Apparatus for cleaning electrolyte injector

Abstract

An injector cleaning system for use with an electrolyte injection system is disclosed. The cleaning system includes condensing container that contains a cleaning solution. The condensing container is constructed to circulate the cleaning solution through the injection system to remove contaminants. The cleaning system also includes a distillation container that is constructed to collect the contaminated cleaning solution within the injection system. The distillation container boils the contaminated cleaning solution to create a cleaning solution vapor and then transfers the vapor to the condensing container, where the vapor is condensed into a cleaning solution for re- circulation through the injection system.

Description

[0001] APPARATUS FOR CLEANING ELECTROLYTE INJECTOR

[0002] CROSS-REFERENCE TO RELATED APPLICATIONS

[0003]

[0001] This application is related to the following applications and patents, each of which is hereby incorporated by reference in its entirety: US 10,608,284 issued on 3 / 31 / 20; US 10,998,143 issued on 5 / 4 / 21; US 10,784,532 issued on 9 / 22 / 20; US 11,088,396 issued 8 / 10 / 21; US 10,873,070 issued on 12 / 22 / 2020; US 11,342,615 issued on 5 / 24 / 22; PCT / US20 / 26086 filed on 4 / 1 / 2020; PCT / US22 / 31594 filed on 5 / 31 / 22; PCT / US23 / 11864 filed on 1 / 30 / 23; PCT / US23 / 17720 filed on 4 / 6 / 2023; PCT / US23 / 28104 filed on 7 / 19 / 23; PCT / US23 / 28105 filed on 7 / 19 / 23; PCT / US23 / 35766 filed on 10 / 24 / 23; PCT / US24 / 16784 filed on 2 / 21 / 23; PCT / US24 / 18746 filed on 3 / 6 / 24; PCT / US24 / 16784 filed on 2 / 21 / 24; PCT / US24 / 25771 filed on 4 / 23 / 24; US Application 63 / 418703 filed on 10 / 24 / 22; US Application 63 / 461252 filed on 4 / 22 / 23; US Application 63 / 461387 filed on 4 / 24 / 23; US Application 63 / 470174 filed on 5 / 31 / 23; US Application 63 / 534213 filed on 8 / 22 / 23; US Application 63 / 450745 filed on 3 / 8 / 23; and US Application 63 / 652616 filed on 5 / 28 / 24

[0004] FIELD OF THE INVENTION

[0005]

[0002] Embodiments of the invention relate to a system for cleaning an electrolyte injection system using a liquefied gas solvent as a cleaning fluid.

[0006] BACKGROUND OF THE INVENTION

[0007]

[0003] Conventional battery cells use a liquid-based electrolyte to transfer charge between the positive and negative electrodes. These electrolytes are often composed of a salt and a solvent. The salt may be of a lithium type or another type of cation such as sodium, potassium, etc. The solvent may use a carbonate, ester, nitrile, ether, phosphate, or other liquid-based solvents. The solvent may also comprise a liquefied gas solvent such as methyl fluoride, difluoromethane, difluoroethane, etc. Most often these are organic liquid electrolyte solutions that are highly sensitive to moisture and are thus used in a dry room environment when injecting cells with the electrolyte to avoid atmospheric contamination.

[0004] To maintain high purity of electrolyte injected into the cell, and to ensure consistency and accuracy from fill to fill, the electrolyte injection system’s wetted components must be frequently cleaned. For example, the salt may be highly corrosive to metals when exposed to small amounts of moisture; thus, it is imperative to frequently clean electrolyte injector components to remove potentially corrosive materials from damaging the components. This can be a frequent cleaning step between each individual cell fill or a more infrequent cleaning step performed between groups of cells. The cleaning fluid is often dimethyl carbonate, used because it efficiently cleans the salt and solvent components and is non-toxic and low-cost.

[0008]

[0005] The problem, however, is that the cleaning fluid is easily contaminated with residual electrolyte and cannot be reused for further cleaning. Thus, in the current state of the art, the contaminated fluid is collected and disposed of as hazardous waste, adding to the high cost of the cleaning step. The cleaning process can also be inefficient with the time involved in switching tanks of cleaning fluids, reducing throughput and increasing cost. The cleaning fluids may also be highly flammable, as is the case with dimethyl carbonate, leading to a fire hazard and lowering safety of the overall system.

[0009]

[0006] A new cleaning system is disclosed herein which reduces waste, improves safety and reduces maintenance cost. This cleaning system uses a liquefied gas solvent as a cleaning fluid to flush the electrolyte injector system. The cleaning fluid picks up contaminates and is itself collected after cleaning the electrolyte injector system. The contaminated cleaning fluid that is collected may then be evaporated off, leaving behind the solid or low vapor pressure components. The evaporated components may then be purified and reused to clean the system again.

[0010] SUMMARY OF THE INVENTION

[0011]

[0007] An injector cleaning system for use with an electrolyte injection system is disclosed. The cleaning system includes a condensing container that contains a cleaning solution. The condensing container is constructed to circulate the cleaning solution through the injection system to remove contaminants. The cleaning system also includes a distillation container that is constructed to collect the contaminated cleaning solution within the injection system. The distillation container boils the contaminated cleaning solution to create a cleaning solution vapor and transfers the vapor to the condensing container, where the vapor is condensed into a cleaning solution for recirculation through the injection system.

[0008] The cleaning system may have a plurality of valves constructed and positioned to selectively circulate the cleaning solution to certain components of the injection system. A valve may be positioned between the condensing container and the electrolyte injection system to regulate the flow of the cleaning solution into injection system. Another valve may be positioned between the distillation container and the injection system to regulate the flow of the contaminated cleaning solution into the distillation container.

[0012]

[0009] The distillation container may have a heater / cooler that assists in boiling the contaminated cleaning solution. The condensing container may have a heater / cooler that assists in condensing the cleaning solution vapor. A fluid circulation pump may be used that creates a pressure differential within the injector cleaning system that assists in boiling the contaminated cleaning solution and in condensing the cleaning solution vapor. A vacuum pump may be used to vent the cleaning system.

[0013]

[0010] The cleaning system may have an absorbent / desiccant container containing an absorbent / desiccant fluidly connected to the distillation container and to the condensing container. A regeneration gas container may be used to pass / circulate a gas through the absorbent / desiccant container to dry the absorbent / desiccant container. The absorbent / desiccant container may also have a heater / cooler.

[0014] [Oi l] The distillation container and / or the condensing container may contain an absorbent / desiccant. The distillation container and / or the condensing container may have a window sight. A spectrometer may be used to measure the spectral characteristics through either one or both window sights.

[0015]

[0012] The cleaning solution may be a liquified gas. Examples of such a liquified gas include, fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1,1 -difluoroethane, 1,2-difluoroethane, 1,1,1 -trifluoroethane, 1,1,2- trifluoroethane, 1,1,1,2-tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chloride fluoride, phosphoryl fluoride, phosphoryl chloride fluoride, sulfuryl fluoride, sulfuryl chloride fluoride, 1-fluoropropane, 2- fluoropropane, 1,1 -difluoropropane, 1,2-difluoropropane, 2,2-fluoropropane, 1,1, 1- trifluoropropane, 1 , 1 ,2-trifluoropropane, 1,2,2-trifluoropropane, fluoroethylene, cis-1,2- fluoroethylene, 1,1 -fluoroethylene, 1 -fluoropropylene, 2-propylene, chlorine, chloromethane, bromine, iodine, ammonia, methyl amine, dimethyl amine, trimethyl amine, molecular oxygen, molecular nitrogen, carbon monoxide, carbon dioxide, sulfur dioxide, dimethyl ether, methyl vinyl ether, difluoro ethylene, nitrous oxide, nitrogen dioxide, nitrogen oxide, carbon disulfide, hydrogen fluoride, hydrogen chloride, methane, ethane, propane, butane, ethylene, propylene, butylene, and any combination thereof.

[0016]

[0013] Additional aspects, alternatives and variations, as would be apparent to persons of skill in the art, are also disclosed herein and are specifically contemplated as included as part of the invention. The invention is set forth only in the claims as allowed by the patent office in this or related applications, and the following summary descriptions of certain examples are not in any way to limit, define or otherwise establish the scope of legal protection.

[0017] BRIEF DESCRIPTION OF THE DRAWINGS

[0018]

[0014] The invention can be better understood with reference to the following figures. The components within the figures are not necessarily to scale, emphasis instead being placed on clearly illustrating example aspects of the invention. In the figures, like reference numerals designate corresponding parts throughout the different views and / or embodiments. Furthermore, various features of different disclosed embodiments can be combined to form additional embodiments, which are part of this disclosure. It will be understood that certain components and details may not appear in the figures to assist in more clearly describing the invention.

[0019]

[0015] FIG. 1A illustrates an injection system and a cleaning system in a configuration to fill electrolyte into a battery / electrochemical cell.

[0020]

[0016] FIG. IB illustrates a neat cleaning fluid circuit that cleans specific components of the injection system.

[0021]

[0017] FIG. 1C illustrates a neat cleaning fluid circuit that cleans all the components of the injection system.

[0022]

[0018] FIG. 2 illustrates a cleaning system with an absorbent / desiccant container to further purify the cleaning fluids.

[0023]

[0019] FIG. 3 illustrates a cleaning system where the neat cleaning fluid container and the absorbent / desiccant container are the same container.

[0024]

[0020] FIG. 4 illustrates a cleaning system where the absorbent / desiccant container and the contaminated cleaning fluid container are the same container.

[0021] FIG. 5 illustrates a cleaning system where the contaminated cleaning fluid container is relocated closer to the injection port.

[0025]

[0022] FIG. 6 illustrates a cleaning system with a cell emulator to clean the injection port more efficiently.

[0026]

[0023] FIG. 7A illustrates a cleaning system with a fluid circulation pump that propels the cleaning fluid through the injections system.

[0027]

[0024] FIG. 7B illustrates a cleaning system with a fluid circulation pump that propels the cleaning fluid through the injections system.

[0028]

[0025] FIG. 8 is a schematic illustrating a processor controlling the various components of the injection and cleaning systems.

[0029] DETAILED DESCRIPTION OF THE INVENTION

[0030]

[0026] Reference is made herein to some specific examples of the present invention, including any best modes contemplated by the inventor for carrying out the invention. Examples of these specific embodiments are illustrated in the accompanying figures. While the invention is described in conjunction with these specific embodiments, it will be understood that it is not intended to limit the invention to the described or illustrated embodiments. To the contrary, it is intended to cover alternatives, modifications, and equivalents as may be included within the spirit and scope of the invention, as defined by the appended claims.

[0031]

[0027] In the following description, numerous specific details are set forth to provide a thorough understanding of the present invention. Example embodiments of the present invention may be implemented without some or all these specific details. In other instances, process operations well known to persons of skill in the art have not been described in detail in order not to obscure unnecessarily the present invention. Various techniques and mechanisms of the present invention will sometimes be described in singular form for clarity. However, it should be noted that some embodiments include multiple iterations of a technique or multiple mechanisms, unless noted otherwise. Similarly, various steps of the methods shown and described herein are not necessarily performed in the order indicated, or performed at all in certain embodiments. Accordingly, some implementations of the methods discussed herein may include more or fewer steps than those shown or described. Further, the techniques and mechanisms of the present invention will sometimes describe a connection, relationship or communication between two or more entities. It should be noted that a connection or relationship between entities does not necessarily mean a direct, unimpeded connection, as a variety of other entities or processes may reside or occur between any two entities. Consequently, an indicated connection does not necessarily mean a direct, unimpeded connection, unless otherwise noted.

[0032]

[0028] The following list of example features corresponds with the attached figures and is provided for ease of reference, where like reference numerals designate corresponding features throughout the specification and figures:

[0033]

[0029] 1 : Electrolyte Container

[0034]

[0030] 1.1 : Heater / Cooler

[0035]

[0031] 2: Electrolyte Buffer Container

[0036]

[0032] 2.1 : Heater / Cooler

[0037]

[0033] 3 : Electrolyte Loading Volume

[0038]

[0034] 3.1 : Heater / Cooler

[0039]

[0035] 4: Neat Cleaning Fluid Container

[0040]

[0036] 4.1 : Heater / Cooler

[0041]

[0037] 4.2: Window Sight

[0042]

[0038] 5: Absorbent / Desiccant Container

[0043]

[0039] 5.1 : Heater / Cooler

[0044]

[0040] 5.2: Window Sight

[0045]

[0041] 5.3: Absorbent / Desiccant

[0046]

[0042] 6: Contaminated Cleaning Fluid Collection Container

[0047]

[0043] 6.1 : Heater / Cooler

[0048]

[0044] 6.2: Window Sight

[0049]

[0045] 7.1-7.17: Valves

[0050]

[0046] 8: Spectrometer

[0051]

[0047] 9: Electrochemical (Battery) Cell

[0052]

[0048] 10: Neat Cleaning Fluid

[0053]

[0049] 10.2: Contaminated Cleaning Fluid

[0054]

[0050] 11 : Electrolyte

[0055]

[0051] 12: Electrolyte Injection System

[0056]

[0052] 13 : Electrolyte Injection Port

[0053] 14: Regeneration Gas Container

[0057]

[0054] 15: Vacuum Pump

[0058]

[0055] 16.1-16.7: Injector Cleaning System

[0059]

[0056] 17: Cell Emulator

[0060]

[0057] 18, 18A, 18B: Fluid Circulation Pump

[0061]

[0058] 19: Processor

[0062]

[0059] 20.1 Cleaning Fluid Circuit

[0063]

[0060] 20.2 Cleaning Fluid Circuit

[0064]

[0061] 21 : Pressure Sensor

[0065]

[0062] 22: Fluid Level Sensor

[0066]

[0063] 25: Distillation Container

[0067]

[0064] 30: Condensing Container

[0068]

[0065] To improve the cleaning efficiency of the electrolyte injection system, distillation of the cleaning fluid is a component process of the cleaning system. Referencing FIG. 1A, an injector system 12 is shown that may include an electrolyte container 1, an electrolyte buffer container 2, an electrolyte loading volume 3, and an electrolyte injection port 13, which make up the basic system components for injecting electrolyte into an electrochemical cell 9, previously described in detail within a separate disclosure incorporated herein by reference.

[0069]

[0066] This system is improved further by an injector cleaning system 16.1 connected to the electrolyte injection system 12. Specifically, the injector cleaning system 16.1 may further include a contaminated cleaning fluid collection container 6 and a neat cleaning fluid container 4. The temperature differential between containers 6 and 4 causes contaminated cleaning fluid from the collection container 6 to recondense into the neat cleaning fluid container 4 as a neat cleaning fluid 10, free from electrolyte residue. In this setup, the contaminated cleaning fluid collection container 6 is the distillation container 25, and the neat cleaning fluid container 4 is the condensing container 30.

[0070]

[0067] The neat cleaning fluid 10 is circulated through the injection system 12, removing the electrolyte residue and turning the neat cleaning fluid 10 into a contaminated cleaning fluid 10.2 that is collected. The cleaning system 16.1 may have a plurality of valves that allows the neat cleaning fluid 10 to be targeted to specific components. Only sectional cleaning of the electrolyte injection system 12 may be preferred from a time efficiency standpoint, such that the electrolyte 11 may remain within certain sections of the injection system 12 during cleaning. For example, valves 7.8, 7.4, 7.2, 7.6, 7.13 and 7.10 may be opened to direct the neat cleaning fluid 10 into the electrolyte buffer tank 2. This cleaning fluid circuit 20.1 is shown in FIG. IB. If, however, the user would like to clean out the entire electrolyte injection system 12, then valves 7.8, 7.4, 7.2, 7.3, 7.14 and 7.10 may be opened, resulting in the cleaning fluid circuit 20.2 shown in FIG. 1C. Shown in FIG. 6 is a cell emulator 17 that may be used to ensure complete cleaning of the electrolyte injection port 13. The actuation of the plurality of valves to target specific components within the injection system 12 may be manually performed or may be automated with a processor 19, as shown in FIG. 8.

[0071]

[0068] The collected contaminated cleaning fluid 10.2 within the collection container 6 can then be heated by the heater / cooler 6.1, bringing its temperature high enough such that the cleaning fluid can boil off, travel through the valve 7.9, and condense in the neat cleaning fluid container 4. The electrolyte residue washed from the system 12 remains within collection container 6. The neat fluid container 4 may have a heater / cooler 4.1 that may cool the container 4 to accelerate the condensation. The actuation of the heater / coolers 6.1 and 4.1 may be manually performed or may be automated with a processor 19, as shown in FIG. 8.

[0072]

[0069] FIG. 2 illustrates a cleaning system 16.2 with an absorbent / desiccant container 5 that holds an absorbent / desiccant 5.3. The distilled cleaning fluid may optionally be passed through an absorbent / desiccant 5.3 to dry the cleaning fluid of water moisture or other less desirable solvent materials. It may be preferable to allow the contaminated cleaning fluid to remain in the absorbent / desiccant container 5 for a sufficient time to allow the fluid to thoroughly dry prior to use within the system.

[0073]

[0070] The resulting cleaning fluid may be transferred through valve 7.9 into the neat fluid container 4. The absorbent / desiccant container 5 also has a heater / cooler 5.1 that controls the temperature to facilitate efficient contaminant removal. From here, the neat cleaning fluid may again be reused, eliminating waste cleaning fluid and making for a more efficient process. In this setup, the contaminated cleaning fluid collection container 6 is the distillation container 25, and the neat cleaning fluid container 4 is the condensing container 30.

[0074]

[0071] The heater / coolers 4.1, 5.1, and 6.1 may be tuned to adjust the temperature of containers 4, 5, and 6 to move the cleaning fluid throughout the system. Similarly, the temperatures of the electrolyte buffer tank 2 and the electrolyte loading volume 3 may be adjusted through the heater / coolers 2.1 and 3.1 to move the cleaning fluid through the system. The temperature differential between the components may also create a pressure differential that moves the fluid through the system. In addition, or as an alternative, a fluid circulation pump 18 may be used to circulate the cleaning fluid (see FIG. 7).

[0075]

[0072] The absorbent / desiccant container 5 may be heated by a heater / cooler 5.1 to dry off and to regenerate absorbent / desiccant 5.3. The materials used as an absorbent / desiccant that preferably absorb moisture, such as a silica gel, molecular sieves, etc. During heating, a valve 7.15 may be opened to exhaust out any moisture from the system. This drying may optionally be done with a regeneration gas stored in container 14, such as inert gas or hydrogen, being flowed over the absorbent / desiccant 5.3. A vacuum pump 15 may optionally be used to purge the system of any remaining processes gas or moisture prior to use.

[0076]

[0073] The actuation of the heater / coolers 6.1, 5.1 and 4.1, the fluid circulation pump 18 and the vacuum pump 15 may be manually performed or may be automated with a processor 19, as shown in FIG. 8.

[0077]

[0074] The design and method for improved efficiency of the cleaning system uses a distillation process to reuse cleaning fluid. This process requires heating or cooling of elements to ensure proper cleaning and distillation of the cleaning fluid. This heating or cooling may require a wide temperature differential to effectively boil or condensate the cleaning fluid. To lower the energy input and time it might take to create a wider temperature differential, the cleaning fluid may optionally be a liquefied gas solution. The liquefied gas solution may have good absorbent properties for electrolyte residue. By using a liquefied gas solution as the cleaning fluid, distillation may be made more easily at more moderate temperatures. Further, water moisture contamination may more effectively be removed if distillation occurs at lower temperatures, to prevent water boil-off during the distillation process.

[0078]

[0075] For example, the boiling point and freezing point of dimethyl carbonate are +90 °C and +4 °C, respectively, and the boiling point and freezing point of a liquefied gas solution cleaning fluid composed of difluoroethane are -24 °C and -117 °C, respectively. Since the boiling point of water is +100 °C and the freezing point of water is 0 °C, water contamination may more easily be removed from the cleaning fluid using a liquefied gas solution cleaning fluid due to the wider different in boiling point between water and the liquefied gas solvent. The reduced moisture content will make for a more reliable process and will minimize moisture that may be introduced into the cell’s electrolyte, prolonging life of the cell and maintaining higher performance.

[0079]

[0076] The liquefied gas cleaning solution may include the following: fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1,1- difluoroethane, 1,2-difluoroethane, 1,1,1 -trifluoroethane, 1,1,2-trifluoroethane, 1, 1,1,2- tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chloride fluoride, phosphoryl fluoride, phosphoryl chloride fluoride, sulfuryl fluoride, sulfuryl chloride fluoride, 1 -fluoropropane, 2-fluoropropane, 1,1- difhioropropane, 1,2-difluoropropane, 2, 2-fluoropropane, 1,1,1-trifluoropropane, 1,1,2- trifluoropropane, 1,2,2-trifluoropropane, fluoroethylene, cis-l,2-fluoroethylene, 1,1- fluoroethylene, 1-fluoropropylene, 2-propylene, chlorine, chloromethane, bromine, iodine, ammonia, methyl amine, dimethyl amine, trimethyl amine, molecular oxygen, molecular nitrogen, carbon monoxide, carbon dioxide, sulfur dioxide, dimethyl ether, methyl vinyl ether, difluoro ethylene, nitrous oxide, nitrogen dioxide, nitrogen oxide, carbon disulfide, hydrogen fluoride, hydrogen chloride, methane, ethane, propane, butane, ethylene, propylene, butylene, and any other listed liquefied gas solvent or liquid solvent listed herein by reference, or any combination thereof. Of course, if the liquefied gas solution which has a vapor pressure above atmospheric pressure is used as cleaning fluid, components of the injection system should be rated to handle increased pressures required to safely contain the cleaning fluid from release.

[0080]

[0077] In another embodiment of the invention, instead of using an absorb ent / desiccant to remove water vapor from the cleaning fluid, or in addition to using an absorbent / desiccant, a cooling element 5.1 may be used such that the container 5 can form a cold trap to freeze water into ice, a solid form that remains in the container 5. The cooling element 5.1 thereby removes water vapor or simply-put, moisture from the cleaning fluid via condensing the water vapor (hitherto dissolved in the cleaning fluid) into ice, and the condensation may or may not be used in conjunction with using a desiccant / absorbent material to trap water. It should be noted that the temperature of the cooling element 5.1 should be set to below the freezing point of water and above the boiling point of the cleaning fluid to allow for the condensation of water into ice in the contaminated cleaning fluid into the container 5 and the condensation of the neat cleaning fluid into the neat cleaning fluid container 4, which will separate water vapor (wetness or moisture is a contaminant when present in cleaning fluid) from the neat cleaning fluid, which may then be recirculated and reused in the cleaning system.

[0081]

[0078] In another embodiment of the present invention shown in FIG. 3, the cleaning system 16.3 combines containers 4 and 5 into a single container such that the absorbent / desiccant container 5 stores the neat cleaning fluid 10. In this setup, the absorbent / desiccant container 5 is the condensing container 30, and the contaminated cleaning fluid collection container 6 is the distillation container 25.

[0082]

[0079] In another embodiment of the present invention shown in FIG. 4, the cleaning system 16.4 combines containers 5 and 6 into a single container such that the absorbent / desiccant container 5 collects the contaminated cleaning fluid 10.2 and absorbs the moisture from it.

[0083]

[0080] FIG. 5 illustrates a cleaning system 16.5 where the collection container 6 is near the injector 13. It would be apparent that the location of the collection container 6 can be adjusted. In this setup, the contaminated cleaning fluid collection container 6 is the distillation container 25, and the neat cleaning fluid container 4 is the condensing container 30.

[0084]

[0081] Shown in FIG. 6, the cleaning system 16.6 has a cell emulator 17 that can be connected to the electrolyte injection port 13 in the same manner as the connection with the electrochemical / battery cell 9, ensuring that the cleaning fluid rinses all wet components within the injection system 12.

[0085]

[0082] FIG. 7A illustrates a cleaning system 16.7 with a fluid circulation pump 18 that circulates the cleaning fluid. Additional pumps 18A and 18B may be added to the cleaning system 16.7 as shown in FIG. 7B. The pump 18 creates a pressure differential, which allows the fluid to boil into a gas from one container and to condensate back into a fluid in the next container. Thus, even when using the circulation pump 18, the contaminated fluid is cleaned through distillation. The circulation pump 18 may be used in lieu of, or in addition to, the heater / coolers (1.1, 2.1, 3.1, 4.1, 5.1, 6. 1) to circulate the cleaning fluid. The cleaning system 16.7 may also have spectrometers 8 to detect the level of contaminates in the system. The spectrometer 8 may be connected to the processor 19, as shown in FIG. 8.

[0086]

[0083] In FIGS. 5, 6, 7A and 7B, the contaminated cleaning fluid collection container 6 is the distillation container 25, and the neat cleaning fluid container 4 is the condensing container 30.

[0087]

[0084] FIG. 8 is a schematic showing the valves, pumps, and heater / coolers controlled by a processor 19. Because the heater / coolers (1.1, 2.1, 3.1, 4.1, 5.1, 6.1) may have integrated temperature sensors, temperature data is reported to the processor 19. Alternatively, separate temperature sensors may be used. The processor 19 may automate the cell injection procedure as well as automate the injector cleaning procedure. The processor 19 may also connect to the pressure sensor(s) 21 and to the fluid level sensor(s) 22 to accurately monitor the fluid levels in the various containers.

[0088]

[0085] Containers (4, 5, 6) may include sight windows (4.2, 5.2, 6.2) to examine visually or by spectroscopy (via spectrometer 8) the level of contamination within those containers. This allows for a rapid visual indication of the level of contamination collected from the system over time and when it is appropriate for an operator of the cleaning system to replace the cleaning fluid, absorbent / desiccant, or cleaning system components.

[0089]

[0086] The neat cleaning fluid container 4, the absorbent / desiccant container 5, the collection container 6, and / or the electrolyte injection system 12 may be in direct or indirect thermal contact. When the cleaning fluid is boiled and recondensed, the heat of condensation or heat loss due to evaporation may be captured and transferred to the next container. This reduces the amount of energy consumed by the cleaning system 16. Direct thermal contact means the containers are physically touching or share a wall. Indirect thermal contact means the containers share a thermal exchange fluid, such as water or another fluid that circulates between both containers and carries heat from one to the other.

[0090]

[0087] The neat cleaning fluid container 4, the absorbent / desiccant container 5, and the collection container 6 may be any suitable metal, ceramic, or plastic apparatus capable of holding a liquefied gas electrolyte that has a vapor pressure above an atmospheric pressure of 100 kPa at a temperature of 293.15 K. In some embodiments the containers may be larger than 1 cubic centimeter, larger than 10 cubic centimeters, larger than 100 cubic centimeters, larger than 1000 cubic centimeters, larger than 10000 cubic centimeters, larger than 100000 cubic centimeters, or larger than 1000000 cubic centimeters. In some embodiments, the containers may vary in capacity from one another.

[0088] Throughout the injection system, there are a variety of tubes which allow fluid connection from container to container, etc. In some figures, these tubes are drawn as sometimes having the end of the tube submerged under the liquid line of the fluid. However, it should be understood this is only for illustration purposes and the end of the tube, depending on the state of the system and the fluid line of each container, the end of the tube may reside above the liquid line of the fluid as well.

[0089] The heater / coolers (1.1 , 2.1, 3.1, 4.1, 5.1, 6.1) may be, but are not limited to: heating blankets, heating tape, heating rope, heat engines, electric heaters, heat pumps, Peltier module, or thermally regulated enclosures. The heater / coolers may have built-in temperature sensors. Alternatively, separate temperature sensors may be used.

[0091]

[0090] The valves (7.1 through 7.17) may include, but are not limited to: ball valves, diaphragm valves, needle valves, and / or butterfly valves

[0092]

[0091] The various components of the described setups are connected by metal, plastic, or ceramic tubing of various sizes. In some embodiments, for example, the tubing may be, but is not limited to: 1 / 16-inch, 1 / 8-inch, 1 / 4-inch, 1 / 2-inch, 1-inch, or 2-inch outer diameter.

[0093]

[0092] While this document contains many specifics, these should not be construed as limitations on the scope of any invention or of what may be claimed, but rather as descriptions of features that may be specific to a particular embodiment of the invention. Certain features that are described in this patent document in the context of separate embodiments can also be implemented in combination in a single embodiment. Conversely, various features that are described in the context of a single embodiment can also be implemented in multiple embodiments separately or in any suitable sub-combination. Moreover, although features may be described above as acting in certain combinations and even initially claimed as such, one or more features from a claimed combination can in some cases be excised from the combination, and the claimed combination may be directed to a sub-combination or a variation of a sub-combination.

Claims

CLAIMS1. A setup for injecting an electrolyte (11) into an electrochemical energy storage device (9), the setup comprising: an electrolyte injection system (12) comprising: an electrolyte container (1) containing the electrolyte (11); and an electrolyte injection port (13) fluidly connected to the electrolyte container (1), wherein the port (13) is constructed to connected to the electrochemical energy storage device (9); an injector cleaning system (16.1-16.7) fluidly connected to the electrolyte injection system (12), wherein the injector cleaning system (16.1-16.7) comprises: a condensing container (30) containing a cleaning solution (10), the condensing container (30) fluidly connected to the electrolyte injection system (12) and constructed to circulate the cleaning solution (10) through the electrolyte injection system (12) to remove contaminants; and a distillation container (25) fluidly connected to the electrolyte injection system (12) and constructed to collect the contaminated cleaning solution (10.2) within the electrolyte injection system (12); wherein the distillation container (25) is constructed to: boil the contaminated cleaning solution (10.2) to create a cleaning solution vapor; and transfer the cleaning solution vapor to the condensing container (30); and wherein the condensing container (30) is constructed to condense the cleaning solution vapor into a cleaning solution for re-circulation through the electrolyte injection system (12).

2. The setup of claim 1, wherein the injector cleaning system (16.1-16.7) further comprises:a first valve (7.8) between the condensing container (30) and the electrolyte injection system (12), constructed to regulate the flow of the cleaning solution (10) into the electrolyte injection system (12); and a second valve (7.10) between the distillation container (25) and the electrolyte injection system (12), constructed to regulate the flow of the contaminated cleaning solution (10.2) into the distillation container (25).

3. The setup of claim 1, wherein the injector cleaning system (16.1-16.7) further comprises a plurality of valves constructed to selectively circulate the cleaning solution (10) to certain components of the electrolyte injection system (12).

4. The setup of claim 1, wherein the electrolyte injection system (12) further comprises: an electrolyte buffer container (2); and an electrolyte loading volume (3).

5. The setup of claim 1, wherein: the distillation container (25) comprises a first heater / cooler (6.1) that assists in boiling the contaminated cleaning solution (10.2); and the condensing container (30) comprises a second heater / cooler (4.1) that assists in condensing the cleaning solution vapor.

6. The setup of claim 1, further comprising a fluid circulation pump (18) that creates a pressure differential within the injector cleaning system (16.1-16.7) that assists in boiling the contaminated cleaning solution (10.2) and in condensing the cleaning solution vapor.

7. The setup of claim 1, wherein the injector cleaning system (16.1-16.7) further comprises an absorbent / desiccant container (5) containing an absorbent / desiccant (5.3) fluidly connected to the distillation container (25) and to the condensing container (30).

8. The setup of claim 7, further comprising a regeneration gas container (14) constructed to pass a gas through the absorbent / desiccant container (5) to dry the absorbent / desiccant (5.3).

9. The setup of claim 7, wherein the absorbent / desiccant container (5) comprises a heater / cooler (5.1).

10. The setup of claim 1, wherein the distillation container (25) contains an absorbent / desiccant (5.3).

11. The setup of claim 1, wherein the condensing container (30) contains an absorbent / desiccant (5.3).

12. The setup of claim 1, wherein the distillation container (25) and the condensing container (30) each have a window sight (4.2, 6.2).

13. The setup of claim 12, further comprising a spectrometer (8) to measure the spectral characteristics through either one or both window sights (4.2, 6.2).

14. The setup of claim 1, further comprising a vacuum pump (15) constructed to vent the injector cleaning system (16.1-16.7).

15. The setup of claim 1, wherein the cleaning solution (10) comprises a liquified gas.

16. The setup of claim 15, wherein the liquified gas is selected from the following: fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1,1-difluoroethane, 1,2- difluoroethane, 1,1,1 -trifluoroethane, 1,1,2-trifluoroethane, 1, 1,1,2- tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chloride fluoride, phosphoryl fluoride, phosphoryl chloride fluoride, sulfuryl fluoride, sulfuryl chloride fluoride, 1 -fluoropropane, 2-fluoropropane, 1,1- difluoropropane, 1,2-difluoropropane, 2, 2-fluoropropane, 1,1,1-trifluoropropane, 1,1,2-trifluoropropane, 1 ,2,2-trifluoropropane, fluoroethylene, cis-l,2-fluoroethylene, 1,1 -fluoroethylene, 1- fluoropropylene, 2-propylene, chlorine, chloromethane, bromine, iodine, ammonia, methyl amine, dimethyl amine, trimethyl amine, molecular oxygen, molecular nitrogen, carbon monoxide, carbon dioxide, sulfur dioxide, dimethyl ether, methyl vinyl ether, difluoro ethylene, nitrous oxide, nitrogen dioxide, nitrogen oxide, carbon disulfide, hydrogen fluoride, hydrogen chloride, methane, ethane, propane, butane, ethylene, propylene, butylene, and any combination thereof.

17. An injector cleaning system (16.1-16.7) for use with an electrolyte injection system (12) that includes an electrolyte container (1) containing an electrolyte (11); and an electrolyte injection port (13) fluidly connected to the electrolyte container (1), the port (13) constructed to fill an electrochemical energy storage device (9), the injector cleaning system (16.1-16.7) comprising: a condensing container (30) containing a cleaning solution (10), the condensing container (30) fluidly connected to the electrolyte injection system (12) and constructed to circulate the cleaning solution (10) through the electrolyte injection system (12) to remove contaminants; a distillation container (25) fluidly connected to the electrolyte injection system (12) and constructed to collect the contaminated cleaning solution (10.2) within the electrolyte injection system (12); wherein the distillation container (25) is constructed to: boil the contaminated cleaning solution (10.2) to create a cleaning solution vapor; and transfer the cleaning solution vapor to the condensing container (30); and wherein the condensing container (30) is constructed to condense the cleaning solution vapor into a cleaning solution for re-circulation through the electrolyte injection system (12).

18. The injector cleaning system (16.1 -16.7) of claim 17, further comprising a plurality of valves constructed to selectively circulate the cleaning solution (10) to certain components of the electrolyte injection system (12).

19. The injector cleaning system (16.1-16.7) of claim 17, further comprising: a first valve (7.8) between the condensing container (30) and the electrolyte injection system (12), constructed to regulate the flow of the cleaning solution (10) into the electrolyte injection system (12); and a second valve (7.10) between the distillation container (25) and the electrolyte injection system (12), constructed to regulate the flow of the contaminated cleaning solution (10.2) into the distillation container (25).

20. The injector cleaning system (16.1-16.7) of claim 17, wherein: the distillation container (25) comprises a first heater / cooler (6.1) that assists in boiling the contaminated cleaning solution (10.2); and the condensing container (30) comprises a second heater / cooler (4.1) that assists in condensing the cleaning solution vapor.

21. The injector cleaning system (16.1-16.7) of claim 17, further comprising a fluid circulation pump (18) that creates a pressure differential within the injector cleaning system (16. 1-16.7) that assists in boiling the contaminated cleaning solution (10.2) and in condensing the cleaning solution vapor.

22. The injector cleaning system (16. 1-16.7) of claim 17, further comprising an absorbent / desiccant container (5) containing an absorbent / desiccant (5.3) fluidly connected to the distillation container (25) and to the condensing container (30).

23. The injector cleaning system (16.1-16.7) of claim 22, further comprising a regeneration gas container (14) constructed to pass a gas through the absorbent / desiccant container (5) to dry the absorbent / desiccant (5.3).

24. The injector cleaning system (16.1 -16.7) of claim 22, wherein the absorbent / desiccant container (5) comprises a heater / cooler (5.1).

25. The injector cleaning system (16.1-16.7) of claim 17, wherein the distillation container (25) contains an absorbent / desiccant (5.3).

26. The injector cleaning system (16.1-16.7) of claim 17, wherein the condensing container (30) contains an absorbent / desiccant (5.3).

27. The injector cleaning system (16.1-16.7) of claim 17, wherein the distillation container (25) and the condensing container (30) each has a window sight (4.2, 6.2).

28. The injector cleaning system (16.1-16.7) of claim 27, further comprising a spectrometer (8) to measure the spectral characteristics through either one or both window sights (4.2, 6.2).

29. The injector cleaning system (16. 1-16.7) of claim 17, further comprising a vacuum pump (15) constructed to vent the injector cleaning system (16.1-16.7).

30. The injector cleaning system (16.1-16.7) of claim 17, wherein the cleaning solution (10) comprises a liquified gas.

31. The injector cleaning system (16.1-16.7) of claim 30, wherein the liquified gas is selected from the following: fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1, 1 -difluoroethane, 1,2- difluoroethane, 1,1,1 -trifluoroethane, 1 , 1 ,2-trifluoroethane, 1,1, 1,2- tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chloride fluoride, phosphoryl fluoride, phosphoryl chloride fluoride, sulfuryl fluoride, sulfuryl chloride fluoride, 1 -fluoropropane, 2-fluoropropane, 1,1- difluoropropane, 1,2-difluoropropane, 2, 2-fluoropropane, 1,1,1- trifluoropropane, 1,1,2-trifluoropropane, 1,2,2-trifluoropropane,fluoroethylene, cis-l,2-fluoroethylene, 1,1 -fluoroethylene, 1- fluoropropylene, 2-propylene, chlorine, chloromethane, bromine, iodine, ammonia, methyl amine, dimethyl amine, trimethyl amine, molecular oxygen, molecular nitrogen, carbon monoxide, carbon dioxide, sulfur dioxide, dimethyl ether, methyl vinyl ether, difluoro ethylene, nitrous oxide, nitrogen dioxide, nitrogen oxide, carbon disulfide, hydrogen fluoride, hydrogen chloride, methane, ethane, propane, butane, ethylene, propylene, butylene, and any combination thereof.

32. An injector cleaning system (16.1-16.7) for use with an electrolyte injection system (12) that includes an electrolyte container (1) containing an electrolyte (11), wherein an electrolyte injection port (13) fluidly connected to the electrolyte container (1), the port (13) constructed to fill an electrochemical energy storage device (9), the injector cleaning system (16.1-16.7) comprising: a condensing container (30) containing a cleaning solution (10), the condensing container (30) fluidly connected to the electrolyte injection system (12) and constructed to circulate the cleaning solution (10) through the electrolyte injection system (12) to remove contaminants; and a distillation container (25) fluidly connected to the electrolyte injection system (12) and constructed to collect the contaminated cleaning solution (10.2) within the electrolyte injection system (12); wherein the distillation container (25) is constructed to: boil the contaminated cleaning solution (10.2) to create a cleaning solution vapor; and transfer the cleaning solution vapor to the condensing container (30); and wherein the condensing container (30) is constructed to condense the cleaning solution vapor into a cleaning solution for re-circulation through the electrolyte injection system (12); a first heater / cooler (6.1) that assists in boiling the contaminated cleaning solution (10.2); anda second heater / cooler (4.1) that assists in condensing the cleaning solution vapor; a plurality of valves constructed to selectively circulate the cleaning solution (10) to certain components of the electrolyte injection system (12); and a processor (19) connected to the first heater / cooler (6.1), the second heater / cooler (4.1) and the series of valves and constructed to: create a cleaning fluid circuit (20.1, 20.2) by actuating individual valves within the plurality; and actuate the first heater / cooler (6.1) and the second heater / cooler (6.2) to propel the cleaning solution (10) through the cleaning fluid circuit (20.1, 20.2).

33. The injector cleaning system (16.1-16.7) of claim 32, further comprising a fluid circulation pump (18) connected to the processor (19), wherein the processor (19) actuates the fluid circulation pump (19) to create a pressure differential within the injector cleaning system (16.1-16.7) that assists in propelling the cleaning solution (10) through the cleaning fluid circuit (20.1, 20.2).

34. The injector cleaning system (16.1-16.7) of claim 32, further comprising a vacuum pump (15) connected to the processor (19), wherein the processor (19) actuates the vacuum pump (15) to vent the injector cleaning system (16.1-16.7).

35. The injector cleaning system (16.1-16.7) of claim 32, wherein the distillation container (25) and the condensing container (30) each has a window sight (4.2, 6.2), wherein the system further comprises a spectrometer (8) connected to the processor (19), and wherein the processor (19) receives spectral characteristics detected by the spectrometer (8) through either one or both window sights (4.2, 6.2).

36. The injector cleaning system (16.1-16.7) of claim 32, wherein the cleaning solution (10) comprises a liquified gas.

7. The injector cleaning system (16.1 -16.7) of claim 36, wherein the liquified gas is selected from the following: fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1,1-difluoroethane, 1,2- difluoroethane, 1,1,1 -trifluoroethane, 1 , 1 ,2-trifluoroethane, 1 , 1 , 1 ,2- tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chloride fluoride, phosphoryl fluoride, phosphoryl chloride fluoride, sulfuryl fluoride, sulfuryl chloride fluoride, 1 -fluoropropane, 2-fluoropropane, 1,1- difluoropropane, 1,2-difluoropropane, 2, 2-fluoropropane, 1,1,1- trifluoropropane, 1,1,2-trifluoropropane, 1,2,2-trifluoropropane, fluoroethylene, cis-l,2-fluoroethylene, 1,1 -fluoroethylene, 1- fluoropropylene, 2-propylene, chlorine, chloromethane, bromine, iodine, ammonia, methyl amine, dimethyl amine, trimethyl amine, molecular oxygen, molecular nitrogen, carbon monoxide, carbon dioxide, sulfur dioxide, dimethyl ether, methyl vinyl ether, difluoro ethylene, nitrous oxide, nitrogen dioxide, nitrogen oxide, carbon disulfide, hydrogen fluoride, hydrogen chloride, methane, ethane, propane, butane, ethylene, propylene, butylene, and any combination thereof.

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