CN115341306B - Graphene aerogel fiber and preparation method thereof - Google Patents
Graphene aerogel fiber and preparation method thereof Download PDFInfo
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- CN115341306B CN115341306B CN202211161888.8A CN202211161888A CN115341306B CN 115341306 B CN115341306 B CN 115341306B CN 202211161888 A CN202211161888 A CN 202211161888A CN 115341306 B CN115341306 B CN 115341306B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention relates to graphene aerogel fibers and a preparation method thereof. According to the preparation method, the mixed solution of graphene oxide and polyvinyl alcohol is obtained in a solution blending mode, the mixed solution is concentrated into a spinning solution, the spinning solution is discharged into an ethanol bath for cold spinning, the graphene oxide/polyvinyl alcohol aerogel fiber is obtained through freeze drying, and the graphene aerogel fiber is obtained through chemical reduction.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a graphene aerogel fiber and a preparation method thereof.
Background
Aerogel is a lightweight porous material with three-dimensional nano-network structure, high specific surface area, low density and high porosity, and is also a solid material with the lowest heat conductivity reported at present. Therefore, the aerogel is used for high-efficiency heat insulation in various fields of manned aerospace, aviation, fire protection, construction, chemical industry and the like. Based on the demand of special clothes such as space suit, fire suit and the like on high-performance heat-insulating fabrics, researchers develop related researches on aerogel fibers. Besides, the aerogel fiber has the characteristic of large external surface area, and has wide application prospect in the fields of rapid adsorption, catalytic loading, energy storage and the like. The prior art discloses that GO solution is discharged as spinning solution into liquid nitrogen, frozen fibers are formed with liquid nitrogen as a cold source, GO aerogel fibers are obtained by freeze-drying with a freeze dryer, and final rGO aerogel fibers are obtained by annealing in a tube furnace to reduce GO (Xu, z.; zhang, y.; li, p.; gao, c.; strong, conducive, lightweight, neat Graphene Aerogel Fibers with Aligned ports.acs Nano 2012,6 (8), 7103-7113).
The current methods for preparing aerogel fibers are mainly divided into two categories: firstly, discharging spinning solution into liquid nitrogen through simple liquid nitrogen as a cold source to form frozen fibers, and freeze-drying through a freeze dryer to remove moisture under the condition of keeping a network structure in the fibers to obtain aerogel fibers; another method needs to design a cooling device specifically to achieve the purpose of freezing the fiber, and the method has the problems of complex process and the like.
The present invention has been made in view of the above-mentioned circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the graphene aerogel fiber and the preparation method thereof, and the graphene aerogel fiber prepared by the method has the advantages of controllable pore diameter, ordered pore arrangement, simple preparation method and no need of a specific cooling device.
The first object of the invention is to provide a method for preparing graphene aerogel fibers in low-temperature liquid, which comprises the steps of cold spinning graphene oxide spinning solution in an ethanol bath, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen.
Further, the ethanol bath is formed by mixing ethanol and liquid nitrogen according to the volume ratio of 1:1-5:2.
Further, the temperature of the ethanol bath is-100 to-30 ℃.
The freezing point of the ethanol is-114 ℃ and is lower than-100 ℃, and the temperature of the ethanol bath is controlled between-100 ℃ and-30 ℃ because the ethanol can be frozen.
Further, the method specifically comprises the following steps:
(1) Mixing graphene oxide solution and polyvinyl alcohol solution, stirring, and concentrating to obtain spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning to obtain frozen fibers, and performing freeze drying on the frozen fibers to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And reducing the graphene oxide/polyvinyl alcohol aerogel fiber, washing with water, soaking in ethanol, and naturally drying to obtain the graphene aerogel fiber.
Further, in the step (1), the concentration of graphene oxide in the graphene oxide solution is 4-6mg/ml, and the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 18-22mg/ml.
Further, in the step (1), the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 7-11:1.
Graphene oxide should occupy the main body in the application, and excessive polyvinyl alcohol ratio can affect various properties of subsequent materials, such as conductive properties. Too small a polyvinyl alcohol ratio can affect the viscosity of the spinning solution, thereby affecting the formation of gel fibers and the mechanical properties of subsequent fibers.
Further, stirring for 4-5 days in the step (1), and concentrating until the concentration of the graphene oxide is 23-27mg/ml.
Because mechanical stirring is adopted to endow the spinning solution with shearing orientation, the concentration of the spinning solution mainly depends on natural evaporation, so that the stirring period is longer and 4-5 days are required; the concentration of the graphene oxide is 23-27mg/ml, and the purpose of the graphene oxide is mainly to ensure that the viscosity of the spinning solution is high enough to obtain gel fibers.
Further, the discharge speed of the spinning solution in the step (2) is 50-100ml/h, the inner diameter of the spinning needle is 1050-1550 μm, the freeze-drying temperature is-65 to-45 ℃, and the pressure is 4-12Pa.
The aim of the discharge speed of 50-100ml/h and the inner diameter of the spinning needle of 1050-1550 μm is to ensure the formation of gel fiber, and the parameters of the freeze drying condition are the working parameter range of the freeze dryer.
Further, the step (3) is reduced to the state that the graphene oxide/polyvinyl alcohol aerogel fiber is put into 55-57% hydroiodic acid by mass fraction, reduced for 10-14h at 75-85 ℃, washed by water until the solution is colorless, soaked in absolute ethyl alcohol for 0.8-1.2h, and repeated for a plurality of times until the absolute ethyl alcohol is colorless.
The purpose of reducing for 10-14h at 75-85 ℃ is to ensure that the graphene oxide is fully reduced, and the purpose of subsequent water washing and absolute ethyl alcohol soaking is to wash off iodine simple substances remained on the fibers.
The graphene oxide solution can be prepared by adopting an improved Hummers method, can also be prepared by adopting other methods, is not particularly limited by the preparation method of the graphene oxide solution, and is prepared by any method within the protection scope of the invention.
The second object of the invention is to provide the graphene aerogel fiber prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the graphene aerogel fiber is prepared by using low-temperature liquid prepared by ethanol under the condition of non-liquid nitrogen ultralow temperature, the mixed solution of graphene oxide and polyvinyl alcohol is obtained in a solution blending mode, the mixed solution is concentrated into spinning solution, the spinning solution is discharged into an ethanol bath for cold spinning, the graphene oxide/polyvinyl alcohol aerogel fiber is obtained by freeze drying, and the graphene aerogel fiber is obtained through chemical reduction.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a process flow for preparing graphene aerogel fibers in a cryogenic liquid according to the present invention;
FIG. 2 is a cross-sectional morphology of graphene aerogel fibers prepared in comparative example 1 and examples 1-5 prior to reduction;
FIG. 3 is a cross-sectional morphology of the graphene aerogel fibers prepared in comparative example 1 and examples 1-5 after reduction;
FIG. 4 is a graph of tensile strength versus temperature for graphene aerogel fibers prepared in comparative example 1 and examples 1-5;
FIG. 5 is a cross-sectional morphology of the graphene aerogel fibers prepared in comparative example 2 before and after reduction;
fig. 6 is a stress-strain graph of graphene aerogel fibers prepared in comparative example 2 and example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
Example 1
The method for preparing graphene aerogel fibers in low-temperature liquid in the embodiment comprises the following specific preparation method:
(1) Mixing a graphene oxide solution and a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 18mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9:1, stirring for 4 days, and concentrating until the concentration of graphene oxide is 25mg/ml to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 1:1, the temperature of the ethanol bath is-100 ℃, the discharging speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and performing freeze drying on the frozen fibers in a freeze dryer, wherein the freeze drying temperature is-65 ℃ and the pressure is 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And (3) placing the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydroiodic acid, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 2
The method for preparing graphene aerogel fibers in low-temperature liquid in the embodiment comprises the following specific preparation method:
(1) Mixing a graphene oxide solution and a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 20mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9:1, stirring for 4 days, and concentrating until the concentration of graphene oxide is 25mg/ml to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 11:10, the temperature of the ethanol bath is-80 ℃, the discharging speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and performing freeze drying on the frozen fibers in a freeze dryer, wherein the freeze drying temperature is-65 ℃ and the pressure is 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And (3) placing the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydroiodic acid, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 3
The method for preparing graphene aerogel fibers in low-temperature liquid in the embodiment comprises the following specific preparation method:
(1) Mixing a graphene oxide solution and a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 22mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9:1, stirring for 4 days, and concentrating until the concentration of graphene oxide is 25mg/ml to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 6:5, the temperature of the ethanol bath is-65 ℃, the discharging speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and performing freeze drying on the frozen fibers in a freeze dryer, wherein the freeze drying temperature is-65 ℃ and the pressure is 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And (3) placing the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydroiodic acid, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 4
The method for preparing graphene aerogel fibers in low-temperature liquid in the embodiment comprises the following specific preparation method:
(1) Mixing a graphene oxide solution and a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 20mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9:1, stirring for 4 days, and concentrating until the concentration of graphene oxide is 25mg/ml to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 2:1, the temperature of the ethanol bath is-50 ℃, the discharging speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and performing freeze drying on the frozen fibers in a freeze dryer, wherein the freeze drying temperature is-65 ℃ and the pressure is 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And (3) placing the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydroiodic acid, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 5
The method for preparing graphene aerogel fibers in low-temperature liquid in the embodiment comprises the following specific preparation method:
(1) Mixing a graphene oxide solution and a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 19mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9:1, stirring for 4 days, and concentrating until the concentration of graphene oxide is 25mg/ml to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 5:2, the temperature of the ethanol bath is-30 ℃, the discharging speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and performing freeze drying on the frozen fibers in a freeze dryer, wherein the freeze drying temperature is-65 ℃ and the pressure is 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And (3) placing the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydroiodic acid, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Comparative example 1
The preparation method of the graphene aerogel fiber of the present comparative example is the same as that of example 2, except that the ethanol bath in step (2) is replaced with liquid nitrogen at a temperature of-196 ℃.
Comparative example 2
The preparation method of the graphene aerogel fiber of the present comparative example is the same as that of example 3, except that the spinning solution in step (1) is replaced by a pure GO solution from the mixed solution of graphene oxide and polyvinyl alcohol.
Test example 1
The graphene aerogel fibers prepared in examples 1-5 were tested for pore size and tensile strength as shown in table 1.
TABLE 1
It can be seen from table 1 that as the volume ratio of ethanol to liquid nitrogen increases, the temperature of the ethanol bath increases from-100 ℃ to-30 ℃ and the pore size increases from 1.65 μm to 8.25 μm, mainly because the freezing rate will have an effect on ice crystal nucleation and growth, as the temperature of the ethanol bath gradually decreases, the freezing rate increases, resulting in more ice crystals nucleating, and thus more smaller pores. The final fiber tensile strength increased from 0.38Mpa to 0.90Mpa and then decreased to 0.29Mpa, demonstrating that the ordered porous structure can improve the mechanical properties of the fiber.
Test example 2
The cross-sectional morphology of the graphene aerogel fibers prepared in comparative example 1 and examples 1 to 5 before and after reduction are shown in fig. 2 and 3, respectively, a to f in fig. 2 are the cross-sectional morphology of the graphene oxide/polyvinyl alcohol aerogel fibers before reduction in comparative example 1 and examples 1 to 5, respectively, and a to f in fig. 3 are the cross-sectional morphology of the graphene oxide/polyvinyl alcohol aerogel fibers after reduction in comparative example 1 and examples 1 to 5, respectively.
As can be seen from fig. 2 and 3, as the gel fiber gradually enters the low temperature ethanol bath, water within the fiber first crystallizes and nucleates near the fiber surface and then grows in the radial direction to form ordered ice crystals, while the GO/PVA solutes are repelled and compressed by the ice crystals, which are subsequently removed by freeze drying to give an ordered porous structure with the outward dispersion along the center, and the reduced pore structure is largely preserved with only slight shrinkage, and the morphology of the fiber obtained by freezing with liquid nitrogen and ethanol baths is not very different.
Test example 3
The graphene aerogel fibers prepared in comparative example 1 and examples 1-5 were tested for tensile strength versus temperature curves as shown in fig. 4.
As shown in FIG. 4, as the temperature of the freezing medium was changed from liquid nitrogen to a low-temperature ethanol bath and the ethanol bath was gradually increased, the tensile strength of the prepared fiber was increased from 0.36Mpa to 0.90Mpa and then decreased to 0.29Mpa, and it was concluded that the tensile strength of the prepared fiber was at most 0.90Mpa when the temperature of the ethanol bath was-65 ℃.
Test example 4
The cross-sectional morphology and stress-strain graphs of the graphene aerogel fibers prepared in comparative example 2 before and after reduction are shown in fig. 5 and 6, respectively, in fig. 5 a, b are cross-sectional morphology of the graphene oxide aerogel fibers before and after reduction in comparative example 2, and in fig. 6, stress-strain graphs of the graphene aerogel fibers prepared in comparative example 2 and example 3, respectively.
As shown in fig. 5, the cross-sectional morphology of the pure GO aerogel fiber before and after reduction is not greatly changed compared with that of the GO/PVA aerogel fiber, but it can be seen from the observation of fig. 6 that the tensile strength of the pure GO aerogel fiber after reduction is only less than 0.2MPa, and the tensile strength of the pure GO aerogel fiber after reduction is reduced by several times compared with that of the GO/PVA aerogel fiber, so that it is concluded that the addition of PVA helps to improve the mechanical properties of the fiber.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A method for preparing graphene aerogel fibers in a cryogenic liquid, the method comprising the steps of:
(1) Mixing graphene oxide solution and polyvinyl alcohol solution, stirring, and concentrating to obtain spinning solution;
(2) Discharging the spinning solution into an ethanol bath for cold spinning to obtain frozen fibers, and performing freeze drying on the frozen fibers to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) The graphene oxide/polyvinyl alcohol aerogel fiber is reduced, washed, soaked in ethanol and naturally dried to obtain the graphene aerogel fiber;
the ethanol bath is formed by mixing ethanol and liquid nitrogen, and the ethanol and the liquid nitrogen are mixed according to the volume ratio of 1:1-5:2;
the temperature of the ethanol bath is-100 to-30 ℃.
2. The method for preparing graphene aerogel fibers in a low-temperature liquid according to claim 1, wherein the concentration of graphene oxide in the graphene oxide solution in the step (1) is 4-6mg/ml, and the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 18-22mg/ml.
3. The method for preparing graphene aerogel fibers in a low-temperature liquid according to claim 1, wherein the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution in the step (1) is 7-11:1.
4. The method for preparing graphene aerogel fibers in a low-temperature liquid according to claim 1, wherein the graphene aerogel fibers are stirred in the step (1) for 4-5 days and concentrated to the concentration of graphene oxide of 23-27mg/ml.
5. The method for preparing graphene aerogel fibers in a low-temperature liquid according to claim 1, wherein the discharge speed of the spinning solution in the step (2) is 50-100ml/h, the inner diameter of a spinning needle is 1050-1550 μm, the temperature of freeze drying is-65 to-45 ℃, and the pressure is 4-12Pa.
6. The method for preparing graphene aerogel fibers in low-temperature liquid according to claim 1, wherein in the step (3), the graphene oxide/polyvinyl alcohol aerogel fibers are put into hydroiodic acid with the mass fraction of 55-57%, reduced for 10-14h at 75-85 ℃, washed with water until the solution is colorless, soaked in absolute ethyl alcohol for 0.8-1.2h, and repeated for a plurality of times until the absolute ethyl alcohol is colorless.
7. A graphene aerogel fiber prepared by the method of any one of claims 1-6.
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