CN104599863A - Method for preparation of composite material, composite material and application thereof - Google Patents
Method for preparation of composite material, composite material and application thereof Download PDFInfo
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- CN104599863A CN104599863A CN201510021386.9A CN201510021386A CN104599863A CN 104599863 A CN104599863 A CN 104599863A CN 201510021386 A CN201510021386 A CN 201510021386A CN 104599863 A CN104599863 A CN 104599863A
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- composite material
- foamy graphite
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- nickel hydroxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a method for preparation of a composite material. The method comprises the following steps that S1, foamy graphite with a three-dimensional porous structure is provided; S2, the foamy graphite is added to a potassium hydroxide solution to be activated, and then is washed and dried, so that activated foamy graphite is obtained; S3, the activated foamy graphite is added to mixed acid to be acidized under the ultrasonic condition, and then is washed and dried, so that acidized foamy graphite is obtained; S4, the acidized foamy graphite is added to a nickel sulfate solution to form uniform suspension liquid through mixing, a precipitating agent is slowly and dropwise added to the suspension liquid, and is washed and dried after hydro-thermal processing is accomplished, so that the composite material made of the foamy graphite and nickel hydroxide nanowires is obtained. The invention further provides the composite material prepared through the method for preparation of the composite material, and application of the composite material serving as an electrode material to a capacitor. All in all, the method for preparation of the composite material is simple in process, easy to control and beneficial to large-scale production, and the provided composite material has high specific capacitance and excellent cycle stability when the composite material serves as the electrode material.
Description
Technical field
The present invention relates to a kind of material, relate more specifically to a kind of prepare composite material method, composite material and application thereof.
Background technology
Along with climate warming and environmental pollution increasingly sharpen, people start the reproducible new forms of energy sought outside fossil energy gradually, and as solar energy, wind energy and biological energy source etc., this also just becomes global study hotspot.High performance energy storage device is then the prerequisite that human society effectively utilizes these reproducible new forms of energy, thus receives much concern.
Ultracapacitor is as a kind of novel energy-storage travelling wave tube, there is higher energy density compared with traditional capacitor, have higher power density compared with conventional batteries, also have charging interval short, long service life and the advantage such as maintenance cost is low, application prospect is very wide simultaneously.
Different according to the principle of ultracapacitor storage power, can be divided three classes: based on the double electric layer capacitor of porous carbon electrode and the energy storage of electrolyte interface electric double layer, based on the Faradic pseudo-capacitor of the redox reaction energy storage of metal oxide and conductive polymer surfaces, and the mixed capacitor that said two devices has concurrently.The electrode material being commonly used for ultracapacitor comprises material with carbon element and metal oxide.But material with carbon element is lower as the ratio capacitance of electrode material, and metal oxide is as the less stable of electrode material.
Summary of the invention
The present invention aims to provide a kind of method preparing composite material, and the composite material obtained by the method has higher ratio capacitance and good stability simultaneously.
The invention provides a kind of method preparing composite material, comprise the following steps: S1, the foamy graphite with three-dimensional porous structure is provided; S2, joins described foamy graphite in potassium hydroxide solution and activates, and obtains activating foamy graphite after washing drying; S3, joins described activation foamy graphite in nitration mixture and carry out acidifying under ultrasonic, obtains acidifying foamy graphite after washing drying; And S4, described acidifying foamy graphite is joined in nickel sulfate solution and is mixed to form unit for uniform suspension, precipitation reagent is slowly added drop-wise in described suspension, the dry composite material obtaining foamy graphite and nickel hydroxide nano line of washing after hydrothermal treatment consists.
In the present invention, foamy graphite is a kind of graphited porous carbon materials, there is satisfactory electrical conductivity and high-specific surface area, it is applied to ultracapacitor as electrode material and the interfacial electric double layer formed between electrode and electrolyte can be utilized to realize energy storage, there is not electrochemical reaction, therefore there is good cyclical stability.But it is lower that foamy graphite is found its single electrode ratio capacitance, cannot provide high-energy-density.The advantages such as nickel hydroxide is a kind of potential electrode material, has cheap, chemistry redox stability of characteristics, and theoretical ratio capacitance is high.But it is poor that nickel hydroxide is found its cycle performance.The present invention selects the monodimension nanometer material of nickel hydroxide, the i.e. nano thread structure of nickel hydroxide, it effectively can prevent the reunion of nickel hydroxide in charge and discharge process, alleviate volume electrode material to expand, maintain the stability of material, in addition, in charge and discharge cycles process, this one-dimensional nano structure makes nickel hydroxide, in transverse direction (diameter) and longitudinal (length) both direction, small change occur, be conducive to discharging the stress produced, make material in cyclic process, obtain better structural stability.The present invention will have the nickel hydroxide nano line of higher structural stability, the composite material with three-dimensional porous structure is combined into the porous foam graphite of high-specific surface area, make full use of both respective advantage and synergistic function thereof, obtain a kind of electrode material for super capacitor with high specific capacitance and excellent cyclical stability.
Described step S1 comprises: at sucrose and the ammonium chloride of the mixing of tubular type kiln roasting, thus provide described foamy graphite.Should be appreciated that, preparing foamy graphite by other means for being also feasible in the present invention, as long as the foamy graphite provided has three-dimensional porous structure.
The mol ratio of described sucrose and ammonium chloride is 0.5-2.5, and sintering temperature is 1000-1500 DEG C.In this step, sucrose forms foamy graphite through high-temperature roasting carbonization.Preferably, this roasting process carries out 2-5 hour under an argon atmosphere.
In described step S2, the mass ratio of described foamy graphite and described potassium hydroxide is 0.1-1, preferred 0.1-0.5.Should be appreciated that, in this step, the foamy graphite of other ratios and potassium hydroxide are also feasible, as long as can pore-creating and increase specific area.The concentration of described potassium hydroxide solution is 5-10mol/L.Preferably, this activation process carries out 10-30 hour.
In described step S3, described nitration mixture is sulfuric acid and nitric acid, and wherein, the volume ratio of sulfuric acid and nitric acid is 3:1-1:3.Should be appreciated that, in this step, other nitration mixture is also feasible, as long as can introduce oxygen-containing functional group, thus increases the attachment position of nickel hydroxide nano line.Preferably, this acidization carries out 2-5 hour.
In described step S4, described precipitation reagent is nickel hydroxide, NaOH or urea.Should be appreciated that, other the precipitation reagent hydroxy that can provide also can with in the present invention.
In described step S4, with vigorous stirring precipitation reagent is slowly added drop-wise in described suspension.By this vigorous stirring, precipitation reagent and nickelous sulfate Homogeneous phase mixing are reacted.
In described step S4, the mass ratio of described acidifying foamy graphite and described nickelous sulfate is 0.02-0.1.Preferably, the mass ratio of described acidifying foamy graphite and described nickelous sulfate is 0.03-0.82.
The mol ratio of described nickelous sulfate and described precipitation reagent is 1-3.Should be appreciated that, in this step, the nickelous sulfate of other ratios and precipitation reagent are also feasible, as long as guarantee the hydroxyl reaction of nickelous sulfate and precipitation reagent release, thus at the Surface Creation nickel hydroxide of acidifying foamy graphite.Preferably, the mass ratio of nickelous sulfate and NaOH is 1.By a large amount of experiments, applicant finds, selecting NaOH to carry out precipitating than selecting urea to carry out the better effects if precipitated, although urea at high temperature decomposes and can produce hydroxyl, being undertaken precipitating the composite material obtained by urea in certain embodiments and cannot meet application requirement.Should be appreciated that, by carrying out suitably preferably the technological parameter of urea as precipitation reagent, still can provide the composite material as electrode material of optimization.
Described hydrothermal temperature is 100-180 DEG C.Should be appreciated that, it is also feasible that other temperature carry out hydro-thermal reaction, as long as nickel hydroxide can be made in water heating kettle to form nano thread structure.More particularly, the diameter of formed nano wire can be regulated by controlling this hydrothermal temperature and compactedness.Preferably, the diameter of the nano wire formed is between 20-40nm.
The present invention also provides a kind of composite material prepared according to said method, and described composite material is the composite material of foamy graphite and nickel hydroxide nano line.In this composite material, nickel hydroxide is attached to the surface of foamy graphite with the form of nano wire.
The present invention also provides above-mentioned composite material on the capacitor as the application of electrode material.By experiment, applicant finds, this composite material has higher ratio capacitance and good stability simultaneously.
The mass percent of the nickel hydroxide in described composite material is 30-85%.
The initial feed preparing composite material of the present invention is the foamy graphite with three-dimensional porous structure, the activation foamy graphite particularly obtained after activation step, it has larger specific area and more pore structure, wherein, this specific area is conducive to the attachment of nickel hydroxide nano line, thus improve the utilance of electrode material, and this pore structure is conducive to the transmission of electrolyte.In addition, the method preparing composite material of the present invention comprises acidifying foamy graphite and nickelous sulfate is mixed to form suspension in the solution, then precipitation reagent is under agitation slowly added drop-wise to the step producing precipitation in this mixed solution, make nickel hydroxide homogeneous nucleation on foamy graphite, thus finally guarantee that the nano wire that hydro-thermal is formed is evenly distributed in foamy graphite, form complex three-dimensional structures.In a word, the method route preparing composite material of the present invention is simple, be easy to control, and be conducive to large-scale production, and the composite material provided has larger ratio capacitance and excellent cyclical stability.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram according to composite material of the present invention;
Fig. 2 a is the scanning electron microscopy according to activation foamy graphite of the present invention;
Fig. 2 b is the scanning electron microscopy according to composite material of the present invention;
Fig. 2 c is the scanning electron microscopy of the amplification according to the nickel hydroxide nano line in composite material of the present invention;
Fig. 3 a is the single electrode ratio capacitance comparison diagram according to composite material of the present invention, independent nickel hydroxide, foamy graphite; And
Fig. 3 b is the unipolar cycle performance figure of composite material according to the present invention as electrode material.
Embodiment
Below in conjunction with accompanying drawing, provide preferred embodiment of the present invention, and be described in detail.
The mass percent of embodiment 1 nickel hydroxide nano line is the preparation of the composite material of 85%
(1) with sucrose and ammonium chloride with the ratio of mol ratio 1:2 1000 DEG C, roasting 2 hours under argon gas atmosphere, obtain the foamy graphite with three-dimensional porous structure.
(2) foamy graphite joins (mass ratio 0.1 in the potassium hydroxide solution of 7mol/L, the quality of the potassium hydroxide namely in potassium hydroxide solution is 10 times of the quality of foamy graphite) in stir 4 hours, leave standstill 20 as a child to filter afterwards, 60 DEG C of dryings obtain after 24 hours activating foamy graphite.
(3) activation foamy graphite and nitration mixture (volume ratio is sulfuric acid: nitric acid=1:1), ultrasonic lower acidifying 2 hours, obtain acidifying foamy graphite after washing drying.
(4) acidifying foamy graphite is joined (mass ratio 0.06) in nickel sulfate solution and be mixed to form unit for uniform suspension, NaOH (nickelous sulfate and NaOH mol ratio are 1) solution is under agitation slowly added drop-wise in described suspension, wherein, the concentration of nickelous sulfate is 0.06g/mL.Water heating kettle hydrothermal treatment consists is put into 24 hours at 100 DEG C.The dry composite material obtaining foamy graphite and nickel hydroxide nano line of finally washing.
As shown in Figure 1, all peak distributions and standard card chip value (JCPDS No.41-1424) fit like a glove the X ray result of this composite material, prove that the nickel hydroxide nano line obtained is α-(NiOH)
2,calculating its cell parameter is a=0.81067nm, b=0.29520nm c=1.37165nm.
The preparation of embodiment 2 composite material
(1) with sucrose and ammonium chloride with the ratio of mol ratio 2.5:1 1500 DEG C, roasting 5 hours under argon gas atmosphere, obtain the foamy graphite with three-dimensional porous structure.
(2) foamy graphite joins in potassium hydroxide solution and stirs 4 hours in (mass ratio 1), leaves standstill 20 and as a child filters afterwards, and 60 DEG C of dryings obtain after 24 hours activating foamy graphite.
(3) activation foamy graphite and nitration mixture (sulfuric acid: nitric acid=3:1), ultrasonic lower acidifying 5 hours, obtain acidifying foamy graphite after washing drying.
(4) described acidifying foamy graphite is joined (mass ratio 0.03) in nickel sulfate solution and be mixed to form unit for uniform suspension, maintain vigorous stirring and NaOH (nickelous sulfate and NaOH mol ratio are 3) solution is slowly added drop-wise in described suspension.Hydrothermal treatment consists 24 hours at 180 DEG C.Finally wash the composite material that drying (baking temperature is 80 DEG C) obtains foamy graphite and nickel hydroxide nano line.
Stereoscan photograph as shown in Figure 2, wherein, Fig. 2 a can find out, activation foamy graphite has three-dimensional porous structure, and Fig. 2 b can find out, foamy graphite and nickel hydroxide weave in, the structure that formation loose structure and nano wire run through mutually, wherein, some nanowire growths are on the surface of foamy graphite, some nano wires and foamy graphite weave in, both are evenly compounded to form composite material in general.Fig. 2 c is the nickel hydroxide nano line amplified separately, and the diameter of nano wire is between 20-40nm.
The mass percent of embodiment 3 nickel hydroxide nano line is the preparation of the composite material of 30%
(1) with sucrose and ammonium chloride with the ratio of mol ratio 1:2 1500 DEG C, roasting 2 hours under argon gas atmosphere, obtain the foamy graphite with three-dimensional porous structure.
(2) foamy graphite joins in potassium hydroxide solution and stirs 4 hours in (mass ratio 1), leaves standstill 20 and as a child filters afterwards, and 60 DEG C of dryings obtain after 24 hours activating foamy graphite.
(3) activation foamy graphite and nitration mixture (sulfuric acid: nitric acid=3:1), ultrasonic lower acidifying 2 hours, obtain acidifying foamy graphite after washing drying.
(4) described acidifying foamy graphite is joined (mass ratio 0.82) in nickel sulfate solution and be mixed to form unit for uniform suspension, NaOH (nickelous sulfate and NaOH mol ratio are 1) solution is under agitation slowly added drop-wise in described suspension.Hydrothermal treatment consists 24 hours at 100 DEG C.The dry composite material obtaining foamy graphite and nickel hydroxide nano line of finally washing.
Embodiment 4 utilizes urea to carry out the preparation of the composite material precipitated
(1) with sucrose and ammonium chloride with the ratio of mol ratio 2.5:1 1300 DEG C, roasting 3 hours under argon gas atmosphere, obtain the foamy graphite with three-dimensional porous structure.
(2) foamy graphite joins in potassium hydroxide solution and stirs 4 hours in (mass ratio 1), leaves standstill 20 and as a child filters afterwards, and 60 DEG C of dryings obtain after 24 hours activating foamy graphite.
(3) activation foamy graphite and nitration mixture (sulfuric acid: nitric acid=3:1), ultrasonic lower acidifying 5 hours, obtain acidifying foamy graphite after washing drying.
(4) described acidifying foamy graphite is joined (mass ratio 0.06) in nickel sulfate solution and be mixed to form unit for uniform suspension, urea (nickelous sulfate and urea mol ratio are 1) solution is under agitation slowly added drop-wise in described suspension.Hydrothermal treatment consists 24 hours at 100 DEG C.The dry composite material obtaining foamy graphite and nickel hydroxide nano line of finally washing.
Reference examples 1, activation foamy graphite
(1) with sucrose and ammonium chloride with the ratio of 1:2 1000 DEG C, roasting 2 hours under argon gas atmosphere, obtain the foamy graphite with three-dimensional porous structure.
(2) foamy graphite joins in potassium hydroxide solution and stirs 4 hours in (mass ratio 0.1), leaves standstill 20 and as a child filters afterwards, and 60 DEG C of dryings obtain after 24 hours activating foamy graphite.
Reference examples 2, nickel hydroxide nano line
Sodium hydroxide solution is under agitation slowly added drop-wise in nickel sulfate solution.Hydrothermal treatment consists 24 hours at 100 DEG C.Finally wash drying and obtain nickel hydroxide nano line.
Application examples
The product prepare embodiment 1-4 and reference examples 1-2 and superconduction carbon, PTFE mix according to the ratio of 80:15:5, are coated onto in nickel foam, obtain work electrode after compressing tablet drying.Capacity measurement adopts three-electrode system, and active material is work electrode, Pt electrode as to electrode, Hg-Hg
2cl
2electrode, as reference electrode, carries out constant current charge-discharge test in 6M KOH solution, after calculating to electrode ratio capacitance, the results are shown in Table 1.
Table 1
Nickel hydroxide nano line-foamy graphite of the present invention (30-85%) when the mass percent of nickel hydroxide is higher has higher ratio capacitance and good cyclical stability as shown in Table 1, and nickel hydroxide nano line and the combination both foamy graphite have given full play to both advantage.In the scope of above-mentioned 30-85%, along with the rising of the mass percent of the foamy graphite as material with carbon element, cyclical stability increases.And NaOH as the product obtained when precipitation reagent than urea as better during precipitation reagent.
In addition, applicant, by the composite material of the mass percent of a large amount of different hydro nickel oxide, utilizes different acidificatoin time to contrast, and time the mass percent of discovery nickel hydroxide is 85%, ratio capacitance is higher, and stability is also good.Wherein in an embodiment, although higher as specific capacity when precipitation reagent with urea, the less stable of circulation, the composite material that this embodiment provides cannot effectively be applied.Fig. 3 gives ratio capacitance and the cyclical stability of embodiment 1, as can be seen from the figure, the ratio capacitance of composite material of the present invention is apparently higher than independent nickel hydroxide and foamy graphite, illustrate that their compound can improve the performance of material, can also retain 90% after the cyclical stability 3000 times of material in addition, be the electrode material with applications well prospect.
In sum, nickel hydroxide nano line-foamy graphite composite material of the present invention has higher specific area, more pore passage structure, and the nano wire pattern of nickel hydroxide greatly can both improve electrical property and the stability of material.And last handling process is simple, can large-scale application in follow-up commercial Application and industrial amplification process.
Above-described, be only preferred embodiment of the present invention, and be not used to limit scope of the present invention, the above embodiment of the present invention can also make a variety of changes.Namely every claims according to the present patent application and description are done simple, equivalence change and modify, and all fall into the claims of patent of the present invention.The not detailed description of the present invention be routine techniques content.
Claims (10)
1. prepare a method for composite material, it is characterized in that, said method comprising the steps of:
S1, provides the foamy graphite with three-dimensional porous structure;
S2, joins described foamy graphite in potassium hydroxide solution and activates, and obtains activating foamy graphite after washing drying;
S3, joins described activation foamy graphite in nitration mixture and carry out acidifying under ultrasonic, obtains acidifying foamy graphite after washing drying; And
S4, joins described acidifying foamy graphite in nickel sulfate solution and is mixed to form unit for uniform suspension, be slowly added drop-wise to by precipitation reagent in described suspension, the dry composite material obtaining foamy graphite and nickel hydroxide nano line of washing after hydrothermal treatment consists.
2. method according to claim 1, is characterized in that, in described step S4, described precipitation reagent is nickel hydroxide, NaOH or urea.
3. method according to claim 1, is characterized in that, in described step S4, is slowly added drop-wise in described suspension by precipitation reagent with vigorous stirring.
4. method according to claim 1, is characterized in that, in described step S4, the mass ratio of described acidifying foamy graphite and described nickelous sulfate is 0.02-0.1.
5. method according to claim 4, is characterized in that, the mass ratio of described acidifying foamy graphite and described nickelous sulfate is 0.03-0.82.
6. method according to claim 4, is characterized in that, the mol ratio of described nickelous sulfate and described precipitation reagent is 1-3.
7. method according to claim 1, is characterized in that, described hydrothermal temperature is 100-180 DEG C.
8. the composite material that the method according to any one of the claims prepares, is characterized in that, described composite material is the composite material of foamy graphite and nickel hydroxide nano line.
9. one kind according to Claim 8 described in composite material on the capacitor as the application of electrode material.
10. application according to claim 9, is characterized in that, the mass percent of the nickel hydroxide in described composite material is 30-85%.
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| CN106920962A (en) * | 2017-04-25 | 2017-07-04 | 华南理工大学 | A kind of nickel oxide/graphite composite nano materials for lithium ion battery and preparation method and application |
| CN114875430A (en) * | 2022-04-19 | 2022-08-09 | 中国科学院过程工程研究所 | Graphite-based bifunctional electrosynthesis hydrogen peroxide catalytic material and preparation method thereof |
| CN115974114A (en) * | 2023-03-18 | 2023-04-18 | 河北坤天新能源股份有限公司 | Quick-filling graphite composite material and preparation method thereof |
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| CN104599863B (en) | 2017-07-18 |
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