KR20060112438A - High specific gravity and flame retardant core-sheath composite fiber - Google Patents
High specific gravity and flame retardant core-sheath composite fiber Download PDFInfo
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- KR20060112438A KR20060112438A KR1020050034892A KR20050034892A KR20060112438A KR 20060112438 A KR20060112438 A KR 20060112438A KR 1020050034892 A KR1020050034892 A KR 1020050034892A KR 20050034892 A KR20050034892 A KR 20050034892A KR 20060112438 A KR20060112438 A KR 20060112438A
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- 239000000835 fiber Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000003063 flame retardant Substances 0.000 title claims abstract description 37
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical group N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 230000005484 gravity Effects 0.000 title claims abstract description 20
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 45
- 239000011574 phosphorus Substances 0.000 claims abstract description 45
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000008358 core component Substances 0.000 claims abstract description 29
- 239000000306 component Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 15
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 14
- 229910052788 barium Inorganic materials 0.000 claims abstract description 12
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 12
- -1 flame retardant phosphorus compound Chemical class 0.000 claims abstract description 11
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 8
- XMYONIRNSCCGKW-UHFFFAOYSA-N OC(C(=O)O)(C)[PH2]=O Chemical class OC(C(=O)O)(C)[PH2]=O XMYONIRNSCCGKW-UHFFFAOYSA-N 0.000 claims description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 125000001188 haloalkyl group Chemical group 0.000 claims description 3
- 125000005059 halophenyl group Chemical group 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920006149 polyester-amide block copolymer Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 229920000728 polyester Polymers 0.000 description 17
- 238000000034 method Methods 0.000 description 14
- 238000009987 spinning Methods 0.000 description 14
- 229920000642 polymer Polymers 0.000 description 9
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 7
- 238000006068 polycondensation reaction Methods 0.000 description 7
- 239000012209 synthetic fiber Substances 0.000 description 7
- 229920002994 synthetic fiber Polymers 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- OAQNJOLLBTVWFD-UHFFFAOYSA-N OC(=O)C1=CC=CC=C1P(O)=O Chemical compound OC(=O)C1=CC=CC=C1P(O)=O OAQNJOLLBTVWFD-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000002542 deteriorative effect Effects 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 150000002903 organophosphorus compounds Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000002013 dioxins Chemical class 0.000 description 1
- 125000003106 haloaryl group Chemical group 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Multicomponent Fibers (AREA)
Abstract
본 발명은 고비중 및 고난연성 코어-시스형 복합섬유에 관한 것으로서, 코어성분(1)을 시스성분(2)이 감싸고 있는 형태인 코어(Core)-시스(Sheath)형 복합섬유에 있어서, 상기 코어성분(1)은 난연성 인화합물을 함유하여 인 함량이 0~0.7중량%이며 바륨술포네이트 입자 함량이 5~70중량%인 열가소성 중합체이고, 상기 시스성분(2)은 난연성 인화합물을 함유하여 인 함량이 0.05~3.0중량%인 열가소성 중합체이고, 상기 시스성분(2)내 인 함량이 코어성분(1)내 인 함량 보다 2,000ppm 이상 높은 것을 특징으로 한다.The present invention relates to a high specific gravity and highly flame-retardant core-sheath composite fiber, in the core-sheath composite fiber in which the core component (1) is wrapped around the sheath component (2), The core component (1) is a thermoplastic polymer containing a flame retardant phosphorus compound and having a phosphorus content of 0 to 0.7% by weight and a barium sulfonate particle content of 5 to 70% by weight, and the sheath component (2) contains a flame retardant phosphorus compound. Phosphorus content is 0.05 ~ 3.0% by weight thermoplastic polymer, characterized in that the phosphorus content in the sheath component (2) is 2,000ppm or more higher than the phosphorus content in the core component (1).
본 발명은 비중이 높아 드레이프성(Drape property)이 우수하고 난연성이 특히 뛰어나 커튼등의 인테리어 소재용 원사로 매우 유용하다.The present invention is very useful as a yarn for interior materials such as curtains because of its high specific gravity and excellent drape property and excellent flame retardancy.
Description
도1 내지 도3은 본 발명에 따른 코어-시스형 복합섬유의 단면 예시도.1 to 3 is a cross-sectional view of the core-sheath composite fiber according to the present invention.
*도면중 주요 부분에 대한 부호 설명* Description of symbols on the main parts of the drawings
1 : 코어성분 2 : 시스성분1
본 발명은 고비중 및 고난연성을 갖는 코어-시스형 복합섬유에 관한 것으로서, 더욱 상세하게는 비중이 높아 드레이프성(Drape Property)이 우수함과 동시에 뛰어난 난연성을 갖고 있어서 커텐등의 인테리어 소재용 원사로 유용한 코어-시스형 복합섬유에 관한 것이다.The present invention relates to a core-sheath type composite fiber having a high specific gravity and high flame retardancy, and more particularly, a specific gravity is high, which is excellent in drape property and at the same time excellent flame retardancy. A useful core-sheath composite fiber.
폴리에스테르등과 같은 열가소성 중합체는 기계적 성질과 성형성등이 우수하여 섬유 또는 필름등의 성형재료로 널리 사용 된다.Thermoplastic polymers such as polyester have excellent mechanical properties and moldability and are widely used as molding materials for fibers or films.
그러나, 열가소성 중합체로 제조된 합성섬유는 난연성과 드레이프성이 부족하여 커텐등의 인테리어 소재용 원사로는 부적합한 문제가 있었다.However, synthetic fibers made of thermoplastic polymers have insufficient flame retardancy and drape properties, and thus are unsuitable as yarns for interior materials such as curtains.
합성섬유에 난연성을 부여하는 종래기술로서는 합성섬유로 제조된 직물을 염가공할 때 염욕내에 할로겐계 난연제를 첨가하는 후처리 가공 방법과 합성섬유의 중합시 할로겐계 난연제 또는 인계 난연제를 첨가하는 방법등이 알려져 있다Conventional techniques for imparting flame retardancy to synthetic fibers include post-treatment methods for adding halogen-based flame retardants to salt baths when fabricating fabrics made of synthetic fibers, and methods for adding halogen-based flame retardants or phosphorus-based flame retardants during polymerization of synthetic fibers. Is known
그러나, 상기의 후처리 가공방법은 세탁 및 마찰시 난연제가 탈락하여 난연성이 떨어지고 화재시 디옥신등의 유독가스가 발생하는 문제점이 있고, 중합시 난연제를 첨가하는 방법은 합성섬유를 변색시키거나 열안정성 및 내광성을 저하 시키는 문제가 있었다.However, the post-treatment processing method has a problem in that the flame retardant is dropped during washing and friction, resulting in inferior flame retardancy and toxic gases such as dioxins during fire, and the method of adding a flame retardant during polymerization discolors synthetic fibers or heat. There was a problem of lowering stability and light resistance.
한편, 미국, 유럽등에서는 연소시 디옥신이 발생되는 문제점이 있는 할로겐계 난연섬유의 사용 규제가 강화되고 있다.On the other hand, in the United States, Europe, the use of halogen-based flame retardant fiber, which has a problem that dioxin occurs during combustion is tightening.
미국특허 4033936호, 미국특허 3941752호 및 일본 특공소 59-191716, 특공소 60-101144호에서는 난연성 폴리에스테르를 제조하는 종래기술로서, 유기 인화합물의 중축합 반응이 어느 정도 진행된 후에 페닐포스폰산 지방족글리콜에스테르를 폴리에스테르의 반응성분과 함께 중축합시켜 난연성을 부여하는 방법, 아릴포스폰산 단량체를 미리 15~60wt% 함유시키고 공중합한 후 기존의 폴리에스테르와 배합하는 방법, 유기 인화합물을 BHT 반응시 첨가하고 이를 중축합하여 폴리에스테르를 제조하는 방법 및 마그네슘, 망간 등의 무기물과 유기 인화합물을 첨가하여 난연성을 부여하는 방법등을 게재하고 있으나, 공정이 복잡하고, 실직적으로 인화합물의 잔존율이 낮아 충분한 난연성을 얻기 어려운 문제점이 있다. 그뿐만 아니라 난연 폴리에스테르 제조를 위하여 사용하는 난연제가 황색을 띠게 되어 이를 폴리에스테르와 공중합하여 섬유로 사용할 경우 섬유의 색조가 황색으로 변하게 되므로 색상이 양호한 폴리에스테르를 얻기 어려운 문제점이 있다.U.S. Patent No. 4033936, U.S. Pat. Method to impart flame retardancy by polycondensation of glycol ester with reactive component of polyester, to contain 15 ~ 60wt% of arylphosphonic acid monomer in advance, copolymerize with existing polyester, and organic phosphorus compound during BHT reaction Adding a polycondensate and adding a polycondensate, and adding a inorganic and organophosphorus compounds such as magnesium and manganese to impart flame retardancy, but the process is complicated, There is a problem that it is difficult to obtain low flame retardancy. Not only that, the flame retardant used for the production of flame retardant polyester becomes yellow, and when it is used as a fiber by copolymerizing it with polyester, the color tone of the fiber is changed to yellow, which makes it difficult to obtain a good polyester.
커튼등의 인테리어 소재용 원사에는 우수한 난연성과 함께 양호한 드레이프성 발현을 위해 높은 비중이 요구 된다.Yarns for interior materials such as curtains are required to have a high specific gravity in order to express good drape property with excellent flame retardancy.
합성섬유의 비중을 높이기 위한 종래기술로서는 통상의 합성섬유내에 바륨술페이트 입자등을 첨가하는 방법이 제안된바 있으나, 상기방법은 방사 조업성이 저하되어 세섬도화가 곤란하고 균일한 염색이 곤란한 문제점이 있었다. As a conventional technique for increasing the specific gravity of synthetic fibers, a method of adding barium sulphate particles or the like into conventional synthetic fibers has been proposed. However, the above method has a problem in that the fineness of the fineness is difficult and uniform dyeing is difficult due to poor spinning operation. There was this.
본 발명은 이상에서 살펴본 종래의 문제점등을 해결할 수 있도록, 방사조업성 및 염색성의 저하 없이도 비중이 높으며, 섬유표면부의 인 함량이 높아 초기 연소에 대한 난연성이 우수하여 커튼등의 인테리어 소재용 원사로 적합한 코어-시스형 복합섬유를 제공하기 위한 것이다.The present invention has a high specific gravity even without deterioration in spinning operation and dyeing properties to solve the problems described above, and has a high phosphorus content of the fiber surface part, which is excellent in flame retardancy against initial combustion, and thus as a yarn for interior materials such as curtains. To provide a suitable core-sheath composite fiber.
본 발명은 코어-시스형 복합섬유의 코어성분내에 바륨설페이트 입자를 첨가 하여 방사조업성의 저하 없이도 비중을 높이고, 쉬스성분내의 인 함량을 코어성분내의 인 함량보다 높게하여 초기 연소에 대한 난연성이 뛰어나 인테리어 소재용 원사로 특히 유용한 코어-시스형 복합섬유를 제공하고자 한다.The present invention adds barium sulphate particles to the core component of the core-sheath composite fiber to increase specific gravity without deteriorating spinning operation, and to increase the phosphorus content in the sheath component than the phosphorus content in the core component, thereby providing excellent flame retardancy against initial combustion. To provide a particularly useful core-sheath composite fiber as a yarn for a material.
이와 같이 과제들을 달성하기 위한 본 발명의 고비중 및 고난연성 코어-시스형 복합섬유는, 코어성분(1)을 시스성분(2)이 감싸고 있는 형태인 코어(Core)-시스 (Sheath)형 복합섬유에 있어서, 상기 코어성분(1)은 난연성 인화합물을 함유하여 인 함량이 0~0.7중량%이며 바륨술포네이트 입자 함량이 5~70중량%인 열가소성 중합체이고, 상기 시스성분(2)은 난연성 인화합물을 함유하여 인 함량이 0.05~3.0중량%인 열가소성 중합체이고, 상기 시스성분(2)내 인 함량이 코어성분(1)내 인 함량 보다 2,000ppm 이상 높은 것을 특징으로 한다.The high specific gravity and high flame retardant core-sheath composite fiber of the present invention for achieving the above problems is a core-sheath composite in which the
이하, 첨부한 도면등을 통하여 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
먼저 본 발명은 도1 내지 도3과 같이 코어성분(1)을 시스성분(2)이 감싸고 있는 코어-시스형(Core-Sheath Type) 단면 구조를 갖는다.First, the present invention has a core-sheath type cross-sectional structure in which the
도1 내지 도3은 본 발명의 단면 예시도 이다.1 to 3 are cross-sectional views of the present invention.
상기의 코어성분(1)은 바륨설포네이트 입자 함량이 코어성분(1)의 전체 중량대비 5~70중량%이고, 인 함량이 코어성분(1)의 전체중량 대비 0~0.7중량%가 되도록 난연성 인화합물이 함유되어 있는 열가소성 중합체이다.The core component (1) is flame retardant so that the barium sulfonate particle content is 5 to 70% by weight based on the total weight of the core component (1), and the phosphorus content is 0 to 0.7% by weight relative to the total weight of the core component (1). It is a thermoplastic polymer containing phosphorus compound.
상기 바륨설포네이트 입자의 입자크기는 0.3~0.6㎛인 것이 방사조업성 향상에 보다 바람직하다.Particle size of the barium sulfonate particles is more preferably 0.3 ~ 0.6㎛ to improve the spinning operation.
코어성분(1)의 단면적은 코어-시스형 복합섬유의 전체 단면적 대비 10~80%인 것이 바람직하다.The cross-sectional area of the core component (1) is preferably 10 to 80% of the total cross-sectional area of the core-sheath composite fiber.
코어성분(1)의 단면적 비율이 상기 범위를 벗어날 경우에는 코어-시스형 복합섬유의 단면형성성과 방사조업성이 저하될 수도 있다.When the ratio of the cross-sectional area of the core component 1 is out of the above range, the cross-sectional formability and spinning operation property of the core-sheath composite fiber may be deteriorated.
코어성분(1)내 바륨설포네이트 입자의 함량이 5중량% 미만을 경우에는 코어-시스형 복합섬유의 비중이 낮아져 드레이프성이 저하되고, 70중량%를 초과할 경우 에는 방사조업성이 저하된다.When the content of the barium sulfonate particles in the core component (1) is less than 5% by weight, the specific gravity of the core-sheath composite fiber is lowered, and the drape property is lowered. .
코어성분내 인 함량이 0.7중량%를 초과하는 경우에는 공중합에 의한 물성이 저하에 의해 연신공정시 사절이 생기기 쉬워 방사작업성이 나빠진다.When the phosphorus content in the core component exceeds 0.7% by weight, the threading property is liable to occur during the stretching process due to the decrease in physical properties due to copolymerization, resulting in poor spinning workability.
한편, 본 발명을 구성하는 시스성분(2)은 시스성분(2)의 전체중량 대비 인 함량이 0.05~3.0중량%인 열가소성 중합체 이다.On the other hand, the sheath component (2) constituting the present invention is a thermoplastic polymer having a phosphorus content of 0.05 to 3.0% by weight relative to the total weight of the sheath component (2).
아울러, 본 발명은 시스성분(2)내 인 함량이 코어성분(1)내 인 함량 보다 2,000ppm 이상 높은 것을 특징으로 한다. In addition, the present invention is characterized in that the phosphorus content in the cis component (2) is 2,000 ppm or more higher than the phosphorus content in the core component (1).
또한, 본 발명은 코어-시스형 복합섬유내 함유된 총 인 함량이 코어-시스형 복합섬유의 전체 중량 대비 0.15~2.0중량% 이다.In addition, in the present invention, the total phosphorus content contained in the core-sheath composite fiber is 0.15 to 2.0 wt% based on the total weight of the core-sheath composite fiber.
상기의 시스성분(2)내 인 함량이 0.05중량% 미만이거나, 시스성분(2)내 인 함량이 코어성분(1)내 인 함량 보다 2,000ppm 미만으로 높거나, 코어-시스형 복합섬유내에 함유된 총 인 함량이 0.15중량% 미만인 경우에는 초기연소에 대한 난연성이 저하된다.The phosphorus content in the sheath component (2) is less than 0.05% by weight, or the phosphorus content in the sheath component (2) is less than 2,000 ppm higher than the phosphorus content in the core component (1), or is contained in the core-sheath composite fiber If the total phosphorus content is less than 0.15% by weight, the flame resistance to initial combustion is lowered.
한편, 상기의 시스성분(2)내 인 함량이 3.0중량%를 초과하거나 코어-시스형 복합섬유내 함유된 인 함량이 2.0중량%를 초과하는 경우에는 공중합에 의한 물성저하에 의해 연신 공정시 사절이 생기기 쉬어 방사작업성이 저하된다.On the other hand, when the phosphorus content in the sheath component (2) is more than 3.0% by weight or the phosphorus content in the core-cis type composite fiber exceeds 2.0% by weight, the trimming process is performed during the stretching process due to the decrease of physical properties by copolymerization. This tends to occur and the workability of the spinning is lowered.
코어성분(1)과 시스성분(2)을 구성하는 열가소성 중합체는 각각 폴리에스테르 또는 폴리아미드 등 이다.The thermoplastic polymers constituting the core component (1) and the sheath component (2) are polyester or polyamide, respectively.
코어성분(1)과 시스성분(2)내에 함유된 난연성 인화합물은 하기 일반식(Ⅰ)의 히드록시 포스피닐 프로판산 유도체인 것이 난연성 및 방사조업성 향상에 보다 바람직하다.The flame retardant phosphorus compounds contained in the core component (1) and the cis component (2) are more preferably hydroxy phosphinyl propanoic acid derivatives of the following general formula (I) for the improvement of flame retardancy and spinning operability.
[상기식에서 R 및 R1은 메틸, 페닐, 할로페닐, 알킬, 할로알킬 또는 할로아닐이다][Wherein R and R 1 are methyl, phenyl, halophenyl, alkyl, haloalkyl or haloaniyl]
상기 일반식(Ⅰ)의 히드록시 포스피닐 프로판산 유도체는 하기 일반식(Ⅱ)의 이염화 인화합물과 아크릴산 또는 메타크릴산을 110℃가 넘지 않는 온도에서 반응시켜 제조할 수 있다. The hydroxy phosphinyl propanoic acid derivatives of the general formula (I) may be prepared by reacting a phosphorus dichloride compound of the general formula (II) with acrylic acid or methacrylic acid at a temperature not exceeding 110 ° C.
[상기식에서, R1은 메틸, 페닐, 할로페닐, 알킬, 할로알킬 또는 할로아릴이다][Wherein R 1 is methyl, phenyl, halophenyl, alkyl, haloalkyl or haloaryl]
본 발명의 코어-시스형 복합섬유를 제조하는 방법중 일례를 살펴보면 아래와 같다.Looking at one example of a method for producing a core-sheath composite fiber of the present invention.
먼저, 폴리에스테르등의 열가소성 중합체를 중합할 때 중합용 모노머들과 함께 바륨술포네이트 또는 바륨술포네이트와 상기 일반식(Ⅰ)의 히드록시 포스피닐 프로판산 유도체를 앞에서 설명한 함량 범위내로 첨가하여 코어성분(1)용 중합체를 제조한다.First, when polymerizing a thermoplastic polymer such as polyester, barium sulfonate or barium sulfonate and the hydroxy phosphinyl propanoic acid derivative of the general formula (I) together with the monomers for polymerization are added within the content ranges described above. The polymer for (1) is manufactured.
한편, 폴리에스테르등의 열가소성 중합체를 중합할 때 중합용 모노머들과 함께 상기 일반식(Ⅰ)의 히드록시 포스피닐 프로판산 유도체를 인 함량이 0.05~3.0중량%가 되도록 첨가하여 시스성분(2)용 중합체를 제조한다.Meanwhile, when polymerizing a thermoplastic polymer such as polyester, the hydroxy phosphinyl propanoic acid derivative of the general formula (I) together with the monomers for polymerization is added so that the phosphorus content is 0.05 to 3.0% by weight, and the cis component (2) To prepare a polymer.
다음으로, 상기와 같이 제조된 코어성분용 중합체와 시스성분용 중합체를 통상의 코어-시스용 복합 방사 구금으로 복합방사 한 후, 연신 및 권취하여 본 발명의 코어-시스형 복합 섬유를 제조한다.Next, after the composite spinning for the core component polymer and the sheath component polymer prepared as described above in a conventional composite spinneret for core-sheath, it is drawn and wound to prepare the core-sheath composite fiber of the present invention.
본 발명은 코어성분(1)내에 바륨설퍼네이트 입자가 함유되어 방사조업성 저하없이도 코어-시스형 복합섬유의 비중이 크게 높아져 드레이프성이 향상된다.In the present invention, the barium sulfonate particles are contained in the core component 1, so that the specific gravity of the core-sheath composite fiber is greatly increased without deterioration in spinning operation properties, thereby improving drape.
아울러, 본 발명은 시스성분(2)내에 보다 많은 인 함량이 함유되어 초기 연소에 대한 난연성이 특히 우수하다.In addition, the present invention contains more phosphorus content in the sheath component (2), which is particularly excellent in flame retardancy against initial combustion.
이하, 실시예 및 비교실시예를 통하여 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail through Examples and Comparative Examples.
그러나, 본 발명은 하기 실시예들에 의해 권리범위가 한정되는 것은 아니다.However, the present invention is not limited by the following examples.
실시예1Example 1
테레프탈산 17.3㎏, 에틸렌글리콜 7.43㎏을 반응기에 넣고 테트라에틸암모늄 하이드록사이드 4.2g을 첨가하여 반응온도가 245℃ 될 때까지 반응시켜 올리고머(BHET)를 제조하였다. 여기에 중축합 촉매로 삼산화 안티몬 또는 안티몬 아세테이트를 폴리머내 안티몬 함량이 350ppm이 되도록 투입하고 보조촉매로 코발트 아세테이트를 삼산화 안티몬 또는 안티몬 아세테이트 양의 20% 수준으로 투입하고 2-카르 복시 페닐 포스핀산을 중합체내 인 함량이 10,000ppm(30중량%)가 되도록 투입한 다음 약 20분간 교반하여 이를 중축합 반응기로 이송한 후 1시간에 걸쳐 상압에서 1mmHg로의 고진공 상태로 감압하여 반응온도가 285℃에 이를 때까지 4시간 30분동안 중축합을 실시하여 쉬스용 난연 폴리에스테르를 중합하였다. 17.3 kg of terephthalic acid and 7.43 kg of ethylene glycol were added to the reactor, and 4.2 g of tetraethylammonium hydroxide was added to the reaction until the reaction temperature was 245 ° C., thereby preparing an oligomer (BHET). To the polycondensation catalyst, antimony trioxide or antimony acetate was added so that the antimony content in the polymer was 350 ppm, and cobalt acetate was added at a level of 20% of the amount of antimony trioxide or antimony acetate as a cocatalyst, and 2-carboxyphenyl phosphinic acid was used as a polymer. After inputting so that the endogenous content is 10,000ppm (30% by weight), it is stirred for about 20 minutes, transferred to a polycondensation reactor, and decompressed at a high vacuum of 1mmHg at atmospheric pressure over 1 hour, when the reaction temperature reaches 285 ° C. Polycondensation was carried out for 4 hours and 30 minutes until the polymerization of the flame retardant polyester for the sheath.
이때 중합체의 고유점도는 0.665이었다.At this time, the intrinsic viscosity of the polymer was 0.665.
다음으로, 테레프탈산 17.3㎏, 에틸렌글리콜 7.43㎏을 반응기에 넣고 테트라에틸암모늄 하이드록사이드 4.2g을 첨가하여 반응온도가 245℃ 될 때까지 반응시켜 올리고머(BHET)를 제조하였다. 여기서 중축합 촉매로 삼산화 안티몬 또는 안티몬 아세테이트를 폴리머내 안티몬 함량이 350ppm이 되도록 투입하고 보조촉매로 코발트 아세테이트를 삼산화 안티몬 또는 안티몬 아세테이트 양의 20% 수준으로 투입하고 2-카르복시 페닐 포스핀산에 중합체내 인 함량이 3,500ppm(0.6중량%)가 되도록 투입함과 동시에 입자크기가 0.5㎛인 바륨설포네이트 입자를 중합체 전체 중량 대비 30중량%가 되도록 투입한 다음, 약 20분간 교반하여 이를 중축합 반응기로 이송한 후 1시간에 걸쳐 상압에서 1mmHg로의 고진공 상태로 감압하여 반응온도가 285℃에 이를 때까지 4시간 30분동안 중축합을 실시하여 코어용 난연 폴리에스테르를 중합하였다. 이때 이중합체의 고유점도는 0.654이었다. Next, 17.3 kg of terephthalic acid and 7.43 kg of ethylene glycol were added to the reactor, and 4.2 g of tetraethylammonium hydroxide was added to the reaction until the reaction temperature became 245 ° C, thereby preparing an oligomer (BHET). Here, antimony trioxide or antimony acetate was added as a polycondensation catalyst so that the antimony content in the polymer was 350ppm, and cobalt acetate was added at a level of 20% of the amount of antimony trioxide or antimony acetate as a cocatalyst and phosphorus in 2-carboxyphenyl phosphinic acid was added. At the same time, the content is 3,500 ppm (0.6% by weight), and the barium sulfonate particles having a particle size of 0.5 μm are added at 30% by weight based on the total weight of the polymer, followed by stirring for about 20 minutes to be transferred to the polycondensation reactor. After depressurizing to a high vacuum at 1 mmHg at atmospheric pressure over 1 hour, polycondensation was carried out for 4 hours and 30 minutes until the reaction temperature reached 285 ° C. to polymerize the flame retardant polyester for the core. At this time, the intrinsic viscosity of the dipolymer was 0.654.
상기와 같이 제조된 쉬스용 난연 폴리에스테르와 코어용 난연 폴리에스테르를 각각 54 : 46의 단면적 비율로 사용하여 도1의 단면형태로 복합방사 하여 170데니어/36필라멘트의 복합섬유를 제조 하였다.Sheath flame-retardant polyester and the core flame-retardant polyester prepared as described above using a cross-sectional ratio of 54:46, respectively, composite spinning in the cross-sectional shape of Figure 1 to prepare a composite fiber of 170 denier / 36 filaments.
이때, 방사속도는 3,000m/분으로 하고 냉각에어 풍속은 0.5m/분으로 하였다.At this time, the spinning speed was 3,000 m / min and the cooling air wind speed was 0.5 m / min.
다음으로, 상기와 같이 제조된 복합섬유를 통상의 방법으로 연신 및 가연 한 후 이를 경사 및 위사로 사용하여 직물을 제조 하였다.Next, the composite fiber prepared as described above was stretched and twisted in a conventional manner, and then used as warp and weft yarn to prepare a fabric.
제조된 직물의 난연성 및 드레이프성을 평가한 결과는 표2와 같다.Table 2 shows the results of evaluating the flame retardancy and drape of the fabric.
실시예2 및 비교실시예1 ~ 비교실시예2Example 2 and Comparative Example 1 to Comparative Example 2
쉬스용 난연 폴리에스테르내 인 함량, 코어용 난연 폴리에스테르내 인 함량과 바륨설포네이트 함량을 표1과 같이 변경한 것을 제외하고는 실시예1과 동일하게 복합섬유 및 그의 직물을 제조하였다.A composite fiber and its fabric were prepared in the same manner as in Example 1 except that the phosphorus content in the sheath flame retardant polyester, the phosphorus content in the flame retardant polyester and the barium sulfonate content were changed as shown in Table 1.
제조된 직물의 난연성 및 드레이프성을 평가하는 결과는 표2와 같다.The results of evaluating the flame retardancy and drape of the fabrics produced are shown in Table 2.
본 발명에 있어서 각종 물성은 아래와 같은 방법으로 평가하였다.Various physical properties in the present invention were evaluated by the following method.
· 한계산소지수(LOI법,%)Limit oxygen index (LOI method,%)
KS-M 3032 방법으로 평가 하였다.It was evaluated by the KS-M 3032 method.
· 45°경사법45 ° slope
KS-K 0580 방법으로 평가 하였다.It was evaluated by the KS-K 0580 method.
· 방사작업성(%)Radio workability (%)
일주일 동안 방사작업을 실시하여 만권율을 측정하고, 이를 방사작업성 로 평가하였다.One week of spinning was carried out to measure the winding power, which was evaluated as radio workability.
· 드레이프성Drape
전문가 10명의 관능검사로 평가하였다. Sensory evaluation was performed by 10 experts.
10명중 8명 이상이 양호하다고 판정하면 우수로, 10명중 5명~7명이 양호하다고 판정하면 보통으로, 10명중 4명 이하가 양호다고 판정하면 불량으로 각각 구분하였다.When 8 or more out of 10 people were judged to be good, they were classified as excellent. When 5 to 7 out of 10 people were judged to be good, they were classified as poor.
본 발명은 코어성분내에 바륨설페이트 입자가 함유되어 방사 조업성의 저하 없이도 복합섬유의 비중을 효과적으로 향상 시켜 뛰어난 드레이프 성질을 발현한다.In the present invention, barium sulfate particles are contained in the core component, thereby effectively improving the specific gravity of the composite fiber without deteriorating spinning operability to express excellent drape properties.
아울러, 본 발명은 코어성분내 인 함량 보다 쉬스성분내 인 함량이 높아 초기 연소에 대한 난연성이 우수하다.In addition, the present invention has a high phosphorus content in the sheath component than the phosphorus content in the core component is excellent in flame retardancy for the initial combustion.
그로인해, 본 발명은 커튼등의 인테리어 소재용 원사로 특히 유용하다.Therefore, the present invention is particularly useful as yarn for interior materials such as curtains.
Claims (7)
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020050034892A KR20060112438A (en) | 2005-04-27 | 2005-04-27 | High specific gravity and flame retardant core-sheath composite fiber |
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| KR1020050034892A KR20060112438A (en) | 2005-04-27 | 2005-04-27 | High specific gravity and flame retardant core-sheath composite fiber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100915458B1 (en) * | 2007-06-15 | 2009-09-04 | 웅진케미칼 주식회사 | Flame retardant and low melting polyester fiber and method of making the same |
| WO2010011068A3 (en) * | 2008-07-24 | 2010-05-27 | 경북대학교 산학협력단 | Flame-retardant screen fabric for window coverings and method of manufacturing the same |
| KR101041159B1 (en) * | 2010-12-06 | 2011-06-13 | 유진섬유 주식회사 | Heat-sealed fiber with excellent flame retardancy and light shielding properties and textile products using the same |
| US20240401244A1 (en) * | 2021-01-29 | 2024-12-05 | Toray Industries, Inc. | Fabric, fabric body and seat |
-
2005
- 2005-04-27 KR KR1020050034892A patent/KR20060112438A/en not_active Ceased
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100915458B1 (en) * | 2007-06-15 | 2009-09-04 | 웅진케미칼 주식회사 | Flame retardant and low melting polyester fiber and method of making the same |
| WO2010011068A3 (en) * | 2008-07-24 | 2010-05-27 | 경북대학교 산학협력단 | Flame-retardant screen fabric for window coverings and method of manufacturing the same |
| KR101041159B1 (en) * | 2010-12-06 | 2011-06-13 | 유진섬유 주식회사 | Heat-sealed fiber with excellent flame retardancy and light shielding properties and textile products using the same |
| US20240401244A1 (en) * | 2021-01-29 | 2024-12-05 | Toray Industries, Inc. | Fabric, fabric body and seat |
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