JP2009275339A - Fiber-producing apparatus and method for producing fiber - Google Patents

Fiber-producing apparatus and method for producing fiber Download PDF

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Publication number
JP2009275339A
JP2009275339A JP2009098052A JP2009098052A JP2009275339A JP 2009275339 A JP2009275339 A JP 2009275339A JP 2009098052 A JP2009098052 A JP 2009098052A JP 2009098052 A JP2009098052 A JP 2009098052A JP 2009275339 A JP2009275339 A JP 2009275339A
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Japan
Prior art keywords
melt
fiber
nozzle
gas
discharge nozzle
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JP2009098052A
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Japanese (ja)
Inventor
Kunio Miyazawa
Katsuhiro Nagayama
Toshiyuki Nakano
恵之 中野
邦夫 宮澤
勝博 長山
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Hyogo Prefecture
Jfe Chemical Corp
Jfeケミカル株式会社
兵庫県
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Priority to JP2008108721 priority Critical
Application filed by Hyogo Prefecture, Jfe Chemical Corp, Jfeケミカル株式会社, 兵庫県 filed Critical Hyogo Prefecture
Priority to JP2009098052A priority patent/JP2009275339A/en
Publication of JP2009275339A publication Critical patent/JP2009275339A/en
Application status is Pending legal-status Critical

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/06Feeding liquid to the spinning head
    • D01D1/09Control of pressure, temperature or feeding rate
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/0023Electro-spinning characterised by the initial state of the material the material being a polymer melt

Abstract

A fiber manufacturing apparatus and a fiber manufacturing method capable of stably manufacturing a fiber having a smaller fiber diameter by an electrospinning method.
A first nozzle portion that discharges a melt into a fine thread when a fiber is produced by electrospinning by discharging a melt of a polymer material or a pitch-based material into a fine thread from a melt discharge nozzle. A melt discharge nozzle 5 having a first nozzle unit 51 and a second nozzle unit 52 that discharges the melt discharged from the first nozzle unit 51 into a fine thread while pressurizing with a gas is used.
[Selection] Figure 2

Description

  The present invention relates to a fiber manufacturing apparatus and manufacturing method using an electrospinning method (electrostatic spinning method).

In recent years, it is expected to be applied to electronics fields such as electric guns for electric wires and light emitters on semiconductor substrates, various sensors, environment-friendly fields such as high-performance filters, medical fields such as scaffolds for regenerative medicine, wound protection materials, etc. Thus, there is an increasing demand for ultrafine fibers having a diameter of sub-micrometer or less.
As a method for producing such ultrafine fibers, there is a method of removing sea components from sea-island composite spinning or polymer blends by dissolving them with a suitable solvent and taking out the island components as sub-micrometer order fibers. Since a solvent that can be dissolved has to be used, there is a drawback in that the type of polymer is limited and the versatility is poor. Therefore, the importance of the electrospinning method has been reconsidered as a method for spinning ultrafine fibers having a fiber diameter of sub-micrometer or less without using a composite spinning method or a blend spinning method, and has attracted attention.

As a spinning method of ultrafine fibers using an electrospinning method, a spinning raw material pitch composed of an optically isotropic pitch and / or an optically anisotropic pitch is used under a temperature condition where the viscosity of the spinning raw material pitch is 10 poises or less. And a gas preheated to a temperature lower by 50 ° C. or higher than the temperature at which the viscosity of the spinning raw material pitch becomes 10 poises or less, and the discharge direction of the spinning raw material pitch from the periphery of the spinning nozzle. A method is known in which a spinning raw material pitch is spun into ultrafine carbon fibers by flowing out in the same direction and parallel to the discharged fibers (see Patent Document 1).
In addition, as another technique for spinning ultrafine fibers, a technique in which a polymer substance is dissolved in a solvent to form a solution, and compressed air is ejected while discharging from a spinning nozzle to which a high voltage is applied to form ultrafine fibers. Is also known (see Patent Document 2).

Japanese Patent No. 2680183 Japanese Patent No. 4047286

However, the method disclosed in Patent Document 1 has a problem that although a carbon fiber having a fiber diameter of 1.1 to 1.2 μm is obtained, an ultrafine fiber having a fiber diameter of sub-micrometer or less cannot be obtained. On the other hand, in the technique disclosed in Patent Document 2, since the polymer material solution is spun, it is not necessary to spin the polymer material, which is a spinning raw material, by special heating. For this reason, although the spinneret is easy to insulate, there is a problem that a high-molecular material or a pitch-based material that is not completely soluble in a solvent cannot be spun. That is, since a portion to which a high voltage is applied (usually a metal having conductivity) or a portion through which a solution is passed does not reach a high temperature, plastic, ceramic, or the like can be used as an insulating material. Although ceramics can withstand high temperatures, the coefficient of thermal expansion differs from that of metal, so that bonding is difficult and dielectric breakdown may occur. In addition, the liquid crystalline polymer / pitch-based material cannot be spun in a liquid crystal state, and has a problem that properties such as high elasticity and high thermal conductivity are not exhibited because it is solution spinning.
The present invention has been made by paying attention to the above-mentioned problems, and its purpose is to produce fibers that can stably produce fibers that are finer in fiber diameter and are expected to exhibit characteristics by electrospinning. It is to provide an apparatus and a fiber manufacturing method.

  In order to solve the above-mentioned problem, a fiber manufacturing apparatus according to the invention described in claim 1 is a fiber manufacturing apparatus used when a fiber is manufactured from a melt of a polymer material or a pitch-based material by an electrospinning method. A storage container for storing the melt, a melt discharge nozzle for discharging the melt stored in the storage container in a thin thread shape, a collector disposed opposite to the melt discharge nozzle, and the melt And a melt charging means for charging the melt by applying a voltage between the discharge nozzle and the collector, and the melt discharge nozzle is narrowed from the first nozzle portion and the first nozzle portion. And a second nozzle portion that discharges the melt discharged in the form of a thread into a fine thread while pressurizing the melt with a gas.

A fiber manufacturing apparatus according to a second aspect of the present invention is the fiber manufacturing apparatus according to the first aspect, wherein the gas is an inert gas, and the lower limit temperature of the gas is the melting point or softening point of the melt −50 ° C. And a gas temperature adjusting means for adjusting the upper limit temperature to the melting point or softening point of the melt + 130 ° C.
A fiber manufacturing apparatus according to a third aspect of the present invention is the fiber manufacturing apparatus according to the first or second aspect, further comprising electromagnetic induction heating means for heating the melt.

  According to a fourth aspect of the present invention, there is provided a fiber manufacturing method in which a fiber is produced from a melt of a polymer material or a pitch-based material by an electrospinning method. A melt discharge nozzle that discharges the molten material into a thin thread shape, a collector that is disposed to face the melt discharge nozzle, and a voltage that is applied between the melt discharge nozzle and the collector, A melt charging means for charging the melt discharged from the discharge nozzle, wherein the melt discharge nozzle gasses the melt discharged from the first nozzle portion in the form of a fine thread. A fiber is manufactured using a fiber manufacturing apparatus having a second nozzle portion that discharges in a fine thread shape while being pressurized by the above.

The fiber manufacturing method according to the invention described in claim 5 is the fiber manufacturing method according to claim 4, wherein the gas is an inert gas, and the minimum temperature of the gas is the melting point or softening point of the melt of -50 ° C. The upper limit temperature is the melting point or softening point of the melt + 130 ° C.
A fiber manufacturing method according to a sixth aspect of the present invention is the fiber manufacturing method according to the fourth or fifth aspect, wherein the melt is heated by electromagnetic induction heating means.
The fiber manufacturing method according to the invention described in claim 7 is the fiber manufacturing method according to any one of claims 4 to 6, wherein the fibers collected by the collector are infusibilized, carbonized, or carbonized. And graphitizing.

  According to the first, third, fourth, and sixth aspects of the invention, the melt discharged from the first nozzle portion in the form of a fine thread is discharged from the second nozzle portion in the form of a fine thread while being pressurized by the gas. Thereby, since the diameter of the melt discharged in the form of a fine thread from the melt discharge nozzle toward the collector becomes thinner, fibers with a smaller fiber diameter can be stably manufactured by the electrospinning method. As a result, hydrogen storage materials from the production of carbon nanofibers, electrode materials for capacitors and fuel cells, solar cell electrode materials, scaffolds for regenerative medicine using biodegradable polymer nanofibers, various high-performance filters and battery separators, etc. It can be used for specific application fields.

According to invention of Claim 2 and 5, by using inert gas as a gas which pressurizes the melt discharged from a 2nd nozzle part in a thin thread form, rapid oxidation, explosion, etc. of a fiber are prevented. be able to.
According to the seventh aspect of the present invention, a carbon fiber having a smaller fiber diameter can be stably produced by the electrospinning method.

It is a figure which shows one Embodiment of the fiber manufacturing apparatus which concerns on this invention. It is a figure which shows one Example of a melt discharge nozzle. FIG. 3 is a diagram showing the fiber diameter of pitch-based fibers obtained in Example 1. FIG. 3 is a view showing the fiber diameter of pitch-based fibers obtained in Comparative Example 1. 5 is a diagram showing the fiber diameter of pitch-based fibers obtained in Comparative Example 2. FIG.

Hereinafter, the fiber manufacturing apparatus and the fiber manufacturing method according to the present invention will be described with reference to FIGS.
FIG. 1 is a diagram showing a schematic configuration of a fiber manufacturing apparatus according to one embodiment of the present invention, and FIG. 2 is a diagram showing a main part of the fiber manufacturing apparatus according to one embodiment of the present invention, as shown in FIG. The fiber manufacturing apparatus according to an embodiment of the present invention includes a storage container 2 that stores the polymer material or the pitch-based material melt 1.
The storage container 2 is made of, for example, stainless steel, and an electric heater 3 is wound around the outer peripheral surface of the storage container 2 in order to keep the melt 1 stored in the storage container 2 in a molten state. .

When the storage container 2 is heated by electromagnetic induction, it is preferable that the storage container 2 is formed of iron or stainless steel in that the heating effect by electromagnetic induction is reduced unless the metal has a certain large electrical resistance, such as aluminum or copper. Is not suitable as a metal for induction heating because of its low electrical resistance. In this case, in order to keep the melt 1 stored in the storage container 2 in a molten state, for example, a coil is wound in a non-contact manner as electromagnetic induction heating means on the outside of the storage container 2.
Further, the storage container 2 has a sealed structure, and for example, nitrogen gas pressurized to about 0.3 to 0.7 MPa is supplied from the nitrogen gas supply line 4 to the storage container 2. Yes. The melt 1 is melted in a container different from the storage container 2 and then supplied into the storage container 2 by a gear pump or the like.

The melt 1 stored in the storage container 2 is discharged in the form of a fine thread from the melt discharge nozzle 5. The melt discharge nozzle 5 is provided at the lower end of the storage container 2 in the figure, and the melt 1 discharged from the melt discharge nozzle 5 is captured as a fiber on the right side of the melt discharge nozzle 5 in the figure. A flat plate-shaped collector 6 is arranged.
As shown in FIG. 2, the melt discharge nozzle 5 has a first nozzle portion 51 that discharges the melt 1 stored in the storage container 2 in the form of a fine thread, and the first nozzle portion 51. Is provided with a second nozzle portion 52 for discharging the melt 1 discharged from the first nozzle portion 51 into a fine thread shape while being pressurized with a pressurized gas such as nitrogen gas.

The second nozzle portion 52 includes a cylindrical barrel 52a formed on the outer periphery of the first nozzle portion 51, and a nozzle guide 52b that forms a nozzle port 53 of about 0.5 mm on the tip side of the barrel 52a. The barrel 52a is provided with a pressurized gas supply port 54 for supplying a pressurized gas such as nitrogen gas into the second nozzle portion 52.
The barrel 52a is formed of a material having good thermal conductivity (for example, stainless steel), and the melt 1 supplied from the storage container 2 into the first nozzle portion 51 is melted on the outer peripheral surface of the barrel 52a. In order to maintain the state, an electric heater (not shown) is wound.

  When the storage container 2 is heated by electromagnetic induction, the barrel 5 is preferably made of a material having electrical conductivity and good thermal conductivity (for example, iron, stainless steel, aluminum, copper, etc.). In addition to maintaining the polymer material or pitch material in a molten state by heat transfer from the container 2, the polymer material or pitch material is charged by applying a high voltage to the barrel 52a or the like. Further, when the barrel 52a is formed of a metal having a certain degree of electrical resistance such as stainless steel, a polymer for causing electromagnetic induction heating is wound around the barrel 52a in a non-contact manner so that the polymer is the same as above. It is also possible to keep the material or pitch-based material in a heated / molten state.

When electromagnetic induction heating is used, the electrical system related to the heater is not required to have a specification that can withstand high voltages (usually, the heater wire is thickened), and the current generated in the voltage generator that applies the high voltage is close. There is no risk of flowing into the electric heater and backflowing to the power source of the electric heater.
The collector 6 is disposed so as to face the melt discharge nozzle 5, and between the collector 6 and the melt discharge nozzle 5, in order to charge the melt 1 discharged from the melt discharge nozzle 5, A voltage is applied from a voltage generator 7 as a melt charging means.

  As described above, as a melt discharge nozzle that discharges the melt 1 stored in the storage container 2 in the form of a fine thread, the melt discharge nozzle 5 as shown in FIG. 2, that is, the melt 1 that discharges the melt 1 in the form of a thin thread. When a melt discharge nozzle 5 having one nozzle portion 51 and a second nozzle portion 52 that discharges the melt 1 from the first nozzle portion 51 with a gas while being pressurized with a gas is used, The melt 1 discharged in a fine thread form from the nozzle part 51 is discharged in a fine thread form from the second nozzle part 52 while being pressurized by gas. Thereby, since the diameter of the melt discharged in the form of a fine thread from the melt discharge nozzle toward the collector becomes thinner, fibers having a smaller fiber diameter can be obtained by the electrospinning method.

  A coal tar pitch material having a softening temperature of 200 ° C. is used as the melt 1 stored in the storage container 2. Storage container: stainless steel storage container (capacity: 10 mL), melt discharge nozzle diameter: 0.20 mm, storage Raw material temperature in the container: 330 ° C., raw material temperature in the melt discharge nozzle: 330 ° C., pressurized gas: nitrogen gas, pressurized gas preheating temperature: 330 ° C., melt discharge speed: 1000 mm / s, voltage application condition: collector As a ground electrode, a voltage of 35 kV is applied to the storage container and the melt discharge nozzle, the distance from the melt discharge nozzle tip to the collector is 80 mm, and the nitrogen gas pressure in the storage container is 0.3 MPa. From the nozzle 5, it discharged in the form of a fine thread. Then, the melt 1 discharged from the melt discharge nozzle 5 is collected as a fiber by the collector 6, and the collected fiber is infusible in air at 180 ° C., and then an inert gas (nitrogen gas) atmosphere. The carbon fiber diameter obtained by heating to 1000 ° C. and carbonizing and graphitizing at 2700 ° C. in an argon gas atmosphere was measured with a scanning electron microscope. As a result, the fiber diameter of the carbon fiber was around 500 nm as shown in FIG.

  The melt is collected as a fiber under the same conditions as in Example 1 except that the pressurized gas preheating temperature is 150 ° C., and then infusible, carbonized, graphitized and carbonized under the same conditions as in Example 1. Fiber was obtained. The fiber diameter of the obtained carbon fiber was measured with a scanning electron microscope. As a result, the fiber diameter of the carbon fiber was around 550 nm.

  A liquid crystal pitch having a softening point of 280 ° C. prepared using coal tar as a raw material was used. This is filled in a stainless steel container (capacity 10 mL), a stainless steel 27G nozzle (inner diameter 0.20 mm) is attached to the lower end of the container, and the preheated gas can be circulated to the outside as shown in FIG. An outer cylinder like this was attached. In addition, an electromagnetic induction heater capable of temperature control was wound around the outer cylinder. It should be noted that a normal temperature controller (plurality) is arranged to control the pitch temperature in the container to 350 ° C. and the nozzle temperature to 350 ° C., and nitrogen gas preheated to 350 ° C. is 100 m at the nozzle tip interval. The flow rate was set to a linear velocity of / s. A voltage of 25 kV generated by a high voltage generator was applied to the container, and a ground electrode was placed at a position 120 mm directly below the nozzle. Thereafter, the sealed container was spun by applying a nitrogen pressure of 0.5 MPa. Spinning proceeded well and very fine pitch fibers were obtained. When this was infusibilized and carbonized, and graphitized at 2700 ° C., ultrafine carbon fibers having a thermal conductivity of 400 to 600 W / mK were obtained.

Comparative Example 1

  Except not applying a high voltage between the melt discharge nozzle 5 and the collector 6, carbon fiber was obtained on the same conditions as Example 1, and the fiber diameter of the obtained carbon fiber was measured with the scanning electron microscope. As a result, the fiber diameter of the carbon fiber was 1-2 μm as shown in FIG.

Comparative Example 2

Carbon fibers were obtained under the same conditions as described above except that no pressurized gas was supplied to the second nozzle portion 52 of the melt discharge nozzle 5, and the fiber diameter of the obtained carbon fibers was measured with a scanning electron microscope. As a result, the fiber diameter of the carbon fiber was around 1 μm as shown in FIG.
In FIGS. 4 and 5, some thick fibers are generated when the temperature immediately after the start of spinning does not reach a steady state and are contaminated.

Comparative Example 3

The liquid crystal pitch used in Example 2 was dissolved in quinoline to form a solution and spun at room temperature. At this time, since there is no need to heat, the electromagnetic induction heater was removed. As in Example 2, a nitrogen gas of 180 to 200 ° C. was flowed so as to obtain a linear velocity of 100 m / s at the interval between the nozzle tips (through a PTFE tube having insulation properties and heat resistance up to 260 ° C. The ground electrode was placed at a position 120 mm directly below the nozzle with an applied voltage of 25 kV. The reason for setting the temperature of the nitrogen gas to 180 to 200 ° C. is to volatilize quinoline immediately after spinning to maintain a fine thread shape. The produced ultrafine pitch fibers were infusibilized, carbonized, and then graphitized, and the carbon fibers obtained had a thermal conductivity of 20 to 50 W / mK.
When Example 1 and Comparative Example 1 are compared, Example 1 can obtain a carbon fiber having a fiber diameter of submicrometer or less, while Comparative Example 1 can obtain a carbon fiber having a fiber diameter of submicrometer or less. I understand that there is no. This is because Example 1 applied a voltage between the melt discharge nozzle 5 and the collector 6 to spin the carbon fiber, whereas Comparative Example 1 applied a voltage between the melt discharge nozzle 5 and the collector 6. This is because the carbon fiber was spun without application of.

  Next, when Example 1 and Comparative Example 2 are compared, Example 1 can obtain a carbon fiber having a fiber diameter of submicrometer or less, whereas Comparative Example 2 has a fiber diameter of submicrometer or less. It turns out that it cannot be obtained. In the first embodiment, the melt 1 discharged from the first nozzle portion 51 of the melt discharge nozzle 5 is spouted from the second nozzle portion 52 while being compressed with gas to spin carbon fibers. On the other hand, in the comparative example 2, the melt 1 discharged from the first nozzle portion 51 of the melt discharge nozzle 5 is discharged from the second nozzle portion 52 in a fine thread shape without being pressurized by the gas, and thus carbon fiber. This is because of spinning.

  Accordingly, when a fiber is produced from a melt of a polymer material or a pitch-based material by an electrospinning method, the melt 1 is used as a melt discharge nozzle that discharges the melt of the polymer material or the pitch-based material into a thin thread shape. There are provided a first nozzle portion 51 that discharges in a fine thread shape, and a second nozzle portion 52 that discharges the melt 1 discharged from the first nozzle portion 51 in a thin thread shape while pressurizing it with a gas such as nitrogen gas. By using the melt discharge nozzle 5 formed as described above, a fiber having a smaller fiber diameter can be obtained by an electrospinning method.

Further, in the comparison between Example 3 and Comparative Example 3, since Comparative Example 3 is spun in a solution state, the liquid crystal pitch at the corner is spun without molecular orientation, whereas in Example 3, the liquid crystal is spun. Spinning is performed while the pitch is molecularly oriented. Therefore, it can be understood that the thermal conductivity was high.
In one embodiment of the present invention shown in FIG. 1, a solid polymer material or pitch-based material is melted in a container different from the storage container 2 and supplied to the storage container 2 with a gear pump or the like. However, you may make it melt | dissolve the polymer substance or pitch type substance of a solid state with the storage container 2. FIG.

  In the embodiment of the present invention shown in FIG. 1, the storage container 2 that stores the melt 1 of the polymer material or the pitch-based material is formed of stainless steel. The material is not particularly limited, and can be arbitrarily selected according to the type of polymer material or pitch-based material. Furthermore, when the storage container 2 is formed of stainless steel, glass, or the like, the storage container 2 can be manufactured at low cost. However, when the melt stored in the storage container 2 is a highly corrosive melt, platinum, nickel, etc. The storage container 2 may be formed of a noble metal or ceramic.

In the embodiment of the present invention shown in FIG. 1 as the storage container 2 for storing the melt 1 of the polymer material or the pitch-based material, the one integrally formed of stainless steel is shown. For example, the storage container 2 may be composed of a plurality of parts in consideration of maintenance. In this case, it is desirable to devise so that the melt does not leak due to the internal pressure, and it is preferable to interpose a packing made of aluminum, copper or PTFE between the parts.
In the embodiment of the present invention shown in FIG. 1, the melt 1 stored in the storage container 2 is discharged in a thin thread form from one melt discharge nozzle 5, but the number of the melt discharge nozzles 5 is Either singular or plural may be used. However, a plurality is more preferable in terms of productivity.

  In the first embodiment, the temperature of the melt 1 discharged from the melt discharge nozzle 5 is set to 330 ° C. to produce ultrafine fibers. However, the present invention is not limited to this, and from the melt discharge nozzle 5 If the melt 1 is discharged in the form of a fine thread from the melt discharge nozzle 5 under a temperature condition in which the viscosity of the discharged melt 1 is 1 to 100 poise, the fiber diameter is sub-micrometer as in the first embodiment. An ultrafine fiber of a meter or less can be obtained.

In the first embodiment, nitrogen gas is used as the pressurized gas supplied into the second nozzle portion 52 of the melt discharge nozzle 5. However, the present invention is not limited to this. For example, air, helium gas, argon gas is used. May be used instead of nitrogen gas. However, it is preferable to avoid the use of air because the fiber may generate heat or ignite at a high temperature exceeding 300 ° C. due to rapid oxidation.
A preferable type of gas is an inert gas that does not oxidize fibers, such as helium, nitrogen, and argon. The lower limit temperature of the gas is preferably −50 ° C. from the melting point or softening point of the melt, and the upper limit temperature of the gas is preferably + 130 ° C. from the melting point or softening point of the melt. Here, the temperature of −50 ° C. from the melting point or softening point of the melt is a temperature of −50 ° C. from the melting point of the melt or −50 ° C. from the softening point, and + 130 ° C. from the melting point or softening point of the melt. The temperature means a temperature of + 130 ° C. from the melting point of the melt or + 130 ° C. from the softening point.

When the gas temperature is lower than −50 ° C. from the melting point or softening point of the melt, the melt discharge portion at the tip of the first nozzle portion 51 is cooled too much, and the viscosity of the melt increases. The melt may not be discharged well. Also, if the gas temperature exceeds + 130 ° C. from the melting point or softening point of the melt, the viscosity of the melt may be lowered, and the discharged material may become particulate, or the melt may be thermally altered or deteriorated. .
When the temperature of the storage container, melt discharge nozzle, etc. and the pressurized gas temperature are below 260 ° C, insulation is achieved by inserting a heat-resistant polytetrafluoroethylene (PTFE) tube between the gas temperature control means and the melt discharge nozzle. Therefore, a normal gas heater can be used as the gas temperature adjusting means. When it exceeds 260 ° C., an electromagnetic induction method is preferable as the gas temperature adjusting means.

In the first embodiment, the collector 6 is grounded to apply a positive voltage to the melt discharge nozzle 5 from the viewpoint of safety, but the collector 6 may be a positive electrode or a negative electrode.
In Example 1, a voltage of 35 kV was applied between the melt discharge nozzle 5 and the collector 6 to produce ultrafine fibers, but the present invention is not limited to this. However, when the voltage applied between the melt discharge nozzle 5 and the collector 6 is less than 0.5 kV, the melt 1 is difficult to separate from the melt discharge nozzle 5, and when the voltage exceeds 100 kV, the melt discharge nozzle 5. Therefore, it is preferable that the voltage applied between the melt discharge nozzle 5 and the collector 6 is 0.5 to 100 kV.

  In Example 1, although the distance from the front-end | tip of the melt discharge nozzle 5 to the collector 6 was set to 80 mm, an ultrafine fiber was manufactured, it is not limited to this. However, if the distance from the tip of the melt discharge nozzle 5 to the collector 6 is less than 10 mm, dielectric breakdown is likely to occur between the melt discharge nozzle 5 and the collector 6, and if it exceeds 200 mm, the fiber is pulled by an electric field. Since the diameter of the melt discharged from the melt discharge nozzle 5 becomes difficult to be reduced, the distance from the tip of the melt discharge nozzle 5 to the collector 6 is preferably 10 to 200 mm.

  As the melt 1 stored in the storage container 2, in Example 1, a coal tar pitch material having a softening temperature of 200 ° C. was used, but is not limited thereto. For example, if the melt 1 stored in the storage container 2 is a polymer substance, polyethylene terephthalate (PET), polypropylene terephthalate (PPT), polybutylene terephthalate (PBT), polyvinylidene fluoride (FVDF), polyacrylonitrile (PAN) ), Polyacrylic acid, polymethyl methacrylate (PMMA), polystyrene (PS), polycarbonate, polymethylpentene (PMP), polyvinyl chloride (PVC), polyethylene (PE), polypropylene (PP), polyamide (polyamide) 6, polyamide 66, polyamide 610, polyamide 12, polyamide 46, polyamide 9T, etc.), polyurethane, aramid, polyimide (PI), polybenzoimidazole (PBI), polybenzoxazole (PBO), poly Vinyl alcohol (PVA), cellulose, cellulose acetate, cellulose acetate butyrate, polyvinylpyrrolidone (PVP), polyethyleneimide (PEI), polyoxymethylene (POM), polyethylene oxide (PEO), ethylene polysuccinate , Polysulfide ethylene, polypropylene oxide, polyvinyl acetate, polyaniline, ethylene polyterephthalate, polyhydroxybutyric acid, polyethylene oxide, polylactic acid (PLA), polyglycolic acid (PGA), polyethylene glycol (PEG), polycaprolactone, Examples thereof include polypeptides, proteins, collagen, and a plurality of copolymers and mixtures thereof. Moreover, if the melt 1 is a pitch-type substance, coal tar pitch, petroleum pitch, etc. are mentioned. Further, a material obtained by mixing organic or inorganic powder, whisker, or the like with the above material may be used as a polymer material or a pitch-based material.

As a method of charging the melt 1 by applying a voltage between the melt discharge nozzle 5 and the collector 6, a method of applying a voltage to the tip of the melt discharge nozzle 5 and a melt in the melt discharge nozzle 5 are used. 1 to apply a voltage, but it is preferable to apply a voltage to the melt 1 in the melt discharge nozzle 5 from the viewpoint of simplicity of the apparatus.
In the embodiment of the present invention shown in FIG. 1, the collector 6 that collects the melt 1 discharged as a fine thread from the melt discharge nozzle 5 as a fiber is shown as a flat plate. However, the present invention is not limited to this. For example, a rotating drum or a rotating belt (belt conveyor) may be used. However, from the viewpoint of production efficiency, a rotary collector is preferable to a static flat plate.
The shape of the fiber aggregate collected by the collector 6 is not limited to a short fiber, but is not particularly limited to a planar nonwoven fabric, a filament, a three-dimensional structure such as a tubular structure. Moreover, it is also possible to laminate | stack the ultrafine fiber manufactured by the method of this invention directly on a film or a nonwoven fabric.

  DESCRIPTION OF SYMBOLS 1 ... Melt, 2 ... Storage container, 3 ... Electric heater, 4 ... Nitrogen gas supply line, 5 ... Melt discharge nozzle, 51 ... 1st nozzle part, 52 ... 2nd nozzle part, 6 ... Collector, 7 ... voltage generator.

Claims (7)

  1. A fiber manufacturing apparatus used when a fiber is manufactured from a melt of a polymer material or a pitch-based material by an electrospinning method,
    A storage container for storing the melt; a melt discharge nozzle for discharging the melt stored in the storage container into a thin thread; a collector disposed opposite to the melt discharge nozzle; and the melt discharge A melt charging means for applying a voltage between the nozzle and the collector to charge the melt, and the melt discharge nozzle is formed of a first nozzle portion and a fine thread shape from the first nozzle portion And a second nozzle portion that discharges the melt discharged into a fine thread while pressurizing with a gas.
  2.   The gas is an inert gas, and has gas temperature adjusting means for adjusting the lower limit temperature of the gas to the melting point or softening point of the melt of −50 ° C. and the upper limit temperature to the melting point or softening point of the melt of + 130 ° C. The fiber manufacturing apparatus according to claim 1.
  3.   The fiber manufacturing apparatus according to claim 1, further comprising electromagnetic induction heating means for heating the melt.
  4. When producing a fiber from a melt of a polymer material or a pitch material by an electrospinning method,
    A storage container for storing the melt; a melt discharge nozzle for discharging the melt stored in the storage container into a thin thread; a collector disposed opposite to the melt discharge nozzle; and the melt discharge A melt charging means for charging a melt discharged from the melt discharge nozzle by applying a voltage between the nozzle and the collector, and the melt discharge nozzle includes a first nozzle portion; A fiber is manufactured using a fiber manufacturing apparatus having a second nozzle part that discharges the melt discharged in a thin thread form from the first nozzle part into a fine thread while pressurizing with a gas. Method.
  5.   The said gas is an inert gas, The minimum temperature of this gas is melting | fusing point or softening point -50 degreeC of the said melt, and upper limit temperature is melting | fusing point or softening point +130 degreeC of the said molten material, The fiber manufacturing method as described in 2.
  6.   The fiber manufacturing method according to claim 4 or 5, wherein the melt is heated by electromagnetic induction heating means.
  7.   The fiber production method according to any one of claims 4 to 6, wherein the fiber collected by the collector is infusibilized and then carbonized or carbonized and graphitized.
JP2009098052A 2008-04-18 2009-04-14 Fiber-producing apparatus and method for producing fiber Pending JP2009275339A (en)

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JP2008108721 2008-04-18
JP2009098052A JP2009275339A (en) 2008-04-18 2009-04-14 Fiber-producing apparatus and method for producing fiber

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JP2009098052A JP2009275339A (en) 2008-04-18 2009-04-14 Fiber-producing apparatus and method for producing fiber

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