KR0131835B1 - Manufacturing method of split ultra-fine fiber - Google Patents

Manufacturing method of split ultra-fine fiber

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Publication number
KR0131835B1
KR0131835B1 KR1019950018731A KR19950018731A KR0131835B1 KR 0131835 B1 KR0131835 B1 KR 0131835B1 KR 1019950018731 A KR1019950018731 A KR 1019950018731A KR 19950018731 A KR19950018731 A KR 19950018731A KR 0131835 B1 KR0131835 B1 KR 0131835B1
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South Korea
Prior art keywords
split
polyamide
weight
during
under
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KR1019950018731A
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Korean (ko)
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KR970001629A (en
Inventor
홍윤광
양광웅
오영수
이은주
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김상응
주식회사삼양사
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Priority to KR1019950018731A priority Critical patent/KR0131835B1/en
Publication of KR970001629A publication Critical patent/KR970001629A/en
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Publication of KR0131835B1 publication Critical patent/KR0131835B1/en

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144—Alcohols; Metal alcoholates
    • 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
    • D01D5/32—Side-by-side structure; Spinnerette packs therefor
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D02G3/045—Blended or other yarns or threads containing components made from different materials all components being made from artificial or synthetic material
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46—Compounds containing quaternary nitrogen atoms

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Multicomponent Fibers (AREA)

Abstract

The invention offers a method for manufacturing split pattern complex fiber without slope lines, to shorten process time by rapid and stable split during the process of split pattern complex fiber. Sodiumsulfoisophthalic acid 4.5 mole% is mixed, polymerized to terephthalic acid during polymerization; added adipe acid 2.0 mole % during the slurry process; and after an ester exchange reaction under 250 deg.C for 3 hours, a reaction under 20 deg.C for 3 hours produces an original viscosity 0.54 polyester resin. From polyamide polymerization, hexamethylenediamine 0.2 mole % is mixed to caprolactam under 5 atmospheric pressure at 255 deg.C for 24 hours, then extracted and dried producing a final relative viscosity 2.67 polyamide resin whose terminal amine is 72 per kg. Complex spinning of the produced polyester resin and polyamide resin at the ratio of 77: 23 makes a 120 denier, 48 filament, 8 split composite yarn, which is then woven to be 3/1 twill by a water jet weaving machine. Woven textile is treated during the refining process and sodium carbonate 2 w/t %, unitolsity 812 w/t %, sodium hydroxide 2.0 w/t %, 4th grade ammonium chloride 1 w/t %, and 2 phenoxy ethanol 3 w/t % added as a swelling agent to the polyamide; and treated in a rotary washer under 120 deg.C for 30 minutes for a loss rate of 23 %, and finally set for forming under 190 deg.C for 30 seconds.

Description

분할형 극세사의 제조방법Manufacturing method of split microfiber

본 발명은 분할형 극세사의 제조방법에 관한 것으로, 좀 더 구체적으로는 열가소성 폴리에스테르 수지와 폴리아미드 수지를 통상의 방법으로 복합 방사하여 얻은 8∼24개로 분할된 분할형 복합섬유를 2-페녹시에탄올에 의해 폴리아미드 부분을 팽윤시키고 동시에 알칼리 감량을 촉진시키기 위해 수산화나트륨과 침투제로 4급 암모늄염을 첨가하여 감량함으로써 빠른 시간내에 안정하면서도 균일하게 분할형 극세섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a split microfiber, and more particularly, to 2-phenoxy split type composite fiber divided into 8 to 24 pieces obtained by complex spinning a thermoplastic polyester resin and a polyamide resin in a conventional manner. The present invention relates to a method for producing a split microfiber in a stable and uniform manner in a short time by adding and reducing a quaternary ammonium salt with sodium hydroxide and a penetrating agent to swell the polyamide portion with ethanol and at the same time promote alkali reduction.

분할형 극세사의 제조방법은 분할된 섬유를 사용하여 제·편직을 실시하는 방법, 제·편직 후 복합방사한 섬유중에서 한 성분을 용출시켜 분할형 섬유를 제조하는 방법, 제·편직후 복합사를 팽윤제에 의해 팽윤시켜 분할하는 방법 등으로 크게 세가지로 나누어 볼 수 있다.The manufacturing method of the split microfiber yarn is a method of weaving and knitting using divided fibers, a method of producing a split fiber by eluting one component from the composite spun yarn after weaving and knitting, and a composite yarn after weaving and knitting. It can be divided into three types by the method of swelling and dividing with a swelling agent.

이중에서 제·편직 후 팽윤제에 의해 분할사를 제조하는 방법은 벤질 알콜, 페닐에틸알콜 등의 유화 분산액에 의해 폴리아미드 부분이 팽윤되어 분할사를 제조하는 방법으로 일본 특공소 53-35633호에 기재되어 있으나, 사용된 벤질알콜은 물에 대한 용해도가 낮기 때문에 후가공 공정에서 경사줄이 발생하는 문제점이 발생되었다.Among them, a method of manufacturing a divided yarn by a swelling agent after weaving and knitting is a method of producing a divided yarn by swelling the polyamide portion by an emulsion dispersion such as benzyl alcohol or phenylethyl alcohol. Although described, the used benzyl alcohol has a low solubility in water, causing a problem in that the oblique line occurs in the post-processing process.

또한, 분할을 용이하게 하기 위하여 알칼리 금속염과 알콜 또는 알칼리 금속염과 토금속으로된 용액에 폴리아미드 부분을 팽윤시켜 분할하는 방법이 일본특공평 2-264070호에 기재되어 있으나, 상기 화합물은 물에 대한 용해도가 낮고 온도 의존성이 높기 때문에 가공시 온도 저하에 따라 결정으로 석출되고 가공시 석출된 화합물의 재용해로 국부적인 고농도가 생겨 부분적인 강도 저하를 가져오고, 용해되지 못하는 농도에서는 섬유가 충분히 분할하지 않는 결점이 있다. 또한, 상기 용액의 수산화 나트륨을 첨가하면 폴리아미드 부분이 팽융되지 않는 문제가 발생하기 때문에 수산화나트륨의 사용은 불가능하였다.Further, in order to facilitate the division, a method of swelling and dividing a polyamide portion in a solution of an alkali metal salt and an alcohol or an alkali metal salt and an earth metal is described in Japanese Patent Application Laid-Open No. 2-264070, but the compound has a solubility in water. Because of its low temperature and high temperature dependence, it precipitates as crystals with decreasing temperature during processing, causing local high concentration due to redissolution of the precipitated compound during processing. There is a flaw. In addition, the use of sodium hydroxide was not possible because the addition of sodium hydroxide in the solution caused a problem that the polyamide portion did not swell.

또한, 일본특개평 5-117968호에는 폴리에스테르 및 폴리아미드로 이루어진 분할형 복합사의 제조시 팽윤제로 에틸렌글리콜 모노페닐에테르, 알칼리제 및 무기염을 사용하는 방법이 공지되어 있지만, 후가공시 경사불이 발생하는 단점이 있었다.In addition, Japanese Patent Laid-Open No. 5-117968 discloses a method of using ethylene glycol monophenyl ether, an alkali agent and an inorganic salt as swelling agent in the production of a split composite yarn composed of polyester and polyamide. There was a disadvantage.

따라서, 본 발명의 목적은 분할형 복합섬유의 가공시 경사줄이 발생하지 않으며 균일하고 안정하게 빠른시간내에 분할되어 가공시간을 단축시킬 수 있는 분할형 복합섬유의 제조방법을 제공하는데 있다.Accordingly, an object of the present invention is to provide a method for producing a split-type composite fiber which is not generated inclined lines during processing of the split-type composite fiber and is divided in a uniform and stable fast time to shorten the processing time.

본 발명자들은 상기의 목적을 달성하기 위하여 폴리에스테르와 폴리아미드를 통상의 방법으로 복합 방사하여 제·편직 후 폴리아미드 부분을 팽윤제로 2-페녹시에탄올을 사용하여 팽윤시킴으로써 폴리아미드 부분과 폴리에스테르 부분의 표면장력을 적게 만들고, 동시에 알칼리 감량을 촉진시키기 위해 폴리에스테르와 친화력이 우수한 침투제인 4급 암모늄염과 수산화나트륨을 첨가하여 폴리에스테르와 폴리아미드가 균일하고 안정하게 분할된 분할형 극세사를 얻을 수 있었다.In order to achieve the above object, the present inventors composite-spun polyester and polyamide in a conventional manner to swell the polyamide portion using 2-phenoxyethanol as a swelling agent after weaving and knitting. In order to reduce surface tension and promote alkali reduction, quaternary ammonium salt and sodium hydroxide, which are good penetrants with polyester, were added to obtain a split microfiber with uniform and stable division of polyester and polyamide. .

본 발명을 좀 더 구체적으로 설명하면 다음과 같다.The present invention is described in more detail as follows.

본 발명에서는 열가소성 개질 폴리에스테르와 폴리아미드를 통상의 방법으로 복합 방사하여 8∼24개로 분할된 분할형 복합사를 제조한 후, 팽윤제인 2-페녹시에탄올 1.0∼6.0중량%을 사용하고 알칼리 감량 촉진을 위해 수산화나트륨 1.0∼4.0중량%과 침투제인 4급 암모늄염을 0.5∼2중량% 첨가하여 알칼리 감량과 동시에 분할 가공을 행하여 분할형 복합섬유를 제조하였다.In the present invention, the composite-modified polyester and polyamide are spun in a conventional manner to prepare a divided composite yarn divided into 8 to 24 pieces, and then 1.0 to 6.0% by weight of 2-phenoxyethanol, which is a swelling agent, is used to reduce alkali. In order to facilitate the promotion, 1.0 to 4.0% by weight of sodium hydroxide and 0.5 to 2% by weight of a quaternary ammonium salt as a penetrant were added, and the split type fiber was prepared simultaneously with the reduction of alkali.

본 발명에서 사용된 팽윤제인 2-페녹시에탄올 침투제인 4급 암모늄염과반응공정에서 문제를 일으키지 않으며, 그 사용량은 1.0∼6.0중량%, 특히 3.0∼5.0중량%가 바람직하였다. 만일 그 사용량이 0.1중량% 미만이면 폴리아미드의 팽윤이 충분히 일어나지 않으며, 6.0중량% 초과일 경우 후가공 처리후 직물의 촉감이 나빠지고 원사의 물성이 변화되는 문제점이 있다.In the reaction process with the quaternary ammonium salt which is the 2-phenoxyethanol penetrant which is the swelling agent used in this invention, it does not cause a problem, and the usage-amount is 1.0-6.0 weight%, especially 3.0-5.0 weight%. If the amount is less than 0.1% by weight of the polyamide swelling does not occur sufficiently, if more than 6.0% by weight there is a problem that the texture of the fabric worsens after the post-treatment treatment and the physical properties of the yarn is changed.

알칼리 감량을 촉진하기 위해 사용되는 수산화나트륨의 사용량은 1.0∼4.0중량%이며 양호한 특성을 얻을 수 있었으며, 만일 그 사용량이 0.1중량% 미만인 경우 감량 및 충분한 분할을 이룰 수 없기 때문에 염색 후 염색줄이 발생하며, 4.0중량% 초과인 경우 과다한 감량에 의한 직물의 강도 저하를 초래하였다.The amount of sodium hydroxide used to promote alkali reduction was 1.0 to 4.0% by weight, and good characteristics could be obtained.If the amount is less than 0.1% by weight, dyeing lines are generated after dyeing because the weight loss and sufficient division cannot be achieved. In case of more than 4.0% by weight, the strength of the fabric was reduced due to excessive weight loss.

또한, 침투제인 4급 암모늄염은 수산화나트륨과 반응하여 감량을 촉진시키는 작용을 하며, 그 사용랑은 0.5∼2.0중량%이며, 특히 1중량% 첨가시에 가장 효과적이었다. 만일, 첨가량이 0.5중량% 미만인 경우 알칼리와 반응하는 농도가 극히 낮아 충분한 효과를 얻지 못하고, 2중량%를 초과하면 폴리에스테르 영역에 지나친 손상을 입게 되어 직물 강도가 저하되는 문제점이 있다.In addition, the quaternary ammonium salt, which is a penetrant, reacts with sodium hydroxide to promote a weight loss, and its use is 0.5 to 2.0% by weight, particularly at 1% by weight. If the added amount is less than 0.5% by weight, the concentration reacting with the alkali is extremely low to obtain a sufficient effect. If the amount is more than 2% by weight, the polyester region is excessively damaged and fabric strength is lowered.

[실시예 1]Example 1

통상의 폴리에스테르 중합 반응기에서, 테레프탈산에 소듐설포이소프탈산 4.5몰%를 혼합하여 중합하고 슬러리 제조과정에서 아디프산 2.0몰%를 첨가하고 250℃ 에서 3시간 동안 에스테르 교환반응시킨 후, 280℃ 에서 3시간 반응시켜 고유점도 0.54인 이용성 폴리에스테르 수지를 얻는다.In a conventional polyester polymerization reactor, 4.5 mol% of sodium sulfoisophthalic acid is mixed with terephthalic acid for polymerization, and 2.0 mol% of adipic acid is added in the slurry preparation process and transesterified at 250 ° C for 3 hours, and then 280 ° C. Reaction is carried out for 3 hours to obtain a water-soluble polyester resin having an inherent viscosity of 0.54.

통상의 폴리아미드 중합 반응기에서, 카프로락탐에 헥사메틸렌디아민 0.2몰%를 혼합하여 255℃, 5기압하에서 24시간 반응시킨 후, 추출 건조하여 최종 상대점도 2.67, 말단 아민기가 72meg/kg인 폴리아미드 수지를 얻는다.In a conventional polyamide polymerization reactor, 0.2 mol% of hexamethylenediamine is mixed with caprolactam and reacted at 255 DEG C at 5 atmospheres for 24 hours, followed by extraction and drying to obtain a polyamide resin having a final relative viscosity of 2.67 and a terminal amine group of 72 meg / kg. Get

상기 제조한 폴리에스테르 수지와 폴리아미드 수지를 77:23으로 복합 방사하여 120 데이나, 48 필라멘트, 8분할의 복합사를 제조한 후, 워터젯트 직기로 3/1 능직으로 제직하였다.The polyester resin and the polyamide resin prepared above were composite spun at 77:23 to prepare 120 yarns, 48 filaments, and 8-split composite yarns, and then were woven into 3/1 twill using a waterjet loom.

제직한 직물을 정련공정에서 탄산나트륨 2중량%, 정련제로 유니톨시티 812중량%, NaOH 2.0중량%, 4급 암모늄염 1중량% 및 폴리아미드에 팽윤제로 작용하는 2-페녹시에탄올 3중량%를 첨가하여 로타리 워셔에서 120℃ 의 온도로 30분 동안 처리하여 감량율이 약 23%가 되도록 하였고, 형태 고정의 위해 190℃ 에서 30초간 셋팅하였다.In the refining process, 2% by weight of sodium carbonate, 812% by weight of unitolity, 2.0% by weight of NaOH, 1% by weight of quaternary ammonium salt, and 3% by weight of 2-phenoxyethanol acting as a swelling agent to polyamide The treatment was carried out at a rotary washer at a temperature of 120 ° C. for 30 minutes to reduce the loss to approximately 23%.

이와 같이 처리한 시료를 현미경 사진으로 분할도를 확인하고 강도 및 터치감을 평가하여 그 결과를 표 1에 나타내었다.The sample treated in this way was confirmed by the micrograph, the degree of division and the strength and touch was evaluated and the results are shown in Table 1.

[비교예 1]Comparative Example 1

실시예 1과 동일한 방법으로 제조한 섬유를 정련공정에서 NaOH 0.5중량%, 2-페녹시에탄올 0.5중량%, 4급 암모늄염 0.4중량%를 첨가한 것을 제외하고 실시예 1과 동일하게 실시한 후 그 결과를 표 1에 나타내었다.The fiber prepared in the same manner as in Example 1 was subjected to the same procedure as in Example 1 except that 0.5% by weight of NaOH, 0.5% by weight of 2-phenoxyethanol, and 0.4% by weight of quaternary ammonium salt were added in the refining process. Is shown in Table 1.

[비교예 2]Comparative Example 2

실시예 1과 동일한 방법으로 제조한 섬유를 정련 공정에서 NaOH 5중량%, 2-페녹시에탄올 7중량%, 4급 암모늄염 3중량%를 첨가한 것을 제외하고 실시예 1과 동일하게 실시한 후 그 결과를 표 1에 나타내었다.The fiber prepared in the same manner as in Example 1 was subjected to the same procedure as in Example 1 except that 5% by weight of NaOH, 7% by weight of 2-phenoxyethanol, and 3% by weight of quaternary ammonium salt were added in the refining process. Is shown in Table 1.

※ 물성 측정 방법※ How to measure physical properties

1. 강도 : 직물의 인장시험법 (JIS L1068 근거)1. Strength: Tensile test method of fabric (based on JIS L1068)

2. 분할도 : 전자 현미경(SEM)에 의한 단면사진 촬영2. Segmentation: Cross-sectional photograph taken by electron microscope (SEM)

3. 터치감 : 핸들 측정기(KES-3 측정기)로 평가3. Touch feeling: evaluated by the handle measuring instrument (KES-3 measuring instrument)

Claims (4)

열가소성 개질 폴리에스테르와 폴리아미드를 통상의 방법으로 복합방사하여 8∼24개로 분할된 분할형 복합사를 제조한 후 2-페녹시에탄올, 수산화나트륨 및 4급 암모늄염을 첨가하여 알칼리 감량과 분할 공정을 실시함을 특징으로 하는 분할형 극세사의 제조방법.Composite spinning of thermoplastic modified polyester and polyamide was carried out in a conventional manner to prepare a split composite yarn divided into 8 to 24 pieces, followed by the addition of 2-phenoxyethanol, sodium hydroxide and quaternary ammonium salts to reduce alkali and split the process. Method for producing a split microfiber, characterized in that carried out. 제1항에 있어서, 2-페녹시에탄올의 사용량은 1.0∼6.0중량%임을 특징으로 하는 분할형 극세사의 제조방법.The method of claim 1, wherein the amount of 2-phenoxyethanol used is 1.0 to 6.0% by weight. 제1항에 있어서,수산화나트륨의 사용량은 1.0∼4.0중량%임을 특징으로 하는 분할형 극세사의 제조방법.The method of claim 1, wherein the amount of sodium hydroxide used is 1.0 to 4.0 wt%. 제 1 항에 있어서, 4급 암모늄염의 사용량은 0.5∼2.0중량%임을 특징으로 하는 분할형 극세사의 제조방법.The method of claim 1, wherein the quaternary ammonium salt is used in an amount of 0.5 to 2.0 wt%.
KR1019950018731A 1995-06-30 1995-06-30 Manufacturing method of split ultra-fine fiber KR0131835B1 (en)

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