JP7327694B2 - 立体網状構造体の製造方法 - Google Patents
立体網状構造体の製造方法 Download PDFInfo
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- D04H13/00—Other non-woven fabrics
- D04H13/001—Making non-woven fabrics from staple fibres, filaments or yarns, bonded to at least one web-like material, e.g. woven, knitted non-woven fabric, paper, leather, during consolidation
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
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- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47C—CHAIRS; SOFAS; BEDS
- A47C27/00—Spring, stuffed or fluid mattresses or cushions specially adapted for chairs, beds or sofas
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- D04H1/43914—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece characterised by the shape of the fibres hollow fibres
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- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
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- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
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- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
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Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Artificial Filaments (AREA)
- Materials For Medical Uses (AREA)
- Biological Depolymerization Polymers (AREA)
Description
[1]見かけ密度が0.005g/cm3~0.30g/cm3であり、
厚みが10mm~100mmであり、
線状繊維を含み、前記線状繊維は、繊維径が0.2mm~2.0mmであり、結晶融解エンタルピーが16J/g以上であり、重量平均分子量が35000以上のポリブチレンアジペートテレフタレート系樹脂を含むことを特徴とする生分解性の立体網状構造体。
[2]前記線状繊維は、三次元ランダムループ構造を形成している[1]に記載の生分解性の立体網状構造体。
[3]前記結晶融解エンタルピーが30J/g以下である[1]または[2]に記載の生分解性の立体網状構造体。
[4]クッションに用いられるものである[1]~[3]のいずれかに記載の生分解性の立体網状構造体。
[5]前記ポリブチレンアジペートテレフタレート系樹脂の重量平均分子量は、150000以下である[1]~[4]のいずれかに記載の生分解性の立体網状構造体。
[6]前記線状繊維は、融点が100℃以上、120℃以下である[1]~[5]のいずれかに記載の生分解性の立体網状構造体。
[7]前記線状繊維は、中空断面形状を有している[1]~[6]のいずれかに記載の生分解性の立体網状構造体。
[8]前記線状繊維の中空率は、1%以上、30%以下である[7]に記載の生分解性の立体網状構造体。
[9]前記線状繊維の中空率は、2%以上、25%以下である[7]に記載の生分解性の立体網状構造体。
[10]前記結晶融解エンタルピーが17J/g以上である[1]~[9]のいずれかに記載の生分解性の立体網状構造体。
[11]前記結晶融解エンタルピーが28J/g以下である[1]~[10]のいずれかに記載の生分解性の立体網状構造体。
[12]前記ポリブチレンアジペートテレフタレート系樹脂の重量平均分子量は、37000以上である[1]~[11]のいずれかに記載の生分解性の立体網状構造体。
[13]前記ポリブチレンアジペートテレフタレート系樹脂の重量平均分子量は、120000以下である[1]~[12]のいずれかに記載の生分解性の立体網状構造体。
立体網状構造体の含水率(%)={(真空乾燥前の立体網状構造体の質量)―(真空乾燥後の立体網状構造体の質量)}/(真空乾燥前の立体網状構造体の質量)×100
立体網状構造体を10cm×10cmの大きさに切断し、それぞれ10箇所から線状繊維を約5mmの長さで採集した。次いで、光学顕微鏡を用いて採集した線状繊維の繊維径測定箇所にピントを合わせて径を測定し、10箇所の繊維径の平均値(n=10)を求めた。
立体網状構造体からランダムに10本の線状繊維を取り出した。次いで線状繊維を輪切りにし、繊維軸方向に立てた状態でスライドガラスに載せ、光学顕微鏡で輪切り方向の繊維断面を観察した。この際、繊維断面が中空断面である線状繊維のみを選択し、繊維の外周線内の面積(a)と中空面積(b)をそれぞれ算出し、下記式に基づいて中空率を算出し、選択した中空線状繊維の中空率の平均値を求めた。
中空率(%)=(b)/(a)×100
立体網状構造体を縦横方向に10cm×10cmの大きさに切断し、得られた試料を無荷重で24時間放置した後、高分子計器株式会社製の高分子計器製FD-80N型測厚器にて中心1か所の高さを測定し、その試料の高さを立体網状構造体の厚みとした。更に、試料を電子天秤に載せて試料重さを計測した。試料の高さと縦横の面積(100cm2)を乗じて試料の体積を求め、試料の重さを体積で除して、見かけ密度を求めた。当該操作を3回行って、立体網状構造体の厚みと、見かけ密度との平均値(n=3)を求めた。
TAインスツルメント社製の示差走査熱量計Discovery DSC25を用い、立体網状構造体からサンプルを採取し、サンプル質量は2.0mg±0.1mgに秤量し、昇温速度20℃/分、窒素雰囲気下の条件で測定した吸発熱曲線から、吸熱ピーク(融解ピーク)温度を求めた。当該操作を3回行って、融点の平均値(n=3)を求めた。
立体網状構造体からサンプルを採取し、サンプル質量は2.0mg±0.1mgに秤量し、TAインスツルメント社製の示差走査熱量計Discovery DSC25を用い、昇温速度20℃/分、窒素雰囲気下の条件で測定した吸発熱曲線から吸熱ピーク(融解ピーク)の積分値から結晶融解エンタルピー(J/g)を求めた。詳細には、吸熱ピーク(融解ピーク)の積分値は、当該吸熱ピーク(融解ピーク)に係る曲線が低温側のベースラインから離れ始める点を開始点とし、高温側のベースラインに接し始める点を終了点とし、当該開始点と終了点と結ぶ直線を引き、当該直線と曲線により囲まれた部分について積分することにより求めた。当該操作を3回行って、結晶融解エンタルピーの平均値(n=3)を求めた。また上記開始点を融解開始オンセット温度(℃)とした。
立体網状構造体を細かく切り刻んで原料とし、80℃で2時間以上、真空乾燥した後に、空気中の水分を出来るだけ含まないように、手早くメルトフローレート(MFR)測定を実施した。東洋精機製作所社製のメルトインデックサ F-F01機を用いて、ISO1133に準拠してメルトフローレートの測定を行った。測定温度は190℃、荷重は2.16kgとした。当該操作を3回行って、メルトフローレートの平均値(n=3)を求めた。
立体網状構造体からサンプルを採取し、試料のばらつきを軽減するため、試料は通常の10倍の40mgを細かく裁断し、溶解させた。試料溶液を、クロロホルムで希釈して試料濃度を0.05%に調製した。0.2μmのメンブランフィルターでろ過し、得られた試料溶液のGPC分析を以下の条件で実施した。分子量は標準ポリスチレン換算で算出した。
装置:TOSOH HLC-8320GPC
カラム:TSKgel SuperHM-H×2+TSKgel SuperH2000(TOSOH)
溶媒:クロロホルム
流速:0.6ml/min
濃度:0.05%
注入量:20μL
温度:40℃
検出器:RI, UV254nm
(8)70℃圧縮残留歪み
立体網状構造体を10cm×10cmの大きさに切断し、得られた試料について上記(2)に記載の方法で処理前の厚み(c)を測定した。厚みを測定したサンプルを50%圧縮状態に保持できる冶具に挟み、70℃に設定した乾燥機に入れて22時間放置した。その後、サンプルを取り出し、冷却して圧縮歪みを除いて30分放置した後の厚み(d)を求めた。これらの厚みを、{(c)-(d)}/(c)×100の式に当てはめて70℃圧縮残留歪みを求めた。当該操作を3回行って、70℃圧縮残留歪みの平均値(n=3)を求めた。
立体網状構造体を10cm×10cmの大きさに切断し、得られた試料を23℃±2℃の環境下に無荷重で24時間放置した。次いで、23℃±2℃の環境下で島津製作所製オートグラフ AG-X plusを用いて、ISO2439(2008)E法に準拠して計測した。具体的には、直径(φ)50mmの加圧板を試料の中心位置に配置して、荷重が0.5Nになったときの厚みを計測し、それを初期厚みとした。このときの加圧板の位置をゼロ点として、速度100mm/分で初期厚みの75%まで予備圧縮を1回行い、同じ速度で加圧板をゼロ点まで戻した後、そのままの状態で4分間放置した。その後、即座に速度100mm/分で初期厚みの25%まで圧縮を行って、その際の荷重を測定し、その加重を25%圧縮時硬度(N/φ50mm)とした。当該操作を3回行って、25%圧縮時硬度の平均値(n=3)を求めた。
溶融樹脂を吐出用のノズルのノズル面より17cm下に冷却水面が位置するように水槽を配置し、水温12℃とし、水槽内に一対の引取りコンベアを水面上に一部が出るように配置した。引取りコンベアは幅20cmのステンレス製エンドレスネットを有しており、ノズル面の幅方向とコンベアを平行に配置し、エンドレスネットの開口幅を30mmとし、側面部を成形するためにアルミ板をネット方向に対して90度の向きで配置させ水を1.0L/分の速度で流し側面部とした。
樹脂の固形分100質量%に対して仕込み量0.30質量%で水を加えたこと、外径5.0mm、内径4.4mmでトリプルブリッジの中空形成断面のオリフィスを孔間ピッチ8mmの千鳥配列で形成したノズルを用いて、紡糸温度を231℃、単孔吐出量を1.5g/分、引き取り速度を0.92m/分、乾燥温度を105℃にしたこと以外は、実施例1と同様にして立体網状構造体得た。当該立体網状構造体の線状繊維の断面形状は中空形状であった。
樹脂の固形分100質量%に対して仕込み量0.40質量%で水を加えたこと、紡糸温度を230℃、乾燥温度を90℃にしたこと以外は、実施例2と同様にして立体網状構造体を得た。
樹脂の固形分100質量%に対して仕込み量0.01質量%で水を加えたこと、紡糸温度を240℃、ノズル面-冷却水距離を25cmにしたこと以外は、実施例3と同様にして立体網状構造体を得た。
原料である樹脂を乾燥させた後に水を加え無かったこと、単孔吐出量を0.5g/分、引き取り速度を0.64m/分にしたこと以外は、実施例1と同様にして立体網状構造体を得た。
樹脂の固形分100質量%に対して仕込み量0.20質量%で水を加えたこと、紡糸温度を190℃、ノズル面-冷却水距離を30cmとしたこと以外は、実施例3と同様にして立体網状構造体を得た。
紡糸温度を210℃、単孔吐出量を1.0g/分、引き取り速度を1.28m/分にしたこと以外は、実施例5と同様にして網状構造体を得た。
樹脂の固形分100質量%に対して水2.5質量%を加えたこと、単孔吐出量を0.9g/分、ノズル面-冷却水距離を18cm、引き取り速度を0.52m/分にしたこと以外は、実施例1と同様にして立体網状構造体を得た。
樹脂の固形分100質量%に対して仕込み量0.02質量%で水を加えたこと、アニーリングを行わずに乾燥を20~25℃で2日間行ったこと以外は、実施例4と同様にして立体網状構造体を得た。
紡糸温度を230℃、引き取り速度を1.54m/分、乾燥温度を107℃にしたこと以外は、実施例2と同様にして網状構造体を得た。
Claims (4)
- ポリブチレンアジペートテレフタレート樹脂の固形分100質量%に対して0.005質量%以上2.0質量%以下の仕込み量で水を前記ポリブチレンアジペートテレフタレート樹脂に加える工程、
前記ポリブチレンアジペートテレフタレート樹脂を該樹脂の融点+20℃以上、融点+180℃未満の紡糸温度でノズルより下方に向け吐出する工程、
溶融状態で吐出された連続線状体を互いに融着して3次元網状構造体を形成しつつ、水面が前記ノズルのノズル面から15cm以上、40cm以下の距離離れている冷却槽中の冷却水に前記3次元網状構造体入れる工程、及び
得られた前記3次元網状構造体に対して70℃以上、105℃以下の条件でアニーリング処理を行う工程を含み、
前記アニーリング処理後の前記連続線状体は、結晶融解エンタルピーが16J/g以上、30J/g以下であり、重量平均分子量が35000以上、150000以下のポリブチレンアジペートテレフタレート樹脂を、前記連続線状体100質量%中、98質量%以上の含有量で含み、
前記ポリブチレンアジペートテレフタレート樹脂は、全成分100モル%中、アジピン酸成分、テレフタル酸成分、及びブタンジオール成分を合計99モル%以上の量で含むことを特徴とする立体網状構造体の製造方法。 - 前記アニーリング処理後の前記連続線状体は、融点が100℃以上、120℃以下である請求項1に記載の立体網状構造体の製造方法。
- 前記アニーリング処理後の前記連続線状体は、中空断面形状を有している請求項1または2に記載の立体網状構造体の製造方法。
- 前記アニーリング処理後の前記連続線状体は、中空率が1%以上、30%以下である請求項3に記載の立体網状構造体の製造方法。
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