KR101792080B1 - Manufacturing method of elution type knitted fabric - Google Patents
Manufacturing method of elution type knitted fabric Download PDFInfo
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- KR101792080B1 KR101792080B1 KR1020100140441A KR20100140441A KR101792080B1 KR 101792080 B1 KR101792080 B1 KR 101792080B1 KR 1020100140441 A KR1020100140441 A KR 1020100140441A KR 20100140441 A KR20100140441 A KR 20100140441A KR 101792080 B1 KR101792080 B1 KR 101792080B1
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- 239000004744 fabric Substances 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 238000010828 elution Methods 0.000 title 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000835 fiber Substances 0.000 claims abstract description 39
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920000728 polyester Polymers 0.000 claims abstract description 30
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 28
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 11
- ULFSNQUHLQGAMF-UHFFFAOYSA-N COC(=O)C1=CC([Na])=CC(C(=O)OC)=C1S(O)(=O)=O Chemical compound COC(=O)C1=CC([Na])=CC(C(=O)OC)=C1S(O)(=O)=O ULFSNQUHLQGAMF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract 6
- 239000002131 composite material Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 18
- 239000003963 antioxidant agent Substances 0.000 claims description 9
- 239000012760 heat stabilizer Substances 0.000 claims description 9
- 239000002518 antifoaming agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 239000007809 chemical reaction catalyst Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 3
- 241000475481 Nebula Species 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 abstract description 8
- 230000000379 polymerizing effect Effects 0.000 abstract description 2
- 208000016261 weight loss Diseases 0.000 description 9
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 230000004580 weight loss Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- 238000005886 esterification reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000013585 weight reducing agent Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 238000012643 polycondensation polymerization Methods 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- -1 sodium sulfonate salt Chemical class 0.000 description 2
- RYRZSXJVEILFRR-UHFFFAOYSA-N 2,3-dimethylterephthalic acid Chemical compound CC1=C(C)C(C(O)=O)=CC=C1C(O)=O RYRZSXJVEILFRR-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- ARCGXLSVLAOJQL-UHFFFAOYSA-N anhydrous trimellitic acid Natural products OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000002601 radiography Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
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Classifications
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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
- 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
- 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
-
- 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
- D01F1/10—Other agents for modifying properties
-
- 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
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
- Y10S264/26—Composite fibers made of two or more materials
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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)
- Manufacturing & Machinery (AREA)
- Multicomponent Fibers (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
어느 한 영역이 테레프탈산, 이소프탈산, 디메틸 5- 소디오술포 이소프탈레이트를 포함하는 산과, 에틸렌글리콜, 디에틸렌글리콜, 폴리에틸렌글로콜을 포함하는 디올을 중합하여 형성된 수용성 중합물을 포함하는 수용성 폴리에스테르계 복합섬유를 포함하여 형성되는 용출형 편직물 제조방법을 제공한다.A water-soluble polyester-based polymer comprising a water-soluble polymer formed by polymerizing an acid containing terephthalic acid, isophthalic acid, dimethyl 5-sodiosulfoisophthalate, and a diol containing ethylene glycol, diethylene glycol, or polyethylene glycol A method for producing a release-type knitted fabric comprising a conjugate fiber.
Description
본 발명은 수용성 폴리에스테르계 복합섬유를 함유하는 용출형 편직물 제조방법에 관한 것으로서, 특히 CHDM과 같은 추가 성분없이 수용성을 발현할 수 있는 용출형 편직물 제조방법에 관한 것이다. The present invention relates to a process for producing a dissolution type knitted fabric containing a water-soluble polyester-based conjugate fiber, and more particularly to a process for producing a dissolution type knitted fabric capable of exhibiting water solubility without additional components such as CHDM.
일반적으로 수용성 폴리에스테르는 섬유, 접착제, 생분해 소재 등 다양한 분야에서 응용되고 있다. 특히 섬유분야에 있어서는 극세사를 제조하는 원료로 사용되는 경우도 있다. Generally, water-soluble polyesters are applied in various fields such as fibers, adhesives, and biodegradable materials. In particular, in the field of fibers, it may be used as a raw material for producing microfibers.
이러한 수용성 폴리에스테르는 제조하는 방법으로는 5-소듐설포이소프탈산 및 그 유도체을 사용하여 폴리에스테르 분자쇄중에 소듐설포네이트 염을 갖게 하여 수용화시키거나 디카르복실산을 글리콜성분과 반응시킨 후 트리멜리틱안하이드라이드 등과 다시 반응시켜 말단 및 분자쇄 중에 카르복실기를 도입시킨후 암모니아 및 아민류 등의 알칼리 성분으로 염을 형성시켜 수용화시키는 방법이 알려져 있다.Such water-soluble polyesters can be prepared by using 5-sodium sulfoisophthalic acid and derivatives thereof to obtain a sodium sulfonate salt in a polyester molecular chain to be hydrated or reacted with a glycol component, Melichtic hydride and the like to introduce a carboxyl group into the terminal and molecular chain and then to form a salt with an alkali component such as ammonia and amines to thereby allow the carboxyl group to be hydrolyzed.
구체적으로 대한민국 공개특허 1994-14494에서는 "디카르복실산에 글리콜 성분을 반응시켜서 되는 수용성 폴리에스테르 수지조성물에 있어서, 상기 디카르복실산에 글리콜성분을 반응시켜 제조된 에스테르올리고머에 디카르복실산 1몰에 대하여 부틸테트라카르복실산 단독 또는 트리멜리틱안하이드라이드와의 혼합물을 3∼10몰비 투입하여 제조된 것으로 점도가 0.15∼0.8dl/g이고, 산가가 40∼100㎎/g인 것을 특징으로 하는 수용성 폴리에스테르 수지조성물"을 제안하고 있다. Specifically, Korean Patent Laid-Open Publication No. 1994-14494 discloses a water-soluble polyester resin composition obtained by reacting a glycol component with a dicarboxylic acid, wherein an ester oligomer prepared by reacting a glycol component with the dicarboxylic acid is reacted with a dicarboxylic acid 1 And having a viscosity of from 0.15 to 0.8 dl / g and an acid value of from 40 to 100 mg / g, in the form of a mixture of butyltetracarboxylic acid alone or trimellitic acid hydride in a molar ratio of 3 to 10, Soluble polyester resin composition "
또 국제공개특허 WO2002/57334에서는 "a) 1,4-사이클로헥산디메타놀 (CHDM) 및 디카복실산을 포함하는 수성 또는 메타놀성 슬러리를 제조하되, 상기 슬러리를 CHDM의 융점 미만의 온도로 유지하는 단계, b) 슬러리를 반응기에 공급하는 단계, c) 에스테르화를 수행하기에 충분한 온도 및 압력에서, 선택적으로는 적합한 촉매의 존재하에 슬러리를 에스테르화하는 단계, d) 예비중합체를 형성하는 단계, 및 e) 중축합을 수행하기에 충분한 온도 및 압력에서 적합한 촉매의 존재하에 예비중합체를 중축합하여 폴리에스테르를 형성하는 단계를 포함하는 폴리에스테르의 제조 방법"을 제안하면서 CHDM을 포함하는 수용성 폴리에스테르의 제조방법을 제안하고 있다. WO2002 / 57334 discloses a process for preparing an aqueous or methanolic slurry comprising a) 1,4-cyclohexanedimethanol (CHDM) and dicarboxylic acid, maintaining the slurry at a temperature below the melting point of CHDM , b) feeding the slurry to a reactor, c) esterifying the slurry, optionally at a temperature and pressure sufficient to effect the esterification, in the presence of a suitable catalyst, d) forming a prepolymer, and e) polycondensing the prepolymer in the presence of a suitable catalyst at a temperature and pressure sufficient to effect polycondensation to form the polyester, "proposes a process for preparing a water soluble polyester comprising CHDM .
상기 개시된 기술은 CHDM을 추가하는 것은 Tg를 높이기 위함인데, 실질적으로 Tg에 큰 영향을 미치지도 않으며, 감량가공을 하는 경우 감량률이 저하되는 문제점이 있었다.
The above-described technique is to increase the Tg by adding CHDM, but it does not substantially affect the Tg substantially, and there is a problem that the weight loss rate is reduced when the weight reduction processing is performed.
본 발명은 상기와 같은 문제를 해결하기 위해, CHDM 이나 아민기등 종래 수용성을 발현하기 위해 포함되는 성분을 제거하고도 수용성을 발현할 수 있는 수용성 폴리에스테르계 복합섬유를 함유하는 용출형 편직물 제조방법을 제공하는데 있다.
또한 본 발명은 수용단계 내지 감량가공이 용이한 수용성 폴리에스테르계 복합섬유를 함유하는 용출형 편직물 제조방법을 제공하는데 있다. Disclosure of the Invention In order to solve the above problems, the present invention provides a process for producing a dissolution type knitted fabric comprising a water-soluble polyester-based conjugate fiber capable of exhibiting water solubility even when a component contained in CHDM, .
Another object of the present invention is to provide a process for producing a release-type knitted fabric comprising a water-soluble polyester-based composite fiber which is easy to be handled or processed in a reduced amount.
삭제delete
상기 목적을 달성하기 위해 본 발명은 복합섬유에 있어서, 어느 한 영역이 테레프탈산, 이소프탈산, 디메틸 5- 소디오술포 이소프탈레이트를 포함하는 산과, 에틸렌글리콜, 디에틸렌글리콜, 폴리에틸렌글로콜을 포함하는 디올을 중합하여 형성된 수용성 폴리에스테르계 중합물을 포함하는 수용성 폴리에스테르계 복합섬유를 제공한다.In order to attain the above object, the present invention provides a conjugate fiber characterized in that any one region is composed of an acid containing terephthalic acid, isophthalic acid, dimethyl 5-sodiosulfoisophthalate, and an acid including ethylene glycol, diethylene glycol, polyethylene glycol A water-soluble polyester-based composite fiber comprising a water-soluble polyester-based polymer formed by polymerizing a diol.
또한 본 발명은 상기 중합시 비스-β-히드록시에틸테레프탈레이트가 더 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber comprising bis-beta-hydroxyethyl terephthalate at the time of polymerization.
또한 본 발명은 상기 중합시 반응촉매, 소포제, 산화방지제, 열안정제로 이루어진 군에서 1 이상 선택된 첨가제가 더 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber comprising at least one additive selected from the group consisting of a reaction catalyst, a defoaming agent, an antioxidant, and a heat stabilizer.
또한 본 발명은 상기 산의 투입량으로 테레프탈산이 60 내지 70몰%, 이소프탈산이 20 내지 30몰%, 디메틸 5- 소디오술포 이소프탈레이트이 10 내지 20몰%인 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber having 60 to 70 mol% of terephthalic acid, 20 to 30 mol% of isophthalic acid and 10 to 20 mol% of dimethyl 5-sodium diisocyanate as an input amount of the acid.
또한 본 발명은 상기 디올의 투입량으로 에틸렌글리콜이 60 내지 90몰%, 디에틸렌글리콜이 10 내지 30몰%인 수용성 폴리에스테르계 복합섬유를 제공한다.Further, the present invention provides a water-soluble polyester-based composite fiber having an ethylene glycol content of 60 to 90 mol% and a diethylene glycol content of 10 to 30 mol% as an input amount of the diol.
또한 본 발명은 상기 폴리에틸렌글리콜의 분자량이 300 내지 2000(수평균분자량)이며, 중합물 중 5 내지 10중량%로 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based conjugate fiber wherein the polyethylene glycol has a molecular weight of 300 to 2000 (number average molecular weight) and 5 to 10% by weight of the polymer.
또한 본 발명은 상기 산과 디올이 1:1 내지 1:10 중량%의 비율로 중합되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber wherein the acid and the diol are polymerized in a ratio of 1: 1 to 1:10 wt%.
또한 본 발명은 상기 촉매가 중합물 중 0.1 내지 0.5중량%로 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber comprising the catalyst in an amount of 0.1 to 0.5 wt% of the polymer.
또한 본 발명은 상기 소포제가 중합물 중 0.01 내지 0.05중량%로 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber wherein the defoaming agent is contained in an amount of 0.01 to 0.05% by weight based on the weight of the polymer.
또한 본 발명은 상기 산화방지제가 중합물 중 500 내지 800ppm로 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber wherein the antioxidant is contained in an amount of 500 to 800 ppm of the polymer.
또한 본 발명은 상기 열안정제가 중합물 중 100 내지 500ppm로 포함되는 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber wherein the heat stabilizer is contained in an amount of 100 to 500 ppm of the polymer.
또한 본 발명은 상기 중합물의 고유점도(IV)가 0.450 내지 0650dl/g인 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based composite fiber having an intrinsic viscosity (IV) of 0.450 to 0650 dl / g.
또한 본 발명은 상기 중합물의 Tg가 35 내지 50℃인 수용성 폴리에스테르계 복합섬유를 제공한다.The present invention also provides a water-soluble polyester-based conjugate fiber having a Tg of 35 to 50 캜.
또한 본 발명은 상기 복합섬유가 분할형 또는 추출형일 수 있으며 상기 중합물이 복수개의 도메인이 분할된 파이(segmented pie), 해도(island in sea), 시스 코어(sheath core) 사이드바이사이드(side by side) 형상, 평행형, 방사형, 다심형, 모자이크상, 매트릭스-분산형, 성운형 등으로 이루어진 군에서 수용성 폴리에스테르계 복합섬유를 제공한다.In addition, the present invention is characterized in that the composite fibers may be split or extracted and the polymerisation may be divided into a plurality of segmented pie, island in sea, sheath core side by side Water-soluble polyester-based conjugated fibers are provided in the group consisting of water-absorbent resin, water-absorbent resin, water-absorbent resin,
또한 본 발명은 수용성 폴리에스테르계 복합섬유의 제조방법에 있어서, 디메틸 5- 소디오술포 이소프탈레이트과 에틸렌글리콜을 반응촉매와 혼합하는 단계; 상기 혼합 후 비스-β-히드록시에틸테레프탈레이트를 투입하는 단계; 상기 투입 후 테레프탈산, 이소프탈산, 디메틸글리콜을 반응하는 단계; 상기 반응물에 폴리에틸렌글리콜을 투입하는 단계; 상기 반응물에 소포제, 산화방지제, 열안정제로 이루어진 군에서 1이상 선택된 첨가제를 투입하는 단계; 상기 중합물을 포함하여 복합방사하는 단계를 포함하는 수용성 폴리에스테르계 복합섬유의 제조방법을 제공한다.The present invention also provides a method for producing a water-soluble polyester-based composite fiber, comprising the steps of: mixing dimethyl 5-sodiosulfoisophthalate and ethylene glycol with a reaction catalyst; Introducing bis -? - hydroxyethyl terephthalate after the mixing; Reacting terephthalic acid, isophthalic acid, and dimethyl glycol after the charging; Introducing polyethylene glycol into the reaction product; Adding at least one additive selected from the group consisting of antifoaming agents, antioxidants, and heat stabilizers to the reactants; The present invention also provides a method for producing a water-soluble polyester-based conjugated fiber,
또한 본 발명은 상기 디메틸 5- 소디오술포 이소프탈레이트과 에틸렌글리콜의 중량 % 비가 1:8 내지 1:12인 방법을 제공한다.The present invention also provides a process wherein the weight ratio of dimethyl 5-sodiosulfoisophthalate to ethylene glycol is from 1: 8 to 1:12.
또한 본 발명은 상기 테레프탈산과 디메틸글리콜의 중량% 비는 1:1 내지 1:1.5인 방법을 제공한다.The present invention also provides a process wherein the weight% ratio of terephthalic acid and dimethyl glycol is from 1: 1 to 1: 1.5.
또한 본 발명은 상기 이소프탈산과 디메틸글리콜의 중량% 비는 1:1 내지 1:1.5인 방법을 제공한다. The present invention also provides a process wherein the weight% ratio of isophthalic acid to dimethyl glycol is from 1: 1 to 1: 1.5.
본 발명의 일실시예에 의한 복합섬유는 수용성을 발현하기 위해 CHDM이나 아민기 등 별도의 조성성분 없이 수용성을 발현하며, 감량가공이 용이하고 감량율이 높은 장점이 있다. The composite fiber according to an embodiment of the present invention is water-soluble without any additional constituent components such as CHDM or amine groups in order to exhibit water-solubility, has advantages of easy weight reduction and high weight loss rate.
도 1은 본 발명의 바람직한 일실시예에 의한 중합물을 해성분으로 한 복합방사된 해도형 복합섬유의 단면 사진.
도 2는 본 발명의 바람직한 일실시예에 의한 중합물을 해성분으로 한 복합방사된 해도형 복합섬유의 감량 전 사진.
도 3은 본 발명의 바람직한 일실시예에 의한 중합물을 해성분으로 한 복합방사된 해도형 복합섬유의 감량 후 사진.
도 4는 본 발명의 바람직한 일실시예에 의한 중합물을 해성분으로 한 복합방사된 해도형 복합섬유로 편직한 편직물의 감량 가공 전 사진.
도 5는 도 2는 본 발명의 바람직한 일실시예에 의한 중합물을 해성분으로 한 복합방사된 해도형 복합섬유로 편직한 편직물의 감량 가공 후 사진.BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a cross-sectional photograph of a combined radiated sea-island conjugate fiber according to a preferred embodiment of the present invention as a sea component; FIG.
FIG. 2 is a photograph showing a weight loss of a composite radiated sea-island composite fiber obtained by using a polymer as a sea component in accordance with a preferred embodiment of the present invention.
FIG. 3 is a photograph of a sea-island conjugated composite fiber in the form of a sea salt as a polymeric material according to a preferred embodiment of the present invention.
FIG. 4 is a photograph of a knitted fabric knitted with a composite radiated sea-island composite fiber having a polymeric material as a sea component in accordance with a preferred embodiment of the present invention.
FIG. 5 is a photograph of a knitted fabric knitted with a combined radiated sea-island composite fiber in which a polymeric material is a sea component, according to a preferred embodiment of the present invention.
이하 본 발명의 바람직한 일실시예를 상세히 설명하기로 한다. 본 발명을 설명함에 있어, 관련된 공지기능 혹은 구성에 대한 구체적인 설명은 본 발명의 요지를 모호하지 않게 하기 위하여 생략한다.Hereinafter, a preferred embodiment of the present invention will be described in detail. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.
본 명세서에서 사용되는 정도의 용어 "약", "실질적으로" 등은 언급된 의미에 고유한 제조 및 물질 허용오차가 제시될 때 그 수치에서 또는 그 수치에 근접한 의미로 사용되고, 본 발명의 이해를 돕기 위해 정확하거나 절대적인 수치가 언급된 개시 내용을 비양심적인 침해자가 부당하게 이용하는 것을 방지하기 위해 사용된다.The terms "about "," substantially ", etc. used to the extent that they are used herein are intended to be taken to mean an approximation of, or approximation to, the numerical values of manufacturing and material tolerances inherent in the meanings mentioned, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.
본 발명에 의한 수용성 폴리에스테르계 복합섬유을 위한 중합물은 디올(diol)류, 산(acid)류 등을 포함할 수 있다. The polymeric material for the water-soluble polyester-based composite fiber according to the present invention may include diols, acids, and the like.
상기 산류로는 비제한적인 예로서 테레프탈산(TPA), 이소프탈산(IPA), 디메틸 5- 소디오술포 이소프탈레이트(DMS, Dimethyl 5-sodiosulfo Isophthalate)일 수 있다. 이 때 테레프탈산이 60 내지 70몰%, 이소프탈산이 20 내지 30몰%, 디메틸테레프탈산이 10 내지 20몰%로 산류를 구성할 수 있다. 또 디올류로는 비제한적인 예로서 에틸렌글리콜(EG), 디에틸렌글리콜(DEG), 폴리에틸렌글로콜(PEG)일 수 있다. 디올류로서 에틸렌글리콜이 60 내지 90몰%, 디에틸렌글리콜이 10 내지 30몰%로 이루어질 수 있다. Examples of the acids include, but not limited to, terephthalic acid (TPA), isophthalic acid (IPA), and dimethyl 5-sodiosulfo isophthalate (DMS). In this case, terephthalic acid accounts for 60 to 70 mol%, isophthalic acid accounts for 20 to 30 mol%, and dimethylterephthalic acid accounts for 10 to 20 mol%. The diols may be ethylene glycol (EG), diethylene glycol (DEG), or polyethylene glycol (PEG) as non-limiting examples. As the diols, ethylene glycol may be 60 to 90 mol% and diethylene glycol may be 10 to 30 mol%.
본 발명의 중합물을 제조하는 일실시예로서 우선 상기 디메틸 5- 소디오술포 이소프탈레이트 와 에틸렌글리콜을 1:8 내지 1:12의 중량% 비율로 혼합하여 중합을 개시한다 이 때 반응촉매를 전체 중합물에 약 0.1 내지 0.5중량%의 비율로 투입할 수 있다.In one embodiment of the present invention, dimethyl 5-sodiosulfoisophthalate and ethylene glycol are mixed in a weight ratio of 1: 8 to 1:12 by weight to initiate polymerization. At this time, To about 0.1 to 0.5% by weight.
상기 중합이 개시되면 에스테르화 반응을 위해 비스-β-히드록시에틸테레프탈레이트(BHET)를 추가적으로 혼합할 수 있다. 또 상기 중합물에 테레프탈산, 이소프탈산, 디에틸렌글리콜을 반응시켜 에스테르화 반응을 수행할 수 있다. 이 때 상기 테레프탈산과 디에틸렌글리콜의 혼합비는 약 1:1 내지 1:1.5, 상기 이소프탈산과 디에틸렌글리콜의 혼합비는 1:1 내지 1:1.5일 수 있다.
이후 축합중합을 위해 폴리에틸렌글리콜을 추가할 수 있고 상기 폴리에틸렌글리콜은 수평균분자량을 300 내지 2,000인 것이 바람직하며 투입량은 중합물 중 5 내지 10중량%로 포함될 수 있다. When the polymerization is initiated, bis-beta-hydroxyethyl terephthalate (BHET) may be further added for the esterification reaction. Further, the esterification reaction can be carried out by reacting the polymer with terephthalic acid, isophthalic acid and diethylene glycol. The mixing ratio of the terephthalic acid and the diethylene glycol may be about 1: 1 to 1: 1.5, and the mixing ratio of the isophthalic acid and the diethylene glycol may be 1: 1 to 1: 1.5.
Thereafter, polyethylene glycol may be added for the condensation polymerization, and the polyethylene glycol preferably has a number average molecular weight of 300 to 2,000, and the amount of the polyethylene glycol may be 5 to 10% by weight of the polymer.
삭제delete
이후 선택적으로 반응촉매, 소포제, 산화방지제, 열안정제로 이루어진 군에서 1 이상 선택된 첨가제가 더 포함될 수 있다. 이 때 소포제는 중합물 중 0.01 내지 0.05중량%로 포함될 수 있으며, 상기 산화방지제는 중합물 중 500 내지 800ppm로 포함될 수 있으며, 상기 열안정제는 중합물 중 100 내지 500ppm로 포함될 수 있다. Optionally, one or more additives selected from the group consisting of a reaction catalyst, a defoaming agent, an antioxidant, and a heat stabilizer. In this case, the defoaming agent may be included in the polymer in an amount of 0.01 to 0.05 wt%, and the antioxidant may be contained in the polymer in an amount of 500 to 800 ppm, and the heat stabilizer may be contained in the polymer in an amount of 100 to 500 ppm.
상기 중합물은 수용성으로 특히 복합섬유에 있어서 후에 감량가공을 통해 제거되는 경우 극세사를 제조할 수 있다. 이 때 상기 복합섬유는 분할형 또는 추출형으로 제조될 수 있고, 상기 중합물이 복수개의 도메인이 분할된 파이(segmented pie), 해도(island in sea), 시스 코어(sheath core) 또는 사이드바이사이드(side by side)단면 형상으로 배열된 것일 수 있으며, 단면형상이 평행형, 방사형, 다심형, 모자이크상, 매트릭스-분산형, 성운형 등 다양한 형태로 구현될 수 있다. The polymer is water-soluble and can be produced especially when the composite fiber is removed through a weight reduction process. At this time, the composite fiber may be produced in a split type or an extraction type, and the polymer may be a segmented pie, an island in sea, a sheath core, or a side by side side by side cross-sectional shape, and the cross-sectional shape may be implemented in various forms such as a parallel shape, a radial shape, a polygonal shape, a mosaic shape, a matrix-dispersive shape, and a nebula shape.
상기 중합물은 복합섬유에 있어서, 예를 들어 해도사의 경우 해성분으로 방사될 수 있다. 복합방사법은 이 기술분야의 통상의 지식을 가진 자가 채택할 수 있는 모든 방법을 포함한다.
The polymer can be spun into a conjugate fiber, for example, a sea component in the case of sea chart yarn. Complex radiography includes all methods that can be adopted by those of ordinary skill in the art.
이하 구체적 실시예로서 설명하기로 한다.Hereinafter, a specific embodiment will be described.
실시예 1Example 1
디메틸 5- 소디오술포 이소프탈레이트과 에틸렌글리콜을 투입하여 반응을 개시하고 비스-β-히드록시에틸테레프탈레이트, 테레프탈산, 이소프탈산, 디에틸렌글리콜을 투입하여 에스테르화 반응을 개시하였다. Dimethyl 5-sodiosulfoisophthalate and ethylene glycol were added to initiate the reaction and bis-β-hydroxyethyl terephthalate, terephthalic acid, isophthalic acid and diethylene glycol were added to initiate the esterification reaction.
이 때 디메틸 5- 소디오술포 이소프탈레이트는 분자량이 약 300인 것으로 산류 전체로 10몰%로 투입하였고, 테레프탈산은 분자량 약 150인 것으로 산류 전체로 70몰%로 투입하였고, 이소프탈산은 분자량 약 150인 것으로 산류 전체로 20몰%로 투입하였다. In this case, dimethyl 5-sodiosulfoisophthalate had a molecular weight of about 300 and was added in an amount of 10 mol% as a whole. Terephthalic acid had a molecular weight of about 150 and was added in an amount of 70 mol% based on the total acid. Isophthalic acid had a molecular weight of about 150 By weight and 20% by mole in total.
또 에틸렌글리콜은 분자량 60인 것으로 디올류 기준 70몰%를, 디에틸렌글리콜은 분자량 110인 것으로 30%를 투입하였다. Further, ethylene glycol had a molecular weight of 60, which was 70 mol% based on the diol, and diethylene glycol had a molecular weight of 110, which was 30%.
이후 축합중합을 위해 폴리에틸렌글리콜을 투입하면서 소포제, 산화방지제, 열안정제를 투입하였다. 상기 폴리에틸렌글리콜은 분자량 300으로 전체 중합물에서 7중량%를 차지하게 투입하였고, 기타 소포제는 0.02중량%, 산화방지제는 500ppm, 열안정제는 200ppm을 추가하였다. Then, polyethylene glycol was added for condensation polymerization, and defoamer, antioxidant and heat stabilizer were added. The polyethylene glycol had a molecular weight of 300 and was added to account for 7 wt% of the total polymer. Other defoaming agents were added in an amount of 0.02 wt%, antioxidants in an amount of 500 ppm, and heat stabilizers in an amount of 200 ppm.
상기 중합물에 대하여 IV와 Tg를 측정하였다.IV and Tg were measured for the polymer.
또 상기 중합물을 해성분으로 하고 통상의 폴리에스테르 조성물을 도성분으로 하여 해도사로 복합방사한 후 이를 편직하여 일반수에 감량처리하여 감량률을 측정하였다.
In addition, the polymer was used as a sea component, and a conventional polyester composition was used as a casting component, followed by composite spinning using a sea shell, kneaded, and then subjected to weight loss treatment to measure the weight loss rate.
실시예 2Example 2
실시예 1과 동일하되, 폴리에틸렌글리콜의 분자량이 1,000인 것을 사용하였다.
A polyethylene glycol having a molecular weight of 1,000 was used as in Example 1.
실시예 3Example 3
상기 실시예 1과 동일하되, 에틸렌글리콜의 함량을 90몰%, 디에틸렌글리콜의 함량을 10몰%로 하였다.
The same procedure as in Example 1 was carried out except that the content of ethylene glycol was 90 mol% and the content of diethylene glycol was 10 mol%.
위와 같이 본 발명에 의한 복합섬유는 우수한 감량율을 나타냈다.As described above, the conjugate fiber according to the present invention exhibited a good weight loss rate.
이상에서 설명한 본 발명은 전술한 실시예 및 첨부된 도면에 의해 한정되는 것이 아니고, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환, 변형 및 변경이 가능함은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에게 있어서 명백할 것이다.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.
Claims (18)
(a) 디메틸 5- 소디오술포 이소프탈레이트와 에틸렌글리콜을 1:8 내지 1:12의 혼합비로 준비하여 반응촉매와 혼합하는 단계;
(a) 상기 혼합 후 비스-β-히드록시에틸테레프탈레이트를 투입하는 단계;
(b) 상기 투입 후 테레프탈산과 디에틸렌글리콜을 1:1 내지 1:1.5 비율로, 이소프탈산과 디에틸렌글리콜을 1:1 내지 1:1.5의 비율로 혼합 후 반응하는 단계;
(c) 상기 반응물에 폴리에틸렌글리콜을 투입하는 단계;
(d) 상기 폴리에틸렌글리콜 투입물에 소포제, 산화방지제, 열안정제로 이루어진 군에서 1이상 선택된 첨가제를 투입하여 수용성 중합물을 형성하는 단계;
(e) 상기 수용성 중합물을 포함하는 수용성 폴리에스테르계 복합섬유를 제조하는 단계;
(f) 상기 복합섬유를 포함하는 편직물을 제조하는 단계;
(g) 상기 편직물을 열수에 용출하여 편직물에서 수용성 중합물이 포함되는 영역을 88% 이상 감량하는 단계를 포함하되,
산의 투입량으로 테레프탈산이 60 내지 70몰%, 이소프탈산이 20 내지 30몰%, 디메틸 5- 소디오술포 이소프탈레이트이 10 내지 20몰%인 것을 특징으로 하는 용출형 편직물의 제조방법.A method for producing a release-type knitted fabric formed by including a water-soluble polyester-based composite fiber containing a water-soluble polymer,
(a) preparing dimethyl 5-sodiosulfoisophthalate and ethylene glycol at a mixing ratio of 1: 8 to 1:12 and mixing with a reaction catalyst;
(a) adding bis -? - hydroxyethyl terephthalate after the mixing;
(b) reacting terephthalic acid and diethylene glycol in a ratio of 1: 1 to 1: 1.5, after mixing, of isophthalic acid and diethylene glycol in a ratio of 1: 1 to 1: 1.5;
(c) introducing polyethylene glycol into the reactant;
(d) introducing at least one additive selected from the group consisting of antifoaming agents, antioxidants, and heat stabilizers into the polyethylene glycol feed to form a water soluble polymer;
(e) preparing a water-soluble polyester-based composite fiber comprising the water-soluble polymer;
(f) fabricating a knit fabric comprising the composite fibers;
(g) eluting the knitted fabric in hot water to reduce the area containing the water soluble polymer in the knitted fabric by 88% or more,
Wherein the amount of acid to be added is 60 to 70 mol% of terephthalic acid, 20 to 30 mol% of isophthalic acid, and 10 to 20 mol% of dimethyl 5-sodiosulfoisophthalate.
상기 폴리에틸렌글리콜의 분자량은 300 내지 2000(수평균분자량)이며, 수용성 중합물 중 5 내지 10중량%로 포함되는 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the polyethylene glycol has a molecular weight of 300 to 2000 (number average molecular weight) and 5 to 10% by weight of the water-soluble polymer.
상기 반응촉매는 중합물 중 0.1 내지 0.5중량%로 포함되는 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the reaction catalyst is contained in an amount of 0.1 to 0.5% by weight of the polymer.
상기 소포제는 중합물 중 0.01 내지 0.05중량%로 포함되는 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the defoaming agent comprises 0.01 to 0.05% by weight of the polymer.
상기 산화방지제는 중합물 중 500 내지 800ppm로 포함되는 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the antioxidant is contained in the polymer in an amount of 500 to 800 ppm.
상기 열안정제는 중합물 중 100 내지 500ppm로 포함되는 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the heat stabilizer is contained in 100 to 500 ppm of the polymer.
상기 중합물의 고유점도(IV)가 0.450 내지 0650dl/g인 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the intrinsic viscosity (IV) of the polymer is 0.450 to 0650 dl / g.
상기 중합물의 Tg가 35 내지 50℃인 용출형 편직물의 제조방법.The method according to claim 1,
Wherein the polymer has a Tg of 35 to 50 占 폚.
상기 복합섬유는 분할형 또는 추출형일 수 있으며 상기 중합물이 복수개의 도메인이 분할된 파이(segmented pie), 해도(island in sea), 시스 코어(sheath core) 사이드바이사이드(side by side) 형상, 평행형, 방사형, 다심형, 모자이크상, 매트릭스-분산형, 성운형 등으로 이루어진 군에서 선택되는 것인 용출형 편직물의 제조방법.The method according to claim 1,
The composite fiber may be split or extracted and the polymerisation may be divided into a plurality of segmented pie, island in sea, sheath core side by side shape, parallel Wherein the yarn is selected from the group consisting of yarns, yarns, yarns, yarns, yarns, yarns, yarns, radial yarns, multicore yarns, mosaic yarns, matrix-dispersed yarns, and nebula yarns.
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| KR102115405B1 (en) * | 2013-11-28 | 2020-06-08 | 도레이첨단소재 주식회사 | Complex fiber including water-soluble polyester with improved heat resistance |
| KR102288463B1 (en) * | 2014-12-26 | 2021-08-09 | 도레이첨단소재 주식회사 | Hot-water elutable polyester resin having high heat-resistance and weight loss-rate, and Hot-water elutable polyester composite fiber |
| KR101910430B1 (en) * | 2016-10-07 | 2018-10-23 | 도레이케미칼 주식회사 | Composite fiber for manufacturing flame-retardant hollow fiber for car interior materals and Flame-retardant hollow fiber for car interior materals |
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