KR20070072032A - Industrial high-strength polyester fiber with less permanent deformation-rate and its manufacturing method - Google Patents

Industrial high-strength polyester fiber with less permanent deformation-rate and its manufacturing method Download PDF

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KR20070072032A
KR20070072032A KR1020050135955A KR20050135955A KR20070072032A KR 20070072032 A KR20070072032 A KR 20070072032A KR 1020050135955 A KR1020050135955 A KR 1020050135955A KR 20050135955 A KR20050135955 A KR 20050135955A KR 20070072032 A KR20070072032 A KR 20070072032A
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polyester fiber
strength
rate
temperature
polyester
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KR1020050135955A
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KR101215710B1 (en
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한규찬
심동석
조대환
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주식회사 효성
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/084Heating filaments, threads or the like, leaving the spinnerettes
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44Yarns or threads characterised by the purpose for which they are designed
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04Fibres 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]
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/062Load-responsive characteristics stiff, shape retention
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/063Load-responsive characteristics high strength

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

An industrial high-strength polyester fiber with a low permanent transformation-rate is provided to control the condition of the hood temperature and the quenching air temperature, thereby offering the excellent work property. A polyester chip with the inherent viscosity of 1.0 is melted, spun and drafted so that the high strength polyester fiber is manufactured. At the manufacturing process, the temperature of the hood heater(1) is 400 to 500 degrees centigrade and the quenching air temperature is 10 to 16 degrees centigrade so that the spun mono filament has the non-oriented structure. A proper amount of oil is imparted into the solidified yarn by an oiling roller(4) and then previously drafted at the godet rollers(GR2,GR3). The solidified yarn is secondly drafted by the godet rollers(GR3,GR4) with the high ratio and relaxed and wound by the godet rollers(GR4,GR5). The polyester fiber manufactured by the above process has the strength of above 10.6 g/d, the cut elongation rate of below 12% and the permanent transformation rate of below 1%. The polyester chip is melted by an extruder.

Description

영구 변형율이 적은 산업용 고강력 폴리에스테르 섬유 및 그 제조방법{Industrial high-strength Polyester fiber with less permanent deformation-rate and its manufacturing method}Industrial high-strength polyester fiber with less permanent deformation-rate and its manufacturing method

도 1은 본 발명의 제조공정 개략도.1 is a manufacturing process schematic diagram of the present invention.

도 2는 원사의 시간에 따른 신율 변화 그래프.Figure 2 is a graph of elongation change with time of yarn.

본 발명은 영구 변형율(less permanent deformation rate)이 적은 산업용 고강력 폴리에스테르 섬유 및 그 제조방법에 관한 것으로서, 더욱 상세하게 고강력 특성을 가지면서 높은 모듈러스 및 저신율의 특성을 지녀 지오그리드, 웨빙용 등에 사용되는 산업용 고강력 폴리에스테르 섬유 및 그 제조방법에 관한 것이다.The present invention relates to an industrial high-strength polyester fiber with a low permanent deformation rate and a method of manufacturing the same, and more particularly, to geogrid, webbing, etc., having high modulus and low elongation characteristics. The present invention relates to an industrial high strength polyester fiber used and a method of manufacturing the same.

폴리에스테르 섬유의 강도를 높이기 위한 종래의 방법으로는 고유점도 1.0 이상의 고점도 칩을 용융한 후, 용융된 폴리머 온도를 310℃까지 높여서 충분히 녹이고 후드 길이를 280mm, 후도 온도를 340℃로 설정하고 퀸칭 에어의 온도를 16 ~ 18℃로 하여서 폴리머를 고화시킨다. 이어서 고뎃 롤러에서 저속권취하여 얻은 미연신사를 1단 및 2단으로 연신배율 6.0까지 직접 연신한 후 릴랙스를 시켜 권취하 는 방법이었다.In the conventional method for increasing the strength of polyester fibers, after melting a high viscosity chip having an intrinsic viscosity of 1.0 or higher, the molten polymer temperature is raised to 310 ° C to sufficiently melt, and the hood length is set to 280 mm and the rearward temperature to 340 ° C, and quenched. The temperature of the air is 16-18 ° C. to solidify the polymer. Subsequently, the unstretched yarn obtained by winding at a low speed roller was stretched directly to a draw ratio of 6.0 in one and two stages, and then wound by winding.

이 때 저속 권취로 미연신시의 배향도를 낮추어 고배율의 연신을 부여하여 고강도의 섬유를 얻었다. 상기 방법으로 제조되며 산업용 로프 등의 제품에 널리 사용되는 폴리에스테르 사의 물성은 모듈러스 60g/d ~ 80g/d, 강도 9.5g/d 이하, 절신 13 ~ 18%이고 영구 변형율은 1.5% 이상으로서 매우 높았다.At this time, the orientation degree at the time of unstretching was lowered by low speed winding, the high magnification of stretching was given, and the fiber of high strength was obtained. The physical properties of polyester yarns manufactured by the above methods and widely used in products such as industrial ropes were modulus of 60 g / d to 80 g / d, strength of 9.5 g / d or less, 13 to 18%, and permanent strain of 1.5% or more. .

종래의 방사 기술을 사용하여 더 높은 강도를 얻기 위해서 종래의 연신 배율보다 연신 배율을 높일 경우 방사 사절이 많이 발생하는 공정상 문제와 품질문제가 발생하여 후 공정성이 나빠진다. 그러므로 제조 비용의 상승 및 제품의 질이 저하되어 기존의 기술로는 고강도사를 얻기 힘들었다.In order to obtain higher strength by using a conventional spinning technique, when the stretching ratio is increased than the conventional stretching ratio, process problems and quality problems that cause many yarns are generated, resulting in poor post-processability. Therefore, it is difficult to obtain high-strength yarn with the existing technology due to the increase of manufacturing cost and the deterioration of product quality.

본 발명은 후드 온도의 조건과 퀸칭 에어 온도를 조절함으로서 종래의 연신 배율인 6.3 이상 보다 높은 연신 배율에서도 방사 작업성이 우수하도록 하여서 강도 10.6g/d 이상이고 영구 변형율이 1% 미만인 산업용 고강도 폴리에스테르 섬유를 제조할 수 있도록 하는데 기술적 과제를 둔 것이다.The present invention is to control the conditions of the hood temperature and the quenching air temperature to excellent spinning workability even at a draw ratio higher than the conventional draw ratio of 6.3 or more, so that the industrial high-strength polyester of more than 10.6g / d strength and less than 1% permanent strain The technical challenge is to make the fiber.

본 발명은 산업용 고강력 폴리에스테르 섬유 및 그 제조방법에 관한 것으로서, 보다 상세하게는 고유점도 1.0의 폴리에스테르 칩을 용융압출하여 방사 구금의 노즐을 통하여 방사하고 후드히터 온도를 400 ~ 500℃로 하고, 퀸칭 에어 온도를 10 ~ 16℃ 로 하며, 권취 직전에 방사유제를 부여하고 고뎃 롤러를 통해 높은 연신 배율로 연신함으로써 방사작업성이 우수하고 강도 10.6g/d 이상, 절신 12% 이하, 영구 변형율이 1% 미만인 폴리에스테르 사 및 그 제조방법에 관한 것이다.The present invention relates to industrial high-strength polyester fiber and a method of manufacturing the same, and more particularly, melt-extruded polyester chips having an intrinsic viscosity of 1.0 to spin through nozzles of spinnerets, and the hood heater temperature is 400 to 500 ° C. , Quenching air temperature is 10 ~ 16 ℃, and the spinning oil is applied just before winding and drawn at high draw ratio through high-pressure roller, so it is excellent in spinning workability, strength is more than 10.6g / d, stretching is less than 12%, permanent strain rate The present invention relates to a polyester yarn which is less than 1% and a production method thereof.

본 발명을 예시 도면에 의거 더욱 상세히 설명하면 다음과 같다. Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings.

고유점도가 1.0 인 폴리에스테르 칩을 익스루더에서 용융한다. 후드 히터(1)의 온도를 400 ~ 500℃로 높여 방사된 모노 필라가 최대한 무정 및 무배향의 구조를 가질 수 있도록 후드 내의 퀸칭 에어의 온도를 10 ~ 16℃ 로 낮추어 흡기(2) 및 배기(3) 시켜준다. 고화된 사를 오일링롤러(4)에서 적당량의 오일을 부여한 후 고뎃드 롤러 GR 2 과 GR 3에서 예비 연신을 거친 다음 고뎃드 롤러 GR 3과 GR 4에서 2차 고 비율의 연신을 수행하고 고뎃드 롤러 GR 4와 GR 5 상에서 릴랙스를 시킨 후 권취한다.Polyester chips with an intrinsic viscosity of 1.0 are melted in an extruder. By raising the temperature of the hood heater 1 to 400 to 500 ° C., the temperature of the quenching air in the hood is lowered to 10 to 16 ° C. so that the radiated monofilament can have an amorphous and unoriented structure as much as possible. 3) Let it be. After applying the appropriate amount of oil in the oiling roller (4), the solidified yarn is preliminarily stretched in the high rollers GR 2 and GR 3, and then the second high ratio is drawn in the high rollers GR 3 and GR 4. Relax on wind rollers GR 4 and GR 5 and wind up.

이와 같은 공정에서 제조된 폴리에스테르 사는 방사 작업성이 좋아 얻어지는 원사의 품질이 우수하고 강도와 모듈러스가 매우 높으며 절신과 영구 변형율은 낮아서 지오그리드, 웨빙용 등의 용도로 유용하게 사용될 수 있다.Polyester yarns produced in such a process have good spinning performance, good yarn quality, high strength and modulus, low cutting and permanent strain, and thus can be useful for geogrid and webbing applications.

실시예 및 비교예에서 물성 평가를 수행했던 방법은 아래와 같이 이루어졌다.The method of performing the physical property evaluation in the Example and the comparative example was done as follows.

1) 고유점도(I.V.)1) Intrinsic viscosity (I.V.)

페놀과 1,1,2,2-테트라클로로에탄올 6:4(무게비)로 혼합한 시약(90℃)에 시료 0.1g을 90분간 용해시킨 후 우베로데(Ubbelohde) 점도계에 옮겨 담아 30℃ 항온조에서 10분간 유지시키고, 점도계와 애스피레이터(Aspirator)를 이용하여 용액의 낙하초수를 구한다. 솔벤트의 낙하초수도 상기와 같은 방법으로 구한 아래의 수학식에 의해 R.V.값 및 I.V. 값을 계산하였다.After dissolving 0.1 g of the sample in a reagent (90 ° C.) mixed with phenol and 1,1,2,2-tetrachloroethanol 6: 4 (weight ratio) for 90 minutes, transfer to a Ubbelohde viscometer and place it in a 30 ° C. thermostat. The solution is held for 10 minutes at, and the drop seconds of the solution are obtained by using a viscometer and an aspirator. The number of seconds of falling of the solvent can also be obtained by the following equations obtained from the above equations. The value was calculated.

R.V. = 시료의 낙하초수/솔벤트 낙하초수R.V. = Number of drops of solvent / number of drops of solvent

I.V. = 1/4 × (R.V.- 1/농도CO4) + 3/4 × (In R.V./농도)IV = 1/4 × (RV-1 / concentration CO 4 ) + 3/4 × (In RV / concentration)

2) 원사의 모듈러스와 강신도 측정방법2) Measuring modulus and elongation of yarn

원사를 표준상태인 조건, 즉 25℃ 온도와 상대습도 65%인 상태인 항온 항습실에서 24시간 방치 후 ASTM 2256 방법으로 시료를 인장 시험기를 통해 측정한다.After leaving the yarn in a standard condition, that is, a constant temperature and humidity chamber at a temperature of 25 ° C. and a relative humidity of 65% for 24 hours, the sample is measured by a tensile tester using the ASTM 2256 method.

3) 작업성3) Workability

방사기의 한 장소에서 24시간 동안 관찰하여 고뎃드 롤러상에서 사절이 발생하는 개수를 파악한다.Observe for 24 hours at a location on the spinner to determine the number of trimmings on the high roller.

4) 영구 변형율4) permanent strain

원사를 표준상태, 즉 25℃ 온도와 상대습도 65%인 항온 항습실에서 24시간 방치 한다. 원사 강력의 10%에 해당하는 하중을 주어 6,000분 이상 방치한 후 하중을 제거해 늘어난 신율을 측정한다. (L0 : 시료를 표준상태에서 24시간 방치 후 초하중(0.01g/d)하에서 측정한 길이, L1 : 일정시간 하중을 가한후 제거한 뒤 초하중(0.01g/d)하에서 늘어난 시료의 길이)The yarn is left for 24 hours in a standard condition, that is, a constant temperature and humidity room with a temperature of 25 ° C. and a relative humidity of 65%. Give a load equal to 10% of the yarn strength and leave it for more than 6,000 minutes before removing the load to measure the elongation. (L 0 : Length measured under ultra-load (0.01 g / d) after leaving the sample at standard condition for 24 hours, L 1 : Length of the sample under ultra-load (0.01 g / d) after removing it after applying a certain time load) )

Figure 112005078619426-PAT00001
Figure 112005078619426-PAT00001

실시예 1 ~ 5 및 비교예 1 ~ 6 ;Examples 1-5 and Comparative Examples 1-6;

고유점도 1.00의 폴리에스테르 칩을 지름 0.6mm, 길이와 직경비(L/D)가 3이고 구멍수 192개인 노즐을 통해 용융 폴리머를 압출하고 15℃의 공기로 냉각시킨 다음 집속시켜 오일링하고 고뎃드 롤러 GR 4 속도를 2700m/min의 속도로 하여 1500데니어를 방사하여 표 1의 방사 조건으로 연신하였으며, 얻어진 원사의 영구 변형율을 측정하였다.(도면 2)A polyester chip with an intrinsic viscosity of 1.00 was extruded through a nozzle with a diameter of 0.6 mm, a length and diameter ratio (L / D) of 3, and a hole of 192 holes. 1500 deniers were spun and stretched under the spinning conditions shown in Table 1 at the speed of the chop roller GR 4 at a speed of 2700 m / min, and the permanent strain of the obtained yarn was measured (Fig. 2).

[표 1]TABLE 1

Figure 112005078619426-PAT00002
Figure 112005078619426-PAT00002

본 발명은 후드히터의 온도와 퀸칭 에어 온도를 최적화시킴으로서 높은 모듈러스, 고강도, 저절신율을 나타내며 동시에 영구 변형율이 적은 산업용 고강력 폴리에스테르 섬유를 제조할 수 있다.The present invention optimizes the temperature of the hood heater and the quenching air temperature, thereby producing industrial high strength polyester fibers with high modulus, high strength, low elongation, and low permanent strain.

Claims (2)

고유점도 1.0의 폴리에스테르 칩을 사용하여 산업용 폴리에스테르 섬유를 1단계 공정으로 방사, 연신하여 제조함에 있어서, 후드히터의 온도를 400 ~ 500℃로 하고, 퀸칭 에어 온도를 10 ~ 16℃로 하여 제조하는 것을 특징으로 하는 영구 변형율이 적은 산업용 고강력 폴리에스테르 섬유의 제조방법.In the process of spinning and stretching industrial polyester fibers in a one-step process using a polyester chip having an intrinsic viscosity of 1.0, the hood heater is manufactured at 400 to 500 ° C and the quenching air temperature is set at 10 to 16 ° C. A method for producing an industrial high strength polyester fiber with a small permanent strain. 제 1항의 방법으로 제조되고 아래의 물성을 갖는 것을 특징으로 하는 영구 변형율이 적은 산업용 고강력 폴리에스테르 섬유.Industrial high strength polyester fiber with low permanent strain, characterized by the method of claim 1 and having the following physical properties. 아 래  Below (1) 강도 10.6g/d 이상,(1) strength of at least 10.6 g / d, (2) 절신 12% 이하, (2) less than 12% of the body; (3) 영구 변형율이 1.0% 이하(원사 강력의 10% 이하의 하중에서)(3) Permanent strain is 1.0% or less (at load less than 10% of yarn strength)
KR1020050135955A 2005-12-30 2005-12-30 Industrial high-strength Polyester fiber with less permanent deformation-rate and its manufacturing method KR101215710B1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011002165A2 (en) * 2009-07-02 2011-01-06 (주)효성 Industrial polyethylene terephthalate multifilament
KR101114267B1 (en) * 2011-08-05 2012-02-14 일양산업 주식회사 Eco-geogrid for preventing crack of asphalt and extension and method thereof
KR101429686B1 (en) * 2013-01-14 2014-09-23 주식회사 효성 Process for preparing high viscosity and high intensity industrial polyester fibre

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WO2011002165A3 (en) * 2009-07-02 2011-04-21 (주)효성 Industrial polyethylene terephthalate multifilament
KR101114267B1 (en) * 2011-08-05 2012-02-14 일양산업 주식회사 Eco-geogrid for preventing crack of asphalt and extension and method thereof
KR101429686B1 (en) * 2013-01-14 2014-09-23 주식회사 효성 Process for preparing high viscosity and high intensity industrial polyester fibre

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