Composition of blend of ultrapure zinc bromide and zinc chloride produced by process of reacting chlorine with mixture of zinc bromide and zinc

Abstract

The present disclosure provides various features of a process for producing an ultrapure zinc bromide and zinc chloride fluid blend having reduced metal impurities for use in battery electrolyte blends by reacting chlorine with a mixture of zinc bromide and zinc in a reactor system. The disclosed process can be used for continuous flow or batch processing and uses an aqueous zinc bromide solution as a catalyst in the reaction with chlorine. The rate at which chlorine is added to the reactor at a controlled rate, either in liquid form or in gas form, reacts with the bromide to generate bromine is much faster than in the absence of the aqueous zinc bromide solution. And then filtering out any unreacted zinc to finally form the ultra-pure zinc bromide and zinc chloride fluid blend.

Description

Technical Field

[0001] The present disclosure generally relates to compositions of zinc bromide and zinc chloride blends produced by reacting chlorine with a mixture of zinc bromide and zinc, the blends having reduced metallic impurities for use in battery electrolyte blends. Background Art

[0002] 1. The need to build better zinc bromide flow batteries

[0003] Energy storage devices (batteries) with high energy density, long cycle life and low cost are the eternal goal to meet the growing needs of portable electronic devices, electric vehicles and renewable energy (see Armand M., Tarascon JM Building better batteries. Nature. 2008; 451: 652–657). The electrolytes added to these energy storage devices act as catalysts to make the battery conductive by promoting the movement of ions from the cathode to the anode during charging and the opposite movement during discharge. Ions are charged atoms that lose or gain electrons. The electrolyte of the battery consists of soluble salts, acids or other bases in liquid, gel and dry forms. Electrolytes also include polymers (such as those used in solid-state batteries), solid ceramics and molten salts (such as sodium-sulfur batteries).

[0004] Among several types of batteries, zinc bromide batteries can be divided into two categories: flow batteries and non-flow batteries. A typical ZnBr2 flow battery consists of two reservoirs for storing ZnBr2 electrolyte, which are connected to a reactor by pumps or pipes (see Ke XY, Prahl JM, Alexander JID, Wainright JS, Zawodzinski TA, Savinell RF Rechargeable redox flow batteries: flow fields, stacks, and design considerations. Chem. Soc. Rev. 2018; 47: 8721–8743). The basic redox reaction in these batteries is summarized in the following equation:

[0005] At the positive electrode:

[0006]

[0007] At the negative electrode:

[0008]

[0009] Overall reaction:

[0010]

[0011] This method of preparing metal bromides from free metals and bromine has been reported in the patent literature. For example, U.S. Pat. No. 4,138,354 to Sochol et al. discloses a method for preparing manganese bromide and cobalt bromide from manganese, cobalt bromide and bromine. The process depends on the redox reaction between manganese and cobalt ions and the subsequent reaction of the produced cobalt with an aqueous bromine solution. U.S. Pat. No. 4,248,850 to Keblys teaches the preparation of metal bromides from alkaline metal compounds and bromine in the presence of formaldehyde as a reducing agent. U.S. Pat. No. 4,514,374 to Kirsch teaches the use of lower alkanols as reducing agents. U.S. Pat. No. 1,483,852 to Rosenstein discloses the production of zinc chloride by reacting a lead-zinc alloy with chlorine in water. Lead metal forms an alloy with zinc metal, and lead acts as a catalyst for the reaction of chlorine with zinc. Chlorine reacts with the zinc-lead alloy to generate zinc chloride. The heat generated by the reaction causes the water to evaporate into steam. The concentration of zinc chloride is controlled by the rate at which water drips or flows through zinc particles in a zinc receiving tube. Rosenstein's disclosure states that the process cannot be performed using pure zinc.

[0012] On the other hand, Farr's U.S. Pat. No. 2,415,346 discloses a process for preparing zinc bromide by reacting zinc chloride with hydrobromic acid at boiling temperature while reacting a metal salt of the MY type with an aqueous medium of hydrogen bromide, wherein M is the desired metal, Y is a halogen of lower atomic weight than bromine, and n is the valence of M. The metal salt is then treated with a substantially equal amount of acid in an aqueous solution containing sufficient water to form an azeotropic mixture. A few years later, San Lorenzo et al. (U.S. Pat. No. 4,401,531) introduced a process for producing electrolytic or high purity zinc from raw materials by hydrometallurgical treatment. San Lorenzo's method discloses leaching at a temperature below 70 degrees Celsius at a pH of 2.5+ / -0.4 for 15-45 minutes; the raw material is placed in an acidic aqueous solution to dissolve the zinc. San Lorenzo then filters the solid / liquid and then extracts using an organic acid. The latter is then stripped in an acidic aqueous solution by washing in two or three stages with another aqueous solution and in the final process the zinc is recovered by electrolytic precipitation or crystallization.

[0013] Following in the footsteps of San Lorenzo, Duyvesteyn et al., (U.S. Pat. No. 4,572,771) disclosed a method for recovering zinc from steel mill dust. Duyvesteyn leached the zinc with a mineral acid, added a solid / liquid separation step, and then neutralized it with lime. The total amount of zinc recovered from the precipitation slurry was about 20%, the total amount of zinc recovered from the alkaline zinc solids was about 48.1%, and the total amount of zinc recovered from the galvanizing ash was about 72% (30% metallic zinc).

[0014] Later, U.S. Pat. No. 6,036,937 to Dunaway (also from the applicant) disclosed a method for producing ZnBr2 by (a) dissolving bromine in an aqueous reaction solvent containing a metal halide salt, and (b) contacting metallic zinc with the resulting bromine solution to form a zinc bromide solution that is substantially free of bromine. Alternative methods for producing zinc bromide have also been disclosed in other patent documents, such as U.S. Pat. No. 8,992,882 to Sauer et al. Again, focusing only on the need for zinc bromide that meets zinc-bromine cell purity standards, Sauer proposed a concise method of combining elemental bromine with at least about 1% molar excess of raw zinc metal to about 10% molar excess of raw zinc metal. The zinc metal raw material will contain metallic impurities including one or more of greater than 500 ppm of Pb, at least 3 ppm of Cu, and at least 1 ppm of Fe, and produce a separable zinc bromide composition including less than 1 ppm of Pb, less than 1 ppm of Cu, and less than 1 ppm of Fe. However, this method again does not touch on another aspect that is truly relevant to the battery electrolyte (i.e., zinc chloride). This is mainly because the zinc chloride is expected to be purchased separately from a third-party supplier. In addition, Sauer's process appears to be costly, slow, and is only done in batch mode, and it has been shown to have difficulty removing heat.

[0015] Variations of the general process described above, including the preparation of other halides such as chlorides and the use of other metals such as zinc, can be found, for example, in US Pat. No. 6,117,408; US Pat. No. 7,087,209; US Pat. No. 9,685,543.

[0016] The key problem of zinc-bromine batteries is that a high-purity zinc bromide solution is required for the battery to work properly. Using a low-cost ZnBr2 source, especially using zinc sulfate and sodium bromide to produce a zinc bromide solution, may cause problems due to the presence of a large amount of iron (Fe) impurities. During each charge and discharge cycle, the energy density of the battery changes, and the impurities in the electrolyte begin to exhibit strong non-conductivity, thus seriously affecting the performance of the battery. This means that if it is expected that the ZnBr2 battery can be operated for a long time, a person of ordinary skill in the art will need to remove these impurities (i.e., Fe). Previous literature shows how to achieve a certain purification of zinc brine by using different concentrations of hydrogen peroxide (see Patil, Anil and Pallavi Managave's "The Effect of Peroxide Concentration when Removing Iron from Brine: A Kinetic Study.", a paper published at the SPE Bergen One-Day Seminar (Bergen, Norway, April 2014)), which is used to prepare a ZnBr2 solution when dissolving zinc sulfate and sodium bromide salts, rather than distilled water. This results in all Fe being oxidized to Fe +3 and precipitate out of solution. However, even with this extra step, the spacing between the electrodes is quite large and the electrode area is small, so there are very large ohmic losses in this type of configuration. This means that it is not useful for charge / discharge cycle data. In fact, typical levels of trace metals observed in commercial battery electrolytes made from readily available mixtures of zinc bromide and zinc chloride show that they contain at least 14 ppm of lead (Pb) and sodium (Na), at least 5 ppm of lithium (Li), at least 2 ppm of calcium (Ca) and boron (B); as well as other impurities that are not conducive to proper battery performance. Their pH levels are typically in the range of 3.5-4.5, the density is between 1.58 and 1.62, and the color is orange / yellow, mainly due to residual bromine.

[0017] 2. Exploration of production methods for ultrapure zinc compounds

[0018] Regardless of the method used historically, the ultimate goal of the electrolytic zinc compound production process is always to obtain zinc of the highest purity.

[0019] For example, the "roast, leach and electrodeposition" (RLE) process "roasts" a zinc sulfide concentrate to produce impure zinc oxide (calcined) and SO2 gas, which is then converted to sulfuric acid. The calcined material is then "leached" with sulfuric acid solution recovered from the "electrowinning" stage. Separation of the leached slurry produces an impure solution, which is then purified by cementing with zinc powder. The purified solution is sent to zinc electrowinning to produce zinc plates, which are then sent to the smelting and casting stages. However, impurity concentration levels low enough to achieve extremely high quality electrowinning, nor ultra-pure zinc, have ever been achieved; unless further processing is carried out, which in turn requires a significant investment of time and money.

[0020] Other common methods use the acid from the leaching step to dissolve the zinc, and then selectively extract the dissolved zinc by an organic acid solvent acting as an extractant. Thereafter, the zinc-laden organic acid is treated to recover the zinc in the form of an aqueous solution and the organic solvent is regenerated for subsequent recycling.

[0021] In typical electrolyte production, ZnBr2, bromine complex additive (BCA) and supporting electrolyte (KBr, ZnCl2) are purchased separately from manufacturers with different specifications and impurities. Therefore, it is difficult to obtain consistent results in battery production. This problem is then solved by making the battery large enough, but still has to face other disadvantages, such as:

[0022] ■While running the electrolyte pump, it is necessary to short the terminals on the low impedance shunt once every 1-4 cycles to completely remove the zinc from the battery plates.

[0023] ■ Low area power during charge and discharge (<0.2W / cm2), which translates into excessively high electricity costs.

[0024] ■ Low round-trip DC-DC efficiency up to 80%, significantly lower than lithium-ion batteries, which are typically 90% or more.

[0025] ■Low energy density (about 42Wh / kg).

[0026] ■Complex structures with moving parts.

[0027] Most typically, zinc chloride suppliers offer up to 99% purity because they obtain this product by mixing zinc and hydrogen chloride. This simplifies purification of the chloride since zinc exists in only one oxidation state, 2+, but still requires battery manufacturers to purify their purchased product by recrystallization from hot dioxane or sublimation in a stream of hydrogen chloride gas and then heating the sublimate to 400 degrees Celsius in a stream of dry nitrogen. ZnCl2 has long been used as an electrolyte in electrochemical devices, but until recently, dilute ZnCl2 electrolytes were used, such as mixed with NH4Cl to obtain the best conductive properties.

[0028] Compared with other dilute zinc electrolytes, dilute ZnCl2 electrolytes can show interesting results. In C. Wang, Z. Pei, Q. Meng et al. Toward flexible zinc-ion hybrid capacitors with superhighenergy density and ultralong cycling life: the pivotal role of ZnCl2 salt-based electrolytes Angew. Chem., 133 (2021), pp. 1003-1010; 2m ZnCl2 has been reported to be based on aqueous Zn 2 + In particular, density functional theory (DFT) studies here show that the desolvation energy of [ZnCl]+ is higher than that of Zn in the electrolyte. 2+ The concept of [ZnCl]+ as a cation carrier is interesting, which leads to the answer to the following question: Zn 2+ Or whether [ZnCl]+ is the actual charge carrier for cathode materials in aqueous batteries operating with ZnCl2 (including its salt-in-water electrolyte) as electrolyte. Further investigation of this issue is necessary.

[0029] As the concentration of ZnCl2 is further increased, the viscosity of the electrolyte increases, thereby reducing ionic conductivity. However, the benefits of higher concentrations (i.e., less "dilute" ZnCl2) may potentially outweigh the disadvantages of reduced conductivity by producing interesting properties. This adds to the issue of ZnCl2 purity, which does not provide certainty to battery manufacturers due to variations in electrochemical properties.

[0030] 3. Cost-effective battery system

[0031] It has been known in the art since 1926 that bromine and zinc do not react directly with each other and require the formation of the intermediates ZnO and HBr.

[0032] As can be seen from the above discussion, zinc-bromine flow batteries, and to a certain extent non-flow batteries, are considered a promising next-generation battery technology due to their low cost, high energy density, and abundant constituent materials. See Li, XJ, Li, TY, Xu, PC, Xie, CX, Zhang, YH, Li, XF, A Complexing Agent to Enable a Wide-Temperature Range Bromine-Based Flow Battery for Stationary Energy Storage. Adv. Funct. Mater. 2021, 31, 2100133. However, zinc-bromine batteries produce severe gas, which degrades electrochemical cycling performance and limits their design because the required electrolyte flow system is expensive. The electrolyte flow system prevents the accumulation of these gases in the battery, which makes the importance of minimizing gas generation reactions rarely addressed. However, in order to give flexibility in battery design and widely accept cost-effective ZnBr2 chemistry in consumer applications (such as pouch type), new strategies to prevent gas generation must be developed. Enter the field of deep eutectic solvent (DES) mixtures.

[0033] DES is Lewis or A eutectic mixture of acid and base, which is widely used in various fields (e.g., separation, synthesis, and electromechanical processes) due to its simple preparation, low cost, low toxicity, and adjustable chemical properties. DES can also be used as an electrolyte for batteries, such as DES-based lithium batteries and organic zinc batteries. See J. Song, Y. Si, W. Guo, D. Wang, Y. Fu, Angew's Organosulfide-Based Deep Eutectic Electrolyte for Lithium Batteries. Chem. Int. Ed. 2021, 60, 9881. The ionic liquid-like ion-conducting properties of DES make it a possible electrolyte material choice; however, DES-based battery technology is still in its infancy. Regarding the possible use of DES in battery applications, particular attention is paid to halide-based DES for zinc bromide batteries, given its potential to provide Br-conduction, high solubility of Br2, and capture ability of Br2.

[0034] In A Zinc–Bromine Battery with Deep Eutectic Electrolytes. Adv. Sci. 2022, 9, 2204908. by Heo, J., Shin, K., Kim, H.-T., DES electrolytes were designed by simply mixing ZnBr2, ZnCl2, and MEPBr. Each DES was prepared by simply mixing the required amounts of ZnBr2, ZnCl2, and MEPBr at 115°C without any further treatment. In order to completely dissolve the parent salts, the DES was stored in an oven for more than three days before use. The final product was in the form of a transparent brown liquid. With the anhydrous nature of the electrolyte and the excellent Br2 adsorption capacity, the zinc bromide battery using this DES can operate in a closed serpentine configuration without producing any gas. Experimental and computational analysis elucidated the reconstruction of MEPBr and the formation of zinc halide complex anions. The addition of Cl- not only affects the mobility of the ions, but also improves the cycle stability and reaction kinetics, resulting in better cycle performance of the DES zinc bromide battery containing Cl-. By taking advantage of the non-gassing properties of BCM DES, a flexible pouch DES zinc bromide battery was successfully demonstrated. However, in this method, the extraction with solvent does not include a purification stage, so organic solvents cannot produce high-purity zinc chloride from zinc bromide without additional MEPBr. In addition, the raw materials supplied are very special, which ultimately makes the process unsuitable for large-scale production.

[0035] Enter the world of carbon-zinc batteries, specifically zinc chloride batteries. Introduced around the 1900s, carbon-zinc batteries, with a slightly acidic electrolyte consisting primarily of zinc chloride in water, provided an economical power source for devices requiring light to moderate drainage, thanks to the use of inexpensive materials and time-proven construction. At the time, they were mostly used in flashlights due to their lack of capacity. As technology evolved, the service life of zinc chloride batteries increased due to the use of purer manganese dioxide, the addition of graphite powder to manganese dioxide to reduce internal resistance, better sealing, and the use of purer zinc in the negative electrode. Their service capacity is not a fixed number of ampere hours, as the efficiency of the battery's operation depends on the conditions imposed on it. Service varies with current consumption, operating schedule, and cut-off voltage. However, these batteries are also affected by operating temperature and storage conditions.

[0036] Today, side reactions between impurities in the zinc chloride anode and the ammonium chloride electrolyte have been shown to increase the self-discharge rate and promote corrosion in the battery. Previously, in order to protect the zinc, the zinc was covered with mercury (Hg) to form an amalgam. Given that this is an environmental hazard, batteries are currently produced without mercury, and manufacturers must now use higher purity zinc to prevent local effects and self-discharge. However, the quest to obtain such a pure zinc chloride product has not been considered successful, and therefore the use of a combination of zinc bromide and zinc chloride in the battery electrolyte is not sufficient to extract all the benefits that zinc chloride batteries bring (for example, continuous use in high-drain applications).

[0037] 4. Use of zinc bromide as a catalyst

[0038] Zinc bromide has been shown to be a simple and effective catalyst for the stereoselective rearrangement of α-hydroxy epoxides to semi-naphthols. See Zinc bromide as catalyst for the stereoselective construction of quaternary carbon: improved synthesis of diastereomerically enriched spirocyclic diols; Yong Qiang Tu et al.; Journal of the Chemical Society, Perkin Transactions 1, 2000, No. 22. The significant appeal of this heterogeneous catalyst is mainly due to economic and environmental considerations (low toxicity) because it is generally cheap and readily available. In addition, it can be conveniently and easily removed from the reaction mixture, making the experimental procedure simple. In recent years, the use of ZnBr2 as a catalyst in the synthesis of organic compounds and heterocyclic molecules has been reported in the literature. Nevertheless, to date, the oil and gas industry has mainly used zinc bromide to replace mud in oil wells, while the electrical and metallurgical industries have used it for electrolysis and catalysis.

[0039] 5. Conclusion

[0040] As can be observed, there is no reference that teaches or suggests a process for producing a mixture of zinc bromide and zinc chloride with controlled purity on a commercial basis on both large (continuous) and small (batch) scales for adequate battery production. Therefore, it is desirable to produce zinc bromide and zinc chloride blends directly in a reactor with inexpensive raw materials. Therefore, these would satisfy the need for an inexpensive and simple process for rapid mass production of zinc bromide and zinc chloride blends with controlled purity levels to achieve consistent electrochemical performance. Summary of the invention

[0041] The present invention seeks to address one or more of the above needs by providing a cost-effective method for producing an ultrapure zinc bromide and zinc chloride blend, using an aqueous zinc bromide solution as a catalyst, which is inefficient to produce without zinc bromide. This represents a key step in accelerating the market adoption of zinc batteries as a more sustainable energy storage system, reducing production costs while providing longer service life and more stable voltage output for the electrolyte battery.

[0042] Where other methods fail, i.e., only produce ultra-high purity zinc bromide, the present disclosure achieves more by reacting chlorine with a mixture of zinc bromide and zinc to produce ultra-pure zinc bromide and zinc chloride blends with reduced metal impurities for use in battery electrolyte blends. The method uses large amounts of zinc bromide along with zinc pellets and chlorine. The zinc bromide acts as a catalyst in the reaction, where the real catalyst would be bromine, which is converted to bromide and then converted back to bromine. The ratio of zinc bromide to zinc chloride is 5:1 to 15:1 ZnBr2 to ZnCl2. Pure zinc metal is added to an aqueous solution of zinc bromide, and chlorine gas is then bubbled through the reaction mixture. Cl2 will react with bromide ions (Br-) in the solution to produce chloride ions (i.e., ZnCl2) and bromine. Bromine will react with zinc metal to produce more ZnBr2. This cycle continues until all the Cl2 is used up. Typically, the direct reaction of Cl2 with zinc in a ZnCl2 solution is very slow, which is why in the present invention Cl2 first reacts with Br- to form bromine, which reacts rapidly with zinc in a ZnBr2 solution.

[0043] In general, at the end of the reaction a mixture of zinc bromide and zinc chloride will be produced, which is controlled by the precise amount of Cl2 added to the reactor. In fact, such a level of control can be implemented that the percentage of ultrapure zinc bromide to zinc chloride can be adjusted between 5% and 95%, depending on the desired utility of the battery. The zinc bromide tail will act as a heat sink for this exothermic reaction. The temperature is usually maintained at around 60 to 80 degrees Celsius. For this ultrapure zinc bromide and zinc chloride blend, the trace metal content in parts per million (ppm) is less than 1 ppm of a trace metal selected from the group consisting of: Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti and V; and less than 10 ppm of a metal selected from the group consisting of Ca, K, Na and Mg; the color is close to water white, and the American Public Health Association Color Standard (APHA) color is less than 11.

[0044] This unique battery hybrid benefits from the use of an ultra-pure zinc bromide and zinc chloride “water-in-salt” electrolyte blend that minimizes Fe dissolution (critical for batteries); it increases the cation insertion potential in the cathode and reduces the anion insertion potential in the anode, thereby amplifying the overall cell voltage with a dilute ZnCl2 electrolyte. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] The teachings of the present invention can be readily understood by considering the following detailed description in conjunction with the accompanying drawings.

[0046] Figure 1 is a simplified flow diagram for continuously producing an ultrapure zinc bromide and zinc chloride fluid blend having reduced metallic impurities for use in a battery electrolyte blend by reacting chlorine with a mixture of bromide and zinc in a reactor system in accordance with an embodiment of the present disclosure;

[0047] Figure 2 A simplified flow diagram is shown for batch production of an ultrapure zinc bromide and zinc chloride fluid blend having reduced metallic impurities for use in a battery electrolyte blend by reacting chlorine with a mixture of bromide and zinc in a reactor system in accordance with an embodiment of the present disclosure;

[0048] Figure 3 A simplified block diagram of a quasi-closed loop continuous stirred reactor system for continuously producing a fluid blend of ultrapure zinc bromide and zinc chloride according to an embodiment of the present disclosure is shown; and

[0049] Figure 4 A simplified block diagram of a quasi-closed loop stirred batch reactor system for batch production of ultrapure zinc bromide and zinc chloride fluid blends according to an embodiment of the present disclosure is shown. DETAILED DESCRIPTION

[0050] 1. Introduction

[0051] Reference will now be made in detail to several embodiments of the present disclosure, examples of which are shown in the accompanying drawings. It should be noted that similar or identical reference numerals may be used in the drawings, where feasible, and may indicate similar or identical functions. The accompanying drawings depict embodiments of the present disclosure for illustrative purposes only. Those skilled in the art will readily recognize from the following description that alternative embodiments of the structures, systems, and methods shown therein may be employed without departing from the principles of the disclosure described herein.

[0052] The subject matter which is regarded as the invention is particularly pointed out and distinctly claimed in the concluding portion of the specification.The invention, however, both as to its organization and method of operation, together with objects, features, and advantages thereof, may be best understood by reference to the following detailed description when read in connection with the accompanying drawings.

[0053] 2. Attached photos

[0054] a. Continuous Stirred Tank Reactor (CSTR)

[0055] The present disclosure describes a method for producing an ultrapure zinc bromide and zinc chloride fluid blend having reduced metal impurities for battery electrolyte blends by reacting chlorine with a mixture of ZnBr2 and zinc in a reactor system. The method 101 Figure 1 The process begins at 102 by determining whether continuous processing or batch processing is required. Figure 3 The continuous stirred tank reactor (CSTR) shown, also known as a barrel reactor or back-mix reactor, is a common ideal reactor type in chemical engineering. CSTR generally refers to a model used to estimate key unit operating variables when using a continuous stirred tank reactor to achieve a specified output. The mathematical model (4) is applicable to all fluids: liquids, gases and slurries. It is well known that the CSTR is one of the systems that exhibits complex behaviors such as steady-state multiplicity, limit cycles and disorder.

[0056]

[0057] where F io is the inlet molar flow rate of substance i, F i is the outlet molar flow rate, v i is the stoichiometric coefficient. The reaction rate, r, generally depends on the reactant concentrations and the rate constant (k). The rate constant can be determined by using the known empirical reaction rate adjusted for temperature using the Arrhenius temperature dependence. In general, as the temperature increases, the rate at which the reaction occurs also increases. The residence time, τ, is the average time that a discrete amount of reagent spends within the tank and is calculated by dividing the volume of the vessel by the volumetric flow rate of the fluid through the system. τ is usually expressed as Denoted as , where V is the volume of reactor 302 and F is the volumetric flow rate of the fluid.

[0058] This initial step is critical to embodiments of the present invention as it is used to determine a series of specifications regarding the reactor system 301. Thereafter, at 103, at least 2,100 kg of zinc is added to the reactor 302 using a solid feeder 308 connected to the reactor 302, and at 104, at least 400 kg of an aqueous zinc bromide solution is added to the reactor using a feed port 305 connected to a piping system 306 and then to the reactor 302. The zinc added at 103 typically includes at least 99.99 wt.% zinc; less than 0.0001 wt.% Al and Cd; at least 0.0002 wt.% Fe; and at least 0.0017 wt.% Pb. The aqueous zinc bromide fluid is typically composed of: less than 1 part per million (ppm) of Pb, Cd, As, Cr, Co, Fe, Ni, Nb, Cu, Rh, Pd, Ag, Mg B, and Al; less than 3 ppm of Hg, V, Mo, and Ru; less than 6 ppm of Li; and less than 8 ppm of Ca. In addition, the pH level of the aqueous zinc bromide fluid is typically 5.5 to 5.6, and the APHA color value is less than 11.

[0059] At 105, piping system 306 and centrifugal circulation pump 307 are used to mix the zinc added at 103 with the aqueous zinc bromide solution added at 104 in reactor 102 at a rate between 75 and 150 liters per minute. This mixing step is circulated through a heat exchanger 309, which obtains water from a reservoir or city connection 310. The heat exchanger 309 is used to adjust the temperature of the reactor to 20 degrees Celsius to 80 degrees Celsius. Water cooling at heat exchanger 309 needs to be carried out at a rate of at least 350 liters per minute so that dissolution (and future reactions) in reactor 302 can occur. Therefore, the cooling capacity of heat exchanger 309 is about 70kW. With the help of centrifugal circulation pump 307, the added aqueous zinc bromide solution is mixed 105 with the added zinc at a flow rate of 75 to 150 liters per minute (LPM).

[0060] At 105, the added zinc is mixed with the added aqueous zinc bromide solution and when the temperature in the reactor is at least 20 degrees Celsius, a step 106 of producing a reaction by adding chlorine to the reactor at a rate of at least 4 kilograms per minute using a piping system when the temperature in the reactor is at least 20 degrees Celsius is performed. Chlorine (which can be in liquid or gaseous form) is added to the reactor 302 at a rate of at least 4 kilograms per minute (kg / min) through the feed port 305 at 106; while being continuously mixed by the centrifugal circulation pump 307, a reaction is produced, as shown in the following equations (5) and (6):

[0061] ZnBr2+Cl2→ZnCl2+Br2 (5)

[0062] Zn+Br2→ZnBr2 (6)

[0063] Once the resulting reaction 106 is proven to be stable, embodiments of the present disclosure allow the addition of chlorine 106 to be gradually increased to 45 kilograms per hour. Then, by continuously adding chlorine at a rate of at least 4 kilograms per minute and mixing the zinc bromide fluid aqueous solution with the added zinc, the reaction 106 will be heated to less than 80 degrees Celsius at 107. Although the heat exchanger 309 will maintain the temperature between the ranges, once the temperature indicator 311 of the reactor 102 reaches 79 degrees Celsius, the chlorine feed 312 will be stopped at 108. Although the chlorine feed 106 will be stopped at 108, zinc will be added to the reactor at 109 using a solid feeder connected to the reactor, and will be dissolved at a rate of at least 40 kilograms per hour to help reduce and maintain the temperature in the reactor 302 below 80 degrees Celsius. At this point, the dissolution indicator sensor in the reactor 302 will determine whether at least 16.4 wt.% zinc chloride has been obtained. Reaching such a level will indicate that the process of the present invention has produced an ultra-pure zinc bromide and zinc chloride fluid blend in the reactor at 110. Thereafter, if the dissolution indicator determines that such minimum wt. % of zinc chloride has not been reached, the disclosed embodiment of the present invention will repeat the following steps at 111: (i) adding at least 2100 kg of zinc to the reactor using a solid feeder connected to the reactor; (ii) adding at least 400 kg of an aqueous zinc bromide solution to the reactor using a feed port connected to a piping system and then connected to the reactor; (iii) mixing the added aqueous zinc bromide solution with the added zinc in the reactor using a centrifugal circulation pump connected to the piping system at a flow rate of between 75 liters and 150 liters per minute; and (iv) when the temperature in the reactor is at least 20 degrees Celsius, using the piping system to pump at least 100 kg of zinc bromide solution into the reactor at a flow rate of at least 100 kg per minute. (v) heating the reaction to less than 80 degrees Celsius by continuously adding chlorine at a rate of at least 4 kilograms per minute and mixing the added aqueous zinc bromide solution with the added zinc; (vi) when the temperature in the reactor reaches 79 degrees Celsius, stopping the addition of chlorine to the reactor at a rate of at least 4 pounds per minute using the piping system; (vii) adding zinc to the reactor at a rate of at least 40 kilograms per hour using a solid feeder connected to the reactor; and (viii) producing an ultrapure zinc bromide and zinc chloride fluid blend in the reactor; until the ratio of the ultrapure zinc bromide and zinc chloride fluid blend produced in the reactor reaches a minimum of 16.4 weight percent zinc chloride in the decanter;

[0064] When the dissolution indicator in reactor 302 determines that a minimum of 16.4 wt. % zinc chloride has been reached, system 301 will begin decanting 112, using a decanting valve 313 connected to reactor 302 to blend the resulting ultrapure zinc bromide and zinc chloride fluid blend into a decanting tank 314 at a maximum rate of 550 kg per hour.

[0065] Thereafter, or in continuous operation with the process cycle described above, and in order to maintain the achieved minimum 16.4 wt.% zinc chloride, the system 301 will begin feeding an aqueous zinc bromide solution into the reactor at 113 using a piping system 306 connected to the reactor 302 at a rate of at least 400 kilograms per hour. Similarly, in continuous operation, the system will begin at 114 decanting the resulting ultrapure zinc bromide and zinc chloride fluid blend from the decanting tank 314 to the storage tank 316 at a flow rate of 75 to 150 liters per minute using a water white fluid pump 315 connected to the decanting tank 302. The storage tank will be composed of a building material, typically in the form of epoxy vinyl ester resins, which have a low styrene content with an optimized epoxy backbone to achieve excellent thermal and corrosion resistance properties. These resins generally have superior stability compared to traditional vinyl ester resins, thereby providing manufacturers with additional flexibility in storage and handling. The storage tanks are then used to meet the demand for the ultrapure zinc bromide and zinc chloride fluid blend of the present invention produced, and their levels will be monitored using submersible level transmitters or sensors with automatic calibration algorithms that provide accurate level readings of the stored ultrapure zinc bromide and zinc chloride fluid blend. This level monitoring system uses wireless ultrasonic sensors to calculate the level of the ultrapure zinc bromide and zinc chloride fluid blend by measuring the distance between the sensor and the surface of the fluid.

[0066] According to an embodiment of the present disclosure, in a continuous stirred tank reactor (CSTR) system 301, to produce an ultrapure zinc bromide and zinc chloride fluid blend at 110, trace amounts of unreacted zinc metal will remain at the bottom of the reactor 302. Therefore, in order to continuously operate the system 301 while maintaining the quality of the ultrapure zinc bromide and zinc chloride fluid blend produced, it is necessary to remove trace amounts of unreacted zinc from the reactor 302 at 115 through a filter. The filter characteristics include a micron rating of 5 μm; an initial efficiency of at least 97%; and a media type polypropylene microfiber material. The polypropylene microfiber contains about 3.5-5.5 square meters of usable filter and also helps to absorb any unwanted trace oil that may leak from the multiple devices used in the present disclosure; thereby ensuring the characteristics of the ultrapure zinc bromide and zinc chloride fluid blend:

[0067] Between 5% and 95% by weight of zinc bromide;

[0068] Between 5% and 95% by weight of zinc chloride;

[0069] Between 2.55% and 48.5% chloride by weight;

[0070] Between 3.55% and 67.45% bromide by weight;

[0071] Between 22.4% and 35.6% zinc by weight;

[0072] Less than 1 ppm of trace metals selected from the group consisting of Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti, and V;

[0073] Less than 10 ppm of metals selected from the group consisting of Ca, K, Na and Mg;

[0074] Density between 16 and 21 ppg measured at 20 degrees Celsius;

[0075] pH levels between -1.7 and 2.0;

[0076] APHA color less than 11; and

[0077] Less than 40 ppm free bromine.

[0078] Finally, in order to maintain the ratio of the ultrapure zinc bromide and zinc chloride fluid blend produced in the reactor at a minimum of 16.4% zinc chloride in the decanter, the continuous stirred tank reactor (CSTR) process repeats the following steps: (i) adding at least 2,100 kg of zinc to the reactor using a solid feeder connected to the reactor; (ii) adding at least 400 kg of aqueous zinc bromide to the reactor using a feed port connected to a piping system and then connected to the reactor; (iii) mixing the added aqueous zinc bromide with the added zinc in the reactor at a rate of between 75 liters and 150 liters per minute using a centrifugal circulation pump connected to the piping system; (iv) generating a reaction by adding chlorine to the reactor at a rate of at least 4 kg per minute using the piping system when the temperature in the reactor is at least 20 degrees Celsius; (v) heating the reaction to 400 °C by continuously adding chlorine at a rate of at least 4 kg per minute and mixing the added aqueous zinc bromide with the added zinc. below 80 degrees Celsius; (vi) when the temperature in the reactor reaches 79 degrees Celsius, stopping the addition of chlorine to the reactor at a rate of at least 4 pounds per minute using the piping system; (vii) adding zinc to the reactor at a rate of at least 40 kilograms per hour using a solid feeder connected to the reactor; (viii) producing an ultrapure zinc bromide and zinc chloride fluid blend in the reactor; (x) using a decanting valve connected to the reactor, decanting the produced ultrapure zinc bromide and zinc chloride fluid blend into a decanting tank at a maximum rate of 550 kilograms per hour; (xi) using a piping system connected to the reactor to add an aqueous zinc bromide solution to the reactor at a rate of at least 400 kilograms per hour; (xii) using a water white fluid pump connected to the decanting tank, decanting the produced ultrapure zinc bromide and zinc chloride fluid blend from the decanting tank to a storage tank at a flow rate of 75 to 150 liters per minute; and (xiii) removing trace amounts of unreacted zinc from the reactor through a filter.

[0079] b.Batch

[0080] Go to Figure 2 , which is shown in 201 Figure 4 A simplified flow diagram of a method for producing an ultrapure zinc bromide and zinc chloride fluid blend by reacting chlorine with a mixture of bromide and zinc in a batch reactor system 401. The produced ultrapure zinc bromide and zinc chloride fluid blend has reduced metal impurities for use in a battery electrolyte blend.

[0081] Chemical production companies have long been seeking better ways to process materials. One of the main topics of debate is batch processing versus continuous flow. The two types of processing may look different in different industries, for example, drug manufacturing in the pharmaceutical industry versus liquid waste processing in the mining industry, but regardless of the application, they have more similarities than differences. Specifically, according to the disclosure of the present invention; batch processing involves grouping bulk materials through each step of the disclosed method. Under batch processing, the processing of subsequent batches must wait until the current batch is processed. However, when demand is small, batch processing or production gives it the advantage of lower initial setup costs and the ability to adjust bulk materials to meet unique supply needs. However, the problem of catalytic reactions still exists, so no technical solution has been proposed to date for producing ultra-pure zinc bromide and zinc chloride fluid blends. The above-mentioned problems have been solved by the specific disclosure of the present invention.

[0082] When producing an ultrapure zinc bromide and zinc chloride fluid blend in a batch production mode as shown at 102, the process begins by adding at least 1500 grams of an aqueous zinc bromide solution to a reactor 402 at 202, and then adding at least 68.1 grams of zinc to the reactor at 203. The solution typically contains 1,500 grams of an aqueous zinc bromide solution, but less than 2,500 grams of an aqueous zinc bromide solution. Thereafter, at 204, mixing of the added at least 1500 grams of an aqueous zinc bromide solution with at least 68.1 grams of zinc is performed using an agitator. Mixing 204 is typically performed by an agitator-type agitator arrangement 403 having an overhead drive unit 405 mounted centrally on a drive shaft 404. Impeller blades 406 are mounted on shaft 404. Mixing 204 will be performed at a rate of 270 to 350 revolutions per minute. A variety of blade designs are used, and typically the blades cover about two-thirds of the diameter of the reactor 407. Thereafter, when the temperature of the reactor reaches at least 20 degrees Celsius, a reaction is produced at 205 by adding chlorine at a rate of less than 5 grams per minute using a stirrer type agitator arrangement 403. Over a period of 30 minutes (to avoid a sudden increase in temperature), when the temperature of the reactor 402 reaches 20 degrees Celsius, at least 80.1 grams of chlorine (in liquid form or gaseous form) are added at a rate of 5 grams (gr) per minute (min) at 205 through an inlet pipe 410. The 205 produces a reaction at 205 by adding less than 80.1 grams of chlorine at a rate of less than 5 grams per minute when the temperature of the reactor has reached 20 degrees Fahrenheit; while continuously mixing 204, the produced reaction is heated 206 to less than 80 degrees Celsius by continuously adding chlorine at a rate of less than 5 grams per minute. In order to keep the temperature within range and avoid reaching the boiling point of any element in the reactor 402, a combination of a coil condenser 408 is used to insert cooler air, while a circulator 409 is used to extract and dissipate any hot air around the reactor 402. An outlet tube 411 connected to the reactor 402 helps to dissipate or remove any gas that accumulates therein.

[0083] When the temperature of the thermocouple 407 detects that the reaction temperature has reached 79 degrees Celsius, the addition of chlorine at a rate of less than 5 grams per minute is stopped at 207 when the temperature in the reactor reaches 79 degrees Celsius at 208 for a maximum of 14 hours. Thereafter, the addition of zinc bromide aqueous solution and zinc with the added chlorine is stopped at 209 and mixed at 18 hours. The ultrapure zinc bromide and zinc chloride fluid blend in the reactor 402 will be produced at 210, and traces of unreacted zinc metal will be removed from the reactor 402 at 211 using a Buchner funnel under vacuum through a glass microfiber filter. The filter includes: a filtration rate of 41 seconds; an air flow rate of 2.6s / 100ml / in 2 ; Basis weight is 121g / m 2; maximum operating temperature of 550°C; particle retention in liquid of 2.7 μm; thickness of 675 μm; water flow rate of 681 ml / min; and diameter of at least 7 mm. In batch processing, this provides the following properties for ultrapure zinc bromide and zinc chloride fluid blends:

[0084] Between 5% and 95% by weight of zinc bromide;

[0085] Between 5% and 95% by weight of zinc chloride;

[0086] Between 2.55% and 48.5% chloride by weight;

[0087] Between 3.55% and 67.45% bromide by weight;

[0088] Between 22.4% and 35.6% zinc by weight;

[0089] Less than 1 ppm of trace metals selected from the group consisting of Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti, and V;

[0090] Less than 10 ppm of metals selected from the group consisting of Ca, K, Na and Mg;

[0091] Density between 16 and 21 ppg measured at 20 degrees Celsius;

[0092] pH levels between -1.7 and 2.0;

[0093] APHA color less than 11; and

[0094] Less than 40 ppm free bromine.

[0095] 4. Examples of test results

[0096] For comparison purposes of the present disclosure, a baseline was established using commercially available zinc chloride from Spectrum Mfg., etc. A 75.5 wt.% aqueous zinc bromide solution from Company A was used and mixed in the same manner as described in the present disclosure, specifically Figure 2 and use Figure 4 The fluid properties of the resulting zinc bromide and zinc chloride fluid blend were: 4.04 wt.% Cl; 48 wt.% Br; 23 wt.% Zn; pH of -0.56; and 0 ppm Br2. The ICP metal ppm was mostly less than 1, except for Ca, K, Na, and Si between 1 and 4 ppm.

[0097] Following the same batch processing, at least four different examples were performed considering that the main chemical reactions expected were (5) and (6).

[0098] The ranges of charge, molarity and weight used are described in the table below. Likewise, the ranges of final solution masses, including the mass of unreacted zinc and the weight of the filtrate, are:

[0099] Charge Moore Theoretical charge (g) Actual weight zinc pills 1.04-3 68.1-196.14 68.77-205.87 <![CDATA[75.5 wt.% of ZnBr2]]> 5.1 1531 1532.41-1539.2 water 16.7 300 250–287.25 <![CDATA[Cl2]]> 1.00 71.9 71 Final solution mass 1921-1971 1924-2101.58 Unreacted Zn 1.83-137.99 Filtrate weight 1851-1933.43

[0100] The resulting properties of ultrapure zinc bromide and zinc chloride fluid blends for four examples using the process of the present disclosure are shown in the following table:

[0101] Examples Density at 60F, ppg Cl,％ Br,％ Zn, % pH <![CDATA[Br2ppm]]> 1 17.40 3.3825 43.3749 20.892 1.04 40 2 16.84 4.009 41.3336 20.565 0.76 28 3 16.79 3.6814 41.6979 20.421 0.98 0 4 16.79 3.7754 41.6594 20.549 1.03 0

[0102] Finally, a comparative example is performed to show when there is no aqueous zinc bromide solution in the reactor. The reaction system is thoroughly cleaned before the reaction to eliminate any bromine / bromide species involved in the previous reaction. For this experiment, the zinc chloride feed was prepared by dissolving 1,020 grams of zinc chloride in 1,020 grams of water; therefore, the concentration of the feed was 50.0% (by weight). In fact, 100 grams of chlorine was injected into the mixture of zinc pellets and zinc chloride over 42 minutes (2.38 g / min) while stirring at about 350 rpm and under coolant circulation at 52 degrees Celsius. At the end of the chlorine injection, the temperature rose by 4.3 degrees Celsius and then dropped again. During the chlorine injection, the color of the reaction changed from water white to light yellow, and turned water white again after stirring for 85 minutes. The reaction mixture was cooled to room temperature and left to stand overnight, after which the zinc pellets were removed and weighed, and a liquid sample was submitted for analysis. At the end of the process in this example, theoretical analysis showed that:

[0103] Based on the weight of zinc reacted, there should be:

[0104] (276.33-254.98) / 65.38=0.327 mol (7)

[0105] The ZnCl2 formed should be:

[0106] 0.327 mol x 136.29 g / mol = 44.50 g (8)

[0107] The actual consumption of Cl2 should be:

[0108] 0.327 mol x 70.91 g / mol = 23.15 g (9)

[0109] The escaped Cl2 should be:

[0110] 100.0-23.15=76.85g (10)

[0111] Therefore, the total of all ingredients (in grams) should be:

[0112] ZnCl2 zinc pills Cl2 total 2040.00 276.33 100 2416.33

[0113] Nevertheless, the mass collected after treatment (in grams) totals 2265.98 grams, divided into 2011 grams of filtrate and 254.98 grams of dried zinc. The total loss is therefore equivalent to 105.35 grams (2265.98-2416.33).

[0114] Since 21.35 grams of zinc were consumed, the newly formed zinc chloride should be 44.50 grams, which will produce a zinc chloride concentration of (44.50+1,020) / (44.50+2,040)=51.07% after the reaction.

[0115] In contrast, the Cl-% value of 26.2 obtained from the IC analysis indicated that the ZnCl2% should be 50.36%, which means that 14.71 grams of zinc chloride were formed from the reaction of 7.06 g zinc and 7.65 g chlorine.

[0116] The Zn% value obtained from the ICP analysis is 24.3, indicating that the ZnCl2% should be 50.65%. Since zinc may associate with other anions in the solution, some of which may be derived from chlorine, the concentration of zinc chloride calculated based on zinc cations or consumed zinc metal may be higher than the concentration of zinc chloride actually formed. Therefore, the value of Cl-% should be the most accurate data. Therefore, the Cl-% obtained from the IC analysis shows that the total zinc chloride concentration increased by 0.36% after the reaction. This means that 14.71g of zinc chloride is formed by the reaction of 7.06g of zinc and 7.65g of chlorine. Compared with the total amount of 276g of zinc pellets and 100g of chlorine added to the reactor, the extent of the reaction between zinc and chlorine is very small (7.65 / 100=7.65%). Side reactions may exist, but the extent may be equally small.

[0117] The final characteristics of this instance are as follows:

[0118] Density at 60F, ppg Cl-％ <![CDATA[Br - %]]> Zn% pH Free bromine, ppm 13.10 26.2 <0.1 24.3 2.56 Not Detected

[0119] Mass balance calculation:

[0120] 4. Abbreviations and definitions not defined elsewhere

[0121] It is noted here that, as used in this specification and the appended claims, the singular forms "a / an" and "the" include plural referents unless the context clearly dictates otherwise. Similarly, since gerunds are derived from their respective verb forms, they include their word references and verbs include gerunds unless the context clearly dictates otherwise.

[0122] Unless otherwise indicated, all percentages, parts and ratios are based on the total weight of the compositions of the present invention. All such weights associated with listed ingredients are based on the active level and, therefore, do not include solvents or by-products that may be included in commercially available materials, unless otherwise indicated. The term "weight percent" may be expressed herein as "wt. %". Unless otherwise indicated, all molecular weights used herein are weight average molecular weights expressed in grams per mole.

[0123] As used herein, "aqueous solution", "aqueous fluid solution" or "aqueous fluid" is generally a solution composed of water and ions, atoms or molecules that have lost or gained electrons, and is electrically conductive. "Zinc bromide aqueous fluid" includes at least 25 wt.% water (based on the weight of zinc bromide), trace metals selected from the group consisting of Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti and V in a purity of less than 1 ppm; and less than 10 ppm of metals selected from the group consisting of Ca, K, Na and Mg;

[0124] Although the present disclosure has been described in conjunction with certain preferred embodiments of the present disclosure in the foregoing description, and many details have been set forth for the purpose of illustration, the present invention should not be unduly limited to the foregoing contents set forth for the purpose of illustration. On the contrary, various modifications and alternative embodiments will be apparent to those skilled in the art, as defined in the claims set forth below, without departing from the true scope of the present invention. In addition, it should be understood that the structural features or method steps shown or described in any one of the embodiments herein may also be used in other embodiments. References to "one embodiment" or "embodiment" and variations thereof throughout the specification mean that the specific features, structures or characteristics described in conjunction with the embodiment are included in at least one embodiment. Therefore, the phrases "in one embodiment" or "in an embodiment" appearing in various places in this specification do not necessarily all refer to the same embodiment.

[0125] As used herein, "and / or" placed between a first entity and a second entity refers to one of the following: (a) a first entity, (b) a second entity, and (c) a first entity and a second entity. Multiple elements listed with "and / or" should be interpreted in the same manner, i.e., "one or more elements" of the elements so combined. In addition, the terms "including", "consisting of", "comprising", and "having" as used in the claims and description herein should be considered to indicate an open group that may contain unspecified other elements. The terms "one", "an", and words in the singular form should be considered to contain plural forms of the same word, so that these terms mean that one or more something is provided. The terms "one" or "single" can be used to indicate that one and only one of something is meant. Similarly, when a specific number of things is meant, other specific integer values, such as "two", can be used.

[0126] Unless otherwise stated, when a range of any type is disclosed or claimed, it is intended to be disclosed or claimed individually every possible number that the range could reasonably encompass, including any sub-ranges encompassed therein.

Claims

1. A method for producing an ultrapure zinc bromide and zinc chloride fluid blend having reduced metallic impurities for use in a battery electrolyte blend by reacting chlorine with a mixture of zinc bromide and zinc in a reactor system, the method comprising the steps of: (i) adding at least 2100 kg of zinc to the reactor using a solid feeder connected to the reactor; (ii) adding at least 400 kg of an aqueous solution of zinc bromide to the reactor using a feed port connected to a piping system and in turn to the reactor; (iii) mixing the added aqueous zinc bromide solution with the added zinc in the reactor at a flow rate of between 75 liters and 150 liters per minute using a centrifugal circulation pump connected to the piping system; (iv) producing a reaction by adding chlorine at a rate of at least 4 kg per minute to the reactor using the piping system when the temperature in the reactor is at least 20 degrees Celsius; (v) heating the reaction to less than 80 degrees Celsius by continuously adding chlorine at a rate of at least 4 kilograms per minute and mixing the added aqueous zinc bromide solution with the added zinc; (vi) when the temperature in the reactor reaches 79 degrees Celsius, stopping the use of the piping system to add chlorine to the reactor at a rate of at least 4 pounds per minute; (vii) adding zinc to the reactor at a rate of at least 40 kg per hour using the solid feeder connected to the reactor; (viii) producing an ultrapure fluid blend of zinc bromide and zinc chloride in said reactor; (ix) repeating steps (iii) to (viii) until the ratio of the ultrapure zinc bromide and zinc chloride fluid blend produced in the reactor reaches a minimum of 16.4% zinc chloride in the decanter; (x) decanting the resulting ultrapure zinc bromide and zinc chloride fluid blend into a decanting tank at a maximum rate of 550 kg per hour using a decanting valve connected to the reactor; (xi) adding the aqueous zinc bromide solution to the reactor at a rate of at least 400 kilograms per hour using the piping system connected to the reactor; (xii) decanting the resulting ultrapure zinc bromide and zinc chloride fluid blend from the decanting tank to a storage tank at a flow rate of 75 to 150 liters per minute using a water-white fluid pump connected to the decanting tank; (xiii) removing trace amounts of unreacted zinc from the reactor via a filter; and (xiv) repeating steps (iii) to (viii) and (x) to (xiii) to maintain the ratio of the ultrapure zinc bromide and zinc chloride fluid blend produced in the reactor to a minimum of 16.4% zinc chloride in the decanter tank.

2. The method of producing an ultrapure zinc bromide and zinc chloride fluid blend in a reactor system according to claim 1, wherein the reactor system further comprises: a heat exchanger connected to the reactor via the piping system and the pump, the reactor having the solid feeder for adding the zinc, the piping system for adding the aqueous zinc bromide solution and the chlorine, and the pump for mixing the aqueous zinc bromide solution; a decanting valve connected to the reactor and the decanting tank; a water-white fluid pump connected to the decanting tank and the storage tank; and and a control system for performing the steps of adding, mixing, generating, heating, stopping and removing.

3. The process for producing ultrapure zinc bromide and zinc chloride fluid blend in a reactor system as claimed in claim 1, wherein in the step of producing a reaction by adding chlorine to the reactor at a rate of at least 4 kg per minute using the piping system when the temperature in the reactor is at least 20 degrees Celsius, the chlorine can be in liquid form or in gaseous form.

4. The method for producing an ultrapure zinc bromide and zinc chloride fluid blend in a reactor system according to claim 1, wherein in the step of producing an ultrapure zinc bromide and zinc chloride fluid blend in the reactor, the ultrapure zinc bromide and zinc chloride fluid blend further comprises: Zinc bromide between 5% and 95%; Between 5% and 95% zinc chloride; Between 2.55% and 48.5% chloride by weight; Between 3.55% and 67.45% bromide by weight; Between 22.4% and 35.6% zinc by weight; Less than 1 ppm of trace metals selected from the group consisting of Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti, and V; Less than 10 ppm of metals selected from the group consisting of Ca, K, Na and Mg; Density between 16 and 21 ppg measured at 70 degrees Fahrenheit; pH levels between -1.7 and 2.0; APHA color less than 11; and Less than 40 ppm free bromine.

5. The method for producing an ultrapure zinc bromide and zinc chloride blend in a reactor system according to claim 1, wherein the filter in the step of removing trace amounts of unreacted zinc from the reactor through a filter further comprises: The micron rating is 5μm; Initial efficiency is at least 97%; as well as Medium polypropylene microfiber material.

6. A method for producing an ultrapure zinc bromide and zinc chloride fluid blend having reduced metallic impurities for use in a battery electrolyte blend by reacting chlorine with a mixture of zinc bromide and zinc in a reactor system, the method comprising the steps of: (i) adding at least 1500 grams of aqueous zinc bromide solution to a reactor; (ii) adding at least 68.1 grams of zinc to the reactor; (iii) mixing the added at least 1500 grams of aqueous zinc bromide solution with the at least 68.1 grams of zinc using a stirrer; (iv) when the temperature of the reactor reaches at least 20 degrees Celsius, using the agitator to cause a reaction by adding chlorine at a rate of less than 5 grams per minute; (v) heating the resulting reaction to less than 80 degrees Celsius by continuously adding chlorine at a rate of less than 5 grams per minute; (vi) when the temperature in the reactor reaches 79 degrees Celsius for a maximum of 14 hours, stopping the addition of chlorine at a rate of less than 5 grams per minute; (vii) stopping mixing the aqueous zinc bromide solution and the zinc with the added chlorine at 18 hours; (viii) producing an ultrapure fluid blend of zinc bromide and zinc chloride in said reactor; and (ix) Traces of unreacted zinc metal were removed from the reactor under vacuum using a Buchner funnel through a glass microfiber filter.

7. The method of producing an ultrapure zinc bromide and zinc chloride fluid blend in a reactor system according to claim 6, wherein the reactor system further comprises a coil condenser for maintaining the temperature below 80 degrees Celsius, a thermocouple for measuring the temperature inside the reactor, a circulator for exchanging air, an inlet pipe for adding chlorine to the reactor, an outlet pipe for removing accumulated gas in the reactor, and a control system for performing the adding, mixing, generating, heating, stopping and removing steps.

8. The method of producing an ultrapure zinc bromide and zinc chloride fluid blend in a reactor system according to claim 6, wherein the step of mixing said added at least 1500 grams of aqueous zinc bromide solution with said at least 68.1 grams of zinc using an agitator is performed by said agitator at a speed of 270 to 350 revolutions per minute.

9. The method of producing an ultrapure fluid blend of zinc bromide and zinc chloride in a reactor system according to claim 6, wherein the step of producing a reaction using the agitator by adding chlorine at a rate of less than 5 grams per minute is performed in a period of less than 30 minutes when the temperature of the reactor reaches at least 20 degrees Celsius.

10. The method for producing an ultrapure zinc bromide and zinc chloride fluid blend in a reactor system according to claim 6, wherein in the step of producing the ultrapure zinc bromide and zinc chloride fluid blend in the reactor, the ultrapure zinc bromide and zinc chloride fluid blend further comprises: Zinc bromide between 5% and 95%; Between 5% and 95% zinc chloride; Between 2.55% and 48.5% chloride by weight; Between 3.55% and 67.45% bromide by weight Less than 1 ppm of trace metals selected from the group consisting of Ag, Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Fe, Li, Mn, Mo, Nb, Ni, P, Pb, Sb, Se, Si, Sn, Sr, Ti and V; Less than 10 ppm of metals selected from the group consisting of Ca, K, Na and Mg; Density between 16 and 21 ppg measured at 70 degrees Fahrenheit; Between 22.4% and 35.6% zinc by weight; pH levels between -1.7 and 2.0; APHA color less than 11; and Less than 40 ppm free bromine.

11. The method of producing ultrapure zinc bromide and zinc chloride blend in a reactor system according to claim 6, wherein the filter in the step of removing trace amounts of unreacted zinc metal from the reactor through a glass microfiber filter using a Buchner funnel under vacuum further comprises: The filtration speed is 41 seconds; The airflow rate is 2.6s / 100ml / in2; Basis weight: 121g / m 2 ; The maximum operating temperature is 550℃; Particle retention in liquid is 2.7 μm; Thickness: 675 μm; The water flow rate is 681 ml / min; and The diameter is at least 7 mm.

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