JP4224820B2 - ポリウレタン糸およびその製造方法 - Google Patents
ポリウレタン糸およびその製造方法 Download PDFInfo
- Publication number
- JP4224820B2 JP4224820B2 JP2004097860A JP2004097860A JP4224820B2 JP 4224820 B2 JP4224820 B2 JP 4224820B2 JP 2004097860 A JP2004097860 A JP 2004097860A JP 2004097860 A JP2004097860 A JP 2004097860A JP 4224820 B2 JP4224820 B2 JP 4224820B2
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- JP
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- Prior art keywords
- polyurethane
- yarn
- cellulose ester
- solution
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000004814 polyurethane Substances 0.000 title claims description 127
- 238000004519 manufacturing process Methods 0.000 title claims description 11
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- 229920002678 cellulose Polymers 0.000 claims description 41
- 238000009987 spinning Methods 0.000 claims description 29
- 239000000126 substance Substances 0.000 claims description 23
- 229920005862 polyol Polymers 0.000 claims description 22
- 150000003077 polyols Chemical class 0.000 claims description 22
- 239000010419 fine particle Substances 0.000 claims description 19
- 125000005442 diisocyanate group Chemical group 0.000 claims description 14
- 229910010272 inorganic material Inorganic materials 0.000 claims description 9
- 239000011147 inorganic material Substances 0.000 claims description 8
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- 229920006217 cellulose acetate butyrate Polymers 0.000 claims description 5
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- 239000000470 constituent Substances 0.000 claims description 4
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- 239000000243 solution Substances 0.000 description 49
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- 239000004744 fabric Substances 0.000 description 20
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 9
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- 239000002994 raw material Substances 0.000 description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- QCOGKXLOEWLIDC-UHFFFAOYSA-N N-methylbutylamine Chemical compound CCCCNC QCOGKXLOEWLIDC-UHFFFAOYSA-N 0.000 description 4
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 4
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- 238000010528 free radical solution polymerization reaction Methods 0.000 description 4
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 4
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- 229920000166 polytrimethylene carbonate Polymers 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
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- 238000002845 discoloration Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 150000002334 glycols Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920003226 polyurethane urea Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 description 2
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- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
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- 125000003277 amino group Chemical group 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
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- 239000011324 bead Substances 0.000 description 2
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- 125000002091 cationic group Chemical group 0.000 description 2
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- 150000001880 copper compounds Chemical class 0.000 description 2
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
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Description
すなわち、主構成成分がポリオール及びジイソシアネートであるポリウレタンからなる弾性糸であって、かつ、セルロースエステルおよび微粒子状無機物を含有し、前記セルロースエステルがセルロースアセテートブチレートを主成分とするものであり、前記微粒子状無機物がカーボン微粒子であることを特徴とするポリウレタン糸である。
まず本発明で使用するポリウレタンについて述べる。
ポリウレタンを構成する重合原料構成成分として、本発明で使用されるポリオールとしては、ポリエーテル系グリコール、ポリエステル系グリコール、ポリカーボネートジオール等が好ましい。そして、特に柔軟性、伸度を糸に付与する観点からポリエーテル系グリコールが使用されることが好ましい。
なお、これらの含有量は、ポリウレタン糸の用途に応じて適宜決定すればよい。
本発明におけるポリウレタン弾性糸のセット性、応力緩和、強度、伸度、ヒートセット性、熱軟化点の測定法を説明する。
セット性、応力緩和、強度、伸度は、ポリウレタン糸を“インストロン”4502型引張試験機を用い、引張テストすることにより測定した。
試長5cm(L1)の試料を50cm/分の引張速度で300%伸長し回復させる操作を5回繰返した。このとき、5回目の300%伸長時の応力を(G1)とした。次に試料の長さを300%伸長のまま30秒間保持し、30秒間保持後の応力を(G2)とした。次に試料の伸長を回復せしめ応力が0になった際の試料の長さを(L2)とした。さらに6回目に試料が切断するまで伸長し、この破断時の応力を(G3)、破断時の試料長さを(L3)とした。以下、上記特性は下記式により算出される。
応力緩和=100×((G1)−(G2))/(G1)
セット性=100×((L2)−(L1))/(L1)
伸度=100×((L3)−(L1))/(L1)
ヒートセット性は、下記により測定した。
試料糸をフリーで100℃のスチームで10分間処理し、次にフリーで100℃の沸騰水で2時間処理し、一日、室温で乾燥した。つぎに試料糸(長さ=(L5))を150%伸長した(長さ=2.5×(L5))。この長さのまま115℃のスチームで、1分間処理した。さらに同長さで、120℃の乾熱処理を施し、さらに同長さで、1日室温で放置した。次に、試料糸の伸長状態をはずし、その長さ(L6)を測定した。ヒートセット性の値は下記式により算出される。
ヒートセット性=100×((L6)−(L5))/(L5)
ポリウレタン糸の耐熱性の指標として熱軟化点を測定した。ポリウレタン糸について、レオメトリック社製の動的弾性率測定機RSAIIを用い、昇温速度10℃/分で、動的貯蔵弾性率E’の温度分散を測定した。熱軟化点は、E’曲線が80℃以上130℃以下のプラト領域での接線と、160℃以上にてE’が熱軟化により降下するE’曲線の接線との交点から求めた。
スラリー中の微粒子の平均粒子径は、(株)堀場製作所製のレーザー回折式粒度分布測定装置LA−500型を用いて測定した。また、微粒子状無機物の平均一次粒子径は、電子顕微鏡EF−SEM法を用いて測定した。
ストレッチ布帛を、染色加工、乾燥、仕上げ剤処理、及び仕上げセットという一連の工程を2回繰り返し通過させた。ここで、染色加工は、カチオン染料、120℃の条件で行い、仕上げセットは、180℃、布速20m/min、セットゾーン24mの条件で行なった。
このように染色等の後加工を行なった後のストレッチ布帛の外観品位を、 主に生地の波打ちに注目して、生地を1.8kg/2インチの荷重下で伸長した状態で観察し、次の5段階に判定することにより評価した。
分子量2900のPTMG、MDIおよびエチレングリコールからなるポリウレタン重合原料のDMAC溶液(35重量%)を常法により重合し、ポリマ溶液A1とした。
分子量1800のPTMG、MDI、エチレンジアミン、および末端封鎖剤としてのジエチルアミンからなるポリウレタンウレア重合原料のDMAc溶液(35重量%)を常法により重合し、ポリマ溶液A2とした。
実施例1で調製したセルロースエステル溶液B1に対し、微粒子状無機物として酸化亜鉛微粒子(ニュージャージー・ジンクカンパニー社製、商品名“カドックス”(登録商標)−15)を、さらにDMAcを添加し、酸化亜鉛微粒子とセルロースエステルを含有したスラリーC3を調製した。この調製は、比較例3と同一方法で行った。得られたスラリーC3中には、(酸化亜鉛24.5重量%、セルロースエステル10.5重量%、(それら合計35重量%)が含有されていた。
実施例1で調製したポリマ溶液A1、及び添加剤溶液D1を、それぞれ、98重量%、2重量%の割合で均一に混合し、紡糸溶液F1とした。この紡糸溶液F1を、ゴデローラーと巻取機の速度比を1.40として540m/分の紡糸速度で乾式紡糸して巻取ることにより、18dtexのモノフィラメントのポリウレタン弾性糸を製造した。
次に得られたポリウレタン弾性糸を用いて、実施例1と同様にしてストレッチ布帛を製作し、染色等の後加工を行なった後に、その外観品位を評価した。これの外観品位は1級であり、波打ちがある不満足な結果であった。
比較例3で調製したポリマ溶液A2、及び実施例1で調整した添加剤溶液D1を、それぞれ、98重量%、2重量%の割合で均一に混合し、紡糸溶液F2とした。この紡糸溶液F2を、ゴデローラーと巻取機の速度比を1.20として600m/分の紡糸速度で乾式紡糸して巻取ることにより、20dtexのマルチフィラメント(2fil)のポリウレタン弾性糸(500g巻糸体)を製造した。
次に得られたポリウレタン弾性糸を用いて、実施例1と同様にしてストレッチ布帛を製作し、染色等の後加工を行なった後に、その外観品位を評価した。これの外観品位は2級であり、波打ちが気になる不満足な結果であった。
Claims (7)
- 主構成成分がポリオール及びジイソシアネートであるポリウレタンからなる弾性糸であって、セルロースエステルおよび微粒子状無機物を含有し、前記セルロースエステルがセルロースアセテートブチレートを主成分とするものであり、前記微粒子状無機物がカーボン微粒子であることを特徴とするポリウレタン糸。
- 前記微粒子状無機物の含有量が0.5重量%以上50重量%以下であることを特徴とする請求項1に記載のポリウレタン糸。
- 前記微粒子状無機物の平均一次粒子径が0.01μm〜10μmであることを特徴とする請求項1または2に記載のポリウレタン糸。
- 前記セルロースエステルおよび前記微粒子状無機物の含有量の合計が1重量%以上50重量%以下であることを特徴とする請求項1〜3のいずれかに記載のポリウレタン糸。
- 主構成成分がポリオール及びジイソシアネートであるポリウレタンの溶液に、セルロースエステルおよび微粒子状無機物を添加し、その後、該溶液を紡糸するポリウレタン糸の製造方法であって、前記セルロースエステルとしてセルロースアセテートブチレートを主成分とするものを用い、前記微粒子状無機物としてカーボン微粒子を用いることを特徴とすることを特徴とするポリウレタン糸の製造方法。
- 紡糸方法が乾式であることを特徴とする請求項5に記載のポリウレタン糸の製造方法。
- 紡糸速度が450m/分以上であることを特徴とする請求項5または6に記載のポリウレタン糸の製造方法。
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