CN113270570A - Preparation method of lithium ion battery anode slurry - Google Patents
Preparation method of lithium ion battery anode slurry Download PDFInfo
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- CN113270570A CN113270570A CN202110493134.1A CN202110493134A CN113270570A CN 113270570 A CN113270570 A CN 113270570A CN 202110493134 A CN202110493134 A CN 202110493134A CN 113270570 A CN113270570 A CN 113270570A
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- ion battery
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000006256 anode slurry Substances 0.000 title claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 101
- 239000003292 glue Substances 0.000 claims abstract description 47
- 239000000243 solution Substances 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000006258 conductive agent Substances 0.000 claims abstract description 15
- 239000002033 PVDF binder Substances 0.000 claims abstract description 14
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 13
- 239000011149 active material Substances 0.000 claims abstract description 11
- 238000010790 dilution Methods 0.000 claims abstract description 10
- 239000012895 dilution Substances 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000011267 electrode slurry Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 238000007790 scraping Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 10
- 239000004615 ingredient Substances 0.000 description 4
- 239000007774 positive electrode material Substances 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 3
- 239000010405 anode material Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229920001519 homopolymer Polymers 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
- 230000003446 memory effect Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The embodiment of the invention provides a preparation method of lithium ion battery anode slurry, which comprises the following steps: s1, sequentially adding NMP and PVDF into a stirring device in proportion, and stirring to form a glue solution; s2, dividing the glue solution into a plurality of parts, adding a conductive agent, an additive and an active material into the first part of glue solution, stirring, pouring the rest glue solution into the first part of glue solution, diluting and stirring to form slurry; s3, after the dilution and the stirring are finished, carrying out vacuum defoaming on the slurry; and S4, discharging. The scheme of the invention directly adopts a wet mixing mode, the high solid content stirring is realized by adding the glue solution in batches, then the dilution stirring is realized, the batching time is greatly shortened to 2-2.5h, the batching process is stable, the viscosity is not required to be adjusted repeatedly, the operation steps are simple, the utilization rate of the stirring equipment is greatly improved by 50-100%, thus the preparation time of the slurry is greatly shortened, and the production efficiency is improved.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method of lithium ion battery anode slurry.
Background
The lithium ion battery has the advantages of high specific energy, good safety, excellent high and low temperature performance, no memory effect, long cycle life and the like, is widely regarded in the field of mobile energy storage at present, and becomes a preferred mobile energy storage product of the current new energy automobile. At present, most of the anode batching processes of lithium ion batteries are to prepare glue and then to batching the glue. The method comprises the following steps of preparing glue firstly and then preparing materials, wherein the glue preparing time is generally 3-4 hours, then preparing the materials, the materials are prepared in a mode of dry mixing firstly and wet mixing secondly, and the stirring time of the materials is different from 4-6 hours, so that the preparation time of the slurry is long, and the working efficiency is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and solve the technical problems of long manufacturing time and low working efficiency of the slurry on the market.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the lithium ion battery anode slurry comprises the following steps:
s1, sequentially adding NMP and PVDF into a stirring device in proportion, and stirring to form a glue solution;
s2, dividing the glue solution into a plurality of parts, adding a conductive agent, an additive and an active material into the first part of glue solution, stirring, pouring the rest glue solution into the first part of glue solution, diluting and stirring to form slurry;
s3, after the dilution and the stirring are finished, carrying out vacuum defoaming on the slurry;
and S4, detecting the characteristic parameters of the slurry, and discharging if the characteristic parameters meet the requirements.
Optionally, step S1 includes:
s10, firstly weighing a certain weight of NMP and adding the NMP into a stirring barrel, then weighing a certain weight of PVDF and adding the PVDF into the stirring barrel, and firstly stirring slowly and then stirring rapidly;
s11, lifting the stirring barrel, and scraping materials by using a silica gel plate;
and S12, closing the stirring barrel after the scraping is finished, stirring at a slow speed and a fast speed, simultaneously starting vacuum, and stirring in a vacuum pumping state.
Optionally, in step S10, the rotation speed of slow stirring is 15PRM, the rotation speed of fast stirring is 200PRM, and the stirring time is 20 min; in step S11, the rotation speed of slow stirring is 30PRM, the rotation speed of fast stirring is 2000PRM, and the stirring time is 3 hours; in step S12, a vacuum is applied to-90 KPa or less.
Optionally, before step S1, the cooling circulating water is turned on.
Optionally, step S2 includes:
s20, dividing the glue solution into two parts;
s21, adding the first part of glue solution, the conductive agent and the additive into a stirring device, and stirring at low speed of 20RPM and high speed of 1500RPM for 15 min;
s22, adding the active material, stirring at a low speed of 20RPM (revolution per minute) and at a high speed of 200RPM for 15 min;
and S23, rotating at a low speed of 30RPM and then at a high speed of 2000RPM, wherein the stirring time is 60 min.
Optionally, the mass ratio of the first part of glue solution to the second part of glue solution is as follows: (1-1.5): 1.
optionally, the active material is lithium cobaltate, the conductive agent is a carbon black conductive agent, and the BET specific surface area is more than or equal to 80m2/g。
The invention has the beneficial effects that: compared with the prior art, the preparation method of the lithium ion battery anode slurry has the advantages that the batching preparation process is not dry-mixed, a wet mixing mode is directly adopted, the high solid content stirring is realized firstly by adding the glue solution in batches, then the dilution stirring is realized, the batching time is greatly shortened to 2-2.5h, the batching process is stable, the repeated viscosity adjustment is not needed, the operation steps are simple, the utilization rate of stirring equipment is greatly improved by 50-100%, the preparation time of the slurry is greatly shortened, and the production efficiency is improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
Fig. 1 is a process flow of a method for preparing a lithium ion battery positive electrode slurry according to an embodiment of the present invention;
FIG. 2 is a process flow for preparing glue solution provided by an embodiment of the present invention;
fig. 3 is a flow chart of a slurry preparation process according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The main constituent materials of the lithium ion battery include electrolyte, isolating material, anode and cathode materials and the like. The positive electrode material occupies a large proportion (the mass ratio of the positive electrode material to the negative electrode material is 3: 1-4: 1), and the performance of the lithium ion battery is directly influenced by the performance of the positive electrode material, so that the cost directly determines the cost of the battery. In the embodiment, the lithium battery positive electrode material mainly comprises an active material lithium cobaltate, a conductive agent, a binder, an additive and NMP (N-methylpyrrolidone), wherein the proportion of the lithium cobaltate is 96.0-98.5%; the proportion of the conductive agent is 0.5 to 2.0 percent; the binder is PVDF (polyvinylidene fluoride), and the proportion is 0.6% -1.2%; the additive is PVP (polyvinylpyrrolidone) with the content of 0.02-0.15%. Wherein the conductive agent is carbon black conductive agent, and BET specific surface area is not less than 80m2(ii)/g; PVDF is a homopolymer having a weight-average molecular weight (Mw) of 100 ten thousand (10)6) Da; the content of the lithium cobaltate of the anode is high, and the battery ratio of the lithium ion battery manufactured by using the anode materialThe energy is obviously improved, and the rate discharge capacity and the cycle life are improved.
Further, referring to fig. 1 to 3, the present invention also provides a method for preparing the above-mentioned lithium ion battery positive electrode slurry, including:
s1, sequentially adding NMP and PVDF into a stirring device in proportion, and stirring to form a glue solution;
s2, dividing the glue solution into a plurality of parts, adding a conductive agent, an additive and an active material into the first part of the glue solution, stirring, pouring the rest glue solution into the first part of the glue solution, diluting and stirring to form slurry;
s3, after the dilution and the stirring are finished, carrying out vacuum defoaming on the slurry;
and S4, detecting the characteristic parameters of the slurry, and discharging if the characteristic parameters meet the requirements.
Compared with the method of firstly preparing the glue and then preparing the ingredients, the ingredient preparation process of the technical scheme does not need dry mixing, directly adopts a wet mixing mode, and adds the glue solution in batches to realize firstly high solid content stirring and then diluting and stirring, so that the ingredient time is greatly shortened to 2-2.5h, the ingredient preparation process is stable, the viscosity does not need to be repeatedly adjusted, the operation steps are simple, and the utilization rate of stirring equipment is greatly improved by 50-100%.
In the present embodiment, as shown in fig. 2, specifically, step S1 includes the following sub-steps:
s10, firstly weighing NMP with a certain weight, adding the NMP into a stirring barrel, then weighing PVDF with a certain weight, adding the PVDF into the stirring barrel, and firstly stirring slowly and then stirring rapidly; preferably, the rotation speed of slow stirring is 15PRM, the rotation speed of fast stirring is 200PRM, and the stirring time is 20 min;
s11, lifting the stirring barrel, and scraping materials by using a silica gel plate;
and S12, closing the stirring barrel after the scraping is finished, stirring at a slow speed and a fast speed, and simultaneously starting vacuum to stir in a vacuum state. Wherein the rotation speed of slow stirring is 30PRM, the rotation speed of rapid stirring is 2000PRM, the stirring time is 3h, and the vacuum is pumped to be below-90 KPa.
Specifically, in the glue solution preparation process, the PVDF can be fully fused into the NMP by stirring for multiple times, adopting a stirring mode of firstly slowly stirring and then quickly stirring and matching the silica gel scraper, the components and uniformity of the glue solution are good, and the glue solution prepared once can meet the use amount of the glue solution prepared for multiple times. And vacuumizing in step S12 to avoid water absorption and ensure the purity of the glue solution.
Further, in order to avoid the excessive temperature of the glue solution caused by the exothermic dissolution of PVDF, the cooling circulating water should be started before the step S10, and the water temperature of the cooling circulating water should be fluctuated within a range of +/-5 ℃.
Referring to fig. 3, in the present embodiment, step S2 specifically includes the following sub-steps:
s20, dividing the glue solution into two parts;
wherein the mass ratio of the first glue solution to the second glue solution is as follows: (1-1.5): 1.
s21, adding the first part of glue solution, the conductive agent and the additive into a stirring device, and stirring at low speed of 20RPM and high speed of 1500RPM for 15 min;
s22, adding an active material, stirring at a low speed of 20RPM (revolution per minute) and at a high speed of 200RPM for 15 min;
s23, then, firstly rotating at a low speed of 30RPM and then rotating at a high speed of 2000RPM, stirring for 60min, and stirring the slurry;
at the moment, the solid content reaches 86-90 percent, circulating water is needed to be started to cool the slurry in the stirring process, and the circulating water is the best cooling water at the temperature of 8-15 ℃.
S22, adding an active material, stirring at a low speed of 20RPM (revolution per minute) and at a high speed of 200RPM for 15 min;
and S23, rotating at a low speed of 30RPM and then at a high speed of 2000RPM, wherein the stirring time is 60 min.
Here, the present embodiment employs a double planetary stirring apparatus. The stirring rotating speed can be adjusted to low-speed and high-speed rotating speeds according to the size of actual double-planet stirring equipment; the high-speed dispersing rotating speed of the large-scale stirrer needs to be reduced, the high-speed dispersing rotating speed of the small-scale stirrer needs to be increased, and the high-speed dispersing linear speed of the dispersing disc is less than or equal to 20 m/s. And the mode of high solid content stirring and dilution stirring is adopted, so that the batching time is short, the equipment utilization rate is improved by 50-100%, and the preparation time of the slurry is greatly shortened.
In step S3, specifically: after the dilution and stirring are finished, vacuum defoaming is carried out, the low speed is opened for 10RPM, the high speed is not opened, the vacuum is pumped to be below-90 KPa, and the vacuum defoaming is continuously carried out for 15 min.
Further, the characteristic parameters in step S5 are: and measuring viscosity, solid content and fineness. The slurry prepared at this time can meet the requirements that the solid content is between 77 and 83 percent and the viscosity of the slurry is 3000-8000 mPa.s. When the prepared slurry meets the parameter requirements, a 100-200-mesh screen is used for sieving and discharging.
The invention is a wet mixing mode, has no dust raising in a dry mixing state, adopts a mode of high solid content stirring plus dilution stirring, has short batching time and improves the equipment utilization rate by 50 to 100 percent, the solid content of the slurry prepared by the scheme is 77 to 83 percent, the viscosity of the slurry is 3000 plus 8000mPa.s, the slurry belongs to high solid content slurry, the use amount of NMP is reduced by 10 to 20 percent, the use cost is reduced, the batching process has high content of anode lithium cobalt oxide, the specific energy of the lithium ion battery manufactured by the anode material is obviously improved, the rate discharge capacity is 10 percent, and the cycle life is prolonged by 20 percent.
The invention is not to be considered as limited to the particular embodiments shown and described, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed.
Claims (9)
1. A preparation method of lithium ion battery anode slurry is characterized by comprising the following steps:
s1, sequentially adding NMP and PVDF into a stirring device in proportion, and stirring to form a glue solution;
s2, dividing the glue solution into a plurality of parts, adding a conductive agent, an additive and an active material into the first part of glue solution, stirring, pouring the rest glue solution into the first part of glue solution, diluting and stirring to form slurry;
s3, after the dilution and the stirring are finished, carrying out vacuum defoaming on the slurry;
and S4, detecting the characteristic parameters of the slurry, and discharging if the characteristic parameters meet the requirements.
2. The method for preparing the positive electrode slurry of the lithium ion battery according to claim 1, wherein the step S1 includes:
s10, firstly weighing a certain weight of NMP and adding the NMP into a stirring barrel, then weighing a certain weight of PVDF and adding the PVDF into the stirring barrel, and firstly stirring slowly and then stirring rapidly;
s11, lifting the stirring barrel, and scraping materials by using a silica gel plate;
and S12, closing the stirring barrel after the scraping is finished, stirring at a slow speed and a fast speed, simultaneously starting vacuum, and stirring in a vacuum pumping state.
3. The method for preparing the positive electrode slurry for lithium ion batteries according to claim 2, wherein in step S10, the rotation speed of slow stirring is 15PRM, the rotation speed of fast stirring is 200PRM, and the stirring time is 20 min; in step S11, the rotation speed of slow stirring is 30PRM, the rotation speed of fast stirring is 2000PRM, and the stirring time is 3 hours; in step S12, a vacuum is applied to-90 KPa or less.
4. The method for preparing the positive electrode slurry of the lithium ion battery according to claim 1, wherein before step S1, cooling circulating water is started.
5. The method for preparing the positive electrode slurry of the lithium ion battery according to claim 1, wherein the step S2 includes:
s20, dividing the glue solution into two parts;
s21, adding the first part of glue solution, the conductive agent and the additive into a stirring device, and stirring at low speed of 20RPM and high speed of 1500RPM for 15 min;
s22, adding the active material, stirring at a low speed of 20RPM (revolution per minute) and at a high speed of 200RPM for 15 min;
and S23, rotating at a low speed of 30RPM and then at a high speed of 2000RPM, wherein the stirring time is 60 min.
6. The method for preparing the positive electrode slurry of the lithium ion battery according to claim 4, wherein the temperature of the cooling circulation water in the step S2 is maintained between 8 ℃ and 15 ℃.
7. The preparation method of the lithium ion battery anode slurry according to claim 1, wherein the mass ratio of the first part of glue solution to the second part of glue solution is as follows: (1-1.5): 1.
8. the method for preparing the positive electrode slurry for the lithium ion battery according to claim 1, wherein step S3 specifically comprises: after the dilution and stirring are finished, vacuum defoaming is carried out, the low speed is opened for 10RPM, the high speed is not opened, the vacuum is pumped to be below-90 KPa, and the vacuum defoaming is continuously carried out for 15 min.
9. The method for preparing the positive electrode slurry of the lithium ion battery according to any one of claims 1 to 8, wherein the active material is lithium cobaltate, the conductive agent is a carbon black conductive agent, and the BET specific surface area is not less than 80m2/g。
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| CN118213486A (en) * | 2024-02-21 | 2024-06-18 | 江苏益佳通新能源科技有限公司 | Preparation method and device for double-mechanism long-cycle lithium ion battery positive electrode |
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| CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
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| CN118213486A (en) * | 2024-02-21 | 2024-06-18 | 江苏益佳通新能源科技有限公司 | Preparation method and device for double-mechanism long-cycle lithium ion battery positive electrode |
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