JP5290833B2 - Antistatic fabric manufacturing method and apparel manufacturing method - Google Patents
Antistatic fabric manufacturing method and apparel manufacturing method Download PDFInfo
- Publication number
- JP5290833B2 JP5290833B2 JP2009082071A JP2009082071A JP5290833B2 JP 5290833 B2 JP5290833 B2 JP 5290833B2 JP 2009082071 A JP2009082071 A JP 2009082071A JP 2009082071 A JP2009082071 A JP 2009082071A JP 5290833 B2 JP5290833 B2 JP 5290833B2
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- JP
- Japan
- Prior art keywords
- fabric
- antistatic
- pollen
- sheath
- core
- 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.)
- Expired - Fee Related
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- 239000004744 fabric Substances 0.000 title claims description 78
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000000835 fiber Substances 0.000 claims description 61
- 239000002216 antistatic agent Substances 0.000 claims description 51
- 239000002131 composite material Substances 0.000 claims description 37
- 239000008358 core component Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 26
- 239000000306 component Substances 0.000 claims description 25
- 229920000728 polyester Polymers 0.000 claims description 23
- 239000005871 repellent Substances 0.000 claims description 15
- 230000002940 repellent Effects 0.000 claims description 13
- 125000003118 aryl group Chemical group 0.000 claims description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 230000035699 permeability Effects 0.000 claims description 6
- 239000002759 woven fabric Substances 0.000 claims description 6
- 230000024100 pollen adhesion Effects 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 150000008040 ionic compounds Chemical class 0.000 claims description 3
- 230000000740 bleeding effect Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 description 35
- -1 aromatic carboxylic acids Chemical class 0.000 description 33
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- 238000012545 processing Methods 0.000 description 18
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 14
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 10
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- 125000004432 carbon atom Chemical group C* 0.000 description 8
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- 239000003242 anti bacterial agent Substances 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
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- 125000005702 oxyalkylene group Chemical group 0.000 description 2
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 2
- 150000004714 phosphonium salts Chemical group 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
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- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ZRPKEUVFESZUKX-UHFFFAOYSA-N 2-(2-hydroxyethoxy)benzoic acid Chemical compound OCCOC1=CC=CC=C1C(O)=O ZRPKEUVFESZUKX-UHFFFAOYSA-N 0.000 description 1
- BXGYYDRIMBPOMN-UHFFFAOYSA-N 2-(hydroxymethoxy)ethoxymethanol Chemical compound OCOCCOCO BXGYYDRIMBPOMN-UHFFFAOYSA-N 0.000 description 1
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 1
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- RSROEZYGRKHVMN-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;oxirane Chemical class C1CO1.CCC(CO)(CO)CO RSROEZYGRKHVMN-UHFFFAOYSA-N 0.000 description 1
- QWGRWMMWNDWRQN-UHFFFAOYSA-N 2-methylpropane-1,3-diol Chemical compound OCC(C)CO QWGRWMMWNDWRQN-UHFFFAOYSA-N 0.000 description 1
- DYBIGIADVHIODH-UHFFFAOYSA-N 2-nonylphenol;oxirane Chemical class C1CO1.CCCCCCCCCC1=CC=CC=C1O DYBIGIADVHIODH-UHFFFAOYSA-N 0.000 description 1
- FWQNYUYRXNWOOM-UHFFFAOYSA-N 2-nonylpropanedioic acid Chemical compound CCCCCCCCCC(C(O)=O)C(O)=O FWQNYUYRXNWOOM-UHFFFAOYSA-N 0.000 description 1
- KHZYMPDILLAIQY-UHFFFAOYSA-N 3-(3-carboxyphenyl)benzoic acid Chemical compound OC(=O)C1=CC=CC(C=2C=C(C=CC=2)C(O)=O)=C1 KHZYMPDILLAIQY-UHFFFAOYSA-N 0.000 description 1
- NEQFBGHQPUXOFH-UHFFFAOYSA-N 4-(4-carboxyphenyl)benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC=C(C(O)=O)C=C1 NEQFBGHQPUXOFH-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
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- URRLLRVIUROMEQ-UHFFFAOYSA-N anthracene-1,6-dicarboxylic acid Chemical compound OC(=O)C1=CC=CC2=CC3=CC(C(=O)O)=CC=C3C=C21 URRLLRVIUROMEQ-UHFFFAOYSA-N 0.000 description 1
- XAAYMWLCUICVSL-UHFFFAOYSA-N anthracene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC3=CC(C(=O)O)=CC=C3C=C21 XAAYMWLCUICVSL-UHFFFAOYSA-N 0.000 description 1
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- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- SIFUVXFIMXORMW-UHFFFAOYSA-N benzyl(triphenyl)phosphanium;dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1.C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)CC1=CC=CC=C1 SIFUVXFIMXORMW-UHFFFAOYSA-N 0.000 description 1
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- VBVCYAZECWLFHP-UHFFFAOYSA-N dodecyl benzenesulfonate;tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 VBVCYAZECWLFHP-UHFFFAOYSA-N 0.000 description 1
- XWTOMWARSPYOAY-UHFFFAOYSA-N dodecyl benzenesulfonate;tetraphenylphosphanium Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1.C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 XWTOMWARSPYOAY-UHFFFAOYSA-N 0.000 description 1
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- KBAFDSIZQYCDPK-UHFFFAOYSA-M sodium;octadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCS([O-])(=O)=O KBAFDSIZQYCDPK-UHFFFAOYSA-M 0.000 description 1
- HRQDCDQDOPSGBR-UHFFFAOYSA-M sodium;octane-1-sulfonate Chemical compound [Na+].CCCCCCCCS([O-])(=O)=O HRQDCDQDOPSGBR-UHFFFAOYSA-M 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-O triphenylphosphanium Chemical compound C1=CC=CC=C1[PH+](C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-O 0.000 description 1
Landscapes
- Professional, Industrial, Or Sporting Protective Garments (AREA)
- Multicomponent Fibers (AREA)
- Woven Fabrics (AREA)
Description
本発明は、制電剤を含む制電性ポリマーにより芯成分が形成された芯鞘型複合繊維を含む制電性布帛であって、優れた制電性を有する制電性布帛、および該制電性布帛を用いてなる衣料に関するものである。 The present invention relates to an antistatic fabric comprising a core-sheath composite fiber in which a core component is formed of an antistatic polymer containing an antistatic agent, the antistatic fabric having excellent antistatic properties, and the antistatic fabric. The present invention relates to clothing using an electric fabric.
ポリエステル繊維などの合成繊維を用いた布帛は一般的に静電気を蓄積し易い性質を持ち、衣類のまとわりつきなど着用者に不快感を与えることがある。そして、その対策として、芯成分が制電剤を含む制電性ポリマーにより形成された芯鞘型複合繊維を含む制電性布帛が提案されている（例えば、特許文献１、特許文献２参照）。 Fabrics using synthetic fibers such as polyester fibers generally have the property of easily accumulating static electricity, and may cause discomfort to the wearer such as clinging clothes. And as the countermeasure, the antistatic fabric containing the core-sheath-type composite fiber in which the core component was formed with the antistatic polymer containing an antistatic agent is proposed (for example, refer patent document 1 and patent document 2). .
しかしながら、前記芯鞘型複合繊維において、芯鞘型複合繊維の製糸性を向上させるため、制電性ポリマーにより形成された芯成分が非制電性ポリマーからなる鞘成分で覆われており、制電性布帛の制電性が十分には発現されないという問題があった。 However, in the core-sheath type composite fiber, the core component formed of the antistatic polymer is covered with a sheath component made of a non-antistatic polymer in order to improve the yarn-making property of the core-sheath type composite fiber. There is a problem that the antistatic property of the electric fabric is not sufficiently exhibited.
本発明は上記の背景に鑑みなされたものであり、その目的は、制電剤を含む制電性ポリマーにより芯成分が形成された芯鞘型複合繊維を含む制電性布帛であって、優れた制電性を有する制電性布帛、および該制電性布帛を用いてなる衣料を提供することにある。 The present invention has been made in view of the above background, and an object thereof is an antistatic fabric including a core-sheath type composite fiber in which a core component is formed of an antistatic polymer including an antistatic agent, Another object of the present invention is to provide an antistatic fabric having antistatic properties and a clothing using the antistatic fabric.
本発明者は上記課題を達成するため鋭意検討した結果、制電剤を含む制電性ポリマーにより芯成分が形成された芯鞘型複合繊維を含む布帛に特定の加熱処理を施すことにより、芯成分に含まれる制電剤が鞘成分にブリードアウト（しみ出し）し制電剤が繊維表面に露出することにより、優れた制電性を奏することを見出し、さらに鋭意検討を重ねることにより本発明を完成するに至った。 As a result of intensive studies to achieve the above-mentioned problems, the present inventor has performed a specific heat treatment on a fabric containing a core-sheath type composite fiber in which a core component is formed of an antistatic polymer containing an antistatic agent. It is found that the antistatic agent contained in the component bleeds out into the sheath component and the antistatic agent is exposed on the fiber surface. It came to complete.
かくして、本発明によれば「制電剤を含む芯成分であって芳香族ポリエステル１００重量部に対して（ａ）ポリオキシアルキレン系ポリエーテル０．２〜３０重量部および（ｂ）有機イオン性化合物０．０５〜１０重量部を含有するポリエステルで形成されてなる芯成分と、鞘成分とで形成される、単糸繊度が１．５ｄｔｅｘ以下である芯鞘型複合繊維を含む布帛に、温度１３０℃以上、線圧８０００〜２００００Ｎ／ｍのカレンダー加工を施し、前記芯成分に含まれる制電剤を鞘部にブリードアウトさせることにより、前記芯鞘型複合繊維を、芯成分および鞘成分に制電剤が含まれる芯鞘型複合繊維とすることを特徴とする制電性布帛の製造方法。」が提供される。 Thus, according to the present invention, “ (a) 0.2 to 30 parts by weight of a polyoxyalkylene polyether and (b) organic ionic property with respect to 100 parts by weight of an aromatic polyester, which is a core component containing an antistatic agent . A fabric containing a core-sheath type composite fiber having a single yarn fineness of 1.5 dtex or less, which is formed of a core component formed of polyester containing 0.05 to 10 parts by weight of a compound and a sheath component, The core-sheath composite fiber is converted into a core component and a sheath component by performing calendar processing at 130 ° C. or higher and a linear pressure of 8000 to 20000 N / m and bleeding out the antistatic agent contained in the core component to the sheath portion. There is provided a method for producing an antistatic fabric, characterized in that a core-sheath composite fiber containing an antistatic agent is provided.
本発明において、得られた布帛が織物であり、かつカバーファクター（ＣＦ）が１４００以上であることが好ましい。
ただし、カバーファクター（ＣＦ）は下記式により算出される。
ＣＦ＝（ＤＷｐ／１．１）１／２×ＭＷｐ＋（ＤＷｆ／１．１）１／２×ＭＷｆ
［ＤＷｐは経糸総繊度（ｄｔｅｘ）、ＭＷｐは経糸織密度（本／２．５４ｃｍ）、ＤＷｆ
は緯糸総繊度（ｄｔｅｘ）、ＭＷｆは緯糸織密度（本／２．５４ｃｍ）である。］
In the present invention, the obtained fabric is preferably a woven fabric and the cover factor (CF) is preferably 1400 or more.
However, the cover factor (CF) is calculated by the following formula.
CF = (DWp / 1.1) 1/2 × MWp + (DWf / 1.1) 1/2 × MWf
[DWp is the total warp fineness (dtex), MWp is the warp weave density (main / 2.54 cm), DWf
Is the total weft fineness (dtex), and MWf is the weft weave density (main / 2.54 cm). ]
また、布帛に撥水加工が施されていることが好ましい。また、得られた布帛の摩擦耐電圧が３０００Ｖ以下であることが好ましい。また、得られた布帛の通気度が１０ｃｃ／ｃｍ２・ｓｅｃ以下であることが好ましい。また、得られた布帛の撥水性が４級以上であることが好ましい。また、得られた布帛において、下記に定義する花粉脱落性が７０％以上であることが好ましい。 Moreover, it is preferable that the water repellent finish is given to the fabric. Moreover, it is preferable that the friction withstand voltage of the obtained fabric is 3000 V or less. Further, the air permeability of the obtained fabric is preferably 10 cc / cm 2 · sec or less. Moreover, it is preferable that the water repellency of the obtained fabric is 4th grade or more. Moreover, in the obtained fabric, it is preferable that the pollen detachment property defined below is 70% or more.
タテ１０ｃｍ、ヨコ１０ｃｍの大きさに裁断したシートを、同サイズの、表面が平らなステンレス製平板に貼り付けた後、試料をビニールボックス内に配置し、１ｇの擬似花粉（石松子）をエアブラシにて噴霧し均一に飛散させた。飛散５分後に擬似花粉が均一に付着した試料を取り出し、デジタルカメラ顕微鏡システム（商品名：ＮＹｐｉｘＳ２スーパーシステム、マイクロネット社製）で１００倍に拡大し画面上の擬似花粉付着数（ｎ数＝３）をカウントする。次いで、シートを貼り付けた該平板を上下逆さにした状態で、高さ５ｃｍより１５ｇのおもりを該平板に落下させ、デジタルカメラ顕微鏡システムで擬似花粉付着数を測定した場所と同一の場所での残存擬似花粉付着数（ｎ数＝３）をカウントする。そして、次式で花粉脱落性（％）を求める。
花粉脱落性（％）＝１００−（（残存擬似花粉付着数）／（擬似花粉付着数）×１００）
また、本発明によれば、前記の制電性布帛を用いて衣料を製造する、衣料の製造方法が提供される。
A sheet cut to a size of 10 cm in length and 10 cm in width is affixed to a stainless steel flat plate of the same size, and the sample is placed in a vinyl box, and 1 g of pseudo pollen (Ishimatsuko) is airbrushed. And sprayed uniformly. After 5 minutes of scattering, a sample with pseudo pollen uniformly attached was taken out and magnified 100 times with a digital camera microscope system (trade name: NYpixS2 super system, manufactured by Micronet), and the number of pseudo pollen adhered on the screen (n number = 3) ). Next, in a state where the flat plate to which the sheet is attached is turned upside down, a weight of 15 g from 5 cm in height is dropped on the flat plate, and the same place where the number of pseudo pollen adhesion was measured with a digital camera microscope system. Count the number of remaining pseudo-pollens (n number = 3). And pollen fall-off property (%) is calculated | required by following Formula.
Pollen shedding (%) = 100 − ((number of remaining pseudo pollen deposits) / (number of pseudo pollen deposits) × 100)
Moreover, according to this invention, the manufacturing method of clothing which manufactures clothing using the said antistatic fabric is provided.
本発明によれば、制電剤を含む制電性ポリマーにより芯成分が形成された芯鞘型複合繊維を含む制電性布帛であって、優れた制電性を有する制電性布帛、および該制電性布帛を用いてなる衣料が得られる。 According to the present invention, an antistatic fabric comprising a core-sheath type composite fiber in which a core component is formed of an antistatic polymer containing an antistatic agent, and having an excellent antistatic property, and Apparel using the antistatic fabric is obtained.
以下、本発明の実施の形態について詳細に説明する。
まず、本発明で用いる芯鞘型複合繊維において、芯成分が、制電剤を含む制電性ポリマーにより形成されている。繊維が、制電剤を含む制電性ポリマー単独から形成される場合は、製糸性が低下するため本発明から除外する。
Hereinafter, embodiments of the present invention will be described in detail.
First, in the core-sheath type composite fiber used in the present invention, the core component is formed of an antistatic polymer containing an antistatic agent. In the case where the fiber is formed from an antistatic polymer alone containing an antistatic agent, it is excluded from the present invention because the spinning performance is lowered.
ここで、芯成分を形成するポリマーとしては制電剤を含むポリマーであれば特に限定されない。例えば、特開２００６−１０４６１７号公報に記載されたものでもよいが、芳香族ポリエステル１００重量部に対して（ａ）ポリオキシアルキレン系ポリエーテル０．２〜３０重量部および（ｂ）有機イオン性化合物０．０５〜１０重量部を含有してなる制電性ポリエステルであると、優れた制電性が得られ好ましい。 Here, the polymer forming the core component is not particularly limited as long as it is a polymer containing an antistatic agent. For example, although what was described in Unexamined-Japanese-Patent No. 2006-104617 may be sufficient, (a) 0.2-30 weight part of polyoxyalkylene-type polyether with respect to 100 weight part of aromatic polyester, and (b) organic ionicity An antistatic polyester comprising 0.05 to 10 parts by weight of the compound is preferable because excellent antistatic properties are obtained.
ここで、前記芳香族ポリエステルとしては、二官能性芳香族カルボン酸またはそのエステル形成性誘導体とジオールまたはそのエステル形成性誘導体との反応により得られる重合体を対象とする。 Here, the aromatic polyester is a polymer obtained by a reaction of a difunctional aromatic carboxylic acid or an ester-forming derivative thereof and a diol or an ester-forming derivative thereof.
ここでいう二官能性芳香族カルボン酸としてはテレフタル酸、イソフタル酸、オルトフタル酸、１，５―ナフタレンジカルボン酸、２，５―ナフタレンジカルボン酸、２，６―ナフタレンジカルボン酸、４，４′―ビフェニルジカルボン酸、３，３′―ビフェニルジカルボン酸、４，４′―ビフェニルエーテルジカルボン酸、４，４′―ビフェニルメタンジカルボン酸、４，４′―ビフェニルスルホンジカルボン酸、４，４′―ビフェニルイソプロピリデンジカルボン酸、１，２―ビス（フェノキシ）エタン―４，４′―ジカルボン酸、２，５―アントラセンジカルボン酸、２，６―アントラセンジカルボン酸、４，４′―ｐ―フェニレンジカルボン酸、２，５―ピリジンジカルボン酸、β―ヒドロキシエトキシ安息香酸、ｐ―オキシ安息香酸等をあげることができ、特にテレフタル酸が好ましい。 Examples of the bifunctional aromatic carboxylic acid herein include terephthalic acid, isophthalic acid, orthophthalic acid, 1,5-naphthalenedicarboxylic acid, 2,5-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid, 4,4′- Biphenyl dicarboxylic acid, 3,3'-biphenyl dicarboxylic acid, 4,4'-biphenyl ether dicarboxylic acid, 4,4'-biphenylmethane dicarboxylic acid, 4,4'-biphenyl sulfone dicarboxylic acid, 4,4'-biphenyl isopropyl Redene dicarboxylic acid, 1,2-bis (phenoxy) ethane-4,4'-dicarboxylic acid, 2,5-anthracene dicarboxylic acid, 2,6-anthracene dicarboxylic acid, 4,4'-p-phenylenedicarboxylic acid, 2 , 5-Pyridinedicarboxylic acid, β-hydroxyethoxybenzoic acid, p-oxybenzoic acid Etc. can be mentioned, in particular, terephthalic acid is preferred.
これらの二官能性芳香族カルボン酸は２種以上併用してもよい。なお、少量であればこれらの二官能性芳香族カルボン酸とともにアジピン酸、アゼライン酸、セバシン酸、ドデカンジオン酸の如き二官能性脂肪族カルボン酸、シクロヘキサンジカルボン酸の如き二官能性脂環族カルボン酸、５―ナトリウムスルホイソフタル酸等を１種または２種以上併用することができる。 Two or more of these difunctional aromatic carboxylic acids may be used in combination. In addition, in a small amount, these bifunctional aromatic carboxylic acids and bifunctional aliphatic carboxylic acids such as adipic acid, azelaic acid, sebacic acid and dodecanedioic acid, and bifunctional alicyclic carboxylic acids such as cyclohexanedicarboxylic acid are used. An acid, 5-sodium sulfoisophthalic acid, etc. can be used alone or in combination of two or more.
また、ジオール化合物としてはエチレングリコール、プロピレングリコール、ブチレングリコール、ヘキシレングリコール、ネオペンチルグリコール、２―メチル―１，３―プロパンジオール、ジエチレングリコール、トリメチレングリコールの如き脂肪族ジオール、１，４―シクロヘキサンジメタノールの如き脂環族ジオール等およびそれらの混合物等を好ましくあげることができる。また、少量であればこれらのジオール化合物と共に両末端または片末端が未封鎖のポリオキシアルキレングリコールを共重合することができる。 Examples of diol compounds include ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, neopentyl glycol, aliphatic diols such as 2-methyl-1,3-propanediol, diethylene glycol and trimethylene glycol, and 1,4-cyclohexane. Preferable examples include alicyclic diols such as dimethanol and mixtures thereof. If the amount is small, polyoxyalkylene glycol having both ends or one end unblocked can be copolymerized with these diol compounds.
さらに、ポリエステルが実質的に線状である範囲でトリメリット酸、ピロメリット酸の如きポリカルボン酸、グリセリン、トリメチロールプロパン、ペンタエリスリトールの如きポリオールを使用することができる。 Furthermore, polycarboxylic acids such as trimellitic acid and pyromellitic acid, and polyols such as glycerin, trimethylolpropane, and pentaerythritol can be used within the range where the polyester is substantially linear.
具体的な好ましい芳香族ポリエステルとしてはポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリヘキシレンテレフタレート、ポリエチレンナフタレート、ポリブチレンナフタレート、ポリエチレン―１，２―ビス（フェノキシ）エタン―４，４′―ジカルボキシレート等のほか、ポリエチレンイソフタレート・テレフタレート、ポリブチレンテレフタレート・イソフタレート、ポリブチレンテレフタレート・デカンジカルボキシレート等のような共重合ポリエステルをあげることができる。なかでも機械的性質、成形性等のバランスのとれたポリエチレンテレフタレートおよびポリブチレンテレフタレートが特に好ましい。 Specific preferred aromatic polyesters include polyethylene terephthalate, polybutylene terephthalate, polyhexylene terephthalate, polyethylene naphthalate, polybutylene naphthalate, polyethylene-1,2-bis (phenoxy) ethane-4,4'-dicarboxylate. In addition, there may be mentioned copolyesters such as polyethylene isophthalate / terephthalate, polybutylene terephthalate / isophthalate, polybutylene terephthalate / decane dicarboxylate, and the like. Of these, polyethylene terephthalate and polybutylene terephthalate having a good balance of mechanical properties and moldability are particularly preferable.
かかる芳香族ポリエステルは任意の方法によって合成される。例えばポリエチレンテレフタレートついて説明すれば、テレフタル酸とエチレングリコールとを直接エステル化反応させるか、テレフタル酸ジメチルの如きテレフタル酸の低級アルキルエステルとエチレングリコールとをエステル交換反応させるかまたはテレフタル酸とエチレンオキサイドとを反応させるかして、テレフタル酸のグリコールエステルおよび／またはその低重合体を生成させる第１段反応、次いでその生成物を減圧下加熱して所望の重合度になるまで重縮合反応させる第２段の反応とによって容易に製造される。 Such aromatic polyester is synthesized by any method. For example, for polyethylene terephthalate, terephthalic acid and ethylene glycol are directly esterified, or a lower alkyl ester of terephthalic acid such as dimethyl terephthalate is transesterified with ethylene glycol, or terephthalic acid and ethylene oxide are reacted. In the first stage reaction to produce a glycol ester of terephthalic acid and / or a low polymer thereof, and then the product is heated under reduced pressure to undergo a polycondensation reaction until the desired degree of polymerization is reached. It is easily produced by a stage reaction.
次に、（ａ）ポリオキシアルキレン系ポリエーテルとしては、ポリエステルに実質的に不溶性のものであれば、単一のオキシアルキレン単位からなるポリオキシアルキレングリコールであっても、二種以上のオキシアルキレン単位からなる共重合ポリオキシアルキレングリコールであってもよい。かかるポリオキシアルキレン系ポリエーテルの具体例としては、分子量が４０００以上のポリオキシエチレングリコール、分子量が１０００以上のポリオキシプロピレングリコール、ポリオキシテトラメチレングリコール、分子量が２０００以上のエチレンオキサイド、プロピレンオキサイド共重合体、分子量４０００以上のトリメチロールプロパンエチレンオキサイド付加物、分子量３０００以上のノニルフェノールエチレンオキサイド付加物、並びにこれらの末端ＯＨ基に炭素数が６以上の置換エチレンオキサイドが付加した化合物があげられ、なかでも分子量が１００００〜１０００００のポリオキシエチレングコール、及び分子量が５０００〜１６０００の、ポリオキシエチレングリコールの両末端に炭素数が８〜４０のアルキル基置換エチレンオキサイドが付加した化合物が好ましい。 Next, (a) the polyoxyalkylene polyether may be a polyoxyalkylene glycol composed of a single oxyalkylene unit, as long as it is substantially insoluble in polyester, but two or more oxyalkylenes may be used. It may be a copolymerized polyoxyalkylene glycol composed of units. Specific examples of such polyoxyalkylene polyether include polyoxyethylene glycol having a molecular weight of 4000 or more, polyoxypropylene glycol having a molecular weight of 1000 or more, polyoxytetramethylene glycol, ethylene oxide having a molecular weight of 2000 or more, and a propylene oxide copolymer. Polymers, trimethylolpropane ethylene oxide adducts having a molecular weight of 4000 or more, nonylphenol ethylene oxide adducts having a molecular weight of 3000 or more, and compounds in which a substituted ethylene oxide having 6 or more carbon atoms is added to these terminal OH groups. However, polyoxyethylene glycol having a molecular weight of 10,000 to 100,000 and an alkyl group having 8 to 40 carbon atoms at both ends of the polyoxyethylene glycol having a molecular weight of 5000 to 16000. Compound conversion of ethylene oxide are added are preferred.
かかるポリオキシアルキレン系ポリエーテル化合物の配合量は、前記芳香族ポリエステル１００重量部に対して０．２〜３０重量部の範囲であることが好ましい。０．２重量部より少ないときは親水性が不足して充分な制電性を呈することができないおそれがある。一方３０重量部より多くしてももはや制電性の向上効果は認められず、かえって得られる組成物の機械的性質を損うようになる上、該ポリエーテルがブリードアウトし易くなるため溶融成形時チップのルーダーへのかみこみ性が低下して、成形安定性も悪化するようになるおそれがある。 The blending amount of the polyoxyalkylene polyether compound is preferably in the range of 0.2 to 30 parts by weight with respect to 100 parts by weight of the aromatic polyester. When the amount is less than 0.2 parts by weight, the hydrophilicity is insufficient and sufficient antistatic property may not be exhibited. On the other hand, if the amount is more than 30 parts by weight, the antistatic effect is no longer recognized. On the contrary, the mechanical properties of the resulting composition are impaired, and the polyether is easily bleeded out, so that it is melt molded. There is a possibility that the insertability of the chip into the ruder sometimes decreases and the molding stability also deteriorates.
次に、（ｂ）有機イオン性化合物としては、例えば下記一般式（Ｉ）、（ＩＩ）で示されるスルホン酸金属塩及びスルホン酸第４級ホスホニウム塩を好ましいものとしてあげることができる。 Next, as the (b) organic ionic compound, for example, sulfonic acid metal salts and sulfonic acid quaternary phosphonium salts represented by the following general formulas (I) and (II) can be mentioned as preferable ones.
ＲＳＯ３Ｍ （Ｉ）
式中、Ｒは炭素原子数３〜３０のアルキル基又は炭素原子数７〜４０のアリール基、Ｍはアルカリ金属又はアルカリ土類金属を示す。上記式（Ｉ）においてＲがアルキル基のときはアルキル基は直鎖状であっても又は分岐した側鎖を有していてもよい。ＭはＮａ、Ｋ、Ｌｉ等のアルカリ金属又はＭｇ、Ｃａ等のアルカリ土類金属であり、なかでもＬｉ、Ｎａ、Ｋが好ましい。かかるスルホン酸金属塩は１種のみを単独で用いても２種以上を混合して使用してもよい。好ましい具体例としてはステアリルスルホン酸ナトリウム、オクチルスルホン酸ナトリウム、ドデシルスルホン酸ナトリウム、炭素原子数の平均が１４であるアルキルスルホン酸ナトリウム混合物、ドデシルベンゼンスルホン酸ナトリウム混合物、ドデシルベンゼンスルホン酸ナトリウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸リチウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸マグネシウム（ハード型、ソフト型）等をあげることができる。
RSO 3 M (I)
In the formula, R represents an alkyl group having 3 to 30 carbon atoms or an aryl group having 7 to 40 carbon atoms, and M represents an alkali metal or an alkaline earth metal. In the above formula (I), when R is an alkyl group, the alkyl group may be linear or have a branched side chain. M is an alkali metal such as Na, K, or Li, or an alkaline earth metal such as Mg or Ca. Among these, Li, Na, and K are preferable. Such sulfonic acid metal salts may be used alone or in combination of two or more. Preferred examples include sodium stearyl sulfonate, sodium octyl sulfonate, sodium dodecyl sulfonate, a mixture of sodium alkyl sulfonate having an average of 14 carbon atoms, a mixture of sodium dodecyl benzene sulfonate, sodium dodecyl benzene sulfonate (hard type) Soft type), lithium dodecylbenzenesulfonate (hard type, soft type), magnesium dodecylbenzenesulfonate (hard type, soft type) and the like.
ＲＳＯ３ＰＲ１ Ｒ２ Ｒ３ Ｒ４ （ＩＩ）
式中、Ｒは上記式（Ｉ）におけるＲの定義と同じであり、Ｒ1 、Ｒ2 、Ｒ3 及びＲ4 はアルキル基又はアリール基でなかでも低級アルキル基、フェニル基又はベンジル基が好ましい。かかるスルホン酸第４級ホスホニウム塩は１種のみを単独で用いても２種以上を混合して使用してもよい。好ましい具体例としては炭素原子数の平均が１４であるアルキルスルホン酸テトラブチルホスホニウム、炭素原子数の平均が１４であるアルキルスルホン酸テトラフェニルホスホニウム、炭素原子数の平均が１４であるアルキルスルホン酸ブチルトリフェニルホスホニウム、ドデシルベンゼンスルホン酸テトラブチルホスホニウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸テトラフェニルホスホニウム（ハード型、ソフト型）、ドデシルベンゼンスルホン酸ベンジルトリフェニルホスホニウム（ハード型、ソフト型）等をあげることができる。
RSO 3 PR 1 R 2 R 3 R 4 (II)
In the formula, R is the same as the definition of R in the above formula (I), and R 1 , R 2 , R 3 and R 4 are preferably an alkyl group or an aryl group, particularly a lower alkyl group, a phenyl group or a benzyl group. . Such sulfonic acid quaternary phosphonium salts may be used alone or in combination of two or more. Preferred examples include tetrabutylphosphonium alkyl sulfonate having an average of 14 carbon atoms, tetraphenyl phosphonium alkyl sulfonate having an average of 14 carbon atoms, and butyl alkyl sulfonate having an average of 14 carbon atoms. Triphenylphosphonium, tetrabutylphosphonium dodecylbenzenesulfonate (hard type, soft type), tetraphenylphosphonium dodecylbenzenesulfonate (hard type, soft type), benzyltriphenylphosphonium dodecylbenzenesulfonate (hard type, soft type), etc. Can give.
かかる有機のイオン性化合物は１種でも、２種以上併用してもよく、その配合量は、芳香族ポリエステル１００重量部に対して０．０５〜１０重量部の範囲が好ましい。０．０５重量部未満では制電性向上の効果が小さく、１０重量部を越えると組成物の機械的性質を損なうようになる上、溶融成形時のチップのルーダーかみこみ性が低下して、成形安定性も悪化するようになる。 Such organic ionic compounds may be used alone or in combination of two or more thereof, and the blending amount thereof is preferably in the range of 0.05 to 10 parts by weight with respect to 100 parts by weight of the aromatic polyester. If the amount is less than 0.05 parts by weight, the effect of improving antistatic properties is small, and if it exceeds 10 parts by weight, the mechanical properties of the composition are impaired, and the ruder biteability of the chip during melt molding is reduced. Molding stability also deteriorates.
前記芯鞘型複合繊維の鞘成分を形成するポリマーとしては制電剤を含むポリマーであれば特に限定されないが、前記の芳香族ポリエステルに、前記のような制電剤が含まれるものが好ましい。その際、鞘成分を形成するポリエステルに含まれる制電剤の含有量は芯成分よりも小さいことが好ましい。特に、前記鞘部に含まれる制電剤が、芯部に含まれる制電剤が加熱処理などにより鞘部にブリードアウトしたものであると、製糸性を損わずに優れた制電性が得られ好ましい。特に、芯部に含まれる制電剤がブリードアウトし制電剤が繊維表面に露出していると特に優れた制電性が得られ好ましい。なお、前記芯鞘型複合繊維の芯成分および／または鞘成分には、本発明の目的を損なわない範囲内で必要に応じて着色防止剤、熱安定剤、難燃剤、蛍光増白剤、着色剤抗菌剤、マイナスイオン発生剤等を添加してもよい。 The polymer forming the sheath component of the core-sheath composite fiber is not particularly limited as long as it is a polymer containing an antistatic agent, but the aromatic polyester preferably contains the antistatic agent as described above. At that time, the content of the antistatic agent contained in the polyester forming the sheath component is preferably smaller than that of the core component. In particular, when the antistatic agent contained in the sheath portion is one in which the antistatic agent contained in the core portion is bleeded out to the sheath portion by heat treatment or the like, excellent antistaticity is obtained without impairing the yarn forming property. Obtained and preferred. In particular, when the antistatic agent contained in the core part bleeds out and the antistatic agent is exposed on the fiber surface, particularly excellent antistatic properties can be obtained. The core component and / or the sheath component of the core-sheath type composite fiber may be added with an anti-coloring agent, a heat stabilizer, a flame retardant, a fluorescent brightening agent, or a coloring agent within the range not impairing the object of the present invention. An antibacterial agent, a negative ion generator and the like may be added.
前記芯成分と鞘成分との面積比は（芯成分：鞘成分）１０：９０〜６５：３５の範囲にすることが好ましい。芯成分の面積比が１０：９０より小さい場合には加熱処理を施しても、制電剤が繊維表面に露出しないおそれがある。逆に、６５：３５よりも大きくなる場合は、１０％以上のアルカリ減量を施した場合に、部分的に芯成分の制電性ポリマーが溶出し、制電性能が低下するおそれがある。 The area ratio of the core component to the sheath component is preferably in the range of (core component: sheath component) 10:90 to 65:35. When the area ratio of the core component is smaller than 10:90, the antistatic agent may not be exposed on the fiber surface even if heat treatment is performed. On the other hand, when the ratio is larger than 65:35, the antistatic polymer as the core component partially elutes when the alkali weight loss is 10% or more, and the antistatic performance may be lowered.
本発明において、前記芯鞘型複合繊維の単糸繊度は１．５ｄｔｅｘ以下（好ましくは０．１〜１．２ｄｔｅｘ）であることが好ましい。該単糸繊度が１．５ｄｔｅｘ以下であると、後記のように加熱処理などを施した際に、芯成分に含まれる制電剤が鞘成分にブリードアウトし繊維表面に露出しやすく好ましい。 In this invention, it is preferable that the single yarn fineness of the said core-sheath-type composite fiber is 1.5 dtex or less (preferably 0.1-1.2 dtex). When the single yarn fineness is 1.5 dtex or less, it is preferable that the antistatic agent contained in the core component bleeds out to the sheath component and is exposed to the fiber surface when heat treatment is performed as described later.
また、単糸繊維の断面形状としては、丸断面形状で同心円状に芯鞘構造を有していることが好ましい。かかる芯鞘型複合繊維の総繊度、フィラメント数としては、風合いのソフトの点で総繊度３３〜１４０ｄｔｅｘ、フィラメント数５０〜１５０の範囲が好ましい。また、繊維形態としては、マルチフィラメント（長繊維）であることが好ましい。また、芯鞘型複合繊維には仮撚捲縮加工が施されていることが好ましい。仮撚捲縮加工が施されていない場合は、制電性布帛の風合いが硬くなるおそがある。 The cross-sectional shape of the single yarn fiber is preferably a round cross-sectional shape and a concentric core-sheath structure. The total fineness and the number of filaments of the core-sheath composite fiber are preferably in the range of a total fineness of 33 to 140 dtex and a filament number of 50 to 150 in terms of softness of the texture. Moreover, as a fiber form, it is preferable that it is a multifilament (long fiber). The core-sheath type composite fiber is preferably subjected to false twist crimping. When the false twist crimping process is not performed, the texture of the antistatic fabric may become hard.
前記芯鞘型複合繊維は、例えば下記の製造方法により製造することができる。すなわち、島成分用ポリマー（制電剤を含む制電性ポリマー、好ましくは前記のような制電剤を含むポリエステル）と海成分用ポリマー（制電剤を含むポリマーでもよいが、制電剤を含まないポリマー（例えばポリエステル）が好ましい。）とを用いて常法の芯鞘型複合繊維用口金を用いて芯鞘型未延伸糸を溶融紡糸した後、常法により延伸して延伸糸としてもよいし、紡出時の吐出速度と引き取り速度の比（引き取り速度／吐出速度、以降ドラフトと記す）を１００以上、８００未満の範囲で引き取った未延伸糸を仮撚加工してもよい。ここで、ドラフトが１００以下の場合は芯成分による制電性能の発現が不十分になり、ドラフトが８００以上の場合には制電性能は発現するものの、紡糸性が低下するおそれがある。従ってこの範囲で口金吐出孔径、紡糸速度を適宜設定すればよいが、吐出径をΦ０．１〜０．３ｍｍ、紡糸速度２０００〜４５００ｍ／ｍｉｎ、特に２５００〜３５００ｍ／ｍｉｎの範囲で溶融紡糸すると、容易にかつ効率よく得られるので好ましい。 The core-sheath type composite fiber can be produced, for example, by the following production method. That is, an island component polymer (an antistatic polymer containing an antistatic agent, preferably a polyester containing an antistatic agent as described above) and a sea component polymer (a polymer containing an antistatic agent may be used). A core-sheath-type unstretched yarn is melt-spun using a conventional core-sheath-type composite fiber die using a polymer containing no polymer (for example, polyester). Alternatively, the undrawn yarn taken in the range of 100 to less than 800 in the ratio between the discharge speed and the take-off speed at the time of spinning (take-off speed / discharge speed, hereinafter referred to as draft) may be false twisted. Here, when the draft is 100 or less, the antistatic performance due to the core component becomes insufficient. When the draft is 800 or more, the antistatic performance is exhibited, but the spinnability may be lowered. Accordingly, the nozzle discharge hole diameter and the spinning speed may be set as appropriate within this range. However, when melt spinning in the range of Φ0.1 to 0.3 mm, spinning speed 2000 to 4500 m / min, particularly 2500 to 3500 m / min, It is preferable because it can be obtained easily and efficiently.
該未延伸糸（未延伸マルチフィラメント）を仮撚加工する場合、その方法については特に限定されないが、例えば（１）仮撚具：３軸フリクションデイスクタイプ、（２）仮撚温度：１７０〜３００℃、（３）加工倍率：１．４〜２．４、（４）仮撚数：（１５０００〜３５０００）／（仮撚糸繊度（ｄｔｅｘ））１／２回／ｍ、より好ましくは（２００００〜３００００）／（仮撚糸繊度（ｄｔｅｘ））１／２回／ｍであることが好ましい。その際、空気交絡処理は延伸仮撚加工と別の工程で行ってもよいが、延伸仮撚加工装置にインターレースノズルを設置して延伸仮撚加工直前に施すのが好ましい。このことにより毛羽発生を抑制し取り扱い性に好影響をもたらすことができ、更に、熱セット仮撚後糸条に空気交絡を施すことで完璧に混繊交絡を均一化、糸長方向均一効果から、制電性を有し且つ高級感を発現させることができる。次に、交絡処理が施された未延伸糸は、例えば２段式ヒーターを備えた延伸仮撚加工機に掛けて、捲縮を有する仮撚加工糸とする。 When false twisting the unstretched yarn (unstretched multifilament), the method is not particularly limited. For example, (1) false twisting tool: triaxial friction disk type, (2) false twisting temperature: 170 to 300 (3) Processing magnification: 1.4 to 2.4, (4) Number of false twists: (15000 to 35000) / (false twist yarn fineness (dtex)) 1/2 times / m, more preferably (20,000 to 30000) / (false twist fineness (dtex)) It is preferable that it is 1/2 times / m. At that time, the air entanglement treatment may be performed in a step different from the drawing false twisting process, but it is preferable to perform the air entanglement processing immediately before the drawing false twisting by installing an interlace nozzle in the drawing false twisting apparatus. This suppresses the occurrence of fuzz and can have a positive effect on handling.Furthermore, by applying air entanglement to the yarn after heat setting false twisting, the mixed fiber entanglement is perfectly uniformed, and the uniform effect in the yarn length direction It has antistatic properties and can express a high-class feeling. Next, the undrawn yarn subjected to the entanglement treatment is subjected to, for example, a drawing false twisting machine equipped with a two-stage heater to obtain a false twisted yarn having crimps.
かくして得られた仮撚捲縮加工糸の捲縮率としては、３〜３０％の範囲内であることが好ましい。該捲縮率が３％より小さいと制電撥水織物の風合いが硬くなるおそれがある。逆に、該捲縮率が３０％よりも大きいと、制電性が低下するおそれがある。 The crimp rate of the false twist crimped yarn thus obtained is preferably in the range of 3 to 30%. If the crimp rate is less than 3%, the texture of the antistatic water-repellent fabric may be hard. Conversely, if the crimp rate is greater than 30%, the antistatic property may be reduced.
次いで、前記芯鞘型複合繊維（延伸糸または仮撚捲縮加工糸）を用いて常法により布帛を織編成する。ここで、布帛に含まれる芯鞘型複合繊維の重量割合は３０重量％以上であることが好ましい。布帛に他の繊維が含まれる場合、かかる他の繊維としては、通常のポリエステルからなるポリエステル繊維が好ましい。 Next, a fabric is woven and knitted by a conventional method using the core-sheath type composite fiber (drawn yarn or false twist crimped yarn). Here, the weight ratio of the core-sheath composite fiber contained in the fabric is preferably 30% by weight or more. When the fabric contains other fibers, the other fibers are preferably polyester fibers made of ordinary polyester.
また、布帛の組織は特に限定されず、通常の方法で製編織されたものでよい。例えば、織組織としては、平織、斜文織、朱子織等の三原組織、変化組織、変化斜文織等の変化組織、たて二重織、よこ二重織等の片二重組織、たてビロードなどが例示される。層数も単層でもよいし、２層以上の多層でもよい。編物の場合は、よこ編物であってもよいしたて編物であってもよい。よこ編組織としては、平編、ゴム編、両面編、パール編、タック編、浮き編、片畔編、レース編、添え毛編等が好ましく例示され、たて編組織としては、シングルデンビー編、シングルアトラス編、ダブルコード編、ハーフトリコット編、裏毛編、ジャガード編等が例示される。層数も単層でもよいし、２層以上の多層でもよい。また、製編織方法も通常の織編機（例えば、通常のウオータージェットルームやエアージェットルーム）を用いた通常の方法でよい。 Moreover, the structure | tissue of a fabric is not specifically limited, What was knitted and woven by the normal method may be used. For example, weaving structures include plain weave, oblique weaving, satin weaving, etc., changing structure, changing weaving, etc., changing double weaving, weft double weaving, etc. Examples are velvet. The number of layers may be a single layer or a multilayer of two or more layers. In the case of a knitted fabric, a weft knitted fabric or a newly knitted fabric may be used. Preferred examples of the weft knitting structure include flat knitting, rubber knitting, double-sided knitting, pearl knitting, tuck knitting, float knitting, one-sided knitting, lace knitting, bristle knitting, and the like. Single atlas knitting, double cord knitting, half tricot knitting, back hair knitting, jacquard knitting and the like are exemplified. The number of layers may be a single layer or a multilayer of two or more layers. The knitting and weaving method may be a normal method using a normal knitting and knitting machine (for example, a normal water jet loom or an air jet loom).
次いで、前記鞘成分に制電剤が含まれない場合には、前記の布帛に加熱処理を施すことにより、芯鞘型複合繊維の芯成分を形成する制電性ポリマーに含まれる制電剤を、鞘成分にブリードアウトさせ繊維表面に露出させる。 Next, when the sheath component does not contain an antistatic agent, the antistatic agent contained in the antistatic polymer that forms the core component of the core-sheath-type composite fiber is obtained by subjecting the fabric to a heat treatment. The sheath component is bleed out and exposed to the fiber surface.
ここで、前記加熱処理としては、カレンダー加工またはエンボス加工（特に好ましくはカレンダー加工による加圧加熱加工が好ましい）。その際、カレンダー加工の条件としては、温度１３０℃以上（より好ましくは１４０〜１９５℃）、線圧８０００〜２００００Ｎ／ｃｍの範囲内であることが好ましい。 Here, as the heat treatment, calendering or embossing (particularly preferably, pressure heating by calendering is preferred). At that time, the calendering conditions are preferably a temperature of 130 ° C. or higher (more preferably 140 to 195 ° C.) and a linear pressure of 8000 to 20000 N / cm.
かかる加熱処理により、芯鞘型複合繊維の芯成分を形成する制電性ポリマーに含まれる制電剤が繊維表面に露出する。なぜ加熱処理により制電剤が繊維表面に露出するのかはまだ明らかにされていないが、加熱処理の際の熱により分子運動が激しくなり、その結果、成分を形成する制電性ポリマーに含まれる制電剤が繊維表面に露出するのではないかと推定している。 By such heat treatment, the antistatic agent contained in the antistatic polymer that forms the core component of the core-sheath composite fiber is exposed on the fiber surface. The reason why the antistatic agent is exposed to the fiber surface by heat treatment is not yet clarified, but the heat during the heat treatment increases the molecular motion, resulting in the antistatic polymer forming the component. It is estimated that the antistatic agent is exposed on the fiber surface.
なお、制電剤が芯成分や鞘成分に含まれるかどうかは、例えば下記の方法により判定することができる。すなわち、前記芯鞘型複合繊維を、カチオン染料（ローダミンＢ、保土谷化学工業）５％ｏｗｆ、酢酸０．５ｇ／Ｌで、５０℃、４０分染色を行ない、その後、水洗、０．５ｇ／Ｌの酢酸溶液４０℃で１０分間洗浄を行い、再度水洗を行った後乾燥させ、芯鞘型複合繊維の横断面を、拡大光学写真撮影することにより判定することができる。また、制電剤が繊維表面に露出している場合は、染色されていることを測色装置により判定してもよい。その際、測色装置で測定してａ＊値が１０以上の場合、制電剤が繊維表面に露出していると判定するとよい。
また、制電剤が芯成分や鞘成分に含まれるかどうか分析機器により直接測定してもよい。
Whether the antistatic agent is contained in the core component or the sheath component can be determined by, for example, the following method. That is, the core-sheath type composite fiber was dyed with a cationic dye (Rhodamine B, Hodogaya Chemical Industries) 5% owf, acetic acid 0.5 g / L at 50 ° C. for 40 minutes, and then washed with water, 0.5 g / L The L-acetic acid solution was washed at 40 ° C. for 10 minutes, washed again with water and then dried, and the cross-section of the core-sheath composite fiber can be determined by taking an enlarged optical photograph. Further, when the antistatic agent is exposed on the fiber surface, it may be determined by a color measuring device that the antistatic agent is dyed. At that time, when the a * value is 10 or more as measured by a color measuring device, it may be determined that the antistatic agent is exposed on the fiber surface.
Moreover, you may measure directly with an analytical instrument whether an antistatic agent is contained in a core component or a sheath component.
また、前記加熱処理の前および／または後に、布帛に撥水加工を施すことは好ましいことである。ここで、撥水加工としては通常のものでよい。例えば、特許第３１３３２２７号公報や特公平４−５７８６号公報に記載された方法が好適である。すなわち、撥水剤として市販のふっ素系撥水剤（例えば、旭硝子（株）製、アサヒガードＬＳ−３１７）を使用し、必要に応じてメラミン樹脂、触媒を混合して撥水剤の濃度が３〜１５重量％程度の加工剤とし、ピックアップ率５０〜９０％程度で、該加工剤を用いて織物の表面を処理する方法である。加工剤で織物の表面を処理する方法としては、パッド法、スプレー法などが例示され、なかでも、加工剤を織物内部まで浸透させる上でパッド法が最も好ましい。なお、前記ピックアップ率とは、加工剤の織物（加工剤付与前）重量に対する重量割合（％）である。 In addition, it is preferable that the fabric is subjected to water repellent treatment before and / or after the heat treatment. Here, the water repellent finish may be a normal one. For example, the methods described in Japanese Patent No. 3133227 and Japanese Patent Publication No. 4-5786 are suitable. That is, a commercially available fluorine-based water repellent (for example, Asahi Guard LS-317, manufactured by Asahi Glass Co., Ltd.) is used as the water repellent, and the concentration of the water repellent is adjusted by mixing melamine resin and catalyst as necessary. In this method, the surface of the woven fabric is treated with the processing agent at a pickup rate of about 50 to 90% with a processing agent of about 3 to 15% by weight. Examples of the method for treating the surface of the woven fabric with the processing agent include a pad method and a spray method. Among them, the pad method is most preferable for allowing the processing agent to penetrate into the woven fabric. In addition, the said pick-up rate is the weight ratio (%) with respect to the textile fabric (before processing agent provision) weight of a processing agent.
また、前記加熱処理および／または撥水加工の、前および／または後において、常法のアルカリ減量加工、染色仕上げ加工、起毛加工、紫外線遮蔽あるいは抗菌剤、消臭剤、防虫剤、蓄光剤、再帰反射剤、マイナスイオン発生剤等の機能を付与する各種加工を付加適用してもよい。 In addition, before and / or after the heat treatment and / or water repellent treatment, conventional alkali weight loss processing, dyeing finishing processing, raising processing, ultraviolet shielding or antibacterial agent, deodorant, insect repellent, phosphorescent agent, Various processes that provide functions such as a retroreflective agent and a negative ion generator may be additionally applied.
かくして得られた制電性布帛に含まれる芯鞘型複合繊維において、芯成分だけでなく鞘成分にも制電剤が含まれるので優れた制電性を奏する。その際、布帛の摩擦耐電圧としては洗濯前で３０００Ｖ以下（特に好ましくは１０００Ｖ以下）であることが好ましい。また、布帛に含まれる芯鞘型複合繊維の単糸繊度が小さいので、布帛がソフトな風合いを呈する。特に、芯鞘型複合繊維が仮撚捲縮加工糸である場合には、布帛が特にソフトな風合いを呈する。 In the core-sheath type composite fiber contained in the antistatic fabric thus obtained, the antistatic agent is contained not only in the core component but also in the sheath component, so that excellent antistatic properties are exhibited. At that time, the friction withstand voltage of the fabric is preferably 3000 V or less (particularly preferably 1000 V or less) before washing. Moreover, since the single yarn fineness of the core-sheath type composite fiber contained in the fabric is small, the fabric exhibits a soft texture. In particular, when the core-sheath type composite fiber is a false twist crimped yarn, the fabric exhibits a particularly soft texture.
また、かかる制電性布帛において、下記式により算出されるカバーファクター（ＣＦ）が１４００以上（好ましくは１５００〜３０００）の織物であると、低通気性となりスポーツ衣料などとして好適に使用できるので好ましい。
ＣＦ＝（ＤＷｐ／１．１）１／２×ＭＷｐ＋（ＤＷｆ／１．１）１／２×ＭＷｆ
ただし、ＤＷｐは経糸総繊度（ｄｔｅｘ）、ＭＷｐは経糸織密度（本／２．５４ｃｍ）、ＤＷｆは緯糸総繊度（ｄｔｅｘ）、ＭＷｆは緯糸織密度（本／２．５４ｃｍ）である。
その際、布帛の通気度が１０ｃｃ／ｃｍ２・ｓｅｃ以下であることが好ましい。なお、布帛の通気度が１０ｃｃ／ｃｍ２・ｓｅｃ以下とするには、前記のように、織物のカバーファクター（ＣＦ）を大きくし、かつカレンダー加工を施すとよい。
Further, in such an antistatic fabric, a fabric having a cover factor (CF) calculated by the following formula of 1400 or more (preferably 1500 to 3000) is preferable because it has low air permeability and can be suitably used as sports clothing. .
CF = (DWp / 1.1) 1/2 × MWp + (DWf / 1.1) 1/2 × MWf
However, DWp is the total warp fineness (dtex), MWp is the warp weave density (main / 2.54 cm), DWf is the total weft fineness (dtex), and MWf is the weft weave density (main / 2.54 cm).
At that time, the air permeability of the fabric is preferably 10 cc / cm 2 · sec or less. In order to set the air permeability of the fabric to 10 cc / cm 2 · sec or less, it is preferable to increase the cover factor (CF) of the fabric and perform calendering as described above.
また、本発明の制電性布帛において、布帛の撥水性が４級以上であることが好ましい。なお、布帛の撥水性を４級以上とするには、前記のように布帛に撥水加工を施すとよい。
また、本発明の制電性布帛において、下記に定義する花粉脱落性が７０％以上であると、スポーツ衣料などとして好適に使用することができ好ましい。なお、花粉脱落性が７０％以上とするには、前記のようなカレンダー加工と撥水加工を施すとよい。
Further, in the antistatic fabric of the present invention, the water repellency of the fabric is preferably quaternary or higher. In addition, in order to make the water repellency of the fabric 4th or higher, the fabric may be subjected to water repellent treatment as described above.
In addition, in the antistatic fabric of the present invention, the pollen shedding as defined below is preferably 70% or more because it can be suitably used as sports clothing. In addition, in order to make pollen detachment property 70% or more, it is preferable to perform the calendar process and the water repellent process as described above.
＜花粉脱落性評価＞タテ１０ｃｍ、ヨコ１０ｃｍの大きさに裁断したシートを、同サイズの、表面が平らなステンレス製平板に貼り付けた後、試料をビニールボックス内に配置し、１ｇの擬似花粉（石松子）をエアブラシにて噴霧し均一に飛散させた。飛散５分後に擬似花粉が均一に付着した試料を取り出し、デジタルカメラ顕微鏡システム（商品名：ＮＹｐｉｘＳ２スーパーシステム、マイクロネット社製）で１００倍に拡大し画面上の擬似花粉付着数（ｎ数＝３）をカウントする。次いで、シートを貼り付けた該平板を上下逆さにした状態で、高さ５ｃｍより１５ｇのおもりを該平板に落下させ、デジタルカメラ顕微鏡システムで擬似花粉付着数を測定した場所と同一の場所での残存擬似花粉付着数（ｎ数＝３）をカウントする。そして、次式で花粉脱落性（％）を求める。
花粉脱落性（％）＝１００−（（残存擬似花粉付着数）／（擬似花粉付着数）×１００）
<Evaluation of pollen shedding> A sheet cut to a size of 10 cm in length and 10 cm in width is pasted on a stainless steel flat plate of the same size, and the sample is placed in a vinyl box. (Ishimatsuko) was sprayed with an airbrush and dispersed uniformly. After 5 minutes of scattering, a sample with pseudo pollen uniformly attached was taken out and magnified 100 times with a digital camera microscope system (trade name: NYpixS2 super system, manufactured by Micronet), and the number of pseudo pollen adhered on the screen (n number = 3) ). Next, in a state where the flat plate to which the sheet is attached is turned upside down, a weight of 15 g from 5 cm in height is dropped on the flat plate, and the same place where the number of pseudo pollen adhesion was measured with a digital camera microscope system. Count the number of remaining pseudo-pollens (n number = 3). And pollen fall-off property (%) is calculated | required by following Formula.
Pollen shedding (%) = 100 − ((number of remaining pseudo pollen deposits) / (number of pseudo pollen deposits) × 100)
次に、本発明の衣料は前記の制電性布帛を用いてなる衣料である。かかる衣料は前記の制電性布帛を用いているので優れた制電性を有しかつソフトな風合いを呈する。また、前記のカレンダー加工および撥水加工を施している場合は、優れた花粉脱落性を有するので、花粉脱落性衣料として使用することもできる。 Next, the garment of the present invention is a garment made of the above antistatic fabric. Such clothing uses the above-described antistatic fabric, and therefore has excellent antistatic properties and a soft texture. In addition, when the calendering and water-repellent finishing are performed, it has excellent pollen shedding and can be used as pollen shedding clothes.
次に本発明の実施例及び比較例を詳述するが、本発明はこれらによって限定されるものではない。なお、実施例中の各測定項目は下記の方法で測定した。 Next, although the Example and comparative example of this invention are explained in full detail, this invention is not limited by these. In addition, each measurement item in an Example was measured with the following method.
（１）固有粘度
オルソ−クロルフェノールに溶解し、ウベローデ粘度管を用い、３５℃で測定した。
(1) Intrinsic viscosity Dissolved in ortho-chlorophenol and measured at 35 ° C using an Ubbelohde viscosity tube.
（２）複屈折率
光学顕微鏡とコンペンセーターを用いて、繊維の表面に観察される偏光のリターデーションから求めた。
(2) Birefringence index It calculated | required from the retardation of the polarization observed on the surface of a fiber using an optical microscope and a compensator.
（３）捲縮率
仮撚加工糸サンプルに０．０４４ｃＮ／ｄｔｅｘの張力を掛けてカセ枠に巻き取り、約３３００ｄｔｅｘのカセを作成した。該カセの一端に、０．０１７７ｃＮ／ｄｔｅｘおよび０．１７７ｃＮ／ｄｔｅｘの２個の荷重を負荷し、１分間経過後の長さＳ０（ｃｍ）を測定した。次いで、０．１７７ｃＮ／ｄｔｅｘの荷重を除去した状態で、１００℃の沸水中にて２０分間処理した。沸水処理後０．０１７７ｃＮ／ｄｔｅｘの荷重を除去し、２４時間自由な状態で自然乾燥し、再び０．０１７７ｃＮ／ｄｔｅｘおよび０．１７７ｃＮ／ｄｔｅｘの荷重を負荷し、１分間経過後の長さを測定しＳ１（ｃｍ）とした。次いで、０．１７７ｃＮ／ｄｔｅｘの荷重を除去し、１分間経過後の長さを測定しＳ２とし、次の算式で捲縮率を算出し、１０回の測定値の平均値で表した。
捲縮率（％）＝［（Ｓ１−Ｓ２）／Ｓ０］×１００
(3) Crimp rate A false twisted yarn sample was wound on a cassette frame by applying a tension of 0.044 cN / dtex to produce a cassette of about 3300 dtex. Two loads of 0.0177 cN / dtex and 0.177 cN / dtex were applied to one end of the cassette, and the length S0 (cm) after 1 minute was measured. Subsequently, it was treated in boiling water at 100 ° C. for 20 minutes with the load of 0.177 cN / dtex removed. Remove the load of 0.0177 cN / dtex after boiling water treatment, let it dry naturally for 24 hours, load 0.0177 cN / dtex and 0.177 cN / dtex again, and adjust the length after 1 minute. Measurement was made S1 (cm). Next, the load of 0.177 cN / dtex was removed, the length after 1 minute was measured and set to S2, and the crimp rate was calculated by the following formula, and expressed as the average value of 10 measurements.
Crimp rate (%) = [(S1-S2) / S0] × 100
（４）仮撚加工糸の強度、伸度
ＪＩＳ Ｌ―１０１３―７５に準じて測定した。
(4) Strength and elongation of false twisted yarn Measured according to JIS L-1013-75.
（５）風合い
試験者３人が官能評価により下記の３段階に評価した。３級：ソフトでしなやかな感触がある。２級：ややソフト感が乏しいが反撥性は感じられる。１級：カサカサした触感あるいは硬い触感である。
(5) Texture Three testers evaluated the following three levels by sensory evaluation. Level 3: Soft and supple feel. Second grade: Slightly soft, but feels repellent. First grade: Rough touch or hard touch.
（６）摩擦帯電圧測定法
初期（洗濯前）と洗濯２０回後の試験片について、試験片を回転させながら摩擦布で摩擦し、発生した帯電圧を測定した。Ｌ１０９４帯電性試験方法Ｂ法（摩擦帯電圧測定法）に従った。
(6) Friction voltage measurement method About the test piece in the initial stage (before washing) and after 20 washings, the test piece was rubbed with a friction cloth while rotating, and the generated charged voltage was measured. L1094 electrification test method B method (friction voltage measurement method) was followed.
（７）通気度
ＪＩＳ Ｌ１０９６−８．２７．１Ａ法により測定した。
(7) Air permeability Measured according to JIS L1096-8.27.1A method.
（８）撥水性
ＪＩＳ Ｌ１０９２−６．２（スプレー法）により測定した。
(8) Water repellency: Measured according to JIS L1092-6.2 (spray method).
（９）芯成分と鞘成分について制電剤の有無を調べるテスト
試料を、カチオン染料（ローダミンＢ、保土谷化学工業）５％ｏｗｆ、酢酸０．５ｇ／Ｌで、５０℃、４０分染色を行なった。その後、水洗、０．５ｇ／Ｌの酢酸溶液４０℃で１０分間洗浄を行い、再度水洗を行った後、乾燥させた。次いで、試料に含まれる芯鞘型複合繊維について、横断面の拡大光学写真を撮影し制電剤の有無を判定した。
(9) Test for checking presence or absence of antistatic agent for core component and sheath component Sample was dyed with cationic dye (rhodamine B, Hodogaya Chemical Industry) 5% owf, acetic acid 0.5g / L at 50 ° C for 40 minutes. I did it. Thereafter, washing with water, washing with a 0.5 g / L acetic acid solution at 40 ° C. for 10 minutes, washing with water again, and drying were performed. Next, with respect to the core-sheath type composite fiber contained in the sample, an enlarged optical photograph of a cross section was taken to determine the presence or absence of the antistatic agent.
（１０）花粉脱落性評価
タテ１０ｃｍ、ヨコ１０ｃｍの大きさに裁断したシートを、同サイズの、表面が平らなステンレス製平板に貼り付けた後、試料をビニールボックス内に配置し、１ｇの擬似花粉（石松子）をエアブラシにて噴霧し均一に飛散させた。飛散５分後に擬似花粉が均一に付着した試料を取り出し、デジタルカメラ顕微鏡システム（商品名：ＮＹｐｉｘＳ２スーパーシステム、マイクロネット社製）で１００倍に拡大し画面上の擬似花粉付着数（ｎ数＝３）をカウントする。次いで、シートを貼り付けた該平板を上下逆さにした状態で、高さ５ｃｍより１５ｇのおもりを該平板に落下させ、デジタルカメラ顕微鏡システムで擬似花粉付着数を測定した場所と同一の場所での残存擬似花粉付着数（ｎ数＝３）をカウントする。そして、次式で花粉脱落性（％）を求める。
花粉脱落性（％）＝１００−（（残存擬似花粉付着数）／（擬似花粉付着数）×１００）
(10) Pollen shedding evaluation A sheet cut to a size of 10 cm in length and 10 cm in width is pasted on a stainless steel flat plate of the same size, and then the sample is placed in a vinyl box, and 1 g pseudo Pollen (Ishimatsuko) was sprayed with an air brush and dispersed uniformly. After 5 minutes of scattering, a sample with pseudo pollen uniformly attached was taken out and magnified 100 times with a digital camera microscope system (trade name: NYpixS2 super system, manufactured by Micronet), and the number of pseudo pollen adhered on the screen (n number = 3) ). Next, in a state where the flat plate to which the sheet is attached is turned upside down, a weight of 15 g from 5 cm in height is dropped on the flat plate, and the same place where the number of pseudo pollen adhesion was measured with a digital camera microscope system. Count the number of remaining pseudo-pollens (n number = 3). And pollen fall-off property (%) is calculated | required by following Formula.
Pollen shedding (%) = 100 − ((number of remaining pseudo pollen deposits) / (number of pseudo pollen deposits) × 100)
［実施例１］
テレフタル酸ジメチル１００部、エチレングリコール６０部、酢酸カルシウム１水塩０．０６部（テレフタル酸ジメチルに対して０．０６６モル％）および整色剤として酢酸コバルト４水塩０．０１３部（テレフタル酸ジメチルに対して０．０１モル％）をエステル交換反応缶に仕込み、この反応物を窒素ガス雰囲気下で４時間かけて１４０℃から２２０℃まで昇温し、反応缶中に生成するメタノールを系外に留去しながらエステル交換反応させた。エステル交換反応終了後、反応混合物に安定剤としてリン酸トリメチル０．０５８部（テレフタル酸ジメチルに対して０．０８０モル％）、および消泡剤としてジメチルポリシロキサンを０．０２４部加えた。次に、１０分後に、反応混合物に三酸化アンチモン０．０４１部（テレフタル酸ジメチルに対して０．０２７モル％）を添加し、同時に過剰のエチレングリコールを留去しながら２４０℃まで昇温し、その後、反応混合物を重合反応缶に移した。次いで１時間４０分かけて７６０ｍｍＨｇから１ｍｍＨｇまで減圧するとともに２４０℃から２８０℃まで昇温して重縮合反応せしめた後、下記化学式
100 parts of dimethyl terephthalate, 60 parts of ethylene glycol, 0.06 part of calcium acetate monohydrate (0.066 mol% with respect to dimethyl terephthalate) and 0.013 part of cobalt acetate tetrahydrate as a color adjuster (terephthalic acid) 0.01 mol% with respect to dimethyl) was charged into a transesterification reactor, and the reaction product was heated from 140 ° C. to 220 ° C. over 4 hours under a nitrogen gas atmosphere. The ester exchange reaction was carried out while distilling out. After completion of the transesterification reaction, 0.058 parts of trimethyl phosphate (0.080 mol% with respect to dimethyl terephthalate) as a stabilizer and 0.024 parts of dimethylpolysiloxane as an antifoaming agent were added to the reaction mixture. Next, after 10 minutes, 0.041 part of antimony trioxide (0.027 mol% with respect to dimethyl terephthalate) was added to the reaction mixture, and the temperature was raised to 240 ° C. while distilling off excess ethylene glycol. Thereafter, the reaction mixture was transferred to a polymerization reactor. Next, after reducing the pressure from 760 mmHg to 1 mmHg over 1 hour and 40 minutes and raising the temperature from 240 ° C. to 280 ° C. to cause the polycondensation reaction,
一方、常法により、制電剤を含有しないポリエチレンテレフタレートからなるポリマー（固有粘度０．６０、鞘成分用ポリマー）を得た。
次いで、乾燥ポリマーを紡糸設備にて各々常法で溶融し、スピンブロックを通して、スピンパックに導入した。該スピンパックに組み込まれた円形吐出孔を７２個穿設した紡糸口金（通常の芯鞘型繊維用紡糸口金）から、通常のクロスフロー型紡糸筒からの冷却風で冷却・固化し、紡糸油剤を付与しつつ一つの糸条として集束し、３０００ｍ／ｍｉｎの速度で引き取り、複屈折率０．０３５の１４０ｄｔｅｘ／７２フィラメントのポリエステル未延伸糸を得た。
On the other hand, a polymer made of polyethylene terephthalate containing no antistatic agent (inherent viscosity 0.60, polymer for sheath component) was obtained by a conventional method.
Next, the dried polymer was melted in a usual manner in a spinning facility and introduced into a spin pack through a spin block. A spinneret (ordinary core-sheath fiber spinneret) having 72 circular discharge holes incorporated in the spin pack is cooled and solidified with cooling air from a normal cross-flow type spinning cylinder, and a spinning oil agent As a single yarn, the yarn was bundled and taken up at a speed of 3000 m / min to obtain a 140 dtex / 72 filament polyester undrawn yarn having a birefringence of 0.035.
該ポリエステル未延伸糸を、帝人製機製２１６錘建ＨＴＳ−１５Ｖに掛け、前段、後段とで、孔径１．８ｍｍの圧空吹き出し孔を有するインターレースノズルを通過させつつ６０ｎＬ／ｍｉｎの流量で交絡度が５０個／ｍとなるように空気交絡を施し、延伸倍率１．６０、第１ヒーター（非接触タイプ）温度２５０℃の条件に設定し、直径６０ｍｍ、厚み９ｍｍのウレタンディスクを仮撚ディスクとして、走行角４３度で仮撚数×（仮撚糸繊度（ｄｔｅｘ））１／２が２６０００近傍となるように延伸仮撚を行い、速度８００ｍ／ｍｉｎでチーズ形状に巻き取り、８４ｄｔｅｘ／７２フィラメント（平均単糸繊度１．１７ｄｔｅｘ）の制電芯鞘型複合繊維からなる仮撚捲縮加工糸（捲縮率１５％、強度３．８ｃＮ／ｄｔｅｘ）を得た。 The polyester unstretched yarn is applied to Teijin Seiki's 216 Tajiken HTS-15V, and the entanglement degree is 60 nL / min at a flow rate of 60 nL / min while passing through an interlace nozzle having a 1.8 mm hole diameter in the front and rear stages. Air entanglement is performed so as to be 50 pieces / m, the draw ratio is 1.60, the first heater (non-contact type) temperature is set to 250 ° C., and a urethane disk having a diameter of 60 mm and a thickness of 9 mm is used as a false twist disk. Stretch false twist so that the number of false twists x (false twist fineness (dtex)) 1/2 is around 26000 at a running angle of 43 degrees, wound into a cheese shape at a speed of 800 m / min, and 84 dtex / 72 filaments (average A false twist crimped yarn (crimp rate 15%, strength 3.8 cN / dtex) made of an anti-core sheath-type composite fiber having a single yarn fineness of 1.17 dtex) was obtained.
一方、制電剤を含有しないポリエチレンテレフタレートからなるポリマー（固有粘度０．６０）単独で用いること以外は上記と同様にして、ポリエチレンテレフタレート仮撚捲縮加工糸８４ｄｔｅｘ／７２フィラメントを得た。
次いで、通常のウオータージェットルームを使用し、前記ポリエチレンテレフタレート仮撚捲縮加工糸８４ｄｔｅｘ／７２フィラメントを経糸に、一方、前記制電仮撚捲縮加工糸８４ｄｔｅｘ／７２フィラメント（芯鞘型複合繊維）を緯糸として平組織にて生機織物を得て、次いで常法の染色工程にて染色した後、下記の処理液（加工剤）をパッドし、ピックアップ率７０％で搾液し、１３０℃で３分間乾燥後１７０℃で４５秒間熱処理を行った後、ロール温度１６０℃、１１５２９Ｎ／ｃｍ（１１７６ｋｇｆ／ｃｍ）の条件でカレンダー加工を行い、制電性布帛（カバーファクター１９９２）を得た。
On the other hand, a polyethylene terephthalate false twisted yarn 84 dtex / 72 filament was obtained in the same manner as described above except that a polymer (inherent viscosity 0.60) made of polyethylene terephthalate containing no antistatic agent was used alone.
Next, using a normal water jet loom, the polyethylene terephthalate false twisted crimped yarn 84 dtex / 72 filament is used as a warp, while the antistatic false twisted crimped yarn 84 dtex / 72 filament (core-sheath type composite fiber) Is used as a weft to obtain a woven fabric in a plain structure and then dyed in a conventional dyeing process. Then, the following treatment liquid (processing agent) is padded and squeezed at a pick-up rate of 70%. After drying for 1 minute, heat treatment was performed at 170 ° C. for 45 seconds, and then calendering was performed under the conditions of a roll temperature of 160 ° C. and 11529 N / cm (1176 kgf / cm) to obtain an antistatic fabric (cover factor 1992).
＜加工剤組成＞
・ふっ素系撥水剤 １０．０ｗｔ％
（旭硝子（株）製、アサヒガードＬＳ−３１７）
・メラミン樹脂 ０．３ｗｔ％
（住友化学（株）製、スミテックスレジンＭ−３）
・触媒 ０．３ｗｔ％
（住友化学（株）製、スミテックスアクセレレータＡＣＸ）
・水 ８９．４ｗｔ％
<Processing agent composition>
・ Fluorine-based water repellent 10.0wt%
(Asahi Guard LS-317, manufactured by Asahi Glass Co., Ltd.)
・ Melamine resin 0.3wt%
(Sumitomo Chemical Co., Ltd., Sumtex Resin M-3)
・ Catalyst 0.3wt%
(Sumitomo Chemical Co., Ltd., Smithex Accelerator ACX)
・ Water 89.4wt%
他方、染料を使用せずに同様の加工工程を施した制電性布帛を製造し、（制電剤の有無を調べる染色テスト）をしたところ、芯成分に含まれる制電剤が鞘成分にブリードアウトし、鞘成分にも制電剤が含まれていることが確認できた。また、海島型複合繊維の単繊維表面へ制電剤が露出しており、測色装置でａ＊値を測定したところ、ａ＊値は１０以上であった。
得られた制電性布帛において、初期（洗濯前）の撥水性が５級と撥水性にも優れていた。また、初期（洗濯前）の摩擦帯電圧が経５４０Ｖ、緯７２０Ｖ、洗濯２０回後の摩擦帯電圧が経１２００Ｖ、緯１５００Ｖと大変優れた制電性を有しており、花粉脱落性は９２％と大変優れたものであった。また、ソフトな風合い（３級）を呈するものであった。
次いで、該前記制電性布帛を用いてスポーツ衣料（ウインドブレーカー）を得た。その際、カレンダー加工および撥水加工を施した面が外気側になるよう縫製した。かかるスポーツ衣料（ウインドブレーカー）を着用したところ、静電気が発生せず、ソフトな風合いを呈するものであった。
On the other hand, when the antistatic fabric which performed the same processing process without using dye and manufactured (the dyeing test which checks the presence or absence of an antistatic agent), the antistatic agent contained in a core component becomes a sheath component. It bleeded out, and it was confirmed that the sheath component contained an antistatic agent. Further, the antistatic agent was exposed on the surface of the single fiber of the sea-island composite fiber, and the a * value was 10 or more when the a * value was measured with a color measuring device.
In the obtained antistatic fabric, the water repellency at the initial stage (before washing) was excellent in the fifth grade and the water repellency. The initial (before washing) friction band voltage is 540V, 720V, and the friction band voltage after 20 washings is 1200V, 1500V. % Was very good. Moreover, the soft texture (3rd grade) was exhibited.
Next, a sports apparel (windbreaker) was obtained using the antistatic fabric. At that time, it was sewn so that the surface subjected to the calendering and water repellent treatment was on the outside air side. When such sports apparel (windbreaker) was worn, no static electricity was generated and a soft texture was exhibited.
［比較例１］
実施例１において用いた芯成分用ポリマーのみを用いて、該ポリマー単独からなる制電仮撚捲縮加工糸８４ｄｔｅｘ／７２フィラメントを得て、これ以外は実施例１と同様に実施した。
結果、製糸性が悪く安定生産不可なものであった。
[Comparative Example 1]
Using only the core component polymer used in Example 1, an antistatic false twist crimped yarn 84 dtex / 72 filament made of the polymer alone was obtained, and the other processes were performed in the same manner as in Example 1.
As a result, the yarn production was poor and stable production was impossible.
［比較例２］
実施例１において、制電仮撚捲縮加工糸の総繊度／フィラメントを１１０ｄｔｅｘ／１０フィラメント（単糸繊度１１デシテックス）に変更すること以外は実施例１と同様に実施した。
得られた制電性布帛において、初期の撥水性が５級と撥水性に優れていた。花粉脱落性は８４％と優れたものであったが、初期の摩擦帯電圧が経１１００Ｖ、緯１３００Ｖ、洗濯２０回後の摩擦帯電圧が経１９００Ｖ、緯３１００Ｖと制電性が十分ではなく、また風合いが硬いものであった。
他方、染料を使用せずに同様の加工工程を施した制電性布帛を製造し、（制電剤の有無を調べる染色テスト）をしたところ、芯鞘型複合繊維の単繊維表面への制電剤の露出が確認できなかった。なお、ａ＊値は１０未満であった。
[Comparative Example 2]
In Example 1, it implemented similarly to Example 1 except having changed the total fineness / filament of the antistatic false twist crimped yarn into 110 dtex / 10 filament (single yarn fineness 11 dtex).
In the obtained antistatic fabric, the initial water repellency was grade 5 and excellent in water repellency. Pollen detachment was excellent at 84%, but the initial frictional band voltage was 1100V, weft 1300V, the friction band voltage after 20 washings was 1900V, weft 3100V, and the antistatic property was not enough, The texture was hard.
On the other hand, when an antistatic fabric subjected to the same processing steps without using a dye and subjected to a (dyeing test for examining the presence or absence of an antistatic agent), a core-sheath composite fiber is controlled on the surface of a single fiber. The exposure of the electric agent could not be confirmed. The a * value was less than 10.
［比較例３］
実施例１において、カレンダー加工を施さなかったこと以外は実施例１と同様に実施した。
得られた制電性布帛において、初期の撥水性が５級と撥水性に優れていた。花粉脱落性は８６％と優れたものであったが、初期の摩擦帯電圧が経１５００Ｖ、緯１８００Ｖ、洗濯２０回後の摩擦帯電圧が経１６００Ｖ、緯２０００Ｖと制電性が十分ではなかった。
他方、染料を使用せずに同様の加工工程を施した制電性布帛を製造し、（制電剤の有無を調べる染色テスト）をしたところ、芯鞘型複合繊維の単繊維表面への制電剤の露出が確認できなかった。なお、ａ＊値は１０未満であった。
[Comparative Example 3]
In Example 1, it carried out like Example 1 except not having performed calendar processing.
In the obtained antistatic fabric, the initial water repellency was grade 5 and excellent in water repellency. Pollen detachment was excellent at 86%, but the initial frictional band voltage was 1500V and weft 1800V, and the friction band voltage after 20 washings was 1600V and weft 2000V, and the antistatic property was not sufficient. .
On the other hand, when an antistatic fabric subjected to the same processing steps without using a dye and subjected to a (dyeing test for examining the presence or absence of an antistatic agent), a core-sheath composite fiber is controlled on the surface of a single fiber. The exposure of the electric agent could not be confirmed. The a * value was less than 10.
本発明によれば、制電剤を含む制電性ポリマーにより芯成分が形成された芯鞘型複合繊維を含む制電性布帛であって、優れた制電性を有する制電性布帛、および該制電性布帛を用いてなる衣料が得られ、その工業的価値は極めて大である。 According to the present invention, an antistatic fabric comprising a core-sheath type composite fiber in which a core component is formed of an antistatic polymer containing an antistatic agent, and having an excellent antistatic property, and Apparel using the antistatic fabric is obtained, and its industrial value is extremely large.
Claims (8)
ただし、カバーファクター（ＣＦ）は下記式により算出される。However, the cover factor (CF) is calculated by the following formula.
ＣＦ＝（ＤＷｐ／１．１）CF = (DWp / 1.1) １／２1/2 ×ＭＷｐ＋（ＤＷｆ／１．１）× MWp + (DWf / 1.1) １／２1/2 ×ＭＷｆ× MWf
［ＤＷｐは経糸総繊度（ｄｔｅｘ）、ＭＷｐは経糸織密度（本／２．５４ｃｍ）、ＤＷｆは緯糸総繊度（ｄｔｅｘ）、ＭＷｆは緯糸織密度（本／２．５４ｃｍ）である。］ [DWp is the total warp fineness (dtex), MWp is the warp weave density (main / 2.54 cm), DWf is the total weft fineness (dtex), and MWf is the weft weave density (main / 2.54 cm). ]
タテ１０ｃｍ、ヨコ１０ｃｍの大きさに裁断したシートを、同サイズの、表面が平らなステンレス製平板に貼り付けた後、試料をビニールボックス内に配置し、１ｇの擬似花粉（石松子）をエアブラシにて噴霧し均一に飛散させた。飛散５分後に擬似花粉が均一に付着した試料を取り出し、デジタルカメラ顕微鏡システム（商品名：ＮＹｐｉｘＳ２スーパーシステム、マイクロネット社製）で１００倍に拡大し画面上の擬似花粉付着数（ｎ数＝３）をカウントする。次いで、シートを貼り付けた該平板を上下逆さにした状態で、高さ５ｃｍより１５ｇのおもりを該平板に落下させ、デジタルカメラ顕微鏡システムで擬似花粉付着数を測定した場所と同一の場所での残存擬似花粉付着数（ｎ数＝３）をカウントする。そして、次式で花粉脱落性（％）を求める。 A sheet cut to a size of 10 cm in length and 10 cm in width is affixed to a stainless steel flat plate of the same size, and the sample is placed in a vinyl box, and 1 g of pseudo pollen (Ishimatsuko) is airbrushed. And sprayed uniformly. After 5 minutes of scattering, a sample with pseudo pollen uniformly attached was taken out and magnified 100 times with a digital camera microscope system (trade name: NYpixS2 super system, manufactured by Micronet), and the number of pseudo pollen adhered on the screen (n number = 3) ). Next, in a state where the flat plate to which the sheet is attached is turned upside down, a weight of 15 g from 5 cm in height is dropped on the flat plate, and the same place where the number of pseudo pollen adhesion was measured with a digital camera microscope system. Count the number of remaining pseudo-pollens (n number = 3). And pollen fall-off property (%) is calculated | required by following Formula.
花粉脱落性（％）＝１００−（（残存擬似花粉付着数）／（擬似花粉付着数）×１００）Pollen shedding (%) = 100 − ((number of remaining pseudo pollen deposits) / (number of pseudo pollen deposits) × 100)
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