase or feed solution (102) flows from EX3 to EX2 to EX1, while the organic phase (106) flows against the aqueous phase or feed solution (102) in the extraction unit operation of the solvent extraction system (100). Although the flow of the organic solution (106) is against the flow of the aqueous phase or feed solution (102) in the solvent extraction system, in each extraction stage (EX1, EX2, or EX3), the flows of the organic solution (106) and the aqueous phase or feed solution (102) are parallel (in the same direction), as disclosed herein.
[0086] In the solvent extraction system (100), the scrubbing (indicated by "SC") unit operation is carried out in two stages (SC1 and SC2). The organic phase (102) from extraction stage 3 (EX3) exits the extraction unit operation and enters scrubbing stage 1 (SC1) via a connector (B04) that allows fluid flow from extraction stage 3 (EX3) to scrubbing stage 1 (SC1). After the completion of the scrubbing stage 1 (SC1) operation, the organic phase (106) flows from scrubbing stage 1 (SC1) to scrubbing stage 2 (SC2) via a connector (B05). In scrubbing stage 2 (SC2), hydrochloric acid (HCl) may be added via port (A05), and then, after the completion of the scrubbing stage 2 (SC2) operation, the hydrochloric acid flows into scrubbing stage 1 (SC1) via connector (A06). Similar to the extraction unit, the flows of the organic and aqueous phases are opposite to each other in the overall system (100); however, the flows may be parallel in each stage (SC1 or SC2) disclosed herein in order to remove impurities during the scrubbing unit operation. Once scrubbing stage 1 (SC1) is complete, the scrubbing HCl solution may be added to extraction stage 3 (EX3) via the connector (A07).
[0087] The acid used in the scrubbing stage is not particularly limited and may vary depending on the design and application requirements. The pH of the unit operation is adjusted to enhance selectivity by adding the acid, thereby aiding in the purification of the target species.
[0088] In the solvent extraction system (100), the stripping (indicated by "ST") unit operation is carried out in two stages (ST1 and ST2). The organic phase (102) from scrubbing stage 2 (SC2) exits the scrubbing unit operation and enters stripping stage 1 (ST1) via a connector (B06) that allows fluid flow from scrubbing stage 2 (SC2) to stripping stage 1 (ST1). After the completion of the stripping stage 1 (ST1) operation, the organic phase (106) flows from stripping stage 1 (ST1) to stripping stage 2 (ST2) via a connector (B07). The stripping solution containing HCl is prepared in the stripping solution preparation unit (STF). The stripping solution preparation unit receives HCl via port A08 and the aqueous phase flowing from washing stage 1 (WA1) to the stripping solution preparation unit (STF) via connection (A13), and prepares the stripping solution. The stripping solution flows from the stripping solution preparation unit (STF) to stripping stage 2 (ST2) via connection (A09), and one of the stripping stages is performed. Upon completion, the aqueous solution flows from stripping stage 2 (ST2) to stripping stage 1 (ST1) via connection (A10). After the completion of stripping stage 1, the aqueous rich strip (116) exits stripping stage 1 (ST1) via port (A11). As with other unit operations, the flow of the organic phase between the stages (ST1 and ST2) of the stripping unit operation is opposite to the flow of the aqueous solution, while in each unit operation (ST1 or ST2), the flows of the two phases may be parallel (or in the same direction).
[0089] Similar to the scrubbing stage, the acid used in the stripping stage is not particularly limited and may vary depending on the design and application requirements. The pH of the stripping unit operation is adjusted by adding further acid to aid in the extraction of target species from the organic phase to the aqueous phase. This step also aids in the regeneration of the organic phase, which can be recycled in the process for further processing.
[0090] In the solvent extraction system (100), the washing (indicated by "WA") unit operation is carried out in one stage (WA1), however, it should be noted that additional stages, such as two, three, four, five, or six, are also included in the art disclosed herein, though not limited to these. The organic phase (102) from the stripping stage 2 (ST2) exits the stripping unit operation and enters the washing stage 1 (WA1) via a connection (B08) that allows fluid flow from the stripping stage 2 (ST2) to the washing stage 1 (WA1). In the washing stage 1 (WA1), water (H2O) may be added via a port (A12), and after the completion of the washing stage 1 (WA1), the aqueous phase flows from the washing stage 1 (WA1) to the stripping solution compounding unit (STF) via a connection (A13).
[0091] Once the washing unit operation is complete, the organic phase (106) flows from washing stage 1 (WA1) to pre-neutralization stage 1 (PN1) via connection (B09). Sodium hydroxide (NaOH) may be added to pre-neutralization stage 1 (PN1) via port (A14) to neutralize the acidity of the organic phase (106). After the completion of pre-neutralization stage 1 (PN1), the aqueous phase exits pre-neutralization stage 1 (PN1) via connection (A15) and enters washing stage 1 (WA1), while the organic phase (106) exits the system via outlet (B10). The organic phase (106) may be recycled back to extraction stage 1 (EX1) via inlet (B01).
[0092] As should be understood from the disclosure herein, the first and second solvent phases vary depending on the unit operation being performed. In the extraction stage, where the target species is present in the aqueous phase, the first solvent phase is the aqueous phase and the second solvent phase is the organic phase. However, this is reversed in subsequent unit operations. For example, in the stripping unit operation, the organic phase contains the target species and is therefore the first solvent phase, and the aqueous phase is the second solvent phase.
[0093] In a further embodiment, this specification describes a process for the purification of one or more target species, wherein the process is It includes a scrubbing step and an extraction step that is in fluid communication with the scrubbing step, and a stripping step that is in fluid communication with the scrubbing step, The process relates to a method disclosed herein, wherein at least one of the extraction step, scrubbing step, and stripping step includes the method disclosed herein.
[0094] In further embodiments, this specification describes a system for the purification of one or more target species, wherein the system is It includes an extraction stage that is in fluid communication with a scrubbing stage, and a stripping stage that is in fluid communication with a scrubbing stage, The present invention relates to a system in which at least one of an extraction stage, a scrubbing stage, and a stripping stage comprises the system disclosed herein.
[0095] Extraction steps, scrubbing steps, stripping steps, and other steps such as washing steps or pre-neutralization steps are not particularly limited and should be understood by those skilled in the art. These steps include the respective stages above in this specification for the extraction of a target species, in which appropriate process steps are performed using the methods and systems disclosed herein.
[0096] The methods and systems disclosed herein can help improve the dynamics of metal ion transfer during contact between aqueous and organic phases. This is achieved by replacing a conventional mixer-cetera contactor with a combination of one or more columns having a cetera (i.e., a "RapidSX™ contactor") at each stage, as disclosed herein. In addition, the methods and systems disclosed herein can help achieve near-plug-flow behavior, meaning that all solutions are mixed for approximately the same amount of time. This differs from conventional mixers and cetera, where the residence time distribution faces difficulties, and the mixer contactor is enlarged to ensure that the solutions are properly mixed in order to achieve high separation and purity targets. [Examples]
[0097] The above disclosure generally describes the present invention. A more complete understanding can be obtained by referring to the following specific embodiments. These embodiments are described for illustrative purposes only and are not intended to limit the scope of the invention. Modifications of form and substitution of equivalents are attempted where circumstances may suggest or provide convenience. Without further description, it is assumed that those skilled in the art can construct and utilize the constructs of the present invention and practice the claimed methods using the prior descriptions and the following exemplary examples. Accordingly, the following working embodiments focus specifically on typical aspects of the invention and are not to be construed as limiting in any way to the remainder of this disclosure. Certain terms are used herein, but such terms are intended to be descriptive and not limiting.
[0098] Example 1: Use of a set of RapidSX™ contactors to isolate REE. As shown in Figure 7, an SX circuit was staged using a single-column RapidSX® contactor of the type shown in Figure 3. The SX circuit consisted of three extraction stages (EX1, EX2, and EX3), two scrub stages (SC1 and SC2), two strip stages (ST1 and ST2), one strip supply box (STF), one washing stage (WA1), and one pre-neutralization stage (PN1). Each RapidSX® contactor utilized a 2-inch diameter, 10-foot PVC column filled with 3 mm diameter spherical polypropylene beads. Perforated plates were inserted at the top and bottom of each column to maintain the beads in place. Each column was connected to a 4-inch diameter, 2-foot PVC column. The aqueous and organic phases were introduced into the top of each column via flexible hoses. The aqueous and organic phases were then discharged from the bottom and top of the setter, respectively, via flexible hoses.
[0099] The pre-neutralized organic phase was placed in stage EX1, passed through each subsequent stage, and then returned to stage EX1. The aqueous supply solution was placed in stage EX3, passed through stages EX2 and EX1, and then stage EX1 was dispensed as a raffinate aqueous solution. A small amount of 50% NaOH was also added to stage EX3 as a means of controlling the pH during extraction.
[0100] Diluted HCl was used as the scrubbing solution, which was added to stage SC2, then flowed into stage SC1, and then stage EX3 was removed from stage SC1.
[0101] The stripping solution contained 5N HCl, and the output from the washing unit operation was mixed in the strip supply box, then transferred to stage ST2, flowed from stage ST2 to stage ST1, and dispensed as a rich strip aqueous solution.
[0102] Water was introduced into the washing unit operation at stage WA1 and then discharged into the strip supply box.
[0103] Diluted NaOH was introduced into the pre-neutralization unit via stage PN1, and then discharged to stage WA1.
[0104] The specific objective of the SX circuit described above was the separation of REE La-Ce-Pr-Nd from REE Sm-Eu-Gd-Tb-Dy-Ho-Er-Tm-Yb-Lu-Y. Table 1 shows the assay (parts per million (ppm)) of the initial Ce-depleted chloride system feed solution and the relative distribution of REE as a percentage of total REE (TREE). [Table 1]
[0105] The organic phase consisted of 33% by volume of Cyanex® 572 extractant dissolved in Exxon D80. The flow rate ratio between the organic phase and the aqueous phase through the extraction unit operation was set to 4:1, and the organic phase was flowed through the circuit at a rate of 1.2 L / min.
[0106] Table 2 shows the assay results for the generated raffinate in ppm and the relative distribution of the TREE. The purity of the raffinate relative to the target La-Ce-Pr-Nd element compared to the existing TREE was 99.9%. [Table 2]
[0107] All publications, patents, and patent applications cited herein are incorporated herein by reference to the same extent that each individual publication, patent, or patent application is specifically and individually shown to be incorporated by reference in whole.
[0108] Embodiment 1. A method for separating one or more target species from a first solvent phase, wherein the method is The method involves passing a first solvent phase containing one or more target species, and a first portion of a second solvent phase, through a first set of one or more columns containing a discontinuous packing medium, wherein the first solvent phase and the second solvent phase are immiscible with each other, and the flow of the first solvent phase and the second solvent phase through the first set of one or more columns is parallel. A method comprising the step of bringing a first solvent phase and a second solvent phase into contact with each other to enable the extraction of one or more target species from the first solvent phase to the second solvent phase.
[0109] 2. The method of Embodiment 1, wherein a first set of one or more columns is upright and the flow of the first solvent phase and the second solvent phase is downward.
[0110] 3. The method of Embodiment 1 or 2, wherein the discontinuous packing medium comprises a first zone containing a first discontinuous medium and a second zone containing a second discontinuous medium, the first discontinuous medium containing hydrophobic particles and the second discontinuous medium containing hydrophilic particles.
[0111] 4. The method of Embodiment 1 or 2, wherein the particles have a diameter of approximately 5 mm or less.
[0112] 5. The method of Embodiment 4, wherein the particles have a diameter in the range of about 1 to about 3 mm.
[0113] 6. A method according to any one of Embodiments 1 to 5, wherein the particles are substantially spherical or oval-shaped beads.
[0114] 7. The method according to Embodiment 6, wherein the beads are polymer beads or glass beads.
[0115] 8. Any one of Embodiments 1 to 7, wherein one or more columns are contactor columns.
[0116] 9. Any one of Embodiments 1 to 8, further comprising the step of passing the first solvent phase and the second solvent phase through a condenser to condense the first solvent phase and the second solvent phase.
[0117] 10. The method of Embodiment 9, wherein the coagulator includes a further discontinuous medium.
[0118] 11. The method of Embodiment 10, wherein further discontinuous media are present within the cartridge.
[0119] 12. Any one of Embodiments 1 to 11, further comprising separating a first solvent phase and a second solvent phase after passing them through a first set of one or more columns.
[0120] 13. The method of Embodiment 12, further comprising the step of recycling the first solvent phase and / or the second solvent phase.
[0121] 14. Passing a first solvent phase and a second portion of the second solvent phase through a second set of one or more columns containing a discontinuous packing medium, wherein the flows of the first solvent phase and the second solvent phase are parallel. The method of Embodiment 12 or 13 further comprises enabling the first solvent phase and the second solvent phase to come into contact with each other, thereby enabling the extraction of one or more target species from the first solvent phase to the second solvent phase.
[0122] 15. The method of Embodiment 14, further comprising separating the first solvent phase and the second solvent phase after passing them through a second set of one or more columns.
[0123] 16. The method of Embodiment 15, further comprising the step of recycling the first solvent phase and / or the second solvent phase.
[0124] 17. A system for extracting one or more target species from a first solvent phase to a second solvent phase, wherein the system is A first set comprising one or more columns containing a discontinuous packing medium, A system configured for the parallel flow of a first solvent phase and a second solvent phase in a first set of one or more columns, allowing contact between the first solvent phase and the second solvent phase as the solvent flows through a discontinuous packed medium.
[0125] 18. The system of Embodiment 17, wherein a first set of one or more columns is upright and configured for downward flow of a first solvent phase and a second solvent phase.
[0126] 19. The system of embodiment 17 or 18, further comprising a manifold for enabling the flow of a first solvent phase and / or a second solvent phase into a first set of one or more columns.
[0127] 20. Any one of the systems from Embodiments 17 to 19, wherein the particles have a diameter of approximately 5 mm or less.
[0128] 21. The system of Embodiment 20, wherein the particles have a diameter in the range of approximately 1 to approximately 3 mm.
[0129] 22. A system according to any one of embodiments 17 to 21, wherein the particles are substantially spherical or oval-shaped beads.
[0130] 23. A system according to Embodiment 22, wherein the beads are polymer beads or glass beads.
[0131] 24. One of the systems from any one of embodiments 17 to 23, wherein one or more columns are contactor columns.
[0132] 25. Any one of the systems of Embodiments 17 to 24, further comprising a flocculant located downstream of a first set of one or more columns, wherein the flocculant flocces a first solvent phase and a second solvent phase.
[0133] 26. The system of Embodiment 25, wherein the coagulator includes a further discontinuous medium.
[0134] 27. The system of embodiment 26, wherein further discontinuous media are present within the cartridge.
[0135] 28. The system of Embodiment 26 or 27, wherein the further discontinuous medium is a hydrophilic discontinuous medium.
[0136] 29. The system of Embodiment 26 or 27, wherein the further discontinuous medium is a hydrophobic discontinuous medium.
[0137] 30. Any one of the systems from Embodiments 17 to 29, further comprising a first setra tank that enables separation of a first solvent phase and a second solvent phase after passing through a first set of one or more columns.
[0138] 31. The system of Embodiment 30 further comprises a recycling control means in fluid communication with a first setra tank that enables the recycling of the separated first solvent phase and / or separated second solvent phase after passing through a first set of one or more columns.
[0139] 32. Further comprising a second set of one or more columns containing a discontinuous packing medium, A system according to embodiment 30 or 31, wherein the system is configured for the parallel flow of a first solvent phase and a second solvent phase, and allows contact between the first solvent phase and the second solvent phase as the solvent flows through a discontinuously packed medium.
[0140] 33. The system of embodiment 32 further comprises a second setra tank that enables separation of the first solvent phase and the second solvent phase after passing through a second set of one or more columns.
[0141] 34. The system of Embodiment 32 further comprises a recycling control means in fluid communication with a second setra tank that enables the recycling of the separated first solvent phase and / or separated second solvent phase after passing through a second set of one or more columns.
[0142] 35. A process for the purification of one or more target species, wherein the process is It includes a scrubbing step and an extraction step that is in fluid communication with the scrubbing step, and a stripping step that is in fluid communication with the scrubbing step, A process in which at least one of the extraction step, the scrubbing step, and the stripping step includes a method defined in any one of embodiments 1 to 16.
[0143] 36. A process of embodiment 35, further comprising a washing step in fluid communication with a stripping step, and a pre-neutralization step in fluid communication with a washing step.
[0144] 37. A process of Embodiment 36, wherein at least one of the washing step and the pre-neutralization step includes a method defined in any one of Embodiments 1 to 16.
[0145] 38. A system for purifying one or more target species, wherein the system is It includes an extraction stage that is in fluid communication with a scrubbing stage, and a stripping stage that is in fluid communication with a scrubbing stage, A system comprising at least one of an extraction stage, a scrubbing stage, and a stripping stage, the system as defined in any one of embodiments 17 to 34.
[0146] 39. The system of embodiment 38, further comprising a cleaning stage having fluid communication with a stripping stage, and a pre-neutralization stage having fluid communication with the cleaning stage.
[0147] 40. The system of Embodiment 39, wherein at least one of the washing stage and the pre-neutralization stage comprises a system defined in any one of Embodiments 17 to 34.
[0148] Preferred embodiments of the present invention are described in detail herein, but it will be understood by those skilled in the art that modifications can be made without departing from the spirit of the invention or the scope of the appended claims. [Table 3]
Claims
1. A method for separating one or more target species from a first solvent phase, wherein the method is The method involves passing the first solvent phase containing one or more target species and a first portion of the second solvent phase through a first set of one or more columns containing a discontinuous packing medium, wherein the first solvent phase and the second solvent phase are immiscible with each other, and the flows of the first solvent phase and the second solvent phase are parallel. A method comprising enabling the first solvent phase and the second solvent phase to come into contact with each other, thereby enabling the extraction of one or more target species from the first solvent phase to the second solvent phase.
2. The method according to claim 1, wherein a first set of one or more columns is upright and the flow of the first solvent phase and the second solvent phase is downward.
3. The method according to claim 1 or 2, wherein the discontinuous packing medium comprises a first zone containing a first discontinuous medium and a second zone containing a second discontinuous medium, the first discontinuous medium containing hydrophobic particles and the second discontinuous medium containing hydrophilic particles.
4. The method according to any one of claims 1 to 3, wherein the discontinuous packing medium includes particles having a diameter of about 5 mm or less.
5. The method according to claim 4, wherein the particles have a diameter in the range of about 1 to about 3 mm.
6. The method according to any one of claims 1 to 5, wherein the particles are substantially spherical or oval-shaped beads.
7. The method according to claim 6, wherein the beads are polymer beads.
8. The method according to any one of claims 1 to 7, wherein one or more of the columns are contactor columns.
9. The method according to any one of embodiments 1 to 7, further comprising the step of passing the first solvent phase and the second solvent phase through a condenser to condense the first solvent phase and the second solvent phase.
10. The method according to claim 9, wherein the coagulator includes a further packing medium.
11. The method according to claim 10, wherein the further filling medium is present in the cartridge.
12. The method according to any one of claims 1 to 11, further comprising separating the first solvent phase and the second solvent phase after passing them through a first set of one or more columns.
13. The method according to claim 12, further comprising the step of recycling the first solvent phase and / or the second solvent phase.
14. The first solvent phase and the second portion of the second solvent phase are passed through a second set of one or more columns containing a discontinuous packing medium, wherein the flow of the first solvent phase and the second solvent phase is parallel. The method according to claim 12 or 13, further comprising enabling the first solvent phase and the second solvent phase to come into contact with each other, thereby enabling the extraction of one or more target species from the first solvent phase to the second solvent phase.
15. The method according to claim 14, further comprising separating the first solvent phase and the second solvent phase after passing them through a second set of one or more columns.
16. The method according to claim 15, further comprising the step of recycling the first solvent phase and / or the second solvent phase.
17. A system for extracting one or more target species from a first solvent phase to a second solvent phase, wherein the system is A first set comprising one or more columns containing a discontinuous packing medium, The system is configured for the parallel flow of the first solvent phase and the second solvent phase in a first set of one or more columns, and allows contact between the first solvent phase and the second solvent phase as the solvent flows through the discontinuously packed medium.
18. The system according to claim 17, wherein a first set of one or more columns is upright and configured for downward flow of the first solvent phase and the second solvent phase.
19. The system according to claim 17 or 18, further comprising a manifold for enabling the flow of the first solvent phase and / or the second solvent phase to a first set of one or more columns.
20. The system according to any one of claims 17 to 19, wherein the particles have a diameter of about 5 mm or less.
21. The system according to claim 20, wherein the particles have a diameter in the range of about 1 to about 3 mm.
22. The system according to any one of claims 17 to 21, wherein the particles are substantially spherical or oval-shaped beads.
23. The system according to claim 22, wherein the beads are polymer beads.
24. The system according to any one of claims 17 to 23, wherein one or more of the columns are contactor columns.
25. The system according to any one of claims 17 to 24, further comprising a flocculant located downstream of a first set of one or more columns, wherein the flocculant flocces the first solvent phase and the second solvent phase.
26. The system according to embodiment 25, wherein the coagulator includes a further packing medium.
27. The system according to embodiment 26, wherein the aforementioned additional filling medium is present in the cartridge.
28. The system according to embodiment 26 or 27, wherein the further filling medium is a hydrophilic discontinuous medium.
29. The system according to embodiment 26 or 27, wherein the further filling medium is a hydrophobic discontinuous medium.
30. The system according to any one of claims 17 to 29, further comprising a first setra tank that enables separation of the first solvent phase and the second solvent phase after passing through a first set of one or more columns.
31. The system according to claim 30, further comprising a recycling control means in fluid communication with the first setra tank, which enables the recycling of the separated first solvent phase and / or separated second solvent phase after passing through the first set of one or more columns.
32. Further comprising a second set of one or more columns containing a discontinuous packing medium, The system according to claim 30 or 31, wherein the system is configured for the parallel flow of the first solvent phase and the second solvent phase, and allows contact between the first solvent phase and the second solvent phase as the solvent flows through the discontinuously packed medium.
33. The system according to claim 32, further comprising a second setra tank that enables separation of the first solvent phase and the second solvent phase after passing through a second set of one or more columns.
34. The system according to claim 33, further comprising a recycling control means in fluid communication with a second setra tank that enables recycling of the separated first solvent phase and / or separated second solvent phase after passing through a second set of one or more columns.
35. A process for purifying one or more target species, wherein the process comprises: It includes an extraction step that is in fluid communication with the scrubbing step, and a stripping step that is in fluid communication with the scrubbing step, A process comprising at least one of the extraction step, the scrubbing step, and the stripping step, using a method defined in any one of claims 1 to 16.
36. The process according to claim 35, further comprising a cleaning step in fluid communication with the stripping step, and a pre-neutralization step in fluid communication with the cleaning step.
37. The process according to claim 36, wherein at least one of the washing step and the pre-neutralization step includes a method defined in any one of claims 1 to 16.
38. A system for purifying one or more target species, wherein the system is It includes an extraction stage that is in fluid communication with a scrubbing stage, and a stripping stage that is in fluid communication with the scrubbing stage, A system comprising at least one of the extraction stage, scrubbing stage, and stripping stage, which is defined in any one of claims 17 to 34.
39. The system according to claim 38, further comprising a cleaning stage having fluid communication with the stripping stage, and a pre-neutralization stage having fluid communication with the cleaning stage.
40. The system according to claim 39, wherein at least one of the washing stage and the pre-neutralization stage comprises a system defined in any one of claims 17 to 34.