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WO2018199354A1 - Appareil de filage servant à produire des nanofibres composites à deux composants, et procédé de production de nanofibres composites à deux composants l'utilisant - Google Patents

Appareil de filage servant à produire des nanofibres composites à deux composants, et procédé de production de nanofibres composites à deux composants l'utilisant Download PDF

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Publication number
WO2018199354A1
WO2018199354A1 PCT/KR2017/004445 KR2017004445W WO2018199354A1 WO 2018199354 A1 WO2018199354 A1 WO 2018199354A1 KR 2017004445 W KR2017004445 W KR 2017004445W WO 2018199354 A1 WO2018199354 A1 WO 2018199354A1
Authority
WO
WIPO (PCT)
Prior art keywords
spinning
tube
tube body
liquid distribution
polygonal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2017/004445
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English (en)
Korean (ko)
Inventor
김학용
김태우
채수형
박미라
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Woorinano Co
Industry Academic Cooperation Foundation of Chonbuk National University
Original Assignee
Woorinano Co
Industry Academic Cooperation Foundation of Chonbuk National University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Woorinano Co, Industry Academic Cooperation Foundation of Chonbuk National University filed Critical Woorinano Co
Priority to PCT/KR2017/004445 priority Critical patent/WO2018199354A1/fr
Publication of WO2018199354A1 publication Critical patent/WO2018199354A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • 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

Definitions

  • the present invention relates to a spinning device for producing two-component composite nanofibers and a method of manufacturing a two-component composite nanofibers using the same. More specifically, the present invention can produce a high quality two-component composite nanofiber web with high productivity per unit time and processability.
  • the present invention relates to a spinning tube, and also to a method for producing a high quality two-component composite nanofiber web using the spinning tube.
  • bicomponent composite nanofiber of the present invention is used to mean both core-sheath composite nanofibers and side-by-side composite nanofibers, and the "core-sheath composite nanofibers” The term is used with the meaning including eccentric core-cis type composite nanofibers.
  • the production of nanofibers through electrospinning is 0.1 ⁇ 1 g per hour and the solution discharge is very low, 1.0 ⁇ 5.0 mL per hour [D. H. H. Renecker et al., Nanotechnology 2006, VOl 17, 1123].
  • Nano Letters, 2007, Vol7 (4) 1081 is a SnO 2 in one nozzle having an internal diameter of 0.4 mm among the composite nozzles in which two nozzles are arranged side by side. Feed the precursor solution and TiO 2 to the remaining nozzles with an internal diameter of 0.7 mm A method of manufacturing TiO 2 / SnO 2 composite inorganic nanofibers in a side-by-side form by electrospinning after supplying a precursor solution is disclosed.
  • the conventional method depends only on electrostatic force, the discharge amount per nozzle per unit time This very low productivity is low, there was a problem that the nozzle replacement and cleaning is difficult.
  • Polymer, 2003, Vol. 44, 6353 uses a teflon needle with an internal diameter of 0.7 mm and a thickness of 0.2 mm, which is used to simultaneously pump two solutions with a cylinder pump so that the two solutions merge at the needle section.
  • a method of producing a composite side-side composite nanofiber by electrospinning by supplying a platinum electrode in a solution is disclosed.
  • the conventional method also depends only on electrostatic force, the discharge amount per nozzle per unit time is very low, resulting in high productivity. Falling, there was a problem that the nozzle replacement and cleaning is difficult.
  • the present invention can minimize the work risk due to high voltage application, can greatly improve the productivity of the two-component composite nanofibers, and prevent the droplet phenomenon when manufacturing nanofibers to improve the quality of the two-component composite nanofiber web It is to provide a spinning device for producing a two-component composite nanofibers that can be improved.
  • Another object of the present invention is to provide a method for producing a high quality two-component composite nanofibers with high productivity using the spinning tube for producing a two-component composite nanofibers.
  • the spinning device for producing a two-component composite nanofiber is (i) a spinning tube main body (Ta) having one form selected from a cylindrical shape and a conical shape; Consists of a polygonal tube-shaped hollow portion (Tb) formed along the longitudinal direction of the spinning tube body (Ta), the corner portions of the polygonal tube-shaped hollow portion (Tb) and the outer peripheral surface of the spinning tube body (Ta) Spinning tube (T) having a contacting structure and (ii) Spinning liquid distribution tube body (1a) connected to the spinning tube (T), and having a shape selected from cylindrical and conical, the spinning liquid distribution The spinning on each of the corners of the polygonal tube-like hollow portion 1b and the polygonal tube-like hollow portion 1b formed in the tube body 1a along the longitudinal direction of the spinning solution distribution tube body 1a.
  • Consists of a nozzle (1c) is provided along the longitudinal direction of the distribution tube body (1a), the corner portion of the polygonal tube-like hollow portion (1b) is in contact with the outer peripheral surface of the spinning liquid distribution tube body (1a) Consists of a spinning solution distribution tube (1) having a.
  • the present invention (i) by rotating the spinning tube (T) and the spinning liquid distribution tube (1) a high voltage to the spinning tube (T) and the spinning liquid distribution tube (1) with a voltage generator (6) And (ii) the first spinning solution is supplied into the nozzle 1c constituting the spinning solution distribution tube 1, and at the same time into the polygonal tubular hollow part 1b constituting the spinning solution distribution tube 1.
  • the first spinning solution supplied into the nozzle 1c of the spinning liquid distribution tube and the polygonal tubular hollow portion 1b of the spinning liquid distribution tube.
  • the second spinning solution to the collector 2 in which the high voltage is applied by the voltage generator 6 through the corner of the polygonal tube-shaped hollow part Tb forming the spinning tube T by using centrifugal force and electric force. Spinning produces bicomponent composite nanofibers.
  • the bicomponent composite nanofibers can be manufactured with high productivity (discharge amount), solvent volatilization and recovery are easy, and the spinning solution falls on the collector in a solution state instead of fibrous. It also effectively prevents (drop phenomenon) to improve the quality of the two-component composite nanofiber web.
  • FIG. 1 is a process schematic diagram of producing a bicomponent composite nanofiber according to the present invention.
  • Figure 2 is a schematic diagram showing the mechanism by which the core-sheath bicomponent composite nanofibers are formed in the spinning tube (T) for producing a bicomponent composite nanofiber of 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 polygonal tube-shaped hollow 1b formed in the spinning solution distribution tube 1 of the present invention.
  • FIG. 5 is a scanning electron microscope photograph of the bicomponent composite nanofibers prepared in Example 1.
  • Figure 6 is a scanning electron microscope photograph of the hollow carbon nanofibers prepared in Example 2.
  • a longitudinal direction of the spinning liquid distribution tube body 1a is formed in each of the corner portions of the polygonal tube-shaped hollow part 1b and the polygonal tube-shaped hollow part 1b formed along the longitudinal direction of the distribution tube main body 1a.
  • Spinning liquid dispensing tube (1) comprising a nozzle (1c) is provided along the side, the edge portion of the polygonal tube-like hollow portion (1b) is in contact with the outer peripheral surface of the spinning liquid dispensing tube body (1a) It includes;
  • One or two or more nozzles 1c are provided along the longitudinal direction of the main body 1a of the spinning tube at each corner portion of the polygonal tubular hollow portion 1b constituting the spinning liquid distribution tube 1.
  • the spinning tube (T) and the spinning liquid distribution tube (1) may be integrally manufactured and formed from the beginning, or may be separately manufactured and then connected to each other by assembling.
  • the first spinning solution is supplied into the nozzle 1c using the first spinning solution supply pipe 3a
  • the second spinning solution is supplied into the polygonal tubular hollow portion 1b using the second spinning solution supply pipe 3b. To supply.
  • A spinning solution for forming a core
  • B sheath-forming
  • the first spinning solution (A: spinning solution for forming a core) has a polygonal tube-shaped hollow part constituting the spinning tube through a nozzle 1c having a relatively small diameter constituting the spinning liquid distribution tube. Since it is supplied to the part Tb ', it is supplied to the corner part Tb' of the polygonal tube-shaped hollow part which comprises a spinning tube through the polygonal tube-shaped hollow part 1b of a relatively large diameter spinning liquid distribution tube.
  • the solution flow is relatively faster than the two spinning solution (B: cis forming spinning solution) to maintain the core shape throughout the length of the corner portion (Tb '), and to maintain the core shape of the first spinning solution (A: core formation
  • the spinning solution is wrapped around the second spinning solution (B: spinning solution for forming the sheath) to maintain the core-sheath shape over the entire length of the corner portion Tb 'of the polygonal tubular hollow part constituting the spinning tube.
  • Prize In the corner portion (Tb ') the top end of the core-sheath type bicomponent composite nanofibers is formed.
  • the manufacturing mechanism of the core-sheath bicomponent composite nanofiber according to the present invention described above is completely different from the mechanism for producing the core-sheath bicomponent composite nanofiber by arranging two nozzles in a core-sheath form. .
  • the present invention since two-component composite nanofibers are simultaneously manufactured in a plurality of corner portions (Tb '), productivity is greatly improved as compared with the conventional nozzle type method, and various shapes can be changed by changing the shape of the spinning liquid distribution tube (1).
  • the two-component composite nanofibers can be prepared.
  • the two-component composite nanofibers are core-sheath type composite nanofibers or side by side type composite nanofibers, and the core-sheath composite fiber is an eccentric core-sheath type. It may be a composite nanofiber.
  • a core forming spinning solution (first spinning solution) is supplied into the nozzle 1c constituting the spinning solution distribution tube 1, and a sheath forming spinning solution is provided into the polygonal tubular hollow part 1b. (Second spinning solution) was supplied to produce a core-cis type composite nanofiber.
  • the side-by-side composite nanofibers It can be prepared.
  • one of two different polymer solutions is used as the first spinning solution supplied into the nozzle 1c constituting the spinning liquid distribution tube 1, and the remaining one is used as the spinning liquid distribution tube 1.
  • the core-sheath composite nanofibers or side-by-side composite nanofibers are manufactured using the second spinning solution supplied into the polygonal tubular hollow part 1b constituting the core.
  • a hollow fiber is prepared by dissolving the core of the core-sheath composite nanofiber prepared as described above with an organic solvent or the like.
  • one of two precursor solutions containing different inorganic materials is used as the first spinning solution supplied into the nozzle 1c constituting the spinning liquid distribution tube 1, and the other one is used.
  • a bicomponent composite inorganic nanofiber is produced by using the second solution supplied into the polygonal tubular hollow portion 1b constituting the spinning solution distribution tube 1.
  • the polymer solution is used as the first spinning solution supplied into the nozzle 1c constituting the spinning liquid distribution tube 1, and the precursor solution containing the inorganic material is used as the spinning liquid distribution tube 1.
  • a core-sheath composite nanofiber is prepared in which the core component is a polymer and the sheath component is made of an inorganic material, using the second spinning solution supplied into the polygonal tubular hollow portion 1b.
  • an inorganic hollow fiber is prepared.
  • the polygonal solution constituting the spinning solution distribution tube 1 using the precursor solution containing the inorganic material as the first spinning solution supplied into the nozzle 1c constituting the spinning solution distribution tube, and the polymer solution It is used as a second spinning solution supplied into the tubular hollow portion 1b to prepare a core-cis-type composite nanofiber in which the core component is an inorganic material and the sheath component is composed of a polymer.
  • porous carbon nanofibers are manufactured by using a spinning tube provided with two or more nozzles 1c at each corner portion of the polygonal tubular hollow part 1b constituting the spinning liquid distribution tube 1.
  • the hollow carbon nanofibers or porous carbon nanofibers prepared as described above are useful as filter materials, secondary battery membrane materials, electrode materials, high functional clothing materials, drug delivery materials, and the like.
  • Polymethyl methacrylate was dissolved in dimethylformamide as a solvent to prepare a polymethyl methacrylate 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.
  • a cylindrical spinning tube main body Ta having an outer diameter of 45 mm and a length of 8 mm and 12 formed along the longitudinal direction of the spinning tube main body Ta is shown.
  • Spinning tube (T) having a structure consisting of a rectangular tube-shaped hollow portion (Tb), the corner portion of the octagonal tube-shaped hollow portion (Tb) is in contact with the outer peripheral surface of the radiating tube body (Ta) and (ii) 12)
  • a polygonal tubular hollow having a cylindrical shape and a spinning liquid distribution tube body 1a, which is formed along the longitudinal direction of the spinning liquid distribution tube body 1a inside the spinning liquid distribution tube body 1a.
  • It consists of twelve nozzles 1c with a diameter of 0.7 mm provided in each of the portion 1b and the corner portions of the twelve polygonal tubular hollow portion 1b along the longitudinal direction of the radiating tube body 1a.
  • the corner portions of the pentagonal tubular hollow portion 1b are formed outside the spinning liquid distribution tube body 1a.
  • the spinning liquid distribution tube (1) While rotating the spinning liquid distribution tube (1) having a structure in contact with the surface at 350rpm, a voltage generator 6 applied a voltage of 35kV to the spinning tube (T) and the spinning liquid distribution tube (1)
  • the polymethyl methacrylate solution (the first spinning solution) is supplied into the nozzle 1c having a diameter of 0.7 mm, which forms the spinning liquid distribution tube 1, and at the same time, the octagonal body forming the spinning liquid distribution tube 1 is formed.
  • the corner part of the pentagonal tubular hollow part Tb which comprises the spinning tube T using centrifugal force and an electric force.
  • the polyacrylonitrile solution (second spinning solution) as a polymer solution was supplied at 0.25cc per minute and the polymethylmethacrylate solution (first spinning solution) was supplied at 0.20cc per minute. At this time, the distance between the collector 2 and the spinning tube 1 was 35 cm.
  • the polymethyl methacrylate component which is a core component
  • the structure of the polyacrylonitrile, which is a cis component is enclosed outside the polymethyl methacrylate component, which is the core component.
  • the core-cis type bicomponent composite nanofibers prepared in FIG. 1 were stabilized at 240 ° C. for 30 minutes in air, and then heat-treated at 800 ° C. for 2 hours and 30 minutes in a nitrogen atmosphere to prepare hollow carbon nanofibers. Scanning electron micrographs of the prepared hollow carbon nanofibers were as shown in FIG. 6. 6 shows that the hollow part is well formed.
  • Tb is the hollow tube-shaped hollow part of the spinning tube
  • d distance between the nozzle 1c and the corner vertex of the polygonal tubular hollow part 1b nearest to the nozzle.
  • Tb ' Hollow corner of polygonal tube of spinning tube
  • the present invention can be used to produce high quality bicomponent composite nanofibers with high productivity.

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

Abstract

L'appareil de filage servant à produire des nanofibres composites à deux composants, selon la présente invention, comprend : (i) un tube de filage (T) qui comprend un corps (Ta) de tube de filage de forme cylindrique ou conique et une partie creuse tubulaire polygonale (Tb) formée le long de la direction de la longueur du corps (Ta) de tube de filage, à l'intérieur du corps (Ta) de tube de filage et qui possède une structure dans laquelle les zones de sommet de la partie creuse tubulaire polygonale (Tb) sont en contact avec la surface circonférentielle externe du corps (Ta) de tube de filage; et (ii) un tube de distribution (T) de solution de filage qui est relié au tube de filage (T), qui comprend un corps (1a) de tube de distribution de solution de filage de forme cylindrique ou conique, une partie creuse tubulaire polygonale (1b) formée le long de la direction de la longueur du corps (1a) de tube de distribution de solution de filage, à l'intérieur du corps (1a) de tube de distribution de solution de filage, et des buses (1c) installées le long de la direction de la longueur du corps (1a) de tube de distribution de solution de filage, dans les zones de sommet respectives de la partie creuse tubulaire polygonale (1b), et qui possède une structure dans laquelle les zones de sommet de la partie creuse tubulaire polygonale (1b) sont en contact avec la surface circonférentielle externe du corps (1a) de tube de distribution de solution de filage. La présente invention utilise simultanément une force électrostatique et une force centrifuge, ce qui permet de produire des nanofibres composites à deux composants avec une productivité élevée (volume d'évacuation), facilite la volatilisation et la récupération du solvant, empêche efficacement un phénomène (goutte) dans lequel une solution de filage goutte sur un collecteur dans un état en solution, non pas dans un état fibreux, et améliore ainsi la qualité d'une nappe de nanofibres composites à deux composants.
PCT/KR2017/004445 2017-04-26 2017-04-26 Appareil de filage servant à produire des nanofibres composites à deux composants, et procédé de production de nanofibres composites à deux composants l'utilisant Ceased WO2018199354A1 (fr)

Priority Applications (1)

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PCT/KR2017/004445 WO2018199354A1 (fr) 2017-04-26 2017-04-26 Appareil de filage servant à produire des nanofibres composites à deux composants, et procédé de production de nanofibres composites à deux composants l'utilisant

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PCT/KR2017/004445 WO2018199354A1 (fr) 2017-04-26 2017-04-26 Appareil de filage servant à produire des nanofibres composites à deux composants, et procédé de production de nanofibres composites à deux composants l'utilisant

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003313721A (ja) * 2002-04-25 2003-11-06 Toray Ind Inc 多葉断面フィラメント糸
KR100607416B1 (ko) * 2005-05-10 2006-08-01 전북대학교산학협력단 전기방사를 이용한 연속상 필라멘트의 제조방법 및 이로제조된 연속상 필라멘트
KR20130012733A (ko) * 2011-07-26 2013-02-05 중앙대학교 산학협력단 전기방사용 복합 노즐, 이를 포함하는 전기방사 장치, 이를 이용하여 제조되는 나노 섬유 구조체 및 나노 막대
KR101558213B1 (ko) * 2014-07-25 2015-10-12 주식회사 우리나노 나노섬유 제조용 전기방사튜브 시스템
KR20160116236A (ko) * 2015-03-27 2016-10-07 주식회사 우리나노 원심력을 이용한 다성분 나노섬유 방사기구 및 이를 이용한 다성분 나노섬유의 제조방법
KR20170055597A (ko) * 2015-11-11 2017-05-22 주식회사 우리나노 2성분 복합 나노섬유 제조용 방사장치 및 이를 이용한 2성분 복합 나노섬유의 제조방법

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003313721A (ja) * 2002-04-25 2003-11-06 Toray Ind Inc 多葉断面フィラメント糸
KR100607416B1 (ko) * 2005-05-10 2006-08-01 전북대학교산학협력단 전기방사를 이용한 연속상 필라멘트의 제조방법 및 이로제조된 연속상 필라멘트
KR20130012733A (ko) * 2011-07-26 2013-02-05 중앙대학교 산학협력단 전기방사용 복합 노즐, 이를 포함하는 전기방사 장치, 이를 이용하여 제조되는 나노 섬유 구조체 및 나노 막대
KR101558213B1 (ko) * 2014-07-25 2015-10-12 주식회사 우리나노 나노섬유 제조용 전기방사튜브 시스템
KR20160116236A (ko) * 2015-03-27 2016-10-07 주식회사 우리나노 원심력을 이용한 다성분 나노섬유 방사기구 및 이를 이용한 다성분 나노섬유의 제조방법
KR20170055597A (ko) * 2015-11-11 2017-05-22 주식회사 우리나노 2성분 복합 나노섬유 제조용 방사장치 및 이를 이용한 2성분 복합 나노섬유의 제조방법

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