CN110344125B - Batch electrospinning device and method for preparing nanofiber membranes by same - Google Patents
Batch electrospinning device and method for preparing nanofiber membranes by same Download PDFInfo
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- CN110344125B CN110344125B CN201910719966.3A CN201910719966A CN110344125B CN 110344125 B CN110344125 B CN 110344125B CN 201910719966 A CN201910719966 A CN 201910719966A CN 110344125 B CN110344125 B CN 110344125B
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- spray head
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- fiber
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- 238000001523 electrospinning Methods 0.000 title claims abstract description 23
- 239000002121 nanofiber Substances 0.000 title claims abstract description 19
- 239000012528 membrane Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 7
- 239000007921 spray Substances 0.000 claims abstract description 54
- 238000009987 spinning Methods 0.000 claims abstract description 47
- 239000000835 fiber Substances 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 238000000151 deposition Methods 0.000 claims abstract description 18
- 230000008021 deposition Effects 0.000 claims abstract description 15
- 238000003860 storage Methods 0.000 claims abstract description 15
- 230000033001 locomotion Effects 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000013049 sediment Substances 0.000 claims abstract description 6
- 230000005684 electric field Effects 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 5
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000010041 electrostatic spinning Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005147 X-ray Weissenberg Methods 0.000 description 1
- 238000001467 acupuncture Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a batch electrospinning device and a method for preparing nanofiber membranes by the same, wherein the batch electrospinning device comprises a solution tank, a spray head, a metering pump, a liquid storage tank, a driving system, a fiber depositor, a three-dimensional motion platform and a high-voltage power supply; the spray head is arranged in the solution tank and comprises a rotary needle and a plurality of annular flow limiting rings; the annular flow-limiting rings are coaxially arranged with the rotating needle, and are equidistantly arranged along the axial direction of the rotating needle; the lower end of the rotary needle extends out of the solution tank and is connected with a driving system; the solution tank is sequentially communicated with the metering pump and the liquid storage tank; the fiber deposition device is arranged above the spray head, and the position of the fiber deposition device in the working range is changed through the three-dimensional motion platform; the high-voltage power supply is electrically connected with the fiber sediment device, and the solution tank, the spinning solution and the spray head are grounded. The invention utilizes the Wessenberg effect and the capillary phenomenon to supply liquid to the spray head, and solves the problems of low fiber manufacturing yield, easy blockage of the spray head and the like in the prior art.
Description
Technical Field
The invention belongs to the technical field of electrostatic spinning, and particularly relates to a batch electrospinning device and a method for preparing a nanofiber membrane by using the same.
Background
The electrostatic spinning technology is used as one of the nanofiber manufacturing technologies, and is widely applied due to the advantages of simple technology, various spinnability materials and the like. The electrostatic spinning device mainly comprises a high-voltage power supply, a spray head, a collecting device and the like, wherein the high-voltage power supply enables a high-voltage electric field to be generated between the spray head and the collecting device, at the moment, charges are accumulated on the surface of hanging liquid drops at the spray head opening, the liquid drops gradually form taylor cones and are sprayed to the collecting device, and along with the processes of jet whip, stretching, splitting and the like, the liquid drops are finally deposited on the collecting device in a nanofiber form.
The traditional electrostatic spinning technology uses a single needle point as a spinneret, and a single jet flow is generated in the electrohydraulic coupling process, so that the yield is not ideal; in addition, when the viscosity of the spinning solution is high, the spinning needle is easy to be blocked, and the electrospinning is interrupted. Therefore, the single needle electrospinning yield is typically 0.02g/h, which cannot meet the yield requirements of batch electrospun nanofiber membranes. In this regard, researchers in the field of electrospinning have conducted research on mass electrospinning apparatuses.
The Elmarco company supplies the spinning solution by using a cylindrical rotating electrode, so that the spinning yield is effectively improved, and world patent application is filed (WO 2005024101). In addition, the technologies of bubble batch electrospinning, roller electrode batch electrospinning, wire electrode batch electrospinning and the like can well solve the problems that the traditional spinning head is easy to block and difficult to clean, and a plurality of superfine jet streams are formed, so that the spinning efficiency is improved.
Disclosure of Invention
The invention aims to: the invention aims to overcome the defects of the prior art and provide a batch electrospinning device which is not easy to block a spinning head and easy to clean, can form a plurality of superfine jet flows and improve the spinning efficiency and a method for preparing a nanofiber membrane.
The technical scheme is as follows: the aim of the invention is achieved by the following technical scheme:
the invention provides a batch electrospinning device, which comprises a solution tank, a spray head, a metering pump, a liquid storage tank, a driving system, a fiber sediment device, a three-dimensional motion platform and a high-voltage power supply, wherein the spray head is arranged on the solution tank;
the spray head is arranged in the solution tank and comprises a rotary needle and a plurality of annular flow limiting rings; the annular flow-limiting rings are coaxially arranged with the rotating needle, and the annular flow-limiting rings are equidistantly arranged along the axial direction of the rotating needle; the lower end of the rotary needle extends out of the solution tank and is connected with a driving system; the solution tank is sequentially communicated with the metering pump and the liquid storage tank; the fiber deposition device is arranged above the spray head, and the position of the fiber deposition device in the working range is changed through the three-dimensional motion platform; the high-voltage power supply is electrically connected with the fiber sediment device, and the solution tank, the spinning solution and the spray head are grounded.
The driving system is arranged below the solution tank and comprises a rotating motor, a coupler and a motor controller; the output shaft of the rotating motor is in transmission connection with the spray head through a coupler, and the spray head is driven by a driving system to rotate around the axis of the spray head; the rotating motor is electrically connected with the motor controller.
At least one spray head is arranged in the solution tank, and the spray heads are uniformly arranged in the solution tank.
The diameter of the outer surface of the rotary needle is 1 mu m-1 mm, and the length is 50 mu m-1 cm.
The inner diameter of the annular flow-limiting ring is 100 mu m-2 mm, the width is 300 mu m-5 mm, and the section of the annular flow-limiting ring is rectangular.
The distance between the fiber sediment device and the top of the spray head is 5 mm-100 cm.
The invention also provides a preparation method for preparing the nanofiber membrane by adopting the batch electrospinning device, which comprises the following steps:
1) Storing the prepared spinning solution into a liquid storage tank;
2) Setting the liquid supply speed of a metering pump, and pumping the spinning liquid into a solution tank;
3) Setting the rotating speed of a rotating motor, and driving a rotating needle to rotate around the axis of the rotating motor so that the spinning solution climbs to the top of the spray head;
4) Setting the output voltage of a high-voltage power supply, forming a Taylor cone by the spinning solution at the top of a spray head under the action of a shearing force and a high-voltage electric field, spraying the Taylor cone to a fiber depositor in a jet flow mode, and finally depositing the Taylor cone on the fiber depositor in a nanofiber membrane mode;
5) And (3) by setting a three-dimensional motion platform, the prepared nanofiber membrane is transported out of the spinning area in time.
Preferably, the flow rate of the liquid supplied by the metering pump is 10 mu l/hr to 100ml/hr.
Preferably, the rotating speed of the rotating motor ranges from 1 RPM to 8000RPM.
Preferably, the output voltage range of the high-voltage power supply is 1-70 kV.
The beneficial effects are that:
(1) The batch electrospinning device is provided with the rotating needle, when the rotating needle rotates, the spinning solution can spontaneously supply the solution to the top of the spray head along the axial direction of the rotating needle, the solution consumption speed is automatically matched with the spinning speed, and the uniformity of fibers is improved;
(2) The batch electrospinning device is provided with a plurality of annular current limiting rings, and the thickness of the solution at the periphery of a rotating needle is controlled; meanwhile, the solution can be conveyed in the gap between the rotary needle and the annular flow-limiting ring to generate capillary phenomenon, which is beneficial to the solution conveying;
(3) According to the batch electrospinning device, the plurality of annular current-limiting rings are uniformly arrayed along the axial direction of the rotary needle, and a certain gap is reserved between the adjacent annular current-limiting rings, so that the contact area between the solution and the annular current-limiting rings is reduced, and the problem of nozzle blockage is avoided to a certain extent;
(4) When the rotating needle is driven by the rotating motor to spin, the spinning solution near the rotating needle can generate a Wessenberg phenomenon; the batch electrospinning device utilizes the Wessenberg effect and the capillary phenomenon to supply liquid to the spray head, and solves the problems of low fiber manufacturing yield, easy blockage of the spray head and the like in the prior art.
Drawings
FIG. 1 is a schematic structural view of a batch electrospinning apparatus according to the present invention.
In the figure: 1-rotating motor, 2-solution tank, 3-liquid storage tank, 4-shower nozzle, 41-rotating needle, 42-annular flow-limiting ring, 5-metering pump, 6-high voltage power supply, 7-Taylor cone, 8-three-dimensional motion platform, 9-fiber deposition device, 10-motor controller, 11-jet, 12-coupling and 13-spinning solution.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific embodiments and drawings, but the scope of the present invention is not limited to the embodiments.
Example 1:
as shown in fig. 1: a batch electrospinning device comprises a solution tank 2, a spray head 4, a metering pump 5, a liquid storage tank 3, a driving system, a fiber sediment device 9, a three-dimensional motion platform 8 and a high-voltage power supply 6.
The spray head 4 is arranged in the solution tank 2, and the spray head 4 consists of a rotary needle 41 and 4 annular flow-limiting rings 42; the annular flow-limiting rings 42 are coaxially arranged with the rotary needle 41, the annular flow-limiting rings 42 are equidistantly arranged along the axial direction of the rotary needle 41, and the lower end of the rotary needle 41 extends out of the solution tank 2 and is connected with a driving system; the spin speed of the rotating needle 41 ranges from 1 to 8000RPM. Wherein the rotary needle 41 can be a medical acupuncture needle, a tungsten probe and the like, the diameter of the outer surface is 1 mu m-1 mm, and the length is 50 mu m-1 cm; the annular restrictor 42 has an inner diameter ranging from 100 μm to 2mm and a width ranging from 300 μm to 5mm, and a rectangular cross section.
The driving system is arranged below the solution tank 2 and consists of a rotating motor 1, a coupling 12 and a motor controller 10; the output shaft of the rotating motor 1 is in transmission connection with the spray head 4 through a coupling 12, and the spray head 4 is driven by a driving system and can smoothly rotate around the axis of the spray head; the rotating electric machine 1 is electrically connected with the motor controller 10, and the output rotation speed of the rotating electric machine 1 can be controlled by setting the motor controller 10, so that the rotation speed of the spray head 4 is controlled.
A metering pump 5 is arranged between the solution tank 2 and the liquid storage tank 3, the solution tank 2 is communicated with the metering pump 5 and the liquid storage tank 3, the liquid supply speed of the metering pump 5 to the solution tank 2 is controlled, and the spinning solution 13 in the liquid storage tank 3 can be pumped into the solution tank 2, so that the solution height of the spinning solution 13 in the solution tank 2 meets the spinning requirement; the flow rate of the liquid supplied by the metering pump 5 is 10 mu l/hr to 100ml/hr.
The fiber deposition device 9 is arranged above the spray head 4, and the position of the fiber deposition device 9 in the working range can be changed through the three-dimensional movement platform 8, so that the spinning interval is changed, and the formed nanofiber membrane can be conveyed out of the fiber deposition area; the high-voltage power supply 6 is electrically connected with the fiber deposition device 9, the solution tank 2, the spinning solution 13 and the spray head 4 are grounded, and the electric interference of the high-voltage electric field to the rotating motor 1 and related circuits can be avoided by adopting a solution grounding mode; the fiber deposition device 9 is a collection plate or a roller or a parallel electrode or an electrode net and other various collection devices in the spinning technical field, and the distance between the fiber deposition device and the spray head 4 is 5 mm-100 cm; the voltage output range of the high-voltage power supply 6 is 1-70 kV.
Example 2:
based on the apparatus of example 1, this example relates to a method for preparing a nanofiber membrane as follows:
the assembly is assembled according to FIG. 1, wherein the outer diameter of the rotating needle 41 is 200 μm, the length of the rotating needle 41 is 50cm, the inner diameter of the annular flow-limiting ring 42 is 800 μm, the width is 100 μm, the distance between adjacent annular flow-limiting rings 42 is 500 μm, and the pole spacing between the fiber depositor 9 and the spray head 4 is 15cm;
1) The prepared spinning solution 13 (12% polyoxyethylene PEO solution, alcohol, distilled water and volume ratio of alcohol to distilled water 1:1) is stored in a liquid storage tank 3;
2) Setting the liquid supply speed of the metering pump 5 to 800 mu l/hr, and pumping the spinning liquid 13 into the solution tank 2;
3) Setting the rotating speed of the rotating motor 1 to 4900RPM, driving the rotating needle 41 to rotate around the axis of the rotating needle, and enabling the spinning solution 13 to climb to the top of the spray head 4 at the moment;
4) Setting the output voltage of the high-voltage power supply 6 to be 46kV, forming a Taylor cone 7 by the spinning solution 13 at the top of the spray head 4 under the action of a shearing force and a high-voltage electric field, spraying the spinning solution to the fiber depositor 9 in a jet flow mode, and finally depositing the spinning solution on the fiber depositor 9 in a nanofiber membrane mode;
5) And (3) by setting a three-dimensional motion platform 8, the prepared nanofiber membrane is transported out of the spinning area in time.
Further supplementary to this embodiment, the structure, dimensions and assembly relationship of the rotating needle 41 and the annular restrictor ring 42 are determined, provided that it is first ensured that the spinning dope 13 is capable of undergoing the wessenberg effect and the capillary effect therebetween.
Further to supplement the description of the embodiment, the metering pump 5 and the liquid storage tank 3 are arranged, and the continuous liquid supply is mainly carried out on the solution tank 2, so that the speed of pumping the spinning solution 13 is ensured to be equal to the speed of spraying the consumed spinning solution 13, the liquid level of the spinning solution 13 in the solution tank 2 is ensured to be unchanged, and the stability of the Weissenberg effect and the capillary phenomenon is ensured.
The key technology of the technical scheme provided by the invention is that the spray head 4 is composed of a rotary needle 41 and 4 annular current-limiting rings 42, and the spray head 4 of the embodiment mainly has the following two innovation points: first, when the rotating needle 41 is driven by the rotating motor 1 to spin, the spinning solution 13 near the rotating needle 41 will generate a wessenberg phenomenon; second, there are 4 annular restrictor rings 42, and the spinning solution 13 may also exhibit capillary phenomenon when the spinning solution is transported between the outer surface of the rotating needle 41 and the inner surface of the annular restrictor rings 42. The spinning simultaneously has the wessenberg effect and the capillary effect in the spray head 4, so that the spinning solution 13 in the solution tank 2 is stably and continuously conveyed to the tip of the spray head 4, and is subjected to electrohydraulic coupling under the action of an electric field, and finally deposited on the fiber depositor 9 in the form of a nanofiber membrane.
As described above, although the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limiting the invention itself. Various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method for preparing a nanofiber membrane by adopting a batch electrospinning device is characterized by comprising the following steps of: the batch electrospinning device comprises a solution tank, a spray head, a metering pump, a liquid storage tank, a driving system, a fiber deposition device, a three-dimensional motion platform and a high-voltage power supply;
the spray head is arranged in the solution tank and comprises a rotary needle and a plurality of annular flow limiting rings; the annular flow-limiting rings are arranged on the periphery of the rotating needle, are coaxially arranged with the rotating needle, and are equidistantly arranged along the axial direction of the rotating needle; the lower end of the rotary needle extends out of the solution tank and is connected with a driving system; the solution tank is sequentially communicated with the metering pump and the liquid storage tank; the fiber deposition device is arranged above the spray head, and the position of the fiber deposition device in the working range is changed through the three-dimensional motion platform; the high-voltage power supply is electrically connected with the fiber deposition device, and the solution tank, the spinning solution and the spray head are grounded;
the preparation method comprises the following steps:
1) Storing the prepared spinning solution into a liquid storage tank;
2) Setting the liquid supply speed of a metering pump, and pumping the spinning liquid into a solution tank;
3) Setting the rotating speed of a rotating motor, and driving a rotating needle to rotate around the axis of the rotating motor so that the spinning solution climbs to the top of the spray head;
4) Setting the output voltage of a high-voltage power supply, forming a Taylor cone by the spinning solution at the top of a spray head under the action of a shearing force and a high-voltage electric field, spraying the Taylor cone to a fiber depositor in a jet flow mode, and finally depositing the Taylor cone on the fiber depositor in a nanofiber membrane mode;
5) And (3) by setting a three-dimensional motion platform, the prepared nanofiber membrane is transported out of the spinning area in time.
2. The method of manufacturing according to claim 1, characterized in that: the driving system is arranged below the solution tank and comprises a rotating motor, a coupler and a motor controller; the output shaft of the rotating motor is in transmission connection with the spray head through a coupler, and the spray head is driven by a driving system to rotate around the axis of the spray head; the rotating motor is electrically connected with the motor controller.
3. The method of manufacturing according to claim 1, characterized in that: at least one spray head is arranged in the solution tank, and the spray heads are uniformly arranged in the solution tank.
4. The method of manufacturing according to claim 1, characterized in that: the diameter of the outer surface of the rotary needle is 1 mu m-1 mm, and the length is 50 mu m-1 cm.
5. The method of manufacturing according to claim 1, characterized in that: the inner diameter of the annular flow-limiting ring is 100 mu m-2 mm, the width is 300 mu m-5 mm, and the section of the annular flow-limiting ring is rectangular.
6. The method of manufacturing according to claim 1, characterized in that: the distance between the fiber sediment device and the spray head is 5 mm-100 cm.
7. The method of manufacturing according to claim 1, characterized in that: the flow rate of the liquid supplied by the metering pump is 10 mu l/hr-100 ml/hr.
8. The method of manufacturing according to claim 1, characterized in that: the rotating speed of the rotating motor is 1-8000 RPM.
9. The method of manufacturing according to claim 1, characterized in that: the output voltage of the high-voltage power supply is 1-70 kV.
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CN201910719966.3A CN110344125B (en) | 2019-08-06 | 2019-08-06 | Batch electrospinning device and method for preparing nanofiber membranes by same |
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CN201910719966.3A CN110344125B (en) | 2019-08-06 | 2019-08-06 | Batch electrospinning device and method for preparing nanofiber membranes by same |
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CN110344125B true CN110344125B (en) | 2024-02-02 |
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CN111364108B (en) * | 2020-03-24 | 2021-10-15 | 陕西工业职业技术学院 | Electrostatic spinning injection system |
CN111394806B (en) * | 2020-04-20 | 2023-07-18 | 南京工业职业技术学院 | Preparation device and preparation method of three-dimensional fiber membrane |
CN115262004A (en) * | 2022-08-03 | 2022-11-01 | 江南大学 | Free liquid level multi-jet electrostatic spinning device and method for producing nano fibers |
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