JP2022147094A - Flame-retardant fabric and fiber product - Google Patents
Flame-retardant fabric and fiber product Download PDFInfo
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- JP2022147094A JP2022147094A JP2021048204A JP2021048204A JP2022147094A JP 2022147094 A JP2022147094 A JP 2022147094A JP 2021048204 A JP2021048204 A JP 2021048204A JP 2021048204 A JP2021048204 A JP 2021048204A JP 2022147094 A JP2022147094 A JP 2022147094A
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- retardant fabric
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- aromatic polyamide
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- 239000000835 fiber Substances 0.000 title claims abstract description 115
- 239000004744 fabric Substances 0.000 title claims abstract description 65
- 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 title claims abstract description 35
- 239000003063 flame retardant Substances 0.000 title claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000004760 aramid Substances 0.000 claims abstract description 53
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 11
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 7
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 3
- 239000005871 repellent Substances 0.000 claims description 32
- 230000002940 repellent Effects 0.000 claims description 29
- 239000004753 textile Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000013557 residual solvent Substances 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 3
- 239000001023 inorganic pigment Substances 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- 239000012860 organic pigment Substances 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 12
- 238000009987 spinning Methods 0.000 description 11
- -1 urethane compound Chemical class 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 10
- 150000001408 amides Chemical class 0.000 description 9
- 229920000742 Cotton Polymers 0.000 description 8
- 229920000728 polyester Polymers 0.000 description 8
- 230000015271 coagulation Effects 0.000 description 7
- 238000005345 coagulation Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- YCGKJPVUGMBDDS-UHFFFAOYSA-N 3-(6-azabicyclo[3.1.1]hepta-1(7),2,4-triene-6-carbonyl)benzamide Chemical compound NC(=O)C1=CC=CC(C(=O)N2C=3C=C2C=CC=3)=C1 YCGKJPVUGMBDDS-UHFFFAOYSA-N 0.000 description 4
- 238000012695 Interfacial polymerization Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000009941 weaving Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002964 rayon Substances 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
- 239000004693 Polybenzimidazole Substances 0.000 description 2
- 239000004697 Polyetherimide Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 150000004984 aromatic diamines Chemical class 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 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 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001230 polyarylate Polymers 0.000 description 2
- 229920002480 polybenzimidazole Polymers 0.000 description 2
- 229920002577 polybenzoxazole Polymers 0.000 description 2
- 229920002530 polyetherether ketone Polymers 0.000 description 2
- 229920001601 polyetherimide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- YDYSEBSNAKCEQU-UHFFFAOYSA-N 2,3-diamino-n-phenylbenzamide Chemical compound NC1=CC=CC(C(=O)NC=2C=CC=CC=2)=C1N YDYSEBSNAKCEQU-UHFFFAOYSA-N 0.000 description 1
- GOJFAKBEASOYNM-UHFFFAOYSA-N 2-(2-aminophenoxy)aniline Chemical compound NC1=CC=CC=C1OC1=CC=CC=C1N GOJFAKBEASOYNM-UHFFFAOYSA-N 0.000 description 1
- MYEWQUYMRFSJHT-UHFFFAOYSA-N 2-(2-aminophenyl)sulfonylaniline Chemical compound NC1=CC=CC=C1S(=O)(=O)C1=CC=CC=C1N MYEWQUYMRFSJHT-UHFFFAOYSA-N 0.000 description 1
- LNTGGPJSADTYSG-UHFFFAOYSA-N 2-(2-carbonochloridoylphenoxy)benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1OC1=CC=CC=C1C(Cl)=O LNTGGPJSADTYSG-UHFFFAOYSA-N 0.000 description 1
- WEEOFHJAGVFCFD-UHFFFAOYSA-N 2-n-chlorobenzene-1,2-diamine Chemical compound NC1=CC=CC=C1NCl WEEOFHJAGVFCFD-UHFFFAOYSA-N 0.000 description 1
- RPKCLSMBVQLWIN-UHFFFAOYSA-N 2-n-methylbenzene-1,2-diamine Chemical compound CNC1=CC=CC=C1N RPKCLSMBVQLWIN-UHFFFAOYSA-N 0.000 description 1
- 125000003504 2-oxazolinyl group Chemical group O1C(=NCC1)* 0.000 description 1
- QDBOAKPEXMMQFO-UHFFFAOYSA-N 4-(4-carbonochloridoylphenyl)benzoyl chloride Chemical compound C1=CC(C(=O)Cl)=CC=C1C1=CC=C(C(Cl)=O)C=C1 QDBOAKPEXMMQFO-UHFFFAOYSA-N 0.000 description 1
- LHSXSRQUGCHBPG-UHFFFAOYSA-N 4-(aminomethoxy)aniline Chemical compound NCOC1=CC=C(N)C=C1 LHSXSRQUGCHBPG-UHFFFAOYSA-N 0.000 description 1
- IWRVPXDHSLTIOC-UHFFFAOYSA-N 4-phenyldiazenylbenzene-1,3-diamine Chemical compound NC1=CC(N)=CC=C1N=NC1=CC=CC=C1 IWRVPXDHSLTIOC-UHFFFAOYSA-N 0.000 description 1
- HPFMWXQXAHHFAA-UHFFFAOYSA-N 5-chlorobenzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC(Cl)=CC(C(Cl)=O)=C1 HPFMWXQXAHHFAA-UHFFFAOYSA-N 0.000 description 1
- CGXXBHCRXCEKCP-UHFFFAOYSA-N 5-methoxybenzene-1,3-dicarbonyl chloride Chemical compound COC1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 CGXXBHCRXCEKCP-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920002845 Poly(methacrylic acid) Chemical class 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 1
- QSRFYFHZPSGRQX-UHFFFAOYSA-N benzyl(tributyl)azanium Chemical compound CCCC[N+](CCCC)(CCCC)CC1=CC=CC=C1 QSRFYFHZPSGRQX-UHFFFAOYSA-N 0.000 description 1
- TVXZUNWYERZMIX-UHFFFAOYSA-N benzyl(tributyl)azanium dodecyl benzenesulfonate Chemical compound C(CCCCCCCCCCC)OS(=O)(=O)C1=CC=CC=C1.C(CCC)[N+](CC1=CC=CC=C1)(CCCC)CCCC TVXZUNWYERZMIX-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-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
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- ASTWQNQEEBYIKI-UHFFFAOYSA-N hexyl benzenesulfonate tetrabutylphosphanium Chemical compound C(CCCCC)OS(=O)(=O)C1=CC=CC=C1.C(CCC)[P+](CCCC)(CCCC)CCCC ASTWQNQEEBYIKI-UHFFFAOYSA-N 0.000 description 1
- 125000005647 linker group Chemical group 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229920006277 melamine fiber Polymers 0.000 description 1
- MPXAYYWSDIKNTP-UHFFFAOYSA-N n-(2-aminophenyl)acetamide Chemical compound CC(=O)NC1=CC=CC=C1N MPXAYYWSDIKNTP-UHFFFAOYSA-N 0.000 description 1
- VIUHYPPHBQZSPF-UHFFFAOYSA-N naphthalene-1,4-dicarbonyl chloride Chemical compound C1=CC=C2C(C(=O)Cl)=CC=C(C(Cl)=O)C2=C1 VIUHYPPHBQZSPF-UHFFFAOYSA-N 0.000 description 1
- NZZGQZMNFCTNAM-UHFFFAOYSA-N naphthalene-2,6-dicarbonyl chloride Chemical compound C1=C(C(Cl)=O)C=CC2=CC(C(=O)Cl)=CC=C21 NZZGQZMNFCTNAM-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006306 polyurethane fiber Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000009999 singeing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Abstract
Description
本発明は、メタ型全芳香族ポリアミド繊維を含み、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れた難燃性布帛および繊維製品に関する。 TECHNICAL FIELD The present invention relates to flame-retardant fabrics and textile products that contain meta-type wholly aromatic polyamide fibers, have extremely excellent flame retardancy, are environmentally friendly, and have excellent water repellency and tear strength.
従来、防護服、消防防火服、消防活動服、救助服、難燃ワークウェア、警察制服、自衛隊衣服、軍服などの用途で、難燃性を有する布帛が用いられている。
一方、近年では、難燃性だけでなく、環境に配慮した撥水性および引裂き強力にも優れた難燃性布帛が求められている。撥水性を有する布帛としては、これまで各種提案されているが、難燃性、環境に配慮した撥水性および引裂き強力の点でまだ満足とは言えなかった（例えば、特許文献１～３）。
Conventionally, flame-retardant fabrics have been used in applications such as protective clothing, fire fighting clothing, fire fighting clothing, rescue clothing, flame-retardant workwear, police uniforms, Self-Defense Forces clothing, and military uniforms.
On the other hand, in recent years, there has been a demand for a flame-retardant fabric that is not only flame-retardant but also environmentally friendly and has excellent water repellency and tear strength. Various water-repellent fabrics have been proposed so far, but they have not been satisfactory in terms of flame retardancy, environmentally friendly water repellency and tear strength (eg, Patent Documents 1 to 3).
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、メタ型全芳香族ポリアミド繊維を含み、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れた難燃性布帛および繊維製品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 of the present invention is to include a meta-type wholly aromatic polyamide fiber, have extremely excellent flame retardancy, and is environmentally friendly and has excellent water repellency and tear strength. Another object of the present invention is to provide flame-retardant fabrics and textile products.
本発明者は上記の課題を達成するため鋭意検討した結果、本発明を完成するに至った。
かくして、本発明によれば「メタ型全芳香族ポリアミド繊維を含む布帛であって、炭化水素系化合物、シリコーン系化合物、ウレタン系化合物、アクリル系化合物、およびワックスからなる群から選択されるいずれかを含む撥水剤を含み、かつＩＳＯ１５０２５：２０００Ａ法で規定される燃焼試験で残炎時間が２秒以下であることを特徴とする難燃性布帛。」が提供される。
The present inventor has completed the present invention as a result of intensive studies to solve the above problems.
Thus, according to the present invention, "a fabric containing a meta-type wholly aromatic polyamide fiber, which is selected from the group consisting of a hydrocarbon compound, a silicone compound, a urethane compound, an acrylic compound, and a wax and having an afterflame time of 2 seconds or less in a combustion test specified by ISO 15025:2000A method.” is provided.
その際、布帛にアルキルフルオロポリマーが含まれないことが好ましい。また、布帛にブロックイソシアネートが含まれることが好ましい。また、メタ型全芳香族ポリアミド繊維が布帛質量対比５０質量％以上含まれることが好ましい。また、前記メタ型全芳香族ポリアミド繊維において、残存溶媒量が０．１質量％以下であることが好ましい。また、前記メタ型全芳香族ポリアミド繊維において、結晶化度が１５～５０％の範囲内であることが好ましい。 At that time, it is preferable that the fabric does not contain an alkylfluoropolymer. It is also preferred that the fabric contains a blocked isocyanate. Moreover, it is preferable that the meta-type wholly aromatic polyamide fiber is contained in an amount of 50% by mass or more relative to the mass of the fabric. Moreover, in the meta-type wholly aromatic polyamide fiber, the amount of residual solvent is preferably 0.1% by mass or less. Further, the meta-type wholly aromatic polyamide fiber preferably has a degree of crystallinity in the range of 15 to 50%.
本発明の難燃性布帛において、ＪＩＳ Ｌ １０９２ スプレー法により測定した撥水度が４級以上であることが好ましい。また、布帛の目付けが１２０～３００ｇ／ｍ２ の範囲内であることが好ましい。また、ＪＩＳ Ｌ０２１７法に規定された洗濯（但し、ＪＡＦＥＴ標準配合洗剤を使用）を１０回行った後において、ＪＩＳ Ｌ １０９２ スプレー法により測定した撥水度が３級以上であることが好ましい。また、引裂き強力が１０Ｎ以上であることが好ましい。また、ＩＳＯ５０７７に規定される方法で５回洗濯した後の収縮率が５％以下であることが好ましい。また、ＩＳＯ１７４９３に規定される１８０℃５分間の熱処理を行った際の熱収縮率が５％以下であることが好ましい。また、前記メタ型全芳香族ポリアミド繊維が、有機染料、有機顔料または無機顔料を含むことが好ましい。 The flame-retardant fabric of the present invention preferably has a water repellency of grade 4 or higher as measured by the JIS L 1092 spray method. Moreover, it is preferable that the basis weight of the fabric is within the range of 120 to 300 g/m 2 . In addition, it is preferable that the water repellency measured by the JIS L 1092 spray method is grade 3 or higher after washing 10 times as specified in the JIS L0217 method (using a JAFET standard compound detergent). Moreover, it is preferable that the tear strength is 10 N or more. Moreover, it is preferable that the shrinkage rate after washing five times by the method specified in ISO5077 is 5% or less. In addition, it is preferable that the heat shrinkage rate is 5% or less when subjected to heat treatment at 180° C. for 5 minutes as defined in ISO17493. Moreover, it is preferable that the meta-type wholly aromatic polyamide fiber contains an organic dye, an organic pigment, or an inorganic pigment.
また、本発明によれば、前記の難燃性布帛を用いてなり、防護服、消防防火服、消防活動服、救助服、ワークウェア、警察制服、自衛隊衣服、および軍服からなる群より選択されるいずれかの繊維製品が提供される。 Further, according to the present invention, the flame-retardant fabric is used, and is selected from the group consisting of protective clothing, fire protection clothing, fire fighting clothing, rescue clothing, workwear, police uniforms, self-defense force clothing, and military clothing. Any textile product is provided.
本発明によれば、メタ型全芳香族ポリアミド繊維を含み、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れた難燃性布帛および繊維製品が得られる。 According to the present invention, flame-retardant fabrics and textiles containing meta-type wholly aromatic polyamide fibers, having extremely excellent flame retardancy, and being environmentally friendly and excellent in water repellency and tear strength can be 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、本発明で用いるメタ型全芳香族ポリアミド繊維（メタ型アラミド繊維）とは、その繰返し単位の８５モル％以上がｍ－フェニレンイソフタルアミドであるポリマーからなる繊維である。かかるメタ型全芳香族ポリアミドは、１５モル％未満の範囲内で第３成分を含んだ共重合体であっても差しつかえない。 BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail. First, the meta-type wholly aromatic polyamide fiber (meta-aramid fiber) used in the present invention is a fiber made of a polymer in which 85 mol % or more of the repeating units are m-phenylene isophthalamide. Such a meta-type wholly aromatic polyamide may be a copolymer containing a third component within the range of less than 15 mol %.
このようなメタ型全芳香族ポリアミドは、従来から公知の界面重合法により製造することができ、そのポリマーの重合度としては、０．５ｇ／１００ｍｌの濃度のＮ－メチル－２－ピロリドン溶液で測定した固有粘度（Ｉ．Ｖ．）が１．３～１．９ｄｌ／ｇの範囲のものが好ましく用いられる。 Such a meta-type wholly aromatic polyamide can be produced by a conventionally known interfacial polymerization method. Those having a measured intrinsic viscosity (I.V.) in the range of 1.3 to 1.9 dl/g are preferably used.
上記メタ型全芳香族ポリアミドにはアルキルベンゼンスルホン酸オニウム塩が含有されていてもよい。アルキルベンゼンスルホン酸オニウム塩としては、ヘキシルベンゼンスルホン酸テトラブチルフォスフォニウム塩、ヘキシルベンゼンスルホン酸トリブチルベンジルフォスフォニウム塩、ドデシルベンゼンスルホン酸テトラフェニルフォスフォニウム塩、ドデシルベンゼンスルホン酸トリブチルテトラデシルフォスフォニウム塩、ドデシルベンゼンスルホン酸テトラブチルフォスフォニウム塩、ドデシルベンゼンスルホン酸トリブチルベンジルアンモニウム塩等の化合物が好ましく例示される。なかでもドデシルベンゼンスルホン酸テトラブチルフォスフォニウム塩、またはドデシルベンゼンスルホン酸トリブチルベンジルアンモニウム塩は、入手しやすく、熱的安定性も良好なうえ、Ｎ－メチル－２－ピロリドンに対する溶解度も高いため特に好ましく例示される。 The meta-type wholly aromatic polyamide may contain an onium alkylbenzenesulfonate. Examples of alkylbenzenesulfonic acid onium salts include tetrabutyl phosphonium hexylbenzene sulfonate, tributylbenzyl phosphonium hexyl benzene sulfonate, tetraphenyl phosphonium dodecyl benzene sulfonate, tributyl tetradecyl phosphate dodecylbenzene sulfonate. Compounds such as nium salts, tetrabutylphosphonium dodecylbenzenesulfonate, tributylbenzylammonium dodecylbenzenesulfonate and the like are preferably exemplified. Among them, dodecylbenzenesulfonate tetrabutylphosphonium salt or dodecylbenzenesulfonate tributylbenzylammonium salt is particularly useful because it is readily available, has good thermal stability, and has high solubility in N-methyl-2-pyrrolidone. It is preferably exemplified.
上記アルキルベンゼンスルホン酸オニウム塩の含有割合は、十分な染色性の改良効果を得るために、ポリ－ｍ－フェニレンイソフタルアミドに対して２．５モル％以上、好ましくは３．０～７．０モル％の範囲にあるものが好ましい。 The content of the alkylbenzenesulfonic acid onium salt is 2.5 mol% or more, preferably 3.0 to 7.0 mol, relative to poly-m-phenyleneisophthalamide, in order to obtain a sufficient effect of improving dyeability. % range is preferred.
また、ポリ－ｍ－フェニレンイソフタルアミドとアルキルベンゼンスルホン酸オニウム塩を混合する方法としては、溶媒中にポリ－ｍ－フェニレンイソフタルアミドを混合、溶解し、それにアルキルベンゼンスルホン酸オニウム塩を溶媒に溶解する方法などが用いられそのいずれを用いてもよい。このようにして得られたドープは、従来から公知の方法により繊維に形成される。 As a method of mixing poly-m-phenylene isophthalamide and onium alkylbenzenesulfonate, poly-m-phenylene isophthalamide is mixed and dissolved in a solvent, and then onium alkylbenzenesulfonate is dissolved in the solvent. etc., and any of them may be used. The dope thus obtained is formed into fibers by conventionally known methods.
メタ型全芳香族ポリアミド繊維に用いるポリマーは、染着性や耐変褪色性を向上させる等目的で、下記の式（１）で示される反復構造単位を含む芳香族ポリアミド骨格中に、反復構造の主たる構成単位とは異なる芳香族ジアミン成分、または芳香族ジカルボン酸ハライド成分を、第３成分として芳香族ポリアミドの反復構造単位の全量に対し１～１０ｍｏｌ％となるように共重合させることも可能である。
－（ＮＨ－Ａｒ１－ＮＨ－ＣＯ－Ａｒ１－ＣＯ）－ ・・・式（１）
ここで、Ａｒ１はメタ配位または平行軸方向以外に結合基を有する２価の芳香族基である。
The polymer used for the meta-type wholly aromatic polyamide fiber has a repeating structure in the aromatic polyamide skeleton containing the repeating structural unit represented by the following formula (1) for the purpose of improving dyeability and discoloration resistance. It is also possible to copolymerize an aromatic diamine component or an aromatic dicarboxylic acid halide component different from the main structural unit of as a third component in an amount of 1 to 10 mol% with respect to the total amount of repeating structural units of the aromatic polyamide. is.
-(NH-Ar1-NH-CO-Ar1-CO)- Formula (1)
Here, Ar1 is a divalent aromatic group having a bonding group other than meta-coordination or parallel axis direction.
また、第３成分として共重合させることも可能であり、式（２）、（３）に示した芳香族ジアミンの具体例としては、例えば、ｐ－フェニレンジアミン、クロロフェニレンジアミン、メチルフェニレンジアミン、アセチルフェニレンジアミン、アミノアニシジン、ベンジジン、ビス（アミノフェニル）エーテル、ビス（アミノフェニル）スルホン、ジアミノベンズアニリド、ジアミノアゾベンゼン等が挙げられる。式（４）、（５）に示すような芳香族ジカルボン酸ジクロライドの具体例としては、例えば、テレフタル酸クロライド、１，４－ナフタレンジカルボン酸クロライド、２，６－ナフタレンジカルボン酸クロライド、４，４’－ビフェニルジカルボン酸クロライド、５－クロルイソフタル酸クロライド、５－メトキシイソフタル酸クロライド、ビス（クロロカルボニルフェニル）エーテルなどが挙げられる。 It is also possible to copolymerize as a third component. Specific examples of the aromatic diamines represented by formulas (2) and (3) include p-phenylenediamine, chlorophenylenediamine, methylphenylenediamine, Acetylphenylenediamine, aminoanisidine, benzidine, bis(aminophenyl)ether, bis(aminophenyl)sulfone, diaminobenzanilide, diaminoazobenzene and the like. Specific examples of aromatic dicarboxylic acid dichlorides represented by formulas (4) and (5) include terephthalic acid chloride, 1,4-naphthalenedicarboxylic acid chloride, 2,6-naphthalenedicarboxylic acid chloride, 4,4 '-biphenyldicarboxylic acid chloride, 5-chloroisophthalic acid chloride, 5-methoxyisophthalic acid chloride, bis(chlorocarbonylphenyl)ether and the like.
Ｈ２Ｎ－Ａｒ２－ＮＨ２ ・・・式（２）
Ｈ２Ｎ－Ａｒ２－Ｙ－Ａｒ２－ＮＨ２ ・・・式（３）
ＸＯＣ－Ａｒ３－ＣＯＸ ・・・式（４）
ＸＯＣ－Ａｒ３－Ｙ－Ａｒ３－ＣＯＸ ・・・式（５）
H 2 N—Ar2—NH 2 Formula (2)
H 2 N-Ar2-Y-Ar2-NH 2 Formula (3)
XOC-Ar3-COX Formula (4)
XOC-Ar3-Y-Ar3-COX Formula (5)
ここで、Ａｒ２はＡｒ１とは異なる２価の芳香族基、Ａｒ３はＡｒ１とは異なる２価の芳香族基、Ｙは酸素原子、硫黄原子、アルキレン基からなる群から選ばれる少なくとも１種の原子又は官能基であり、Ｘはハロゲン原子を表す。 Here, Ar2 is a divalent aromatic group different from Ar1, Ar3 is a divalent aromatic group different from Ar1, Y is at least one atom selected from the group consisting of an oxygen atom, a sulfur atom and an alkylene group. or a functional group, and X represents a halogen atom.
また、メタ型全芳香族ポリアミド繊維の結晶化度は、染料の吸尽性がよく、より少ない染料でまたは染色条件が弱くても狙いの色に調整し易いという点で、１５～５０％であることが好ましい。さらには、染料の表面偏在が起こり難く耐変褪色性も高い点および実用上必要な寸法安定性も確保できる点で１５～２５％であることがより好ましい。 In addition, the degree of crystallinity of the meta-type wholly aromatic polyamide fiber is 15 to 50% in terms of good dye exhaustion and easy adjustment to the desired color even with less dye or under weak dyeing conditions. Preferably. Furthermore, it is more preferably 15 to 25% from the viewpoint that uneven distribution of the dye on the surface is unlikely to occur, the resistance to discoloration and fading is high, and the practically necessary dimensional stability can be ensured.
また、メタ型全芳香族ポリアミド繊維の残存溶媒量は、メタ型全芳香族ポリアミド繊維の優れた難燃性能を損なわない点で、０．１質量％以下（好ましくは０．００１～０．１質量％）であることが好ましい。 In addition, the residual solvent amount of the meta-type wholly aromatic polyamide fiber is 0.1% by mass or less (preferably 0.001 to 0.1 % by mass).
前記メタ型全芳香族ポリアミド繊維は以下の方法により製造することができ、特に後述する方法により、結晶化度や残存溶媒量を上記範囲とすることができる。
メタ型全芳香族ポリアミドポリマーの重合方法としては、特に限定する必要はなく、例えば特公昭３５－１４３９９号公報、米国特許第３３６０５９５号公報、特公昭４７－１０８６３号公報などに記載された溶液重合法、界面重合法を用いてもよい。
The meta-type wholly aromatic polyamide fiber can be produced by the following method, and the degree of crystallinity and residual solvent amount can be controlled within the above ranges by the method described later.
The method for polymerizing the meta-type wholly aromatic polyamide polymer is not particularly limited. A legal, interfacial polymerization method may be used.
紡糸溶液としては、とくに限定する必要はないが、上記溶液重合や界面重合などで得られた、芳香族コポリアミドポリマーを含むアミド系溶媒溶液を用いても良いし、上記重合溶液から該ポリマーを単離し、これをアミド系溶媒に溶解したものを用いても良い。 The spinning solution is not particularly limited, but may be an amide solvent solution containing the aromatic copolyamide polymer obtained by the above solution polymerization or interfacial polymerization, or the polymer may be extracted from the above polymerization solution. It may also be used after it has been isolated and dissolved in an amide solvent.
ここで用いられるアミド系溶媒としては、Ｎ，Ｎ－ジメチルホルムアミド、Ｎ，Ｎ－ジメチルアセトアミド、Ｎ－メチル－２－ピロリドン、ジメチルスルホキシドなどを例示することができるが、とくにＮ，Ｎ－ジメチルアセトアミドが好ましい。 Examples of the amide-based solvent used here include N,N-dimethylformamide, N,N-dimethylacetamide, N-methyl-2-pyrrolidone, dimethylsulfoxide and the like, and particularly N,N-dimethylacetamide. is preferred.
上記の通り得られた共重合芳香族ポリアミドポリマー溶液は、さらにアルカリ金属塩又はアルカリ土類金属塩を含むことにより安定化され、より高濃度、低温での使用が可能となり好ましい。好ましくはアルカリ金属塩及びアルカリ土類金属塩がポリマー溶液の全重
量に対して１質量％以下、より好ましくは０．１質量％以下である。
紡糸・凝固工程においては、上記で得られた紡糸液（メタ型全芳香族ポリアミド重合体溶液）を凝固液中に紡出して凝固させる。
The copolymerized aromatic polyamide polymer solution obtained as described above is preferably stabilized by further containing an alkali metal salt or an alkaline earth metal salt, and can be used at a higher concentration and at a lower temperature. Preferably, the alkali metal salt and alkaline earth metal salt is 1% by weight or less, more preferably 0.1% by weight or less, relative to the total weight of the polymer solution.
In the spinning/coagulating step, the spinning solution (meta-type wholly aromatic polyamide polymer solution) obtained above is spun into the coagulating solution and coagulated.
紡糸装置としては特に限定されるものではなく、従来公知の湿式紡糸装置を使用することができる。また、安定して湿式紡糸できるものであれば、紡糸口金の紡糸孔数、配列状態、孔形状等は特に制限する必要はなく、例えば、孔数が１０００～３００００個、紡糸孔径が０．０５～０．２ｍｍのスフ用の多ホール紡糸口金等を用いてもよい。
また、紡糸口金から紡出する際の紡糸液（メタ型全芳香族ポリアミド重合体溶液）の温度は、２０～９０℃の範囲が適当である。
The spinning device is not particularly limited, and a conventionally known wet spinning device can be used. In addition, the number of spinning holes, the arrangement state, the shape of the holes, etc. of the spinneret do not have to be particularly limited as long as they can be stably wet-spun. A multi-hole spinneret or the like for staple fibers of up to 0.2 mm may be used.
The temperature of the spinning solution (meta-type wholly aromatic polyamide polymer solution) during spinning from the spinneret is suitably in the range of 20 to 90°C.
繊維を得るために用いる凝固浴としては、実質的に無機塩を含まない、アミド系溶媒、好ましくはＮＭＰの濃度が４５～６０質量％の水溶液を、浴液の温度１０～５０℃の範囲で用いる。アミド系溶媒（好ましくはＮＭＰ）の濃度が４５質量％未満ではスキンが厚い構造となってしまい、洗浄工程における洗浄効率が低下し、繊維の残存溶媒量を低減させることが困難となる。一方、アミド系溶媒（好ましくはＮＭＰ）の濃度が６０質量％を超える場合には、繊維内部に至るまで均一な凝固を行うことができず、このためやはり、繊維の残存溶媒量を低減させることが困難となる。なお、凝固浴中への繊維の浸漬時間は、０．１～３０秒の範囲が適当である。 As the coagulation bath used to obtain the fiber, an amide solvent substantially free of inorganic salts, preferably an aqueous solution of NMP with a concentration of 45 to 60% by mass, is used at a bath liquid temperature of 10 to 50 ° C. use. If the concentration of the amide-based solvent (preferably NMP) is less than 45% by mass, the skin will have a thick structure, the washing efficiency in the washing process will decrease, and it will be difficult to reduce the amount of residual solvent in the fibers. On the other hand, when the concentration of the amide-based solvent (preferably NMP) exceeds 60% by mass, uniform coagulation cannot be performed up to the inside of the fiber, and for this reason, it is also necessary to reduce the amount of residual solvent in the fiber. becomes difficult. It should be noted that the immersion time of the fiber in the coagulation bath is suitably in the range of 0.1 to 30 seconds.
引続き、アミド系溶媒、好ましくはＮＭＰの濃度が４５～６０質量％の水溶液であり、浴液の温度を１０～５０℃の範囲とした可塑延伸浴中にて、３～４倍の延伸倍率で延伸を行う。延伸後、１０～３０℃のＮＭＰの濃度が２０～４０質量％の水溶液、続いて５０～７０℃の温水浴を通して十分に洗浄を行う。
洗浄後の繊維は、温度２７０～２９０℃にて乾熱処理を施し、上記の結晶化度および残存溶媒量の範囲を満たすメタ型全芳香族ポリアミド繊維を得ることができる。
Subsequently, the film is stretched at a draw ratio of 3 to 4 times in a plastic drawing bath, which is an amide-based solvent, preferably an aqueous solution having a NMP concentration of 45 to 60% by mass, and the temperature of the bath liquid is in the range of 10 to 50°C. Draw. After stretching, the film is thoroughly washed with an aqueous solution of 20 to 40% by mass of NMP at 10 to 30°C, followed by a hot water bath at 50 to 70°C.
The washed fibers are subjected to a dry heat treatment at a temperature of 270 to 290° C. to obtain meta-type wholly aromatic polyamide fibers satisfying the above ranges of crystallinity and residual solvent amount.
前記メタ型全芳香族ポリアミド繊維において、繊維は、長繊維（マルチフィラメント）でもよいし短繊維でもよい。特に、他の繊維と混紡する上で繊維長２５～２００ｍｍの短繊維が好ましい。また、単繊維繊度としては１～５ｄｔｅｘの範囲が好ましい。なお、前記メタ型全芳香族ポリアミド繊維が、有機染料または有機顔料または無機顔料を含んでいてもよい。 In the meta-type wholly aromatic polyamide fiber, the fiber may be a long fiber (multifilament) or a short fiber. In particular, short fibers with a fiber length of 25 to 200 mm are preferred for blending with other fibers. Further, the single fiber fineness is preferably in the range of 1 to 5 dtex. The meta-type wholly aromatic polyamide fiber may contain an organic dye, an organic pigment, or an inorganic pigment.
本発明において、布帛は前記メタ型全芳香族ポリアミド繊維だけで構成されていてもよいが、さらにポリエステル繊維が含まれていることが好ましい。布帛にポリエステル繊維が含まれていると、後記のようなオキサゾリン基を有する架橋剤や、アクリル系樹脂および／またはウレタン系樹脂からなるバインダーのＳＰ値（溶解パラメータ）がポリエステル繊維に近くポリエステル繊維に固着しやすいので、抗菌性の洗濯耐久性を向上させることができ好ましい。その際、布帛に含まれるポリエステル繊維の質量としては布帛質量対比２～２０質量％の範囲内であることが好ましい。ポリエステル繊維の重量が該範囲よりも大きいと難燃性が低下するおそれがある。逆にポリエステル繊維の重量が該範囲よりも小さいと抗菌性の洗濯耐久性が低下するおそれがある。 In the present invention, the fabric may be composed only of the meta-type wholly aromatic polyamide fiber, but preferably further contains polyester fiber. When polyester fibers are included in the fabric, the SP value (solubility parameter) of the crosslinking agent having an oxazoline group as described later and the binder made of acrylic resin and / or urethane resin is close to that of polyester fiber. Since it easily adheres, it is preferable because it can improve the washing durability of the antibacterial property. At that time, the weight of the polyester fiber contained in the fabric is preferably in the range of 2 to 20% by weight based on the weight of the fabric. If the weight of the polyester fiber exceeds this range, the flame retardancy may be lowered. Conversely, if the weight of the polyester fiber is less than this range, the antibacterial durability to washing may deteriorate.
また、布帛にさらに、メタ型全芳香族ポリアミド繊維、パラ型全芳香族ポリアミド繊維、全芳香族ポリエステル繊維、ポリベンズオキサゾール（ＰＢＯ）繊維、ポリベンズイミダゾール（ＰＢＩ）繊維、ポリベンズチアゾール（ＰＢＴＺ）繊維、ポリイミド（ＰＩ）繊維、ポリスルホンアミド（ＰＳＡ）繊維、ポリエーテルエーテルケトン（ＰＥＥＫ）繊維、ポリエーテルイミド（ＰＥＩ）繊維、ポリアリレート（ＰＡｒ）繊維、メラミン繊維、フェノール繊維、フッ素系繊維、ポリフェニレンスルフィド（ＰＰＳ）繊維などの難燃繊維が含まれていることが好ましい。
その際、かかる難燃性繊維において限界酸素指数（ＬＯＩ）が２０以上であることが好ましい。
In addition, the fabric further includes meta-type wholly aromatic polyamide fiber, para-type wholly aromatic polyamide fiber, wholly aromatic polyester fiber, polybenzoxazole (PBO) fiber, polybenzimidazole (PBI) fiber, and polybenzthiazole (PBTZ). Fiber, polyimide (PI) fiber, polysulfonamide (PSA) fiber, polyetheretherketone (PEEK) fiber, polyetherimide (PEI) fiber, polyarylate (PAr) fiber, melamine fiber, phenol fiber, fluorine fiber, polyphenylene Preferably, flame retardant fibers such as sulfide (PPS) fibers are included.
In this case, the limiting oxygen index (LOI) of such flame-retardant fibers is preferably 20 or more.
また、布帛にさらに、セルロース繊維（好ましくは難燃レーヨン繊維）、ポリオレフィン繊維、アクリル繊維、コットン繊維、獣毛繊維、ポリウレタン繊維、ポリ塩化ビニル繊維、ポリ塩化ビニリデン繊維、アセテート繊維、ポリカーボネート繊維などが含まれていると、吸水性、染色性、着用快適性などが付加され好ましい。 Further, the fabric may further include cellulose fiber (preferably flame-retardant rayon fiber), polyolefin fiber, acrylic fiber, cotton fiber, animal hair fiber, polyurethane fiber, polyvinyl chloride fiber, polyvinylidene chloride fiber, acetate fiber, polycarbonate fiber, and the like. If it is contained, water absorption, dyeability, wearing comfort and the like are added, which is preferable.
また、導電繊維は、規格ＩＳＯ１１６１２にて必須であることが記載されており、難燃素材として、布帛での静電気を防ぐことは必要であることより、導電繊維が布帛に含まれていることが好ましい。 In addition, it is stated that the conductive fiber is essential in the standard ISO11612, and it is necessary to prevent static electricity in the fabric as a flame-retardant material. preferable.
ここで、これらの繊維は混紡されていることが好ましい。その際、メタ型全芳香族ポリアミド繊維の優れた耐熱性と難燃性を発揮させるために、まずメタ型全芳香族ポリアミド繊維が布帛質量対比５０質量％以上であることが好ましい。 Here, these fibers are preferably blended. At that time, in order to exhibit the excellent heat resistance and flame retardancy of the meta-type wholly aromatic polyamide fiber, it is preferable that the meta-type wholly aromatic polyamide fiber accounts for 50% by mass or more of the mass of the fabric.
本発明において、布帛の製造方法は特に限定するものではなく、公知のいかなる方法でも用いる可能である。例えば、上記繊維の紡績糸を混綿して紡績糸を得た後、単糸または双糸にてレピア織機などを用いて、綾織、平織などの組織に製織することが好ましい。 In the present invention, the fabric manufacturing method is not particularly limited, and any known method can be used. For example, it is preferable to obtain a spun yarn by blending the spun yarn of the above fibers, and then weave the yarn into a structure such as twill weave or plain weave using a rapier loom or the like with a single yarn or two-ply yarn.
本発明の難燃性布帛は、非フッ素系撥水剤として、炭化水素系化合物、シリコーン系化合物、ウレタン系化合物、アクリル系化合物、およびワックスからなる群から選択されるいずれかを含む撥水剤を含む。環境配慮の点で、また優れた引裂き強力を得る上で、アルキルフルオロポリマーなどのフッ素系撥水剤は含まないことが好ましい。必要に応じて、架橋剤（例えば、ブロックイソシアネートなど）、制電剤、メラミン樹脂、触媒を混合して撥水剤の濃度が３～１５質量％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ことが好ましい。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る。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好ましい。前記ピックアップ率とは、織物（加工剤付与前）重量に対する加工剤の質量割合（％）である。 The flame-retardant fabric of the present invention contains, as a non-fluorine-based water repellent agent, one selected from the group consisting of hydrocarbon compounds, silicone compounds, urethane compounds, acrylic compounds, and waxes. including. From the point of view of environmental friendliness and from the standpoint of obtaining excellent tear strength, it is preferred not to contain fluorine-based water repellents such as alkylfluoropolymers. If necessary, a cross-linking agent (for example, blocked isocyanate, etc.), an antistatic agent, a melamine resin, and a catalyst are mixed to form a processing agent having a water repellent concentration of about 3 to 15% by mass, and a pick-up rate of 50 to 90%. It is preferable to treat the surface of the textile using the finishing agent. A pad method, a spray method, etc. are illustrated as a method of treating the surface of a textile with a processing agent. Among them, the pad method is preferable in order to allow the processing agent to permeate into the interior of the woven fabric. The pickup rate is the mass ratio (%) of the finishing agent to the weight of the fabric (before application of the finishing agent).
非フッ素系撥水剤として具体的には、炭化水素系化合物として、脂肪族系炭化水素、脂肪族カルボン酸、オレフィン、ポリアクリル酸エステルまたはポリメタクリル酸エステルなどを用いることができる。シリコーン系化合物として、アミノ変性シリコーン、エポキシ変性シリコーン、カルボキシ変性シリコーンなどを用いることができる。市販されているものでは、炭化水素系化合物は、明成化学工業（株）製のメイシールドＰ－７００や日華化学（株）製のＮｅｏｓｅｅｄＮＲ－１５８、ＮＲ－７０８０、ダイキン（株）製のＵｎｉｄｙｎｅＸＦ５００１、ＸＦ５００２などが好ましく例示される。シリコーン系化合物は、日華化学（株）製のＮｅｏｓｅｅｄＮＲ－８０００、ＮＲ－８８００などが好ましく例示される。 Specific examples of the non-fluorine water repellent include hydrocarbon compounds such as aliphatic hydrocarbons, aliphatic carboxylic acids, olefins, polyacrylic acid esters, polymethacrylic acid esters, and the like. Amino-modified silicone, epoxy-modified silicone, carboxy-modified silicone and the like can be used as the silicone-based compound. Among commercially available hydrocarbon compounds, Mayshield P-700 manufactured by Meisei Chemical Industry Co., Ltd., Neoseed NR-158 and NR-7080 manufactured by Nicca Chemical Co., Ltd., and Unidyne XF5001 manufactured by Daikin Co., Ltd. , XF5002 and the like are preferably exemplified. Preferred examples of silicone compounds include Neoseed NR-8000 and NR-8800 manufactured by Nicca Chemical Co., Ltd.
本発明の難燃性布帛は、メタ型全芳香族ポリアミド繊維を含み、かつ前記のような非フッ素系撥水剤を含むので、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れる。 The flame-retardant fabric of the present invention contains the meta-type wholly aromatic polyamide fiber and the non-fluorine-based water repellent agent as described above, so it has extremely excellent flame retardancy and is environmentally friendly and water repellent. and excellent tear strength.
ここで、ＩＳＯ１５０２５：２０００Ａ法で規定される燃焼試験で残炎時間が２秒以下であることが重要である。残ジンは２．０秒以下が好ましい。また、ＪＩＳ Ｌ １０９２ スプレー法により測定した撥水度が４級以上であることが好ましい。また、布帛の目付けが１２０～３００ｇ／ｍ２ の範囲内であることが好ましい。また、ＪＩＳ Ｌ０２１７法に規定された洗濯（但し、ＪＡＦＥＴ標準配合洗剤を使用）を１０回行った後において、ＪＩＳ Ｌ １０９２ スプレー法により測定した撥水度が３級以上であることが好ましい。 Here, it is important that the afterflame time is 2 seconds or less in the combustion test specified by the ISO15025:2000A method. The residual gin is preferably 2.0 seconds or less. Moreover, it is preferable that the water repellency measured by the JIS L 1092 spray method is grade 4 or higher. Moreover, it is preferable that the basis weight of the fabric is within the range of 120 to 300 g/m 2 . In addition, it is preferable that the water repellency measured by the JIS L 1092 spray method is grade 3 or higher after 10 washes specified by the JIS L0217 method (using a JAFET standard compound detergent).
また、経方向または緯方向の引裂き強力が１０Ｎ以上（より好ましくは４５～９０Ｎ）であることが好ましい。また、引裂き強力が撥水剤除去後に下がることが好ましい。特に（撥水剤付与後布帛／撥水剤付与前）が１．１以上（より好ましくは１．１～１．５）であることが好ましい。なお、引裂き強力はＪＩＳ Ｌ１０９６Ｄ法に規定される方法で測定するものとする。また、測定方法は、例えば、撥水剤付与前の布帛を測定した後、撥水剤を付与し、撥水剤付与後の布帛を測定してもよいし、撥水剤付与後の布帛の引裂強力を測定したのち、布帛から撥水剤を除去して、撥水剤付与前とした布帛の引裂強力を測定してもよい。 Also, the tear strength in the warp or weft direction is preferably 10 N or more (more preferably 45 to 90 N). Moreover, it is preferable that the tear strength is lowered after the water repellent agent is removed. In particular, it is preferable that the ratio (fabric after application of water repellent agent/before application of water repellent agent) is 1.1 or more (more preferably 1.1 to 1.5). The tear strength shall be measured by the method specified in JIS L1096D method. Further, the measurement method may be, for example, measuring the fabric before applying the water repellent agent, applying the water repellent agent, and measuring the fabric after applying the water repellent agent, or measuring the fabric after applying the water repellent agent. After measuring the tear strength, the water repellent agent may be removed from the fabric, and the tear strength of the fabric before applying the water repellent agent may be measured.
また、ＩＳＯ５０７７に規定される方法で５回洗濯した後の収縮率（経と緯の平均）が５％以下であることが好ましい。また、ＩＳＯ１７４９３に規定される１８０℃５分間の熱処理を行った際の熱収縮率（経と緯の平均）が５％以下であることが好ましい。 Further, it is preferable that the shrinkage rate (average of warp and weft) after washing five times by the method specified in ISO5077 is 5% or less. In addition, it is preferable that the heat shrinkage (average of warp and weft) when heat-treated at 180° C. for 5 minutes specified in ISO 17493 is 5% or less.
次に、本発明の繊維製品は前記の布帛を用いてなる、防護服、消防防火服、消防活動服、救助服、ワークウェア、警察制服、自衛隊衣服、および軍服からなる群より選択されるいずれかの繊維製品である。かかる繊維製品は前記の布帛を用いているので、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れる。 Next, the textile product of the present invention is any one selected from the group consisting of protective clothing, fire protection clothing, firefighting clothing, rescue clothing, workwear, police uniforms, self-defense force clothing, and military clothing using the above fabric. It is a textile product. Since such a textile product uses the fabric described above, it has extremely excellent flame retardancy, is environmentally friendly, and is excellent in water repellency and tear strength.
以下、実施例をあげて本発明を詳細に説明するが、本発明はこれらによって何ら限定されるものではない。なお、実施例中の各物性は下記の方法により測定したものである。 EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited by these examples. In addition, each physical property in an Example is measured by the following method.
（１）目付け
ＪＩＳ Ｌ １０９６ Ａ法で規定される方法で測定した。
(1) Fabric weight Measured by the method specified in JIS L 1096 A method.
（２）燃焼性
ＩＳＯ１５０２５：２０００ Ａ法で規定される方法で測定した。
(2) Flammability Measured by the method specified in ISO15025:2000 A method.
（３）撥水性
ＪＩＳ Ｌ １０９２ スプレー法により撥水度（級）を測定した。
(3) Water repellency The water repellency (class) was measured by the JIS L 1092 spray method.
（４）乾熱収縮率
ＩＳＯ１７４９３に規定される１８０℃５分間の熱処理を行った際の熱収縮率を測定した。ｎ数５で経と緯について測定し両者の平均をとった。
(4) Dry Heat Shrinkage The thermal shrinkage was measured after heat treatment at 180° C. for 5 minutes as specified in ISO17493. The warp and latitude were measured with n number of 5, and the average of both was taken.
（５）残存溶媒量
原繊維を約８．０ｇ採取し、１０５℃で１２０分間乾燥させた後にデシケーター内で放冷し、繊維質量（Ｍ１）を秤量した。続いて、この繊維について、メタノール中で１．５時間、ソックスレー抽出器を用いて還流抽出を行い、繊維中に含まれるアミド系溶媒の抽出を行った。抽出を終えた繊維を取り出して、１５０℃で６０分間真空乾燥させた後にデシケーター内で放冷し、繊維質量（Ｍ２）を秤量した。繊維中に残存する溶媒量（アミド系溶媒質量）は、得られるＭ１およびＭ２を用いて、下記式により算出した。
残存溶媒量（％）＝［（Ｍ１－Ｍ２）／Ｍ１］×１００
(5) Amount of Residual Solvent Approximately 8.0 g of fibril was sampled, dried at 105° C. for 120 minutes, allowed to cool in a desiccator, and the fiber mass (M1) was weighed. Subsequently, this fiber was subjected to reflux extraction using a Soxhlet extractor in methanol for 1.5 hours to extract the amide solvent contained in the fiber. After the extraction, the fibers were taken out, vacuum-dried at 150° C. for 60 minutes, allowed to cool in a desiccator, and the fiber mass (M2) was weighed. The amount of solvent remaining in the fiber (amide solvent mass) was calculated by the following formula using the obtained M1 and M2.
Residual solvent amount (%) = [(M1-M2) / M1] × 100
（６）結晶化度
Ｘ線回折測定装置（リガク社製 ＲＩＮＴ ＴＴＲIII）を用い、原繊維を約１ｍｍ径
の繊維束に引きそろえて繊維試料台に装着して回折プロファイルを測定した。測定条件は
、Ｃｕ－Ｋα線源（５０ｋＶ、３００ｍＡ）、走査角度範囲１０～３５°、連続測定０．１°幅計測、１°／分走査でおこなった。実測した回折プロファイルから空気散乱、非干渉性散乱を直線近似で補正して全散乱プロファイルを得た。次に、全散乱プロファイルから非晶質散乱プロファイルを差し引いて結晶散乱プロファイルを得た。結晶化度は、結晶散乱プロファイルの面積強度（結晶散乱強度）と全散乱プロファイルの面積強度（全散乱強度）から、次式により求めた。
結晶化度（％）＝［結晶散乱強度／全散乱強度］×１００
(6) Crystallinity Using an X-ray diffractometer (RINT TTR III manufactured by Rigaku), the fibrils were aligned into a fiber bundle with a diameter of about 1 mm, mounted on a fiber sample stage, and the diffraction profile was measured. The measurement conditions were Cu-Kα radiation source (50 kV, 300 mA), scanning angle range 10 to 35°, continuous measurement 0.1° width measurement, and scanning 1°/min. A total scattering profile was obtained by correcting air scattering and incoherent scattering from the measured diffraction profile by linear approximation. The crystalline scattering profile was then obtained by subtracting the amorphous scattering profile from the total scattering profile. The degree of crystallinity was obtained from the area intensity of the crystal scattering profile (crystal scattering intensity) and the area intensity of the total scattering profile (total scattering intensity) by the following formula.
Crystallinity (%) = [crystal scattering intensity/total scattering intensity] × 100
（７）布帛の引裂き強力
ＪＩＳ Ｌ１０９６Ｄ法で規定される方法で、撥水剤付与前と撥水剤付与後の布帛を測定した。経方向の引裂き強力をＮ数５で測定し平均値を引裂き強力とした。
(7) Tear strength of fabric The fabric was measured before and after applying the water repellent agent by the method specified by JIS L1096D method. The tear strength in the warp direction was measured with an N number of 5, and the average value was taken as the tear strength.
［メタ型全芳香族ポリアミド繊維の製造］
メタ型全芳香族ポリアミド繊維は、次の方法で作製した。
特公昭４７－１０８６３号公報記載の方法に準じた界面重合法により製造した、固有粘度（Ｉ．Ｖ．）が１．９のポリメタフェニレンイソフタルアミド粉末２０．０質量部を、－１０℃に冷却したＮ－メチル－２－ピロリドン（ＮＭＰ）８０．０質量部中に懸濁させ、スラリー状にした。引き続き、懸濁液を６０℃まで昇温して溶解させ、透明なポリマー溶液を得た。該ポリマー溶液に、ポリマー対比３．０質量％の２－［２Ｈ－ベンゾトリアゾール－２－イル］－４－６－ビス（１－メチル－１－フェニルエチル）フェノール粉末（水への溶解度：０．０１ｍｇ／Ｌ）およびリン系難燃剤を混合溶解させ、減圧脱法して紡糸液（紡糸ドープ）とした。
[Production of meta-type wholly aromatic polyamide fiber]
A meta-type wholly aromatic polyamide fiber was produced by the following method.
20.0 parts by mass of polymetaphenylene isophthalamide powder having an intrinsic viscosity (I.V.) of 1.9, produced by an interfacial polymerization method according to the method described in JP-B-47-10863, was heated to -10°C. It was suspended in 80.0 parts by mass of cooled N-methyl-2-pyrrolidone (NMP) to form a slurry. Subsequently, the suspension was heated to 60° C. and dissolved to obtain a transparent polymer solution. 2-[2H-benzotriazol-2-yl]-4-6-bis(1-methyl-1-phenylethyl)phenol powder (solubility in water: 0 .01 mg/L) and a phosphorus-based flame retardant were mixed and dissolved, and depressurized to obtain a spinning solution (spinning dope).
［紡糸・凝固工程］
上記紡糸ドープを、孔径０．０７ｍｍ、孔数５００の紡糸口金から、浴温度３０℃の凝固浴中に吐出して紡糸した。凝固液の組成は、水／ＮＭＰ＝４５／５５（質量部）であり、凝固浴中に糸速７ｍ／分で吐出して紡糸した。
[Spinning/coagulation process]
The spinning dope was discharged into a coagulation bath having a bath temperature of 30° C. and spun from a spinneret having a hole diameter of 0.07 mm and a hole number of 500. The composition of the coagulation liquid was water/NMP=45/55 (parts by mass), and was spun by discharging into the coagulation bath at a yarn speed of 7 m/min.
［可塑延伸浴延伸工程］
引き続き、温度４０℃の水／ＮＭＰ＝４５／５５の組成の可塑延伸浴中にて、３．７倍の延伸倍率で延伸を行った。
[Plastic stretching bath stretching step]
Subsequently, the film was stretched at a draw ratio of 3.7 times in a plastic drawing bath having a composition of water/NMP=45/55 at a temperature of 40°C.
［洗浄工程］
延伸後、２０℃の水／ＮＭＰ＝７０／３０の浴（浸漬長１．８ｍ）、続いて２０℃の水浴（浸漬長３．６ｍ）で洗浄し、さらに６０℃の温水浴（浸漬長５．４ｍ）に通して十分に洗浄を行った。
[Washing process]
After stretching, it was washed in a water/NMP = 70/30 bath at 20°C (immersion length 1.8 m), followed by washing in a water bath at 20°C (immersion length 3.6 m), and further in a hot water bath at 60°C (immersion length 5 .4 m) for thorough washing.
［乾熱処理工程］
洗浄後の繊維について、表面温度２８０℃の熱ローラーにて乾熱処理を施し、メタ型全芳香族ポリアミド繊維を得た。
[Dry heat treatment process]
The washed fibers were subjected to dry heat treatment with a hot roller having a surface temperature of 280° C. to obtain meta-type wholly aromatic polyamide fibers.
［原繊維の物性］
得られたメタ型全芳香族ポリアミド繊維の物性は、単繊維繊度１．７ｄｔｅｘ、残存溶媒量０．０８質量％、結晶化度は１９％であった。得られた原繊維を用いて、捲縮加工、カットを行い、長さ５１ｍｍのステープルファイバー（原綿）を得た。
その他の繊維原綿は下記の物を用いた。
[Fibril properties]
The physical properties of the obtained meta-type wholly aromatic polyamide fiber were a single fiber fineness of 1.7 dtex, a residual solvent amount of 0.08% by mass, and a crystallinity of 19%. Using the obtained raw fibers, crimping and cutting were performed to obtain staple fibers (raw cotton) having a length of 51 mm.
Other raw fiber fibers used were as follows.
［後加工］
毛焼、精練、撥水加工、ファイナルセットにて後加工を行った。撥水加工は以下の方法で行った。
[Post-processing]
Post-processing was performed by singeing, scouring, water-repellent finishing, and final setting. Water-repellent finishing was performed by the following method.
［撥水加工］
撥水剤５０ｇ／Ｌと架橋１０ｇ／Ｌをピックアップ率６０％でパッド、ドライ（１００℃、３分）、その後熱処理を１７０℃、２分行った。なお、撥水剤は、実施例１：シリコーン系撥水剤、実施例２：ウレタン系撥水剤、実施例３：炭化水素系撥水剤、比較例１：シリコーン系撥水剤、比較例２：ウレタン系撥水剤、比較例３：フッ素系撥水剤を使用した。
[Water repellent finish]
A water repellent agent of 50 g/L and a cross-linking agent of 10 g/L were applied at a pick-up rate of 60% to a pad, dried (100° C., 3 minutes), and then heat-treated at 170° C. for 2 minutes. The water repellents are Example 1: Silicone water repellent, Example 2: Urethane water repellent, Example 3: Hydrocarbon water repellent, Comparative example 1: Silicone water repellent, Comparative example 2: Urethane-based water repellent, Comparative Example 3: Fluorine-based water repellent was used.
［実施例１］
メタ型全芳香族ポリアミド繊維（ＭＡ）（長さ５１ｍｍ）、導電糸（ＡＳ）（長さ５１ｍｍ）、パラ型全芳香族ポリアミド繊維（ＰＡ）（長さ５１ｍｍ）の各ステープルファイバーを、ＭＡ／ＡＳ／ＰＡ＝９３／２／５の質量比率で混紡した紡績糸４０番手／双糸とし、織密度 経９５本／２５．４ｍｍ、緯６０本／２５．４ｍｍで製織し、目付２００ｇ／ｍ２の綾織物を得た。これを用いて、上記の方法で加工した。結果を表１に示す。
[Example 1]
Each staple fiber of meta-type wholly aromatic polyamide fiber (MA) (length 51 mm), conductive yarn (AS) (length 51 mm), and para-type wholly aromatic polyamide fiber (PA) (length 51 mm), MA/ A spun yarn of 40 counts/two-ply yarn blended at a mass ratio of AS/PA = 93/2/5, weaved at a weaving density of 95 warps/25.4 mm and 60 wefts/25.4 mm, with a basis weight of 200 g/m 2 A twill fabric was obtained. Using this, it was processed by the method described above. Table 1 shows the results.
［実施例２］
メタ型全芳香族ポリアミド繊維（ＭＡ）（長さ５１ｍｍ）、難燃レーヨン繊維（ＦＲ）（長さ５１ｍｍ）、導電糸（ＡＳ）（長さ５１ｍｍ）、パラ型全芳香族ポリアミド繊維（ＰＡ）（長さ５１ｍｍ）の各ステープルファイバーを、ＭＡ／ＦＲ／ＡＳ／ＰＡ＝５８／３５／２／５の質量比率で混紡した紡績糸４０番手／双糸とし、織密度 経９５本／２５．４ｍｍ、緯６０本／２５．４ｍｍで製織し、目付２００ｇ／ｍ２の綾織物を得た。これを用いて、上記の方法で加工した。結果を表１に示す。
[Example 2]
Meta-type wholly aromatic polyamide fiber (MA) (length 51 mm), flame-retardant rayon fiber (FR) (length 51 mm), conductive thread (AS) (length 51 mm), para-type wholly aromatic polyamide fiber (PA) (Length: 51 mm), each staple fiber is blended at a mass ratio of MA / FR / AS / PA = 58 / 35 / 2 / 5, and the spun yarn is 40 counts / two-ply yarn, and the weaving density is 95 / 25.4 mm. and 60 wefts/25.4 mm to obtain a twill fabric having a basis weight of 200 g/m 2 . Using this, it was processed by the method described above. Table 1 shows the results.
［実施例３］
メタ型全芳香族ポリアミド繊維（ＭＡ）（長さ５１ｍｍ）、ポリエステル繊維（ＰＥＴ）（長さ５１ｍｍ）、導電糸（ＡＳ）（長さ５１ｍｍ）、パラ型全芳香族ポリアミド繊維（ＰＡ）（長さ５１ｍｍ）の各ステープルファイバーを、ＭＡ／ＰＥＴ／ＡＳ／ＰＡ＝８３／１０／２／５の質量比率で混紡した紡績糸４０番手／双糸とし、織密度 経９５本／２５．４ｍｍ、緯６０本／２５．４ｍｍで製織し、目付２００ｇ／ｍ２の綾織物を得た。これを用いて、上記の方法で加工した。結果を表１に示す。
[Example 3]
Meta-type wholly aromatic polyamide fiber (MA) (length 51 mm), polyester fiber (PET) (length 51 mm), conductive yarn (AS) (length 51 mm), para-type wholly aromatic polyamide fiber (PA) (length 51 mm) staple fibers are blended at a mass ratio of MA / PET / AS / PA = 83 / 10 / 2 / 5 to make spun yarn 40 count / two-ply yarn, weave density warp 95 / 25.4 mm, weft A twill fabric having a basis weight of 200 g/m 2 was obtained by weaving at 60 threads/25.4 mm. Using this, it was processed by the method described above. Table 1 shows the results.
［比較例１］
メタ型全芳香族ポリアミド繊維（ＭＡ）、コットン（ＣＯ）、パラ型全芳香族ポリアミド繊維（ＰＡ）からなるＭＡ／ＣＯ／ＰＡ＝８５／１０／５の比率で混紡した紡績糸４０番手／双糸とし、織密度 経９５本／２５．４ｍｍ、緯６０本／２５．４ｍｍで製織し、目付２００ｇ／ｍ２の綾織物を得た。これを用いて、上記の方法で加工した。結果を表１に示す。
[Comparative Example 1]
40 count/pair of spun yarn blended at a ratio of MA/CO/PA = 85/10/5 consisting of meta-type wholly aromatic polyamide fiber (MA), cotton (CO), and para-type wholly aromatic polyamide fiber (PA) The yarn was woven at a warp density of 95 threads/25.4 mm and a weft density of 60 threads/25.4 mm to obtain a twill fabric having a basis weight of 200 g/m 2 . Using this, it was processed by the method described above. Table 1 shows the results.
［比較例２］
メタ型全芳香族ポリアミド繊維（ＭＡ）、難燃レーヨン繊維（ＦＲ）、コットン繊維（ＣＯ）、パラ型全芳香族ポリアミド繊維（ＰＡ）、導電糸（ＡＳ）からなるＭＡ／ＦＲ／ＣＯ／ＰＡ／ＡＳ＝３５／３５／２３／５／２の質量比率で混紡した紡績糸４０番手／双糸とし、織密度 経９５本／２５．４ｍｍ、緯６０本／２５．４ｍｍで製織し、目付２００ｇ／ｍ２の綾織物を得た。これを用いて、上記の方法で加工した。結果を表１に示す。
[Comparative Example 2]
MA/FR/CO/PA consisting of meta-type wholly aromatic polyamide fiber (MA), flame-retardant rayon fiber (FR), cotton fiber (CO), para-type wholly aromatic polyamide fiber (PA), and conductive yarn (AS) /AS = 40 count spun yarn blended at a mass ratio of 35/35/23/5/2, and woven at a weaving density of 95 warps/25.4mm and 60 wefts/25.4mm, with a basis weight of 200g. /m 2 of twill fabric was obtained. Using this, it was processed by the method described above. Table 1 shows the results.
［比較例３］
使用した撥水剤を変更すること以外は、実施例１と同様にした。使用した撥水剤は、アルキルフルオロポリマーを１００ｇ／Ｌ付与した。結果を表１に示す。
[Comparative Example 3]
The procedure was the same as in Example 1, except that the water repellent used was changed. The water repellent used was an alkylfluoropolymer of 100 g/L. Table 1 shows the results.
本発明によれば、メタ型全芳香族ポリアミド繊維を含み、極めて優れた難燃性を有し、環境に配慮した撥水性および引裂き強力にも優れた難燃性布帛および繊維製品が提供され、その工業的価値は極めて大である。 According to the present invention, flame-retardant fabrics and textile products containing meta-type wholly aromatic polyamide fibers, having extremely excellent flame retardancy, and being environmentally friendly and having excellent water repellency and tear strength are provided. Its industrial value is extremely large.
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