Device and method for fully recycling waste lithium battery electrolyte

Through the distillation, condensation and absorption steps of the waste lithium battery electrolyte full recovery device, the problem of solvents and electrolytes in lithium batteries cannot be recovered, and efficient resource recovery is achieved.

CN120810052AActive Publication Date: 2025-10-17ZHEJIANG WATER HEALER ENVIRONMENTAL TECH CO LTD +1
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Patent Information

Application Number
CN202511300704.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-12
Publication Date
2025-10-17
Estimated Expiration
2045-09-12

AI Technical Summary

Technical Problem

The existing technology cannot effectively recycle the electrolyte solvent and electrolyte in lithium batteries, resulting in a waste of resources.

Method used

A waste lithium battery electrolyte full recovery device is used, including components such as a solvent extractor, a condenser, an absorption tank and a solvent storage tank. The solvent and electrolyte in the electrolyte are separated and recovered through steps such as distillation, condensation and absorption.

Benefits of technology

The efficient recovery of solvents and electrolytes in lithium batteries is achieved, thus avoiding waste of resources and improving resource utilization.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of electrolyte recovery, and provides a waste lithium battery electrolyte total recovery device and method.The waste lithium battery electrolyte total recovery device comprises a solvent extractor, a first condenser, a conveying part, an absorption tank, a first valve, a first solvent storage tank and a second valve; the conveying part is provided with a flow guide section, a first flow dividing section and a second flow dividing section which are communicated, the first flow dividing section and the second flow dividing section are arranged in parallel, the absorption tank is communicated with the first flow dividing section, and the first valve is communicated with the first flow dividing section; the other end of the first solvent storage tank is communicated with the solvent extractor, and the second valve is communicated with the second shunting section. According to the invention, the problem of waste of solvent and electrolyte resources caused by incapability of recovering the solvent and the electrolyte in the electrolyte can be solved.
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Description

TECHNICAL FIELD

[0001] The application relates to the technical field of electrolyte recovery, in particular to a device and method for full recovery of waste lithium battery electrolyte. BACKGROUND

[0002] The battery comprises a positive electrode, a negative electrode and an electrolyte, the electrolyte is a core component of the battery, contains a large amount of flammable organic solvent, lithium hexafluorophosphate electrolyte and its decomposition products.

[0003] When the battery is recovered, the battery can be first crushed and then pyrolyzed, then the volatile gas is condensed to obtain the electrolyte solvent, then the alkaline solution is sprayed, and finally the spray liquid is disposed as hazardous waste.

[0004] In the related art, the solvent and electrolyte in the electrolyte cannot be recovered, which causes waste of resources of the solvent and electrolyte. SUMMARY

[0005] The application provides a device and method for full recovery of waste lithium battery electrolyte, which can solve the problem that the solvent and electrolyte in the electrolyte cannot be recovered, which causes waste of resources of the solvent and electrolyte.

[0006] In order to achieve the above purpose, the application adopts the following technical solutions:

[0007] In a first aspect, the application provides a device for full recovery of waste lithium battery electrolyte, comprising:

[0008] The solvent extractor is used to contain the filtrate of the lithium battery;

[0009] The first condenser is connected to the solvent extractor;

[0010] The conveying member has a communicating flow guide section, a first shunt section and a second shunt section, and the first shunt section and the second shunt section are connected in parallel;

[0011] The absorption tank is connected to the first shunt section;

[0012] The first valve is connected to the first shunt section, and is used to open or close the communication between the first shunt section and the absorption tank;

[0013] One end of the first solvent storage tank is connected to the second shunt section, and the other end of the first solvent storage tank is connected to the solvent extractor;

[0014] The second valve is connected to the second shunt section, and is used to open or close the communication between the second shunt section and the first solvent storage tank.

[0015] In some embodiments, the delivery member has a third shunt segment in communication with the flow guide segment, the third shunt segment being disposed in parallel with the first shunt segment;

[0016] The device for recycling waste lithium battery electrolyte further comprises:

[0017] A second solvent tank is in communication with the third shunt segment;

[0018] A third valve is in communication with the third shunt segment, and the third valve is used to open or close the communication between the third shunt segment and the second solvent tank;

[0019] A vacuum member is in communication with the solvent extractor.

[0020] In some embodiments, the absorption tank has a first output end and a second output end;

[0021] The device for recycling waste lithium battery electrolyte further comprises:

[0022] A second condenser, one end of the second condenser being in communication with the first output end, and the other end of the second condenser being in communication with the solvent extractor;

[0023] A hydrolysis reactor, the hydrolysis reactor being in communication with the absorption tank through the second output end, and the hydrolysis reactor being in communication with the solvent extractor.

[0024] In some embodiments, the device further comprises:

[0025] An electrolyte leaching device, the electrolyte leaching device being in communication with the solvent extractor, the electrolyte leaching device being used to deliver the filtrate to the solvent extractor, and the electrolyte leaching device being in communication with the first solvent tank.

[0026] In some embodiments, the device further comprises:

[0027] A first filter, the first filter being in communication with the hydrolysis reactor, and the first filter having an inner portion layered into an upper filtrate layer and a lower precipitate layer;

[0028] An organic phase separator, the organic phase separator having an inlet end, a first outlet end and a second outlet end, the inlet end being in communication with the upper filtrate layer, and the first outlet end being in communication with the electrolyte leaching device;

[0029] A primary fluorine extractor, the primary fluorine extractor being in communication with the lower precipitate layer.

[0030] In some embodiments, the device further comprises:

[0031] A phosphorus extractor, the phosphorus extractor being in communication with the second outlet end;

[0032] A second filter, the second filter being in communication with the hydrolysis reactor;

[0033] An impurity metal separator, the impurity metal separator being in communication with the second filter.

[0034] A third filter element is in communication with the impurity metal separator and the primary fluorine extractor;

[0035] A fourth filter element is in communication with the primary fluorine extractor;

[0036] A lithium extractor is in communication with the fourth filter element;

[0037] A fifth filter element is in communication with the lithium extractor;

[0038] A secondary fluorine extractor is in communication with the fifth filter element;

[0039] A sixth filter element is in communication with the secondary fluorine extractor.

[0040] In a second aspect, the present application provides a method for full recovery of waste lithium battery electrolyte, which is applied to a device for full recovery of waste lithium battery electrolyte, and the method comprises the following steps:

[0041] The filtrate of the lithium battery is delivered to the solvent extractor;

[0042] The first valve is opened, the second valve is closed, and the first condenser is adjusted to a first temperature, so that the first part of the volume of the filtrate is sequentially delivered to the absorption tank through the first condenser, the flow guide section of the delivery element, and the first shunt section of the delivery element;

[0043] The first valve is closed, the second valve is opened, and the first condenser is adjusted to a second temperature, so that the second part of the volume of the filtrate is sequentially delivered to the first solvent storage tank through the first condenser, the flow guide section, and the second shunt section of the delivery element.

[0044] In some embodiments, when the first valve is opened and the second valve is closed, the method further comprises:

[0045] The third valve of the device for full recovery of waste lithium battery electrolyte is closed.

[0046] In some embodiments, when the first valve is closed and the second valve is opened, the method further comprises:

[0047] The third valve of the device for full recovery of waste lithium battery electrolyte is closed.

[0048] In some embodiments, the method further comprises the following steps:

[0049] The first valve is closed, the second valve is closed, and the third valve is opened; the first condenser is adjusted to a third temperature, so that the third part of the volume of the filtrate is sequentially delivered to the second solvent storage tank through the first condenser, the flow guide section, and the third shunt section of the delivery element.

[0050] In some embodiments, the method further comprises the following steps:

[0051] The first part of the volume of the filtrate in the absorption tank is sequentially delivered to the hydrolysis reactor and the first filter;

[0052] The filtrate in the upper layer of the filtrate layer in the first filter is delivered to the organic phase separator, and the solid in the lower layer of the precipitate layer in the first filter is delivered to the primary fluorine extractor;

[0053] The aqueous phase in the filtrate in the organic phase separator is delivered to the phosphorus extractor, and the organic phase in the filtrate in the organic phase separator is delivered to the electrolyte leaching device;

[0054] The kettle liquid in the phosphorus extractor is sequentially delivered to the second filter, the impurity metal separator, the third filter, the primary fluorine extractor, the fourth filter, the lithium extractor, the fifth filter, and the secondary fluorine extractor, and then delivered to the sixth filter.

[0055] In some embodiments, nitrogen is introduced into the hydrolysis reactor, water, 1%-2% by mass of hydrochloric acid, and tributyl phosphate are added, the volume of water is 20%-30% of the volume of the kettle liquid in the hydrolysis reactor, the volume of hydrochloric acid is 2%-8% of the volume of the kettle liquid in the hydrolysis reactor, and the amount of tributyl phosphate is 0.005-0.01:1 by mass ratio of lithium hexafluorophosphate in the waste electrolyte; the internal pressure of the hydrolysis reactor is 0.2-0.5 MPa, the hydrolysis temperature is 30-50℃, and the hydrolysis time is 30-90 min;

[0056] And / or, ferric chloride is added to the phosphorus extractor, and the amount of ferric chloride is 1.1-1.3:1 by mass ratio of lithium hexafluorophosphate in the waste electrolyte;

[0057] And / or, the pH of the impurity metal separator is adjusted to 3-4 with a 5% by mass sodium hydroxide solution, and 5% by mass sodium carbonate is added;

[0058] And / or, a 5%-10% by mass calcium hydroxide suspension is added to the primary fluorine extractor, the amount of calcium hydroxide is 2.8-2.9:1 by mass ratio of lithium hexafluorophosphate in the waste electrolyte, the pH is adjusted to 9-10 with a 5% by mass sodium hydroxide solution, the temperature is raised to 50-70℃, and the stirring reaction time is 60-90 min;

[0059] And / or, carbon dioxide is filled into the lithium extractor, the pressure in the lithium extractor is maintained at 0.2-0.3 MPa, and the pressure is maintained at an internal temperature of 60-80℃ for 40-120 min;

[0060] And / or, 5%~10% mass fraction of calcium chloride solution is added into the secondary fluorine extractor, the amount of calcium chloride is 0.2-0.6:1 of the mass ratio of lithium hexafluorophosphate in the waste electrolyte, the pH is adjusted to 9~10 by 5% mass fraction of sodium hydroxide solution, and the stirring reaction is carried out for 30min~60min.

[0061] In some embodiments, the method further comprises the step of:

[0062] delivering the liquor in the electrolyte leaching tank to the solvent extractor;

[0063] delivering the second part of the volume of the filtrate in the first solvent tank to the solvent extractor;

[0064] delivering the gas in the absorption tank to the solvent extractor after passing through the second condenser.

[0065] The device for recycling waste lithium battery electrolyte provided by the embodiment of the present application can solve the problem that the solvent and electrolyte in the electrolyte cannot be recycled, which causes waste of resources of the solvent and electrolyte.

[0066] Therefore, the device for recycling waste lithium battery electrolyte provided by the embodiment of the present application can solve the problem that the solvent and electrolyte in the electrolyte cannot be recycled, which causes waste of resources of the solvent and electrolyte. BRIEF DESCRIPTION OF DRAWINGS

[0067] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or prior art description. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0068] Figure 1 The main structure schematic diagram of the device for recycling waste lithium battery electrolyte provided by the embodiment of the present application;

[0069] Figure 2 The flow chart of the method for recycling waste lithium battery electrolyte provided by the embodiment of the present application.

[0070] Reference signs:

[0071] 100 - solvent extractor;

[0072] 101 - first condenser;

[0073] 102 - transport; 1021 - flow guide section; 1022 - first flow division section; 1023 - second flow division section; 1024 - third flow division section;

[0074] 103 - absorption tank; 1031 - first output; 1032 - second output;

[0075] 104 - first valve;

[0076] 105 - first solvent reservoir;

[0077] 106 - second valve;

[0078] 107 - second solvent reservoir;

[0079] 108 - third valve;

[0080] 109 - vacuum;

[0081] 110 - second condenser;

[0082] 111 - hydrolysis reactor;

[0083] 112 - electrolyte leacher;

[0084] 113 - first filter;

[0085] 114 - organic phase separator; 1141 - liquid inlet; 1142 - first liquid outlet; 1143 - second liquid outlet;

[0086] 115 - primary fluorine extractor;

[0087] 116 - phosphorus extractor;

[0088] 117 - second filter;

[0089] 118 - impurity metal separator;

[0090] 119 - third filter;

[0091] 120 - fourth filter;

[0092] 121 - lithium extractor;

[0093] 122 - fifth filter;

[0094] 123 - secondary fluorine extractor;

[0095] 124 - sixth filter element. DETAILED DESCRIPTION

[0096] In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some but not all of the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative work fall within the protection scope of the present application. The following embodiments and features in the embodiments can be combined with each other without conflict.

[0097] In the prior art, the lithium battery electrolyte contains organic solvents dimethyl carbonate (DMC), diethyl carbonate (DEC), ethylene carbonate (EC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), and electrolyte lithium hexafluorophosphate (LiPF6) and a small amount of metal elements (cobalt Co, nickel Ni, etc.).

[0098] Among them, dimethyl carbonate will begin to decompose obviously at a temperature greater than 150 degrees Celsius to generate methanol and carbon dioxide, and will accelerate decomposition at a temperature greater than 200 degrees Celsius, and may also produce byproducts such as formaldehyde and methane.

[0099] Among them, lithium hexafluorophosphate begins to decompose obviously above 60 degrees Celsius into phosphorus pentafluoride (PF5) and lithium fluoride (LiF) precipitate, and as the temperature increases, the decomposition reaction rate will increase.

[0100] Further, both phosphorus pentafluoride and hydrogen fluoride are dissolved in dimethyl carbonate.

[0101] Further, phosphorus pentafluoride can also react with water to generate phosphorus oxyfluoride (POF3) and hydrogen fluoride (HF), and phosphorus oxyfluoride will further react with water to generate phosphoric acid (H3PO4) and hydrogen fluoride gas.

[0102] In addition, lithium hexafluorophosphate will also decompose under the catalysis of water to generate phosphorus oxyfluoride, lithium fluoride (LiF) precipitate and hydrogen fluoride gas, and phosphorus oxyfluoride will further react with water to generate phosphoric acid (H3PO4) and hydrogen fluoride gas.

[0103] Further, hydrogen fluoride is miscible with water in any proportion at room temperature (20°C).

[0104] Therefore, when pyrolysis is performed after the battery is broken (pyrolysis temperature is greater than or equal to 200 degrees Celsius), the organic solvent dimethyl carbonate in the electrolyte and the electrolyte lithium hexafluorophosphate volatilize, and hydrogen fluoride gas generated by volatilization of lithium hexafluorophosphate volatilizes, and the hydrogen fluoride gas is miscible with the solvent in the alkali solution, so that the solvent and the electrolyte in the electrolyte cannot be recovered, and resources of the solvent and the electrolyte are wasted.

[0105] In order to overcome the defects in the prior art, by setting the solvent extractor, the filtrate of the lithium battery can be distilled to separate the solvent, the electrolyte and the decomposition product of the electrolyte in the filtrate, by setting the first condenser, the distillate can be cooled, by setting the absorption tank, the distilled decomposition product phosphorus pentafluoride and hydrogen fluoride can be absorbed, by setting the first solvent storage tank, the distilled solvent can be stored, the electrolyte and the residual material in the filtrate are stored in the solvent extractor, by setting the first valve and the second valve, the direction of the distillate can be controlled, when the first valve is opened and the second valve is closed, the distillate can be transported to the absorption tank, and when the first valve is closed and the second valve is opened, the distillate can be transported to the first solvent storage tank.

[0106] Therefore, the device for recycling waste lithium battery electrolyte provided by the embodiment of the present application can solve the problem that the solvent and the electrolyte in the electrolyte cannot be recovered, and resources of the solvent and the electrolyte are wasted.

[0107] The content of the present application will be described in detail below with reference to the accompanying drawings, so that those skilled in the art can more clearly and detailedly understand the content of the present application.

[0108] As Figure 1As shown, the embodiment of the present application provides a device for full recovery of waste lithium battery electrolyte, which comprises a solvent extractor 100, a first condenser 101, a conveying member 102, an absorption tank 103, a first valve 104, a first solvent storage tank 105 and a second valve 106. The solvent extractor 100 is used for containing filtrate of the lithium battery. The first condenser 101 is connected to the solvent extractor 100. The conveying member 102 has a communication flow guide section 1021, a first shunt section 1022 and a second shunt section 1023. The first shunt section 1022 and the second shunt section 1023 are connected in parallel. The absorption tank 103 is connected to the first shunt section 1022. The first valve 104 is connected to the first shunt section 1022. The first valve 104 is used for opening or closing the communication between the first shunt section 1022 and the absorption tank 103. One end of the first solvent storage tank 105 is connected to the second shunt section 1023. The other end of the first solvent storage tank 105 is connected to the solvent extractor 100. The second valve 106 is connected to the second shunt section 1023. The second valve 106 is used for opening or closing the communication between the second shunt section 1023 and the first solvent storage tank 105.

[0109] The specific structure of the device and method for full recovery of waste lithium battery electrolyte and various possible implementation manners are described in detail below.

[0110] It should be noted that the fraction flowing out of the first condenser 101 can enter the absorption tank 103 after passing through the first shunt section 1022 and the first valve 104, so that the decomposition products phosphorus pentafluoride and hydrogen fluoride in the filtrate can enter the absorption tank 103.

[0111] It should be noted that water is arranged in the absorption tank 103. The water can react with phosphorus pentafluoride in the filtrate to generate phosphoric acid and hydrogen fluoride, and dissolve the hydrogen fluoride.

[0112] It can be understood that the phosphorus pentafluoride and hydrogen fluoride can be absorbed through the above implementation manner.

[0113] It should be noted that the fraction flowing out of the first condenser 101 can enter the first solvent storage tank 105 after passing through the second shunt section 1023 and the second valve 106, so that the solvent in the filtrate can enter the absorption tank 103.

[0114] It should be noted that when the first solvent tank 105 stores the distilled solvent, the internal temperature of the solvent extractor 100 can be adjusted to above 80 degrees Celsius, so that dimethyl carbonate, diethyl carbonate, ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate can enter the first solvent tank 105 as a fraction at the same time. Or the internal temperature of the solvent extractor 100 can be adjusted to 50-70 degrees Celsius, so that dimethyl carbonate enters the first solvent tank 105 as a fraction, and then the internal temperature of the solvent extractor 100 is adjusted to above 80 degrees Celsius, so that diethyl carbonate, ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate can enter the first solvent tank 105 as a fraction at the same time. Specifically, the extraction method of the solvent is not limited, and can be selected according to actual use requirements.

[0115] The conveying member 102 provided by the embodiment of the present application has a third shunt section 1024 in communication with the flow guide section 1021, and the third shunt section 1024 is arranged in parallel with the first shunt section 1022. The device for fully recycling waste lithium battery electrolyte further comprises a second solvent tank 107, a third valve 108, and a vacuum member 109. The second solvent tank 107 is arranged in communication with the third shunt section 1024. The third valve 108 is arranged in communication with the third shunt section 1024. The third valve 108 is used to open or close the communication between the third shunt section 1024 and the second solvent tank 107. The vacuum member 109 is arranged in communication with the solvent extractor 100.

[0116] It can be understood that through the above-mentioned embodiments, the fraction flowing out of the first condenser 101 can enter the second solvent tank 107 after passing through the third shunt section 1024 and the third valve 108, so that the dimethyl carbonate in the solvent and other components in the solvent are separated.

[0117] In one embodiment, the solvent extractor 100 is heated to between 30 and 50 degrees Celsius, the first condenser 101 is arranged to have a condensation temperature of between 5 and 10 degrees Celsius, then the first valve 104 is opened, and the second valve 106 and the third valve 108 are closed. The fraction in the solvent extractor 100 can flow into the absorption tank 103 after passing through the first condenser 101, the flow guide section 1021, and the first shunt section 1022. The water in the absorption tank 103 can absorb phosphorus pentafluoride and hydrogen fluoride.

[0118] It can be understood that through the above-mentioned embodiments, the corrosive gas in the filtrate can be separated in advance, and is not entrained with the organic solvent. The insoluble matter is mainly the organic solvent.

[0119] Further, after the outlet of the first condenser 101 is free of distillate, the first valve 104 is closed, the vacuum device 109 is opened, and the vacuum degree in the solvent extractor 100 is between -0.095 MPa and -0.0905 MPa, the condensation temperature of the first condenser 101 is adjusted to between -10 degrees Celsius and 0 degrees Celsius, the solvent extractor 100 is heated in stages to between 100 degrees Celsius and 120 degrees Celsius, and the distillate in the solvent extractor 100 can flow into the first solvent storage tank 105 through the first condenser 101, the flow guide section 1021, and the second flow dividing section 1023, or the distillate in the solvent extractor 100 can flow into the second solvent storage tank 107 through the first condenser 101, the flow guide section 1021, and the third flow dividing section 1024.

[0120] It should be noted that the heating in stages to between 100 degrees Celsius and 120 degrees Celsius can be: heating in stages by 50 degrees Celsius to 70 degrees Celsius for 40 minutes to 60 minutes, heating in stages by 80 degrees Celsius to 100 degrees Celsius for 20 minutes to 30 minutes, and then continuing to heat to between 100 degrees Celsius and 120 degrees Celsius.

[0121] Further, when the internal temperature of the solvent extractor 100 is in the range of 50 degrees Celsius to 70 degrees Celsius, the first valve 104 is closed, the second valve 106 is opened, and the third valve 108 is closed, the outflowing distillate flows into the first solvent storage tank 105 through the first condenser 101, the flow guide section 1021, and the second flow dividing section 1023, and is mainly dimethyl carbonate.

[0122] Further, when the internal temperature of the solvent extractor 100 is in the range of 80 degrees Celsius to 100 degrees Celsius, the first valve 104 is closed, the second valve 106 is closed, and the third valve 108 is opened, the outflowing distillate flows into the second solvent storage tank 107 through the first condenser 101, the flow guide section 1021, and the third flow dividing section 1024, and is mainly diethyl carbonate, ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate.

[0123] Further, the organic solvent in the first solvent storage tank 105 is dimethyl carbonate, which can be directly used as a leaching solvent; and the organic solvent in the second solvent storage tank 107 can be subjected to negative pressure rectification to separate diethyl carbonate, propylene carbonate, ethylene carbonate, and methyl ethyl carbonate therefrom.

[0124] It can be understood that, through the above embodiment, the lithium hexafluorophosphate can be prevented from decomposing through heating in stages, and diethyl carbonate, which is the main component in the material, can be concentrated in the first solvent storage tank 105 for reuse in leaching the filtrate of the lithium battery. The material in the solvent extractor 100 is the electrolyte lithium hexafluorophosphate, and the remaining organic solvent in the solvent extractor 100 can prevent the filtrate from being excessively heated, thereby preventing the lithium hexafluorophosphate from decomposing.

[0125] The embodiment of the present application provides the absorption tank 103 with a first output end 1031 and a second output end 1032, and the device for fully recycling waste lithium battery electrolyte further comprises a second condenser 110 and a hydrolysis reactor 111, one end of the second condenser 110 is communicated with the first output end 1031, the other end of the second condenser 110 is communicated with the solvent extractor 100, the hydrolysis reactor 111 is communicated with the absorption tank 103 through the second output end 1032, and the hydrolysis reactor 111 is arranged in communication with the solvent extractor 100.

[0126] It can be understood that, through the above embodiment, the gas in the absorption tank 103 can be conveyed to the solvent extractor 100 through the first output end 1031 and the second condenser 110, the liquid in the absorption tank 103 can be conveyed into the hydrolysis reactor 111 through the second conveying end, and in addition, the kettle liquid in the solvent extractor 100 can be conveyed into the hydrolysis reactor 111.

[0127] In one embodiment, the kettle liquid in the solvent extractor 100 is conveyed into the hydrolysis reactor 111, nitrogen is introduced into a sealed environment, water, hydrochloric acid with a concentration ranging from 1% to 2%, and tributyl phosphate are added. The hydrolysis reactor 111 contains a stirring device, and the hydrolysis reaction is fully stirred. After the hydrolysis reactor 111 is cooled to room temperature, the pressure is released to normal pressure, and solid lithium fluoride can be formed.

[0128] Further, lithium hexafluorophosphate, water, and hydrochloric acid react to generate lithium fluoride, hydrogen fluoride, phosphoric acid and other by-products, nitrogen can be used as an inert protective gas to prevent lithium hexafluorophosphate or generated hydrogen fluoride from being oxidized by oxygen, tributyl phosphate can be used as a solvent or an extractant, and can also promote the precipitation and separation of lithium fluoride.

[0129] The embodiment of the present application provides the device for fully recycling waste lithium battery electrolyte, and the device further comprises an electrolyte leaching device 112, the electrolyte leaching device 112 is arranged in communication with the solvent extractor 100, the electrolyte leaching device 112 is used for conveying filtrate to the solvent extractor 100, and the electrolyte leaching device 112 is in communication with the first solvent storage tank 105.

[0130] It can be understood that by setting the electrolyte leaching device 112, the disassembled, crushed and broken lithium battery and its electrolyte, and the dimethyl carbonate solvent can be contained, so that the disassembled, crushed and broken lithium battery and its electrolyte can be soaked together in the dimethyl carbonate solvent, and the filtrate is delivered to the solvent extractor 100. In some embodiments, by the electrolyte leaching device 112, the filtrate can also be ultrasonically leached and filtered to improve the leaching efficiency of the filtrate and filter the impurities in the filtrate. Further, the electrolyte leaching device 112 is in communication with the first solvent tank 105, so that the dimethyl carbonate in the first solvent tank 105 can be refluxed to the electrolyte leaching device 112 to soak the disassembled, crushed and broken lithium battery and its electrolyte.

[0131] The device for recycling waste lithium battery electrolyte provided by the embodiments of the present application further comprises a first filter 113, an organic phase separator 114 and a primary fluorine extractor 115. The first filter 113 is in communication with the hydrolysis reactor 111, and the inner part of the first filter 113 is layered to form an upper layer of filtrate and a lower layer of precipitate. The organic phase separator 114 has a liquid inlet end 1141, a first liquid outlet end 1142 and a second liquid outlet end 1143. The liquid inlet end 1141 is in communication with the upper layer of filtrate, and the first liquid outlet end 1142 is in communication with the electrolyte leaching device 112. The primary fluorine extractor 115 is in communication with the lower layer of precipitate.

[0132] It can be understood that by setting the first filter 113, the product in the hydrolysis reactor 111 can be filtered, and the solid lithium fluoride forms the lower layer of precipitate, and the other substances that are not precipitated form the upper layer of filtrate. By setting the organic phase separator 114, the filtrate in the upper layer of filtrate can be separated into water phase and organic phase, and the separated organic phase can be delivered to the electrolyte leaching device 112 for recycling. By setting the primary fluorine extractor 115, the solid lithium fluoride in the lower layer of precipitate can be collected.

[0133] In one embodiment, the volume of water used in the hydrolysis reactor 111 is between 20% and 30% of the volume of the liquid in the reactor; the volume of hydrochloric acid used is between 2% and 8% of the volume of the liquid in the reactor; and the mass ratio of the amount of phosphoric acid tributyl ester to the amount of lithium hexafluorophosphate in the waste electrolyte is 0.005-0.01:1.

[0134] Further, the internal pressure of the hydrolysis reactor 111 by introducing nitrogen is between 0.2 Mpa and 0.5 Mpa, the hydrolysis temperature is between 30 degrees Celsius and 50 degrees Celsius, and the hydrolysis time is between 30 minutes and 90 minutes.

[0135] It can be understood that the kettle liquid in the solvent extractor 100 contains a small amount of organic solvent and lithium hexafluorophosphate, which is decomposed into lithium fluoride precipitate, phosphoric acid and hydrogen fluoride, and the hydrogen fluoride is basically dissolved in water under pressure. The phosphoric acid tributyl ester can be complexed with phosphorus-containing substances to inhibit the vaporization of phosphorus-containing substances. The organic phase solvent separated by the organic separator is separated by extraction and can be refluxed to the electrolyte leaching device 112.

[0136] The device for fully recycling waste lithium battery electrolyte provided by the embodiment of the present application further comprises a phosphorus extractor 116, a second filter 117, an impurity metal separator 118, a third filter 119, a fourth filter 120, a lithium extractor 121, a fifth filter 122, a secondary fluorine extractor 123 and a sixth filter 124. The phosphorus extractor 116 is in communication with the second liquid outlet 1143, the second filter 117 is in communication with the hydrolysis reactor 111, the impurity metal separator 118 is in communication with the second filter 117, the third filter 119 is in communication with the impurity metal separator 118 and the primary fluorine extractor 115, the fourth filter 120 is in communication with the primary fluorine extractor 115, the lithium extractor 121 is in communication with the fourth filter 120, the fifth filter 122 is in communication with the lithium extractor 121, and the sixth filter 124 is in communication with the secondary fluorine extractor 123.

[0137] It can be understood that by arranging the phosphorus extractor 116, the phosphoric acid in the water phase solvent can react to generate phosphorus-containing precipitates to recover the phosphorus in the water phase solvent, by arranging the impurity metal separator 118, the impurity metal can be removed from the water phase solvent after the removal of phosphorus, by arranging the primary fluorine extractor 115, the fluorine can be recovered from the water phase solvent after the removal of impurity metal, by arranging the lithium extractor 121, the lithium can be recovered from the water phase solvent after the recovery of fluorine, and by arranging the secondary fluorine extractor 123, the fluorine can be recovered from the water phase solvent after the recovery of lithium. Thus, the organic solvent, high-value lithium, fluorine and phosphorus elements in the waste lithium battery electrolyte can be fully recovered, and the impurity metal in the waste lithium battery can be removed. By arranging the second filter 117, the third filter 119, the fourth filter 120, the fifth filter 122 and the sixth filter 124, different impurities in the water phase solvent can be filtered to achieve different precipitation and filtration and separation of the filtrate in different stages.

[0138] In one embodiment, in the phosphorus extractor 116, ferric chloride is added and stirred for 20 to 40 minutes, and then the stirred solution is delivered to the second filter 117. The solid separated by the second filter 117 is ferric phosphate, and the filtrate separated by the second filter 117 is delivered to the impurity metal separator 118.

[0139] Further, the amount of ferric chloride is 1.1-1.3:1 by mass ratio of lithium hexafluorophosphate in the waste electrolyte.

[0140] It can be understood that, through the above-mentioned embodiments, the phosphoric acid reacts with the ferric chloride to generate a ferric phosphate precipitate.

[0141] It should be noted that the waste lithium battery contains impurity metals such as nickel and cobalt.

[0142] In an embodiment, the impurity metal separator 118 adjusts the pH to 3-4 with a 5% concentration of sodium hydroxide solution, slowly adds a 5% mass fraction of sodium carbonate solution until no precipitate is generated, and is transported to the third filter 119 to separate a carbonate solid containing impurity metals such as nickel and cobalt; the filtrate separated by the third filter 119 is transported to the primary fluorine extractor 115.

[0143] It can be understood that, through the above-mentioned embodiments, the impurity metals such as nickel and cobalt and the excess ferric chloride react with the sodium carbonate solution to generate a metal carbonate precipitate.

[0144] Further, the precipitate can be dissolved with an acid to realize recycling of metal elements such as nickel, cobalt, and iron.

[0145] In an embodiment, in the primary fluorine extractor 115, a calcium hydroxide suspension with a mass fraction of 5%-10% is added, the mass ratio of calcium hydroxide to lithium hexafluorophosphate in the waste electrolyte is 2.8-2.9:1, the pH is adjusted to 9-10 by a 5% mass fraction of sodium hydroxide solution, the primary fluorine extractor 115 is heated to 50-70 degrees Celsius, and the stirring reaction time is 60-90 minutes. The solid separated by the fourth filter 120 is calcium fluoride, and the filtrate filtered by the fourth filter 120 is transferred to the lithium extractor 121.

[0146] Further, the solid separated by the fourth filter 120 is calcium fluoride, a 5% hydrochloric acid solution is added to wash the alkaline impurities, and after drying, calcium fluoride with a purity of more than 98% is obtained, which can also be used to prepare high-purity hydrogen fluoride by acidolysis.

[0147] It can be understood that, through the above-mentioned embodiments, the appropriate amount of calcium hydroxide is added, and the pH is adjusted by a sodium hydroxide solution to dissolve the solid lithium fluoride and precipitate the fluorine element, without introducing excess calcium elements to avoid affecting the purity of lithium carbonate in the subsequent lithium extraction.

[0148] Further, the lithium fluoride and the calcium hydroxide are converted into soluble lithium hydroxide and insoluble calcium fluoride.

[0149] In one embodiment, carbon dioxide is introduced into the lithium extractor 121 and the pressure is maintained to react until no precipitation is produced. Lithium carbonate solid is filtered through the fifth filter element 122 and dried to obtain battery-grade lithium carbonate. The filtrate after filtering through the fifth filter element 122 is transported to the secondary fluorine extractor 123.

[0150] Furthermore, the carbon dioxide charging pressure in the lithium extractor 121 is maintained at 0.2 MPa to 0.3 MPa, and the pressure is maintained at an internal temperature of 60 to 80 degrees Celsius for 40 to 120 minutes.

[0151] It can be understood that, through the above embodiment, lithium carbonate can be extracted.

[0152] In one embodiment, a 5% to 10% by mass calcium chloride solution is added to the secondary fluorine extractor 123, with a mass ratio of calcium chloride to lithium hexafluorophosphate in the spent electrolyte of 0.2-0.6:1. The pH is adjusted to 9-10 using a 5% sodium hydroxide solution, and the reaction is stirred for 30 to 60 minutes. The solid matter separated by the sixth filter element 124 is calcium fluoride.

[0153] It can be understood that, through the above embodiment, the remaining fluorine element in the filtrate after lithium extraction can be effectively precipitated, so that the residual concentration of fluorine element can be reduced to within 10 ppm.

[0154] like Figure 2 As shown, an embodiment of the present application provides a method for fully recycling waste lithium battery electrolyte, which is applied to the device for fully recycling waste lithium battery electrolyte provided in any of the above embodiments, and the method includes the following steps:

[0155] S701: transporting the filtrate of the lithium battery to the solvent extractor 100;

[0156] S702: Open the first valve 104 and close the second valve 106 to adjust the first condenser 101 to a first temperature, so that a first portion of the volume of filtrate passes through the first condenser 101, the guide section 1021 of the conveying member 102, and the first diversion section 1022 of the conveying member 102 in sequence, and is conveyed to the absorption tank 103;

[0157] S703: Close the first valve 104, open the second valve 106, and adjust the first condenser 101 to the second temperature so that the second partial volume of filtrate passes through the first condenser 101, the guide section 1021 and the second diversion section 1023 of the conveying member 102 in sequence and is conveyed to the first solvent storage tank 105.

[0158] It can be understood that through the above implementation, the solvent extractor 100 can distill the filtrate of the lithium battery to separate the solvent, electrolyte and decomposition product of the electrolyte in the filtrate, by setting the first condenser 101, the distilled fraction can be cooled, by setting the absorption tank 103, the distilled decomposition product phosphorus pentafluoride and hydrogen fluoride can be absorbed, by setting the first solvent storage tank 105, the distilled solvent can be stored, the electrolyte and residual substances in the filtrate will be stored in the solvent extractor 100, by setting the first valve 104 and the second valve 106, the direction of the distilled fraction can be controlled, when the first valve 104 is opened and the second valve 106 is closed, the fraction can be transported to the absorption tank 103, when the first valve 104 is closed and the second valve 106 is opened, the fraction can be transported to the first solvent storage tank 105.

[0159] Therefore, the device for recycling waste lithium battery electrolyte provided by the embodiment of the present application can solve the problem that the solvent and electrolyte in the electrolyte cannot be recycled, which causes waste of resources of the solvent and electrolyte.

[0160] The embodiment of the present application provides a method for recycling waste lithium battery electrolyte, which comprises the following steps:

[0161] It can be understood that through the above implementation, when the first condenser 101 is adjusted to the first temperature, the fraction flowing out of the first condenser 101 can only pass through the flow guide section 1021 of the conveying member 102 and the first shunt section 1022 of the conveying member 102, and be transported to the absorption tank 103, so that the fraction is transported into the absorption tank 103.

[0162] The embodiment of the present application provides a method for recycling waste lithium battery electrolyte, which comprises the following steps:

[0163] It can be understood that through the above implementation, when the first condenser 101 is adjusted to the second temperature, the fraction flowing out of the first condenser 101 can only pass through the flow guide section 1021 and the second shunt section 1023 of the conveying member 102, and be transported to the first solvent storage tank 105, so that the fraction is transported into the first solvent storage tank 105.

[0164] The embodiment of the present application provides a method for recycling waste lithium battery electrolyte, which comprises the following steps:

[0165] Close the first valve 104, close the second valve 106, open the third valve 108, and adjust the first condenser 101 to the third temperature, so that the third part of the filtrate sequentially passes through the first condenser 101, the flow guide section 1021 and the third flow section 1024 of the conveying member 102, and is conveyed to the second solvent tank 107.

[0166] It can be understood that the fraction flowing out of the first condenser 101 can enter the second solvent tank 107 through the third flow section 1024 and the third valve 108, so that the dimethyl carbonate in the solvent and other components in the solvent are separated.

[0167] The method for fully recycling waste lithium battery electrolyte provided by the embodiment of the application further includes the following steps:

[0168] The first part of the volume of the filtrate in the absorption tank 103 is sequentially conveyed to the hydrolysis reactor 111 and the first filter 113;

[0169] The filtrate in the upper filtrate layer in the first filter 113 is conveyed to the organic phase separator 114, and the solid in the lower precipitate layer in the first filter 113 is conveyed to the primary fluorine extractor 115;

[0170] The aqueous phase in the filtrate in the organic phase separator 114 is conveyed to the phosphorus extractor 116, and the organic phase in the filtrate in the organic phase separator 114 is conveyed to the electrolyte leaching device 112;

[0171] The kettle liquid in the phosphorus extractor 116 sequentially passes through the second filter 117, the impurity metal separator 118, the third filter 119, the primary fluorine extractor 115, the fourth filter 120, the lithium extractor 121, the fifth filter 122, the secondary fluorine extractor 123, and is conveyed to the sixth filter 124.

[0172] It can be understood that through the above embodiment, the first part of the volume of the filtrate in the absorption tank 103 can be fully recycled for lithium, fluorine and phosphorus elements, and impurity metals in the first part of the volume of the filtrate can be removed.

[0173] It should be noted that nitrogen is introduced into the hydrolysis reactor 111, water, 1%-2% mass fraction of hydrochloric acid and phosphoric acid tributyl ester are added, the volume of water is 20%-30% of the volume of the kettle liquid in the hydrolysis reactor 111, the volume of hydrochloric acid is 2%-8% of the volume of the kettle liquid in the hydrolysis reactor 111, and the amount of phosphoric acid tributyl ester is 0.005-0.01:1 in mass ratio of lithium hexafluorophosphate in the waste electrolyte; the internal pressure of the hydrolysis reactor 111 is 0.2-0.5 MPa, the hydrolysis temperature is 30-50℃, and the hydrolysis time is 30-90 min.

[0174] It can be understood that the kettle liquid in the solvent extractor 100 contains a small amount of organic solvent and lithium hexafluorophosphate, which is decomposed into lithium fluoride precipitation, phosphoric acid and hydrogen fluoride, and the hydrogen fluoride is basically dissolved in water under pressure. The phosphoric acid tributyl ester can be complexed with phosphorus-containing substances to inhibit the vaporization of phosphorus-containing substances. The organic phase solvent separated by the organic separator is separated by extraction and can be refluxed to the electrolyte leaching device 112.

[0175] It should be noted that the iron chloride is added to the phosphorus extractor 116, and the mass ratio of the amount of iron chloride to lithium hexafluorophosphate in the waste electrolyte is 1.1-1.3:1.

[0176] It can be understood that through the above embodiment, the phosphoric acid reacts with the iron chloride to generate iron phosphate precipitation.

[0177] It should be noted that the impurity metal separator 118 is adjusted to a pH of 3-4 with a 5% mass fraction of sodium hydroxide solution, and 5% mass fraction of sodium carbonate is added.

[0178] It can be understood that through the above embodiment, the impurity metals such as nickel and cobalt and excess iron chloride react with the sodium carbonate solution to generate metal carbonate precipitate.

[0179] It should be noted that a 5%-10% mass fraction of calcium hydroxide suspension is added to the primary fluorine extractor 115, the mass ratio of the amount of calcium hydroxide to lithium hexafluorophosphate in the waste electrolyte is 2.8-2.9:1, and the pH is adjusted to 9-10 by 5% mass fraction of sodium hydroxide solution, and the temperature is raised to 50-70°C, and the stirring reaction time is 60-90 min.

[0180] It can be understood that through the above embodiment, the appropriate amount of calcium hydroxide is added, and the pH is adjusted by sodium hydroxide solution, which can dissolve the solid lithium fluoride and precipitate the fluorine element, and does not introduce excess calcium element to avoid affecting the purity of lithium carbonate during subsequent lithium extraction.

[0181] It should be noted that the lithium extractor 121 is filled with carbon dioxide, the pressure in the lithium extractor 121 is maintained at 0.2-0.3 MPa, and the pressure is maintained at an internal temperature of 60-80°C for 40-120 min.

[0182] It can be understood that through the above embodiment, the lithium carbonate can be extracted.

[0183] It should be noted that a 5%-10% mass fraction of calcium chloride solution is added to the secondary fluorine extractor 123, the mass ratio of the amount of calcium chloride to lithium hexafluorophosphate in the waste electrolyte is 0.2-0.6:1, the pH is adjusted to 9-10 by 5% mass fraction of sodium hydroxide solution, and the stirring reaction time is 30-60 min.

[0184] It can be understood that through the above embodiment, the residual fluorine element in the filtrate after lithium extraction can be effectively settled, so that the residual concentration of fluorine element can be reduced to within 10 ppm.

[0185] The method for full recovery of waste lithium battery electrolyte provided by the embodiment of the application further includes the following steps:

[0186] The kettle liquid in the electrolyte leaching device 112 is transported to the solvent extractor 100;

[0187] The second part of the volume of the filtrate in the first solvent tank 105 is transported to the solvent extractor 100;

[0188] The gas in the absorption tank 103 is transported to the solvent extractor 100 after passing through the second condenser 110.

[0189] It can be understood that through the above embodiment, the organic solvent can be recovered, the corrosive gas can be preliminarily separated, and the dimethyl carbonate with a large content can be collected and directly reused as the leaching solvent in the solvent extractor 100.

[0190] In one embodiment, a method for full recovery of waste lithium battery electrolyte includes the following steps:

[0191] Step one: the broken lithium battery and dimethyl carbonate are transported to the electrolyte leaching device 112, after the dimethyl carbonate leaches the broken lithium battery, waste electrolyte liquid containing 8% lithium hexafluorophosphate is formed, and 500 kg of the liquid is transported to the solvent extractor 100.

[0192] Step two: the solvent extractor 100 is heated to 30-50 degrees Celsius, the first condenser 101 is set to a condensation temperature of 10 degrees Celsius, the first valve 104 is opened, the second valve 106 is closed, and the third valve 108 is closed, the distillate is introduced into the absorption tank 103, water is used to absorb the phosphorus pentafluoride and hydrogen fluoride gas therein, the insoluble substances in the absorption tank 103 are condensed by the second condenser 110 and then returned to the solvent extractor 100, and the liquid in the absorption tank 103 is transported to the hydrolysis reactor 111.

[0193] Step three: after the first condenser 101 outlet without distillate distillation, close the first valve 104, open the vacuum 109, and keep the solvent extractor 100 vacuum degree-0.095Mpa, set the condenser 1 condensing temperature to-10 degrees Celsius, the solvent extractor 100 is heated to 70 degrees Celsius in stages, keep 50 minutes, open the second valve 106 door, close the third valve 108, the outflow fraction is passed into the first solvent tank 105, at this time, the distillate is 275 kilograms of dimethyl carbonate; close the second valve 106, open the third valve 108, continue to heat to 90 degrees Celsius for 20 minutes, continue to heat to 120 degrees Celsius, during which the outflow fraction is passed into the second solvent tank 107, at this time, the distillate is 150 kilograms in total; further separation of diethyl carbonate, ethylene carbonate, diethyl carbonate, and methyl ethyl carbonate can be obtained by negative pressure rectification. Subsequently, after observing that the material kettle liquid in the solvent extractor 100 does not boil, stop heating.

[0194] Step four: the kettle liquid in the solvent extractor 100 is transported to the hydrolysis reactor 111, nitrogen is introduced into the hydrolysis reactor 111 under a sealed environment to a pressure of 0.3Mpa, 15 L of water, 2L of 2% hydrochloric acid, and 0.5 kilograms of tributyl phosphate are added, the hydrolysis reactor 111 is set to a hydrolysis temperature of 40 degrees Celsius, the stirring hydrolysis time is 50 minutes, after the hydrolysis reactor 111 cools to room temperature, it is depressurized to normal pressure, passes through the first filter 113, separates the solid material as lithium fluoride, and transports the lithium fluoride to the primary fluorine extractor 115; the filtrate enters the organic phase separator 114, after extraction and separation, the aqueous phase is transported to the phosphorus extractor 116, and the organic phase is transported back to the electrolyte leaching device 112 after drying.

[0195] Step five: in the phosphorus extractor 116, 46.8 kilograms of iron chloride are added, wherein the mass ratio of iron chloride to lithium hexafluorophosphate is 1.1:1, stirring for 30 minutes, then transported to the second filter 117, separating the solid material, and the filtrate is transported to the impurity metal separator 118, wherein the solid is dried to be 38.8 kilograms of iron phosphate.

[0196] Step six: in the impurity metal separator 118, the pH is adjusted to 3 with 5% sodium hydroxide solution, 5% mass fraction of sodium carbonate solution is slowly added until no precipitate is generated, transported to the third filter 119 to separate the solid; the filtrate is transported to the primary fluorine extractor 115. The solid is the carbonate of nickel, cobalt, and other impurity metals and excess iron, which is dried to be 7.5 kilograms, and can be further acid-dissolved and precipitated to gradient extract nickel, cobalt, iron, and other metal elements

[0197] Step seven: in the first fluorine extractor 115, 54.5 kg of 10% mass fraction calcium hydroxide suspension is added, the mass ratio of calcium hydroxide to lithium hexafluorophosphate is 2.8:1, the pH is adjusted to 9 by 5% sodium hydroxide solution, the temperature is raised to 60 degrees Celsius, and the stirring reaction is carried out for 8 minutes. The solid is separated by the fourth filter 120, and the filtrate is transferred to the lithium extractor 121. After drying, 57.1 kg of calcium fluoride with a purity of 98.5% is obtained.

[0198] Step eight: in the lithium extractor 121, carbon dioxide is filled to make the internal pressure of the lithium extractor 121 0.2 Mpa, and the stirring reaction is carried out until no precipitate is generated. The solid is filtered by the fifth filter 122, and after drying, 18.9 kg of battery-grade lithium carbonate is obtained. The filtrate is transported to the second fluorine extractor 123.

[0199] Step nine: in the second fluorine extractor 123, 10% mass fraction calcium chloride solution is added, the calcium chloride content is 11.5 kg, the mass ratio of calcium chloride to lithium hexafluorophosphate is 0.4:1, the pH is adjusted to 9 by 5% sodium chloride solution, the stirring reaction is carried out for 50 minutes, and the solid calcium fluoride is separated by the sixth filter 124. After drying, 3.5 kg is obtained, and the residual fluorine element concentration in the filtrate is 8 ppm.

[0200] It should be noted that the terms "one embodiment", "an embodiment", "exemplary embodiment", "some embodiments", etc. in the specification are intended to indicate that the described embodiment can include a particular feature, structure, or characteristic, but not necessarily every embodiment. In addition, such terms are not necessarily mutually exclusive. Furthermore, the terms "comprise" and "comprising" are intended to indicate that the described embodiment can include a particular feature, structure, or characteristic, but not necessarily every embodiment. In addition, such terms are not necessarily mutually exclusive.

[0201] In general, the terms used should be understood to have been used in a context. For example, the term "one or more" used in the specification can be used to describe any feature, structure, or characteristic in the singular sense or in the combination of features, structures, or characteristics in the plural sense, at least in part according to the context. Similarly, terms such as "a" or "said" can be understood to convey singular usage or plural usage, at least in part according to the context.

[0202] It should be readily understood that "on," "over," and "above" in the present application are to be interpreted in the broadest context, such that "on" means not only "directly on" but also includes the meaning of "on" with intervening features or layers therebetween, and "over" or "above" includes not only the meaning of "over" or "above" but also the meaning of "over" or "above" with no intervening features or layers therebetween (i.e., directly on).

[0203] In addition, spatially relative terms, such as "beneath", "below", "lower", "above", "upper" and the like, can be used herein for ease of description to describe one element or feature's relationship to another element(s) or feature(s) as illustrated in the figures. The spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientations depicted in the figures. The devices can be otherwise oriented (rotated 90° or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.

[0204] Finally, it should be noted that the above-described embodiments are merely intended for describing and illustrating, not limiting, the technical solutions of the present application; even though the present application has been described in detail with reference to the above-described embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the above-described embodiments, or equivalently replace some or all of the technical features thereof; and such modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A device for fully recovering waste lithium battery electrolyte, characterized in that: include: A solvent extractor (100), the solvent extractor (100) being used to contain a filtrate of a lithium battery; A first condenser (101), connected to the solvent extractor (100); A conveying member (102), the conveying member (102) comprising a flow guiding section (1021), a first flow diversion section (1022), and a second flow diversion section (1023) that are connected to each other, the first flow diversion section (1022) and the second flow diversion section (1023) being arranged in parallel; an absorption tank (103), connected to the first diversion section (1022); a first valve (104) connected to the first diversion section (1022), the first valve (104) being used to open or close the communication between the first diversion section (1022) and the absorption tank (103); a first solvent storage tank (105), wherein one end of the first solvent storage tank (105) is connected to the second diversion section (1023), and the other end of the first solvent storage tank (105) is connected to the solvent extractor (100); The second valve (106) is connected to the second diversion section (1023), and the second valve (106) is used to open or close the connection between the second diversion section (1023) and the first solvent storage tank (105).

2. The device for fully recovering waste lithium battery electrolyte according to claim 1, characterized in that: The conveying member (102) has a third diversion section (1024) in communication with the guide section (1021), and the third diversion section (1024) is arranged in parallel with the first diversion section (1022); The device for fully recovering waste lithium battery electrolyte also includes: A second solvent storage tank (107), connected to the third diversion section (1024); a third valve (108) connected to the third diversion section (1024), the third valve (108) being used to open or close the communication between the third diversion section (1024) and the second solvent storage tank (107); The vacuum component (109) is connected to the solvent extractor (100).

3. The device for fully recovering waste lithium battery electrolyte according to claim 1 or 2, characterized in that: The absorption tank (103) has a first output end (1031) and a second output end (1032); The device for fully recovering waste lithium battery electrolyte also includes: a second condenser (110), one end of the second condenser (110) being in communication with the first output end (1031), and the other end of the second condenser (110) being in communication with the solvent extractor (100); The hydrolysis reactor (111) is connected to the absorption tank (103) via the second output end (1032), and the hydrolysis reactor (111) is connected to the solvent extractor (100).

4. The device for fully recovering waste lithium battery electrolyte according to claim 3, characterized in that: Also includes: An electrolyte extractor (112) is connected to the solvent extractor (100), and the electrolyte extractor (112) is used to transport the filtrate to the solvent extractor (100); and the electrolyte extractor (112) is connected to the first solvent storage tank (105).

5. The device for fully recovering waste lithium battery electrolyte according to claim 4, characterized in that: Also includes: A first filter element (113) is connected to the hydrolysis reactor (111); the first filter element (113) is internally layered to form an upper filtrate layer and a lower sedimentation layer; an organic phase separator (114), the organic phase separator (114) comprising a liquid inlet (1141), a first liquid outlet (1142), and a second liquid outlet (1143), the liquid inlet (1141) being in communication with the upper filtrate layer, and the first liquid outlet (1142) being in communication with the electrolyte leachator (112); The primary fluorine extractor (115) is connected to the lower sedimentation layer.

6. The device for fully recovering waste lithium battery electrolyte according to claim 5, characterized in that: Also includes: a phosphorus extractor (116), connected to the second liquid outlet (1143); a second filter element (117), connected to the hydrolysis reactor (111); an impurity metal separator (118), connected to the second filter element (117); a third filter element (119), which is connected to the impurity metal separator (118) and is also connected to the primary fluorine extractor (115); a fourth filter element (120) disposed in communication with the primary fluorine extractor (115); a lithium extractor (121), connected to the fourth filter element (120); a fifth filter element (122), connected to the lithium extractor (121); a secondary fluorine extractor (123), connected to the fifth filter element (122); The sixth filter element (124) is connected to the secondary fluorine extractor (123).

7. A method for fully recovering waste lithium battery electrolyte, characterized in that: The device for fully recovering waste lithium battery electrolyte according to any one of claims 1 to 6 comprises the following steps: transporting the filtrate from the lithium battery to a solvent extractor (100); Opening the first valve (104), closing the second valve (106), and adjusting the first condenser (101) to a first temperature, so that the first partial volume of the filtrate sequentially passes through the first condenser (101), the guide section (1021) of the conveying member (102), and the first diversion section (1022) of the conveying member (102), and is conveyed to the absorption tank (103); The first valve (104) is closed, the second valve (106) is opened, and the first condenser (101) is adjusted to a second temperature, so that the second partial volume of the filtrate passes through the first condenser (101), the guide section (1021), and the second diversion section (1023) of the conveying member (102) in sequence and is conveyed to the first solvent storage tank (105).

8. The method for fully recovering waste lithium battery electrolyte according to claim 7, characterized in that: When the first valve (104) is opened and the second valve (106) is closed, the method further comprises: The third valve (108) of the device for fully recovering waste lithium battery electrolyte is closed.

9. The method for fully recovering waste lithium battery electrolyte according to claim 7, characterized in that: When the first valve (104) is closed and the second valve (106) is opened, the method further comprises: The third valve (108) of the device for fully recovering waste lithium battery electrolyte is closed.

10. The method for fully recovering waste lithium battery electrolyte according to claim 8 or 9, characterized in that: The following steps are also included: The first valve (104) is closed, the second valve (106) is closed, and the third valve (108) is opened; the first condenser (101) is adjusted to a third temperature, so that the third partial volume of the filtrate passes through the first condenser (101), the guide section (1021), and the third diversion section (1024) of the conveying member (102) in sequence, and is conveyed to the second solvent storage tank (107).

11. The method for fully recovering waste lithium battery electrolyte according to claim 7, characterized in that: The following steps are also included: The first portion of the volume of the filtrate in the absorption tank (103) is sequentially transported to the hydrolysis reactor (111) and the first filter element (113); The filtrate in the upper filtrate layer in the first filter element (113) is transported to the organic phase separator (114), and the solid matter in the lower sedimentation layer in the first filter element (113) is transported to the primary fluorine extractor (115); The aqueous phase in the filtrate in the organic phase separator (114) is transported to a phosphorus extractor (116), and the organic phase in the filtrate in the organic phase separator (114) is transported to an electrolyte leacher (112); The kettle liquid in the phosphorus extractor (116) is sequentially passed through the second filter element (117), the impurity metal separator (118), the third filter element (119), the primary fluorine extractor (115), the fourth filter element (120), the lithium extractor (121), the fifth filter element (122), and the secondary fluorine extractor (123), and then transported to the sixth filter element (124).

12. The method for fully recovering waste lithium battery electrolyte according to claim 11, characterized in that: Nitrogen is introduced into the hydrolysis reactor (111), and water, 1%-2% by mass of hydrochloric acid and tributyl phosphate are added, wherein the volume of water is 20%-30% of the volume of the kettle liquid in the hydrolysis reactor (111), the volume of hydrochloric acid is 2%-8% of the volume of the kettle liquid in the hydrolysis reactor (111), and the mass ratio of tributyl phosphate to lithium hexafluorophosphate in the waste electrolyte is 0.005-0.01:1; the internal pressure of the hydrolysis reactor (111) is 0.2MPa-0.5MPa, the hydrolysis temperature is 30°C-50°C, and the hydrolysis time is 30min-90min; and / or, ferric chloride is added to the phosphorus extractor (116), and the mass ratio of ferric chloride to lithium hexafluorophosphate in the waste electrolyte is 1.1-1.3:1; and / or, the impurity metal separator (118) is adjusted to a pH of 3-4 with a 5% by mass sodium hydroxide solution, and 5% by mass sodium carbonate is added; And / or, a 5% to 10% by mass calcium hydroxide suspension is added to the primary fluorine extractor (115), the mass ratio of calcium hydroxide to lithium hexafluorophosphate in the waste electrolyte is 2.8 to 2.9:1, and the pH is adjusted to 9 to 10 by a 5% by mass sodium hydroxide solution, the temperature is raised to 50° C. to 70° C., and the stirring reaction time is 60 min to 90 min; and / or, carbon dioxide is filled into the lithium extractor (121), the pressure in the lithium extractor (121) is maintained at 0.2 MPa to 0.3 MPa, and the pressure is maintained at an internal temperature of 60° C. to 80° C. for 40 min to 120 min; And / or, a 5% to 10% by mass calcium chloride solution is added to the secondary fluorine extractor (123), the mass ratio of calcium chloride to lithium hexafluorophosphate in the waste electrolyte is 0.2-0.6:1, the pH is adjusted to 9-10 by a 5% by mass sodium hydroxide solution, and the reaction is stirred for 30 min to 60 min.

13. The method for fully recovering waste lithium battery electrolyte according to claim 11, characterized in that: The following steps are also included: transporting the kettle liquid in the electrolyte leaching device (112) to the solvent extractor (100); delivering a second portion of the volume of the filtrate in the first solvent storage tank (105) to the solvent extractor (100); The gas in the absorption tank (103) is transported to the solvent extractor (100) after passing through the second condenser (110).

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