Processes for separating aqueous phase from an emulsion
Patent Information
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- BASF CORPORATON
- Filing Date
- 2024-07-23
- Publication Date
- 2026-06-03
AI Technical Summary
Conventional processes for removing entrained aqueous material from organic effluents are limited in effectiveness and capital cost intensive, necessitating a more efficient and cost-effective method for separating the aqueous phase from emulsions in solvent extraction and recycling processes.
The process involves contacting the emulsion with an electro-coalescer unit that applies a direct-current (DC) voltage field, causing fine aqueous droplets to coalesce into larger droplets, which are then separated from the organic phase. The electro-coalescer unit includes a housing and porous electrodes coated with a dielectric and hydrophobic polymer.
This process effectively reduces the aqueous phase content in the organic phase by up to 80-90%, improving the purity of subsequent products and reducing the transfer of impurities downstream, thus enhancing the efficiency and cost-effectiveness of solvent extraction and recycling processes.
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Figure US2024039125_30012025_PF_FP_ABST
Abstract
Description
PROCESSES FOR SEPARATING AQUEOUS PHASE FROM AN EMULSIONBACKGROUNDCertain operations, including mining operations and battery recycling operations, involve solvent extraction and / or refining processes, including resource recovery, treatment, and / or purification processes. In processes (e.g., solvent extraction) where organic and aqueous might come in contact and / or be mixed together and then later separated in a separation step to achieve certain outcomes, there may be a need to further remove an aqueous phase from organic effluent after the separation step. The remaining or entrained aqueous material in the organic phase may form an emulsion with the organic phase and may also carry undesired impurities that may need to be removed prior to subsequent processes. Conventional processes or unit operations for removing entrained aqueous material from an emulsion have been shown to be limited in their effectiveness and are capital cost intensive. Accordingly, there is a desire for one or more processes that provide cost effective removal of most if not all entrained aqueous material from such organic effluents.FIELDEmbodiments herein generally relate to processes for separating aqueous phase from an emulsion, e.g., a water-in-oil emulsion. Specifically, processes are described herein for separating aqueous phase from an emulsion derived from a metal solvent extraction process, a wash process, a stripping process, and / or other processes related to organic / aqueous separation.SUMMARYA process for reducing an aqueous phase content entrained in an organic phase of an emulsion is provided. The process can include contacting the emulsion with an electro-coalescer unit that can provide a voltage field. The voltage field may be a direct-current (DC) voltage field, and alternating-current (AC) voltage field, or a combination of the foregoing. It is more preferably a DC voltage field. The aqueous phase can include fine droplets, and the fine droplets can coalesce to form larger droplets. At least some of the fine droplets can have a size of less than about 100 micro-meters (pm). The process can include separating the larger droplets from the emulsion. The electro-coalescer unit can include a housing and at least two porous electrodes coated with at leastone polymer. The emulsion can be derived from one or more intermediate steps of an extraction process.BRIEF DESCRIPTION OF DRAWINGSThe various aspects and advantages of the embodiments of the present invention will become apparent to those skilled in the art upon an understanding of the following detailed description of the invention, read in light of the accompanying drawings which are made a part of this specification. In the drawings:Figure 1 depicts an illustrative schematic of an exemplary process for reducing an aqueous phase content entrained in an organic phase of an emulsion, according to one or more embodiments.Figure 2 depicts an illustrative schematic of an extraction process, according to one or more embodiments.Figure 3 depicts an illustrative schematic for a metal recovery process including one or more electro-coalescers, two are shown, for reducing an aqueous phase content in the emulsion, according to one or more embodiments described.Figure 4 depicts an alternative embodiment of the illustrative schematic from Figure 3, according to one or more embodiments.Figure 5 depicts another alternative embodiment of the illustrative schematic from Figure 3, according to one or more embodiments.DETAILED DESCRIPTIONA detailed description will now be provided. Each of the appended claims defines a separate invention, which for infringement purposes is recognized as including equivalents to the various elements or limitations specified in the claims. Depending on the context, all references to the “invention”, in some cases refer to certain specific or preferred embodiments only. In other cases, references to the “invention” refer to subject matter recited in one or more, but not necessarily all, of the claims. It is to be understood that the following disclosure describes several exemplary embodiments for implementing different features, structures, or functions of the invention. Exemplary embodiments of components, arrangements, and configurations are described below to simplify the present disclosure; however, these exemplary embodiments are provided merely as examples and are not intended to limit the scope of the invention. Additionally, the presentdisclosure may repeat reference numerals and / or letters in the various exemplary embodiments and across the Figures provided herein. This repetition is for the purpose of simplicity and clarity and does not necessarily dictate a relationship between the various exemplary embodiments and / or configurations discussed in the Figures. Moreover, the formation of a first feature over or on a second feature in the description that follows includes embodiments in which the first and second features are formed in direct contact and also includes embodiments in which additional features are formed interposing the first and second features, such that the first and second features are not in direct contact. The exemplary embodiments presented below can be combined in any combinations, i.e., any element from one exemplary embodiment can be used in any other exemplary embodiment, without departing from the scope of the disclosure. The figures are not necessarily drawn to scale and certain features and certain views of the figures can be shown exaggerated in scale or in schematic for clarity and or conciseness.Additionally, certain terms are used throughout the following description and claims to refer to particular components. As one skilled in the art will appreciate, various entities may refer to the same component by different names, and as such, the naming convention for the elements described herein is not intended to limit the scope of the invention, unless otherwise specifically defined herein. Also, the naming convention used herein is not intended to distinguish between components that differ in name but not function. Furthermore, in the following discussion and in the claims, the terms “including” and “comprising” are used in an open-ended fashion, and thus should be interpreted to mean “including, but not limited to.”Further, the term “or” is intended to encompass both exclusive and inclusive cases, e.g., “A or B” is intended to be synonymous with “at least one of A and B,” unless otherwise expressly specified herein. The indefinite articles “a” and “an” refer to both singular forms (i.e., “one”) and plural referents (i.e., one or more) unless the context clearly dictates otherwise. The terms “up” and “down”; “upward” and “downward”; “upper” and “lower”; “upwardly” and “downwardly”; “above” and “below”; and other like terms used herein refer to relative positions to one another and are not intended to denote a particular spatial orientation since the apparatus and processes of using the same can be equally effective at various angles or orientations.Each of the inventions will now be described in greater detail below, including specific or preferred embodiments, versions and examples, but the inventions are not limited to these embodiments, versions, or examples, which are provided to enable a person having ordinary skill in the art to make and use the inventions, when the information in this disclosure is combined with publicly available information and technology.Figure 1 depicts an illustrative schematic of an exemplary process 100 for reducing an aqueous phase 161 content entrained in an organic phase 162 of an emulsion 125, according to one or more embodiments. At least a portion of the aqueous phase 161 entrained in the organic phase 162 can be in the form of droplets, e.g., one or more very small or fine droplets.In the process 100, the emulsion 125 can be contacted with one or more electro-coalescers 103 to efficiently separate droplets from the emulsion 125. The one or more electro-coalescers 103 can each have a DC voltage field, such that upon contacting the DC voltage field the fine droplets can coalesce into larger droplets within the emulsion 125. The larger coalesced droplets can be removed or separated from the emulsion 125 by settling, sinking, centrifuging, or other separations processes for separating droplets from the emulsion 125. For example, a tank 104 can be used to settle the coalesced droplets to form a separated droplet stream 115 and a separated organic stream 131. The separation of at least a portion of the aqueous phase 161 from the emulsion 125 can facilitate the removal of impurities and / or microdroplets from the emulsion 125. Accordingly, by coalescing the fine droplets into larger droplets and separating the larger droplets from the emulsion 125, the emulsion 125 can experience a resultant reduction in aqueous-borne impurities thereby improving the purity of subsequent downstream products.The entrainment of aqueous droplets in an organic phase can increase with mixing and can result in an excessive quantity of fine droplets, or can be present in aged organic (also known recycled organic). Under high shear conditions the aqueous droplets can be broken into very fine droplets resulting in a higher amount of aqueous content in the emulsion 125. Aged organic can be, over time, contaminated by any surface-active compounds used in an overall process, with correspondingly less hydrophobicity and higher impurity content, which can result in a higher aqueous content in the emulsion 125.Conventional processes or unit operations have been shown to be limited in their effectiveness for separating droplets. For example, conventionally, a settler or a centrifuge can be used in the absence of an electrocoalescence step, to separate entrained aqueous from the emulsion 125, but the efficiency would be insufficient.In any of the embodiments of this disclosure, one or more of the fine droplets can have a size of less than about 100 pm. One or more of the entrained aqueous droplets within the emulsion 125 can be larger aqueous droplets and can have a size of greater than from about 100 pm to about 500 pm or greater. The one or more fine droplets can have an average size of less than about 100 pm and the larger droplets can have an average size of greater than about 500 pm. The one or more fine droplets can have an average size of less than about 200 pm, 150 pm, 100 pm, 90 pm, 80 pm, 70 pm, 60 pm, 50 pm, 40 pm, 30 pm, 20 pm, 10 pm, or smaller. The one or more larger aqueous droplets can have an average size of more than about 200 pm, 250 pm, 300 pm, 350 pm, 400 pm, 450 pm, 500 pm, 550 pm, 600 pm, 650 pm, 700 pm, or greater. The one or more fine and larger droplets can include ions including monovalent, divalent, and / or multivalent ions and / or sulfate and / or chloride salts.In one or more embodiments, the aqueous phase 161 can include sulfate, chloride, nitrate, and / or salts of organic acid. Prior to the emulsion 125 contacting the electro-coalescer 103, one or more of a monovalent, divalent, or multivalent salt and / or an organic modifier can be added to the emulsion 125 to facilitate the coalescing process.The aqueous content in the separated organic stream 131 can be less than 1000 ppm, can be less than 500 ppm, can be less than 100 ppm or less. The separated organic stream 131 can be sent for further processing. The separated droplet stream 115 can be removed from the tank 104 via gravity drain or pumping and can be a waste product or, all or a portion, can be utilized as an aqueous additive to other processes.The electro-coalescer 103 can include a housing and at least two porous electrodes. For example, the porous electrodes may include a conductive mesh, or a perforated metal plate, or a combinationof these. Each electrode can include independent electrical connections. A first DC voltage can be applied to and maintained on the first porous electrode and a second DC voltage can be applied to and maintained on the second porous electrode. Generally, the first and second DC voltages applied to first and second porous electrodes are different, in order to generate an electric field between the two or more electrodes. One or more of the respective electrodes can be grounded. The voltage difference between the electrodes can be about 50 to about 500 V DC. A gap distance measured between the two electrodes can be between about 0.25 mm to about 5 mm. The electrocoalescer 103 can be operated at a voltage difference of about 100 V DC to about 500 V DC. The electro-coalescer 103 can be operated at a voltage difference of about 100 V DC to about 400 V DC.The porous electrodes can be coated with a polymer. In embodiments, the porous electrodes can be coated with at least one dielectric and hydrophobic polymer. A porous electrode in any embodiment may be generally a two-dimensional-type or three-dimensional-type structure. An exemplary two-dimensional-type structure is a sheet. Exemplary three dimensional-type structures include a ball (e.g., steel wool ball) or a multi-layer grid (e.g., metal grid). A porous electrode may be woven or non-woven. Other examples for a porous electrode include woven and non-woven mesh, perforated plates, porous sintered metal and / or parallel layered metal strips. In any embodiment, a porous electrode may be a mesh, such as a metal mesh or wire mesh. In any embodiment, the porous electrode may be a stainless steel woven mesh. In any embodiment, a porous electrode may be a perforated plate or perforated sheet. In any embodiment, a porous electrode may be made of (or comprise) a metallic material such as stainless steel and / or titanium and / or a corrosion-resistance metallic material such as Hastelloy. However in the presence of a polymeric coating such corrosion resistant metal for the electrode is not always required. Thus, the electrode materials may comprise conventional metals such as stainless steel or titanium.In any embodiment, a porous electrode may be coated, which may include a partial and / or a complete coating. In any embodiment, the coating may include a dielectric coating, a hydrophobic coating, and combinations thereof. The coating may be a single coating having both a dielectric function and a hydrophobic function. In other embodiments, separate coatings may serve the respective functions of dielectric coating and hydrophobic coating. The coating can generally serveto prevent possible short circuiting and provide an initial large drop contact angle. The dielectric coating may be referred to as an insulating dielectric coating.In one or more embodiments, the coating may include first applying a layer of the insulating dielectric coating and then applying a layer of hydrophobic coating on the insulating dielectric coating. Exemplary insulating dielectric coatings include insulating dielectric polymers, such as poly (methyl methacrylate) (PMMA) and poly (styrene-co-methyl methacrylate) (PS / PMMA) . An exemplary hydrophobic coating is a fluoropolymer-based film. In one or more embodiments, the coating can be a polymer serving both a dielectric function and a hydrophobic function. Such coatings may be applied by any suitable method, such as spin coating, dip coating, or other similar coating methods generally known to the person having ordinary skill in the art.To contact the one or more electro-coalescers 103, the emulsion 125 can pass through a first porous electrode, a second porous electrode, and / or a third porous electrode, and so on until the emulsion 125 exits the electric field between the electrodes and / or exits the one or more electro-coalescers 103.The one or more electro-coalescers 103 can be operated at atmospheric pressure. Due to the presence of a coating on the electrodes, little current may pass from the first electrode to the second electrode, and thus the power consumption can be much lower than other technologies. For example, a known example system is the Petreco Metercell that is operated under pressure (e.g., higher cost of housing) and at a high voltage of 5-50 kV with higher power consumption and therefore higher operating cost.The electro-coalescer 103 can have one or more internal cleaning and purging gear to fully or partially remove particulate matter 123 that may build up on the porous electrodes, and thus clean the porous electrodes. The particulate matter 123 can be or include particles, solids, and / or semi solids. The internal cleaning and purging gear can be or include one or more wipers or scrubbers, not shown. The one or more internal cleaning and purging mechanisms can divert the particulate matter 123 that may build up on the porous electrodes from the porous electrodes.The emulsion 125 can be derived from one or more intermediate steps of a metal recovery process. For example, the one or more intermediate steps can include an extraction process that can include one or more metal solvent extraction steps, one or more wash steps, one or more stripping steps and / or a combination thereof within the metal recovery process. The extraction process can be for recovering metals such as Ni, Li, Co, and / or Mn recovery from a battery material recycling process. The emulsion 125 can be derived from one or more intermediate steps of a black mass recycle process, wherein a black mass can be or include ground post-consumer batteries. As used herein “black mass” may refer to solids material obtained from recycling of the batteries. The emulsion 125 can be derived from a battery production intermediate and / or by-product material recovery and recycling process that can include mixed metal sulfate recovery, metal hydroxide recovery, metal oxide recovery, cathode material recycling, metal recovery from LiNiCh delithiation processes, and / or metal recovery from LiNiCh (LNO) acid processing. The emulsion 125 can be derived from an emulsion of an intermediate step in cathode recycling materials that can include nickel cobalt manganese oxide (NCM), nickel cobalt aluminum oxide (NCA), nickel cobalt manganese aluminum oxide (NCMA), lithium cobalt oxides (LCO), lithium iron phosphate (LFP), and / or lithium nickel oxide (LiNiCh or LNO).The emulsion 125 can be derived from copper metal production or copper salt production. For example, in the processing of copper oxide-containing ores, the copper can be leached from the oxide mineral ores with sulfuric acid as a lixiviant, where the resulting leach solution can be sent for further processing by solvent extraction with an organic extractant, where the emulsion 125 can be derived. When the copper in the ore is present as a secondary sulfide type mineral, the copper can be leached from the ore with an acid such as sulfuric acid as the lixiviant together with a suitable oxidizing species such as ferric ion. The resulting leach solution can be similarly further processed by solvent extraction where the emulsion 125 can be derived. Ores containing copper present as a primary sulfide mineral may need to be initially processed in a more aggressive oxidizing environment such as a pressure vessel in the presence of an oxidizing species, such as ferric ion and oxygen, in order to solubilize the copper. The resulting leach solution from such a process can be further processed by solvent extraction where the emulsion 125 can be derived. The emulsion 125 can be derived from an ammonia leaching system such as the production of copper and nickel from an ammoniacal leach of a mixed hydroxide precipitate. An alternative leachingsolution in copper mining can employ hydrochloric acid. The presence of hydrochloric acid would not be compatible with conventional electro-coalescer units that do not employ polymer coated porous electrodes or compatible material for wetted parts. But the presently disclosed polymer- coated porous electrodes would mitigate any potential damage from hydrochloric acid.The emulsion 125 can be derived from a leaching process of precious metals such as gold and platinum group metals (PGM’s). In such a process, impure precious metals can be leached from ores or other PGM-containing materials under highly oxidizing conditions optionally in the presence of chlorine gas to solubilize the precious metals.Figure 2 depicts an illustrative schematic of an extraction process 200, according to one or more embodiments. In one or more embodiments, the extraction process 200 can be a solvent extraction (SX) process and can include multiple extraction and stripping units each of which can include a contact step (e.g., mixing) and a settling step (e.g., holding in a settler). An electro-coalescer 103 can be used to efficiently remove the entrained aqueous phase from the organic phase after the organic phase is used for extraction (or stripping steps performed upon the organic phase) to reduce impurities carried within the aqueous phase. Example of these are described in figures 2 and 3 of PCT Publication No. W02022120311 Al (herein incorporated by reference).In an embodiment, the extraction process 200 can include extraction of one or more metals of interest, e.g. Li, or impurities such as Ca. Examples of such extraction processes can be found, for example in PCT Publication No. W02022120311A1, which is herein incorporated by reference, (e.g., in figure 2 (Ca SX), figure 3 (Li SX)) and in U.S. Patent Publication No. 2021 / 0130927, which is herein incorporated by reference.During the extraction process 200, a relatively metal-rich aqueous phase 213 can be contacted in step 203 with an immiscible organic phase 214 that can include a selective organic extractant. One or more metals can be transferred across the interface of the organic phase 214 and aqueous phase 213 to form a metal-loaded organic phase. Fine aqueous droplets can develop within the organic phase 214 upon the action of mixer 208. The resulting mixture can be directed to a settling vessel 204 where at least a portion of the relatively metal-poor aqueous phase 221 can be settled out ofthe metal-loaded organic phase or otherwise allowed to separate based on density and / or immiscibility characteristics. However, the metal-loaded organic phase leaving the settling vessel 204 can contain fine aqueous droplets and can form or result in the emulsion 125. In any embodiment of the present disclosure, the emulsion 125 may be provided as the emulsion 125 of Figure 1 above. The separated phases can be forwarded for additional processing. In an embodiment, the extraction process 200 can be part of mining operations and / or battery recycling operations.Figure 3 depicts an illustrative schematic diagram for a metal recovery system 300. Such system 300 may include one or more electro-coalescers 103 (two are shown), for reducing an aqueous phase content in the emulsion 125, according to one or more embodiments described. The metal recovery system 300 can be for conducting a process for recovering nickel, lithium, or some other metal produced from an effluent 313 emanating from a treatment system 301. The treatment system 301 can be for delithiating a lithium nickel oxide (LiNiCh) material. Example embodiments for delithiation of a lithium nickel oxide (LiNiCh) material can be found in PCT Publication No. W02020093041A1, titled “METHODS FOR EXTRACTING ELEMENTS FROM A SOLUTION,” which publication is herein incorporated by reference. For simplicity, and for illustrative purposes, and without limiting the scope of this disclosure or any claims, throughout the rest of this disclosure when referring to instant Figures 3, 4 and 5, example embodiments are directed to a process for delithiation of a lithium nickel oxide (LiNiO?) material which can be utilized for, among other uses, removing Li and Ni from solutions.In one or more embodiments, the treatment process system 301 can include contacting a lithium nickel oxide 310 with sulfuric acid 311 in an acid treatment step 302. A solid-liquid separation step 323 can separate a delithiated LiNiCh solid 312 and the effluent 313, and nickel can be removed from the effluent 313 by the extraction process 200 (such as a metal solvent extraction step 308).The metal recovery process 300 can include one or more extraction processes 200 for extracting a metal of interest (e.g., nickel, lithium, or other metals) from the effluent stream 313. For example, the one or more extraction processes 200 can include one or more metal solvent extraction steps308, one or more wash steps 309, and / or one or more stripping steps 305. The one or more metal solvent extraction steps 308 can include contacting the effluent stream 313 with an organic extractant 314 within a vessel that can be or include the mixer 208 and the settling vessel 204 configured to mix the effluent stream 313 and the organic extractant 314, or any number of streams, and settle a resultant mixture.The mixer-settler 208 / 204 can separate the resultant mixture as a metal-loaded separated organic stream or emulsion 125 and an aqueous phase or stream 316. The stream 316 emanating from the mixer-settler 208 / 204 can be called a raffinate, which can be an aqueous depleted of the metal of interest (relatively metal-poor) after contacting and settling. The raffinate can have other metals of interest (such as Li), which can be separated in downstream process such as metal solvent extraction, crystallization, precipitation, solid-liquid separation, etc. For example, the one or more embodiments depicted in Fig 3 can separate Ni in the form of pure Ni salt. By utilizing a different organic extractant and process conditions, stream 316 can be directed into one or more metal extraction processes 200 (not shown), to separate Li from stream 316.The emulsion 125 can optionally be washed in the one or more wash steps 309 to remove impurities from the emulsion 125. The one or more wash steps 309 can utilize treated water 317 to remove one or more impurities that may be present in the emulsion 125. The treated water 317 can have a conductivity less than about 1 to 10 microSiemens per cm (pS / cm). For example, the treated water 317 can be or include deionized water or water generated by reverse osmosis with very low conductivity. The mixer-settler 208 / 204 at the wash step 309 can separate the resultant mixture as the emulsion 125 and an aqueous phase or stream 396.The electro-coalescer 103 can eliminate, or alternatively, reduce the necessity for one or more of the wash stages 309. The one or more wash stages 309 can be inefficient, often cannot adequately remove entrained aqueous phase, may consume significant amounts of water, and may increase investment costs.In one or more embodiments, the metal solvent extraction step 308 can be used to extract Ni and / or Li from the effluent 313 (e.g., aqueous phase containing dilute or impure metal(s) of interest). Themetal solvent extraction step 308 can include a contact step within the mixer-settler 208 / 204 to extract a metal of interest (e.g., nickel), by contacting aqueous and an organic extractant. In any embodiment, the organic extractant may be selective for a metal of interest. In some embodiments, the organic extractant may be a nickel selective extractant, such as an oxime, or a carboxylic acid such as neodecanoic acid or versatic acid.The resulting emulsion 125 can include aqueous phase content in the form of one or more entrained aqueous droplets and an organic phase. The entrained aqueous droplets can be present in the emulsion 125 as aqueous content that did not separate or settle in the mixer-settler 208 / 204 step into the stream 316.The emulsion 125 can be contacted with the one or more electro-coalescers 103, such that at least some fine aqueous droplets can be made to coalesce into larger droplets within the emulsion 125. The tank 104 can be used to settle the coalesced droplets to form a separated droplet stream 115 and a purified metal-loaded separated organic stream 343. A filtration or solids removal step 307 can be optionally used prior to the electro-coalescer 103 to fully or partially remove particles, solids, semi solids 123 that may be present in the emulsion 125, to inhibit clogging of electrodes in the electro-coalescer 103. Example devices to be used to promote filtration or solids removal in step 307 can include one or more basket filters, one or more self-cleaning filters, one or more bag filters, one or more centrifuges (decanting, sedimenting, or filtering), or other devices capable of filtration or solid removal from a stream.The purified metal-loaded separated organic stream 343 can be stripped of metal in the one or more stripping steps 305. For example, the one or more stripping steps 305 can strip metal from loaded organic and result in a Ni salt product 347. Consequently, another emulsion 125 may emanate from stripping step 305 (use of like numeral 125 in various Figures does not necessarily refer to an emulsion of same chemical composition, but rather, any emulsion amenable to phase separation promoted by electrocoalescence). The emulsion 125 emanating from stripping step 305 can be contacted with a second electro-coalescer 103 and a second tank 104 to remove aqueous material 115 from the emulsion 125 emanating from stripping step 305. The purified strippedorganic (i.e., having had at least a portion of its metal content stripped therefrom) 387 can be introduced into the metal solvent extraction step 308.The metal containing product (nickel, lithium or both) 347 can be optionally processed through a crystallizer step 306 and the solid-liquid separation step 323 (separating crystallized pure salt 322 from filtrate or mother liquor). The resulting product 322 can be optionally in the form of a nickel salt.In the one or more stripping steps 305, the pH of the nickel-rich solution emanating from the mixersettler 208 / 204 can be lowered by contact with a stream 321 that can comprise an acid, such as H2SO4, HC1, or other suitable acid. An acid can be optionally added to reduce the pH from the pH of the extraction solution(s) to optionally at or less than about 3.0, optionally 2.0, or lower, to thereby strip the Ni from the Ni rich solution and move it into an aqueous phase as a Ni salt for subsequent isolation or use. The resulting solution(s) from the one or more strip stages can be passed to a collection tank for direct use, cleaning or wash, or may be subjected to further processes whereby the lithium may precipitate so as to be collectable and optionally usable for one or more downstream processes or for the formation of other materials. The extracted nickel, lithium, or both can be optionally washed, the liquid materials filtered, and the products suitable for use in one or more downstream processes.Figure 4 depicts an alternative embodiment of the illustrative schematic from Figure 3, according to one or more embodiments. In Figure 4, drain lines 430 depict potential alternative flow paths for aqueous material that may be separated from the one or more tanks 104. The aqueous material can be directed to any process step to better utilize and recycle the aqueous material captured throughout the metal recovery process 300.Figure 5 depicts another alternative embodiment of the illustrative schematic from Figure 3, according to one or more embodiments. In Figure 5, the wash step 309 can be optionally located after the electro-coalescer 103 and the tank 104. The stream 553 emanating from the tank 104 can be a metal-loaded separated organic stream 553 that can be at least partially purified in the wash step 309 and can result in the purified metal-loaded separated organic stream 343.In one or more embodiments for hydrometallurgical processes, desired target metal(s) can be leached in a suitable lixiviant into an aqueous solution and intermediate steps within the one or more hydrometallurgical processes can result in the emulsion 125. Lixiviant examples can include sulfuric acid or ammonia. The lixiviants can be non-selective, and non-target metals can also be leached into the same aqueous matrix, to form an impure aqueous leach solution. The metal solvent extraction step 308 can involve contacting the impure aqueous leach solution with an organic solution containing a selective metal extractant. An example selective metal extractant can include salicyaldoximes in a hydrocarbon diluent, and used for copper extraction.
[0001] In any embodiment of the present disclosure, a metal extractant compound (that may be selective or non selective extractants for metal ions) may be mixed in an organic solvent, sometimes referred to as a diluent, to form an extractant organic phase. The organic solvent may include or be composed of a major portion of kerosene or diesel fuel or other hydrocarbon-based organic solvent, e.g., C10-C14 hydrocarbon. The extractant organic phase may optionally include one or more modifiers and / or additives. The concentration of the one or more metal extractant compound in the extractant organic phase may be 5-50 wt%, e.g., 10-20 wt%. If the concentration of the one or more metal extractant compound in the extractant organic phase is too high, the extractant organic phase may acquire too high a viscosity, either before or after metal loading. If the concentration of the one or more metal extractant compound in the extractant organic phase is too low, the efficiency of metal extraction from an aqueous phase may be too low.Mass transfer of the desired metal(s) can be promoted by generating the emulsion 125 of the aqueous and organic phase with a mechanical mixer. Once mass transfer of the desired metal(s) has taken place, the emulsion 125 can be allowed to separate back into the two respective phases due to inherent immiscibility and density characteristics between aqueous phase and organic solution. The separation into two respective phases can be facilitated by holding in settling vessel 204 (or any other suitable separation apparatus). Extraction of the desired metal(s) can take place in one or more extraction stages. The organic phase leaving the final extraction stage can then be sent to one or more stripping stages 305. The metal-loaded organic can be contacted with a suitable aqueous phase where the desired metal(s) can be stripped from the organic phase back into anaqueous phase. An example of an aqueous strip solution can be a high sulfuric acid containing solution, useful for stripping copper from a salicyaldoxime containing organic phase. The same procedure can be followed for stripping whereby mass transfer can take place at the interface of an emulsion mechanically generated between the organic and strip aqueous phase. The organic, now depleted in the desired metal(s), can be then sent back to the one or more intermediate steps of the extraction process 200. The organic phase leaving the final extraction settler or final strip settler may not be completely devoid of the aqueous phase that it was in contact with. Fine droplets of entrained aqueous can still be present in the settled organic phase. This is problematic, for example, when deleterious elements present in the original leach liquor are physically entrained across from extraction to strip and subsequently contaminate the strip liquor. Examples of such deleterious elements are manganese, chloride, nitrate, arsenic and fluoride that can be present in copper leach and metal solvent extraction processes. The desired metal(s) present in the strip aqueous solution can be recovered by, for example, electrowinning or precipitation, and any deleterious elements can affect the efficiency of the final metal recovery process or contaminate the final product.Another embodiment may include a process comprising selectively extracting Ca from a mother liquor (e.g., the mixture of metals of interest e.g., Li and Ni). The mother liquor is contact with a Ca selective organic extractant solution to thereby load Ca into an organic phase by solvent extraction. The aqueous phase is thus depleted in Ca (termed "raffinate") but may still contain metals of interest (e.g., Ni and Li), which can be separated in subsequent processes. The Ca-loaded organic phase from solvent extraction can be transferred to a stripping step, similar to the stripping step 305, to unload Ca from the organic phase and be removed. The organic phase leaving this stripping step can still contain entrained aqueous material which can contain impurities such as Ca, and, if it is returned back to the solvent extraction step, may increase the impurity level of the mother liquor stream that is processed in the next step, i.e., Ni precipitation. Thus, this kind of stripped organic phase that contains entrained aqueous material may be suitably subjected to electrocoalescence in accordance with embodiments of this disclosure. Examples of organic extractant that can be used in the Ca extraction process are di-(2-ethylhexyl) phosphoric acid (D2EPHA) with formula (CgHnOjzPChH as an extractant (or any other suitable organic extractants). The organic may have a concentration of 30% v / v of D2EPHA. An example oforganic extractants for Li extraction are such lithium selective extractant as an oxime, a trialkylphosphine oxide, an acid, or any combination (or any other suitable Li-selective organic extractants).In an embodiment, the present disclosure provides processes for reducing the aqueous phase in an emulsion derived from a solvent extraction. In an embodiment, the present disclosure provides a process for reducing the aqueous phase in an emulsion where the emulsion is derived from a metal solvent extraction step. Processes disclosed herein can enhance removal efficiency of aqueous phase from the emulsion phase up to about 80% to about 90% compared to conventional removal / separation processes that can remove a small portion of entrained aqueous but not as much as the processes described herein. Advantages of the processes described herein include that the amount / number of impurities that are transferred downstream (for example, to a stripping circuit and in reverse back to an extraction step), are reduced.In an embodiment, the metal solvent extraction step can include providing the aqueous phase containing dilute or impure metal(s) of interest. The metal(s) can include any metals, individually or in combination, for example one or more of nickel, lithium, copper, molybdenum, vanadium, tungsten, cobalt, manganese, zinc, yttrium, lanthanides, actinides and other transition metals susceptible to extraction by an organic extractant.The aqueous phase can be contacted with an immiscible organic phase containing a selective organic extractant. In an embodiment, mass transfer of the desired metal(s) can take place at the interface of the organic phase and aqueous phase. Preferably, droplets of each of these respective phases may be generated by the mixer 208 to facilitate mass transfer. Once mass transfer has taken place, the emulsion can be directed to a settling vessel where the two phases are allowed to separate, for example, based on their density and / or immiscibility characteristics. In an embodiment, the separated phases can be separately forwarded to a subsequent step. At this stage, the separated phases may not be completely devoid of the other phase and in particular, microdroplets of entrained aqueous phase can be transferred with the separated organic phase to a subsequent step, such as stripping.In embodiments of the present disclosure that pertain to solvent extraction, the ratio for initial contact of organic phase to aqueous phase may be 1 : 1 w / w (respectively), or 2: 1 w / w, or 3 : 1 w / w, or 6: 1 w / w, or other ratio. One or more stages of extraction may take place, and it may be performed batchwise, or continuously, or a combination of batchwise and continuous. Typically, there will be a settling tank after the contact of aqueous metal-rich phase with extractant organic phase. That is, once the aqueous metal-rich phase contacts the extractant organic phase, a mixture (e.g., an emulsion) comprising an organic metal-rich phase and an aqueous metal-poor phase. The mixture (e.g., emulsion) is settled in a settling tank to permit a portion of aqueous metal-poor phase to be removed from the mixture to form an aqueous-depleted organic metal-rich phase. The aqueous-depleted organic metal-rich phase is supplied to a electro-coalescence process in an electro-coalescer unit.In an embodiment, the process of the present disclosure may further include stripping the metal from the separated emulsion in a stripping circuit. In an embodiment, the Electro-Coalescer 103 can be installed after the metal solvent extraction step and / or stripping step of an overall extraction process. In an embodiment, the emulsion can be broken down by adding a divalent salt and / or organic modifier (e.g., adding tributyl phosphate or tri decanol to the organic) prior to use of the Electro-Coalescer.In any embodiment of the present disclosure, an electrical conductivity for the aqueous phase of the emulsion may be at or above 70000 pS / cm, owing to salt content. Any embodiment of the present disclosure contemplates the aqueous phase of an emulsion having a room temperature conductivity of greater than about 3000 pS / cm (4000, 5000, 10000, 20000, etc.) , or less than about 80000 pS / cm (less than 70000, 60000, 50000 etc.), or a value in the range of 3000 to 80000 pS / cm, (or in the range of 10000-70000 pS / cm, etc.).Without being limited by theory, the use of porous polymer-coated electrodes may consume less electric current for the various described processes as compared to porous electrodes that do not include the organic polymer. Application of polymers layers may prevent short circuiting between the electrodes and may provide initially large contact angle between droplet and coated porous electrode. Application of an electric field to one or more porous electrodes enhances the wettingproperties of the electrodes, causing the droplet’s contact angle to decrease, hence spreading on the surface, thereby improving the adherence of the aqueous droplets on the surfaces of the porous layers. The porous layers may provide increased surface area for the fluid to contact, thereby giving more area for contact of the dispersed phase droplets. Additionally, the polymeric layers may confer stability against acidic streams that contact the porous electrode. The coating may inhibit corrosion induced by acid streams. In the present disclosure, it is contemplated to contact the porous polymer-coated electrodes with streams having a pH that is sometimes as low as pH from 1 to 4. Corrosion of uncoated electrodes induced by acidic components in the aqueous phase may be especially exacerbated if the holding tank or housing within which the electric coalescence process takes place, is under pressure. However corrosion of uncoated electrodes can also occur even if the emulsion within the holding tank is at atmospheric pressure. Such deleterious situations are mitigated by use of the presently disclosed polymer-coated porous electrodes in an electrocoalescer unit.In many embodiments, the polymeric coating applied to the porous electrode should not inhibit the creation or maintenance of a DC electric field by the respective electrodes of the electrocoalescer unit. In particular if at least one layer of the polymeric coating is a dielectric material, then the electric field should not be inhibited.The present disclosure may further be described in its various aspects, by making reference to any one or more of the following numbered paragraphs:1. A process for reducing an aqueous phase content entrained in an organic phase of an emulsion, including: contacting the emulsion with an electro-coalescer that contains a direct-current (DC) voltage field, wherein the aqueous phase includes fine droplets, and the fine droplets coalesce to form larger droplets, wherein at least some of the fine droplets have a size of less than about 100 micro-meters, separating the larger droplets from the emulsion, wherein the electro-coalescer includes a housing and at least two porous electrodes coated with at least one polymer, and wherein the emulsion is derived from one or more intermediate steps of an extraction process.2. The process of paragraph 1 , wherein the one or more intermediate steps of the extraction process includes a metal solvent extraction step, a wash step, a stripping step, or a combination thereof.3. The process of paragraph 1 or 2, wherein the at least one polymer is a dielectric and hydrophobic polymer.4. The process according to any of paragraphs 1 to 3, wherein the emulsion is a mixture of aqueous and organic phases.5. The process according to any of paragraphs 1 to 4, wherein the emulsion is derived from one of a metal recovery process, a battery material recycling process, a black mass recycle process, or a battery production intermediate and by-product material recovery and recycling process.6. The process according to any of paragraphs 1 to 5, where a solid removal step is optionally used before the Electro-Coalescer to remove at least some particulate matter from the emulsion.7. The process according to any of paragraphs 1 to 6, where there is a cleaning and purging mechanism used to remove solids within the electro-coalescer and to clean the electrodes.8. The process according to any of paragraphs 1 to 7, where a solid removal step is optionally utilized before the electro coalescer to remove particles larger than pores of one or more electrodes disposed within the electro-coalescer.9. The process according to any of paragraphs 1 to 8, where there is a cleaning and purging mechanism used to remove solids within the electro-coalescer and to clean the electrodes.10. The process according to any of paragraphs 1 to 9, wherein the larger droplets have an average size of greater than about 500 micro-meters.11. The process according to any of paragraphs 1 to 10, wherein separating the larger droplets includes settling, sinking, centrifuging, and other methods of separating of droplets from the emulsion.12. The process according to any of paragraphs 1 to 11, wherein the separation of the larger droplet of aqueous phase from the emulsion results in a higher purity product or an intermediate stream.13. The process according to any of paragraphs 1 to 12, wherein the emulsion contains metal ions.14. The process according to any of paragraphs 1 to 13, wherein the one or more intermediate steps of the extraction process includes: providing an aqueous phase containing one or more dilute or impure metals, contacting the aqueous phase with an immiscible organic phase containing a selective organic extractant, transferring the one or more metals at the interface of the fine droplets of organic and aqueous generated by a mixer from the aqueous phase to the organic phase, directing the resulting mixture to a settling vessel where the two phases are allowed to separatebased on their density and / or immiscibility characteristics, and forwarding separated phases to a next step of the extraction process.15. The process according to any of paragraphs 1 to 14, wherein the aqueous phase includes sulfate or chloride.16. The process according to any of paragraphs 1 to 15, wherein the aqueous phase includes nitrate or salts of organic acids.17. The process according to any of paragraphs 1 to 16, wherein the separation of the aqueous phase from the emulsion facilitates the removal of impurities and / or microdroplets from the emulsion.18. The process according to any of paragraphs 1 to 17, wherein the Electro-Coalescer is at a voltage of about 100 V DC to about 500 V DC.19. The process according to any of paragraphs 1 to 18, wherein the Electro-Coalescer is at a voltage of about 100 to about 400 V DC.20. The process according to any of paragraphs 1 to 19, wherein the one or more metal ions are one or more of nickel, lithium, copper, molybdenum, vanadium, tungsten, cobalt, zinc, yttrium, lanthanides, and actinides21. The process according to any of paragraphs 1 to 20, wherein the emulsion is derived from one of oxide copper acid leaching system, secondary sulfide copper acid leaching system, primary sulfide copper acid leaching system, chloride leaching systems, ammonia leaching systems, cyanide leaching systems.22. The process according to any of paragraphs 1 to 21, wherein the one or more intermediate steps of the extraction process includes a metal solvent extraction step and a stripping step, and, wherein metal ions are stripped from the separated larger droplets in a stripping circuit.23. The process according to any of paragraphs 1 to 22, wherein the Electro-Coalescer is installed after a metal solvent extraction step.24. The process according to any of paragraphs 1 to 23, wherein the Electro-Coalescer is installed after the stripping step.25. The process according to any of paragraphs 1 to 24, wherein (i) the Electro-Coalescer can be installed after or before a wash stage within the extraction process, (ii) the number of wash stages can be reduced in the extraction process, or (iii) the Electro-Coalescer can replace one or more wash stages in the extraction process.26. The process according to any of paragraphs 1 to 25, wherein the one or more intermediate steps of the extraction process are part of mining operations.27. The process according to any of paragraphs 1 to 26, wherein the one or more intermediate steps of the extraction process is part of battery recycling operations.28. The process according to any of paragraphs 1 to 27, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 1000 ppm29. The process according to any of paragraphs 1 to 28, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 500 ppm30. The process according to any of paragraphs 1 to 29, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 100 ppm31. The process according to any of paragraphs 1 to 30, wherein prior to the emulsion contacting the Electro-Coalescer, one or more of a monovalent, divalent or multivalent salt and / or an organic modifier is added to the emulsion to speed up the coalescing process.32. The process according to any of paragraphs 1 to 31, wherein separating the larger droplets from the emulsion after contact with the electro-coalescer includes directing the emulsion to a settling vessel and withdrawing the coalesced aqueous stream from the settling vessel.33. The process according to any of paragraphs 1 to 32, where a part of the coalesced aqueous stream is recycled back to raffinate, wastewater, or other step within the extraction process.34. The process according to any of paragraphs 1 to 33, wherein the electro-coalescer can be installed after the stripping step.35. A process for reducing an aqueous phase content entrained in an organic phase of an emulsion, the process comprising: mixing, with a first aqueous phase, a first organic phase comprising at least one extractant compound for extracting at least one target metal, the first organic phase optionally further comprising the at least one target metal, to form an emulsion of the first aqueous phase in the first organic phase; optionally removing at least a portion of the first aqueous phase from the emulsion in a first demixing operation to provide an partially dewatered emulsion of the first organic phase including droplets of residual first aqueous phase; andsubjecting the (optionally partially dewatered) emulsion to an electric field across at least two polymer-coated porous electrodes in an electro-coalescer unit to coalesce relatively fine droplets of residual first aqueous phase into relatively larger droplets and facilitate removal of residual first aqueous phase from the first organic phase, to form a water-depleted second organic phase.36. The process according to paragraph 35, wherein the first organic phase further comprises the at least one target metal.37. The process according to paragraph 36, wherein the first aqueous phase is metal-poor, for stripping the at least one target metal from the organic phase.38. The process according to paragraph 36, wherein the first aqueous phase comprises a stripping agent.39. The process according to paragraph 38, wherein the stripping agent comprises an inorganic acid.40. The process according to paragraph 35, wherein the first organic phase substantially does not comprise the at least one target metal.41. The process according to paragraph 40, wherein the first aqueous phase is metal-rich, for loading the first organic phase with at least one target metal.42. The process according to paragraph 41, wherein the first aqueous phase is metal-rich, and loading the first organic phase with at least one target metal comprises the steps of: providing the first aqueous phase containing the at least one target metal, contacting the first aqueous phase with the first organic phase containing a selective organic extractant, mixing the first aqueous phase and the first organic phase to generate fine droplets of the first organic phase and first aqueous phase to promote transfer of the at least one target metal from the first aqueous phase to the first organic phase, and optionally directing the resulting mixture to a settling vessel where the two phases are allowed to separate based on their density and / or immiscibility characteristics.43. The process according to any of paragraphs 41 to 42, wherein the metal-rich first aqueous phase is derived from ore leaching or recycled battery material leaching.44. The process according to any of paragraphs 35 to 43, wherein polymer-coated porous electrodes comprises at least one polymer coating which includes a dielectric and hydrophobic polymer.45. The process according to any of paragraphs 35 to 44, wherein the polymer-coated porous electrodes comprises at least two polymer layers, at least one of which is a dielectric and at least one of which is a hydrophobic polymer.46. The process according to any of paragraphs 35 to 45, wherein the electro-coalescer unit comprises at least a housing and the at least two polymer-coated porous electrodes.47. The process according to any of paragraphs 35 to 46, wherein the first demixing operation is conducted and comprises settling, sinking, centrifuging, or other methods of demixing.48. The process according to any of paragraphs 35 to 47, wherein the electric field is a direct-current (DC) voltage field, an alternating-current (AC) voltage field, or comprises a combination of DC voltage field and AC voltage field.49. The process according to any of paragraphs 35 to 48, wherein the electric field is a direct-current (DC) voltage field of optionally under 1000 V.50. The process according to any of paragraphs 35 to 49, wherein the emulsion is derived from one of a metal recovery process, a battery material recycling process, a black mass recycle process, or a battery production intermediate and by-product material recovery and recycling process.51. The process according to any of paragraphs 35 to 49, wherein the emulsion is derived from: oxide copper acid leaching system, secondary sulfide copper acid leaching system, primary sulfide copper acid leaching system, chloride leaching systems, ammonia leaching systems, and / or cyanide leaching systems.52. The process according to any of paragraphs 35 to 51, wherein a solid removal step is conducted before subjecting the emulsion to the electric field, to remove at least some particulate matter from the emulsion.53. The process according to any of paragraphs 35 to 52, wherein cleaning and purging is conducted to remove solids from the electro-coalescer unit and to optionally clean the electrodes.54. The process according to any of paragraphs 35 to 53, wherein the relatively larger droplets have an average size of greater than about 500 pm.55. The process according to any of paragraphs 35 to 54, wherein removal of residual first aqueous phase from the first organic phase to form a water-depleted second organic phase comprises one or more of: settling, sinking, centrifuging, or other methods of separating of the relatively larger droplets from the emulsion.56. The process according to any of paragraphs 35 to 55, wherein removal of residual first aqueous phase from the first organic phase to form a water-depleted second organic phase results in a higher purity product or an intermediate stream.57. The process according to any of paragraphs 35 to 56, wherein the first aqueous phase includes sulfate or chloride.58. The process according to any of paragraphs 35 to 57, wherein the first aqueous phase includes nitrate or salts of organic acids.59. The process according to any of paragraphs 35 to 58, wherein the electric field is at a voltage of about 100 V DC to about 500 V DC.60. The process according to any of paragraphs 35 to 59, wherein the electric field is at a voltage of about 100 V DC to about 400 V DC.61. The process according to any of paragraphs 35 to 60, wherein the at least one target metal comprises ions of nickel, lithium, copper, molybdenum, manganese, vanadium, tungsten, cobalt, zinc, yttrium, lanthanides, and / or actinides.62. The process according to any of paragraphs 35 to 61, wherein the aqueous content in the water-depleted second organic phase after contact with the electro-coalescer unit is less than 1000 ppm, preferably less than 500 ppm, more preferably less than 100 ppm.63. The process according to any of paragraphs 35 to 62, wherein prior to subjecting the emulsion to an electric field, one or more of a monovalent, divalent or multivalent salt and / or an organic modifier is added to the emulsion to speed up the coalescing process.64. The process according to any of paragraphs 35 to 63, wherein at least some of the relatively fine droplets have a size of less than about 100 pm.65. The process according to any of paragraphs 35 to 64, wherein mixing the first aqueous phase with the first organic phase is facilitated by a mixer.66. A process for reducing an aqueous phase content entrained in an organic phase of an emulsion formed in one or more steps of a metal solvent extraction, the process comprising:mixing a metal-rich aqueous phase comprising at least one target metal with a first organic phase comprising an extractant compound for the at least one target metal, to facilitate mass transfer of the at least one target metal from the metal-rich aqueous phase to the first organic phase, and form an emulsion of metal-poor aqueous phase in a metal-loaded organic phase; optionally removing at least a portion of the metal-poor aqueous phase from the emulsion in a first demixing operation to provide a partially dewatered emulsion of the metal- loaded organic phase including droplets of residual metal-poor aqueous phase; and subjecting the (optionally partially dewatered) emulsion to an electric field across at least two polymer-coated porous electrodes in an electro-coalescer unit to coalesce relatively fine droplets of residual metal-poor aqueous phase into relatively larger droplets and facilitate removal of residual metal-poor aqueous phase from the metal-loaded organic phase, to form a water- depleted metal-loaded organic phase.67. The process according to paragraph 66, wherein the electric field is a direct- current (DC) voltage field, an alternating-current (AC) voltage field, or comprises a combination of DC voltage field and AC voltage field.68. The process according to paragraph 66 or 67, wherein the electric field is a direct- current (DC) voltage field of optionally under 1000 V.69. The process according to any of paragraphs 66 to 68, wherein the electro-coalescer unit comprises at least a housing and the at least two polymer-coated porous electrodes.70. The process according to any of paragraphs 66 to 69, wherein the first demixing operation is conducted and comprises settling, sinking, centrifuging, or other methods of demixing.71. The process according to any of paragraphs 66 to 70, wherein the metal-rich aqueous phase is formed from the contact of a lixiviant with an ore of the at least one target metal, or is formed from contact of recycled battery materials comprising the at least one target metal with an aqueous acid or base.72. The process according to any of paragraphs 66 to 71 , wherein the extractant compound for the at least one target metal is in a dissolved and / or suspended state in a water-immiscible diluent (such as an organic liquid such as a hydrocarbon liquid such as kerosene) to form the first organic phase.73. A process for reducing an aqueous phase content entrained in a stripped organic phase of an emulsion, the process comprising: mixing a first organic phase comprising at least one extractant compound, the organic phase further comprising the at least one target metal, with a first aqueous phase comprising a stripping agent for stripping the at least one target metal from the organic phase, to form an emulsion of the first aqueous phase in a metal-depleted organic phase; optionally removing at least a portion of the first aqueous phase from the emulsion in a first demixing operation to provide a partially dewatered emulsion of metal-depleted organic phase including droplets of residual first aqueous phase; and subjecting the (optionally partially dewatered) emulsion to an electric field across at least two polymer-coated porous electrodes in an electro-coalescer unit to coalesce relatively fine droplets into relatively larger droplets and facilitate removal of residual first aqueous phase from the first organic phase, to form a water-depleted second organic phase.74. The process according to paragraph 73, wherein the stripping agent comprises an inorganic acid.75. The process according to any of paragraphs 73 to 74, wherein the water-depleted second organic phase is recycled.While the present disclosure has been discussed in terms of certain embodiments, it should be appreciated that the present disclosure is not so limited. The embodiments are explained herein by way of example, and there are numerous modifications, variations and other embodiments that can be employed that would still be within the scope of the present disclosure.It is to be understood that the disclosed subject matter is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The disclosed subject matter is capable of other embodiments and of being practiced and carried out in various ways. The examples set forth in this document are for illustrative purposes and all elements of the example may not be required or exhaustive. Accordingly, other implementations are within the scope of the following claims. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of description and should not be regarded as limiting. As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for thedesigning of other structures, methods, and systems for carrying out the several purposes of the disclosed subject matter. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the disclosed subject matter.Certain embodiments and features have been described using a set of numerical upper limits and a set of numerical lower limits. It should be appreciated that ranges including the combination of any two values, e.g., the combination of any lower value with any upper value, the combination of any two lower values, and / or the combination of any two upper values are contemplated unless otherwise indicated. Certain lower limits, upper limits, and ranges appear in one or more claims below. All numerical values are “about” or “approximately” the indicated values, unless otherwise specifically stated, and take into account experimental error and variations that would be expected by a person having ordinary skill in the art. Accordingly, various embodiments of the disclosure may deviate from the numbers, values, and ranges disclosed herein without departing from the intended scope.Although the term “at least one” or “one or more” may often be used in the specification, claims and drawings, the terms “a”, “an”, “the”, “said”, etc. also signify “at least one,” “one or more,” “the one or more,” or “the at least one” in the specification, claims and drawings.The term “and / or,” as used herein, refers to and encompasses any and all possible combinations of one or more of the associated listed items.Various terms have been defined above. To the extent a term used in a claim is not defined above, it should be given the broadest definition persons in the pertinent art have given that term as reflected in at least one printed publication or issued patent. Furthermore, all patents, test procedures, and other documents cited in this application are fully incorporated by reference to the extend such disclosure is not inconsistent with this application and for all jurisdictions in which such incorporation cam be permitted.Although the disclosed subject matter has been described and illustrated in the foregoing exemplary embodiments, it is understood that the present disclosure has been made only by wayof example, and that numerous changes in the details of implementation of the disclosed subject matter can be made without departing from the spirit and scope of the disclosed subject matter. For example, the steps and / or limitations in the specification, drawings, and / or claims can be performed in an order other than the order set forth in the specification, drawings, and / or claims. In addition, it should be understood that any figures which highlight the functionality and advantages are presented for example purposes only. The disclosed methodology and system are each sufficiently flexible and configurable such that they can be utilized in ways other than that shown. For example, other steps can be provided, or steps can be eliminated, from the described flows, and other components can be added to, or removed from, the described systems. It should be, therefore, expressly understood that such modifications and adaptations can be devised without departing from the basic scope thereof, and the scope thereof can be determined by the claims that follow.Finally, it is the applicant's intent that only claims that include the express language "means for" or "step for" be interpreted under 35 U.S.C. 112(f). Claims that do not expressly include the phrase "means for" or "step for" are not to be interpreted under 35 U.S.C. 112(f).
Claims
CLAIMS1. A process for reducing an aqueous phase content entrained in an organic phase of an emulsion, comprising: contacting the emulsion with an electro-coalescer that contains a direct-current (DC) voltage field; wherein the aqueous phase comprises fine droplets and the fine droplets coalesce to form larger droplets; wherein at least some of the fine droplets have a size of less than about 100 micrometers; separating the larger droplets from the emulsion; wherein the electro-coalescer comprises a housing and at least two porous electrodes coated with at least one polymer; and wherein the emulsion is derived from one or more intermediate steps of an extraction process.
2. The process of claim 1 , wherein the one or more intermediate steps of the extraction process comprises a metal solvent extraction step, a wash step, a stripping step, or a combination thereof.
3. The process of claim 1, wherein the at least one polymer is a dielectric and hydrophobic polymer.
4. The process of claim 1, wherein the emulsion is a mixture of aqueous and organic phases.
5. The process of claim 1, wherein the emulsion is derived from one of a metal recovery process, a battery material recycling process, a black mass recycle process, or a battery production intermediate and by-product material recovery and recycling process.
6. The process of claim 1, where a solid removal step is optionally used before the ElectroCoalescer to remove at least some particulate matter from the emulsion.
7. The process of claim 1, where there is a cleaning and purging mechanism used to remove solids within the electro-coalescer and to clean the electrodes.
8. The process of claim 1, where a solid removal step is optionally utilized before the electro coalescer to remove particles larger than pores of one or more electrodes disposed within the electro-coalescer.
9. The process of claim 1 , where there is a cleaning and purging mechanism used to remove solids within the electro-coalescer and to clean the electrodes.
10. The process of claim 1, wherein the larger droplets have an average size of greater than about 500 micro-meters.
11. The process of claim 1, wherein separating the larger droplets comprises settling, sinking, centrifuging, and other methods of separating of droplets from the emulsion.
12. The process of claim 1, wherein the separation of the larger droplet of aqueous phase from the emulsion results in a higher purity product or an intermediate stream.
13. The process of claim 1, wherein the emulsion contains metal ions.
14. The process of claim 1, wherein the one or more intermediate steps of the extraction process comprises: providing an aqueous phase containing one or more dilute or impure metals, contacting the aqueous phase with an immiscible organic phase containing a selective organic extractant, transferring the one or more metals at the interface of the fine droplets of organic and aqueous generated by a mixer from the aqueous phase to the organic phase; directing the resulting mixture to a settling vessel where the two phases are allowed to separate based on their density and / or immiscibility characteristics, and forwarding separated phases to a next step of the extraction process.
15. The process of claim 1, wherein the aqueous phase comprises sulfate or chloride16. The process of claim 1, wherein the aqueous phase comprises nitrate or salts of organic acids.
17. The process of claim 1, wherein the separation of the aqueous phase from the emulsion facilitates the removal of impurities and / or microdroplets from the emulsion.
18. The process of claim 1, wherein the Electro-Coalescer is at a voltage of about 100 V DC to about 500 V DC.
19. The process of claim 18, wherein the Electro-Coalescer is at a voltage of about 100 to about 400 V DC.
20. The process of claim 13, wherein the one or more metal ions are one or more of nickel, lithium, copper, molybdenum, vanadium, tungsten, cobalt, zinc, yttrium, lanthanides, and actinides21. The process of claim 15, wherein the emulsion is derived from one of oxide copper acid leaching system, secondary sulfide copper acid leaching system, primary sulfide copper acid leaching system, chloride leaching systems, ammonia leaching systems, cyanide leaching systems.
22. The process of claim 1, wherein the one or more intermediate steps of the extraction process comprises a metal solvent extraction step and a stripping step, and, wherein metal ions are stripped from the separated larger droplets in a stripping circuit.
23. The process of claim 22, wherein the Electro-Coalescer is installed after a metal solvent extraction step.
24. The process of claim 22, wherein the Electro-Coalescer is installed after the stripping step.
25. The process of claim 1, wherein (i) the Electro-Coalescer can be installed after or before a wash stage within the extraction process, (ii) the number of wash stages can be reduced in the extraction process, or (iii) the Electro-Coalescer can replace one or more wash stages in the extraction process.
26. The process of claim 1, wherein the one or more intermediate steps of the extraction process are part of mining operations.
27. The process of claim 1, wherein the one or more intermediate steps of the extraction process is part of battery recycling operations.
28. The process of claim 1, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 1000 ppm29. The process of claim 1, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 500 ppm30. The process of claim 1, wherein the aqueous content in the organic after a settling step following contact with the electro-coalescer is less than 100 ppm31. The process of claim 1, wherein prior to the emulsion contacting the Electro-Coalescer, one or more of a monovalent, divalent or multivalent salt and / or an organic modifier is added to the emulsion to speed up the coalescing process.
32. The process of claim 1, wherein separating the larger droplets from the emulsion after contact with the electro-coalescer comprises directing the emulsion to a settling vessel and withdrawing the coalesced aqueous stream from the settling vessel.
33. The process of claim 32, where a part of the coalesced aqueous stream is recycled back to raffinate, wastewater, or other step within the extraction process.
34. The process of claim 2, wherein the electro-coalescer can be installed after the stripping step.