KR101243846B1 - Preparation method of superfine pitch fiber - Google Patents
Preparation method of superfine pitch fiber Download PDFInfo
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- KR101243846B1 KR101243846B1 KR1020050128196A KR20050128196A KR101243846B1 KR 101243846 B1 KR101243846 B1 KR 101243846B1 KR 1020050128196 A KR1020050128196 A KR 1020050128196A KR 20050128196 A KR20050128196 A KR 20050128196A KR 101243846 B1 KR101243846 B1 KR 101243846B1
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- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
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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
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2101/00—Inorganic fibres
- D10B2101/10—Inorganic fibres based on non-oxides other than metals
- D10B2101/12—Carbon; Pitch
- D10B2101/122—Nanocarbons
Abstract
본 발명은 초미세 핏치섬유의 제조방법에 관한 것으로서, The present invention relates to a method for producing ultra fine pitch fibers,
핏치섬유의 제조방법에 있어서, 테트라하이드로푸란과, 테트라하이드로푸란의 중량에 대하여 0.1∼20중량%의 퀴놀린의 혼합용제 용액에 등방성 핏치를 용해한 용액을 전기방사방법으로 방사하는 것을 특징으로 하며, A method of producing pitch fibers, characterized in that the solution of isotropic pitch dissolved in a mixed solvent solution of tetrahydrofuran and quinoline in an amount of 0.1 to 20% by weight based on the weight of tetrahydrofuran is characterized by spinning by electrospinning method,
테트라하이드로푸란과 퀴놀린의 혼합용제 용액에 등방성 핏치를 용해한 용액을 전기방사방법으로 방사하여, 직경이 1㎛ 이하인 초미세 핏치섬유를 제조할 수 있고, 다양한 용도의 탄소재료의 나노전구체로서 사용이 가능하므로 제조된 핏치계 나노섬유로부터 핏치계 나노탄소섬유나 활성화에 의하여 핏치계 나노활성탄소섬유를 제조할 수 있는 효과가 있다.A solution of isotropic pitch dissolved in a mixed solvent solution of tetrahydrofuran and quinoline is spun by an electrospinning method to produce an ultrafine pitch fiber having a diameter of 1 μm or less, and can be used as a nano precursor of various carbon materials. Therefore, there is an effect that the pitch-based nano-activated carbon fibers by the pitch-based nano-carbon fibers or activation from the prepared pitch-based nanofibers.
핏치섬유, 전기방사, 퀴놀린, 탄소 Pitch Fiber, Electrospinning, Quinoline, Carbon
Description
도 1은 종래의 핏치섬유의 제조방법에 의해 제조된 핏치섬유를 나타내는 전자현미경 사진.1 is an electron micrograph showing a pitch fiber produced by a conventional method for manufacturing the pitch fiber.
도 2는 본 발명의 일실시예에 의한 초미세 핏치섬유의 제조방법에 의해 제조된 초미세 핏치섬유를 나타내는 전자현미경 사진.Figure 2 is an electron micrograph showing the ultra-fine pitch fibers prepared by the method for producing ultra-fine pitch fibers according to an embodiment of the present invention.
본 발명은 초미세 핏치섬유의 제조방법에 관한 것으로서, 보다 상세하게는 핏치의 전기방사에서 용매로서 테트라하이드로푸란(THF)과 함께 0.1∼20중량%의 퀴놀린(Quinoline) 용액을 혼합하여 사용함에 의하여 기존의 방법에 비하여 더욱 미세한 핏치섬유를 제조할 수 있는 초미세 핏치섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing ultra-fine pitch fibers, and more particularly, by mixing 0.1-20% by weight of quinoline solution with tetrahydrofuran (THF) as a solvent in the electrospinning of pitch. It relates to a method of producing ultra-fine pitch fibers that can produce a finer pitch fibers compared to the conventional method.
일반적으로 전기방사방법은 고분자물질의 미세섬유화 방법으로서 사용되고 있으며, 따라서 다양한 분자량 분포를 갖는 핏치에 있어서 이를 응용할 경우 미세 한 핏치계 섬유를 제조할 수 있으며, 핏치계 미세섬유로부터 핏치계 미세탄소섬유나 활성화에 의하여 핏치계 미세활성탄소섬유(pitch-based activated carbon fibers, ACFs)를 제조할 수 있다. In general, the electrospinning method is used as a microfibrillation method of a polymer material, and thus, when it is applied to a pitch having various molecular weight distributions, a fine pitch-based fiber can be produced, and the pitch-based microcarbon fiber or Pitch-based activated carbon fibers (ACFs) may be prepared by activation.
그러나 핏치는 일반적인 고분자물질과는 달리 다양한 물질의 혼합물로 이루어져 있으므로, 전기방사에 의한 섬유화가 용이하지 않은 특징을 가지고 있다. 따라서 핏치의 전기방사를 위하여 기존의 방법에서는 원료를 분급 등의 방법에 의하여 개질하거나 또는 혼합용매를 사용하는 방법에 의하여 전기방사를 시도하고 있었다.However, pitch is composed of a mixture of various materials, unlike the general high-molecular material, it has a feature that is not easy to fiberize by electrospinning. Therefore, in the conventional method for the electrospinning of the pitch, the electrospinning was attempted by modifying the raw materials by a classification method or by using a mixed solvent.
종래의 기술로서 공개특허공보 제2003-0020327호(2003.03.08일자)에는 전기방사에 의하여 핏치계 나노탄소섬유를 제조하는 방법에 대해 개시되어 있으며, 방사를 원활하게 하기 위하여 디메틸포름아미드(dimethyl formamide, DMF) 및 테트라하이드로푸란(tetrahydrofuran, THF) 등에 의하여 분급(Fractionation)하여 일정 수준의 분자량 분포를 갖는 핏치를 먼저 제조한 후 이를 THF 용액에 용해하여 전기방사하는 방법이 개시되어 있었다. As a conventional technique, Korean Patent Laid-Open Publication No. 2003-0020327 (Dec. 08, 2003) discloses a method for producing pitch-based nanocarbon fibers by electrospinning, and in order to facilitate spinning, dimethyl formamide , DMF), tetrahydrofuran (THF) and the like (Fraction) to produce a pitch having a certain molecular weight distribution by the first (Fraction), and then dissolving it in THF solution has been disclosed a method of electrospinning.
그러나 이 방법은 원료핏치를 먼저 분급에 의하여 제조하게 되므로, 분급된 핏치의 분자량 분포등의 물성이 분급하기 이전의 핏치와는 다르며, 번거로운 분급과정을 거치게 되는 문제점이 있었다.However, this method is manufactured by first classifying the raw material pitch, the physical properties such as the molecular weight distribution of the classified pitch is different from the pitch before classifying, there was a problem that goes through a cumbersome classification process.
또한, 공개특허공보 제2004-0097043호(2004.11.17일자)에는 30% 까지의 DMF 및 THF의 혼합용액을 이용하여 3∼6㎛ 직경의 전기방사섬유를 제조하는 방법이 개시되어 있었다. In addition, Korean Patent Laid-Open Publication No. 2004-0097043 (December 17, 2004) discloses a method for producing electrospun fibers having a diameter of 3 to 6 μm using a mixed solution of up to 30% of DMF and THF.
이 방법에 의하면 분급과정을 거치지 않으므로 공정이 단순해지지만 DMF 및 THF의 점도특성상 이보다 미세한 섬유의 제조는 곤란하다는 문제점을 가지고 있었다. According to this method, the process is simplified because it does not go through a classification process, but it is difficult to produce finer fibers due to the viscosity characteristics of DMF and THF.
또한, 핏치섬유의 직경이 소정의 크기 이하로 제조되어야 하는 경우에는 방사되는 동안에도 지속적으로 연신이 일어나야 되므로, THF만을 핏치의 용매로 사용하는 경우에는 휘발속도가 매우 빠르므로 미세한 핏치섬유의 제조가 곤란하다는 문제점도 있었다. In addition, when the diameter of the pitch fiber is to be manufactured to a predetermined size or less, the stretching must occur continuously during spinning, when using only THF as the solvent of the pitch volatilization rate is very fast, so the production of fine pitch fibers There was also a problem that was difficult.
본 발명은 상기와 같은 종래의 문제점을 해소하기 위해 안출한 것으로서, 전기방사에 있어서 핏치의 용매로서 테트라하이드로푸란(THF)과 함께 퀴놀린(Quinoline) 용액을 소량 혼합하여 사용함에 의하여 기존의 방법에 비하여 더욱 미세한 핏치섬유를 제조할 수 있는 초미세 핏치섬유의 제조방법을 제공하는 것을 그 목적으로 한다. The present invention has been made to solve the above conventional problems, compared to the conventional method by using a small amount of quinoline solution with tetrahydrofuran (THF) as a solvent of pitch in electrospinning. It is an object of the present invention to provide a method for producing ultra fine pitch fibers that can produce finer pitch fibers.
상기와 같은 목적을 달성하기 위한 본 발명은, 핏치섬유의 제조방법에 있어서, 테트라하이드로푸란 및 퀴놀린을 포함하는 혼합용제 용액을 준비하는 단계와, 상기 혼합용제 용액에 등방성 핏치를 용해한 핏치용액을 준비하는 단계와, 상기 핏치용액을 전기방사방법으로 방사하여 핏치섬유를 형성하는 단계를 포함하는 것을 특징으로 한다. 여기서, 상기 퀴놀린은 상기 혼합용제 용액의 전체 중량에 대하여 0.1~20중량%로 포함된다. The present invention for achieving the above object, in the method of manufacturing the pitch fiber, preparing a mixed solvent solution containing tetrahydrofuran and quinoline, and preparing a pitch solution in which isotropic pitch is dissolved in the mixed solvent solution And spinning the pitch solution by an electrospinning method to form pitch fibers. Here, the quinoline is contained in 0.1 to 20% by weight based on the total weight of the mixed solvent solution.
보다 바람직하게, 상기 핏치용액에는 상기 혼합용제 용액 100중량부에 대하여 상기 등방성 핏치의 중량이 30~40중량부로 포함되고, 상기 전기방사방법에서는 인가전압이 10∼45㎸인 것을 특징으로 한다.More preferably, the pitch solution contains 30 to 40 parts by weight of the isotropic pitch with respect to 100 parts by weight of the mixed solvent solution, the electrospinning method is characterized in that the applied voltage is 10 to 45 kW.
이하, 첨부도면을 참조하여 본 발명의 바람직한 일실시예를 더욱 상세히 설명한다. Hereinafter, with reference to the accompanying drawings will be described in detail a preferred embodiment of the present invention.
도 2는 본 발명의 일실시예에 의한 초미세 핏치섬유의 제조방법에 의해 제조된 초미세 핏치섬유를 나타내는 전자현미경 사진이다.Figure 2 is an electron micrograph showing the ultrafine pitch fibers produced by the method for producing an ultrafine pitch fiber according to an embodiment of the present invention.
본 실시예에 따른 초미세 핏치섬유의 제조방법은 전기방사에서 등방성 핏치를 용해하기 위한 용매로서 일반적으로 널리 사용하는 테트라하이드로푸란(tetrahydrofuran, THF)에 소정량의 퀴놀린(quinoline)을 혼합하여 사용한다. Ultrafine pitch fiber according to the present embodiment is a method for dissolving isotropic pitch in electrospinning is used by mixing a predetermined amount of quinoline (tetrahydrofuran, THF) commonly used as a solvent. .
일반적으로 휘발성이 강한 THF 만을 용매로서 사용하는 경우 전기방사되는 동안 용액의 신속한 휘발에 의하여 핏치섬유가 제조하게 된다. In general, when only volatile THF is used as a solvent, pitch fibers are prepared by rapid volatilization of the solution during electrospinning.
그러나 핏치섬유의 직경이 소정의 크기 이하로 제조되어야 하는 경우에는 방사되는 동안에도 지속적으로 연신이 일어나야 되므로 THF만을 사용하는 경우에는 휘발속도가 매우 빠르므로 미세한 섬유의 제조가 곤란하였다. 또, 퀴놀린을 용매로 사용하는 경우에는 휘발성이 너무 낮아 콜렉터에 포집된 핏치섬유중의 용매가 충분히 휘발되지 않으므로, 섬유간에 융착이 일어나서 섬유로서의 역할을 할 수 없게 된다. However, when the diameter of the pitch fiber is to be manufactured to a predetermined size or less, the stretching must occur continuously during spinning, so when using only THF volatilization rate is very fast, it was difficult to produce a fine fiber. In addition, when quinoline is used as a solvent, the volatility is so low that the solvent in the pitch fibers collected in the collector is not sufficiently volatilized, so that fusion occurs between the fibers and cannot serve as a fiber.
따라서 본 실시예에서는 전기방사에서 등방성 핏치를 용해하기 위한 혼합용제 용매로서 THF와, THF의 중량에 대해 0.1∼20중량%의 퀴놀린을 혼합하여 사용함 에 의하여 직경이 1㎛이하인 초미세 핏치섬유를 제조할 수 있게 된 것이다.Therefore, in the present embodiment, by using a mixed solvent solvent for dissolving isotropic pitch in electrospinning, THF and quinoline (0.1-20% by weight based on the weight of THF) are used to prepare ultrafine pitch fibers having a diameter of 1 μm or less. You can do it.
THF에 대한 퀴놀린의 농도는 THF의 중량에 대해 20중량%를 초과하지 않는 것이 바람직하다. 즉, 퀴놀린의 농도가 20중량%를 초과하는 경우에는 전술한 바와 같이 콜렉터에 포집된 핏치섬유중에 용매가 잔류하게 되어 계속되는 방사에 의하여 섬유간에 융착이 일어나서 섬유의 형태를 유지할 수 없게 되므로 바람직하지 않다. It is preferred that the concentration of quinoline to THF does not exceed 20% by weight relative to the weight of THF. That is, when the concentration of quinoline is more than 20% by weight, the solvent remains in the pitch fibers collected in the collector as described above, which is not preferable because the fusion occurs between the fibers due to the continuous spinning to maintain the form of the fibers. .
또한, 퀴놀린의 농도가 THF의 중량에 대해 0.1중량% 미만인 경우에는 퀴놀린의 역할이 미미하여 휘발속도가 상승하므로 이와 같은 효과를 기대하기 어렵다. 따라서 퀴놀린의 농도는 0.1∼20중량%로 적용하는 것이 바람직하며, 최적의 효과를 나타내기 위해서는 0.1∼10중량%로 적용하는 것이 더욱 바람직하다.In addition, when the concentration of quinoline is less than 0.1% by weight based on the weight of THF, the role of quinoline is insignificant, so that the volatilization rate is increased, such an effect is difficult to expect. Therefore, the concentration of quinoline is preferably applied at 0.1 to 20% by weight, and more preferably at 0.1 to 10% by weight in order to achieve the optimum effect.
본 실시예의 초미세 핏치섬유의 제조방법에 의하여 전기방사를 행하는 경우 혼합용제 용액 전체에 대한 핏치의 농도(중량비)는 30중량% 보다 작으면 핏치섬유가 방사중 절단되고, 40중량% 보다 크면 방사가 잘 이루어지지 않으므로, 30∼40중량%(즉, 혼합용제 용액 100중량부에 대하여 30~40중량부)정도가 바람직하나, 이는 핏치의 연화점이나 제조하고자 하는 핏치섬유의 직경에 따라서 적절히 가감할 필요가 있으므로 이를 제한하지는 않는다. When the electrospinning is carried out by the method of producing the ultra fine pitch fibers of the present embodiment, when the concentration (weight ratio) of the pitch is less than 30 wt% with respect to the entire mixed solvent solution, the pitch fibers are cut during spinning. Since 30 is not good, it is preferably about 30 to 40% by weight (ie, 30 to 40 parts by weight based on 100 parts by weight of the mixed solvent solution), which may be appropriately added or subtracted depending on the softening point of the pitch or the diameter of the pitch fiber to be manufactured. It does not limit it because it is necessary.
또한 인가하는 전압은 10㎸ 보다 낮으면 반응속도가 느리고, 45㎸ 보다 높으면 과부하의 위험이 있으므로 10∼45㎸의 범위로 설정하여 사용하는 것이 바람직하나, 본 발명에서는 이를 제한하지는 않는다.In addition, if the applied voltage is lower than 10 kV, the reaction rate is slow, and if the voltage is higher than 45 kV, there is a risk of overload, but it is preferable to use it in the range of 10 to 45 kV, but the present invention is not limited thereto.
이하, 본 발명의 초미세 핏치섬유 제조방법을 적용한 실시한 실시예 1과, 종래의 방법을 적용한 비교예 1에 의거해서 구체적으로 설명한다.Hereinafter, it demonstrates concretely based on Example 1 which applied the ultrafine pitch fiber manufacturing method of this invention, and the comparative example 1 which applied the conventional method.
그러나 하기의 실시예 1은 본 발명을 보다 쉽게 이해하기 위하여 제공되는 것일 뿐 본 발명이 하기의 실시예 1에 한정되는 것은 아니다. However, Example 1 below is provided only to more easily understand the present invention, and the present invention is not limited to Example 1 below.
(실시예 1)(Example 1)
THF 90중량% 및 퀴놀린 10중량%의 농도로 혼합한 혼합용매의 전체중량에 대하여 40중량%의 연화점 260℃인 석유계 등방성 핏치를 용해하여 핏치용액을 제조하였다. A pitch solution was prepared by dissolving a 40 wt% petroleum isotropic pitch having a softening point of 260 ° C. based on the total weight of the mixed solvent mixed at a concentration of 90 wt% THF and 10 wt% quinoline.
이 용액을 노즐-콜렉터간 거리 15cm, 인가전압 25㎸로 하여 전기방사하였다. 그 결과 도 2에 표시된 바와 같이 대략 0.26㎛의 직경을 갖는 초미세 핏치섬유가 제조되었다. This solution was electrospun with a nozzle-collector distance of 15 cm and an applied voltage of 25 kV. As a result, an ultra fine pitch fiber having a diameter of approximately 0.26 μm was prepared as shown in FIG. 2.
또한, 도 2의 하단에는 10개의 점으로 이루어진 치수기준이 2㎛를 나타내고 있으므로, 실시예 1의 초미세 핏치섬유의 직경이 1㎛ 이하 임을 명확하게 나타내고 있다.In addition, since the dimension reference which consists of ten points shows 2 micrometers in the lower part of FIG. 2, it shows clearly that the diameter of the ultrafine pitch fiber of Example 1 is 1 micrometer or less.
(비교예 1) (Comparative Example 1)
연화점 260℃인 석유계 등방성 핏치를 THF에 대하여 중량비로 40%를 용해하여 핏치용액을 제조하였다. A pitch solution was prepared by dissolving a petroleum-based isotropic pitch having a softening point of 260 ° C. in a weight ratio of THF.
이 용액을 노즐-콜렉터간 거리 15cm, 인가전압 25㎸로 하여 전기방사하였다. 그 결과 도 1에 표시된 바와 같이 약 5∼7㎛의 직경을 갖는 핏치섬유가 제조되었다.This solution was electrospun with a nozzle-collector distance of 15 cm and an applied voltage of 25 kV. As a result, pitch fibers having a diameter of about 5 to 7 μm were prepared as shown in FIG. 1.
또한, 도 1의 하단에는 10개의 점으로 이루어진 치수기준이 5㎛를 나타내고 있으므로, 비교예 1의 핏치섬유의 직경이 5㎛ 이상 임을 명확하게 나타내고 있다.In addition, since the dimension reference which consists of ten points shows 5 micrometers in the lower part of FIG. 1, it clearly shows that the diameter of the pitch fiber of the comparative example 1 is 5 micrometers or more.
이상 설명한 본 발명은 그 기술적 사상 또는 주요한 특징으로부터 벗어남이 없이 다른 여러 가지 형태로 실시될 수 있다. 따라서 상기 실시예는 모든 점에서 단순한 예시에 지나지 않으며 한정적으로 해석되어서는 안 된다. The present invention described above can be embodied in many other forms without departing from the spirit or main features thereof. Therefore, the above embodiments are merely examples in all respects and should not be interpreted limitedly.
이상에서 살펴본 바와 같이, 본 발명은 테트라하이드로푸란과 퀴놀린의 혼합용제 용액에 등방성 핏치를 용해한 용액을 전기방사방법으로 방사하여, 직경이 1㎛ 이하인 초미세 핏치섬유를 제조할 수 있고, 다양한 용도의 탄소재료의 나노전구체로서 사용이 가능하므로 제조된 핏치계 나노섬유로부터 핏치계 나노탄소섬유나 활성화에 의하여 핏치계 나노활성탄소섬유를 제조할 수 있는 효과가 있다.As described above, the present invention is to spin a solution in which isotropic pitch is dissolved in a mixed solvent solution of tetrahydrofuran and quinoline by the electrospinning method, to produce ultra-fine pitch fibers having a diameter of 1 μm or less, Since it can be used as a nano-precursor of the carbon material, there is an effect that can be produced from the pitch-based nano-fibers or the pitch-based nano-active carbon fibers by the activation of the pitch-based nanofibers.
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| KR20030020327A (en) * | 2003-01-15 | 2003-03-08 | 양갑승 | Preparation of pitch-based carbon nano fiber webs and activated carbon nano fiber webs by electrostatic spinning |
| KR20050014033A (en) * | 2005-01-18 | 2005-02-05 | (주) 아모센스 | Preparation method of nano-porous carbon fibers through carbonization of electrospun nano-fibers |
| KR100490832B1 (en) | 2002-09-05 | 2005-05-19 | (주)카보닉스 | Method of preparing catalyst for removal of nox |
| KR100623004B1 (en) | 2004-10-20 | 2006-09-19 | 전남대학교산학협력단 | Electrospinning of Pitch Solution Dissolved in Mixed Solvents and Preparation of Ultrafine Carbon Fiber Web and Ultraactive Carbon Fiber Web |
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| KR100490832B1 (en) | 2002-09-05 | 2005-05-19 | (주)카보닉스 | Method of preparing catalyst for removal of nox |
| KR20030020327A (en) * | 2003-01-15 | 2003-03-08 | 양갑승 | Preparation of pitch-based carbon nano fiber webs and activated carbon nano fiber webs by electrostatic spinning |
| KR100623004B1 (en) | 2004-10-20 | 2006-09-19 | 전남대학교산학협력단 | Electrospinning of Pitch Solution Dissolved in Mixed Solvents and Preparation of Ultrafine Carbon Fiber Web and Ultraactive Carbon Fiber Web |
| KR20050014033A (en) * | 2005-01-18 | 2005-02-05 | (주) 아모센스 | Preparation method of nano-porous carbon fibers through carbonization of electrospun nano-fibers |
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