KR20160077238A - Method for increasing pH of spandex by using inorganic additives - Google Patents

Method for increasing pH of spandex by using inorganic additives Download PDF

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KR20160077238A
KR20160077238A KR1020140185663A KR20140185663A KR20160077238A KR 20160077238 A KR20160077238 A KR 20160077238A KR 1020140185663 A KR1020140185663 A KR 1020140185663A KR 20140185663 A KR20140185663 A KR 20140185663A KR 20160077238 A KR20160077238 A KR 20160077238A
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spandex
polymer
present
fabric
inorganic additive
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홍수림
강연수
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주식회사 효성
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Priority to PCT/KR2015/012404 priority patent/WO2016104955A1/en
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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
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • 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
    • 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
    • D01D5/04—Dry spinning methods
    • 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
    • D01D5/06—Wet spinning methods
    • 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
    • D01D5/08—Melt spinning methods
    • 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
    • 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
    • D01F1/103—Agents inhibiting growth of microorganisms
    • 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
    • D10B2401/00—Physical properties
    • D10B2401/13—Physical properties anti-allergenic or anti-bacterial

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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)
  • Artificial Filaments (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

본 발명은 무기 첨가제를 이용한 스판덱스 원단의 pH 향상 방법으로서, 스판덱스 중합물에 무기 첨가제, 예를 들면 산화칼슘(CaO)을 해당 중합물의 고형분을 기준으로 약 0.5중량% 내지 약 10.0중량%를 첨가하여서 되는 것을 특징으로 한다.The present invention relates to a method for improving the pH of a spandex fabric using an inorganic additive, wherein an inorganic additive such as calcium oxide (CaO) is added to the spandex polymer in an amount of about 0.5 wt% to about 10.0 wt% based on the solids content of the polymer .

Description

무기 첨가제를 이용한 스판덱스 원단의 pH의 향상방법{Method for increasing pH of spandex by using inorganic additives}TECHNICAL FIELD The present invention relates to a method for improving the pH of a spandex fabric using an inorganic additive,

본 발명은 무기 첨가제를 이용한 스판덱스 원단의 pH 향상방법에 관한 것이다. 더욱 상세하게, 본 발명은 무기 첨가제인 산화칼슘(CaO)을 첨가하여 스판덱스 원단의 pH의 수준을 증가시키는 방법에 관한 것이다. The present invention relates to a method for improving the pH of a spandex fabric using an inorganic additive. More particularly, the present invention relates to a method for increasing the level of pH of a spandex fabric by adding an inorganic additive, calcium oxide (CaO).

스판덱스 섬유는 일반적으로 폴리우레탄 수지 조성물인 방사용액을 노즐을 통해 압출하고, 용매는 증발 및 건조하기 위해 가열기체를 도입하는 건식방사; 방사 수욕을 통과시켜 용매를 용출시키면서 동시에 폴리머를 응고시키는 습식방사, 아민 쇄연장제를 함유하는 반응액 중에 이소시아네이트를 지닌 전구체(prepolymer) 용액을 노즐을 통해 압출시켜 쇄연장 반응시키는 화학방사, 또는 폴리우레탄 수지 조성물을 가열용융상태에서 노즐을 통해 압출하고 냉각시키는 용융방사를 통해 제조된다.Spandex fibers are generally prepared by extruding a spinning liquid, a polyurethane resin composition, through a nozzle, the solvent being dry spinning to introduce a heating gas to evaporate and dry; A chemical spinning process in which a prepolymer solution containing isocyanate is extruded through a nozzle to effect a chain extension reaction in a reaction solution containing wet spinning or amine chain extender which coagulates the polymer while allowing the solvent to pass through a spinning water bath, The urethane resin composition is produced by melt spinning in which the composition is extruded through a nozzle in a heated molten state and cooled.

이와 같은 스판덱스 섬유 원단의 pH는 가공 원단에서 요구되는 사양으로 유해 수준을 확인하는 척도이다. 대부분 약산성에서 중성까지의 값이 요구된다. The pH of such a spandex fiber fabric is a measure of the level of harmfulness required by the fabric. Mostly, values from weakly acidic to neutral are required.

종래에 스판덱스 원단을 상온의 물로 처리하는 경우(ISO 규격)에는 별 문제가 없지만, 원단을 끓는 물에 처리(미국 규격인 AATCC)할 경우에는 pH가 1 정도 수준으로 낮아지는 문제점이 발생하고 있다.Conventionally, there is no problem in the case of processing the spandex fabric with water at normal temperature (ISO standard), but when the fabric is treated with boiling water (AATCC, US standard), the pH is lowered to about 1 level.

따라서, 본 발명은 스판덱스 원단을 끓는 물에서 처리하여도 상기와 같은 문제가 발생하지 않도록 스판덱스 원단의 pH를 향상시키기 위한 방법을 제공하는데 그 목적이 있다. Accordingly, it is an object of the present invention to provide a method for improving the pH of a spandex fabric so that the problem does not occur even if the spandex fabric is treated with boiling water.

본 발명의 무기 첨가제를 이용한 스판덱스 원단의 pH 향상 방법은 A method for improving the pH of a spandex fabric using the inorganic additive of the present invention

스판덱스 중합물에 무기 첨가제, 예를 들면 산화칼슘(CaO)을 해당 중합물의 고형분을 기준으로 약 0.5 중량% 내지 약 10.0중량%를 첨가하여서 되는 것을 특징으로 한다.And an inorganic additive such as calcium oxide (CaO) is added to the spandex polymer in an amount of about 0.5 wt% to about 10.0 wt% based on the solid content of the polymer.

본 발명에 따른 무기 첨가제, 예를 들면 산화칼슘을 스판덱스 중합물에 첨가하여 스판덱스 섬유를 제조함으로써 원사의 pH를 약 5.4 내지 약 5.6 범위까지 향상시킬 수 있다. 그리고 편포(스판덱스 20% 함유)의 경우는 약 4.6 내지 약 4.8까지 향상시킬 수 있다. The pH of the yarn can be increased to a range of from about 5.4 to about 5.6 by preparing the spandex fiber by adding an inorganic additive according to the present invention, for example calcium oxide, to the spandex polymer. And about 4.6 to about 4.8 in the case of a woven fabric (containing 20% of spandex).

이와 같은 본 발명을 다음에서 상세하게 설명하기로 하며, 다음의 실시예는 단지 예시하기 위한 것으로 이를 한정하고자 하는 것은 아니다. The present invention will be described in detail below, and the following embodiments are for illustrative purposes only and do not limit the present invention.

본 발명에서 사용하는 용어 "스판덱스"는 섬유 형성 물질이 85중량% 이상으로 이루어진 장쇄 합성 엘라스토머인인조 섬유를 말한다. 폴리우레탄을 폴리에테르 글리콜, 디이소시아네이트의 혼합물 및 사슬 연장제로부터 제조한 후, 상술한 바와 같이 용융 방사, 건식 방사 또는 습식 방사하여 섬유를 형성한다.As used herein, the term "spandex" refers to man-made fibers which are long-chain synthetic elastomers having a fiber-forming material content of at least 85% by weight. After the polyurethane is prepared from a polyether glycol, a mixture of diisocyanates and a chain extender, fibers are formed by melt spinning, dry spinning or wet spinning as described above.

본 발명의 스판덱스 섬유 제조에 사용되는 폴리우레탄우레아 중합체는 당 분야에 공지된 바와 같이 유기디이소시아네이트 및 고분자 디올을 반응시켜 폴리우레탄우레아 프리폴리머를 제조한 후, 이를 유기용매에 용해시킨 후 디아민과 모노아민을 반응시키는 것에 의해 제조한다.The polyurethane-urea polymer used in the production of the spandex fiber of the present invention may be produced by reacting an organic diisocyanate and a polymeric diol to prepare a polyurethane-urea prepolymer, dissolving the polyurethaneurea prepolymer in an organic solvent, In an organic solvent.

본 발명에서 사용되는 상기 유기 디이소시아네이트로는 4,4’-디페닐메탄디이소시아네이트, 헥사메틸렌디이소시아네이트, 톨루엔디이소시아네이트, 부틸렌디이소시아네이트, 수소화된 P,P-메틸렌디이소시아네이트 등이 있으며, 상기 고분자 디올로는 폴리테트라메틸렌에테르글리콜, 폴리프로필렌글리콜, 폴리카보네이트디올 등이 사용될 수 있다. 상기 디아민류는 사슬연장제로서 사용되며, 이의 예로는 에틸렌디아민, 프로필렌디아민, 하이드라진, 1,2-디아미노프로판 등이 있으며, 본 발명에서는 특히 에틸렌디아민과 1,2-디아미노프로판을 약 80몰%와 약 20몰%의 비율로 혼합된 것을 사용할 수 있다. 또한 모노아민은 사슬종결제로서 사용되며, 이의 예로는 디에틸아민, 모노에탄올아민, 디메틸아민 등이 있다.Examples of the organic diisocyanate used in the present invention include 4,4'-diphenylmethane diisocyanate, hexamethylene diisocyanate, toluene diisocyanate, butylene diisocyanate, hydrogenated P, P-methylene diisocyanate, As the diol, polytetramethylene ether glycol, polypropylene glycol, polycarbonate diol and the like can be used. Examples of the diamines include ethylenediamine, propylenediamine, hydrazine, 1,2-diaminopropane, and the like. In the present invention, ethylenediamine and 1,2-diaminopropane are used in an amount of about 80 Mol% and about 20 mol%. Monoamines are also used as chain terminators, examples of which include diethylamine, monoethanolamine, dimethylamine, and the like.

본 발명에서는 자외선, 대기 스모그, 스판덱스 가공 공정 중 열처리 등에서 스판덱스의 변색, 물성 저하를 방지하기 위하여 산화방지제, 무기 내염소제 및 내광제 등을 첨가하여 폴리우레탄우레아 방사원액을 제조할 수 있다.In the present invention, a polyurethane-urea spinning solution can be prepared by adding an antioxidant, a chlorine-containing agent in an inorganic salt, and an anti-fogging agent in order to prevent discoloration and deterioration of properties of spandex during heat treatment during ultraviolet rays, atmospheric smog, and spandex processing.

그 후에, 생성된 폴리우레탄우레아 용액을 습식 또는 건식 방사하여 스판덱스를 형성할 수 있다.Thereafter, the resultant polyurethane-urea solution can be wet-laid or dry-laid to form a spandex.

본 발명의 한 구현예에 의하면, 스판덱스의 중합물에 산화칼슘(CaO)을 첨가할 경우에 원단의 pH 수준이 증가하는 효과를 알게 된 것으로, 무기 첨가제를, 예를 들면 산화칼슘(CaO)을 스판덱스 중합물에 해당 중합물의 고형분을 기준으로 약 0.5중량% 내지 약 10.0중량%를 첨가하는 것에 의해 달성을 한다.According to one embodiment of the present invention, when the calcium oxide (CaO) is added to the polymer of the spandex, the effect of increasing the pH level of the fabric is found. The inorganic additive is, for example, To about 0.5 wt.% To about 10.0 wt.%, Based on the solids content of the polymer.

본 발명에서 상기 무기 첨가제를 0.5중량% 미만으로 적용할 경우에는 pH의 향상을 기대할 수 없고, 반대로 10중량%를 초과하여 적용할 경우에는 강도 및 신도, 모듈러스 등의 물성이 저하되는 문제를 발생하게 되므로 상기 범위로 첨가하는 것이 바람직하다.In the present invention, when the inorganic additive is used in an amount of less than 0.5% by weight, improvement of the pH can not be expected. On the other hand, when the inorganic additive is used in an amount exceeding 10% by weight, the properties such as strength, elongation and modulus are lowered Therefore, it is preferable to add in the above range.

이와 같은 본 발명을 실시예와 비교예를 들어 상세히 설명하면 다음과 같다. Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples.

실시예 1Example 1

스판덱스 중합물에 산화칼슘을 3.0중량%를 첨가하여 스판덱스 원사를 제조하였다. 제조된 스판덱스 원사의 pH를 측정한 결과 초기에는 10.4이었고, 정련 후에는 9.4, 가공 후에는 5.4를 나타내었다. A spandex yarn was prepared by adding 3.0 weight% of calcium oxide to the spandex polymer. The measured pH of the prepared spandex yarn was 10.4 at the beginning, 9.4 after the refining, and 5.4 after the processing.

실시예들 및 비교예들에서 pH의 측정은 KSK ISO 3071 방법으로 측정하였다. 즉, 시료 2g에 상온 증류수 100ml를 넣고 쉐이킹 플레이트(Shaking Plate)에서 2시간 동안 처리한 후에 시료를 제거하고 pH를 측정하였다. In the examples and comparative examples, the pH was measured by the KSK ISO 3071 method. That is, 100 ml of distilled water at room temperature was added to 2 g of the sample, treated for 2 hours in a shaking plate, and then the sample was removed and the pH was measured.

실시예 2Example 2

스판덱스 중합물에 산화칼슘을 5.0중량%를 첨가하여 스판덱스 원사를 제조하였다. 제조된 스판덱스 원사의 pH를 측정한 결과 초기에는 10.4이었고, 정련 후에는 9.4, 가공 후에는 5.6를 나타내었다. A spandex yarn was prepared by adding 5.0 wt% of calcium oxide to the spandex polymer. The measured pH of the prepared spandex yarn was 10.4 at the beginning, 9.4 after the refining, and 5.6 after the processing.

비교예 1Comparative Example 1

시판 중인 스판덱스 원사(본 출원인의 고내염소성(H350S) 원사)의 pH를 측정한 결과 초기에는 7.3 이었고, 정련 후에는 5.2, 가공 후에는 4.1을 나타내었다. The pH of the commercially available spandex yarn (H350S yarn of the present applicant) was measured to be 7.3 at the initial stage, 5.2 after the scouring and 4.1 after the scouring.

실시예 3Example 3

실시예 1에서 제조한 스판덱스 원사를 20% 함유하는 편포를 제작하였다. 제조된 편포의 pH를 측정한 결과 초기에는 6.6이었고, 정련 후에는 4.6, 가공 후에는 4.6을 나타내었다.A knitted fabric containing 20% of the spandex yarn prepared in Example 1 was produced. As a result of measuring the pH of the prepared knitted fabric, it was 6.6 at the initial stage, 4.6 after the refining and 4.6 after the processing.

실시예 4Example 4

실시예 2에서 제조한 스판덱스 원사를 20% 함유하는 편포를 제작하였다. 제조된 편포의 pH를 측정한 결과 초기에는 6.4이었고, 정련 후에는 4.8, 가공 후에는 4.8을 나타내었다.A knitted fabric containing 20% of the spandex yarn prepared in Example 2 was produced. As a result of measuring the pH of the prepared knitted fabric, it was 6.4 at the initial stage, 4.8 after the refining, and 4.8 after the processing.

비교예 2Comparative Example 2

비교예 1에서 제조한 스판덱스 원사를 20% 함유하는 편포를 제작하였다. 제조된 편포의 pH를 측정한 결과 초기에는 5.8이었고, 정련 후에는 4.2, 가공 후에는 4.2을 나타내었다.
A knitted fabric containing 20% of the spandex yarn prepared in Comparative Example 1 was produced. As a result of measuring the pH of the prepared knitted fabric, it was found to be 5.8 at the initial stage, 4.2 after the scouring and 4.2 after the scouring.

Claims (1)

유기디이소시아네이트와 고분자 디올을 반응시켜서 플리폴러미를 수득하고, 이것을 디아민과 반응시켜서 폴리우레탄 용액을 수득한 후 건식 또는 습식방사하여 스판덱스사를 제조하는 방법에서,
폴리우레탄 용액의 중합물에 무기 첨가제로서 산화칼슘(CaO)을 해당 중합물의 고형분을 기준으로 0.5중량% 내지 10.0중량%를 첨가한 후 건식 또는 습식 방사하여서 되는 것을 특징으로 하는 방법.
In a process for producing a spandex yarn by reacting an organic diisocyanate with a polymer diol to obtain a polypolymer and reacting it with a diamine to obtain a polyurethane solution followed by dry or wet spinning,
Characterized in that calcium fluoride (CaO) is added to the polymer of the polyurethane solution as an inorganic additive in an amount of 0.5% by weight to 10.0% by weight based on the solids content of the polymerized product, followed by dry or wet spinning.
KR1020140185663A 2014-12-22 2014-12-22 Method for increasing pH of spandex by using inorganic additives Ceased KR20160077238A (en)

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KR20190012400A (en) * 2017-07-27 2019-02-11 주식회사 나노텍세라믹스 An additive slurry for the production of polyurethane-urea elastic fibers

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EP0738159A1 (en) * 1993-12-10 1996-10-23 The Procter & Gamble Company pH-MODIFIED POLYMER COMPOSITIONS WITH ENHANCED BIODEGRADABILITY
KR100239204B1 (en) * 1995-06-23 2000-01-15 야마모토 카즈모토 Polyurethane Elastic Fiber and Manufacturing Method thereof
KR100225605B1 (en) * 1995-12-29 1999-10-15 전원중 Method of manufacturing the spandex yarn
JP2003113533A (en) * 2001-10-04 2003-04-18 Toyobo Co Ltd Polyurethane elastic fiber
JP2003113303A (en) * 2001-10-04 2003-04-18 Toyobo Co Ltd Polyurethane composition and polyurethane elastic fiber

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190012400A (en) * 2017-07-27 2019-02-11 주식회사 나노텍세라믹스 An additive slurry for the production of polyurethane-urea elastic fibers
WO2019022532A3 (en) * 2017-07-27 2019-05-02 주식회사 나노텍세라믹스 Additive slurry for polyurethane-urea elastic fiber production

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