KR910009704B1 - Fibrillation method of conjugated yarn - Google Patents

Fibrillation method of conjugated yarn Download PDF

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KR910009704B1
KR910009704B1 KR1019890018936A KR890018936A KR910009704B1 KR 910009704 B1 KR910009704 B1 KR 910009704B1 KR 1019890018936 A KR1019890018936 A KR 1019890018936A KR 890018936 A KR890018936 A KR 890018936A KR 910009704 B1 KR910009704 B1 KR 910009704B1
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fibrillation
composite fiber
weight
alkyl
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KR910012438A (en
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신수일
김익수
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주식회사 선경인더스트리
이승동
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/32Side-by-side structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/42Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
    • D01D5/423Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by fibrillation of films or filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The conjugated fiber of a modified polyester and a polyamide is fibrillated with 0.01-0.5 wt.% anionic surfactant of R-SO3Na [R = alkyl or alkylaryl , 0.01-0.3 wt.% alkali cpd. of M(OH)n [M = 1A or 2A family element; n = 1 or 2 , and at least 0.01 wt.% cpd. of M(CO3)n, MHCO3, (M)nSO4 or M(Cl)n [M = 1A or 2A family element; n = 1 or 2 and/or 0.1-3 wt.% carrier i.e. 2,4-dichlorophenol ether, dimethyl terephthalate, methyldichlorophenoxy acetate or N- alkylnaphthalimide deriv. The modified polyester contains 0.3- 10.0 mol % isphthalate component contg. metal sulfonate of formula (I) [R = H, C1-6 alkyl or aryl; M = alkal metal cpd. .

Description

복합섬유의 피브릴화 방법Fibrillation Method of Composite Fiber

본 발명은 개질폴리에스터와 폴리아마이드를 방사형 복합방사한 4-20분할형 복합섬유의 피브릴화 방법에 관한 것이다.The present invention relates to a fibrillation method of 4-20 split composite fibers in which radially spun composite modified polyester and polyamide.

특히 분할형 복합섬유로 제조된 직편물을 액류염색기내에서 적절한 분할제를 사용하여 직편물의 고유한 물성을 유지할 뿐만 아니라 피브릴화율을 향상시키는 방법에 관한 것이다.In particular, the present invention relates to a method for improving the fibrillation rate as well as maintaining the inherent physical properties of the knitted fabric by using an appropriate dividing agent in a liquid dyeing machine.

종래에는 폴리에스터와 폴리아마이드로 제조된 분할형 복합섬유를 피브릴화시키기 위하여 3가지 방법이 주로 사용되어 왔다.Conventionally, three methods have been mainly used to fibrillate split composite fibers made of polyester and polyamide.

첫째, 복합섬유의 한 성분을 적정한 용매로 사용하여 용해시키거나, 둘째 양성분을 기계적인 방법으로 충격등을 주어 강제로 분리시키거나, 셋째 양성분을 화학처리로 팽윤이나 수축을 일으켜 피브릴화 하였다.Firstly, one component of the composite fiber is used as a suitable solvent to dissolve it, secondly, the cationic component is forcedly separated by impact, etc., or thirdly, the cationic component is swelled or shrunk by chemical treatment, resulting in fibrillation. It was.

이러한 방법들에 대한 기존의 기술들에 대한 문제점으로 용해에 의한 방법은 20%이상의 성분을 용해함에 따른 소재의 손실 및 용제의 독성과 취급방법이 매우 주의를 요하여 분할형 복합섬유의 피브릴화 공정으로 거의 사용되지 않고 있다. 기계적인 방법에 의한 피브릴화 방법은 공정시간이 길고, 피브릴화율이 낮다는 단점을 가지고 있다.As a problem with the existing techniques for these methods, the dissolution method requires fibrillation of split composite fibers due to the loss of material caused by dissolving more than 20% of the components, the toxicity of the solvent, and the handling method. It is rarely used as a process. The fibrillation method by the mechanical method has a long process time and a low fibrillation rate.

화학처리에 의한 복합섬유를 팽윤, 수축시키는 방법은 오늘날 전기 두 방법에 의하여 광범위하게 쓰여지는데, 주로 개미산, 초산, 페놀, 벤질알콜, 베타-페놀에틸알콜, 메타-크레졸, 계면활성제, 가성소다 등을 분할제로 선택 조합하여 사용하고 있다.Swelling and shrinking of composite fibers by chemical treatment are widely used today by two methods, mainly formic acid, acetic acid, phenol, benzyl alcohol, beta-phenol ethyl alcohol, meta-cresol, surfactants, caustic soda, etc. Is selected and used as a splitting agent.

이러한 조성물로 피브릴화된 복합섬유의 직편물은 피브릴화율이 완전하지 못할뿐더러, 페놀 또는 벤질알콜의 유화용액이나 개미산을 사용할 때 폴리아마이드 부분을 용해 또는 가소화를 심하게 일으켜 직편물의 강도, 탄성회복율등을 저하시킬 뿐만 아니라 촉감을 심하게 손상시킨다. 더구나 페놀계 용제는 인체독성이 강하고, 폐수처리 공정을 필수적으로 해야하는 결점이 있었다.The fibrillated composite fibers of such a composition may not have a complete fibrillation rate, and when the emulsion or formic acid of phenol or benzyl alcohol is used, the polyamide portion may be dissolved or plasticized severely, resulting in the strength of the knitted fabric, It not only lowers the elastic recovery rate but also damages the touch badly. In addition, phenolic solvents have a strong human toxicity, and the waste water treatment process must be essential.

상기와 같은 종래의 문제점을 해결하기 위하여 본 발명은 복합섬유의 고유한 광택과 물성을 저하시키지 않는 분할제의 선정 및 조합과 함께 피브릴화 공정을 종래의 윈스, 지거, 로타리워셔, 연속수세기에서 하던 것을 액류염색기에서 진행하여 피브릴화율을 높였다.In order to solve the above conventional problems, the present invention provides a fibrillation process in the conventional wins, jiggers, rotary washers, continuous centuries with the selection and combination of splitting agents that do not degrade the inherent gloss and physical properties of the composite fiber. It was carried out in the liquid dyeing machine to increase the fibrillation rate.

특히 종래의 복합섬유 피브릴화 방법에서는 주로 폴리에스터나 폴리아마이드를 분해시키는 알칼리나 페놀유화용액을 사용함으로서 복합섬유가 가지는 고유한 물성이 저하되었다.In particular, in the conventional composite fiber fibrillation method, the inherent physical properties of the composite fiber are reduced by using an alkali or a phenol emulsion solution mainly decomposing polyester or polyamide.

따라서 본 발명에서는 분할제로 알킬소디움설포네이트 또는 알킬아릴소디움설포네이트와 미량의 알칼리 및 피브릴화 촉진제로 주기율표상의 1A 또는 2A족 원소의 염 또는 캐리어중 하나 또는 두가지를 동시에 병용하므로서 복합섬유를 구성하고 있는 폴리에스터나 폴리아마이드에 상해를 주지않고 피브릴화를 할 수 있었다.Therefore, in the present invention, a composite fiber is formed by simultaneously using one or two of alkyl sodium sulfonate or alkyl aryl sodium sulfonate as a dividing agent and a salt or a carrier of a 1A or 2A group element of the periodic table with trace alkali and fibrillation accelerators. Fibrillation was possible without harming the polyester or polyamide.

이것은 본 발명의 대상이 되는 복합섬유의 소재중 개질 폴리에스터 부분이 금속술폰산염을 함유한 이소프탈레이트 성분이 분자쇄내에 불규칙하게 존재하고 있음으로써 음이온 계면활성제중 알킬소디움술포네이트 또는 알킬아릴소디움술포네이트가 비교적 침투가 빠르고 따라서 폴리아마이드와 개질폴리에스터의 계면에서 표면장력을 저하시켜 물의 침투 및 확산을 용이하게 하여 피브릴화의 조건을 만들게 된다. 뿐만 아니라 주기율표상의 1A 또는 2A족 원소의 염도 폴리아마이드에 대하여 상기와 같은 역할에 기여할 것으로 추측되며, 캐리어는 개질폴리에스터 분자쇄를 완화하여 열수축 온도를 저하시키고 피브릴화 온도인 95℃∼98℃에서의 분자쇄 운동성을 첨가하지 않을 때보다 더 크게 일으켜 복합섬유의 구성소재인 개질폴리에스터의 팽윤 및 수축을 높여서 피브릴화 촉진시킨다. 따라서 용제에 의한 복합섬유의 팽윤 및 수축에 의한 피브릴화 방법에서 발생하는 복합섬유의 용해 및 상해를 본 발명에서는 비용제형을 분할제로 사용함으로써 복합섬유의 물성을 보존할 수 있다.This is because the isophthalate component containing the metal sulfonate in the modified polyester portion of the composite fiber material of the present invention is irregularly present in the molecular chain, and thus alkyl sodium sulfonate or alkyl aryl sodium sulfonate in the anionic surfactant. It is relatively fast to penetrate and thus lowers the surface tension at the interface between the polyamide and the modified polyester, thereby facilitating the penetration and diffusion of water to create the conditions of fibrillation. In addition, the salts of elements 1A or 2A on the periodic table are also believed to contribute to the above role for polyamides, and the carriers relax the modified polyester molecular chain to lower the heat shrinkage temperature and the fibrillation temperature of 95 ° C to 98 ° C. Molecular chain motility in Essence is greater than when not added to increase the swelling and shrinkage of the modified polyester, a component of the composite fibers to promote fibrillation. Therefore, in the present invention, dissolution and injury of the composite fiber generated in the fibrillation method by swelling and shrinking of the composite fiber by the solvent can preserve the physical properties of the composite fiber by using the non-formulation as the dividing agent.

상기의 본 발명의 구성을 보다 상세히 설명하면 다음과 같다.Referring to the configuration of the present invention in more detail as follows.

본 발명의 개질폴리에스터로는 구조식(Ⅰ)의 금속술폰산염을 함유한 이소프탈레이트 성분이 전체 디액시드의 0.3∼10.0몰퍼센트 함유된 폴리에스터 공중합체를 사용하였는데 이때 이소프탈레이트 성분이 0.3퍼센트이하일 경우에는 피브릴화가 곤란하고, 10.0퍼센트를 초과할 경우에는 제사가 곤란하다.As the modified polyester of the present invention, a polyester copolymer containing 0.3-10.0 mole percent of the total diacid in which the isophthalate component containing the metal sulfonate of formula (I) is used, wherein the isophthalate component is less than 0.3 percent Fibrillation is difficult, and when it exceeds 10.0 percent, ritual is difficult.

Figure kpo00001
Figure kpo00001

(단 R은 H 또는 탄소수 1∼6의 알킬기 또는 아릴기를 나타내고, M은 알칼리금속 화합물임)(Where R represents H or an alkyl or aryl group having 1 to 6 carbon atoms and M is an alkali metal compound)

그리고 분할제로는 구조식(Ⅱ)의 음이온계면활성제로써 예를들면 알칼디움설포네이트와 알킬아릴소디움설포네이트 등을 0.01∼0.5중량퍼센트 사용하고, 구조식(Ⅲ)인 미량의 알칼리를 0.01∼0.3중량퍼센트를 사용하였는데 이때 음이온계면활성제의 양이 0.01중량퍼센트 이하일 경우에는 피브릴화가 곤란하고 0.5중량퍼센트 이상에서는 작업성이 불량하였으며 알칼리는 0.01중량퍼센트이하일 경우 피브릴화가 곤란하고 0.3중량퍼센트를 초과할 경우에서는 강도 및 탄성회복율이 저하되는 것을 알았다.As the dividing agent, for example, an alkali surfactant of the structural formula (II) is used, for example, 0.01 to 0.5% by weight of an alkaldium sulfonate and an alkylaryl sodium sulfonate, and 0.01 to 0.3% by weight of a trace alkali of the structural formula (III). In this case, when the amount of the anionic surfactant is 0.01% by weight or less, fibrillation is difficult, workability is poor at 0.5% by weight or more, and when alkali is less than 0.01% by weight, it is difficult to be fibrillated and exceeds 0.3% by weight. It was found that the strength and the elastic recovery rate were lowered at.

Figure kpo00002
Figure kpo00002

(단, R은 알킬기 또는 알킬아릴기임)(Wherein R is an alkyl group or an alkylaryl group)

Figure kpo00003
Figure kpo00003

(단, M은 주기율표상의 1A,2A족 원소이고 n은 1 또는 2임)(Where M is an element of group 1A, 2A on the periodic table and n is 1 or 2)

또한 피브릴화 촉진제로는 주기율표상의 1A 또는 2A족 원소의 염 또는 캐리어중 하나 또는 두가지를 동시에 사용하였는데 주기율표상의 1A 또는 2A족 원소의 염은 구조식(Ⅳ)의 화합물중 하나를 0.01중량퍼센트 이상 사용하였고 캐리어로는 2,4-디클로로페놀의 에테르형, 디메틸테레프탈레이트, 메틸디클로페녹시아세테이트 또는 N-알킬나프탈이미드유도체중에서 하나를 0.1∼3중량퍼센트 사용하였는데 이때 주기율표상의 1A 또는 2A족 원소의 염은 0.01중량퍼센트 미만일 경우 피브릴화가 곤란하였으나 그 이상에서는 양호하였으며 특히 5.0중량퍼센트이하일 경우에 양호하였다. 그리고 캐리어의 경우 0.1중량퍼센트 미만에서는 피브릴화가 곤란하였고 3중량퍼센트를 초과할 경우에는 직편물상에 얼룩을 발생시키는 결점이 있었다.In addition, one or both salts or carriers of group 1A or 2A elements on the periodic table were used simultaneously as the fibrillation promoter. The salts of elements 1A or 2A on the periodic table used 0.01% by weight or more of the compound of formula (IV). As a carrier, 0.1 to 3% by weight of an ether type of 2,4-dichlorophenol, dimethyl terephthalate, methyldichlorophenoxyacetate, or N-alkylnaphthalimide derivative was used. The salt of the element was difficult to fibrillate when less than 0.01% by weight, but it was good above, especially when less than 5.0% by weight. In the case of carriers, fibrillation was difficult at less than 0.1% by weight, and when the carrier was more than 3% by weight, staining occurred on the knitted fabric.

Figure kpo00004
Figure kpo00004

(단, M은 주기율표상의 1A 또는 2A족 원소이고 n은 1 또는 2임)(Where M is an element of group 1A or 2A on the periodic table and n is 1 or 2)

그리고 상기의 캐리어는 특히 기존의 방법에서 발생하는 용제에 의한 인체독성 및 제품의 물성저하가 없을 뿐만아니라 폐수처리가 용이하다는 장점을 갖는다.In addition, the carrier has the advantage of not only the human toxicity due to the solvent generated in the conventional method and the physical properties of the product, but also easy wastewater treatment.

본 발명에 의해 복합섬유를 피브릴화 함으로서 얻어지는 효과는 복합섬유의 피브릴화율을 100% 획득하면서 직편물의 고유한 물성을 보존하는 것이 특징이다. 특히 직편물의 탄성회복율 및 인열강도의 저하가 없으며 자체의 고유한 물성을 발휘할 수 있고, 감량이 일어나지 않아 인장강도의 저하가 없으며, 페놀이나 벤질알콜 유화액의 사용에 비하여 공정 조작성이 단순하고 폐수의 위험성이 거의 없다.The effect obtained by fibrillating the composite fiber by the present invention is characterized by preserving the inherent physical properties of the knitted fabric while obtaining a fibrillation rate of the composite fiber 100%. In particular, there is no reduction of elastic recovery rate and tear strength of the woven fabric, it can exhibit its own physical properties, no loss of tensile strength, and no loss of tensile strength, and simpler process operability compared to the use of phenol or benzyl alcohol emulsion and waste water There is little risk.

본 발명은 복합섬유를 트리코트, 랏셀, 평직, 능직, 이중직 기모지 등으로 사용할 때 높은 피브릴화율을 얻을 뿐만 아니라 직편물 고유의 물성을 보존하여 우수한 제품을 얻을 수 있다.The present invention can obtain a superior product by not only high fibrillation rate but also preserving the inherent physical properties of the woven fabric when using the composite fibers as tricot, ratsel, plain weave, twill, double weave brushing paper.

이하 본 발명의 실시예와 비교예를 설명하면 다음과 같다.Hereinafter, examples and comparative examples of the present invention will be described.

실험에서 사용된 복합섬유는 개질폴리에스터와 폴리아마이드가 70:30의 구성비를 가진 방사형 17분할형 80데니어 36필라멘트를 32게이지로 트리코트 제편한 편물을 사용하였는데, 개질 폴리에스터는 상기의 구조식(Ⅰ)을 갖고 이때 R은 CH3이고, M은 Na이며 디액시스 성분은 2몰퍼센트인 것을 사용하였다.The composite fiber used in the experiment was a tricot-knit knitted fabric of radial 17-divided 80-denier 36 filaments having a composition ratio of modified polyester and polyamide of 70:30 in 32 gauge. I), wherein R is CH 3 , M is Na, and the diaxial component is 2 mol%.

피브릴화 공정은 액류염색기에서 연수를 사용하여 편물의 1회전 시간이 60초, 액량비 20:1로 하여 40℃에서 98℃까지 10분간 승온시켜 98℃에서 20분간 유지하였다.In the fibrillation process, using a soft water in a liquid dyeing machine, the rotation time of the knitted fabric was 60 seconds and the liquid ratio was 20: 1.

이후 50℃까지 24분간 강온시킨 후 수세하여 물성을 측정하였다. 피브릴화시킨 시료의 피브릴화율은 광학 현미경으로 단면을 촬영하여 아래와 같은 식으로 계산하였다.Then, the temperature was lowered to 50 ° C. for 24 minutes and washed with water to measure physical properties. The fibrillation rate of the fibrillated sample was calculated by the following equation by capturing a cross section with an optical microscope.

Figure kpo00005
Figure kpo00005

탄성회복율은 5% 신장 탄성회복율을 측정하였으며, 인열강도는 KS K 0535 시험법인 팬들럼법으로 측정하였다.The elastic recovery rate was measured by 5% elongation elastic recovery rate, the tear strength was measured by the Pandum method, KS K 0535 test method.

[실시예 1]Example 1

도데실벤젠소디움설포네이트 0.1중량퍼센트, 가성소다 0.05중량퍼센트, 소디움설페이트 0.3중량퍼센트, 메틸디클로로페녹시아세테이트를 복합섬유 중량의 2.0중량퍼센트 사용하여 전기의 방법으로 피브릴화를 하였다.0.1% by weight of dodecylbenzenesodium sulfonate, 0.05% by weight of sodium hydroxide, 0.3% by weight of sodium sulfate, and 2.0% by weight of methyldichlorophenoxyacetate were fibrillated by the above method.

[실시예 2]Example 2

도데실벤젠소디움설포네이트 0.1중량퍼센트, 가성소다 0.1중량퍼센트, 소디움설페이트 0.3중량퍼센트를 사용하여 전기의 방법으로 피브릴화를 하였다.Fibrillation was carried out by the above method using 0.1% by weight of dodecylbenzenesodiumsulfonate, 0.1% by weight of caustic soda, and 0.3% by weight of sodium sulfate.

[실시예 3]Example 3

스테아릴소디움설포네이트 0.05중량퍼센트, 가성소다 0.05중량퍼센트, 소디움클로라이드 0.2중량퍼센트, N-알킬나프탈계 캐리어를 복합섬유 중량의 2.0중량퍼센트 사용하여 전기의 방법으로 피브릴화를 하였다.Fibrillation was carried out by the above method using 0.05% by weight of stearylsodiumsulfonate, 0.05% by weight of sodium hydroxide, 0.2% by weight of sodium chloride, and 2.0% by weight of N-alkylnaphthalic carrier.

[비교예 1]Comparative Example 1

페놀 6중량 퍼센트, 음이온계면활성제 1.5중량퍼센트를 사용하여 40℃에서 20분 처리후 90℃에서 30분간 피브릴화를 하였다.6 weight percent phenol and 1.5 weight percent anionic surfactant were used for 20 minutes at 40 ° C. and then fibrillated at 90 ° C. for 30 minutes.

[비교예 2]Comparative Example 2

벤질알콜 5중량 퍼센트, 음이온계면활성제와 비이온계면활성제가 9:1 비율로 조성된 시판계면활성제를 1.2중량퍼센트, 소디움설페이트 0.5중량퍼센트를 사용하여 60℃에서 30분간 처리후 90℃에서 40분간 피브릴화를 하였다.A commercially available surfactant consisting of 5% by weight of benzyl alcohol, 9: 1 ratio of anionic surfactant and nonionic surfactant, and 1.2% of sodium sulfate and 0.5% of sodium sulfate were treated for 30 minutes at 60 ° C, and then 40 minutes at 90 ° C. Fibrillation was carried out.

[비교예 3]Comparative Example 3

벤질알콜 5중량 퍼센트, 음이온계면활성제와 비이온계면활성제가 9:1 비율로 조성된 시판계면활성제를 1.2중량퍼센트, 가성소다 0.5중량퍼센트를 사용하여 60℃에서 30분간 처리후 90℃에서 40분간 피브릴화를 하였다.A commercially available surfactant consisting of 5% by weight of benzyl alcohol, an anionic surfactant and a nonionic surfactant in a 9: 1 ratio, was treated with 1.2% by weight and 0.5% by weight of caustic soda for 30 minutes at 60 ° C, followed by 40 minutes at 90 ° C. Fibrillation was carried out.

[비교예 4][Comparative Example 4]

개미산 0.5중량 퍼센트, 음이온계면활성제가 0.2중량퍼센트를 사용하여 60℃에서 30분간 처리후 90℃에서 40분간 피브릴화를 하였다.0.5% by weight of formic acid and 0.2% by weight of anionic surfactant were treated for 30 minutes at 60 ° C and then fibrillated at 90 ° C.

[표 1]TABLE 1

Figure kpo00006
Figure kpo00006

Claims (6)

개질폴리에스터와 폴리아마이드의 방사형 복합방사된 4-20분할형 복합섬유의 피브릴화에 있어서 음이온계면활성제, 규정농도의 알칼리, 주기율표상의 1A 또는 2A족 원소의 염 또는 캐리어중 하나 또는 두가지를 동시 사용함을 특징으로 하는 복합섬유의 피브릴화 방법.In the fibrillation of radially spun 4-20 split composite fibers of modified polyesters and polyamides, one or both of anionic surfactants, alkalis of specified concentrations, salts or carriers of elements 1A or 2A on the periodic table Fibrillation method of a composite fiber characterized in that used. 제1항에 있어서, 개질폴리에스터는 하기식을 만족하는 금속 술폰산염을 함유한 이소프탈레이트 성분이 전체 디액시드의 0.3∼10.0몰퍼센트 함유된 폴리에스터 공중합체임을 특징으로 하는 복합섬유의 피브릴화 방법.The fibrillation of a composite fiber according to claim 1, wherein the modified polyester is a polyester copolymer containing an isophthalate component containing a metal sulfonate satisfying the following formula: 0.3-10.0 mole percent of the total diacid. Way.
Figure kpo00007
Figure kpo00007
(상기 식중 R은 수소원자 또는 탄소수 1-6의 알킬기 또는 아릴기를 나타낸 것이고, M은 알칼리금속 화합물임)(Wherein R represents a hydrogen atom or an alkyl or aryl group having 1-6 carbon atoms and M is an alkali metal compound)
제1항에 있어서, 음이온계면활성제가 하기식을 만족하는 화합물중 하나로 0.01∼0.5중량퍼센트를 사용하는 것을 특징으로 하는 복합섬유의 피브릴화 방법.The fibrillation method of a composite fiber according to claim 1, wherein the anionic surfactant uses 0.01 to 0.5% by weight as one of the compounds satisfying the following formula. R-SO3NaR-SO 3 Na (상기 식중 R은 알킬기 또는 아릴기임)(Wherein R is an alkyl group or an aryl group) 제1항에 있어서, 알킬기가 하기식을 만족하는 화합물중 하나로 0.01∼0.3중량 퍼센트를 사용하는 것을 특징으로 하는 복합섬유의 피브릴화 방법.The fibrillation method of a composite fiber according to claim 1, wherein the alkyl group uses 0.01 to 0.3% by weight as one of the compounds satisfying the following formula. M(OH)n M (OH) n (상기 식중 M은 주기율표상의 1A 또는 2A족 원소이고 n은 1 또는 2임)(Wherein M is a 1A or 2A group element on the periodic table and n is 1 or 2) 제1항에 있어서, 주기율표상의 1A 또는 2A족 원소의 염은 하기식을 만족하는 화합물중 하나로 0.01중량퍼센트 이상을 사용하는 것을 특징으로 하는 복합섬유의 피브릴화 방법.The fibrillation method of a composite fiber according to claim 1, wherein the salt of a group 1A or 2A element on the periodic table uses 0.01 wt% or more as one of the compounds satisfying the following formula. M(CO3)n또는 MHCO3또는 (M)nSO4또는 M(Cl)n M (CO 3 ) n or MHCO 3 or (M) n SO 4 or M (Cl) n (상기 식중 M은 주기율표상의 1A 또는 2A족 원소이고 n은 1 또는 2임)(Wherein M is a 1A or 2A group element on the periodic table and n is 1 or 2) 제1항에 있어서, 캐리어가 2,4-디클로로페놀의 에테르형, 디메틸테레프탈레이트, 메틸디클로페녹시아세테이트 또는 N-알킬나프탈이미드유도체중에서 하나로 복합섬유 중량에 대하여 0.1-3중량퍼센트 사용하는 것을 특징으로 하는 복합섬유의 피브릴화 방법.The method according to claim 1, wherein the carrier is used in an ether type of 2,4-dichlorophenol, dimethyl terephthalate, methyl dichlorophenoxyacetate, or N-alkyl naphthalimide derivative in an amount of 0.1-3% by weight based on the weight of the composite fiber. Fibrillation method of a composite fiber, characterized in that.
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