JP4526959B2 - Textile products reused after steam sterilization - Google Patents
Textile products reused after steam sterilization Download PDFInfo
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- JP4526959B2 JP4526959B2 JP2005011105A JP2005011105A JP4526959B2 JP 4526959 B2 JP4526959 B2 JP 4526959B2 JP 2005011105 A JP2005011105 A JP 2005011105A JP 2005011105 A JP2005011105 A JP 2005011105A JP 4526959 B2 JP4526959 B2 JP 4526959B2
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- Prior art keywords
- acid
- fiber
- polyamide
- mol
- strength
- 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.)
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- 239000004753 textile Substances 0.000 title description 13
- 238000004659 sterilization and disinfection Methods 0.000 title description 11
- 230000001954 sterilising effect Effects 0.000 title description 10
- 239000000835 fiber Substances 0.000 claims description 76
- 239000004952 Polyamide Substances 0.000 claims description 34
- 229920002647 polyamide Polymers 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 27
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 14
- SXJVFQLYZSNZBT-UHFFFAOYSA-N nonane-1,9-diamine Chemical compound NCCCCCCCCCN SXJVFQLYZSNZBT-UHFFFAOYSA-N 0.000 claims description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N terephthalic acid group Chemical group C(C1=CC=C(C(=O)O)C=C1)(=O)O KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 13
- 125000004427 diamine group Chemical group 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- 125000001142 dicarboxylic acid group Chemical group 0.000 claims description 10
- 125000003118 aryl group Chemical group 0.000 claims description 8
- GAGWMWLBYJPFDD-UHFFFAOYSA-N 2-methyloctane-1,8-diamine Chemical compound NCC(C)CCCCCCN GAGWMWLBYJPFDD-UHFFFAOYSA-N 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- -1 polyethylene terephthalate Polymers 0.000 description 23
- 230000014759 maintenance of location Effects 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229920000728 polyester Polymers 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000004744 fabric Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 238000009987 spinning Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 150000004985 diamines Chemical class 0.000 description 5
- 230000000474 nursing effect Effects 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920001707 polybutylene terephthalate Polymers 0.000 description 4
- 238000009958 sewing Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000005711 Benzoic acid Substances 0.000 description 3
- 235000010233 benzoic acid Nutrition 0.000 description 3
- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 239000000986 disperse dye Substances 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920002215 polytrimethylene terephthalate Polymers 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 229920002292 Nylon 6 Polymers 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000002788 crimping Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002763 monocarboxylic acids Chemical class 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- 229920006122 polyamide resin Polymers 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-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
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 2
- SZHOJFHSIKHZHA-UHFFFAOYSA-N tridecanoic acid Chemical compound CCCCCCCCCCCCC(O)=O SZHOJFHSIKHZHA-UHFFFAOYSA-N 0.000 description 2
- 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
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- XBTRYWRVOBZSGM-UHFFFAOYSA-N (4-methylphenyl)methanediamine Chemical compound CC1=CC=C(C(N)N)C=C1 XBTRYWRVOBZSGM-UHFFFAOYSA-N 0.000 description 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- PXGZQGDTEZPERC-UHFFFAOYSA-N 1,4-cyclohexanedicarboxylic acid Chemical compound OC(=O)C1CCC(C(O)=O)CC1 PXGZQGDTEZPERC-UHFFFAOYSA-N 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- GBURUDXSBYGPBL-UHFFFAOYSA-N 2,2,3-trimethylhexanedioic acid Chemical compound OC(=O)C(C)(C)C(C)CCC(O)=O GBURUDXSBYGPBL-UHFFFAOYSA-N 0.000 description 1
- JCUZDQXWVYNXHD-UHFFFAOYSA-N 2,2,4-trimethylhexane-1,6-diamine Chemical compound NCCC(C)CC(C)(C)CN JCUZDQXWVYNXHD-UHFFFAOYSA-N 0.000 description 1
- WKRCUUPMCASSBN-UHFFFAOYSA-N 2,2-diethylbutanedioic acid Chemical compound CCC(CC)(C(O)=O)CC(O)=O WKRCUUPMCASSBN-UHFFFAOYSA-N 0.000 description 1
- BTUDGPVTCYNYLK-UHFFFAOYSA-N 2,2-dimethylglutaric acid Chemical compound OC(=O)C(C)(C)CCC(O)=O BTUDGPVTCYNYLK-UHFFFAOYSA-N 0.000 description 1
- DPQHRXRAZHNGRU-UHFFFAOYSA-N 2,4,4-trimethylhexane-1,6-diamine Chemical compound NCC(C)CC(C)(C)CCN DPQHRXRAZHNGRU-UHFFFAOYSA-N 0.000 description 1
- JZUMVFMLJGSMRF-UHFFFAOYSA-N 2-Methyladipic acid Chemical compound OC(=O)C(C)CCCC(O)=O JZUMVFMLJGSMRF-UHFFFAOYSA-N 0.000 description 1
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- ZVMAGJJPTALGQB-UHFFFAOYSA-N 2-[3-(carboxymethoxy)phenoxy]acetic acid Chemical compound OC(=O)COC1=CC=CC(OCC(O)=O)=C1 ZVMAGJJPTALGQB-UHFFFAOYSA-N 0.000 description 1
- DNXOCFKTVLHUMU-UHFFFAOYSA-N 2-[4-(carboxymethoxy)phenoxy]acetic acid Chemical compound OC(=O)COC1=CC=C(OCC(O)=O)C=C1 DNXOCFKTVLHUMU-UHFFFAOYSA-N 0.000 description 1
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 1
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 description 1
- WVDRSXGPQWNUBN-UHFFFAOYSA-N 4-(4-carboxyphenoxy)benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1OC1=CC=C(C(O)=O)C=C1 WVDRSXGPQWNUBN-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
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
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- 229920006395 saturated elastomer Polymers 0.000 description 1
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- ACUGTEHQOFWBES-UHFFFAOYSA-M sodium hypophosphite monohydrate Chemical compound O.[Na+].[O-]P=O ACUGTEHQOFWBES-UHFFFAOYSA-M 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003504 terephthalic acids Chemical class 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Polyamides (AREA)
- Artificial Filaments (AREA)
- Woven Fabrics (AREA)
Description
本発明は、病院・介護施設・食品産業・バイオ研究施設などで使用されるユニフォーム等の衣料品やシーツなどの繊維製品に関し、詳しくは、蒸気滅菌処理したのち再使用される繊維製品であって、高温高圧蒸気処理(オートクレーブ処理)による消毒・滅菌処理に対して高い耐久性を示す繊維製品に関する。 The present invention relates to textile products such as uniforms and clothing and sheets used in hospitals, nursing homes, food industries, bio-research facilities, and the like. More specifically, the present invention relates to textile products that are reused after steam sterilization. The present invention relates to a textile product exhibiting high durability against disinfection / sterilization treatment by high-temperature high-pressure steam treatment (autoclave treatment).
従来、病院・介護施設・食品産業・バイオ研究施設では、使用後のユニフォーム等の衣料製品やシーツなどについては、その約８０％にディスポーザブル製品が用いられている。そのため、使用後は医療廃棄物、産業廃棄物として焼却処分されるため、環境問題のおおきなひとつとして指摘されている。 Conventionally, disposable products are used in about 80% of clothing products such as uniforms and sheets after use in hospitals, nursing homes, food industries and bio-research facilities. Therefore, after use, it is incinerated as medical waste and industrial waste.
焼却処分に代えて、再使用（リユース）する方法があり、再使用するためには、一般的に、使用後の繊維製品を高温高圧蒸気処理(オートクレーブ処理)により消毒・滅菌処理する方法が採用されている。従来、病院・介護施設・食品産業・バイオ研究施設で使用されているユニフォームやシーツなどの繊維製品は、ポリエチレンテレフタレート系のポリエステル長繊維を使用したものが多いが、従来のポリエステル系長繊維を使用した製品では、繰り返しオートクレーブ処理により経時的に加水分解による強度劣化を起こし、リユースにも限界があるのが現状である。加えて最近では、オートクレーブ処理の効率化の要求により、より高温処理条件が採用されるようになり、さらにリユース回数が減少するという問題が生じている。この対策として、ポリエステルの耐加水分解性を高めるべく、カルボキシル末端封鎖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、ポリトリエチレンテレフタレート等が発表されている。例えば特開２００２−４１４６公報（特許文献１）には、蒸気滅菌用の布帛としてポリトリメチレンテレフタレート繊維を使用した布帛が適していることが記載されている。 In place of incineration disposal, there is a method of reuse (reuse), and in order to reuse, generally a method of disinfecting and sterilizing treated fiber products by high-temperature high-pressure steam treatment (autoclave treatment) is adopted. Has been. Conventionally, textile products such as uniforms and sheets used in hospitals, nursing homes, food industries, and bio-research facilities often use polyethylene terephthalate-based polyester filaments, but conventional polyester filaments are used. In the present product, strength degradation due to hydrolysis is caused over time by repeated autoclave treatment, and there is a limit to reuse. In addition, recently, due to demands for improving the efficiency of autoclave processing, higher temperature processing conditions have been adopted, and there has been a problem that the number of reuses is further reduced. As measures against this, carboxyl end-capped polyethylene terephthalate, polybutylene terephthalate, polytriethylene terephthalate, and the like have been announced to increase the hydrolysis resistance of polyester. For example, JP-A-2002-4146 (Patent Document 1) describes that a fabric using polytrimethylene terephthalate fiber is suitable as a fabric for steam sterilization.
しかしながら、従来のポリエステルよりは優れているものの本発明品の示す耐久性には至っていない。また、ポリエチレンテレフタレートのみならず、ポリブチレンテレフタレート、ポリトリエチレンテレフタレートにおいてもエステル結合を有しており、これらエステル結合を有するポリマーは強アルカリ条件下加水分解が進行し、容易に強度劣化する弱点も有していることも周知の事実である。 However, although it is superior to the conventional polyester, it does not reach the durability exhibited by the product of the present invention. In addition to polyethylene terephthalate, polybutylene terephthalate and polytriethylene terephthalate also have ester bonds, and these ester-bonded polymers are subject to hydrolysis under strong alkaline conditions and easily deteriorate in strength. It is also a well-known fact that it has.
本発明の目的は、繰り返しのオートクレーブ処理に対し高い耐久性を有し、さらに強アルカリ、強酸に対しても高い耐久性を有する結果、高温高圧蒸気処理により消毒・滅菌処理が行われたのち再使用に適した繊維製品を提供することにある。 The object of the present invention is that it has high durability against repeated autoclave treatment, and also has high durability against strong alkalis and strong acids. It is to provide a textile product suitable for use.
本発明者らは、上記問題点を解決すべく鋭意検討を行ってきた結果、特定の芳香族ジカルボン酸と特定のアルキレンジアミンからなるポリアミド繊維にて達成できることを見いだし、本発明を完成した。 As a result of intensive studies to solve the above problems, the present inventors have found that this can be achieved with a polyamide fiber composed of a specific aromatic dicarboxylic acid and a specific alkylene diamine, thereby completing the present invention.
すなわち、本発明は、使用された繊維製品を高温高圧蒸気を用いて消毒・滅菌処理したのち再使用する繊維製品の再使用方法において、該繊維製品の少なくとも一部が、ジカルボン酸単位の６０モル％以上が芳香族ジカルボン酸であるジカルボン酸単位とジアミン単位の６０モル％以上が炭素数６〜１２の脂肪族アルキレンジアミンであるジアミン単位とからなるポリアミド繊維から構成されていることを特徴とする繊維製品の再使用方法である。そして、好ましくは、該ポリアミド繊維を構成するポリアミドが、実質的に芳香族ジカルボン酸単位と脂肪族ジアミン単位からなり、該芳香族ジカルボン酸単位の９０モル％以上がテレフタル酸であり、該ジアミン単位の９０モル％以上が１，９−ノナンジアミンまたは１，９−ノナンジアミンと２−メチル−１，８−オクタンジアミンとの併用物である繊維製品の再使用方法である。
That is, the present invention relates to a method for reusing a fiber product in which the used fiber product is sterilized and sterilized using high-temperature and high-pressure steam and then reused. At least a part of the fiber product contains 60 mol of dicarboxylic acid units. % Or more is composed of a polyamide fiber composed of a dicarboxylic acid unit which is an aromatic dicarboxylic acid and 60 mol% or more of the diamine unit is a diamine unit which is an aliphatic alkylenediamine having 6 to 12 carbon atoms. This is a method for reusing textile products. Preferably, the polyamide constituting the polyamide fiber is substantially composed of an aromatic dicarboxylic acid unit and an aliphatic diamine unit, and 90 mol% or more of the aromatic dicarboxylic acid unit is terephthalic acid, and the diamine unit Is a method for reusing a textile product in which 90 mol% or more of 1,9-nonanediamine or a combination of 1,9-nonanediamine and 2-methyl-1,8-octanediamine is used .
本発明に用いられるポリアミド繊維を構成するポリアミドは、ジカルボン酸単位とジアミン単位からなり、ジカルボン酸単位の６０モル％以上が芳香族ジカルボン酸であること、およびジアミン単位の６０モル％以上が炭素数６〜１２の脂肪族アルキレンジアミンであることに特徴を有する。 The polyamide constituting the polyamide fiber used in the present invention comprises a dicarboxylic acid unit and a diamine unit, 60 mol% or more of the dicarboxylic acid unit is an aromatic dicarboxylic acid, and 60 mol% or more of the diamine unit is carbon number. It is characterized by being 6-12 aliphatic alkylenediamine.
芳香族ジカルボン酸としては、耐高温高圧蒸気処理性の点でテレフタル酸が好ましく、このテレフタル酸の一部をイソフタル酸、２，６−ナフタレンジカルボン酸、２，７−ナフタレンジカルボン酸、１，４−ナフタレンジカルボン酸、１，４−フェニレンジオキシジ酢酸、１，３−フェニレンジオキシジ酢酸、ジフェン酸、ジ安息香酸、４，４'−オキシジ安息香酸、ジフェニルメタン−４，４'−ジカルボン酸、ジフェニルスルホン−４，４'−ジカルボン酸、４，４'−ビフェニルジカルボン酸等の芳香族ジカルボン酸の１種類または２種類以上で置き換えることもできる。 As the aromatic dicarboxylic acid, terephthalic acid is preferable from the viewpoint of high temperature and high pressure steam resistance, and a part of this terephthalic acid is isophthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, 1,4 -Naphthalenedicarboxylic acid, 1,4-phenylenedioxydiacetic acid, 1,3-phenylenedioxydiacetic acid, diphenic acid, dibenzoic acid, 4,4'-oxydibenzoic acid, diphenylmethane-4,4'-dicarboxylic acid , Diphenylsulfone-4,4′-dicarboxylic acid, 4,4′-biphenyldicarboxylic acid and other aromatic dicarboxylic acids can be substituted with one kind or two or more kinds.
かかる芳香族ジカルボン酸の含有量は、耐高温高圧蒸気処理性の点でジカルボン酸単位の６０モル％以上であり、７５モル％以上であることが好ましく、さらに好ましくは９０モル％以上が芳香族ジカルボン酸である場合である。上記芳香族ジカルボン酸以外のジカルボン酸としては、マロン酸、ジメチルマロン酸、コハク酸、３，３−ジエチルコハク酸、グルタル酸、２，２−ジメチルグルタル酸、アジピン酸、２−メチルアジピン酸、トリメチルアジピン酸、ピメリン酸、アゼライン酸、セバシン酸、スベリン酸等の脂肪族ジカルボン酸；１，３−シクロペンタンジカルボン酸、１，４−シクロヘキサンジカルボン酸等の脂環式ジカルボン酸等を挙げることができ、これらの酸は１種類のみならず２種類以上を併用することができる。 The content of the aromatic dicarboxylic acid is 60 mol% or more, preferably 75 mol% or more, more preferably 90 mol% or more of the dicarboxylic acid unit in terms of high temperature and high pressure steam resistance. This is the case when it is a dicarboxylic acid. Examples of the dicarboxylic acid other than the aromatic dicarboxylic acid include malonic acid, dimethylmalonic acid, succinic acid, 3,3-diethylsuccinic acid, glutaric acid, 2,2-dimethylglutaric acid, adipic acid, 2-methyladipic acid, Aliphatic dicarboxylic acids such as trimethyladipic acid, pimelic acid, azelaic acid, sebacic acid and suberic acid; alicyclic dicarboxylic acids such as 1,3-cyclopentanedicarboxylic acid and 1,4-cyclohexanedicarboxylic acid These acids can be used alone or in combination of two or more.
なかでも、繊維強度、耐オートクレーブ性および耐薬品性の点で、ジカルボン酸単位が１００％芳香族ジカルボン酸であることが好ましい。さらにトリメリット酸、トリメシン酸、ピロメリット酸等の多価カルボン酸を、繊維化・不織布化が容易な範囲内で含有させることもできる。 Especially, it is preferable that a dicarboxylic acid unit is 100% aromatic dicarboxylic acid at the point of fiber strength, autoclave resistance, and chemical resistance. Furthermore, a polyvalent carboxylic acid such as trimellitic acid, trimesic acid, and pyromellitic acid can be contained within a range where fiberization and non-woven fabric can be easily formed.
また、ジアミン単位の６０モル％以上は炭素数が６〜１２の脂肪族アルキレンジアミンで構成されていることが耐高温高圧滅菌処理性の点で必要であり、かかる脂肪族アルキレンジアミンとしては、１，６−ヘキサンジアミン、１，８−オクタンジアミン、１，９−ノナンジアミン、１，１０−デカンジアミン、１，１１−ウンデカンジアミン、１，１２−ドデカンジアミン、２−メチル−１，５−ペンタンジアミン、３−メチル−１，５−ペンタンジアミン、２，２，４−トリメチル−１，６−ヘキサンジアミン、２，４，４−トリメチル−１，６−ヘキサンジアミン、２−メチル−１，８−オクタンジアミン、５−メチル−１，９−ノナンジアミン等の脂肪族ジアミンを挙げることができる。なかでも耐オートクレーブ性の点で、１，９−ノナンジアミンまたは１，９−ノナンジアミンと２−メチル−１，８−オクタンジアミンとの併用が好ましい。この脂肪族アルキレンジアミンの含有量はジアミン単位の６０モル％以上であるが、７５モル％以上、特に９０モル％以上であることが好ましい。 Further, 60 mol% or more of the diamine unit is required to be composed of an aliphatic alkylene diamine having 6 to 12 carbon atoms from the viewpoint of the high temperature and high pressure sterilization resistance. , 6-hexanediamine, 1,8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 1,11-undecanediamine, 1,12-dodecanediamine, 2-methyl-1,5-pentanediamine 3-methyl-1,5-pentanediamine, 2,2,4-trimethyl-1,6-hexanediamine, 2,4,4-trimethyl-1,6-hexanediamine, 2-methyl-1,8- Examples thereof include aliphatic diamines such as octanediamine and 5-methyl-1,9-nonanediamine. Of these, 1,9-nonanediamine or a combination of 1,9-nonanediamine and 2-methyl-1,8-octanediamine is preferred from the viewpoint of autoclave resistance. The content of the aliphatic alkylene diamine is 60 mol% or more of the diamine unit, but is preferably 75 mol% or more, particularly preferably 90 mol% or more.
上述の脂肪族アルキレンジアミン以外のジアミンとしては、エチレンジアミン、プロピレンジアミン、１，４−ブタンジアミン等の脂肪族ジアミン；シクロヘキサンジアミン、メチルシクロヘキサンジアミン、イソホロンジアミン、ノルボルナンジメチルジアミン、トリシクロデカンジメチルジアミン等の脂環式ジアミン；ｐ−フェニレンジアミン、ｍ−フェニレンジアミン、キシリレンジアミン、キシレンジアミン、４，４'−ジアミノジフェニルメタン、４，４'−ジアミノジフェニルスルホン、４，４'−ジアミノジフェニルエ−テル等の芳香族ジアミン、あるいはこれらの混合物を挙げることができ、これらは１種類のみならず２種類以上を併用することができる。 Examples of diamines other than the above-mentioned aliphatic alkylene diamines include aliphatic diamines such as ethylene diamine, propylene diamine, and 1,4-butane diamine; cyclohexane diamine, methyl cyclohexane diamine, isophorone diamine, norbornane dimethyl diamine, tricyclodecane dimethyl diamine, and the like. Alicyclic diamines; p-phenylenediamine, m-phenylenediamine, xylylenediamine, xylenediamine, 4,4′-diaminodiphenylmethane, 4,4′-diaminodiphenylsulfone, 4,4′-diaminodiphenyl ether, etc. These aromatic diamines or mixtures thereof can be used, and these can be used alone or in combination of two or more.
脂肪族アルキレンジアミンとして、１，９−ノナンジアミンと２−メチル−１，８−オクタンジアミンとを併用する場合、ジアミン成分の６０〜１００モル％が１，９−ノナンジアミンと２−メチル−１，８−オクタンジアミンからなり、かつそのモル比は前者：後者＝３０：７０〜９９：１、特に前者：後者＝４０：６０〜９５：５、さらに好ましくは４０：６０〜６０：４０であることが繊維化工程性の点で好ましい。 When 1,9-nonanediamine and 2-methyl-1,8-octanediamine are used in combination as the aliphatic alkylene diamine, 60 to 100 mol% of the diamine component is 1,9-nonanediamine and 2-methyl-1,8. -Made of octanediamine and the molar ratio of the former: the latter = 30: 70 to 99: 1, especially the former: the latter = 40: 60 to 95: 5, more preferably 40:60 to 60:40. It is preferable in terms of fiberizing processability.
以上のことから、本発明を構成するポリアミドとしては、実質的に芳香族ジカルボン酸単位と脂肪族ジアミン単位からなり、該芳香族ジカルボン酸単位の９０モル％以上がテレフタル酸であり、該ジアミン単位の９０モル％以上が１，９−ノナンジアミンまたは１，９−ノナンジアミンと２−メチル−１，８−オクタンジアミンとの併用物である場合である。 From the above, the polyamide constituting the present invention substantially consists of an aromatic dicarboxylic acid unit and an aliphatic diamine unit, and 90 mol% or more of the aromatic dicarboxylic acid unit is terephthalic acid, and the diamine unit 90 mol% or more of 1,9-nonanediamine or a combination of 1,9-nonanediamine and 2-methyl-1,8-octanediamine.
また、本発明に用いられるポリアミドは、その分子鎖における〔ＣＯＮＨ／ＣＨ2 〕の比が１／２〜１／８、とくに１／３〜１／５であることが繊維強度で代表される繊維物性の点で好ましい。 The polyamide used in the present invention is a fiber represented by fiber strength such that the ratio of [CONH / CH 2 ] in the molecular chain is 1/2 to 1/8, particularly 1/3 to 1/5. It is preferable in terms of physical properties.
上述のポリアミドの極限粘度（濃硫酸中３０℃で測定した値）としては、０．６〜２．０ｄｌ／ｇであることが好ましく、より好ましくは０．６〜１．８ｄｌ／ｇの範囲、もっとも好ましくは０．７〜１．６ｄｌ／ｇの範囲である。該極限粘度の範囲内のポリアミドは、繊維化する際の溶融粘度特性が良好であり、さらに得られる繊維強度、耐オートクレーブ性、耐アルカリ性、耐酸性等が優れたものとなる。 The intrinsic viscosity of the polyamide described above (value measured at 30 ° C. in concentrated sulfuric acid) is preferably 0.6 to 2.0 dl / g, more preferably in the range of 0.6 to 1.8 dl / g. Most preferably, it is the range of 0.7-1.6 dl / g. The polyamide within the range of the intrinsic viscosity has good melt viscosity characteristics when fiberized, and further has excellent fiber strength, autoclave resistance, alkali resistance, acid resistance, and the like.
さらに上述のポリアミドは、その分子鎖の末端基の１０％以上が末端封止剤により封止されていることが好ましく、より好ましくは末端の４０％以上、さらに好ましくは末端の７０％以上が封止されている場合である。分子鎖の末端を封止することにより、得られる繊維強度、耐オートクレーブ性、耐アルカリ性、耐酸性等が優れたものとなる。末端封止剤としては、ポリアミド末端のアミノ基またはカルボキシル基と反応性を有する単官能性の化合物であればとくに制限はないが、反応性および封止末端の安定性等の点からモノカルボン酸、モノアミンが好ましい。なかでも、取扱性の容易さ、反応性、封止末端の安定性、価格等の点でモノカルボン酸が好ましい。好適なモノカルボン酸としては、酢酸、プロピオン酸、酪酸、吉草酸、カプロン酸、カプリル酸、ラウリン酸、トリデシル酸、ミリスチン酸、パルミチン酸、ステアリン酸、安息香酸などを挙げることができる。なお、末端の封止率は1 Ｈ−ＮＭＲにより、各末端基に対応する特性シグナルの積分値より求めることができる。 Further, in the above-mentioned polyamide, it is preferable that 10% or more of the end groups of the molecular chain are sealed with an end-capping agent, more preferably 40% or more of the ends, and still more preferably 70% or more of the ends are sealed. This is the case when it is stopped. By sealing the end of the molecular chain, the resulting fiber strength, autoclave resistance, alkali resistance, acid resistance and the like are excellent. The end capping agent is not particularly limited as long as it is a monofunctional compound having reactivity with the amino group or carboxyl group at the end of the polyamide, but monocarboxylic acid from the viewpoint of reactivity and stability of the capping end. Monoamine is preferred. Of these, monocarboxylic acids are preferable in terms of ease of handling, reactivity, stability of the capped ends, price, and the like. Suitable monocarboxylic acids include acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, caprylic acid, lauric acid, tridecylic acid, myristic acid, palmitic acid, stearic acid, benzoic acid and the like. The terminal sealing rate can be determined from the integral value of the characteristic signal corresponding to each terminal group by 1 H-NMR.
上述のポリアミドの製造方法は特に制限されず、結晶性ポリアミドを製造する方法として公知の任意の方法を用いることができる。たとえば、酸クロライドとジアミンとを原料とする溶液重合法あるいは界面重合法、ジカルボン酸またはジカルボン酸のアルキルエステルとジアミンとを原料とする溶融重合法、固相重合法等の方法により製造できる。 The method for producing the above polyamide is not particularly limited, and any known method can be used as a method for producing the crystalline polyamide. For example, it can be produced by a solution polymerization method or an interfacial polymerization method using acid chloride and diamine as raw materials, a melt polymerization method using dicarboxylic acid or an alkyl ester of dicarboxylic acid and diamine as raw materials, or a solid phase polymerization method.
一例を挙げると、末端封止剤、触媒、ジアミン成分およびジカルボン酸成分を一括して反応させ、ナイロン塩を製造した後、一旦２８０℃以下の温度において極限粘度が０．１５〜０．３０ｄｌ／ｇのプレポリマ−とし、さらに固相重合するか、あるいは溶融押出機を用いて重合を行うことにより、容易に製造することができる。重合の最終段階を固相重合を行う場合、減圧下または不活性ガス流通下に行うのが好ましく、重合温度が２００〜２５０℃の範囲であれば、重合速度が大きく、生産性に優れ、着色やゲル化を有効に抑制することができるので好ましい。重合の最終段階を溶融押出機により行う場合、重合温度が３７０℃以下であるとポリアミドの分解がほとんどなく、劣化のないポリアミドが得られるので好ましい。 For example, after the end-capping agent, catalyst, diamine component and dicarboxylic acid component are reacted together to produce a nylon salt, the intrinsic viscosity is 0.15 to 0.30 dl / The polymer can be easily produced by solid-phase polymerization with a prepolymer of g or polymerization using a melt extruder. When solid-phase polymerization is performed as the final stage of polymerization, it is preferably performed under reduced pressure or under an inert gas flow. If the polymerization temperature is in the range of 200 to 250 ° C., the polymerization rate is high, the productivity is excellent, and coloring And gelling can be effectively suppressed. When the final stage of the polymerization is carried out by a melt extruder, it is preferable that the polymerization temperature is 370 ° C. or lower because the polyamide is hardly decomposed and a polyamide having no deterioration is obtained.
重合触媒としてはリン酸、亜リン酸、次亜リン酸またはそれらのアンモニウム塩、それらの金属塩、それらのエステル類を挙げることができ、なかでも次亜リン酸ナトリウムが入手のし易さ、取扱性等の点で好ましい。また、必要に応じて銅化合物等の安定剤、着色剤、紫外線吸収剤、光安定剤、酸化防止剤、帯電防止剤、難燃剤、可塑剤、潤滑剤、結晶化速度遅延剤等を重縮合反応時、またはその後に添加することができる。とくに熱安定剤としてヒンダ−ドフェノ−ル等の有機系安定剤、ヨウ化銅等のハロゲン化銅化合物、ヨウ化カリウム等のハロゲン化アルカリ金属化合物を添加すると、繊維化の際の溶融滞留安定性が向上するので好ましい。 Examples of the polymerization catalyst include phosphoric acid, phosphorous acid, hypophosphorous acid or ammonium salts thereof, metal salts thereof, esters thereof, and among them, sodium hypophosphite is easily available, It is preferable in terms of handleability. If necessary, stabilizers such as copper compounds, colorants, UV absorbers, light stabilizers, antioxidants, antistatic agents, flame retardants, plasticizers, lubricants, crystallization rate retarders, etc. are polycondensed. It can be added during or after the reaction. Especially when an organic stabilizer such as hindered phenol, a copper halide compound such as copper iodide, or an alkali metal halide compound such as potassium iodide is added as a heat stabilizer, the melt retention stability during fiberization Is preferable.
上述のようにして得られたポリアミドは、通常、溶融押出機を用いて溶融紡糸され、延伸が施されるが、スクリュ−型押出機を使用することが好ましい。ポリアミドの融点以上、３６０℃以下の温度で溶融し、３０分以内の溶融滞留時間で口金ノズルより紡出することにより繊維化することができる。溶融温度、滞留時間が上記の範囲内であれば、紡糸時のポリアミドの熱分解を抑制することができる。 The polyamide obtained as described above is usually melt-spun using a melt extruder and stretched, but it is preferable to use a screw-type extruder. It can be fiberized by melting at a temperature not lower than the melting point of polyamide and not higher than 360 ° C., and spinning from a nozzle nozzle with a melt residence time within 30 minutes. When the melting temperature and the residence time are within the above ranges, it is possible to suppress the thermal decomposition of the polyamide during spinning.
前述のごとく紡出した糸条を引取りロ−ラ等により引き取る。この時、必要に応じてノズル直下に加熱または保温ゾ−ンを設けたり、吹き付けチャンバ−等による冷却ゾ−ンを設けたり、紡出した糸条に油剤を塗布してもよい。延伸は加熱浴、加熱蒸気吹き付け、ロ−ラヒ−タ−、接触プレ−トヒ−タ−、非接触プレ−トヒ−タ−等を使用して２７０℃以下で行うことが好ましく、１２０〜２３０℃の範囲で行うことがより好ましい。さらに延伸倍率は２倍以上が好ましく、３倍以上がより好ましい。この時、２７０℃より高い温度で延伸を行うとポリアミドの劣化や結晶の再組織化等が起こり繊維強度が低下する。必要に応じて、延伸に引き続いて、さらに１２０〜２７０℃で定長熱処理、緊張熱処理または弛緩熱処理を行うことができる。上記の方法以外にも紡糸直結延伸を行うことも可能である。 The yarn spun as described above is taken up by a take-up roller or the like. At this time, if necessary, a heating or heat retaining zone may be provided immediately below the nozzle, a cooling zone by a spraying chamber or the like may be provided, or an oil agent may be applied to the spun yarn. Stretching is preferably performed at 270 ° C. or lower using a heating bath, heated steam spray, roller heater, contact plate heater, non-contact plate heater, etc., and 120 to 230 ° C. It is more preferable to carry out in the range. Furthermore, the draw ratio is preferably 2 times or more, more preferably 3 times or more. At this time, if stretching is performed at a temperature higher than 270 ° C., the polyamide is deteriorated, crystals are reorganized, and the fiber strength is lowered. If necessary, subsequent to stretching, constant length heat treatment, tension heat treatment or relaxation heat treatment can be further performed at 120 to 270 ° C. In addition to the above method, it is also possible to perform direct spinning drawing.
また、繊維の繊度は、使用目的に応じて変更することができ、単繊維繊度が１デシッテクス〜３０デシテックス程度とすることができる。さらに、繊維の断面形状も限定されず、円形以外に楕円形、三角断面、十字断面、中空断面など種々の断面の繊維とすることができる。 Moreover, the fineness of the fiber can be changed according to the purpose of use, and the single fiber fineness can be about 1 dtex to 30 dtex. Furthermore, the cross-sectional shape of the fiber is not limited, and it can be a fiber having various cross sections such as an ellipse, a triangular cross section, a cross section, and a hollow cross section other than a circular shape.
このようにして得られたポリアミド繊維は、常法により捲縮付与カットし、ステープルとして紡績糸とすることもできるし、また長繊維の場合、ディスク方式やベルト方式による仮撚加工により捲縮付与したウーリー加工糸とすることもできる。 The polyamide fiber thus obtained can be cut by crimping by a conventional method and can be made into a spun yarn as a staple. In the case of long fibers, crimping is imparted by a false twisting process using a disk method or a belt method. It can also be a woolen yarn.
このようにして得られた紡績糸またはウーリー加工糸は、１４０℃の湿熱処理１５００分後５０％以上の強度保持率を示し、また７０℃の１０％水酸化ナトリウム水溶液中で１００時間処理後の強度保持率が８０％以上であり、また７０℃の１０％硫酸水溶液中で１００時間処理後の強度保持率が８０％以上であり、高度な耐湿熱性、耐アルカリ性、耐酸性を有する繊維である。特に従来のポリアミド繊維の欠点であった、耐酸性にも優れる点は、素材の汎用性をさらに拡大するものである。 The spun or woolen yarn thus obtained exhibits a strength retention of 50% or more after 1500 minutes of wet heat treatment at 140 ° C., and after 100 hours of treatment in a 10% aqueous sodium hydroxide solution at 70 ° C. Strength retention is 80% or more, and strength retention after treatment for 100 hours in 10% sulfuric acid aqueous solution at 70 ° C. is 80% or more, and is a fiber having high heat resistance, alkali resistance, and acid resistance. . The point which is especially excellent in acid resistance which was a defect of the conventional polyamide fiber further expands the versatility of the material.
また、本発明に用いられるポリアミド繊維は、通常ポリエステル繊維に用いられる分散染料にて染色が可能であり、その堅牢度も実使用に適した耐久性を有している。 In addition, the polyamide fiber used in the present invention can be dyed with a disperse dye usually used for polyester fiber, and its fastness has durability suitable for actual use.
このようにして得られた繊維を、織物、編物、あるいは不織布等の繊維製品に供する。本発明に用いられるポリアミド繊維の初期強度は、２．０ｃＮ／ｄｔｅｘ以上であることが好ましい。これは、本発明のポリアミド繊維の場合には、通常のポリエステル繊維の製造方法に準じた製糸条件に準じて容易に達成できる物性である。本発明に用いられるポリアミド繊維は、耐湿熱性に優れるとはいえ、オートクレーブ処理により強度劣化は免れないが、１４０℃湿熱１５００分の処理後も実用可能レベルを目処とすると、初期強力値が２．０ｃＮ／ｄｔｅｘあれば、最大５０％の強度劣化を受けたとしても、１．０ｃＮ／ｄｔｅｘの残留強度があり、強度的には実用上使用可能な下限レベルに留まることができる。 The fibers thus obtained are used for textile products such as woven fabrics, knitted fabrics, and nonwoven fabrics. The initial strength of the polyamide fiber used in the present invention is preferably 2.0 cN / dtex or more. In the case of the polyamide fiber of the present invention, this is a physical property that can be easily achieved according to the spinning conditions in accordance with the normal method for producing a polyester fiber. Although the polyamide fiber used in the present invention is excellent in moisture and heat resistance, strength degradation is unavoidable due to autoclaving, but the initial strength value is 2. If it is 0 cN / dtex, even if it is subjected to a strength deterioration of 50% at the maximum, there is a residual strength of 1.0 cN / dtex, and the strength can remain at a practically usable lower limit level.
上述のポリアミド繊維からなる繊維製品は任意の製造方法で得ることができる。上記より得られた紡績糸あるいは長繊維を用い、任意の規格での織物・編物を製造し、必要により分散染料にて染色加工を施すことができる。最終的なユニフォームやシーツなどの繊維製品を作製する際には、使用する縫い糸も、本発明の紡績糸あるいは長繊維より作成した縫い糸を用いることが好ましい。なぜなら、生地自体の耐湿熱性が優れていても、縫い糸が強度劣化してしまうと、繊維製品が各パーツごとにバラバラになってしまう場合があるからである。 A fiber product made of the above-mentioned polyamide fiber can be obtained by any production method. Using the spun yarn or long fiber obtained as described above, a woven fabric or knitted fabric according to any standard can be produced, and if necessary, dyed with a disperse dye. When producing a final fiber product such as a uniform or a sheet, it is preferable to use a sewing thread produced from the spun yarn or long fiber of the present invention as the sewing thread to be used. This is because, even if the fabric itself has excellent heat and heat resistance, if the sewing thread is deteriorated in strength, the textile product may be separated for each part.
本発明に用いられる繊維製品は、上記したポリアミド繊維１００％で構成されている場合がもっとも好ましいが、一部にそれ以外の繊維が用いられていても良い。
本発明に用いられる繊維製品の具体例としては、病院・介護施設・食品産業・バイオ研究施設等で使用するユニフォームや病院・介護施設等で使用するシーツ、布団カバー、パジャマ、枕カバー、タオル製品などが挙げられる。
The fiber product used in the present invention is most preferably composed of the above-described polyamide fiber 100%, but some other fibers may be used.
Specific examples of the textile products used in the present invention include uniforms used in hospitals, nursing homes, food industries, bio-research facilities, sheets used in hospitals, nursing homes, futon covers, pajamas, pillow covers, towel products Etc.
そして、本発明では、これらのユニフォームやシーツ等は高温高圧蒸気処理により消毒・滅菌処理されるが、高温高圧蒸気処理による消毒・滅菌処理の具体的処理条件としては、１２０〜１４０℃、２〜４気圧で５〜４０分処理する方法が用いられる。 In the present invention, these uniforms, sheets and the like are sterilized and sterilized by high-temperature and high-pressure steam treatment. Specific treatment conditions for disinfection and sterilization by high-temperature and high-pressure steam treatment are 120 to 140 ° C., 2 to 2 A method of treating at 4 atm for 5 to 40 minutes is used.
本発明の繊維製品は、高温高圧蒸気処理により消毒・滅菌処理において劣化が低いことから、このような高温高圧蒸気処理により消毒・滅菌処理される繊維製品として適している。 The textile product of the present invention is suitable as a textile product to be sterilized and sterilized by such a high-temperature and high-pressure steam treatment because the degradation is low in the sterilization and sterilization treatment by the high-temperature and high-pressure steam treatment.
以下、実施例により本発明を詳述するが、本発明はこれら実施例により何等限定されるものではない。なお、実施例中の測定値は以下の方法により測定した値である。
（１）繊維の強度（ｃN／ｄｔｅｘ）
ＪＩＳ Ｌ １０１３の方法に準拠して測定した。
（２）強度保持率
繊維の初期強度をＡ１、処理後の残留強度をＡ２として、強度保持率Ｋ（％）は、下記式にて表される。なお、繊維は任意の２０本を抜き出し、それぞれの強度を測定し、その平均値を用いた。
Ｋ＝｛（Ａ１−Ａ２）／Ａ１｝×１００ （％）
EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited at all by these Examples. In addition, the measured value in an Example is a value measured with the following method.
(1) Fiber strength (cN / dtex)
It measured based on the method of JISL1013.
(2) Strength retention rate Assuming that the initial strength of the fiber is A1 and the residual strength after treatment is A2, the strength retention rate K (%) is expressed by the following formula. In addition, 20 arbitrary fibers were extracted, each strength was measured, and the average value was used.
K = {(A1-A2) / A1} × 100 (%)
（３）１４０℃，１５００分処理後の強度保持率（％）
繊維を１４０℃の飽和水蒸気中に放置した状態で１５００分経過後の繊維の強度を測定し、処理前後の強度の比を求めた。測定した繊維の本数は２０本である。
（４）７０℃，１０％硫酸水溶液処理後の強度保持率（％）
繊維を７０℃の１０重量％濃度の硫酸水溶液中に浸漬し、１００分間放置した後の繊維の強度を測定し、処理前後の強度の比を求めた。測定した繊維の本数は２０本である。
（５）７０℃，１０重量％濃度のＮａＯＨ水溶液処理後の強度保持率（％）
繊維を７０℃の１０％濃度のＮａＯＨ水溶液中に浸漬し、１００分間放置した後の繊維の強度を測定し、処理前後の強度の比を求めた。測定した繊維の本数は２０本である。
（６）洗濯堅牢度
ＪＩＳ Ｌ０８４４Ｂ−１号の方法に準じて測定した。
(3) Strength retention after treatment at 140 ° C for 1500 minutes (%)
The strength of the fiber after 1500 minutes was measured in a state where the fiber was left in saturated steam at 140 ° C., and the strength ratio before and after the treatment was determined. The number of fibers measured is 20.
(4) Strength retention after treatment at 70 ° C and 10% sulfuric acid aqueous solution (%)
The fiber was immersed in a sulfuric acid aqueous solution having a concentration of 10% by weight at 70 ° C. and allowed to stand for 100 minutes. The number of fibers measured is 20.
(5) Strength retention (%) after treatment with a 10% by weight NaOH aqueous solution at 70 ° C.
The fiber was immersed in a 10% NaOH aqueous solution at 70 ° C. and allowed to stand for 100 minutes, and the strength of the fiber was measured to determine the ratio of strength before and after treatment. The number of fibers measured is 20.
(6) Fastness to washing Measured according to the method of JIS L0844B-1.
実施例１
［ポリマーの調製］
テレフタル酸１９．５モル、１，９−ノナンジアミン１０モル、２−メチル−１，８−オクタンジアミン１０モル、安息香酸１．０モル、次亜リン酸ナトリウム−水和物（原料に対して０．１重量％）および蒸留水２．２リットルを、内容積２０リットルのオ−トクレ−ブに添加し、窒素置換を行った。ついで１００℃で３０分間撹拌し、２時間かけて内温を２１０℃に昇温した。この時、オ−トクレ−ブは２２ｋｇ／ｃｍ2まで昇圧した。そのまま１時間反応を続けた後、２３０℃に昇温し、その後２時間、２３０℃に保ち、水蒸気を徐々に抜いて圧力を２２ｋｇ／ｃｍ2 に保持しながら反応を続けた。次に、３０分かけて圧力を１０ｋｇ／ｃｍ2 まで下げ、さらに１時間反応を続けてプレポリマ−を得た。このプレポリマ−を１００℃、減圧下で１２時間乾燥し、２ｍｍ以下の大きさまで粉砕した。粉砕物を２３０℃、０．１ｍｍＨｇ下にて１０時間固相重合することに極限粘度０．９のポリマーを得た。このポリマーの〔ＣＯＮＨ／ＣＨ2 〕の比は１／４であり、末端封止率は９０％である。
Example 1
[Preparation of polymer]
19.5 mol of terephthalic acid, 10 mol of 1,9-nonanediamine, 10 mol of 2-methyl-1,8-octanediamine, 1.0 mol of benzoic acid, sodium hypophosphite-hydrate (0 relative to the raw material) 0.1 wt.%) And 2.2 liters of distilled water were added to an autoclave having an internal volume of 20 liters to perform nitrogen substitution. Subsequently, the mixture was stirred at 100 ° C. for 30 minutes, and the internal temperature was raised to 210 ° C. over 2 hours. At this time, the autoclave was pressurized to 22 kg / cm 2 . The reaction was continued for 1 hour, then the temperature was raised to 230 ° C., and then maintained at 230 ° C. for 2 hours. The reaction was continued while gradually removing water vapor and maintaining the pressure at 22 kg / cm 2 . Next, the pressure was reduced to 10 kg / cm 2 over 30 minutes, and the reaction was continued for another hour to obtain a prepolymer. The prepolymer was dried at 100 ° C. under reduced pressure for 12 hours and pulverized to a size of 2 mm or less. A polymer having an intrinsic viscosity of 0.9 was obtained by subjecting the pulverized product to solid phase polymerization at 230 ° C. and 0.1 mmHg for 10 hours. This polymer has a [CONH / CH 2 ] ratio of 1/4 and a terminal blocking ratio of 90%.
［製糸］
上記ポリマーを、スクリュー型溶融押し出し機を用いて３００℃にて押し出し、０．２５φｍｍの孔が２４個穿孔された口金ノズルより紡出し、２５００ｍ／分で巻き取った後、予熱温度９３℃、延伸倍率２．５倍で延伸しつつ１６０℃接触プレートヒーターに接した後巻取り、８６ｄｔｅｘ、２４フィラメントの長繊維を得た。強度は４．２ｃＮ／ｄｔｅｘ、伸度は３１％であった。本長繊維を、１８０℃のプレート温度にて常法のフリクションディスク型仮撚加工を施し、強度３．８ｃＮ／ｄｔｅｘ，伸度２５％のウーリー加工糸を得た。この加工糸をポリエステル繊維用の分散染料を用いてネイビーブルー色に染色した。
[Yarn making]
The polymer was extruded at 300 ° C. using a screw-type melt extruder, spun from a nozzle nozzle having 24 holes of 0.25 mm, wound at 2500 m / min, and then preheated at 93 ° C. and stretched. The film was wound after contacting with a 160 ° C. contact plate heater while stretching at a magnification of 2.5 times to obtain 86 dtex, 24 filament long fibers. The strength was 4.2 cN / dtex and the elongation was 31%. This long fiber was subjected to a conventional friction disk type false twisting process at a plate temperature of 180 ° C. to obtain a wooly processed yarn having a strength of 3.8 cN / dtex and an elongation of 25%. This processed yarn was dyed in a navy blue color using a disperse dye for polyester fiber.
比較例１：ポリエチレンテレフタレート繊維からなるウーリー加工糸
（株）クラレ製のポリエチレンテレフタレート繊維からなるウーリー加工糸（銘柄CT１２０）、８４ｄｔｅｘ，２４フィラメントを用いた。実施例１と同様の染色を行った。
Comparative Example 1: Woolened yarn made of polyethylene terephthalate fiber Wooly yarn (brand name CT120) made of polyethylene terephthalate fiber manufactured by Kuraray Co., Ltd., 84 dtex, 24 filament was used. The same dyeing as in Example 1 was performed.
比較例２：ポリブチレンテレフタレート繊維からなるウーリー加工糸
市販のポリブチレンテレフタレート樹脂（ポリプラスチック株式会社製）を用い、紡糸温度２６０℃にて０．２５φｍｍの孔が２４個穿孔された口金ノズルより紡出し、５００ｍ／分で巻き取った後、予熱温度６５℃、延伸倍率２．７倍で延伸しつつ１２０℃接触プレートヒーターに接した後巻取り、８４ｄｔｅｘ、２４フィラメントの長繊維を得た。強度は３．１ｃＮ／ｄｔｅｘ、伸度は４２％であった。本長繊維を、１５０℃のプレート温度にて常法のフリクションディスク型仮撚加工を施し、強度３．３ｃＮ／ｄｔｅｘ，伸度３６％のウーリー加工糸を得た。実施例１と同様の染色を行った。
Comparative Example 2: Woolen-processed yarn made of polybutylene terephthalate fiber A commercially available polybutylene terephthalate resin (manufactured by Polyplastics Co., Ltd.) was used and spun from a nozzle nozzle having 24 holes of 0.25 mm at a spinning temperature of 260 ° C. After being wound and wound at 500 m / min, it was wound at a preheating temperature of 65 ° C. and stretched at a stretching ratio of 2.7 times and then contacted with a 120 ° C. contact plate heater to obtain 84 dtex, 24 filament long fibers. The strength was 3.1 cN / dtex, and the elongation was 42%. This long fiber was subjected to a conventional friction disk type false twisting process at a plate temperature of 150 ° C. to obtain a wooly processed yarn having a strength of 3.3 cN / dtex and an elongation of 36%. The same dyeing as in Example 1 was performed.
比較例３：ポリトリメチレンテレフタレート繊維からなるウーリー加工糸
市販のポリトリメチレンテレフタレート樹脂（シェルジャパン株式会社製）を用い、紡糸温度２６０℃にて０．２５φｍｍの孔が２４個穿孔された口金ノズルより紡出し、１０００ｍ／分で巻き取った後、予熱温度７０℃、延伸倍率３．０倍で延伸しつつ１２０℃接触プレートヒーターに接した後巻取り、８５ｄｔｅｘ、２４フィラメントの長繊維を得た。強度は２．９ｃＮ／ｄｔｅｘ、伸度は４７％であった。本長繊維を、１５０℃のプレート温度にて常法のフリクションディスク型仮撚加工を施し、強度３．２ｃＮ／ｄｔｅｘ，伸度４５％のウーリー加工糸を得た。実施例１と同様の染色を行った。
Comparative Example 3: Woolley-processed yarn made of polytrimethylene terephthalate fiber A nozzle made of a commercially available polytrimethylene terephthalate resin (manufactured by Shell Japan Co., Ltd.) and having 24 holes of 0.25φmm at a spinning temperature of 260 ° C. After spinning and winding at 1000 m / min, it was wound at a preheating temperature of 70 ° C. and stretched at a draw ratio of 3.0, and then contacted with a 120 ° C. contact plate heater to obtain a long fiber of 85 dtex and 24 filaments. . The strength was 2.9 cN / dtex, and the elongation was 47%. This long fiber was subjected to a conventional friction disk type false twisting process at a plate temperature of 150 ° C. to obtain a wooly processed yarn having a strength of 3.2 cN / dtex and an elongation of 45%. The same dyeing as in Example 1 was performed.
比較例４：ナイロン６繊維からなるウーリー加工糸
宇部興産製のナイロン６チップを用いて通常の溶融紡糸方法によりナイロンウーリー加工糸（８５ｄｔｅｘ−２４フィラメント）を得た。
Comparative Example 4: Woolened yarn made of nylon 6 fiber A nylon woolened yarn (85 dtex-24 filament) was obtained by a conventional melt spinning method using a nylon 6 chip manufactured by Ube Industries.
実施例２
実施例１において、２−メチル−１，８−オクタンジアミン１０モルの全量を１，９−ノナンジアミン１０モルに置き換える以外は、同一の方法により、ジカルボン酸単位がテレフタル酸、ジアミン単位が１，９−ノナンジアミンであり、末端の９０％が安息香酸により封鎖された極限粘度が０．９５であるポリアミド樹脂を製造した。このポリマーの〔ＣＯＮＨ／ＣＨ2 〕の比は１／４．５である。得られたポリアミド樹脂を口金温度を２０℃ほど実施例１より高める以外は実施例１と同様にして、８６ｄｔｅｘ、２４フィラメントの長繊維を得た。
強度は４．４ｃＮ／ｄｔｅｘ、伸度は２８％であった。本長繊維を、１８０℃のプレート温度にて常法のフリクションディスク型仮撚加工を施し、強度４．０ｃＮ／ｄｔｅｘ，伸度２３％のウーリー加工糸を得た。
Example 2
In Example 1, except that the total amount of 10 moles of 2-methyl-1,8-octanediamine was replaced with 10 moles of 1,9-nonanediamine, the same method was used, but the dicarboxylic acid unit was terephthalic acid and the diamine unit was 1,9. -A polyamide resin having an intrinsic viscosity of 0.95, which was nonanediamine and 90% of the ends blocked with benzoic acid, was produced. The [CONH / CH 2 ] ratio of this polymer is 1 / 4.5. A 86 dtex, 24-filament long fiber was obtained in the same manner as in Example 1 except that the base temperature of the obtained polyamide resin was increased from Example 1 by about 20 ° C.
The strength was 4.4 cN / dtex and the elongation was 28%. This long fiber was subjected to a conventional friction disk type false twisting process at a plate temperature of 180 ° C. to obtain a wooly processed yarn having a strength of 4.0 cN / dtex and an elongation of 23%.
表１に、本発明のポリアミド繊維の実施例と各比較例との強度保持率を示す。本発明のポリアミド繊維は、高温高圧処理に対して良好な強度保持性を示し、また、アルカリ・酸両方についても劣化の進行が極めて少ないことが分かる。一般にポリアミド繊維は、アルカリ性には良好な耐久性を示すものの、酸性条件下では容易に劣化が進行するが、本発明のポリアミド繊維は、耐酸性に優れる利点を有している。また、汎用のポリエステルと同様に分散染色にて染色可能であり、堅牢度も同等である。 Table 1 shows the strength retention of the polyamide fiber examples of the present invention and the comparative examples. It can be seen that the polyamide fiber of the present invention exhibits good strength retention with respect to high-temperature and high-pressure treatment, and the deterioration of both alkali and acid is extremely small. In general, the polyamide fiber exhibits good durability in terms of alkalinity, but easily deteriorates under acidic conditions, but the polyamide fiber of the present invention has an advantage of excellent acid resistance. Moreover, it can be dyed by disperse dyeing similarly to general-purpose polyester, and fastness is equivalent.
以上の実施例および比較例の加工糸を経糸および緯糸として用いてそれぞれ織物を作製し、これらの織物を１．２ｍ×２．４ｍのシーツに仕上げた。その際の縫い糸として、それぞれの実施例および比較例で使用した繊維と同一の繊維からなる糸を使用した。このシーツを病院のベッド用のシーツとして３日間使用した後、１３１℃、２．７気圧で１０分間の加熱加圧蒸気滅菌処理を行い、そして、通常のアニオン系の洗剤で洗濯乾燥させた後、アイロン掛けして、再度病院のベッドのシーツとして使用するリユースを１５回繰り返した。その結果、繊維の強度保持率を表２に示す。 Fabrics were produced using the processed yarns of the above examples and comparative examples as warps and wefts, respectively, and these fabrics were finished into sheets of 1.2 m × 2.4 m. As a sewing thread at that time, a thread made of the same fiber as that used in each of Examples and Comparative Examples was used. After using this sheet as a hospital bed sheet for 3 days, it was subjected to heat and pressure steam sterilization at 131 ° C. and 2.7 atm for 10 minutes, and after washing and drying with a normal anionic detergent. The iron was used and reused as a hospital bed sheet was repeated 15 times. As a result, the fiber strength retention is shown in Table 2.
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