KR101806317B1 - Spinning tube for two-component composited nanofiber and method of manufacturing two-component composited nanofiber thereby - Google Patents

Spinning tube for two-component composited nanofiber and method of manufacturing two-component composited nanofiber thereby Download PDF

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Publication number
KR101806317B1
KR101806317B1 KR1020150150609A KR20150150609A KR101806317B1 KR 101806317 B1 KR101806317 B1 KR 101806317B1 KR 1020150150609 A KR1020150150609 A KR 1020150150609A KR 20150150609 A KR20150150609 A KR 20150150609A KR 101806317 B1 KR101806317 B1 KR 101806317B1
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South Korea
Prior art keywords
tube
spinning solution
nanofiber
composite nanofiber
hollow portion
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KR1020150150609A
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Korean (ko)
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KR20170051557A (en
Inventor
김학용
김태우
채수형
박미라
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주식회사 우리나노
전북대학교산학협력단
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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
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • 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
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • 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
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/34—Core-skin structure; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

A radiation tube (1) for manufacturing a bicomponent composite nanofiber of the present invention comprises (i) a radiation tube main body (1a) having one shape selected from a cylindrical shape and a conical shape, (ii) (Iii) a polygonal tube-shaped hollow portion 1b formed along the longitudinal direction of the radiation tube main body 1a and (iii) a corner portion of the hollow portion 1b on the polygonal tube, And the corner portions of the hollow portion 1b on the polygonal tube are in contact with the outer peripheral surface of the radiation tube main body 1a. The present invention relates to a method for manufacturing a nanofiber composite nanofiber, comprising the steps of: (i) applying a high voltage while rotating a spinning tube 1 for manufacturing the two-component complex nanofiber; (ii) supplying a first spinning solution into the nozzle 1c, (Iii) supplying a second spinning solution different from the first spinning solution into the first spinning solution and the second spinning solution, (iii) rotating the first spinning solution and the second spinning solution in the direction of the collector 2 To produce a two-component composite nanofiber. The present invention relates to a process for producing a two-component composite nanofiber with high productivity (discharge amount) because it uses electrostatic force and centrifugal force at the same time, facilitates solvent volatilization and recovery, (Drop phenomenon) is effectively prevented, thereby improving the quality of the two-component composite nanofiber web.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a spinning tube for manufacturing a two-component composite nanofiber, and a method for manufacturing a two-component composite nanofiber using the spin-

TECHNICAL FIELD The present invention relates to a radial tube for manufacturing a two-component composite nanofiber (hereinafter abbreviated as "radial tube") and a method for manufacturing a two-component composite nanofiber using the same, more specifically, The present invention relates to a radiation tube capable of producing a composite nano-fiber web, and also to a method for producing a high-quality two-component composite nano-fiber web using the radiation tube.

The term " two-component composite nanofiber "of the present invention is used to include both core-sheath type composite nanofiber and side-by-side type composite nanofiber, Is used to mean also an eccentric core-sheath type composite nanofiber.

As a conventional technique for producing cis-core type composite nanofibers, a method of electrospinning a spray solution for forming a sheath and a spinning solution for forming a core through a nozzle of a sheath / core type (double pipe type) with electrostatic force has been widely used.

However, since the above-mentioned conventional method relies solely on the electrostatic force to perform electrospinning, the discharge amount per nozzle unit per unit time per unit time is extremely low to 0.01 g, which leads to a problem of productivity and difficulty in mass production.

In general, the production of nanofibers through electrospinning is 0.1 to 1 g per hour, and the solution discharge rate is very low, ranging from 1.0 to 5.0 mL per hour [D. H. H. Renecker et al., Nanptechnology 2006, Vo 17, 1123]

Specifically, the nano-letter (Nano Letter), 2007, Vol7 (4) 1081 is another prior art as a side-by-two nozzles, one of SnO 2 in a nozzle inside diameter of the composite nozzle arranged in a side-form is 0.4㎜ The precursor solution was supplied, and the other nozzle having an inner diameter of 0.7 mm was charged with TiO 2 A method of producing TiO 2 / SnO 2 composite inorganic nanofibers in a side-by-side configuration is provided. However, since the conventional method depends on only the electrostatic force, the discharge amount per nozzle per unit time The productivity is deteriorated, and nozzle replacement and cleaning are difficult.

In Polymer, 2003, Vol. 44, 6353, a Teflon needle having an inner diameter of 0.7 mm and a thickness of 0.2 mmm was used, and two kinds of solutions were simultaneously injected into a cylinder pump so that two kinds of solutions were combined at the needle part And a platinum electrode is placed in a solution to perform electrospinning to produce a side-by-side composite nanofiber. However, since the conventional method also depends only on the electrostatic force, the discharge amount per nozzle per unit time is very low, There is a problem that it is difficult to remove and replace the nozzle and clean it.

In addition, the above conventional methods have a problem that the phenomenon in which the spinning solution falls on the collector in a solution state not in the form of a fiber (hereinafter referred to as "droplet phenomenon") is severely generated, and the quality of the two-component composite nanofiber web deteriorates.

The object of the present invention is to minimize the risk of work due to the application of high voltage and to greatly improve the productivity of the two-component composite nanofiber and to prevent the droplet phenomenon in the production of the nanofiber, And to provide a radiant tube for manufacturing a bicomponent composite nanofiber that can be improved.

Another object of the present invention is to provide a method for producing high-quality two-component composite nanofibers with high productivity by using a radial tube for producing the two-component composite nanofibers.

In order to achieve the above object, the present invention provides a radiant tube 1 for manufacturing a bicomponent composite nanofiber, comprising: (i) a radiation tube main body 1a having one shape selected from a cylindrical shape and a conical shape; (ii) (1b) formed in the longitudinal direction of the radiation tube main body (1a) in the interior of the radiating tube body (1a) and (iii) the corners of the hollow portion (1b) And a nozzle 1c provided along the longitudinal direction of the main body 1a.

At this time, the corner portions of the hollow portion 1b on the polygonal tube are formed to be in contact with the outer peripheral surface of the radiation tube main body 1a.

The present invention also relates to a method for producing a two-component composite nanofiber, comprising the steps of: (i) rotating the spinning tube 1 for manufacturing the two-component complex nanofiber with a motor 7, (Ii) supplying the first spinning solution into the nozzle 1c constituting the spinning tube 1 for producing the bicomponent composite nanofiber, and (ii) supplying the first spinning solution into the nozzle 1c constituting the spinning tube 1 for manufacturing the bicomponent composite nanofiber, (Iii) supplying the first spinning solution supplied into the nozzle 1c and the second spinning solution supplied into the hollow portion 1b on the polygonal tube into the tube-shaped hollow portion 1b, The second spinning solution is spun in the direction of the collector 2 in which a high voltage is applied by the voltage generator 6 by using centrifugal force and electric force to produce a bicomponent composite nanofiber.

The present invention relates to a process for producing a two-component composite nanofiber with high productivity (discharge amount) because it uses electrostatic force and centrifugal force at the same time, facilitates solvent volatilization and recovery, (Drop phenomenon) is effectively prevented, thereby improving the quality of the two-component composite nanofiber web.

1 is a schematic view of a process for producing a two-component composite nanofiber according to the present invention.
2 is a perspective view schematically showing a spinning tube 1 for producing a two-component composite nanofiber according to the present invention.
3 to 4 are schematic views showing a state in which a nozzle 1c is formed at a corner portion of a hollow 1b on a polygonal tube formed in the radiation tube 1 of the present invention.
Fig. 5 is a transmission electron micrograph of the two-component composite nanofiber prepared in Example 1. Fig.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

As shown in FIGS. 1 and 2, the radiation tube for manufacturing a bicomponent composite nanofiber according to the present invention comprises (i) a radiation tube main body 1a having one shape selected from a cylindrical shape and a conical shape, (ii) A polygonal tube-shaped hollow portion 1b formed in the main body 1a along the longitudinal direction of the radiation tube main body 1a and (iii) an edge portion of the hollow portion 1b on the polygonal tube, And a nozzle 1c provided along the longitudinal direction of the tube main body 1a and the corner portions of the hollow portion 1b on the polygonal tube are in contact with the outer peripheral surface of the radiation tube main body 1a .

One or two or more nozzles 1c are provided along the longitudinal direction of the main body 1a of the radiation tube in each of the corner portions of the hollow portion 1b on the polygonal tube.

Next, as shown in FIG. 1, (i) the spinning tube 1 for manufacturing the two-component complex nanofiber is rotated by a motor 7, Component nano-fiber is produced by applying a high voltage to the radiation tube 1 for producing the two-component composite nanofiber by the voltage generating device 6 and then (i) injecting a first voltage into the nozzle 1c constituting the radiation tube 1 for manufacturing the two- Supplying a spinning solution and supplying a second spinning solution different from the first spinning solution into the polygonal tube-shaped hollow portion 1b constituting the spinning tube 1 for producing the two-component complex nanofiber, (iii) 1c) and the second spinning solution supplied into the hollow portion 1b on the polygonal tube are moved in the direction of the collector 2 in which the high voltage is applied by the voltage generator 6 by using the centrifugal force and the electric force To prepare a two-component composite nanofiber.

At this time, the first spinning solution is supplied into the nozzle 1c by using the first spinning solution distribution plate 3a, and the second spinning solution dispensing plate 3b is fed into the hollow portion 1b on the polygonal tube. Supply the spinning solution.

Wherein the two-component composite nanofiber is a core-sheath type composite nanofiber or a side by side type composite nanofiber, and the core-sheath type composite fiber is an eccentric core- It may be a composite nanofiber.

As an example of implementation, a spinning liquid for forming a core (a first spinning solution) is supplied into a nozzle 1c and a spinning solution for forming a sheath (a second spinning solution) is supplied into a hollow portion 1b on a polygonal tube, - Prepare cis-shaped composite nanofiber.

4, when the radiation tube 1 provided with the two nozzles 1c on each of the corner portions of the hollow portion 1b on the polygonal tube is used, the core-sheath type composite nanofibers Can be produced.

As another embodiment, it is possible to manufacture the side-by-side composite nanofibers by appropriately adjusting the distance (d) between the corner vertex of the hollow portion 1b on the polygonal tube and the nozzle 1c.

As one example of implementation, one of the two different polymer solutions is used as the first spinning solution supplied into the nozzle 1c, and the other one is used as the second spinning solution supplied into the hollow portion 1b on the polygonal tube To prepare a core-sheath type composite nanofiber or a side by side type composite nanofiber.

The core part of the core-sheath type composite nanofiber prepared as described above is dissolved in an organic solvent or the like to produce a hollow fiber.

In another embodiment, one of the two types of precursors containing different minerals is used as the first spinning solution supplied into the nozzle 1c, and the remaining one species is supplied into the polygonal tube-shaped hollow portion 1b As a second solution, to prepare a two-component composite inorganic nanofiber.

The thus prepared two-component composite inorganic nanofiber is stabilized and carbonized to produce a single-component or two-component inorganic nanofiber.

As another embodiment, the polymer solution is used as the first spinning solution supplied into the nozzle 1c, and the precursor containing the inorganic material is used as the second spinning solution supplied into the hollow portion 1b on the polygonal tube, To produce a core-sheath type composite nanofiber composed of a polymer as a component and a sheath component as an inorganic material.

When the core component of the core-sheath type composite nanofiber thus prepared is dissolved in an organic solvent or the like, or is removed by carbonization, an inorganic hollow fiber is produced.

An example of the production of hollow carbon nanofibers using the radiation tube 1 of the present invention is as follows. A water-soluble polyvinyl alcohol solution is used as a first spinning solution supplied into the nozzle 1c, and a polyacrylonitrile solution The core-sheath type composite nanofiber is prepared by using the solution as the second spinning solution supplied into the hollow portion 1b on the polygonal tube, and then the water-soluble polyvinyl alcohol forming the core portion is removed with water to prepare the hollow polyacrylonitrile fiber Then, the hollow polyacrylonitrile fibers thus produced are stabilized and carbonized to produce hollow carbon nanofibers.

At this time, when a radial tube having two or more nozzles 1c provided on each corner of the hollow portion 1b on the polygonal tube is used, the porous carbon nanofibers are produced.

The hollow carbon nanofibers or the porous carbon nanofibers prepared as described above are useful as a filter material, a secondary battery membrane material, an electrode material, a highly functional garment material, and a drug delivery material.

Hereinafter, the present invention will be described in more detail with reference to Examples.

However, the scope of protection of the present invention is not limited by the following examples.

Example  One

Polymethylmethacrylate was dissolved in dimethylformamide as a solvent to prepare a polymethylmethacrylate solution (first spinning solution) having a solid content of 10% by weight.

Polyacrylonitrile was dissolved in dimethylformamide as a solvent to prepare a polyacrylonitrile solution (second spinning solution) having a solid content of 12% by weight.

Next, as shown in Figs. 1 and 2, (i) a radiation tube main body 1a having one shape selected from a cylindrical shape and a conical shape, (ii) (12b) formed in the longitudinal direction of the main body (1a), and (iii) a corner portion of the hollow portion (1b) on the 12th polygonal tube, Which has a structure in which the nozzles 1c having a diameter of 0.7 mm are installed along the circumference of the tube body 1a and the corner portions of the hollow portion 1b on the polygonal tube are in contact with the outer circumferential surface of the radiation tube main body 1a A voltage of 35 kV is applied to the radiation tube 1 by the voltage generator 6 while the tube 1 is rotated by the motor 7 at 350 rpm and then a voltage of 35 kV is applied to the nozzle 1c constituting the radiation tube 1 And the polymethylmethacrylate solution (the first spinning solution) A polyacrylonitrile solution (second spinning solution) is supplied into the polygonal tube-shaped hollow portion 1b constituting the tube 1 and then the supplied spinning solution is supplied to the collector 2 with a voltage of 35 kV applied thereto Cis-core type two-component composite nanofiber was prepared by electrospinning. The polyacrylonitrile solution (the second spinning solution), which is a polymer solution, was supplied at 0.25 cc / min and the polymethylmethacrylate solution (the first spinning solution) was supplied at 0.20 cc / min. The distance between the collector 2 and the radiation tube 1 was 35 cm.

The transmission electron microscope photograph of the cis-core type two-component composite nanofiber prepared as described above was as shown in FIG.

Fig. 5 shows a structure in which a polyacrylonitrile of a sheath component surrounds the outside of a core-component polymethylmethacrylate component having a diameter of about 300 nm.

Example  2

(I) a radiation tube main body 1a having one shape selected from a cylindrical shape and a conical shape as shown in Figs. 1 and 2, (ii) (Iii) 12-polygonal tube-shaped hollow portions 1b are formed along the longitudinal direction of the radiation tube main body 1a in the respective 12-polygonal tube-shaped hollow portions 1b formed along the longitudinal direction of the 12-polygonal tube- (1c) having a diameter of 0.7 mm and the corner portions of the hollow portion (1b) on the polygonal tube are in contact with the outer peripheral surface of the radiation tube main body (1a) A voltage of 35 kV is applied to the radiation tube 1 by the voltage generating device 6 while the motor 7 rotates at 350 rpm and then a voltage of 35 kV is applied to the radiation tube 1 through a receiving polyvinyl alcohol (First spinning solution) is supplied to the spinning tube 1, and at the same time, A polyacrylonitrile solution (second spinning solution) is supplied into the polygonal tube-shaped hollow portion 1b, and then the supplied spinning solution is electrospun in the direction of the collector 2 with a voltage of 35 kV applied thereto, Type composite nanofiber was prepared. The polyacrylonitrile solution (the second spinning solution), which is a polymer solution, was supplied at 0.25 cc / minute, and the polyvinyl alcohol solution (the first spinning solution) was supplied at 0.18 cc / minute. At this time, the distance between the collector 2 and the radiation tube 1 was 35 cm.

The thus-prepared cis-core type two-component composite nano-fibers were washed with water to remove water-soluble polyvinyl alcohol forming the core portion to prepare hollow polyacrylonitrile fibers, and stabilized and carbonized to prepare hollow carbon nanofibers .

1: Radiation tube for manufacturing 2-component composite nanofiber
1a: the body of the radiation tube
1b: hollow portion on the polygonal tube 1c: nozzle
2: Collector 3: Fluid distribution plate
3a: 1st spinning solution (spinning liquid for forming a core) distribution plate
3b: Second spinning solution (spinning solution for forming a sheath)
4: Second spinning solution (spinning liquid for forming a sheath) Supply tank
5: First spinning liquid (spinning liquid for forming a core)
6: voltage generator 7: motor
F: two-component composite nanofiber Fc: core component of two-component composite nanofiber
Fs: sheath portion of two-component composite nanofiber
X: polyacrylonitrile Y: polymethylmethacrylate
d: Distance between the corner 1c of the nozzle 1c and the corner vertex of the hollow portion 1b on the polygonal tube closest to the nozzle.

Claims (10)

(I) a radiation tube main body 1a having one shape selected from a cylindrical shape and a conical shape, (ii) a polygonal shape formed along the longitudinal direction of the radiation tube main body 1a inside the radiation tube body 1a, And a nozzle (1c) provided along the longitudinal direction of the radiation tube main body (1a) at corner portions of the hollow portion (1b) on the polygonal tube, wherein the polygonal tube hollow portion (1b) Characterized in that the corner portions of the tube-shaped hollow portion (1b) are in contact with the outer peripheral surface of the radiation tube main body (1a). 2. The two-component composite nano-tube according to claim 1, characterized in that two or more nozzles (1c) are provided along the longitudinal direction of the main body (1) of the radiating tube in each of the corner portions of the hollow portion (1b) Radiation tubes for making fibers. delete delete delete delete delete delete delete delete
KR1020150150609A 2015-10-29 2015-10-29 Spinning tube for two-component composited nanofiber and method of manufacturing two-component composited nanofiber thereby KR101806317B1 (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
KR101983678B1 (en) 2018-06-28 2019-09-03 (주)엔오엔그리드 Nanofiber radiator
KR20200001684A (en) 2018-06-28 2020-01-07 (주)엔오엔그리드 Continuous production method of nanofilter using nanofiber spinning device and continuous production device of nanofilter

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WO2018199353A1 (en) * 2017-04-26 2018-11-01 주식회사 우리나노 Spinning tube for producing two-ingredient composite nanofibers, and method for producing two-ingredient composite nanofibers using same
KR101959839B1 (en) * 2018-02-28 2019-07-05 주식회사 우리나노 Spinning device for two-component composited nanofiber and method of manufacturing two-component composited nanofiber thereby
CN109023557B (en) * 2018-09-14 2020-11-06 浙江农林大学暨阳学院 Electrostatic spinning device
KR102106268B1 (en) * 2018-10-08 2020-05-06 주식회사 우리나노 Spinning device for side by side type three-component composite nanofibers and method of manufacturing side by side type three-component composite nanofibers thereby
KR102077722B1 (en) * 2018-10-08 2020-02-17 주식회사 우리나노 Spinning device for side by side type multi-component composite nanofibers and method of manufacturing side by side type multi-component composite nanofibers thereby

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KR101263296B1 (en) * 2012-02-22 2013-05-15 주식회사 우리나노 Electrospinning device comprising cylindrical spinning tube with polygon hollow
KR101323581B1 (en) 2012-04-26 2013-10-30 전북대학교산학협력단 Spinning tube for manufacturing nano fiber and method of manufacturing nano fiber by thereby
KR101558213B1 (en) 2014-07-25 2015-10-12 주식회사 우리나노 Electrospining tube system for manfacturing nanofiber

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KR101263296B1 (en) * 2012-02-22 2013-05-15 주식회사 우리나노 Electrospinning device comprising cylindrical spinning tube with polygon hollow
KR101323581B1 (en) 2012-04-26 2013-10-30 전북대학교산학협력단 Spinning tube for manufacturing nano fiber and method of manufacturing nano fiber by thereby
KR101558213B1 (en) 2014-07-25 2015-10-12 주식회사 우리나노 Electrospining tube system for manfacturing nanofiber

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101983678B1 (en) 2018-06-28 2019-09-03 (주)엔오엔그리드 Nanofiber radiator
KR20200001684A (en) 2018-06-28 2020-01-07 (주)엔오엔그리드 Continuous production method of nanofilter using nanofiber spinning device and continuous production device of nanofilter

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