KR0132401B1 - Process for manufacturing a polyester fiber containing small amounts of oligomer - Google Patents

Process for manufacturing a polyester fiber containing small amounts of oligomer

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Publication number
KR0132401B1
KR0132401B1 KR1019930021592A KR930021592A KR0132401B1 KR 0132401 B1 KR0132401 B1 KR 0132401B1 KR 1019930021592 A KR1019930021592 A KR 1019930021592A KR 930021592 A KR930021592 A KR 930021592A KR 0132401 B1 KR0132401 B1 KR 0132401B1
Authority
KR
South Korea
Prior art keywords
oligomer
polyester
low
organic solvent
manufacturing
Prior art date
Application number
KR1019930021592A
Other languages
Korean (ko)
Other versions
KR950011658A (en
Inventor
이학수
정우원
김영준
Original Assignee
하기주
주식회사코오롱
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by 하기주, 주식회사코오롱 filed Critical 하기주
Priority to KR1019930021592A priority Critical patent/KR0132401B1/en
Publication of KR950011658A publication Critical patent/KR950011658A/en
Application granted granted Critical
Publication of KR0132401B1 publication Critical patent/KR0132401B1/en

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Classifications

    • 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
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

A fabrication method of low oligomer polyester yarn is provided to decrease a cutoff rate. The method comprises the steps of: extracting and removing a ring-shaped oligomer by dipping a polyester chip in a low boiling spot organic solvent; and melt-spinning the polyester chip. The organic solvent having low boiling spot is used a chloroform. Thereby, it is possible to easily form low oligomer polyester yarn by removing the ring-shaped oligomer.

Description

저올리고머성 폴리에스테르사의 제조방법Manufacturing method of low oligomeric polyester yarn

본 발명은 고리형오리고머의 함량이 적은 폴리에스테르사의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester yarn having a small content of cyclic oligomers.

폴리에스테르칩 안에는 일반적으로 2.5 중량 %정도의 올리고머가 존재하는 바, 이중에서 대부분은 고리형올리고머이다.Generally about 2.5% by weight of oligomers are present in polyester chips, most of which are cyclic oligomers.

그런데 상기 고리형올리고머는 용융방사할때 많은 문제점을 일으킨다.However, the cyclic oligomers cause many problems when melt spinning.

즉, 폴리에스테르칩 안에 존재하는 고리형올리고머는 용융방사할때 열에 응하여 이동되고 그 결정성이 폴리머보다 크기 때문에 결정형태로 석출하게 된다. 그 결과 사의 절사 또는 곡사의 원인이 되었으며 사의 수분율을 높이는 원인이 되었다. 또 결정화속도를 지연시키는 문제점이 있었다.That is, the cyclic oligomer present in the polyester chip is moved in response to heat during melt spinning and precipitates in crystalline form because its crystallinity is larger than that of the polymer. As a result, it caused the yarn to be cut off or howitzer, and to increase the moisture content of the yarn. In addition, there was a problem of delaying the crystallization rate.

본 발명은 폴리에스테르칩을 저비점유기용제로 처리하여서 폴리에스테르칩내의 고리형올리고머의 함량이 적게 되도록 함을 특징으로 하는바 이하 상세히 설명하면 다음과 같다.The present invention is characterized by reducing the content of the cyclic oligomer in the polyester chip by treating the polyester chip with a low-boiling organic solvent as follows.

본 발명은 용융방사하기전에 폴리에스테르칩을 저비점유기용제에 침지하여 2∼10시간 처리하여서 고리형올리고머를 추출함을 특징으로 하는 저올리고머성 폴리에스테르사의 제조방법이다.The present invention is a method for producing a low oligomeric polyester yarn characterized by extracting a cyclic oligomer by immersing a polyester chip in a low boiling organic solvent before melt spinning for 2 to 10 hours.

본 발명에 사용되는 저비점유기용제로는 클로로포름(CHcl3) 또는 디옥산(Dioxan)이다.Low-boiling organic solvents used in the present invention are chloroform (CHcl 3) or dioxan.

이때 유기용매의 사용량은 폴리에스테르칩 1㎏에 대하여 2∼10ℓ를 사용하였으며 용매를 저속으로 회전시키면서 25oC ∼50oC 의 온도에서 수출하였다.At this time, the amount of the organic solvent was used 2 ~ 10L per 1kg of polyester chip and was exported at a temperature of 25 ° C ~ 50 ° C while rotating the solvent at a low speed.

고리형올리고머의 함량은 추출전에 비하여 50∼90 중량 % 정도 감소되었다.The content of the cyclic oligomer was reduced by 50 to 90% by weight compared to before the extraction.

이어서 고리형올리고머가 추출된 폴리에스테르칩을 105oC 에서 2시간정도 건조시켜서 용매를 증발시킨 다음에 용융방사용으로 제공하였다.Subsequently, the polyester chip from which the cyclic oligomer was extracted was dried at 105 ° C. for about 2 hours to evaporate the solvent, and then used by melt spinning.

본 발명을 실시예에 의거 더욱 구체적으로 설명한다.The present invention will be described in more detail with reference to Examples.

[실시예 1∼4 및 비교예 1][Examples 1 to 4 and Comparative Example 1]

폴리에스테르칩을 표 1의 조건으로 클로로포름을 이용하여 고리형올리고머를 추출한 다음에 추출하지 않은 경우와 대비한 결과는 표 1 과 같다.Table 1 shows the results of comparing the polyester chip with chloroform under the conditions of Table 1 and not extracting the cyclic oligomer.

[평가방법][Assessment Methods]

A)올리고머 함량분석A) oligomer content analysis

폴리에스테르칩→TFA로 녹이고→디옥산으로 올리고머추출→UV/VIS Spec trophotometer이용(254nm)측정Polyester chip → dissolve in TFA → oligomer extraction with dioxane → UV / VIS Spectrophotometer measurement (254nm)

추출하지 않은 것의 함량 2.5 중량 %를 100%로 보고 추출한 후의 함량을 비교하였음.2.5% by weight of the unextracted content as 100% compared with the content after extraction.

B)고리형올리고머감소 정도확인B) Check the degree of ring oligomer reduction

HPLC이용HPLC

분리조건:헥산/디옥산=7/3 용액이용, 유량=1mℓ/분Separation condition: Hexane / dioxane = 7/3 solution use, flow rate = 1 ml / min

감소정도는 LC chart상에서 피크(peak)의 감소를 통해 정성적 확인The degree of reduction is qualitatively confirmed by decreasing the peak on the LC chart.

C)절사율 : 연신이후 감으면서 절사되는 정도확인C) Cutting rate: Check the degree of cutting while winding after stretching

D)수분함량 : Karl-Fischer titrator이용D) Moisture content: using Karl-Fischer titrator

Claims (3)

폴리에스테르칩을 용융방사하여 폴리에스테르사를 제조함에 있어서, 용융방사하기전에 폴리에스테르칩을 저비점유기용제에 침지하여 고리형올리고머를 추출함을 특징으로 하는 저올리고머성 폴리에스테르사의 제조방법.A method for producing a low oligomeric polyester yarn, wherein the polyester chip is melt-spun and the polyester yarn is prepared by immersing the polyester chip in a low boiling organic solvent before melt spinning. 제 1항에서, 저비점유기용제는 클로로포름 또는 디옥산임을 특징으로하는 저올리고머성 폴리에스테르사의 제조방법.The method of claim 1, wherein the low boiling organic solvent is chloroform or dioxane. 제 1 항 또는 제 2 항에서, 클로로포름의 사용량은 칩 1kg에 대하여 2∼10ℓ이고, 20SoC ∼50oC 에서 2∼10시간 추출함을 특징으로 하는 저올리고머성 폴리에스테르사의 제조방법.In the first or claim 2, wherein the amount of chloroform is 2~10ℓ against the chip 1kg, 20S o C ~50 o C 2~10 time extraction prepared's method that oligomeric polyester which is characterized in a.
KR1019930021592A 1993-10-18 1993-10-18 Process for manufacturing a polyester fiber containing small amounts of oligomer KR0132401B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019930021592A KR0132401B1 (en) 1993-10-18 1993-10-18 Process for manufacturing a polyester fiber containing small amounts of oligomer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019930021592A KR0132401B1 (en) 1993-10-18 1993-10-18 Process for manufacturing a polyester fiber containing small amounts of oligomer

Publications (2)

Publication Number Publication Date
KR950011658A KR950011658A (en) 1995-05-15
KR0132401B1 true KR0132401B1 (en) 1998-04-16

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Application Number Title Priority Date Filing Date
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KR950011658A (en) 1995-05-15

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