JP5666837B2 - ナノファイバシート - Google Patents
ナノファイバシート Download PDFInfo
- Publication number
- JP5666837B2 JP5666837B2 JP2010148076A JP2010148076A JP5666837B2 JP 5666837 B2 JP5666837 B2 JP 5666837B2 JP 2010148076 A JP2010148076 A JP 2010148076A JP 2010148076 A JP2010148076 A JP 2010148076A JP 5666837 B2 JP5666837 B2 JP 5666837B2
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- Prior art keywords
- nanofiber
- liquid
- water
- component
- sheet
- 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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Classifications
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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Description
水溶性高分子が水相に溶解しており、かつ油相中に油性成分が含まれているO/Wエマルションを用い、電界紡糸法によって紡糸を行うナノファイバの製造方法を提供するものである。
水溶性高分子が水に溶解してなる第1液と、油性成分を含む第2液とを用い、
電界紡糸法を行うためのキャピラリとして二重管構造のものを用い、該キャピラリの芯部に第2液を流し、かつ鞘部に第1液を流して電界紡糸法を行うナノファイバの製造方法を提供するものである。
(1)第1液の調製
水溶性高分子としてプルラン(林原商事製)を用いた。これを水に溶解させて濃度20%の水溶液を得た。これを第1液として用いた。第1液は80℃に加熱しておいた。
油性成分としてカミツレエキスとセチル−1,3−ジメチルブチルエーテル(花王(株)製のASE166K)の混合物を用いた。この溶液におけるカミツレエキスの濃度は4.20%であった。この溶液に、非イオン界面活性剤であるポリオキシエチレン硬化ヒマシ油(花王(株)製エマノーン(登録商標)CH60)を添加した。この非イオン界面活性剤の濃度は0.3%であった。この溶液0.95mlを80℃に加熱し、そこへ80℃に加熱した4.00mlの水を徐々に添加して混合して転相乳化させた。これによってO/Wエマルションからなる第2液を得た。
第1液と第2液とを質量比で3:1の割合で混合して攪拌し、O/Wエマルションからなる原料液を得た。この原料液における各成分の濃度は、プルラン15.00%、水80.20%、油性成分4.78%、非イオン界面活性剤0.013%であった。
前記で得られた原料液を用い、図2に示す装置によって電界紡糸法を行い、導電性コレクタ33の表面に配置されたポリエチレンテレフタレートフィルム(厚み:25μm)の表面にナノファイバシートを形成した。電界紡糸法の条件は以下のとおりとした。
・印加電圧:25kV
・キャピラリ−コレクタ間距離:185mm
・原料液吐出量:1ml/h
・環境:25℃、50%RH
得られたナノファイバシートにおける各成分の割合は、プルランが75.82%、油性成分が24.11%、界面活性剤が0.07%であった。このナノファイバシートの厚みをライトマチックVL−50A((株)ミツトヨ)で測定したところ30μmであった。また、このナノファイバシートの走査型電子顕微鏡像を図4(a)に示す。更に、第2液に油性の蛍光剤(ナイルレッド)を添加して同条件で電界紡糸法を行い得られたナノファイバシートの蛍光顕微鏡像を図4(b)に示す。図4(b)中、黒い部分が、蛍光剤が存在している部分である。
(1)第1液の調製
実施例1と同様とした。
(2)第2液の調製
油性成分としてシリコーンオイルを用いた。このシリコーンオイルに、非イオン界面活性剤であるポリオキシエチレン硬化ヒマシ油(花王(株)製エマノーン(登録商標)CH60)を添加した。この非イオン界面活性剤の濃度は0.3%であった。このシリコーンオイル0.95mlを80℃に加熱し、そこへ80℃に加熱した4.00mlの水を徐々に添加して混合して転相乳化させた。これによってO/Wエマルションからなる第2液を得た。
(3)原料液の調製
第1液と第2液とを質量比で3:1の割合で混合して攪拌し、O/Wエマルションからなる原料液を得た。この原料液における各成分の濃度は、プルラン15%、水80.2%、油性成分4.787%、非イオン界面活性剤0.013%であった。
(4)電界紡糸法
実施例1と同様とした。
(5)評価
得られたナノファイバシートにおける各成分の割合は、プルランが75.82%、油性成分が24.11%、界面活性剤が0.07%であった。このナノファイバシートの厚みをライトマチックVL−50A((株)ミツトヨ)で測定したところ30μmであった。また、このナノファイバシートの反射電子線像を図5(a)に示す。更に、図5(a)に示す観察視野におけるケイ素及び炭素の分布をEDXによって分析した。その結果を図5(b)及び(c)に示す。図5(a)から明らかなように、本実施例で得られたナノファイバシートにおけるナノファイバは、太径部及び細径部を有することが判る。また図5(b)及び(c)から明らかなように、太径部に中空部を有し、該中空部に油性成分が貯留されていることが判る。つまり本実施例のナノファイバは、図1(a)に示す構造のものであることが判る。
(1)第1液の調製
実施例1と同様とした。
(2)第2液の調製
油性成分としてカミツレエキスを用いた。この溶液に、非イオン界面活性剤であるポリオキシエチレン硬化ヒマシ油(花王(株)製エマノーン(登録商標)CH60)を添加した。この非イオン界面活性剤の濃度は0.3%であった。この溶液1.72mlを80℃に加熱し、そこへ80℃に加熱した2.06mlの水を徐々に添加して混合して転相乳化させた。これによってO/Wエマルションからなる第2液を得た。
(3)原料液の調製
第1液と第2液とを質量比で81:19の割合で混合して攪拌し、O/Wエマルションからなる原料液を得た。この原料液における各成分の濃度は、プルラン16.22%、水75.16%、油性成分8.59%、非イオン界面活性剤0.03%であった。これ以外は実施例1と同様にしてナノファイバシートを得た。得られたナノファイバシートにおける各成分の割合は、プルランが65.3%、油性成分が34.58%、界面活性剤が0.12%であった。このナノファイバシートの厚みをライトマチックVL−50A((株)ミツトヨ)で測定したところ30μmであった。また、このナノファイバシートの走査型電子鏡像を図6に示す。同図から明らかなように、本実施例で得られたナノファイバシートにおけるナノファイバは、太径部及び細径部を有することが判る。このナノファイバは、図4(a)に示すナノファイバよりも、油性成分の配合割合が高く、かつ隣り合う太径部の間隔が狭いので、細径部にも中空部が形成され、該中空部にも油性成分が含まれていると考えられる。
水溶性高分子としてプルラン(林原商事製)を用い、これを水に溶解させ濃度20%の水溶液を得た。これを第1液として用いた。第2液として、油性成分としてのカミツレエキスを用いた。これらの液を用い、図2に示す装置30によって電界紡糸法を行った。この装置30におけるキャピラリ31cとして、図3に示す構造のものを用いた。このキャピラリ31cにおける芯部には第2液を流し、鞘部には第1液を流した。電界紡糸法の条件は以下のとおりとした。これら以外は実施例1と同様にしてナノファイバシートを得た。
・印加電圧:25kV
・キャピラリ−コレクタ間距離:220mm
・第1液吐出量:0.1ml/h
・第2液吐出量:2ml/h
・環境:25℃、50%RH
濃度15%のプルラン溶液中へカミツレエキスを投入し、プルラン16.22%、水75.17%、油性成分8.59%にてスターラーで攪拌したがカミツレエキスとプルラン溶液が分離してしまい均一な溶液を得ることができず、エレクトロスピニング法を行うことができなかった。
実施例1の方法で調製した溶液を、シャーレ上に滴下し乾燥させ、30μmのキャストフィルムを得た。
実施例2の方法で調製した溶液を、シャーレ上に滴下し乾燥させ、30μmのキャストフィルムを得た。
実施例3の方法で調製した溶液を、シャーレ上に滴下し乾燥させ、30μmのキャストフィルムを得た。
実施例1ないし4で得られたナノファイバシート及び比較例2ないし4で得られたキャストフィルムについて、株式会社DHC製の油とり紙による油性成分吸収の有無を目視で観察した。具体的には、これらのシートにあぶらとり紙を押しつけ、次いで剥がした後の色の変化を目視で観察した。また、これらのシートをヒトの皮膚に付着させたときの溶解性を評価した。それらの結果を以下の表1に示す。評価方法は以下に示すとおりである。
約3cmに切り出したシート表面に、株式会社DHC製あぶらとり紙をあてた後に剥がし、あぶらとり紙の色の変化を目視で確認した。
肌上に0.03gの化粧水を滴下し約20mmφに塗り拡げた後、15mmに切り出したシートを乗せた直後の該シートの溶解性を目視で確認し、下記の基準で評価を行った。
○:直ちに溶解し、ピンセットで掴むことができない
×:一部溶解するがシート状で残っている箇所があり、ピンセットで掴むことができる
11 太径部
12 細径部
13 中空部
14 油性成分
Claims (2)
- 水溶性高分子から構成され、かつ中空部を有するナノファイバを含み、ヒトの皮膚に付着させて用いられるナノファイバシートであって、
前記中空部に油性成分が含まれており、
太径部と細径部とを有し、該太径部に前記中空部を有しており、
前記中空部に含まれる前記油性成分が常温で液体であり、
前記ナノファイバにおける前記水溶性高分子の割合が10〜80質量%であり、前記油性成分の割合が20〜90質量%であるナノファイバシート。 - 前記太径部及び前記細径部の双方に前記中空部を有し、該太径部の中空部と該細径部の中空部とが連通している請求項1に記載のナノファイバシート。
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US20020081732A1 (en) * | 2000-10-18 | 2002-06-27 | Bowlin Gary L. | Electroprocessing in drug delivery and cell encapsulation |
JP2006123360A (ja) * | 2004-10-29 | 2006-05-18 | Oji Paper Co Ltd | 積層体およびその製造方法 |
US7856989B2 (en) * | 2004-12-30 | 2010-12-28 | Philip Morris Usa Inc. | Electrostatically produced fast dissolving fibers |
DE102005008926A1 (de) * | 2005-02-24 | 2006-11-16 | Philipps-Universität Marburg | Verfahren zur Herstellung von Nano- und Mesofasern durch Elektrospinning von kolloidalen Dispersionen |
US7575707B2 (en) * | 2005-03-29 | 2009-08-18 | University Of Washington | Electrospinning of fine hollow fibers |
CN1807707B (zh) * | 2006-01-13 | 2010-04-14 | 清华大学 | 一种微纳米尺度下核壳结构复合纤维的制备方法及其应用 |
JP4946076B2 (ja) * | 2006-01-27 | 2012-06-06 | 東洋紡績株式会社 | 溝付きボビンおよびパッケージ |
US8602036B2 (en) * | 2006-08-03 | 2013-12-10 | Philip Morris Usa Inc. | Smoking articles enhanced to deliver additives incorporated within electrospun microfibers and nonofibers, and related methods |
CN100999827A (zh) * | 2006-12-19 | 2007-07-18 | 张爱华 | 一种通过乳液中空超细纤维的制备方法 |
JP2008179629A (ja) | 2006-12-27 | 2008-08-07 | Snt Co | 化粧用シート |
US8353811B2 (en) * | 2007-05-30 | 2013-01-15 | Phillip Morris Usa Inc. | Smoking articles enhanced to deliver additives incorporated within electroprocessed microcapsules and nanocapsules, and related methods |
JP5600005B2 (ja) * | 2007-09-05 | 2014-10-01 | 太陽化学株式会社 | 水溶性電界紡糸シート |
US8974814B2 (en) * | 2007-11-12 | 2015-03-10 | California Institute Of Technology | Layered drug delivery polymer monofilament fibers |
WO2009133059A2 (en) * | 2008-05-02 | 2009-11-05 | Evonik Degussa Gmbh | Nanofiber matrices formed from electrospun hyperbranched polymers |
JP5295943B2 (ja) * | 2008-12-26 | 2013-09-18 | 花王株式会社 | ナノファイバシート |
JP5247557B2 (ja) * | 2009-03-25 | 2013-07-24 | 帝人株式会社 | 無機ナノ粒子−マトリックス材料繊維状複合体及びその製造方法 |
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2011
- 2011-06-28 US US13/703,315 patent/US20130125912A1/en not_active Abandoned
- 2011-06-28 EP EP11800853.1A patent/EP2589693B1/en not_active Not-in-force
- 2011-06-28 CN CN201180024763.4A patent/CN102906317B/zh not_active Expired - Fee Related
- 2011-06-28 WO PCT/JP2011/064809 patent/WO2012002389A1/ja active Application Filing
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CN102906317A (zh) | 2013-01-30 |
JP2012012714A (ja) | 2012-01-19 |
CN102906317B (zh) | 2016-02-03 |
EP2589693A4 (en) | 2014-05-14 |
US20130125912A1 (en) | 2013-05-23 |
WO2012002389A1 (ja) | 2012-01-05 |
EP2589693A1 (en) | 2013-05-08 |
EP2589693B1 (en) | 2017-10-04 |
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