WO2018174106A1 - 吸放湿性に優れたポリアミド繊維 - Google Patents

吸放湿性に優れたポリアミド繊維 Download PDF

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Publication number
WO2018174106A1
WO2018174106A1 PCT/JP2018/011222 JP2018011222W WO2018174106A1 WO 2018174106 A1 WO2018174106 A1 WO 2018174106A1 JP 2018011222 W JP2018011222 W JP 2018011222W WO 2018174106 A1 WO2018174106 A1 WO 2018174106A1
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molecular weight
polyamide
polyamide fiber
moisture absorption
cross
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PCT/JP2018/011222
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English (en)
French (fr)
Japanese (ja)
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林　剛史
澤井　由美子
一 藤井
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東レ株式会社
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Priority to JP2018525621A priority Critical patent/JP6996506B2/ja
Priority to CN201880020739.5A priority patent/CN110462119B/zh
Publication of WO2018174106A1 publication Critical patent/WO2018174106A1/ja

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  • the present invention relates to a polyamide fiber excellent in moisture absorption / release properties, particularly a high moisture absorption / release rate.
  • Synthetic fibers made of thermoplastic resins such as polyamide and polyester are widely used in clothing and industrial applications because they are excellent in strength, chemical resistance, heat resistance and the like.
  • polyamide fiber has excellent hygroscopicity in addition to its unique softness, high tensile strength, color development during dyeing, and high heat resistance, and is widely used for applications such as innerwear and sportswear.
  • polyamide fibers are not sufficiently hygroscopic compared to natural fibers such as cotton, and have problems such as stuffiness and stickiness, and are said to be inferior to natural fibers in terms of comfort.
  • Patent Document 1 proposes a method of producing a polyamide fiber with improved moisture absorption performance with high productivity by blending polyvinyl pyrrolidone as a hydrophilic polymer with polyamide and spinning by a specific production method.
  • Patent Document 2 proposes a polyamide fiber having a small yellowness by containing polyvinylpyrrolidone and a certain amount of pyrrolidone. With this fiber, a fabric excellent in drying speed can be realized.
  • the present invention has the following constitution for the purpose of providing a polyamide fiber having a high moisture absorption / release rate in order to meet the high demands as described above.
  • B) The ratio I L / I H between the peak intensity (I L ) on the low molecular weight side and the peak intensity (I H ) on the high molecular weight side of the molecular weight distribution is 0.02 to 0.10.
  • an unprecedented high moisture absorption / release polyamide fiber can be provided.
  • FIG. 1 illustrates a method for determining the degree of irregularity according to the present invention.
  • FIG. 2 illustrates a method for determining the number of cross-sectional irregularities according to the present invention and the cross-sectional shape of Example 16.
  • FIG. 3 illustrates a cross-sectional shape of Example 17 of the present invention.
  • the polyamide fiber of the present invention contains 3 to 15 wt% of polyvinylpyrrolidone (hereinafter sometimes abbreviated as PVP) and polyamide.
  • PVP polyvinylpyrrolidone
  • the hygroscopic potential is defined as the moisture absorption rate when left in an environment of 30 ° C. ⁇ 90% RH (relative humidity) for 24 hours and the moisture absorption rate when left in an environment of 20 ° C. ⁇ 65% RH for 24 hours. It can be expressed as a difference and is expressed as ⁇ MR.
  • PVP When PVP is 3 wt% or more, this ⁇ MR becomes a good value.
  • PVP can be contained in the polyamide fiber by a known method, and as described in Patent Document 2, it is a preferable example that PVP is prepared and kneaded into polyamide.
  • a more preferable range of the content of PVP is 3.5 to 15 wt%, and most preferable is a range of 4 to 15 wt%.
  • the polyamide of the present invention is not particularly limited.
  • a copolymer polyamide containing a copolymer component such as laurolactam, sebacic acid, terephthalic acid, isophthalic acid, 5-sodium sulfoisophthalic acid, and the like.
  • various additives such as matting agents, flame retardants, antioxidants, ultraviolet absorbers, infrared absorbers, crystal nucleating agents, fluorescent whitening agents, antistatic agents, carbon Etc. may be copolymerized or mixed as required. Even if about 10 wt% is added, the moisture absorption performance is not greatly affected.
  • the polyamide fiber of the present invention has two peaks in its molecular weight distribution, the low molecular weight peak has a molecular weight of 1000 to 2500, the low molecular weight peak intensity (I L ) and the high molecular weight peak.
  • the intensity (I H ) ratio I L / I H needs to be 0.02 to 0.10. It has been discovered that when the molecular weight distribution has a peak at 1000 to 2500, PVP works effectively in the fiber and the moisture absorption / release rate increases. Since PVP is easily dissolved in water, the entanglement between PVP and polyamide has been strengthened conventionally, thereby suppressing the dissolution of PVP into water. Since this entanglement is strong, it is considered that the moisture absorption / release rate does not increase. However, if the entanglement is weak, PVP dissolves in water, suggesting a so-called trade-off relationship in which the moisture absorption performance itself decreases. In order to eliminate this relationship, intensive studies were made to arrive at the present invention.
  • the low molecular weight side peak has a molecular weight of 1000 to 2500, and when the molecular weight is less than 1000, the entanglement between PVP and polyamide is inhibited, so that elution into water occurs and the hygroscopic property does not increase. If the molecular weight is greater than 2500, PVP cannot work effectively, so the moisture absorption rate does not increase.
  • a more preferred low molecular weight side peak is a molecular weight of 1200 to 2200, most preferably a molecular weight of 1400 to 2000.
  • the ratio I L / I H of the peak strength of the low molecular weight side (I L) and high molecular weight side of the peak intensity (I H) is at 0.02-0.10 and dissolution inhibition in water absorbing Wet speed is compatible. If it is less than 0.02, the effect of improving the moisture absorption / release rate is extremely small. Conversely, if it is greater than 0.10, the elution into water cannot be suppressed.
  • a more preferable peak intensity ratio is in the range of 0.03 to 0.10.
  • a low molecular weight polyamide In order to develop a peak on the low molecular weight side, it is preferable to add a low molecular weight polyamide. As described above, various types of main polyamide that forms a peak on the high molecular weight side can be applied. However, the polyamide on the low molecular weight side may be the same as the main polyamide or a different polyamide. The molecular weight distribution having two peaks at the final fiber stage may be used. It is conceivable that the molecular weight of the low molecular weight polyamide added before spinning is shifted by spinning. For example, when held in a molten state for a long time, the molecular weight increases, and when moisture is given in the molten state, the molecular weight decreases.
  • a desired fiber is manufactured through adjustment under these spinning conditions.
  • the simplest method is to cancel the molecular weight distribution of the prepared polyamide and the polyamide used as a fiber as much as possible by offsetting the molecular weight equivalent of the amount that becomes higher in the molten state with moisture. With this method, it is easy to produce the polyamide fiber of the present invention by adding a desired low molecular weight polyamide to the main polyamide before yarn production.
  • the cross-sectional shape of the polyamide fiber of the present invention may be any of general round cross-section and irregular cross-section, hollow or composite with other polyamide fibers, but a more preferable form is an average multi-filament profile 1.1 to 4, and the cross-sectional shape of at least one filament of the multifilament is a multilobal cross section composed of three or more convex portions and three or more concave portions.
  • the irregularity in the present invention is the ratio of the diameter Do of the circumscribed circle and the diameter Di of the inscribed circle of the cross section of an arbitrary one of the multifilaments, as shown in FIG. .
  • the filament for clothing is a multifilament, and a plurality of filaments are bundled.
  • the degree of irregularity of each cross section is measured, and the average value is defined as the degree of irregularity of the present invention.
  • the elliptical cross section may have an irregularity of 1.1 or more.
  • the moisture absorption / release rate is improved because the surface area is larger than a perfect circle. It is also effective to perform false twisting. Since the cross-sectional shape is crushed by false twisting, the surface area increases. It is not necessary for all the multifilaments to have the same cross-sectional shape, and the same effect can be obtained by making a mix of round and irregular cross-sections.
  • the cross-sectional shape is a so-called multi-leaf cross section having a convex portion and a concave portion. Since the surface area is further increased when the cross section has three or more convex portions and three or more concave portions, the moisture absorption and desorption rate is improved. When the number is increased to 5 leaves or 7 leaves, more preferable performance can be obtained.
  • Counting of convex portions and concave portions is performed as shown in FIG. First, a base line having a smooth circular or elliptical cross section is drawn. The base line is drawn so that the cross-sectional area in the base line is the same as the cross-sectional area of the actual cross section. Next, a portion having a continuously large diameter with respect to the base line (A portion in FIG. 2) is defined as a convex portion, and a portion having a continuously small diameter (B portion in FIG. 2) is defined as a concave portion.
  • the polyamide fiber of the present invention is not limited in its fineness and number of filaments.
  • a fineness of about 5 dtex to 22 dtex is used, a fineness of 22 dtex to 56 dtex is preferably used for the inner, and a fineness of more than that is preferably used for the outer.
  • Any number of filaments can be selected.
  • the method for producing the polyamide fiber of the present invention it is necessary to pay attention to the fact that the low molecular weight side peak moves, and it can be controlled by the conditions as described above, but other yarn producing conditions are affected. Is small. For this reason, it is possible to select any of the conventional spinning methods that are preferably used, and the one-step method, which is superior in cost, the two-step method that is the conventional method, POY spinning for false twisting, and composite spinning. The method of doing is mentioned as an example. In addition, known methods such as a base to be used, cooling, an applied oil agent, entanglement, and winding can be applied.
  • the obtained fiber can be subjected to known yarn processing such as false twist processing, twist processing, and composite processing represented by Taslan processing, and there is no decrease in the moisture absorption rate.
  • a process with an irregular cross-sectional shape is a preferable process.
  • it can be developed for any use of woven and knitted fabrics, and is preferably developed for clothing. It is preferably used for inner / underwear such as stockings and underwear, mid-layers, outerwear, etc., and sports inners that require a moisture absorption / release rate are particularly preferred applications.
  • Relative viscosity 0.25 g of a sample was dissolved so as to be 1 g in 100 ml of sulfuric acid having a concentration of 98% by weight, and the flow time (T1) at 25 ° C. was measured using an Ostwald viscometer. Subsequently, the flow-down time (T2) of only 98% by weight sulfuric acid was measured.
  • Fineness 1. Set a fiber sample on a 125 m / round measuring instrument, rotate it 200 times to make a looped skein, and dry it with a hot air dryer (105 ⁇ 2 ° C. ⁇ 60 minutes). The fineness was calculated from the value obtained by measuring the skein mass and multiplying by the official moisture content. The official moisture content of the core-sheath composite yarn was 4.5% by weight.
  • the pump is Waters 515 (manufactured by Waters)
  • the detector is a differential refractometer Waters 410 (manufactured by Waters)
  • the column is Shodex HFIP-806M (two) + HFIP-LG, the flow rate is 0.5 ml / min, the sample
  • the injection volume was 0.1 ml and the temperature was 40 ° C.
  • a PVP calibration curve was prepared in advance, and the content was quantified (the second decimal place was rounded off).
  • the fiber was weighed so that the polyamide resin content in the polyamide fiber was 2.5 mg, and dissolved in 4 ml of hexafluoroisopropanol (0.005N-sodium trifluoroacetate added) at a polymer concentration of 6.2 ppm.
  • GPC measurement was performed using a solution obtained by filtering with a filter having a pore size of 0.45 ⁇ m.
  • the pump is Waters 515 (manufactured by Waters)
  • the detector is a differential refractometer Waters 410 (manufactured by Waters)
  • the column is Shodex HFIP-806M (two) + HFIP-LG, the flow rate is 0.5 ml / min, the sample
  • the injection volume was 0.1 ml and the temperature was 40 ° C.
  • the molecular weight calibration was performed using polymethyl methacrylate.
  • Peak position by the supplied analysis tools read the peak intensity, low molecular weight side peak molecular weight (three significant figures), the ratio I L of the peak strength of the low molecular weight side (I L) and high molecular weight side of the peak intensity (I H) / I H (rounded to the second decimal place) was specified.
  • Average degree of irregularity and number of cross-sectional irregularities Take a cross-sectional photograph (2000 times) of all multifilaments of polyamide fiber and check the diameter of the circumscribed circle (Do) and the diameter of the inscribed circle (Di) of each single yarn The ratio Do / Di was calculated, and the average value of the multifilament Do / Di was defined as the average degree of irregularity (2 significant digits).
  • the number of irregularities in the cross section was the number of irregularities in the cross section of all the multifilaments. For example, in the case of a round cross section, the number of cross-sectional irregularities is 0.
  • a tubular knitted fabric was prepared by adjusting the degree to 50 with a tubular knitting machine.
  • the yarns are appropriately combined so that the total fineness of the fibers fed to the cylindrical knitting machine is 50 to 100 dtex, and when the total fineness exceeds 100 dtex, the yarn is fed to the cylindrical knitting machine. This was carried out with a single piece and adjusted so that the degree was 50 as described above.
  • About 1 to 2 g of this tubular knitted fabric was weighed into a weighing bottle, kept at 110 ° C. for 2 hours and dried to measure the weight (W0).
  • the target substance was kept at 20 ° C. and a relative humidity of 65% for 24 hours, and then the weight was measured (W65).
  • Example 1 A polyamide resin prepared by kneading 2.0 wt% nylon 6 having a weight average molecular weight of 1400 and 3.0 wt% PVP in nylon 6 having a relative viscosity of 2.7 was prepared. In order to prevent the molecular weight from changing after the fiber was formed, the moisture content of the resin was 0.1 wt%, and the time from polymer melting to die discharge was 13 minutes. A polyamide fiber having 33 dtex-26 filaments and all filaments having a round cross section was produced in accordance with a one-step method. The low molecular weight side peak molecular weight of the polyamide fiber was 1430, and the peak intensity ratio I L / I H was 0.04. The obtained polyamide fiber showed excellent characteristics with ⁇ MR of 2.8%, moisture absorption / release rate of 780 ppm / min, and elution rate of 1.8%.
  • Examples 2 and 3 A polyamide fiber was produced in the same manner as in Example 1 except that PVP was 3.7 wt% as Example 2 and PVP was 4.1 wt% as Example 3. Polyamide fibers having low molecular weight side peak molecular weights and peak intensity ratios I L / I H of 1440 and 0.04 in Example 2 and 1430 and 0.04 in Example 3, respectively were obtained. By increasing the amount of PVP, ⁇ MR was also improved to 3.0% and 3.1%, and the moisture absorption / release rate was also improved to 830 ppm / min.
  • Comparative Example 1 A polyamide fiber was produced in the same manner as in Example 1 except that the amount of PVP was 2.5 wt%. The amount of PVP was small, ⁇ MR was insufficient at 2.5%, and the moisture absorption / release rate was not satisfactory.
  • Example 4 A polyamide fiber was produced in the same manner as in Example 3, except that I L / I H of the polyamide fiber was adjusted to 0.02 in Example 4 and 0.07 in Example 5. Although ⁇ MR, which is a conventional index, does not change greatly, increasing the strength of the low molecular weight peak significantly improves the moisture absorption / release rate. In Example 5, a favorable result of 960 ppm / min was obtained.
  • Comparative Examples 2 and 3 The I L / I H of polyamide fiber, Comparative Example 2 In 0.01, was prepared polyamide fibers in the same manner as in Example 3 except that was adjusted to 0.12 in Comparative Example 3.
  • the ⁇ MR was as good as 3.1%, but the moisture absorption / release rate was insufficient in Comparative Example 2, and the dissolution property was insufficient in Comparative Example 3, both of which failed.
  • Examples 6-11 The amount of PVP to be kneaded was 6.0 wt%, and the molecular weight of the low molecular weight nylon 6 was changed to obtain a polyamide fiber having a low molecular weight side peak molecular weight of 1000 to 2500 as shown in Table 3.
  • the results of Examples 6, 7, and 9 to 11 are shown in Table 3, and the result of Example 8 is shown in Table 5.
  • Comparative Examples 4 and 5 Polyamide fibers having low molecular weight side peak molecular weights of 790 and 2830 were prepared and evaluated. When the molecular weight is low, the elution property is insufficient, and when the molecular weight is too high, the moisture absorption / release rate is insufficient.
  • Example 12 Except that containing PVP 13.0 wt% will produce a polyamide fiber in the same manner as in Example 8, the molecular weight of the low molecular weight side peak 1620, I L / I H to obtain a polyamide fiber is 0.04. ⁇ MR was 6.7%, the moisture absorption / release rate was 1080 ppm / min, and the elution rate was 4.3%.
  • Example 13 As another additive, a polyamide fiber was produced in the same manner as in Example 8 except that 2.0 wt% of titanium dioxide was added to obtain a fiber of 11 dtex-10 filament. The effect of adding titanium dioxide was not seen, and the result was good.
  • Example 14 A polyamide fiber was obtained in the same manner as in Example 8 except that the cross-sectional shape of all the filaments was 25% hollow and a fiber of 25 dtex-26 filament was used. Even hollow fibers demonstrated good performance.
  • Examples 15-18 A polyamide fiber was produced in the same manner as in Example 8 except that the cross-sectional shape was changed from the round cross-section as shown in Table 5.
  • Example 15 an elliptical cross section in which the irregularity of all the filaments was 2.5 was used. Compared with Example 8, a slight improvement in moisture absorption / release rate was observed, and the effect of deforming was confirmed.
  • Example 16 all the filaments had a cross-section of four leaves in FIG. In this case, the average degree of irregularity is 1.5 and the number of cross-sectional irregularities is 4. The moisture absorption / release rate of this polyamide fiber increased to 920 ppm / min, and good results were obtained.
  • Example 17 all the filaments had a cross-section of the flat 8 leaf of FIG.
  • the average degree of irregularity is 3.7 and the number of cross-sectional irregularities is 8.
  • the moisture absorption / release rate of this polyamide fiber was 1020 ppm / min, and the effects of the degree of irregularity and the number of cross-sectional irregularities could be confirmed.
  • Example 18 a test was carried out with 13 filaments having a round cross section and the remaining 13 filaments having a 6-leaf cross section with an irregularity of 1.4, and further adding 2 wt% of titanium dioxide.
  • the average degree of irregularity is 1.2, and the number of cross-sectional irregularities is 6. As shown in Table 5, a good moisture absorption / release rate was shown.
  • Example 19 A polyamide resin similar to Example 8 was used as a partially oriented yarn (POY) of 41 dtex-26 filament, and false twisting was performed to obtain a polyamide fiber of 33 dtex-26 filament. Since false twisting was performed, the cross-sectional shape collapsed and the average degree of irregularity was 1.3. Since it collapsed randomly, the number of cross-sectional irregularities was not judged and was set to zero. The moisture absorption / release rate of the obtained fiber was improved as compared with Example 8, and the effect was observed even when the fiber was deformed by false twisting.
  • POY partially oriented yarn
  • Comparative Example 6 A polyamide fiber was produced in the same manner as in Example 8 except that the molecular weight of the low molecular weight side peak was 810, the peak intensity ratio IL / IH was 0.01, and the cross-sectional shape was flat 8-leaf. As is apparent from Table 5, the moisture absorption / release rate was not satisfactory although it was a flat 8-leaf cross section.
  • the polyamide fiber of the invention can provide a polyamide fiber having a high moisture absorption / release rate, and can provide comfortable clothing.
  • Convex part B Concave part

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PCT/JP2018/011222 2017-03-24 2018-03-20 吸放湿性に優れたポリアミド繊維 WO2018174106A1 (ja)

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CN201880020739.5A CN110462119B (zh) 2017-03-24 2018-03-20 吸放湿性优异的聚酰胺纤维

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Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH0369610A (ja) * 1989-06-05 1991-03-26 E I Du Pont De Nemours & Co Ｐｖｐ／パラ―アラミド繊維およびそれを作る方法
JPH07150414A (ja) * 1993-11-26 1995-06-13 Toray Ind Inc 吸湿性ポリアミド繊維及びそれからなるインナーウェア、靴下、スポーツウェア
JPH1112806A (ja) * 1997-04-28 1999-01-19 Toray Ind Inc 吸湿性に優れたインナーウェア
JP2003049066A (ja) * 2001-08-03 2003-02-21 Nippon Shokubai Co Ltd 色調の改良された高吸湿性ポリアミド

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JP3804097B2 (ja) * 1996-03-29 2006-08-02 東レ株式会社 着用快適性に優れたサポートストッキング
US6123760A (en) * 1998-10-28 2000-09-26 Hercules Incorporated Compositions and methods for preparing dispersions and methods for using the dispersions
EP1338616A1 (en) * 2002-02-22 2003-08-27 Dsm N.V. Process for preparing a high-molecular polyamide, polyester, copolyesters or polyester-amide block copolymer
KR101436089B1 (ko) * 2012-02-01 2014-08-29 아주대학교산학협력단 전도성 고분자 블랜드 조성물 및 이의 제조 방법
CN103668535A (zh) * 2012-09-19 2014-03-26 东丽纤维研究所（中国）有限公司 聚酰胺纤维、含聚酰胺纤维的织物及制造方法
CN103882549A (zh) * 2012-12-24 2014-06-25 东丽纤维研究所（中国）有限公司 一种高吸湿防黄变聚酰胺纤维及其制造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0369610A (ja) * 1989-06-05 1991-03-26 E I Du Pont De Nemours & Co Ｐｖｐ／パラ―アラミド繊維およびそれを作る方法
JPH07150414A (ja) * 1993-11-26 1995-06-13 Toray Ind Inc 吸湿性ポリアミド繊維及びそれからなるインナーウェア、靴下、スポーツウェア
JPH1112806A (ja) * 1997-04-28 1999-01-19 Toray Ind Inc 吸湿性に優れたインナーウェア
JP2003049066A (ja) * 2001-08-03 2003-02-21 Nippon Shokubai Co Ltd 色調の改良された高吸湿性ポリアミド

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JPWO2018174106A1 (ja) 2020-01-23
TW201840712A (zh) 2018-11-16
CN110462119B (zh) 2022-03-11
CN110462119A (zh) 2019-11-15
TWI768013B (zh) 2022-06-21
JP6996506B2 (ja) 2022-01-17

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