WO2012077867A1 - Dispositif de fabrication de nanofibres - Google Patents

Dispositif de fabrication de nanofibres Download PDF

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Publication number
WO2012077867A1
WO2012077867A1 PCT/KR2011/003058 KR2011003058W WO2012077867A1 WO 2012077867 A1 WO2012077867 A1 WO 2012077867A1 KR 2011003058 W KR2011003058 W KR 2011003058W WO 2012077867 A1 WO2012077867 A1 WO 2012077867A1
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WIPO (PCT)
Prior art keywords
polymer solution
nozzle
jacket
upward
tip
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PCT/KR2011/003058
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English (en)
Korean (ko)
Inventor
이재환
김익수
Original Assignee
주식회사 톱텍
신슈 다이가쿠
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Publication of WO2012077867A1 publication Critical patent/WO2012077867A1/fr

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    • 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
    • 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
    • D01D13/00—Complete machines for producing artificial threads
    • 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
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • a nanofiber means the fiber which consists of a polymer material and whose average diameter is several nm-several thousand nm.
  • a polymer solution means the solution which melt
  • FIG. 5 (a) is a front view of the nanofiber manufacturing apparatus 900
  • FIG. 5 (b) is a perspective view around the upward nozzle 912
  • FIG. 5 (c) is a front view of the nozzle tip portion 913.
  • a plurality of upward nozzles 912 for discharging a polymer solution upwardly from a discharge port, and a plurality of upward nozzles
  • a nozzle block 910 having a polymer solution supply path 914 for supplying a polymer solution to 912 and a polymer solution recovery path 916 for recovering the polymer solution that has overflowed from an outlet of the upward nozzle 912, and a nozzle block Collector 920 disposed above 910, a power supply device 930 for applying a high voltage between the plurality of upward nozzles 912 and the collector 920, and a polymer solution serving as a raw material of nanofibers.
  • the metering pump 950 for supplying the polymer solution stored in the tank 940 to the polymer solution supply path 914 of the nozzle block 910, and the plurality of upward nozzles 912. Recovering the polymer solution flowed back to the tank 940 Recovery pump 960 is provided.
  • the nozzle tip 913 which is the tip of the upward nozzle 912, has a cylindrical shape with a wide tip as shown in FIGS. 5B and 5C.
  • the nanofiber manufacturing apparatus 900 since the nanofibers are electrospun by discharging the polymer solution from the discharge ports of the plurality of upward nozzles 912, the nanofiber manufacturing apparatus using the conventional downward nozzle
  • the droplet phenomenon (a phenomenon in which agglomerates of a polymer solution which did not radiate from the downward nozzle adheres to the long sheet as it is) does not occur, and it is possible to manufacture high quality nanofibers.
  • the nanofibers are field-spun while overflowing the polymer solution from the discharge ports of the plurality of upward nozzles 912, a sufficient amount of the polymer solution is always supplied to the upward nozzle. It becomes possible to manufacture nanofibers having a uniform quality.
  • nanofiber manufacturing apparatus 900 since it is possible to recover the polymer solution overflowed from the discharge ports of the plurality of upward nozzles 912 and reuse it as a raw material of the nanofibers, reducing the fee for use of the raw materials As a result, nanofibers can be produced at low cost. This also follows the flow of resource saving.
  • the solvent is volatilized from the polymer solution in the process of electric field spinning while overflowing the polymer solution from the discharge port of the upward nozzle, so that the vicinity of the discharge port of the upward nozzle is near. It has been found that there is a problem that a polymer solid is produced, and the polymer solid is attached to the "nanofiber to be a product" to degrade the quality of the nanofiber.
  • An object of the present invention is to provide a nanofiber manufacturing apparatus capable of solving the problem.
  • the nanofiber manufacturing apparatus of the present invention overflows from a plurality of upward nozzles for discharging a polymer solution upward from a discharge port, a polymer solution supply path for supplying the polymer solution to the plurality of upward nozzles, and a discharge port of the plurality of upward nozzles.
  • a nano-fiber manufacturing apparatus makes it possible to, (hereinafter referred to as the nozzle tip end portion), the front end portion of the upstream nozzle and the cylinder characterized in that it contains the axis and an oblique cut along the intersecting plane shape of the cylinder.
  • an angle formed between the axis of the cylinder and the plane is in the range of 15 ° to 60 °.
  • the polymer solution recovery path includes a receiving portion receiving the polymer solution overflowed from the discharge ports of the plurality of upward nozzles, and a plurality of nozzles covering the receiving portions and passing through each upward nozzle. And a plurality of jackets covering the side surfaces of each of the upward nozzles protruding from the plurality of nozzle holes, and the proximal end of the jacket as the jacket proximal end, and the distal end side of the jacket.
  • the said jacket tip part is thinner than the said jacket base part.
  • the jacket base end has a tubular shape with a constant thickness
  • the jacket end part has a tubular shape that gradually decreases in thickness from the connecting end of the jacket end part to the jacket base end. It is desirable to have.
  • the tip of the inclined surface portion formed on the tip side of the nozzle tip portion is preferably located above the tip of the jacket.
  • the interval d1 along the axis of the cylinder between the tip of the inclined surface portion and the tip of the jacket is preferably in the range of 0.1 mm to 2.0 mm.
  • the base end of the inclined surface portion formed on the tip side of the nozzle tip portion is preferably located below the tip of the jacket.
  • the distance d2 along the axis of the cylinder between the base end of the inclined surface portion and the tip of the jacket is preferably in the range of 0.1 mm to 1.0 mm.
  • the area of the area surrounded by the inner circumference of the jacket is S1
  • the nozzle tip portion is When making the area of the area
  • the lid portion further has a lid portion screw portion around the nozzle hole, and the jacket is a jacket side screw portion corresponding to the lid portion screw portion on a proximal side of the jacket base end portion. It is further preferred that the lid part and the jacket are coupled by fitting the lid part side screw part and the jacket side threaded part.
  • the polymer solution supply path further has a polymer solution supply path side threaded portion, and the upward nozzle corresponds to the polymer solution supply path side threaded portion on the proximal side of the upward nozzle.
  • the polymer solution supply path and the upward nozzle are coupled by fitting the polymer solution supply path side threaded portion and the upward nozzle side threaded portion, and the proximal end of the upward nozzle is a polygonal cylinder. It is preferable that it is formed in a shape.
  • a regeneration tank for storing the regenerated polymer solution as a raw material tank for storing the polymer solution as a raw material of the nanofibers, and a regeneration tank for regenerating the recovered polymer solution.
  • an intermediate tank for storing the polymer solution supplied from the raw material tank or the regeneration tank, a first transfer device for transferring the polymer solution from the polymer solution recovery path of the nozzle block to the regeneration tank;
  • a first transfer control device for controlling a transfer operation of the transfer device, a second transfer device for transferring the polymer solution from the raw material tank and the regeneration tank to the intermediate tank, and a transfer operation of the second transfer device It is preferable to further provide a 2nd conveyance control apparatus.
  • the "transfer device” includes a pipe through the polymer solution, a pump for transferring the polymer solution, and the like.
  • the “conveyor control apparatus” includes a valve for controlling whether or not the polymer solution passes and the amount of passage, a controller for controlling the operation of the valve or the pump described above.
  • the device further comprises a conveying device for conveying a long sheet, and at least the nozzle block and the collector, and as a field radiating device for depositing nanofibers on the surface of the long sheet. And a plurality of field radiating devices arranged in series along the conveying direction of the long sheet.
  • the nanofiber manufacturing apparatus of the present invention since the polymer solution is discharged by discharging the polymer fibers from the discharge ports of the plurality of upward nozzles, the nanofiber production using the conventional downward nozzle The droplet phenomenon seen in the case of the device does not occur, and it becomes possible to manufacture high quality nanofibers.
  • the nanofiber manufacturing apparatus of the present invention since a field of the nanofibers are electrospun while overflowing the polymer solution from the discharge ports of the plurality of upward nozzles, a sufficient amount of the polymer solution It is supplied to this upward nozzle, and it becomes possible to manufacture the nanofiber which has uniform quality.
  • the nanofiber production apparatus of the present invention since it is possible to recover the polymer solution that overflowed from the discharge ports of the plurality of upward nozzles and reuse it as a raw material of the nanofiber, as in the case of the conventional nanofiber production apparatus. As a result of reducing the fee for use of raw materials, it becomes possible to manufacture nanofibers at low manufacturing costs. This also follows the flow of resource saving.
  • the nozzle tip portion has a shape in which the cylinder is cut along a plane intersecting the cylinder at an oblique angle, so that the polymer solution that overflows from the discharge port of the upward nozzle has a nozzle. It flows quickly without staying at the tip. Therefore, the amount of solvent volatilized from the polymer solution in the process of electric field spinning can be extremely small, and the amount of polymer solid produced in the vicinity of the discharge port of the upward nozzle can be extremely small.
  • the nanofiber manufacturing apparatus of the present invention solves the problem that the polymer solids adhere to the nanofibers and degrade the quality of the nanofibers even when electrospinning while overflowing the polymer solution from the outlet of the upward nozzle. It becomes possible.
  • the angle formed between the axis of the cylinder and the plane is in the range of 15 ° to 60 °, so that the polymer overflows from the discharge port of the upward nozzle when the angle is 60 ° or less. This is because the solution flows more quickly without staying at the tip of the nozzle, and when the angle is 15 ° or less, the length of the inclined surface of the upward nozzle becomes too long so that the field emission condition is not disturbed. For losing.
  • the amount of solvent volatilized from the polymer solution overflowing from the discharge port of the upward nozzle can be further reduced by the movement of the jacket covering the side surface of the upward nozzle.
  • the jacket tip is thinner than the jacket base, the amount of solvent volatilized from the polymer solution overflowing from the discharge port of the upward nozzle can be further reduced.
  • the jacket base end has a tubular shape with a constant thickness
  • the jacket end part has a tubular shape that gradually decreases in thickness from the connecting end of the jacket end part to the jacket base end.
  • the thickness decreases slowly.
  • the thickness decreases by a fixed ratio.
  • the tip of the inclined surface portion formed on the tip side of the nozzle tip portion is located above the tip of the jacket, so that the electric field formed between the upward nozzle and the collector is stabilized. It is possible to produce nanofibers having a uniform quality.
  • the gap d1 is 2.0. In the case of mm or less, it becomes possible to further reduce the amount of solvent volatilization from the polymer solution overflowing from the discharge port of the upward nozzle, and when the distance d1 is 0.1 mm or more, between the upward nozzle and the collector This is because it is possible to produce nanofibers having a uniform quality since the electric field to be formed is stabilized.
  • the base end of the inclined surface portion formed on the tip side of the nozzle tip portion is located below the tip of the jacket, the amount of solvent volatilization from the polymer solution overflowing from the discharge port of the upward nozzle. Can be further reduced.
  • the distance d2 along the axis of the cylinder between the base end of the inclined surface portion and the tip end of the jacket is within the range of 0.1 mm to 1.0 mm, the distance d2 is 0.1. In the case of mm or more, it is possible to further reduce the amount of solvent volatilization from the polymer solution overflowing from the outlet of the upward nozzle. When the distance d2 is 1.0 mm or less, the polymer solution is collected from the outlet of the upward nozzle. This is because it is made to be sprayed stably toward the, it is possible to manufacture a nanofiber having a uniform quality.
  • the area of the area surrounded by the inner circumference of the jacket is S1
  • the nozzle tip portion is When the area of the area surrounded by the outer circumference is set to S2, the relationship of "S2 ⁇ S1-S2 ⁇ 4 x S2" is satisfied, so that "S1-S2" corresponds to the area of the gap between the upward nozzle and the jacket.
  • the lid portion further has a lid portion screw portion around the nozzle hole, and the jacket is a jacket side screw portion corresponding to the lid portion screw portion on a proximal side of the jacket base end portion.
  • the cover part and the jacket are coupled by fitting the cover part side screw part and the jacket side threaded part, the detachable jacket becomes easy, and a nanofiber manufacturing device is easy to manufacture and maintain. .
  • the polymer solution supply path further has a polymer solution supply path side threaded portion
  • the upward nozzle corresponds to the polymer solution supply path side threaded portion on the proximal side of the upward nozzle.
  • the polymer solution supply path and the upward nozzle are coupled by fitting the polymer solution supply path side threaded portion and the upward nozzle side threaded portion, and the proximal end of the upward nozzle is a polygonal cylinder. As the shape is made, the attachment and detachment of the upward nozzle becomes easy, and the nanofiber production apparatus is easy to manufacture and maintain.
  • the base end portion of the upward nozzle is formed in a polygonal cylindrical shape, the upward nozzle can be easily attached and detached using a tool such as a wrench, and the nanofiber production apparatus is more easily manufactured and maintained.
  • the recovered polymer solution is transferred to a regeneration tank, the composition of the polymer solution is measured and the solvent or other necessary components are added to the polymer solution according to the measurement result. It is possible to regenerate the solution into a polymer solution having the same composition as the original polymer solution or having an extremely close composition. For this reason, according to the nanofiber production apparatus of the present invention, while the overflowed polymer solution is recovered and reused as a raw material of the nanofibers, the spinning conditions (in this case, the composition of the polymer solution) in the field spinning process are maintained for a long time. It becomes possible to keep constant over, and it becomes possible to mass-produce nanofibers with uniform quality.
  • nanofiber manufacturing apparatus of the present invention it becomes possible to mass-produce nanofibers with higher productivity. It is also possible to mass-produce products in which nanofibers are thickly deposited, products in which various kinds of nanofibers are deposited, and the like.
  • medical products such as high-performance and highly sensitive textiles, beauty-related products such as healthcare, skin care, industrial materials such as wiping cloth, filters, and separators for secondary batteries , Medical separators such as capacitor separators, carriers of various catalysts, various sensor materials, electronic / mechanical materials, regenerative medical materials, biomedical materials, medical MEMS materials, biosensor materials, etc.
  • Usable nanofibers can be prepared.
  • FIG. 1 is a front view of a nanofiber manufacturing apparatus according to the embodiment.
  • FIG 3 is a cross-sectional view of the nozzle block in the embodiment.
  • FIG. 5 is a view for explaining a conventional nanofiber manufacturing apparatus.
  • 1 is a front view of a nanofiber manufacturing apparatus 1 according to an embodiment.
  • 2 is a front view of the field emission device 20 in the embodiment. 1 and 2, the case 100, the nozzle block 110, the raw material tank 200, the intermediate tank 230, and the regeneration tanks 270 and 272 are shown as cross-sectional views.
  • FIG. 3 is a cross-sectional view of the nozzle block 110 in the embodiment.
  • 4 is a diagram illustrating main parts of the nozzle block 110 in the embodiment.
  • FIG. 4A is an enlarged view of a range indicated by code A in FIG. 3
  • FIG. 4B is an enlarged view of a range indicated by code B in FIG. 4A
  • FIG. 4C Is a cross-sectional view of the nozzle base 130
  • FIG. 4D is a top view of the upward nozzle 126 and the jacket 134. As shown in FIG.
  • each figure is a schematic diagram, and the magnitude
  • the nanofiber manufacturing apparatus 1 which concerns on an Example has the long conveyed by the conveying apparatus 10 and the conveying apparatus 10 which convey the long sheet W at a predetermined
  • the nanofibers are deposited by the field radiating device 20 for depositing the nanofibers on the sheet W, the heating device 30 for heating the long sheet W in which the nanofibers are deposited, and the field radiating device 20.
  • the conveying apparatus 10, the electric field radiating apparatus 20, the heating apparatus 30, the ventilation system, the measuring apparatus 40, the feed rate control apparatus 50, and the VOC processing apparatus 70 mentioned later Open the main control device 60 (not shown) and the volatile components generated when the nanofibers are deposited on the long sheet W.
  • a VOC processing apparatus 70 (not shown) for extinguishing is removed.
  • the electric field radiating apparatus includes two field radiating apparatuses 20 arranged in series along a predetermined conveying direction in which the long sheet W is conveyed.
  • the conveying apparatus 10 is located between the feeding roller 11 which injects the long sheet W, the winding roller 12 which winds the long sheet W, and the feeding roller 11 and the winding roller 12.
  • the auxiliary roller 13 is provided.
  • the feeding roller 11 and the winding roller 12 are comprised by the structure which is rotationally driven by the drive motor which is not shown in figure.
  • the structure of the field emission apparatus 20 is mentioned later.
  • the heating device 30 is disposed between the field radiating device 20 and the air permeability measuring device 40, and heats the long sheet W in which the nanofibers are deposited.
  • the heating temperature varies depending on the type of the long sheet W or the nanofibers, but for example, the long sheet W can be heated to a temperature of 50 ° C to 300 ° C.
  • the air permeability measuring device 40 a general air permeation measuring device can be used.
  • the electric field radiating device 20 includes a case 100, a nozzle block 110, a collector 150, a power supply device 160, an auxiliary belt device 170, and raw materials.
  • Tank 200, second conveying device 210, second conveying control device 220, intermediate tank 230, supply device 240, feed control device 242, first conveying An apparatus 250, a first transfer control device 260, and regeneration tanks 270, 272 are provided.
  • the case 100 is made of a conductor.
  • the nozzle block 110 includes a plurality of upward nozzles 126, a polymer solution supply path 114, a polymer solution recovery path 120, and a second sensor 142.
  • nozzle blocks having various sizes and various shapes can be used.
  • the nozzle block 110 has, for example, a rectangle of 0.5m to 3m (including square) when viewed from an upper surface thereof. Has the size and shape shown.
  • each upward nozzle 126 is the nozzle base part 130 which is the base end of the upward nozzle 126, the nozzle intermediate part 128 which is the intermediate part of the upward nozzle 126, and the upward nozzle ( It consists of the nozzle tip 132 which is the tip of 126.
  • the upward nozzle 126 and the polymer solution supply path side threaded part 118 are connected to the base end side (base end side of the nozzle base end 130) of the upward nozzle 126. It has a corresponding upward nozzle side threaded portion.
  • the interior of the upward nozzle 126 consists of a cave, which is in communication with the cave in the polymer solution supply path 114.
  • the upward nozzle 126 discharges a polymer solution upward from a discharge port.
  • the upward nozzle 126 is made of a conductor, for example, copper, stainless steel, aluminum, or the like.
  • the plurality of upward nozzles 126 are arranged at a pitch of, for example, 1.5 cm to 6.0 cm.
  • the number of the plurality of upward nozzles 126 is, for example, 36 pieces (6 * 6 pieces when arranged in the same number in the vertical direction) to 21904 pieces (148 pieces * 148 pieces in the case where they are arranged in the portrait).
  • the nozzle tip part 132 is formed in the shape which cut
  • the angle ⁇ formed between the axis of the cylinder and the plane is 50 degrees.
  • An inclined surface portion 133 is formed on the tip side of the nozzle tip portion 132, and the tip of the inclined surface portion 133 is located above the tip of the jacket 134.
  • the distance d1 along the axis of the cylinder between the tip of the inclined surface portion 133 and the tip of the jacket 134 is 0.5 mm.
  • the base end of the inclined surface portion 133 is located below the tip of the jacket 134.
  • the distance d2 along the axis of the cylinder between the base end of the inclined surface portion 133 and the tip end of the jacket 134 is 0.5 mm.
  • the area of the area surrounded by the inner circumference of the jacket 134 is S1.
  • the nozzle intermediate part 128 is formed in a substantially cylindrical shape.
  • the nozzle base end 130 is formed in a hexagonal cylindrical shape as shown in Fig. 4C.
  • the polymer solution supply path 114 has a substantially rectangular parallelepiped shape, has a cave therein, and a plurality of upward nozzles 126 through which the polymer solution from the supply device 240 flows. Supplies).
  • the polymer solution supply path 114 has the connection part 116 with a supply apparatus, and is connected with the supply apparatus 240 at the connection part 116 with this supply apparatus.
  • the polymer solution supply path 114 further has a polymer solution supply path side threaded portion 118.
  • the polymer solution supply path 114 and the upward nozzle 126 are coupled by fitting the polymer solution supply path side threaded portion 118 and the upward nozzle side threaded portion.
  • the polymer solution recovery path 120 is formed from the accommodation portion 121, the groove portion 124, the lid portion 123, and the plurality of jackets 134.
  • the polymer solution recovery path 120 recovers the polymer solution that has overflowed from the discharge ports of the plurality of upward nozzles 126.
  • the accommodating part 121 receives the polymer solution which overflowed from the discharge port of the some upward nozzle 126.
  • the accommodation part 121 is disposed above the polymer solution supply path 114.
  • a slight inclination is formed in the accommodating part 121 toward the groove part 124, and has a function which guides the received polymer solution toward the groove part 124. As shown in FIG.
  • the groove part 124 is arrange
  • the groove part 124 has the connection part 125 with the 1st conveying apparatus in the bottom face, and is connected with the 1st conveying apparatus 250 in the connection part 125 with this 1st conveying apparatus.
  • the cover part 123 covers the accommodating part 121, and has a some nozzle hole through each upward nozzle 126. Moreover, the cover part 123 has the cover part side screw part 122 around the hole for nozzles.
  • the jacket 134 covers the side surface of each upward nozzle 126 which protrudes from the some hole for nozzles.
  • the jacket 134 has a jacket base end 138 on the proximal side of the jacket 134 and a jacket tip 140 on the proximal side of the jacket 134.
  • the jacket tip 140 is thinner than the jacket tip 138.
  • the jacket tip 138 has a cylindrical shape with a constant thickness, and the jacket tip 140 is corresponding. From the connection part 136 of the jacket tip part 140 and the jacket base part 138 to the tip part, it has a cylindrical shape which decreases thickness gradually, specifically at a fixed ratio (refer FIG. 4 (a) and FIG. 4 (d)). .).
  • the jacket 134 has the jacket side screw part corresponding to the cover part side threaded part 122 on the base end side of the jacket base end part 138. As shown in FIG.
  • the cover part 123 and the jacket 134 are couple
  • the second sensor 142 measures the liquid level of the polymer solution in the polymer solution recovery path 120. Specifically, the second sensor 142 is disposed on the wall surface of the groove portion 124 and measures the liquid level of the polymer solution collected in the groove portion 124.
  • the second sensor 124 is made of, for example, an optical fiber sensor.
  • the collector 150 is disposed above the nozzle block 110.
  • the collector 150 is made of a conductor, and is attached to the case 100 via the insulating member 152 as shown in FIG. 2.
  • the field emission device 20 electrospins the nanofibers which discharge the polymer solution from the discharge ports of the plurality of upward nozzles 126 while overflowing the polymer solution from the discharge ports of the plurality of upward nozzles 126.
  • the power supply device 160 applies a high voltage between the plurality of upward nozzles 126 and the collector 150.
  • the positive electrode of the power supply device 160 is connected to the collector 150, and the negative electrode of the power supply device 160 is connected to the nozzle block 110 through the case 100.
  • the auxiliary belt device 170 includes an auxiliary belt 172 that rotates in synchronization with the feeding speed of the long sheet W, and five rollers 174 for assisting the auxiliary belt 172.
  • One or two or more auxiliary belt rollers of the five auxiliary belt rollers 174 are driving rollers, and the remaining auxiliary belt rollers are driven rollers. Since the auxiliary belt 172 is disposed between the collector 150 and the long sheet W, the long sheet W is smoothly conveyed without being pulled by the collector 150 to which a positive high voltage is applied. do.
  • the raw material tank 200 stores the polymer solution used as a raw material of a nanofiber.
  • the raw material tank 200 has an agitator 201 for preventing separation or solidification of the polymer solution therein.
  • the pipe 212 of the second transfer device 210 is connected to the raw material tank 200.
  • the second transfer device 210 transfers the polymer solution from the raw material tank 200 or the regeneration tanks 270 and 272 to the intermediate tank 230.
  • the second transfer device 210 includes a pipe 212 connecting the raw material tank 200 and the intermediate tank 230, and a pipe 214 connecting the regeneration tanks 270, 272 and the intermediate tank 230.
  • Have The end of the pipe 212 is connected to the first storage unit 236 (described later), and the end of the pipe 214 is connected to the pipe 212.
  • the second transfer control device 220 controls the transfer operation of the second transfer device 210.
  • the second transfer control device 220 has valves 222, 224, 226, and 228.
  • the valve 222 controls the transfer of the polymer solution from the raw material tank 200.
  • the valve 224 controls the amount of polymer solution flowing into the intermediate tank 230 from the raw material tank 200 and the regeneration tanks 270 and 272. Control by the valve 224 is performed according to the liquid level measured by the 1st sensor 239 mentioned later.
  • the valve 226 controls the transfer of the polymer solution from the regeneration tank 270.
  • the valve 228 controls the transfer of the polymer solution from the regeneration tank 272.
  • the second transfer control device 220 uses the valves 222, 224, 226, and 228 to transfer the polymer solution from the tank of any one of the raw material tank 200 and the regeneration tanks 270, 272 to the intermediate tank. It controls whether to transfer to 230. Moreover, the 2nd conveyance control apparatus 220 controls the conveyance operation
  • the intermediate tank 230 stores the polymer solution supplied from the raw material tank 200 or the regeneration tanks 270 and 272.
  • the intermediate tank 230 is disposed such that the lower end of the intermediate tank 230 is located above the upper end of each upward nozzle 126.
  • the intermediate tank 230 has a partition 232, a bubble removing filter 234, and a first sensor 239.
  • the partition 232 covers the supply site to which the polymer solution is supplied.
  • the bubble removing filter 234 is disposed at the bottom of the partition wall 232 and removes bubbles from the polymer solution passing therethrough.
  • the bubble removing filter 234 has a mesh structure having an eye of about 0.1 mm, for example.
  • the partition 232 and the bubble removing filter 234 are configured to store the polymer solution after bubbles are removed by the removal filter 234.
  • the second storage part 238 is connected to the polymer solution supply path 114 by the supply path 240. As a result, in the nanofiber manufacturing apparatus 1, the second storage part 238 is connected to the second storage part 238.
  • the stored polymer solution is supplied to the polymer solution supply path 114 of the nozzle block 110.
  • the first sensor 239 measures the liquid level of the polymer solution in the second storage unit 238.
  • the first sensor is made of, for example, an optical fiber sensor.
  • the supply device 240 is composed of one pipe and supplies the polymer solution stored in the second reservoir 238 of the intermediate tank 230 to the polymer solution supply path 114 of the nozzle block 110.
  • the supply apparatus may be at least one with respect to one nozzle block.
  • the supply control apparatus 242 consists of one valve provided in the supply apparatus 240, and controls the supply operation
  • the first transfer device 250 has a pipe 252 and a pump 254, and transfers the polymer solution from the polymer solution recovery path 120 of the nozzle block 110 to the regeneration tanks 270 and 272.
  • the pump 254 generates power for transferring the polymer solution to the regeneration tanks 270 and 272 located above the vicinity of the nozzle block 110.
  • the pump 254 consists of an air diaphragm pump, for example.
  • the first transfer control device 260 controls the transfer operation of the first transfer device 250.
  • the first transfer control device 260 includes valves 264 and 266 and a control device (not shown) of the pump 254.
  • the valve 264 controls the transfer operation of the polymer solution from the polymer solution recovery path to the regeneration tank 270.
  • the valve 266 controls the transfer operation of the polymer solution from the polymer solution recovery path to the regeneration tank 272.
  • the first transfer control device 260 controls whether the polymer solution is transferred to any one of the plurality of regeneration tanks 270 and 272 by the valves 264 and 266.
  • the 1st conveyance control apparatus 260 carries out 1st conveyance according to the liquid level of the polymer solution measured by the 2nd sensor 142 by the control apparatus of the said valve 264, 266 and the pump 254. Control the transfer operation of the device 250.
  • the plurality of regeneration tanks 270 and 272 are regeneration tanks for regenerating the recovered polymer solution and store the regenerated polymer solution.
  • the regeneration tanks 270 and 272 have agitators 271 and 273 therein for preventing separation or solidification of the polymer solution, respectively.
  • the nanofiber manufacturing apparatus 1 includes a nanofiber manufacturing apparatus which makes it possible to recover a polymer solution that has overflowed from the discharge ports of a plurality of upward nozzles and reuse it as a raw material of the nanofibers. do.
  • the nanofiber manufacturing method electro-spins the nanofibers which discharge the polymer solution from the discharge holes of the plurality of upward nozzles 126 while overflowing the polymer solution from the discharge holes of the plurality of upward nozzles 126. It is a nanofiber manufacturing method which makes it possible to collect the polymer solution which overflowed from the discharge opening of the upward nozzle 126 of the, and to reuse it as a raw material of a nanofiber.
  • the polymer solution is transferred from the raw material tank 200 to the intermediate tank 230 using the pipe 212 of the second transfer device 210.
  • the polymer solution which is moved from the first reservoir 232 to the second reservoir 234 through the bubble removing filter 234 in the intermediate tank 230, is supplied through the supply device 240 to the polymer solution.
  • the nanofiber manufacturing apparatus 1 discharges the polymer solution from the discharge ports of the plurality of upward nozzles 126 while overflowing the polymer solution from the discharge ports of the plurality of upward nozzles 126 supplied to the polymer solution supply path 114. Electrospinning the nanofibers.
  • the nanofiber manufacturing apparatus 1 recovers the overflowed polymer solution in the polymer solution recovery path 120.
  • the polymer solution transfers and recovers the regeneration tank 270 using the first transfer device 250 at a portion of the groove portion 124 of the polymer solution recovery path 120.
  • the transfer destination by the first transfer device 250 is switched to the regeneration tank 272 by the first transfer control device 260.
  • the overflowed polymer solution is recovered to the regeneration tank 272, and the polymer solution overflowed into the regeneration tank 270 enters the regeneration tank 270 when the subsequent step is performed in the regeneration tank 270. none.
  • the content rate of the solvent and the additive in the recovered polymer solution is measured.
  • This measurement can be performed by extracting a part of the polymer solution in the regeneration tank 270 as a sample and analyzing the sample. Analysis of a polymer solution can be performed by a conventional method.
  • the required amount of solvent, additives and other components are added to the polymer solution.
  • the recovered polymer solution is regenerated.
  • the polymer solution in the regeneration tank 270 is transferred to the intermediate tank 230 using the pipe 212 of the second transfer device 210.
  • the polymer solution in the regeneration tank 270 is nanofibers. It can be reused as a raw material of.
  • the polymer solution in the regeneration tank 272 is removed by the same method as that after the predetermined amount of the polymer solution is collected in the regeneration tank 270. It can be reused as a raw material of nanofibers.
  • a nonwoven fabric, a woven fabric, a knitted fabric, a film or the like made of various materials can be used.
  • the thickness of a long sheet the thing of 5 micrometers-500 micrometers can be used, for example.
  • the length of a long sheet the thing of 10 m-10 km can be used, for example.
  • polylactic acid polypropylene
  • PVAc polyvinyl acetate
  • PET polyethylene terephthalate
  • PBT polybutylene terephthalate
  • PEN polyethylene naphtha Rate
  • PA Polyamide
  • PUR Polyurethane
  • PVA Polyvinyl Alcohol
  • PAN Polyacrylonitrile
  • PAN Polyetherimide
  • PCL Polycaprolactone
  • PLGA Polylactic acid glycol Acids
  • silk cellulose, chitosan and the like
  • the solvent used for the polymer solution for example, dichloromethane, dimethyl formamide, dimethyl sulfoxide, methyl ethyl ketone, chloroform, acetone, water, formic acid, acetic acid, cyclohexane, THF and the like can be used. You may mix and use multiple types of solvent.
  • the polymer solution may contain additives such as conductivity improvers.
  • Air permeability of the nanofiber nonwoven fabric produced can be set to 0.15cm 3 / cm 2 / s ⁇ 200cm 3 / cm 2 / s.
  • the feed speed can be set to, for example, 0.2 m / min to 100 m / min.
  • the voltage applied to the nozzle block 110 and the collector 150 can be set to 10 kV-80 kV, and it is preferable to set it near 50 kV.
  • the temperature of the spinning zone can be set to 25 ° C, for example.
  • the humidity of the radiation zone can be set to 30%, for example.
  • the nanofiber manufacturing apparatus 1 As in the case of the conventional nanofiber manufacturing apparatus, since the polymer solution is discharged by discharging the polymer solution from the discharge ports of the plurality of upward nozzles 126, conventional nanofibers are discharged.
  • the droplet phenomenon seen in the case of the nanofiber manufacturing apparatus using the downward nozzle does not occur, and it becomes possible to manufacture high quality nanofibers.
  • the field of the nanofibers is electrospun while overflowing the polymer solution from the discharge ports of the plurality of upward nozzles 126.
  • a sufficient amount of polymer solution is always supplied to the upward nozzle, making it possible to produce nanofibers of uniform quality.
  • the nanofiber manufacturing apparatus 1 as in the case of the conventional nanofiber manufacturing apparatus, the polymer solution overflowed from the discharge ports of the plurality of upward nozzles 126 is recovered and used as a raw material of the nanofibers. Since it is possible to reuse, it becomes possible to reduce the fee for use of a raw material, and as a result, it becomes possible to manufacture nanofibers at inexpensive manufacturing cost. This also follows the flow of resource saving.
  • the nozzle tip part 132 since the nozzle tip part 132 has the shape which cut
  • the nanofiber manufacturing apparatus 1 According to the nanofiber manufacturing apparatus 1 according to the embodiment, even when electrospinning while overflowing the polymer solution from the discharge port of the upward nozzle 134, the polymer solids adhere to the nanofibers to improve the quality of the nanofibers. It becomes possible to solve the problem of making it fall.
  • the angle formed between the axis of the cylinder and the plane is in the range of 15 ° to 60 °, the polymer overflows from the discharge port of the upward nozzle 126.
  • the solution flows down more quickly without remaining in the portion of the nozzle tip 132, and the length of the inclined surface of the upward nozzle 126 becomes too long so that the field emission condition is not disturbed.
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, by the function of the jacket 134 which covers the side surface of the upward nozzle 126, a solvent is prevented from the polymer solution which overflows from the discharge port of the upward nozzle 126. It is possible to further reduce the amount of volatilization.
  • the jacket tip 140 is thinner than the jacket proximal end 138, the solvent volatilizes from the polymer solution overflowing from the discharge port of the upward nozzle 126. It is possible to further reduce the amount.
  • the jacket base end 138 has a cylindrical shape with a constant thickness
  • the jacket tip end 140 has the jacket tip end 140 and the jacket base end ( Since it has a cylindrical shape in which the thickness gradually decreases from the connection portion 136 with the tip 136, the amount of solvent volatilized from the polymer solution can be reduced by using the jacket 134 having a simple shape.
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, since the front end of the inclined surface part 133 formed in the front end side of the nozzle front end part 132 is located above the front end of the jacket 134, an upward nozzle Since the electric field formed between 126 and the collector 150 is stabilized, it becomes possible to manufacture nanofibers with uniform quality.
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, since the space
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, since the base end of the inclined surface part 133 formed in the front end side of the nozzle front end part 132 is located below the front end of the jacket 134, an upward nozzle It is possible to further reduce the amount of solvent volatilization from the polymer solution overflowing from the discharge port of 126.
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, since the space
  • the solvent is prevented from the polymer solution overflowing from the discharge port of the upward nozzle 126.
  • the amount of volatilization can be further reduced, and the polymer solution which overflows from the discharge port of the upward nozzle 126 is eliminated from sinking into the gap between the upward nozzle 126 and the jacket 134.
  • the jacket 134 since the cover part 123 and the jacket 134 are couple
  • the polymer solution supply path 114 and the upward nozzle 126 are coupled by the fitting of the polymer solution supply path side threaded portion 118 and the upward nozzle side threaded portion.
  • the attachment / detachment of the upward nozzle 126 becomes easy, and it becomes a nanofiber manufacturing apparatus which is easy to manufacture and maintain.
  • the proximal end (nozzle proximal end 130) of the upward nozzle 126 is formed in a hexagonal tubular shape, the upward nozzle (using a tool such as a wrench) 126) can be easily attached and detached, and a nanofiber manufacturing apparatus is more easily manufactured and maintained.
  • the composition of and simultaneously adding the solvent and other necessary components to the polymer solution according to the result of the measurement it is possible to regenerate the polymer solution into a polymer solution having a composition very close to or equal to that of the original polymer solution.
  • the spinning conditions in an electric field spinning process (in this case, a composition of a polymer solution) are collect
  • recovered making it possible to collect the overflowed polymer solution and to reuse it as a raw material of a nanofiber.
  • the nanofiber manufacturing apparatus 1 which concerns on an Example, it is further provided with the conveying apparatus 10 which conveys the elongate sheet W, and is provided with the nozzle block 110 and the collector 150 at least.
  • the field spinning device for depositing nanofibers on the surface of the long sheet W the field spinning device 20 includes a plurality of field spinning devices 20 arranged in series along the feeding direction of the long sheet W, Higher productivity makes it possible to mass-produce. It is also possible to mass-produce products in which nanofibers are thickly deposited, products in which various kinds of nanofibers are deposited, and the like.
  • the polymer solution is discharged from the discharge holes of the plurality of upward nozzles 126 while overflowing the polymer solution from the discharge holes of the plurality of upward nozzles 126, thereby causing the electric field of the nanofibers.
  • the polymer solution which overflowed from the discharge port of the some upward nozzle 126 was collect
  • the collected polymer solution is transferred to the regeneration tanks 270 and 272, and then the composition of the polymer solution is measured, and the polymer solution is added to the polymer solution according to the measurement result. Played.
  • Table 1 is a table
  • Table 2 is a table which shows the composition of the recovered polymer solution.
  • Table 3 is a table which shows the composition of the recycled polymer solution.
  • "relative weight” in Tables 1-3 has shown the relative weight of each substance at the time of making the weight of polyurethane into 100.
  • the polymer solution could be regenerated into a polymer solution having a composition that was the same as or very close to that of the original polymer solution.
  • the polymer solution was regenerated by adding 40.8 g of dimethyl formamide and 74.6 g of methyl ethyl ketone per 100 g of polyurethane to the recovered polymer solution.
  • the nanofiber production apparatus of the present invention has been described using the nanofiber production apparatus 1 having an angle of 50 ° between the axis and the plane of the cylinder as an example, but the present invention is limited thereto. It is not.
  • the present invention can be applied to a nanofiber production apparatus having an angle between a cylinder axis and a plane in the range of 15 ° to 60 °.
  • the nanofiber production apparatus of the present invention will be described with an example of the nanofiber production apparatus 1 having an interval d1 of 0.5 mm along the axis of the cylinder between the tip of the inclined surface portion and the tip of the jacket.
  • the present invention is not limited to this.
  • the present invention can be applied to a nanofiber production apparatus in which a distance d1 along the axis of the cylinder between the tip of the inclined surface portion and the tip of the jacket is in the range of 0.1 mm to 2.0 mm.
  • the nanofiber production apparatus of the present invention has been described with the example of the nanofiber production apparatus 1 in which the base end of the inclined surface portion formed on the tip side of the nozzle tip portion is located below the tip of the jacket.
  • the invention is not limited to this.
  • the present invention can be applied to a nanofiber manufacturing apparatus in which the base end of the inclined surface portion formed on the tip side of the nozzle tip portion is located at the same height as the tip of the jacket or above the tip of the jacket.
  • the nanofiber production apparatus of the present invention has been described with the example of the nanofiber production apparatus 1 having a distance d2 of 0.5 mm along the axis of the cylinder between the base end of the inclined surface portion and the tip of the jacket.
  • the present invention is not limited to this.
  • the present invention can be applied to a nanofiber production apparatus in which the distance d2 along the axis of the cylinder between the base end of the inclined surface portion and the tip of the jacket is in the range of 0.1 mm to 1.0 mm.
  • the nanofiber production apparatus of the present invention has been described by using the nanofiber production apparatus 1 having two field emission apparatuses 20 as field emission apparatuses, but the present invention is based on this. It is not limited.
  • the present invention may be applied to a nanofiber production apparatus having one, three or more field emission devices.
  • the nanoparticles of the present invention are made using an electrospinning device in which the positive electrode of the power supply device 160 is connected to the collector 150 and the negative electrode of the power supply device 160 is connected to the nozzle block 110.
  • the fiber manufacturing apparatus was demonstrated, this invention is not limited to this.
  • the present invention can also be applied to a nanofiber production apparatus comprising an electric field radiating device in which a positive electrode of a power supply device is connected to a nozzle block, and a negative electrode of the power supply device is connected to a collector.
  • the raw material tank 200 the regeneration tanks 270 and 272, the intermediate tank 230, the first transfer device 250, the first transfer control device 260,
  • the nanofiber manufacturing apparatus of this invention was demonstrated using the nanofiber manufacturing apparatus 1 provided with the 2nd conveying apparatus 210 and the 2nd conveyance control apparatus 220 as an example, this invention is not limited to this. .
  • the present invention may be applied to other nanofiber manufacturing apparatus.
  • the present invention has been described using a nanofiber production apparatus in which one nozzle block is disposed in one field radiating device, but the present invention is not limited thereto.
  • the present invention can be applied to a nanofiber production apparatus in which two nozzle blocks are disposed in one field radiator, and the present invention can be applied to a nanofiber production apparatus in which two or more nozzle blocks are disposed.
  • the nozzle arrangement pitch may be the same for all nozzle blocks, or the nozzle arrangement pitch may be different for each nozzle block.
  • the height position of the nozzle block may be the same for all the nozzle blocks, or the height position of the nozzle block may be different for each nozzle block.
  • a mechanism for reciprocating the nozzle block at a predetermined reciprocating cycle along the width direction of the elongate sheet may be provided.
  • the mechanism electric field spinning is performed while the nozzle block is reciprocated at a predetermined reciprocating cycle, so that the amount of polymer fibers deposited along the width direction of the long city can be made uniform.
  • the reciprocating cycle and the reciprocating distance of the nozzle block may be controlled independently for each field radiating device or for each nozzle block. With such a configuration, it is possible to reciprocate all the nozzle blocks at the same period, and it is also possible to reciprocate each nozzle block at different periods. In addition, it is possible to equalize the reciprocating distance of the reciprocating motion with all the nozzle blocks, and it is also possible to vary the reciprocating distance of the reciprocating motion with each nozzle block.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

L'invention concerne un dispositif de fabrication de nanofibres capable de résoudre le problème de la réduction de la qualité des nanofibres, même lorsqu'une émission de champ est appliquée à une solution de polymère tout en amenant celle-ci en excès par une sortie d'éjection d'une buse ascendante, en accrochant des polymères solides aux nanofibres. Le dispositif de fabrication de nanofibres comporte : une pluralité de buses ascendantes (126), un porte-buses (110) doté d'un conduit (114) d'alimentation en solution de polymère et d'un conduit (120) de récupération de solution de polymère, un collecteur (150) et un dispositif de puissance, et permet l'émission par effet de champ de nanofibres en éjectant la solution de polymère par la sortie d'éjection de la pluralité de buses ascendantes (126) tout en amenant la solution de polymère en excès, ainsi que la récupération de la solution de polymère en excès en vue de sa réutilisation comme matière première pour des nanofibres en même temps, et une partie avant (132) des buses présente la forme d'un cylindre ayant été coupé suivant le plan qui croise obliquement l'axe du cylindre en question.
PCT/KR2011/003058 2010-12-06 2011-04-27 Dispositif de fabrication de nanofibres WO2012077867A1 (fr)

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JP2010-272073 2010-12-06
JP2010272073A JP5698508B2 (ja) 2010-12-06 2010-12-06 ナノ繊維製造装置
KR1020110016679A KR101040057B1 (ko) 2010-12-06 2011-02-24 나노섬유 제조장치
KR10-2011-0016679 2011-02-24

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CN103757719A (zh) * 2014-02-12 2014-04-30 厦门大学 一种纤维毡制备装置

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KR101382571B1 (ko) 2013-04-17 2014-04-17 (주)에프티이앤이 나노섬유 제조용 전기방사장치
CN103290492B (zh) * 2013-05-31 2015-10-28 华中科技大学 一种微径丝或管的制备方法及装置
CN104928767B (zh) * 2014-03-21 2017-06-06 馨世工程教育有限公司 一种静电离心式多功能纺丝设备
KR101688817B1 (ko) * 2014-12-31 2016-12-22 주식회사 에이앤에프 전기방사 방식 패턴 형성 장치
JP6543199B2 (ja) * 2016-01-15 2019-07-10 株式会社リメディオ ノズル、乾式紡糸装置、ノズルセット、及び、ノズル取付方法
CN111441092A (zh) * 2020-05-15 2020-07-24 西安工程大学 一种静电纺丝喷头及具有其的静电纺丝系统及其工作方法

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