KR100762255B1 - Method of manufacturing nano fiber - Google Patents

Method of manufacturing nano fiber Download PDF

Info

Publication number
KR100762255B1
KR100762255B1 KR1020060134579A KR20060134579A KR100762255B1 KR 100762255 B1 KR100762255 B1 KR 100762255B1 KR 1020060134579 A KR1020060134579 A KR 1020060134579A KR 20060134579 A KR20060134579 A KR 20060134579A KR 100762255 B1 KR100762255 B1 KR 100762255B1
Authority
KR
South Korea
Prior art keywords
polymers
polycaprolactone
average molecular
polymer
spinning solution
Prior art date
Application number
KR1020060134579A
Other languages
Korean (ko)
Inventor
이성준
이세근
김호영
도석주
참 김
류원석
Original Assignee
(재)대구경북과학기술연구원
영남대학교 산학협력단
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 (재)대구경북과학기술연구원, 영남대학교 산학협력단 filed Critical (재)대구경북과학기술연구원
Priority to KR1020060134579A priority Critical patent/KR100762255B1/en
Application granted granted Critical
Publication of KR100762255B1 publication Critical patent/KR100762255B1/en

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones

Abstract

A method for manufacturing nanofiber is provided to produce a nonwoven fabric formed of continued nanofiber without beads, by mixing and spinning polymers having the same molecular structure and different molecular weights. A spinning solution is formed by mixing and dissolving a plurality of polymers in a solvent, wherein the polymers have the same molecular structure and different molecular weights(S110). The spinning solution is electro-spun and enriched to prepare nanofiber(S120). Each of the polymers has a weight percents of at least 10%, based on the total weight of the polymers. The plurality of polymers are polycaprolactone substances having different molecular weights.

Description

나노섬유의 제조 방법{Method of manufacturing nano fiber}Method of manufacturing nano fiber

도 1은 본 발명에 따른 나노섬유 제조 방법을 나타내는 순서도이다.1 is a flow chart showing a nanofiber manufacturing method according to the present invention.

도 2는 실시예 1로 제조한 부직포의 전자현미경 사진이다.2 is an electron micrograph of the nonwoven fabric prepared in Example 1. FIG.

도 3은 실시예 2로 제조한 부직포의 전자현미경 사진이다.3 is an electron micrograph of the nonwoven fabric prepared in Example 2. FIG.

도 4는 실시예 3로 제조한 부직포의 전자현미경 사진이다.4 is an electron micrograph of the nonwoven fabric prepared in Example 3. FIG.

도 5는 비교예 1로 제조한 부직포의 전자현미경 사진이다.5 is an electron micrograph of a nonwoven fabric prepared in Comparative Example 1. FIG.

도 6은 비교예 2로 제조한 부직포의 전자현미경 사진이다.6 is an electron micrograph of a nonwoven fabric prepared in Comparative Example 2. FIG.

도 7은 다양한 중량비를 가지는 방사용액의 상대점도를 나타낸 그래프이다.7 is a graph showing the relative viscosity of the spinning solution having various weight ratios.

본 발명은 전기방사를 통해 나노섬유를 제조하는 방법에 관한 것으로, 더욱 상세하게는 이종의 분자량을 가지는 동종의 고분자를 혼합 방사하여 섬유직경이 제어된 나노 섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing nanofibers by electrospinning, and more particularly, to a method for producing nanofibers in which fiber diameter is controlled by mixing and spinning a homogeneous polymer having different molecular weights.

일반적으로 나노섬유를 제조하기 위한 전기방사장치는 기본적으로 고분자 용액이 이송되는 노즐과 전압인가장치 장치 및 수집부(Collector)로 구성된다. 노즐을 빠져나온 고분자 용액은 노즐 끝에서 액적을 형성하게 되는데, 이때 노즐과 수 집부 사이에 고전압의 전기장을 걸어주면 액적은 인장 변형되어 테일러콘(원뿔형의 액적)을 형성하게 되고 충분히 높은 전압 하에서는 테일러콘의 끝에서 얇은 섬유 형태로 방사된다. In general, an electrospinning apparatus for manufacturing nanofibers basically includes a nozzle, a voltage applying device device, and a collector, through which a polymer solution is transferred. The polymer solution exiting the nozzle forms droplets at the tip of the nozzle. When a high voltage electric field is applied between the nozzle and the collector, the droplets are tensilely deformed to form a Taylor cone (conical droplet) at a sufficiently high voltage. At the ends of the cones are spun into thin fibers.

이때, 분자량이 작은 고분자용액인 경우에는 연속된 섬유상이 형성되지 않고 전하를 띤 액적이 형성되어 나노섬유 부직포를 얻을 수가 없다. 또한, 섬유상을 형성 할 수 있는 일정 분자량을 가지는 고분자용액의 경우에도 충분한 농도 이하에서는 고분자 사슬의 엉킴이 충분치 않아 비드가 없는 연속된 섬유상을 얻기가 용이하지 않다. At this time, in the case of a polymer solution having a low molecular weight, continuous fibrous phases are not formed and charged droplets are formed, and thus a nanofiber nonwoven fabric cannot be obtained. In addition, even in the case of a polymer solution having a constant molecular weight capable of forming a fibrous phase, it is not easy to obtain a continuous fibrous without beads due to insufficient entanglement of the polymer chains at a sufficient concentration or less.

이러한 이유로 고분자용액의 전기방사에서는 비드가 없는 연속된 섬유상을 얻기 위해 사슬의 엉킴이 충분하게 일어나는 최적의 성막농도 이상에서 방사를 실시하게 되는데, 이때, 예를 들어 폴리카프로락톤의 경우, 최적의 성막농도 이상에서 방사를 실시했을 때 고분자용액의 표면 장력이 낮아 전기방사시 조건을 제어해도 원하는 미세 직경을 가지는 섬유상을 얻기가 힘든 경우가 발생하게 된다. For this reason, in the electrospinning of the polymer solution, spinning is carried out above the optimum deposition concentration in which chain entanglement is sufficient to obtain a continuous fiber without beads. For example, in the case of polycaprolactone, optimal deposition is performed. When the spinning is carried out at a concentration or higher, the surface tension of the polymer solution is low, so that even when the conditions for the electrospinning are controlled, it is difficult to obtain a fibrous shape having a desired fine diameter.

이러한 단점을 극복하기 위해 대한민국 공개특허 10-2001-0003685호에는 테일러 콘에서 초기에 나오는 스트림의 굵기가 굵더라도 용매의 휘발도를 증가시켜 스트림의 직경을 급속하게 감소시키거나, 고분자의 농도를 크게 낮추지 않는 범위에서 고분자용액의 점도를 낮추면 토출량을 증가시키면서도 제조되는 고분자웹을 형성하는 섬유의 굵기를 증가시키지 않고 원하는 굵기의 섬유상을 가진 고분자 나노부직포를 제조하는 방법에 대한 것이 개시되어 있다.In order to overcome this drawback, Korean Patent Laid-Open Publication No. 10-2001-0003685 discloses that although the initial thickness of the stream in the Taylor cone is large, the volatilization of the solvent is increased to rapidly reduce the diameter of the stream or to increase the concentration of the polymer. A method for producing a polymer nanononwoven fabric having a fibrous fiber having a desired thickness without increasing the thickness of the fibers forming the polymer web produced while increasing the discharge amount by lowering the viscosity of the polymer solution in a range not lowering is disclosed.

상기에 따르면, 고분자용매의 온도가 40℃에서 용매의 비등점 이하의 온도 범위를 갖는 고분자 용액을 이용하여 고분자 미세 섬유상을 가지는 나노섬유를 제조하는 방법이 기재되어 있으나, 휘발성이 우수한 용매의 선정 및 대상 고분자의 범용성이 떨어지는 문제점이 있다. According to the above, a method for producing nanofibers having a polymer microfiber phase using a polymer solution having a temperature range of 40 ° C. or less below the boiling point of the solvent has been described. There is a problem that the versatility of the polymer is poor.

본 발명이 이루고자 하는 기술적 과제는 고분자의 고유특성을 변화시키지 않기 위해 이종의 분자량을 가지는 동종의 고분자를 혼합 방사함으로써, 비드(bead)가 없는 연속된 나노섬유로 구성된 부직포를 제조할 수 있는 나노섬유 제조 방법을 제공하는데 있다.The technical problem to be achieved by the present invention is to make a non-woven fabric consisting of a continuous nanofiber without beads by mixing and spinning a homogeneous polymer having a heterogeneous molecular weight in order not to change the intrinsic properties of the polymer It is to provide a manufacturing method.

상기 기술적 과제를 이루기 위한 본 발명에 따른 나노섬유 제조 방법은 방사 용액 형성 단계 및 방사 및 집적 단계를 구비한다. Nanofiber manufacturing method according to the present invention for achieving the above technical problem comprises a spinning solution forming step and spinning and integration step.

상기 방사 용액 형성 단계에서는 동일한 분자 구조를 가지면서 무게평균 분자량이 상이한 복수의 고분자를 용매에 혼합 용해하여 방사 용액을 형성한다. 상기 방사 및 집적 단계에서는 상기 형성된 방사 용액을 전기방사하여 집적한다.In the spinning solution forming step, a plurality of polymers having the same molecular structure and different weight average molecular weight are mixed and dissolved in a solvent to form a spinning solution. In the spinning and integration step, the formed spinning solution is electrospun and integrated.

이하에서는 본 발명의 구체적인 실시예를 도면을 참조하여 상세히 설명하도록 한다.Hereinafter, specific embodiments of the present invention will be described in detail with reference to the accompanying drawings.

도 1은 본 발명에 따른 나노섬유 제조 방법의 일실시예(100)를 나타내는 것으로서, 방사용액 형성 단계(S110) 및 방사 및 집적 단계(S120)를 구비한다.1 shows an embodiment 100 of a method for manufacturing a nanofiber according to the present invention, and includes a spinning solution forming step (S110) and a spinning and integration step (S120).

방사용액 형성 단계(S110)에서는 나노섬유를 제조하기 위한 고분자 용질이 용매에 용해된 방사용액을 형성한다.In the spinning solution forming step (S110), a polymer solute for preparing nanofibers forms a spinning solution dissolved in a solvent.

본 발명에서는 방사용액의 고분자 용질로서, 예를 들어, 무게평균 분자량이 10,000인 폴리카프로락톤(polycaprolactone)과 무게평균 분자량이 80,000인 폴리카프로락톤과 같이, 동일한 분자 구조를 가지면서 무게평균 분자량이 상이한 복수의 고분자(polymer) 즉, 동종이면서 무게평균 분자량이 이종인 복수의 고분자를 이용한다.In the present invention, as the polymer solute of the spinning solution, for example, polycaprolactone having a weight average molecular weight of 10,000 and polycaprolactone having a weight average molecular weight of 80,000, have the same molecular structure and different weight average molecular weights. A plurality of polymers, that is, a plurality of polymers of the same kind and weight average molecular weight are heterogeneous.

연속된 섬유상을 얻고, 또한 고분사 사슬의 엉킴이 충분히 일어나기 위해서는 무게평균 분자량이 상대적으로 큰 고분자와 무게평균 분자량이 상대적으로 작은 고분자가 적절히 혼합되어야 한다. 따라서, 복수의 고분자 각각은 복수의 고분자 전체 중량에 대하여 적어도 10%의 중량비를 가지는 것이 바람직하다. 예를 들어, 저분자량의 폴리카프로락톤과 중분자량의 폴리카프로락톤이 용질로 이용된다면, 저분자량 폴리카프로락톤의 중량비가 10% ~ 90% 라면, 중분자량 폴리카프로락톤의 중량비는 90% ~ 10%가 된다.In order to obtain a continuous fibrous form and to sufficiently entangle the high-injection chain, a polymer having a relatively large weight average molecular weight and a polymer having a relatively small weight average molecular weight must be mixed properly. Therefore, each of the plurality of polymers preferably has a weight ratio of at least 10% to the total weight of the plurality of polymers. For example, if low molecular weight polycaprolactone and medium molecular weight polycaprolactone are used as the solute, if the weight ratio of low molecular weight polycaprolactone is 10% to 90%, the weight ratio of medium molecular weight polycaprolactone is 90% to 10 Will be%.

고분자 용질의 종류로는 이미 예시한 폴리카프로락톤 외에도 폴리비닐알코올, 폴리에틸렌옥사이드, 폴리에틸렌글리콜, 폴리락트산, 폴리글리콜산, 폴리 D,L-락트산-글리콜산 공중합체의 폴리에스테르, 폴리(발레로락톤), 폴리(하이드록시부티레이트), 폴리(하이드록시발러레이트)와 같은 합성고분자군에서 선택된 어느 하나의 종류일 수 있고, 콜라겐(collagen), 젤라틴(gelatin), 알기네이트(Alginate), 알긴산(alginic acid), 히알루론산(hyaluronic acid), 키틴(chitin), 키토산(Chitosan)과 같은 천연고분자군에서 선택된 어느 하나의 종류일 수 있다.The polymer solutes include polyvinyl alcohol, polyethylene oxide, polyethylene glycol, polylactic acid, polyglycolic acid, polyester of poly D, L-lactic acid-glycolic acid copolymer, poly (valerolactone) ), Poly (hydroxybutyrate), poly (hydroxy valerate) may be any one selected from the group of synthetic polymers, such as collagen (collagen), gelatin (gelatin), alginate, alginic (alginic) acid), hyaluronic acid (hyaluronic acid), chitin (chitin), chitosan (chitosan) may be any one type selected from the group of natural polymers.

용매로는 클로로포름(Chloroform)과 에탄올(Ethanol)의 혼합액을 이용할 수 있으며, 방사용액 형성 단계(S110)에서 형성된 방사 용액에는 데시리터(dl)당 고분자 성분이 10g 정도 포함할 수 있다.As a solvent, a mixed solution of chloroform and ethanol may be used, and the spinning solution formed in the spinning solution forming step S110 may include about 10 g of a polymer component per deciliter (dl).

방사 및 집적 단계(S120)에서는 상기 방사용액 형성 단계(S110)에서 형성된 방사 용액을 전기방사장치의 전압이 걸려있는 노즐을 통해 전기방사하여 수집부(Collector)에 집적한다.In the spinning and integration step (S120), the spinning solution formed in the spinning solution forming step (S110) is electrospun through a nozzle on which the voltage of the electrospinning device is applied and integrated in the collector.

전기방사는 전기방사의 효과를 높이기 위해 전기방사장치의 노즐에 10kV 이상의 충분한 전압을 인가하는 것이 바람직하다.Electrospinning is preferably applied to the nozzle of the electrospinning apparatus a sufficient voltage of 10kV or more to enhance the effect of electrospinning.

수집부에 집적된 나노섬유의 상태는 부직포의 상태가 된다. The state of the nanofibers accumulated in the collecting portion becomes the state of the nonwoven fabric.

다음은 본 발명의 실시예를 통하여 발명의 효과를 실험적으로 살펴보고자 한다. 이하, 구체적인 실시예 및 비교예를 가지고 본 발명의 효과를 상세히 설명하지만, 이들 실시예는 단지 본 발명을 명확하게 이해시키기 위한 것일 뿐 본 발명의 범위를 한정하고자 하는 것은 아니다. The following is to examine the effects of the invention experimentally through the embodiment of the present invention. Hereinafter, the effects of the present invention will be described in detail with specific examples and comparative examples, but these examples are only intended to clearly understand the present invention and are not intended to limit the scope of the present invention.

실시예Example 1 One

무게평균 분자량이 10,000과 80,000인 폴리카프로락톤을 70% : 30%의 중량비로 혼합한 다음, 부피비가 75% : 25%인 클로로포름과 에탄올의 혼합용매에 용해하여 고형성분이 10 g/dl인 방사용액을 제조한 후 전기방사하여 수집부상에 집적시켜 부직포를 형성한다. 전기방사시 전기방사장치의 노즐에 인가되는 전압은 20kV이다. A polycaprolactone having a weight average molecular weight of 10,000 and 80,000 was mixed in a weight ratio of 70%: 30%, and then dissolved in a mixed solvent of chloroform and ethanol having a volume ratio of 75%: 25%, and having a solid component of 10 g / dl. After the use solution is prepared, it is electrospun and accumulated on a collecting part to form a nonwoven fabric. During electrospinning, the voltage applied to the nozzle of the electrospinning apparatus is 20 kV.

실시예 1에 의해 제조된 부직포의 전자현미경 사진은 도 2와 같다. An electron micrograph of the nonwoven fabric prepared in Example 1 is shown in FIG. 2.

실시예Example 2 2

무게평균 분자량이 10,000과 80,000인 폴리카프로락톤을 50% : 50%의 중량비 로 혼합한 다음, 부피비가 75% : 25%인 클로로포름과 에탄올의 혼합용매에 용해하여 고형성분이 10 g/dl 인 방사용액을 제조한 후 전기방사하여 수집부상에 집적시켜 부직포를 형성한다. 전기방사시 전기방사장치의 노즐에 인가되는 전압은 20kV이다. Polycaprolactone having a weight average molecular weight of 10,000 and 80,000 was mixed in a weight ratio of 50%: 50%, and then dissolved in a mixed solvent of chloroform and ethanol having a volume ratio of 75%: 25%, and having a solid component of 10 g / dl. After the use solution is prepared, it is electrospun and accumulated on a collecting part to form a nonwoven fabric. During electrospinning, the voltage applied to the nozzle of the electrospinning apparatus is 20 kV.

실시예 2에 의해 제조된 부직포의 전자현미경 사진은 도 3과 같다.An electron micrograph of the nonwoven fabric prepared in Example 2 is shown in FIG. 3.

실시예Example 3 3

무게평균 분자량이 10,000과 80,000인 폴리카프로락톤을 30% : 70%의 중량비로 혼합한 다음, 부피비가 75% : 25%인 클로로포름과 에탄올의 혼합용매에 용해하여 고형성분이 10 g/dl 인 방사용액을 제조한 후 전기방사하여 수집부상에 집적시켜 부직포를 형성한다. 전기방사시 전기방사장치의 노즐에 인가되는 전압은 20kV이다. Polycaprolactone having a weight average molecular weight of 10,000 and 80,000 is mixed in a weight ratio of 30%: 70%, and then dissolved in a mixed solvent of chloroform and ethanol having a volume ratio of 75%: 25%, and having a solid component of 10 g / dl. After the use solution is prepared, it is electrospun and accumulated on a collecting part to form a nonwoven fabric. During electrospinning, the voltage applied to the nozzle of the electrospinning apparatus is 20 kV.

실시예 3에 의해 제조된 부직포의 전자현미경 사진은 도 4와 같다.An electron micrograph of the nonwoven fabric prepared in Example 3 is as shown in FIG. 4.

도 2 내지 도 4를 참조하면, 실시예 1 내지 실시예 3에 의해 제조된 부직포는 미세 직경을 가지는 섬유상들이 서로 엉켜있는 것을 알 수 있다.2 to 4, it can be seen that the nonwoven fabrics prepared according to Examples 1 to 3 are entangled with each other in the form of fibrous fibers having a fine diameter.

비교예Comparative example 1 One

무게평균 분자량이 10,000인 폴리카프로락톤을 부피비가 75% : 25%인 클로로포름과 에탄올의 혼합용매에 용해하여 고형성분이 10 g/dl 인 방사용액을 제조한 후 전기방사하여 수집부상에 집적시켜 부직포를 형성한다. 전기방사시 전기방사장치의 노즐에 인가되는 전압은 20kV이다. Polycaprolactone having a weight average molecular weight of 10,000 was dissolved in a mixed solvent of chloroform and ethanol having a volume ratio of 75%: 25% to prepare a spinning solution having a solid component of 10 g / dl, followed by electrospinning to be integrated on a collecting part for nonwoven fabric. To form. During electrospinning, the voltage applied to the nozzle of the electrospinning apparatus is 20 kV.

비교예 1에 의해 제조된 부직포의 전자현미경 사진은 도 5와 같다. 도 5를 참조하면, 무게평균 분자량이 10,000인 폴리카프로락톤만을 고분자 용질로 이용할 경우, 섬유상이 형성되지 않고 전하를 띤 액적이 형성되어 있는 것을 알 수 있다.An electron micrograph of the nonwoven fabric prepared in Comparative Example 1 is as shown in FIG. 5. Referring to FIG. 5, when only polycaprolactone having a weight average molecular weight of 10,000 is used as the polymer solute, it can be seen that a charged droplet is formed without forming a fibrous form.

비교예Comparative example 2 2

무게평균분자량이 80,000인 폴리카프로락톤을 부피비가 75% : 25%인 클로로포름과 에탄올의 혼합용매에 용해하여 고형성분이 10 g/dl 인 방사용액을 제조한 후 전기방사하여 수집부상에 집적시켜 부직포를 형성한다. 전기방사시 전기방사장치의 노즐에 인가되는 전압은 20kV이다. Polycaprolactone having a weight average molecular weight of 80,000 was dissolved in a mixed solvent of chloroform and ethanol with a volume ratio of 75%: 25% to prepare a spinning solution having a solid component of 10 g / dl, and then electrospun and integrated onto a collecting part for nonwoven fabric. To form. During electrospinning, the voltage applied to the nozzle of the electrospinning apparatus is 20 kV.

비교예 2에 의해 제조된 부직포의 전자현미경 사진은 도 6과 같다. 도 6을 참조하면, 무게평균 분자량이 80,000인 폴리카프로락톤만을 고분자 용질로 이용할 경우, 섬유상이 형성되었으나, 미세하지 않은 섬유상임을 알 수 있다.An electron micrograph of the nonwoven fabric prepared in Comparative Example 2 is as shown in FIG. 6. Referring to FIG. 6, when only polycaprolactone having a weight average molecular weight of 80,000 is used as the polymer solute, it can be seen that the fibrous form is formed, but the fibrous form is not fine.

도 7은 실시예 1 내지 실시예 3과 비교예 1 및 비교예 2에 이용되는 방사용액의 상대점도를 참고적으로 나타낸 그래프로서, 우벨로드 점도계로 측정된 것이다. 7 is a graph showing the relative viscosity of the spinning solution used in Examples 1 to 3 and Comparative Examples 1 and 2 as a reference, which is measured by a Ubelrod viscometer.

도 7을 참조하면, 무게평균 분자량이 10,000인 폴리카프로락톤와 무게평균 분자량이 80,000인 폴리카프로락톤의 중량비에 따라 상대점도가 다르다는 것을 알 수 있다. 무게평균 분자량 10,000인 폴리카프로락톤의 중량비가 클수록 상대점도는 낮으며, 반대로 무게평균 분자량의 80,000인 폴리카프로락톤의 중량비가 클수록 상대점도는 높은 것을 알 수 있다. Referring to Figure 7, it can be seen that the relative viscosity is different depending on the weight ratio of polycaprolactone having a weight average molecular weight of 10,000 and polycaprolactone having a weight average molecular weight of 80,000. The larger the weight ratio of polycaprolactone having a weight average molecular weight of 10,000, the lower the relative viscosity. On the contrary, the higher the weight ratio of polycaprolactone having a weight average molecular weight of 80,000, the higher the relative viscosity.

따라서, 동일한 종류의 고분자라도 무게평균 분자량이 서로 다른 것들을 적절히 혼합하면 원하는 점도를 얻을 수 있다. Therefore, even if the same type of polymer, the desired viscosity can be obtained by appropriately mixing different weight average molecular weights.

이상에서 본 발명에 대한 기술사상을 첨부 도면과 함께 서술하였지만 이는 본 발명의 바람직한 실시예를 예시적으로 설명한 것이지 본 발명을 한정하는 것은 아니다. 또한 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자라면 누구나 본 발명의 기술적 사상의 범주를 이탈하지 않는 범위 내에서 다양한 변형 및 모방이 가능함은 명백한 사실이다.The technical spirit of the present invention has been described above with reference to the accompanying drawings. However, the present invention has been described by way of example only, and is not intended to limit the present invention. In addition, it is apparent that any person having ordinary knowledge in the technical field to which the present invention belongs may make various modifications and imitations without departing from the scope of the technical idea of the present invention.

상술한 바와 같이, 본 발명에 따른 나노섬유 제조 방법은 이종의 분자량을 가지는 동종의 고분자를 혼합하여 방사함으로써, 고분자가 가지는 고유한 특성을 변화시키지 않고 효과적으로 섬유직경이 제어된 나노섬유를 제조할 수 있다. As described above, the nanofiber manufacturing method according to the present invention by mixing and spinning a homogeneous polymer having a heterogeneous molecular weight, it is possible to effectively produce a nanofiber with a controlled fiber diameter without changing the unique properties of the polymer have.

또한, 본 발명에 따른 나노섬유 제조 방법은 공정이 단순하고, 다양한 고분자 미세섬유상을 갖는 나노섬유를 제조할 수 있는 장점이 있다.In addition, the nanofiber manufacturing method according to the present invention has the advantage that the process is simple, and can produce nanofibers having a variety of polymer microfiber phase.

Claims (5)

전기방사를 통해 나노섬유를 제조하는 방법에 있어서,In the method for producing nanofibers by electrospinning, (a)동일한 분자 구조를 가지면서 무게평균 분자량이 상이한 복수의 고분자를 용매에 혼합 용해하여 방사 용액을 형성하는 단계; 및(a) mixing and dissolving a plurality of polymers having the same molecular structure and different weight average molecular weight in a solvent to form a spinning solution; And (b)상기 형성된 방사 용액을 전기방사하여 집적하는 단계를 구비하는 것을 특징으로 하는 나노섬유 제조 방법.(b) electrospinning the formed spinning solution to integrate. 제1항에 있어서, 상기 복수의 고분자 각각은,The method of claim 1, wherein each of the plurality of polymers, 복수의 고분자 전체 중량에 대하여, 적어도 10%의 중량비를 가지는 것을 특징으로 하는 나노섬유 제조 방법. Method for producing a nanofiber, characterized in that having a weight ratio of at least 10% to the total weight of the plurality of polymers. 제1항에 있어서, 상기 복수의 고분자는, The method of claim 1, wherein the plurality of polymers, 무게평균 분자량이 상이한 폴리카프로락톤(polycaprolactone)들인 것을 특징으로 하는 나노섬유 제조 방법.A method for producing nanofibers, characterized in that polycaprolactones having different weight average molecular weights. 제3항에 있어서, 상기 용매는, The method of claim 3, wherein the solvent, 클로로포름(Chloroform)과 에탄올(Ethanol)의 혼합액인 것을 특징으로 하는 나노섬유 제조 방법.Method for producing nanofibers, characterized in that the mixture of chloroform (Chloroform) and ethanol (Ethanol). 제3항에 있어서, 상기 폴리카프로락톤(polycaprolactone)은, According to claim 3, wherein the polycaprolactone (polycaprolactone), 폴리비닐알코올, 폴리에틸렌옥사이드, 폴리에틸렌글리콜, 폴리락트산, 폴리글리콜산, 폴리 D,L-락트산-글리콜산 공중합체의 폴리에스테르, 폴리(발레로락톤), 폴리(하이드록시부티레이트), 폴리(하이드록시발러레이트), 콜라겐, 젤라틴, 알기네이트, 알긴산, 히알루론산, 키틴 및 키토산으로 이루어진 그룹 중 선택된 어느 하나로 대체할 수 있는 것을 특징으로 하는 나노섬유 제조 방법.Polyvinyl alcohol, polyethylene oxide, polyethylene glycol, polylactic acid, polyglycolic acid, polyester of poly D, L-lactic acid-glycolic acid copolymer, poly (valerolactone), poly (hydroxybutyrate), poly (hydroxy Valorate), collagen, gelatin, alginate, alginic acid, hyaluronic acid, chitin and chitosan can be replaced with any one selected from the group consisting of nanofibers manufacturing method.
KR1020060134579A 2006-12-27 2006-12-27 Method of manufacturing nano fiber KR100762255B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020060134579A KR100762255B1 (en) 2006-12-27 2006-12-27 Method of manufacturing nano fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020060134579A KR100762255B1 (en) 2006-12-27 2006-12-27 Method of manufacturing nano fiber

Publications (1)

Publication Number Publication Date
KR100762255B1 true KR100762255B1 (en) 2007-10-04

Family

ID=39418759

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020060134579A KR100762255B1 (en) 2006-12-27 2006-12-27 Method of manufacturing nano fiber

Country Status (1)

Country Link
KR (1) KR100762255B1 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100926678B1 (en) 2007-12-17 2009-11-17 재단법인대구경북과학기술원 Biodegradable plastic / nano fiber composite support neural conduit manufacturing method.
CN111793900A (en) * 2020-06-15 2020-10-20 中国人民解放军陆军特色医学中心 Chitosan/polycaprolactone composite nanofiber membrane material and application thereof
EP3822402A4 (en) * 2018-07-09 2022-07-27 National Institute for Materials Science Nonwoven fabric, method for manufacturing same, and composition for electrospinning

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060048009A (en) * 2004-06-17 2006-05-18 한국화학연구원 Filament bundle type nano fiber and manufacturing method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060048009A (en) * 2004-06-17 2006-05-18 한국화학연구원 Filament bundle type nano fiber and manufacturing method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100926678B1 (en) 2007-12-17 2009-11-17 재단법인대구경북과학기술원 Biodegradable plastic / nano fiber composite support neural conduit manufacturing method.
EP3822402A4 (en) * 2018-07-09 2022-07-27 National Institute for Materials Science Nonwoven fabric, method for manufacturing same, and composition for electrospinning
JP7391306B2 (en) 2018-07-09 2023-12-05 国立研究開発法人物質・材料研究機構 Nonwoven fabric, method for producing nonwoven fabric, and composition for electrospinning
IL279785B1 (en) * 2018-07-09 2024-04-01 Nat Inst Materials Science Nonwoven fabric, method for manufacturing same, and composition for electrospinning
CN111793900A (en) * 2020-06-15 2020-10-20 中国人民解放军陆军特色医学中心 Chitosan/polycaprolactone composite nanofiber membrane material and application thereof

Similar Documents

Publication Publication Date Title
Almetwally et al. Technology of nano-fibers: Production techniques and properties-Critical review
Khajavi et al. Controlling nanofiber morphology by the electrospinning process
Zhou et al. Manufacturing technologies of polymeric nanofibres and nanofibre yarns
Kanani et al. Effect of changing solvents on poly (ε-caprolactone) nanofibrous webs morphology
KR101519169B1 (en) Production of nanofibers by melt spinning
Li et al. Hierarchically structured PMMA fibers fabricated by electrospinning
EP1957256B1 (en) Method of solution preparation of polyolefin class polymers for electrospinning processing included
AK S et al. Fabrication of poly (Caprolactone) nanofibers by electrospinning
Spasova et al. Perspectives on: criteria for complex evaluation of the morphology and alignment of electrospun polymer nanofibers
KR20040076006A (en) A process of preparing continuous filament composed of nano fiber
WO2005033381A2 (en) Electro-blowing technology for fabrication of fibrous articles and its applications of hyaluronan
JP2002249966A (en) Method for producing fine fibrous polymeric web
Gholipour Kanani et al. Effect of Changing Solvents on Poly (ϵ-Caprolactone) Nanofibrous Webs Morphology.
WO2007111477A1 (en) Method of manufacturing nanofiber web
Mîndru et al. Morphological aspects of polymer fiber mats obtained by air flow rotary-jet spinning
CN101538776A (en) Coaxial polyphosphazene nanofiber composite membrane and preparation method thereof
KR100762255B1 (en) Method of manufacturing nano fiber
Jeun et al. Electrospinning of Poly (L-lactide-co-D, L-lactide)
KR101118081B1 (en) Method of manufacturing nanofiber web
JP2007084946A (en) Splittable conjugate fiber
CN110747521A (en) Three-dimensional electrostatic spinning micro-fiber scaffold with surface nano-structure and preparation method and application thereof
JP7176850B2 (en) Sea-island composite fiber bundle
KR101118079B1 (en) Method of manufacturing nanofiber web
R Jabur et al. Ambient temperature affect the pore size of PVA nanofibers tissues
CN102926135A (en) Biodegradable composite superfine fiber non-woven fabric and preparation method thereof

Legal Events

Date Code Title Description
A201 Request for examination
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20130621

Year of fee payment: 7

FPAY Annual fee payment

Payment date: 20140703

Year of fee payment: 8

FPAY Annual fee payment

Payment date: 20150601

Year of fee payment: 9

FPAY Annual fee payment

Payment date: 20171011

Year of fee payment: 11

FPAY Annual fee payment

Payment date: 20190701

Year of fee payment: 13