KR100231192B1 - A process for manufacturing polyester fiber - Google Patents
A process for manufacturing polyester fiber Download PDFInfo
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- KR100231192B1 KR100231192B1 KR1019970037231A KR19970037231A KR100231192B1 KR 100231192 B1 KR100231192 B1 KR 100231192B1 KR 1019970037231 A KR1019970037231 A KR 1019970037231A KR 19970037231 A KR19970037231 A KR 19970037231A KR 100231192 B1 KR100231192 B1 KR 100231192B1
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- embroidery
- biphenyl
- elongation
- yarn
- plasticizer
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/221—Preliminary treatments
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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
- 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
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/224—Selection or control of the temperature during stretching
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/228—Stretching in two or more steps, with or without intermediate steps
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
- D06M13/03—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons with unsaturated hydrocarbons, e.g. alkenes, or alkynes
- D06M13/07—Aromatic hydrocarbons
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/08—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Artificial Filaments (AREA)
Abstract
본 발명은 폴리에스테르 미연신사를 연신하기전에 가소제/용제의 용액으로 처리한후 다산연신과정에서 열처리하고 이완연신시켜서 자수사용의 물성에 적합한 인장강도 2.0~4.0g/d, 파단신도 15~25%, 열수축율 2% 이하인 자수사를 제조하는 방법임.The present invention is treated with a solution of plasticizer / solvent before stretching the polyester unstretched yarn, then heat treated and relaxedly stretched in the process of fertility stretching, so that the tensile strength suitable for the properties of embroidery 2.0-4.0 g / d, elongation at break 15-25% , Which is a method of manufacturing embroidery thread having a heat shrinkage of 2% or less.
본 발명은 가소제로서 바이페닐을 0.5~5.0중량% 함유시킨 바니페닐/메틸렌클로라이드 용액을 사용하여 45초이내에 처리하고 열처리온도 200~230℃, 이완연신율 0.92~0.97의 조건으로 다단연신하여 제조함을 특징으로하는 방법임.The present invention is prepared by treatment within 45 seconds using a phenylphenyl / methylene chloride solution containing 0.5 ~ 5.0% by weight of biphenyl as a plasticizer, and multi-stretched under conditions of heat treatment temperature 200 ~ 230 ℃, relaxation elongation 0.92 ~ 0.97 It's a feature.
Description
본 발명은 자수사용 폴리에스테르 필라멘트의 제조방법에 관한 것으로서, 더욱 상세하게는 연신전에 폴리에스테르 필라멘트를 가소제/용제로 처리한후 다단연신을 행하여 인장강도와 파단신도 및 열수수축율을 동시에 낮추어줌으로써 자수사용에 적합한 물성을 갖는 폴리에스테르 섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method of manufacturing a polyester filament for embroidery, and more specifically, to a polyester filament before the stretching with a plasticizer / solvent to perform a multi-stage stretching to lower the tensile strength, elongation at break and heat shrinkage at the same time The present invention relates to a method for producing a polyester fiber having suitable physical properties.
일반적으로 자수사는 염색성이 양호하고 자수공정성이 뛰어난 레이온섬유가 주로 사용되어왔다.In general, embroidery yarns have been mainly used for rayon fibers with good dyeability and excellent embroidery process.
그러나, 레이온 섬유는 공해를 유발하는 산업으로 생산설비가 점차 축소되어 가는 과정이며 또, 이것은 연사등 후 공정에서 피부병을 유발시키는 등의 문제 때문에 점차 폴리에스테르 섬유로 대체되어 가는 추세이다.However, rayon fiber is a pollution-causing industry, and its production facilities are gradually being reduced. Also, it is gradually being replaced by polyester fiber due to problems such as causing skin diseases in the post-heating process.
폴리에스테르 섬유가 자수사로 사용되려면 인장강도가 2.0~4.0g/d이고, 파단신도가 15~25%, 열수축율이 2% 이하가 되어야 한다. 인장강도가 2.0g/d 미만이면 연사등 중간공정에서 사절이 일어나기 쉽고, 인장강도가 4.0g/d을 초과하면 자수후 커팅 공정이 불량하여 외관이 불량하여진다.To be used as embroidery yarns, polyester fibers must have a tensile strength of 2.0 to 4.0 g / d, an elongation at break of 15 to 25%, and a heat shrinkage of 2% or less. If the tensile strength is less than 2.0g / d, trimming is likely to occur in intermediate processes such as twisting, and if the tensile strength exceeds 4.0g / d, the cutting process after embroidery is poor and the appearance is poor.
그리고, 파단신도가 15% 미만이면 중간공정에서의 작업성이 불량하며, 파단신도가 25%를 초과하면 자수후 퍼커링(Puckering)현상에 의해 자수표면이 평활치 못하다. 또한, 열수축율이 2%를 초과하면 치즈(cheese)등으로 사염색시 불균염을 초래하고, 불균일한 수축으로 인한 치즈의 사층이 무너지게 되며, 자수후에도 열고정 공정에서 수축이 일어나 원단의 외관이 불량하여 진다. 그러나, 기존의 폴리에스테르 필라멘트는 인장강도가 5.0g/d 정도이고, 파단신도가 30% 수준이며, 열수축율이 8%수준으로 자수사용으로 적합지 못하였다.If the elongation at break is less than 15%, the workability in the intermediate process is poor. If the elongation at break is more than 25%, the embroidery surface is not smooth due to the phenomenon of puckering after embroidery. In addition, if the heat shrinkage exceeds 2%, uneven salts are caused during dyeing with cheese, and the four layers of cheese are collapsed due to uneven shrinking, and shrinkage occurs in the heat setting process even after embroidery. This becomes poor. However, conventional polyester filament has a tensile strength of about 5.0g / d, elongation at break of 30%, heat shrinkage of 8% was not suitable for embroidery use.
또한, 인장강도와 파단신도는 반비례하는 인자들이므로 인장강도와 파단신도를 동시에 낮추기 위해서는 방사 또는 연신과정에서 고온의 열처리를 하여야만 한다. 그러나 이렇게 하면, 과도한 에너지를 받고 제사된 사는 내부의 올리고머가 사단면상의 외층으로 위치하게 되고, 이 사를 연사 후 열고정, 전처리, 염색을 하게되면 올리고머가 마이그레이션되어 염색불량 및 해사성 불량등의 문제점을 야기시키게 된다.In addition, since the tensile strength and the elongation at break are inversely proportional factors, to lower the tensile strength and the elongation at break simultaneously, a high temperature heat treatment must be performed during the spinning or drawing process. However, in this case, the yarns that are subjected to excessive energy are placed in the outer layer on the cross-section, and when the yarns are heat-set, pre-treated and dyed after the yarns, the oligomers are migrated, resulting in poor dyeing and poor degradability. Will cause problems.
이러한 문제점들을 해결하고자 시도되었던 선행기술로서는 한국 특허공보 96-11606 이있다.Korean Patent Publication No. 96-11606 is a prior art attempting to solve these problems.
이 방법은 중합제조시 DMS(디메칠설포네이트)와 디메틸아디페이트를 첨가하여 중합, 제사하고 연신단계에서 4단 연신법을 통해 열처리하므로서 자수사에 적합한 물성을 갖는 폴리에스테르 섬유의 제조방법으로서 공중합물 사용으로 인한 제조 코스트의 상승과 일광 견뢰도가 저하되는 단점이있다.This method is a copolymerization method for producing polyester fibers having physical properties suitable for embroidery yarns by adding DMS (dimethyl sulfonate) and dimethyl adipate during polymerization, and polymerizing and preparing them and heat-treating them through four-stage drawing in the drawing step. There is a disadvantage in that the manufacturing cost is increased due to the use of water and the daylight fastness is lowered.
또한, 한국 특허공고 94-11310 에서는 연신, 전후에 용제처리를 통해 폴리에스테르 섬유의 강도 및 파단신도를 적절하게 조정하려고 하고 있으나 용제처리가 권취된 미연신사 또는, 연신사에 대하여 배치식으로 이루어지므로 권취된 사의 내,외층간의 용제처리 편차에 의한 물성편차가 생기기 쉽고, 열수축율을 2% 미만으로 조절할 수 없었다.In addition, Korean Patent Publication 94-11310 tries to adjust the strength and elongation of polyester fiber appropriately through solvent treatment before and after stretching, but it is made of batch type for undrawn or wound yarn wound with solvent treatment. Variation in physical properties due to solvent treatment variation between the inner and outer layers of the wound yarn is likely to occur, and the heat shrinkage rate cannot be adjusted to less than 2%.
본 발명은 방사후 연신전에 주행상태인 사를 연속적으로 가소제/용제의 용액으로 처리하고 수세, 건조한 후 다단연신함으로서 자수에 적합한 물성을 갖는 폴리에스테르 섬유의 제조방법을 제공하는데 그 목적이 있는 것이다.It is an object of the present invention to provide a method for producing a polyester fiber having physical properties suitable for embroidery by treating a yarn in a running state before stretching after spinning with a solution of a plasticizer / solvent, and washing with water and drying in multiple stages.
이하 본 발명을 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 자수사의 용도에 적합하도록 인장강도가 2.0~4.0g/d, 파단강도가 15~25% 및 열수축율이 2%이하인 폴리에스테르섬유를 제조하기 위하여 방사후 연신전에 폴리에스테르 미연신사를 가소제/용제의 용액으로 처리함을 특징으로 한다.The present invention provides a plasticizer for polyester undrawn yarn before stretching after spinning to produce polyester fibers having a tensile strength of 2.0 to 4.0 g / d, a breaking strength of 15 to 25%, and a heat shrinkage of 2% or less so as to be suitable for use in embroidery yarns. / Is treated with a solution of the solvent.
본 발명에서는 가소제/용제로 바이페닐/메틸렌클로라이드를 사용하였다.In the present invention, biphenyl / methylene chloride was used as the plasticizer / solvent.
바이페닐은 가소제로서 폴리에스테르를 가소화시켜 결정화도를 높이는 물질로 알려져 있으며, 용제인 메틸렌 클로라이드는 바이페닐을 용이하게 용해시키며 동시에 폴리에스테르를 팽윤시켜서 가소제가 섬유내부까지 침투하여 작용할 수 있도록 하는 것이다. 메틸렌 클로라이드액 내의 바이페닐의 농도는 사속도에 따라 다소의 조정이 필요하지만 0.5∼5.0중량%가 좋다.Biphenyl is known as a plasticizer to increase the degree of crystallinity by plasticizing polyester, and methylene chloride, a solvent, dissolves biphenyl easily and simultaneously swells the polyester so that the plasticizer can penetrate into the fiber. Although the biphenyl concentration in methylene chloride liquid requires some adjustment according to the firing speed, 0.5 to 5.0% by weight is preferable.
바이페닐의 농도가 0.5% 미만인 경우 기대하는 수준의 결정화를 일으키지 못하며, 5.0중량%를 초과하는 경우에는 섬유자체의 물성저하가 심하여 사용이 어렵게 된다.If the biphenyl concentration is less than 0.5%, the crystallization does not cause the expected level. If the biphenyl concentration exceeds 5.0% by weight, the physical properties of the fiber itself are severe, making it difficult to use.
또한 가소제/용제의 처리시간은 5~45초로 하는 것이 좋다. 만약 처리시간이 5초 미만이면 기대하는 수준의 결정화를 일으키지 못하여 자수사에 적합한 물성을 얻을 수 없으며, 45초를 초과하면 과도한 결정화가 일어나서 필라멘트간에 융착이 일어난다.In addition, the processing time of the plasticizer / solvent should be 5 to 45 seconds. If the treatment time is less than 5 seconds, the crystallization of the yarn cannot be obtained due to failure of the expected level of crystallization. If the treatment time exceeds 45 seconds, excessive crystallization occurs and fusion occurs between the filaments.
가소화처리는 침지하거나 분사시켜 정해진 시간만큼 처리될 수 있도록 사속과 처리조에서의 체류시간을 조정하였다.The plasticization treatment adjusted the dwell time in the firing speed and treatment tank so that it could be treated by immersion or spraying for a predetermined time.
위와같은 조건으로 가소화 처리를 받은 사는 상온의 물에 연속적으로 수세하고 가열장치를 거쳐 건조시킨 다음 권취된다. 이렇게 얻어진 폴리에스테르 미연신사를 열수수축율을 낮추기 위하여 4단연신하되 이완 연신배율을 0.92~0.97로 하고, 열처리 온도를 200~230℃로 하는 것이 좋다. 이완연신 배율이 0.92미만이면 과도한 이완 때문에 연신사도가 불량해져 사의 롤러 이탈이나 불균일을 초래하고, 0.97을 초과하면 열수수축율이 2%를 초과하게된다. 또한, 열처리온도가 200℃ 미만이면 사의 열수수축율이 2%를 초과하게 되어 자수사로 만드는 과정인 사염가공 공정에서 불균염이나 사층불균일 등의 문제를 일으키며, 230℃를 초과하면 사가 과도하게 열처리를 받아서 딱딱해지거나 융착되는 문제가 있다.The plasticizer treated under the above conditions is washed with water at room temperature continuously, dried by heating, and wound up. The polyester unstretched yarn thus obtained is four-stage stretched to lower the heat shrinkage ratio, but the relaxation stretch ratio is 0.92-0.97, and the heat treatment temperature is 200-230 ° C. If the stretching ratio is less than 0.92, the stretching yarn is poor due to excessive relaxation, leading to roller detachment or nonuniformity of the yarn. If the stretching ratio is more than 0.97, the heat shrinkage ratio exceeds 2%. In addition, when the heat treatment temperature is less than 200 ℃, the heat shrinkage rate of the yarn exceeds 2%, causing problems such as uneven salt and sand layer unevenness in the four-shot process, which is a process of making embroidery yarn, and if the temperature exceeds 230 ℃, the yarn is subjected to excessive heat treatment There is a problem of hardening or fusion.
본 발명에서 인장강도 및 파단신도는 통상의 인장강도 시험기로 측정하였으며, 열수축율은 JIS L1073의 방법에 따라 평가하였는데, 릴수축율 방법을 사용하여 측정하였다.Tensile strength and elongation at break in the present invention was measured by a conventional tensile strength tester, heat shrinkage was evaluated according to the method of JIS L1073, it was measured using the reel shrinkage method.
[실시예 1]Example 1
통상의 방법으로 중합하여 제조한 폴리에스테르 수지를 스크류 압출식 방사기에서 48공의 와이(Y)형 노즐을 통해 방사온도 300℃, 권취속도 1,265m/분으로 권취하면서 바이페닐 1중량%의 메틸렌클로라이드 용액으로 40초간 처리하고 2분간 수세한 후 건열가열장치에서 120℃로 건조하여 365데니어/48필라멘트의 미연신사를 얻었다.Methylene chloride of 1% by weight of biphenyl was wound while the polyester resin prepared by polymerization in a conventional manner was wound at a spinning temperature of 300 ° C. and a winding speed of 1,265 m / min through a 48-hole Y-type nozzle in a screw-extruded spinning machine. The solution was treated with a solution for 40 seconds, washed with water for 2 minutes, and then dried at 120 ° C. in a dry heater to obtain undrawn yarn of 365 denier / 48 filaments.
이 미연신사를 4단연신기에서 연신속도 1,200m/분, 1차 연신배율 1.015, 2차연신배율 1.6, 3차 연신배율 1.2, 이완 연신배율 0.955, 열처리온도 220℃로 연신하여 118데니어/48필라멘트의 연신사를 얻었다. 이렇게 얻어진 연신사의 물성을 측정하여 표1에 나타내었다.The unstretched yarn is drawn in a four-stage drawing machine at a drawing speed of 1,200 m / min, primary draw ratio 1.015, secondary draw magnification 1.6, third draw magnification 1.2, relaxation draw magnification 0.955, and heat treatment temperature of 220 ° C to 118 denier / 48 filaments I got a drawing company. The physical properties of the drawn yarn thus obtained were measured and shown in Table 1.
[실시예 2]Example 2
바이페닐의 함량을 4중량%로하고, 처리시간을 15초로하여 처리한 것을 제외하고는 실시예 1과 동일하게 하였으며, 그결과를 표1에 나타내었다.The content of biphenyl was 4 wt% and the treatment time was 15 seconds, except that the treatment was the same as in Example 1, and the results are shown in Table 1.
[실시예 3]Example 3
미연신사를 4단 연신과정에서 이완연신배율을 0.930, 열처리온도를 230℃로 한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과를 표1에 나타내었다.Undrawn yarn was prepared in the same manner as in Example 1 except that the relaxed draw ratio was 0.930 and the heat treatment temperature was 230 ° C. in the four step drawing process, and the results are shown in Table 1.
[실시예 4]Example 4
4단 연신과정에서 열처리온도를 210℃로 한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과를 표1에 나타내었다.Except that the heat treatment temperature was 210 ℃ in the four-stage stretching process was the same as in Example 1, the results are shown in Table 1.
[비교예 1]Comparative Example 1
바이페닐의 함량을 0.4중량%로 한 것을 제외하고는 실시예 1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except that the biphenyl content of 0.4% by weight was the same as in Example 1, the results are shown in Table 1.
[비교예 2]Comparative Example 2
바이페닐의 함량을 7중량%로 한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except that the biphenyl content of 7% by weight was the same as in Example 1, the results are shown in Table 1.
[비교예 3]Comparative Example 3
바이페닐/메틸렌클로라이드 용액에 사를 50초간 처리한 것을 제외하고는 실시예 1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except for treating the biphenyl / methylene chloride solution in the yarn for 50 seconds was the same as in Example 1, the results are shown in Table 1.
[비교예 4][Comparative Example 4]
열수수축율을 낮추기 위해 열처리를 240℃에서 처리한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except that the heat treatment at 240 ℃ to reduce the heat shrinkage was the same as in Example 1, the results are shown in Table 1.
[비교예 5][Comparative Example 5]
열수수축율을 낮추기 위해 열처리를 190℃에서 처리한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except that the heat treatment at 190 ℃ to reduce the heat shrinkage was the same as in Example 1, the results are shown in Table 1.
[비교예 6]Comparative Example 6
열수수축율을 낮추기 위해 이완연신배율을 0.900으로 처리한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과는 표1에 나타내었다.Except for treating the relaxed stretching ratio to 0.900 in order to lower the heat shrinkage rate was the same as in Example 1, the results are shown in Table 1.
[비교예 7]Comparative Example 7
열수수축율을 낮추기 위해 이완연신배율을 0.990으로 처리한 것을 제외하고는 실시예1과 동일하게 하였으며, 그 결과는 표 1에 나타내었다.Except for treating the relaxed stretching ratio to 0.990 in order to lower the heat shrinkage rate was the same as in Example 1, the results are shown in Table 1.
이와같이 제조된 본 발명의 폴리에스테르 섬유는 인장강도가 2.0g/d~4.0g/d이고, 파단신도가 15~25%이며, 열수수축율이 2% 이하로서 기존의 레이온 자수사를 대체할 수 있는 우수한 물성을 나타내었다.Polyester fiber of the present invention prepared as described above has a tensile strength of 2.0g / d ~ 4.0g / d, elongation at break is 15-25%, heat shrinkage is 2% or less can replace the existing rayon embroidery yarn Excellent physical properties were shown.
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