CN117977034A - Device for recovering metal lithium in waste lithium battery and recovery method thereof - Google Patents
Device for recovering metal lithium in waste lithium battery and recovery method thereof Download PDFInfo
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- CN117977034A CN117977034A CN202211319152.9A CN202211319152A CN117977034A CN 117977034 A CN117977034 A CN 117977034A CN 202211319152 A CN202211319152 A CN 202211319152A CN 117977034 A CN117977034 A CN 117977034A
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- lithium
- waste
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- battery
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 title claims description 10
- 239000002184 metal Substances 0.000 title claims description 9
- 238000011084 recovery Methods 0.000 title abstract description 11
- 238000001238 wet grinding Methods 0.000 claims abstract description 22
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 20
- 230000009467 reduction Effects 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000005374 membrane filtration Methods 0.000 claims abstract description 12
- 238000004062 sedimentation Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 3
- 238000006722 reduction reaction Methods 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001223 reverse osmosis Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000009853 pyrometallurgy Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to a device for recovering metallic lithium in a waste lithium battery and a recovery method thereof, wherein the device comprises a reduction device for reducing battery waste, a wet grinding device for crushing decomposition reduction products, a sedimentation tank for depositing impurities, a membrane filtration device for separating lithium carbonate and a slurry liquid-solid separation device which are sequentially connected, wherein an outlet pipeline of the wet grinding device is connected with an inlet pipeline of the slurry liquid-solid separation device, and an outlet pipeline of the slurry liquid-solid separation device and an outlet pipeline of the membrane filtration device are intersected on a pipeline connected with the wet grinding device. Compared with the prior art, the lithium metal recovery efficiency is high in the using process, no toxic and harmful waste gas and waste liquid are generated, and no pollution is caused to the environment.
Description
Technical Field
The invention relates to the technical field of waste lithium batteries, in particular to a device and a method for recovering metal lithium in waste lithium batteries.
Background
In recent years, environmental problems and shortage of petroleum resources caused by the traditional internal combustion engine automobiles lead people to bring the view to new energy automobiles. The pure electric automobile can truly realize zero emission, and becomes an important development direction of the electric automobile. The lithium ion battery becomes an ideal power source of a new generation of electric automobiles by virtue of the excellent performance. The demand and the yield of the global lithium ion batteries are continuously increased, the quantity of the waste lithium ion batteries is also rapidly increased, however, the yield of the global cobalt and lithium is only slightly increased, the supply side of the cobalt and the lithium is subjected to great pressure according to the current growth speed, and the shortage of raw materials can be predicted to restrict the benign development of the lithium ion battery industry in the near future.
At present, the recovery of waste lithium ion batteries in China is in a starting stage, and a plurality of technical and economic problems are faced, although the lithium batteries are regarded as green energy sources, the carbonate-based organic electrolyte, the LiPF 6 electrolyte and the metal elements contained in the lithium batteries can form potential pollution risks to the environment, and if the lithium batteries are simply buried, huge harm is caused to the environment and human health. The lithium battery contains a large amount of valuable metals, wherein cobalt is about 5-20%, lithium is 5-7%, nickel is 5-10%, and the recovered and spent lithium ion battery has extremely high economic value and can change waste into valuable.
If the lithium in the waste and unqualified lithium batteries can be effectively recovered, the pollution of the waste batteries to the environment can be reduced, and the current situation of insufficient supply of lithium resources can be effectively relieved. The common methods for recovering lithium at present are as follows: pyrometallurgy, hydrometallurgy, bioleaching. At present, pyrometallurgy is mainly adopted, and the method is simple to operate, but has the advantages of higher energy consumption, lower lithium recycling rate, noise pollution, waste pollution and other environmental problems.
Disclosure of Invention
The invention aims to overcome at least one of the defects of the prior art and provide a device and a method for recovering metal lithium in waste lithium batteries. The device has no toxic and harmful waste gas and waste liquid, is clean and environment-friendly, has complete and simple working procedures, and can realize the efficient separation and recovery of lithium in the waste lithium battery.
The aim of the invention can be achieved by the following technical scheme:
One of the objects of the present invention is an apparatus for recovering metallic lithium in waste lithium batteries, comprising a reduction device for reducing battery waste, a wet milling device for breaking down decomposition reduction products, a sedimentation tank for depositing impurities, and a membrane filtration device for separating lithium carbonate, which are connected in sequence.
Further, the device also comprises a slurry liquid-solid separation device, wherein the slurry liquid-solid separation device is positioned between the wet grinding device and the membrane filtration device.
Further, the outlet pipeline of the wet grinding device is connected with the inlet pipeline of the slurry liquid-solid separation device, and the outlet pipeline of the slurry liquid-solid separation device is connected with the wet grinding device.
Further, the outlet pipeline of the membrane filtration device is connected with the wet grinding device.
Further, the reduction equipment is a carbon reduction furnace protected by vacuum or inert gas, the wet grinding equipment is a wet grinding machine, and the material slurry solid separation equipment is a plate filter press or a centrifuge.
The second object of the present invention is a method for recovering metallic lithium from waste lithium batteries using an apparatus for recovering metallic lithium from waste lithium batteries as described above, comprising the steps of:
Placing crushed and separated lithium cobalt oxide, lithium nickel oxide, lithium manganate particles, a small amount of aluminum and copper particles, and graphite powder battery anode powder and carbon powder into reduction equipment, and calcining under inert atmosphere to obtain a reduction product, wherein the reduction product contains lithium carbonate, cobalt, nickel, manganese (or cobalt oxide, nickel oxide, manganese oxide) and other products;
Placing the reduction product in wet milling equipment for full milling, and using a large amount of grinding liquid for full dissolution of lithium carbonate in the reduction product, wherein the lithium carbonate can be slightly dissolved in water, and a large amount of water can be used for dissolving most of the lithium carbonate;
Placing the grinding fluid containing lithium carbonate discharged by the wet grinding equipment into a sedimentation tank, and standing until impurities are deposited;
The supernatant of the sedimentation tank is treated by a membrane filtration device to obtain lithium carbonate solid, because a layer of pure lithium carbonate crystals are deposited on the surface of the membrane, lithium is collected by replacing and cleaning the membrane, and the filtered aqueous solution enters a wet mill again for recycling.
Further, the mass ratio of the battery anode powder to the carbon powder is 10:1.
Further, the temperature of the reduction reaction is 750-850 ℃ and the time is 1-1.5 hours.
Further, the mass ratio of the grinding balls to the reducing products in the wet grinding equipment is 1.5:1,
Further, the mass ratio of the grinding liquid to the materials is 5:1, and the grinding time is 1.5-3 hours.
Further, the polishing liquid is water.
Further, the sedimentation time in the sedimentation tank is not less than 5 hours.
Further, the reverse osmosis membrane aperture of the membrane filtration device is 0.5-1nm.
Compared with the prior art, the invention has the following advantages:
(1) The invention develops a device for recovering metal lithium in a waste lithium battery, which has high lithium metal recovery efficiency in the using process, does not generate any toxic and harmful waste gas and waste liquid, and does not pollute the environment;
(2) The invention designs a recovery method for recovering metal by using a device for recovering metal lithium in a waste lithium battery, which realizes a whole set of procedures for separating and recovering lithium in the waste lithium battery, and has the advantages of simplicity and convenience and strong operability.
Drawings
FIG. 1 is a block diagram of the process flow of the present invention.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
Example 1
The raw material is 5kg of positive electrode powder after mechanical breaking, disassembly and separation, and the lithium content is about 6.7% through detection;
The mass ratio of the positive electrode powder to the carbon powder is 10:1, mixing, and then placing the mixture in a nitrogen protection furnace for reaction, wherein the reaction temperature is 780 ℃ and the reaction time is 1 hour;
The product after the reaction is a plate-shaped object block, and the main components of the product are lithium carbonate, cobalt, nickel, manganese (or cobalt oxide, nickel oxide, manganese oxide) and the like;
grinding balls and reaction products according to the proportion of 1.5:1 in a wet mill, and according to a water to material ratio of 5:1, adding clear water in proportion, and grinding for 2 hours;
the aqueous solution discharged from the grinding was discharged into a deposition tank, and after deposition for 6 hours, the aqueous solution was injected into a membrane filtration apparatus.
Filtering the ground slurry by adopting a centrifugal machine to obtain a dehydration product;
The content of lithium in the dehydrated product is detected to be 0.14%, which shows that lithium carbonate is basically dissolved in water; after the clear solution of the sedimentation tank is treated by the membrane filtration equipment, 1520g of lithium carbonate is obtained, the purity is 99%, and the recovery rate reaches 91.29%.
Comparative example 1
The raw material is 500g of positive electrode powder after mechanical breaking and separation of a ternary lithium battery, and the lithium content is about 6.5%;
the positive electrode powder is placed in a furnace at 700 ℃ for treatment for 1 hour, residual carbon is removed, and pyrolysis reaction is carried out;
Placing the reaction product in 10L of water for cleaning, and then evaporating and filtering the cleaned water solution to obtain a lithium carbonate sample;
139g of lithium carbonate was obtained, and the recovery rate was 81.5%.
Example 1 has improved recovery by approximately 10% compared to comparative example 1, mainly because lithium carbonate has a melting point of 723 c, and is melted and aggregated during heat treatment at a temperature higher than 723 c, resulting in a decrease in the efficiency of leaching later and loss in the reactor, whereas the present invention, after heat treatment at high temperature, adds a wet grinding and crushing process, facilitating dissolution of lithium carbonate.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. The device for recovering the metal lithium in the waste lithium battery is characterized by comprising a reduction device for reducing battery waste, a wet grinding device for crushing decomposition reduction products, a sedimentation tank for depositing impurities and a membrane filtering device for separating lithium carbonate, which are connected in sequence.
2. The apparatus for recovering lithium metal in a lithium scrap battery according to claim 1 further comprising a slurry-liquid-solid separation device, the slurry-liquid-solid separation device being disposed between the wet grinding device and the membrane filtration device.
3. The apparatus for recovering lithium metal in a waste lithium battery according to claim 1, wherein the wet grinding device outlet pipe is connected to the slurry liquid-solid separation device inlet pipe, and the slurry liquid-solid separation device outlet pipe is connected to the wet grinding device.
4. The apparatus for recovering metallic lithium from a waste lithium battery as defined in claim 1, wherein said membrane filtration device outlet line is connected to a wet milling device.
5. A method for recovering metallic lithium in a waste lithium battery using an apparatus for recovering metallic lithium in a waste lithium battery as claimed in any one of claims 1 to 4, characterized in that the method comprises the steps of:
placing the crushed and separated battery anode powder and carbon powder into reduction equipment, and calcining under inert atmosphere to obtain a reduction product;
Fully grinding the reduction product in wet grinding equipment, and fully dissolving lithium carbonate in the reduction product by using grinding liquid;
Placing the grinding fluid containing lithium carbonate discharged by the wet grinding equipment into a sedimentation tank, and standing until impurities are deposited;
and (5) treating the supernatant of the sedimentation tank by using a membrane filtering device to obtain lithium carbonate solid.
6. The method for recycling metallic lithium in a waste lithium battery according to claim 5, wherein the mass ratio of the battery positive electrode powder to the carbon powder is 10:1.
7. The method for recovering lithium metal from a waste lithium battery according to claim 5, wherein the reduction reaction is performed at a temperature of 750-850 ℃ for 1-1.5 hours.
8. The method for recovering lithium metal from waste lithium batteries according to claim 5, wherein the mass ratio of grinding balls to reducing products in said wet grinding apparatus is 1.5:1.
9. The method for recycling metallic lithium in waste lithium batteries according to claim 5, wherein the mass ratio of the grinding fluid to the materials is 5:1, the grinding time is 1.5-3 hours, and the grinding fluid is water.
10. The method for recovering metallic lithium from a waste lithium battery as claimed in claim 5, wherein the sedimentation time in said sedimentation tank is not less than 5 hours, and the reverse osmosis membrane pore size of said membrane filtration device is 0.5-1nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211319152.9A CN117977034A (en) | 2022-10-26 | 2022-10-26 | Device for recovering metal lithium in waste lithium battery and recovery method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211319152.9A CN117977034A (en) | 2022-10-26 | 2022-10-26 | Device for recovering metal lithium in waste lithium battery and recovery method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN117977034A true CN117977034A (en) | 2024-05-03 |
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ID=90848476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211319152.9A Pending CN117977034A (en) | 2022-10-26 | 2022-10-26 | Device for recovering metal lithium in waste lithium battery and recovery method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117977034A (en) |
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2022
- 2022-10-26 CN CN202211319152.9A patent/CN117977034A/en active Pending
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