EP4141153A1 - Monofilament de polyamide - Google Patents

Monofilament de polyamide Download PDF

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Publication number
EP4141153A1
EP4141153A1 EP21817409.2A EP21817409A EP4141153A1 EP 4141153 A1 EP4141153 A1 EP 4141153A1 EP 21817409 A EP21817409 A EP 21817409A EP 4141153 A1 EP4141153 A1 EP 4141153A1
Authority
EP
European Patent Office
Prior art keywords
diameter
fiber diameter
fiber
knots
less
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
EP21817409.2A
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German (de)
English (en)
Inventor
Mizuki KUJIRAI
Sumio Yamaguchi
Sho MURATA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toray Industries Inc
Original Assignee
Toray Industries Inc
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.)
Filing date
Publication date
Application filed by Toray Industries Inc filed Critical Toray Industries Inc
Publication of EP4141153A1 publication Critical patent/EP4141153A1/fr
Pending legal-status Critical Current

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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
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • 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
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/06Feeding liquid to the spinning head
    • D01D1/09Control of pressure, temperature or feeding rate
    • 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
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/10Filtering or de-aerating the spinning solution or melt
    • D01D1/106Filtering

Definitions

  • the present invention relates to a polyamide monofilament. More specifically, it relates to a monofilament suitable for producing filters with excellent filtration performance that can serve as automotive filters, medical filters, and acoustic filters.
  • the present invention provides a polyamide monofilament that contains few knots and thinner filaments and has high uniformity in fiber diameter, thus serving to produce plain gauze fabrics with uniform openings and filters with high filtration performance.
  • polyamide fibers have been widely used for producing clothing, industrial materials, and the like.
  • it has been used very widely in the form of filters of monofilament fabrics (screen gauze fabrics) for automotive filters, medical filters, and acoustic filters.
  • Patent document 1 describes that knots are caused by gelation products of the polymer getting into the thread to prevent full stretching of these portions and proposes a technique that uses a spinning pack containing a sintered filter of metallic short fibers to ensure sufficient dispersion of the gelation products.
  • Patent document 2 is focused on the production of a finer monofilament with high tenacity, high modulus, and uniform fiber diameter in the length direction and reports a technique to produce a polyester monofilament of a core-sheath structure having fewer and smaller knots including very small ones made tangible.
  • Patent document 3 reports a spinneret for melt-spinning that has a discharge hole 1 containing an inflow hole 2, a metering hole 3 having a smaller cross-sectional area than the inflow hole 2, and a relaxation hole 4 having a larger cross-sectional area than the metering hole 3 that are connected in this order.
  • the use of this spinneret for melt-spinning can serve to reduce the frequency of cleaning of the spinneret surface.
  • a melt-spinning method that uses this spinneret for melt-spinning is also reported. The combined use of this spinneret for melt-spinning and the melt-spinning method makes it possible to further reduce the accumulation of dirt on the spinneret surface and reduce the variation in discharge. This is expected to realize the production of filaments with decreased unevenness.
  • Patent document 1 Although the technique proposed in Patent document 1 is effective for suppressing the formation of knots, there are no descriptions about thinning of the thread, and the technique cannot serve sufficiently for solving the problem of thinning. So far, quality evaluations for abnormal fineness have been made based on the rate of capturing knots by a slub catcher and fineness unevenness in the length direction (averaged) measured by a Ustertester, but this can allow local outflow of thin filaments, possibly leading to a serious complaint. This conventional technique is also disadvantageous due to unstable discharge from the spinneret that tends to cause fineness unevenness in the length direction.
  • the upper limit of the diameter of the relaxation hole is as small as 0.75 mm, and accordingly, the accumulated dirt density per unit circumferential length is large, leading to the problem of easy knot formation.
  • the present invention provides a high quality polyamide monofilament useful for production of filters. It has uniform fineness and hardly suffers knot formation. If knots exist, they can cause thread breakage and scum generation during warping and weaving. In addition, if a monofilament having knots is woven, because the knots have larger diameters than the fiber, the resulting woven fabric will suffer clogging in portions adjacent to the knots. As a result, the woven fabric will have largely deteriorated quality. As another problem, as filters with higher quality have been developed, greater attention is now focused on the existence of thinner filaments that have smaller diameters than the normal portions. If thin filaments exist, they will lead to woven fabrics having larger openings that allow foreign objects to pass through and cause inferior filtration. Therefore, it is extremely important to eliminate thin filaments.
  • the present invention provides a polyamide monofilament that contains few knots and thinner filaments and has high uniformity in fiber diameter, thus serving to produce plain gauze fabrics with uniform openings and filters with high filtration performance.
  • the present invention adopts the following constitution to meet the object described above.
  • the present invention can provide a polyamide monofilament that contains few knots and thinner filaments and has high uniformity in fiber diameter, thus serving to produce plain gauze fabrics with uniform openings and filters with high filtration performance.
  • a knot is a lump-like portion extended in the fiber length direction and having an abnormal local fiber diameter. Its fiber diameter is 120% or more of the normal fiber diameter.
  • a thin filament is a portion with a small fiber diameter. Specifically, its diameter is 90% or less of the normal fiber diameter. Knots and thin filaments are examined using an optical profile sensor (PSD-200, manufactured by Sensoptic) under the conditions of a traveling speed of 800 m/min, thread length-directional interval of 0.07 mm, and thread length of 200,000 m.
  • the optical profile sensor records numerical values of fiber diameter, standard deviation of fiber diameter measurements, number and size of knots, and number and size of thin filaments.
  • any 200,000 m section in the fiber length direction contains one or less knot with a diameter 135% or more as large as the fiber diameter and one or less thin filament with a diameter 80% or less as large as the fiber diameter. If the numbers of knots and thin filaments are in these ranges, the monofilament has a high uniformity and can serve to produce plain gauze fabrics with uniform openings and filters with high filtration performance. If there is more than one knot with a diameter 135% or more as large as the fiber diameter, the resulting plain gauze fabric will suffer large openings and clogging in regions adjacent to the knots, leading to a decrease in the uniformity of openings.
  • the plain gauze fabric will suffer large openings, leading to a decrease in the uniformity of openings. If the plain gauze fabric has large openings, it will lead to a filter that allows foreign objects to pass through and suffers a decrease in filtration performance.
  • any 200,000 m section in the fiber length direction contains ten or less knots with a diameter 120% or more and less than 135% as large as the fiber diameter and ten or less thin filaments with a diameter more than 80% and 90% or less as large as the fiber diameter. If the number of knots with a diameter 120% or more and less than 135% as large as the fiber diameter is ten or less, it serves to produce a plain gauze fabric that hardly suffers clogging. The plain gauze fabric will have openings with improved uniformity and serve to produce a filter having enhanced filtration performance.
  • any 200,000 m section in the fiber length direction contains five or less knots with a diameter 120% or more and less than 135% as large as the fiber diameter and five or less thin filaments with a diameter more than 80% and 90% or less as large as the fiber diameter.
  • the polyamide monofilament according to the present invention preferably has a fiber diameter CV% of 1.0% or less as measured over a 200,000 m section in the fiber length direction.
  • the fiber diameter CV% is calculated by dividing the standard deviation of fiber diameter measurements by the average of fiber diameter measurements and represented in percentage. It shows the degree of fineness unevenness in the length direction, and a smaller value indicates a higher uniformity in fiber diameter. If the value of CV% is controlled at 1.0% or less, it serves to produce a monofilament that is free of fineness unevenness in the fiber length direction and high in the uniformity in fiber diameter. It also serves to produce a plain gauze fabric with uniform openings and a filter with high filtration performance.
  • the fiber diameter CV% is more preferably 0.8% or less.
  • the smallest of 50 measurements of the strength-elongation product taken continuously is preferably 90% or more and 100% or less of the average. If knots and thin filaments exist, their sites are likely to act as fracture points and weaken the thread easily, leading to a plain gauze fabric suffering decreased local durability. If it is controlled at 90% or more, it serves to produce a plain gauze fabric with increased durability and a filter with increased durability.
  • the polyamide monofilament according to the present invention preferably has a fineness of 6 to 50 dtex. It is more preferably 8 to 47 dtex. In particular, when used for the production of ultrafine high mesh filters, it preferably has a fineness of 6 to 13 dtex. As described later, furthermore, if the fineness is controlled at 50 dtex or less in producing the polyamide monofilament according to the present invention, the occurrence of cooling unevenness can be suppressed in the air-cooling equipment and this serves to produce a polyamide monofilament that is free of knots and thin filaments and ensures high filtration performance. On the other hand, if it is controlled at 6 dtex or more, it serves to suppress variations in discharge and produce a polyamide monofilament that is free of knots and thin filaments and ensures high filtration performance.
  • the polyamide monofilament according to the present invention preferably has a strength of 4.0 cN/dtex or more and an elongation of 30% to 60%. If they are controlled in these ranges, it ensures the production of a plain gauze fabric with high durability.
  • polyamide is a polymer in which so-called hydrocarbon groups are connected to the backbone chain via amide bonds, and it is preferable for the polyamide to mainly contain polycaproamide or polyhexamethylene adipamide because such a polymer tends to have high dyeability, high washing fastness, and good mechanical properties.
  • the term "mainly” means that, in the case of polycaproamide, ⁇ -caprolactam units that form polycaproamide are mainly contained, and the polyamide mainly contains polyhexamethylenediamine diammonium adipate units. These units preferably account for 80 mol% or more, more preferably 90 mol% or more.
  • the polyamide may have a polymerization degree appropriately set in a range commonly adopted for the production of industrial fibers, but it is preferable for its 98% sulfuric acid relative viscosity to be in the range of 2.0 to 3.3, and more preferably in the range of 2.4 to 3.3. If it is controlled in this range, a polyamide monofilament having a strength required for plain gauze fabrics can be produced with high thread-making performance.
  • the moisture content of the polyamide resin chips used for spinning is preferably adjusted by drying etc. to 0.11% to 0.15%. If it is controlled in this range, it serves to suppress the formation of knots and thin filaments in the polyamide monofilament.
  • the moisture content referred to herein is determined by putting a specimen of the polyamide resin chips in a trace moisture measuring device and evaporating the moisture under the conditions of 230°C and 30 minutes while reading the moisture value.
  • the melt-spinning temperature of the polyamide resin chips is preferably a temperature higher than the melting point of the polyamide resin. Specifically, melt-spinning is performed preferably at a temperature higher by 20°C to 40°C than the melting point. If it is controlled in this range, it serves to suppress the formation of knots and thin filaments in the polyamide monofilament.
  • the basic production process may be carried out by a generally known technique, and examples thereof include continuous implementation of spinning and stretching steps (direct spinning and stretching process) and winding up of an unstretched thread implemented first, followed by stretching thereof (two-stage process).
  • the threads are cooled in an uniflow type chimney 12 designed to blow air in one direction, and the threads are divided into individual ones, supplied with a spinning oil solution from an oil supply guide 13, taken up by the first godet roller 14, stretched between the second godet roller 15 and the third godet roller 16, heat-treated by the third and fourth godet rollers (16, 17), and wound up on a wind-up device 18.
  • the melt-spinning pack used for producing the polyamide monofilament according to the present invention is a melt-spinning pack as described in Patent document 1.
  • the melt-spinning pack contains at least a spinneret, a pressure plate, a metal wire filter, and a sand filter layer or a straightening vane, with a sintered filter made of metallic short fibers having a roughly polygonal cross section being provided between the metal wire filter and the sand filter layer or straightening vane.
  • the filtering accuracy of the metal wire filter, sand filter layer, and straightening vane contained in the melt-spinning pack is improved, and metallic short fibers having a roughly polygonal shape are used so that the metallic short fibers are entangled, thereby enhancing the filtration performance and dispersibility.
  • the polygonal cross section preferably has a shape containing acute angles.
  • the thermally modified gelled polymer is dispersed finely as it hits the acute angle corners of the cross section. Accordingly, as the angles in the cross section become acuter, the thermally modified gelled polymer can be dispersed more finely.
  • the spinneret used to produce the polyamide monofilament according to the present invention is a spinneret for melt-spinning that contains a polymer inflow hole, a metering hole having a smaller cross-sectional area than the inflow hole, and a relaxation hole having a larger cross-sectional area than the metering hole that are connected in this order.
  • low molecular components (monomers, oligomers, etc.) of the polymer is sublimated as it is discharged from the spinneret, and it is accumulated over time as dirt around the polymer discharge holes.
  • a mold release agent such as silicone is applied on the polymer-discharging surface of the spinneret for melt-spinning in order to facilitate the release of the polymer.
  • dirt accumulation around the polymer discharge holes and deterioration in polymer releasability act to destabilize the discharge of the polymer from the spinneret, resulting in thread unevenness in the thread length direction, knot and thin filament formation, and thread breakage.
  • Patent document 3 Japanese Unexamined Patent Publication (Kokai) No. HEI-9-268417 ) describes a melt-spinning spinneret for high speed spinning that is designed to take up threads at a high speed of 2,000 m/min or more, in which the ratio (D2/D1) between the metering hole diameter (D1) and the relaxation hole diameter (D2) is 1.75 to 2.5, with the relaxation hole diameter (D2) being 0.40 to 0.75 mm, so that discharge is stabilized to decrease the fineness unevenness and suppress thread breakage, thereby realizing a decrease in required spinneret surface cleaning frequency.
  • the ratio (D2/D1) between the metering hole diameter (D1) and the relaxation hole diameter (D2) is 1.75 to 2.5, with the relaxation hole diameter (D2) being 0.40 to 0.75 mm, so that discharge is stabilized to decrease the fineness unevenness and suppress thread breakage, thereby realizing a decrease in required spinneret surface cleaning frequency.
  • Fig. 1 shows a typical discharge hole provided in a spinneret used for the present invention.
  • the discharge hole 1 contains an inflow hole 2, a metering hole 3, and a relaxation hole 4 that are connected continuously in the flow direction of the molten polymer.
  • the metering hole 3 is narrowed to a smaller cross section than the inflow hole 2 and works to measure the molten polymer flowing in from the inflow hole 2.
  • the relaxation hole 4 that follows the metering hole 3 has a larger cross section than the metering hole 3 to serve for decreasing the accumulated dirt density per unit circumferential length and relaxing the pressure on the molten polymer, thereby reducing the ballast.
  • the use of a relaxation hole that has a diameter (D2) larger than the diameter (D1) of the metering hole as described above tends to cause a drop in the back pressure on the discharge hole.
  • D1 the metering hole diameter
  • the metering hole is preferably designed so that the ratio (L1/D1) between the diameter (D1) and the length (L1) of the metering hole is in the range of 2.0 to 3.5.
  • the molten polymer If it is controlled in this range, it will be possible for the molten polymer to be discharged stably while maintaining a required back pressure and metering accuracy, and this serves to produce a polyamide monofilament containing few knots and thin filaments and having high uniformity in fiber diameter. It is more preferably 2.5 to 3.0.
  • the ratio (D2/D1) between the metering hole diameter (D1) and the relaxation hole diameter (D2) is preferably 2.6 to 4.0. If it is controlled in this range, the cross section of the molten polymer largely increases as it flows into the relaxation hole that has a larger diameter than the metering hole. Accordingly, the pressure on the molten polymer squeezed in the metering hole is relaxed and this prevents the threads from being caught by the dirt accumulated around the discharge hole, serving to reduce the variations in discharge. It also serves to decrease the rate of shear and stress in the molten polymer, thereby suppressing the generation of frictional heat and reducing dirt accumulation.
  • the increase in the relaxation hole diameter causes an increase in the circumference relative to the discharge rate of the polymer, which serves to decrease the accumulated dirt density per unit circumferential length.
  • the molten polymer is discharged stably to provide a polyamide monofilament with a highly uniform fiber diameter. It is more preferably 3.0 to 3.7.
  • the relaxation hole diameter (D2) is in the range of 0.8 to 1.4 mm. If the relaxation hole diameter (D2) is adjusted in this range, the molten polymer can be discharged stably, and this prevents inclination and twitching of the polymer from being caused by dirt accumulated around the discharge hole. On the other hand, as the discharge is stabilized, inferior discharge is suppressed to prevent the formation of knots and thin filaments, thereby ensuring the production of a polyamide monofilament that shows high filtration performance.
  • the relaxation hole diameter (D2) is less than 0.8 mm
  • the accumulated dirt density per unit circumferential length will be large and it tends to cause dirt accumulation around the discharge hole that leads to inclination and twitching of the polymer.
  • the effect of relaxing the pressure on the molten polymer is weakened and the strain rate of the molten polymer will increase. Accordingly, larger frictional heat will be generated to cause the formation of dirt around the discharge hole, leading to deterioration in discharge stability.
  • the relaxation hole diameter (D2) is 1.4 mm or more, it will be difficult for the polymer to fill the entire discharge hole (relaxation hole in particular) uniformly, and variations in the discharge state will occur easily, leading to not only the formation of knots and thin filaments but also frequent breakage of the spun threads. It is more preferably 1.0 to 1.2 mm.
  • the spinning rate is 300 to 1,000 m/min, preferably 300 to 600 m/min in a two stage process and 300 to 800 m/min in a single stage process. If it is controlled in this range, it will be possible to produce a polyamide monofilament containing few knots and thin filaments and having high uniformity in fiber diameter.
  • a total of 50 measurements were taken from a fiber sample using a Tensilon (registered trademark) tester manufactured by Orientec Co., Ltd. according to JIS L 1013 (2010) under the conditions of elongation at a constant rate, a clamp-to-clamp distance of 50 cm, and a tension speed of 50 cm/min.
  • the tenacity was determined from the maximum tenacity on the tensile strength-elongation curve while the elongation was determined from the elongation at the maximum tenacity point.
  • the strength furthermore, the quotient of the maximum tenacity divided by the total fineness was adopted to represent the strength.
  • the strength-elongation product was calculated by the formula given below. A total of 50 measurements were taken, and the smallest one and the average were determined.
  • Strength-elongation product strength cN / dtex ⁇ 1 + elongation % / 100
  • a sample was rated as acceptable if its coefficient of variation in opening size was 3% or less, which is a value generally used as evaluation criteria for high precision filters.
  • Fig. 3 shows the melt-spinning pack used. It has a spinneret 30, pressure plate 27, metal wire filter 26, sintered filter 25, and sand filter 24.
  • the spinneret 30 has four discharge holes. As illustrated in Fig. 1 , each discharge hole has an inflow hole 2, metering hole 3, and relaxation hole 4, wherein the metering hole diameter (D1) is 0.30 mm, the metering hole length (L1) 0.75 mm, the relaxation hole diameter (D2) 1.0 mm, and the metering hole length (L2) 1.0 mm.
  • the sintered filter 25 is a sintered filter (with a thickness of 2 mm and a filtration accuracy of 40 ⁇ m) containing varied stainless steel short fibers each having a roughly polygonal cross section, a length of 1.0 to 3.0 mm, a converted diameter of 30 to 60 ⁇ m, and an aspect ratio of 10 to 100.
  • Nylon 66 chips with a 98% sulfuric acid relative viscosity of 2.8 was dried to an adjusted moisture content of 0.13% and melted at a melting temperature of 290°C.
  • the discharge rate was adjusted so that the polymer discharge rate of the entire melt-spinning pack was 6.5 g/min, and the polymer was fed to the melt-spinning pack and discharged through a round-hole spinneret in which two discharge holes were arranged circumferentially.
  • the resulting nylon 66 monofilament was evaluated in terms of the number of knots, fineness unevenness, strength-elongation product, and coefficient of variation in filter's opening size.
EP21817409.2A 2020-06-02 2021-05-27 Monofilament de polyamide Pending EP4141153A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2020095968 2020-06-02
PCT/JP2021/020116 WO2021246270A1 (fr) 2020-06-02 2021-05-27 Monofilament de polyamide

Publications (1)

Publication Number Publication Date
EP4141153A1 true EP4141153A1 (fr) 2023-03-01

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Application Number Title Priority Date Filing Date
EP21817409.2A Pending EP4141153A1 (fr) 2020-06-02 2021-05-27 Monofilament de polyamide

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EP (1) EP4141153A1 (fr)
JP (1) JPWO2021246270A1 (fr)
CN (1) CN115427617B (fr)
WO (1) WO2021246270A1 (fr)

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS549225B2 (fr) * 1971-08-09 1979-04-23
TW333562B (en) * 1995-02-09 1998-06-11 Schweizerische Viscose Dimensionally stable polyamide-66-monofilament
DE19600162A1 (de) * 1996-01-04 1997-07-10 Bayer Faser Gmbh Schmelzgesponnene, scheuerbeständige Monofile
TW371679B (en) * 1996-02-21 1999-10-11 Toray Industries Method for producing coarse and fine polyesteramide staple
JPH09268417A (ja) 1996-03-29 1997-10-14 Toray Ind Inc 溶融紡糸用口金および溶融紡糸方法
JP4042585B2 (ja) * 2002-02-18 2008-02-06 東レ株式会社 ポリアミドマルチフィラメントおよびそれからなるブラシ
CN104812949A (zh) * 2012-11-28 2015-07-29 东丽株式会社 衣料用聚酰胺卷曲丝及包含该聚酰胺卷曲丝的衣料用织物
JP6160250B2 (ja) 2013-05-29 2017-07-12 東レ株式会社 ポリアミドモノフィラメントの製造方法
CN110770376B (zh) 2017-08-30 2022-11-08 东丽株式会社 高精细高目数过滤器用单成分聚酯单丝
WO2019208404A1 (fr) * 2018-04-25 2019-10-31 東レ株式会社 Monofilament de polyamide

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CN115427617A (zh) 2022-12-02
CN115427617B (zh) 2024-02-09
WO2021246270A1 (fr) 2021-12-09
JPWO2021246270A1 (fr) 2021-12-09

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