JP2023502241A - 多孔質溶解性固体構造体 - Google Patents
多孔質溶解性固体構造体 Download PDFInfo
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Abstract
Description
本明細書で使用するとき、「可撓性」という用語は、物品が、その長手方向に垂直な中心線に沿って90度で曲げられた場合に、破損することなく、又は著しい破壊を伴わずに、応力に耐える物品の能力を意味する。好ましくは、このような物品は、顕著な弾性変形を受けることができ、5GPa以下、好ましくは1GPa以下、より好ましくは0.5GPa以下、最も好ましくは0.2GPa以下のヤング率によって特徴付けられる。
上記のように、多孔質溶解性固体構造体は、プレミックスとして始まる。プレミックスは、一般に、所望の成分を混合することによって調製される。多孔質溶解性固体構造体の成分としては、例えば、界面活性剤、水溶性ポリマー、可塑剤、水などを挙げることができる。これらについては、以下でより詳細に論じる。プレミックスは、メカニカルミキサーを使用して形成することができる。本明細書で有用なメカニカルミキサーとしては、勾配のあるブレードタービン、又はMAXBLEND(商標)ミキサー(Sumitomo Heavy Industries)が挙げられるが、これらに限定されない。
十分な通気後、通気されたプレミックスは、対向する第1及び第2の側面を有する1枚以上のシートを形成することができる。シート形成工程は、任意の好適な方法で、例えば、押出成形、鋳造、成型、真空成形、プレス、印刷、コーティングなどによって実施することができる。より具体的には、通気されたプレミックスは、(i)それを浅いキャビティ若しくはトレー又は特別に設計されたシート型に鋳造することと、(ii)それを乾燥機の連続ベルト又はスクリーン上に押出成形することと、(iii)それを回転ドラム乾燥機の外面上にコーティングすることと、を行うことによってシートに形成することができる。シートが形成される支持面は、金属(例えば、鋼、クロムなど)、TEFLON(登録商標)、ポリカーボネート、NEOPRENE(登録商標)、HDPE、LDPE、ゴム、ガラスなどの、防食、非干渉、及び/又は非粘着性の材料によって形成されてもよく、又はコーティングされてもよい。好適な製造方法の例は、例えば、CN2019/071751、国際公開第2012138820号及び同第2010077627号に見出すことができ、これらは全て参照により本明細書に組み込まれる。
多孔質溶解性固体構造体は、当技術分野において適切な任意の方法で乾燥させてよい。乾燥中、プロセスは、乾燥時間全体又は乾燥時間の少なくとも半分のいずれかに及ぶ、反重力加熱方向の使用を含み得る。いかなる理論にも束縛されるものではないが、このような反重力加熱方向は、乾燥工程中に形成されたシートの底部領域に向かう過度の介在液体排出を低減又は妨害することができると考えられる。更に、上面が最後に乾燥されるので、形成されたシートの上面付近の気泡を膨張させ、上面に細孔開口を形成するのにより長い時間を可能にする(湿潤マトリックスが乾燥されると、気泡はもはや膨張しないか、又は表面開口を形成することができないため)。その結果、このような反重力加熱による乾燥によって形成される多孔質溶解性固体構造体は、より迅速な溶解、並びに他の予想外の効果を可能にすることができる、改善された連続気泡構造を特徴とする。反重力加熱は、例えば、回転ドラム、伝導ベースの加熱構成などによって提供され得る。
・約85%~100%又は約90%~100%の連続気泡含有率、
・約150μm~約1000μm又は約200μm~約600μmの全体平均孔径、
・約5μm~約200μm、約10μm~約100μm、又は約10μm~約80μmの平均気泡壁厚さ、
・当該多孔質溶解性固体構造体の約0.5重量%~約25重量%、約1重量%~約20%重量%、又は約3重量%~約10%重量%の最終水分含量、
・約0.6mm~約3.5mm、約0.7mm~約3mm、約0.8mm~約2mm、又は約1mm~約1.5mmの範囲の厚さ、
・約50グラム/m2~約250グラム/m2、約80グラム/m2~約220グラム/m2、又は約100グラム/m2~約200グラム/m2の坪量、
・約0.05グラム/cm3~約0.5グラム/cm3、約0.06グラム/cm3~約0.4グラム/cm3、約0.07グラム/cm3~約0.2グラム/cm3、又は約0.08グラム/cm3~約0.15グラム/cm3の密度、
・約0.03m2/g~約0.25m2/g、約0.04m2/g~約0.22m2/g、約0.05m2/g~約0.2m2/g、又は約0.1m2/g~約0.18m2/gの比表面積。
本明細書に記載される多孔質溶解性固体構造体は、例えば、界面活性剤、水溶性ポリマー、可塑剤、添加剤などを含有し得る。多孔質溶解性固体構造体は、例えば、多孔質溶解性固体構造体の約25重量%~約80重量%、約40重量%~約70重量%の総界面活性剤を含み得る。それはまた、多孔質溶解性固体構造体の約10重量%~約40重量%の水溶性ポリマーを含み得る。多孔質溶解性構造体はまた、複数の層を含んでいてもよい。これらの層は、例えば、多孔質溶解性固体構造体の単層で構成され得る。単層多孔質溶解性構造体は、例えば、シートのような任意の適用可能な形態であってよい。多孔質溶解性構造体は、柔軟性であってもよい。多孔質溶解性固体構造体は、例えば、皮膚洗浄剤として使用することができる。多孔質溶解性固体構造体は、連続気泡発泡体であり得る。
界面活性剤は、所望の連続気泡構造を形成するのに十分な量の安定した気泡を作製するために、通気プロセス中に乳化剤として機能し得る。界面活性剤は、所望の洗浄効果を送達するための活性成分としても機能し得る。多孔質溶解性固体構造体は、例えば、イセチオネート界面活性剤、非サルフェートアニオン性界面活性剤、両性界面活性剤、双性イオン性界面活性剤、又は両性界面活性剤と双性イオン性界面活性剤との組み合わせを含み得る。
多孔質溶解性固体構造体は、例えば、多孔質溶解性固体構造体の約18重量%~約38重量%、約22重量%~約34重量%、又は約24重量%~約32重量%の範囲の量の水溶性ポリマーを含み得る。
可塑剤は、当該多孔質溶解性固体構造体の総重量の約4.5%~約20%、約5.5%~約17%、約6.5%~約14%、7.5%~11%の範囲の量で多孔質溶解性固体構造体中に存在し得る。本明細書で使用するのに好適な可塑剤としては、例えば、ポリオール、コポリオール、ポリカルボン酸、ポリエステル、ジメチコンコポリオール、及びこれらの組み合わせを挙げることができる。
上述の成分、例えば、水溶性ポリマー、界面活性剤、及び可塑剤に加えて、多孔質溶解性固体構造体は、その意図される用途に応じて、1つ以上の追加成分を含んでいてもよい。そのような1つ以上の追加成分は、例えば、パーソナルクレンジング活性物質を含み得る。そのような成分はまた、多孔質溶解性固体構造体、例えば、pH調整剤、着色剤、香料など、処方及び/又は審美性に役立つための機能を有し得る。
多孔質溶解性固体構造体が形成されたら、2枚以上のそのようなシートを更に組み合わせ及び/又は処理して、球状、立方体、長方形、楕円形、円筒形、ロッド状、シート状、花形、扇型、星形、ディスク形などが挙げられるがこれらに限定されない、任意の望ましい三次元形状の多層多孔質溶解性固体構造体を形成することができる。シートは、その例として化学的手段、機械的手段、及びこれらの組み合わせが挙げられるがこれらに限定されない、当該技術分野において既知の任意の手段によって、組み合わされ及び/又は処理されてもよい。このような組み合わせ及び/又は処理工程は、本明細書において集合的に「変換」プロセスと称され、すなわち、これは、2枚以上の多孔質溶解性固体構造体を、所望の三次元形状を有する多層多孔質溶解性固体構造体に変換するように機能する。
A)平均細孔径の決定
Hitachi TM3000 Tabletop Microscope(S/N:123104-04)を使用して、試料のSEM顕微鏡写真を取得する。多孔質溶解性固体構造体の試料は、面積が約1cm×1cmであり、より大きなシートから切断される。画像を倍率50Xで収集し、ユニットを15kVで動作させる。最低5つの顕微鏡画像を、各試料にわたってランダムに選択された位置から収集し、平均孔直径が推定される約43.0mm2の総分析面積を得る。
水力直径=「4*細孔面積(m2)/細孔周長(m)」
多孔度は、多孔質溶解性固体構造体によって占有される全空間に対する空隙空間の比率である。多孔度は、空隙空間を閾値化によって区画化し、全ボクセルに対する空隙ボクセルの比率を決定することによって、μCTスキャンから計算することができる。同様に、固体体積分率(solid volume fraction、SVF)は、全空間に対する固体空間の比率であり、SVFは、全ボクセルに対する占有されたボクセルの比率として計算することができる。多孔度及びSVFのいずれも、多孔質溶解性固体構造体の高さ方向における孔径分布、又は多孔質溶解性固体構造体ストラットの平均気泡壁厚などの構造情報を提供しない平均スカラー値である。
連続気泡含有率を、ガス比重瓶法によって測定する。ガス比重瓶法は、体積を正確に測定するガス置換法を使用する一般的な分析技術である。置換媒体としてヘリウム又は窒素のような不活性ガスが使用される。多孔質溶解性固体構造体の試料を既知の体積の計器コンパートメント内に密閉し、適切な不活性ガスを入れ、次いで、別の精密な内部体積に膨張させる。膨張前後の圧力を測定し、これを用いて試料の体積を計算する。
連続気泡パーセント=試料の連続気泡体積/試料の幾何学的体積*100
多孔質溶解性固体構造体の最終水分含量は、Mettler Toledo HX204 Moisture Analyzer(S/N B706673091)を使用することによって得ることができる。最低1gの試料を測定トレー上に置く。次いで、分析時間10分及び温度110℃の追加のプログラム設定で、標準プログラムを実行する。
多孔質溶解性固体構造体の厚さは、Mitutoyo Corporation Digital Disk Stand Micrometer Model Number IDS-1012E(Mitutoyo Corporation,965 Corporate Blvd,Aurora,IL,USA 60504)などのマイクロメーター又は隙間ゲージを用いて得ることができる。そのマイクロメーターは、直径1インチ、重さ約32グラムのプラテンを有し、約0.09psi(6.32gm/cm2)の印加圧力において厚さを測定する。
多孔質溶解性固体構造体の坪量は、その面積当たりの試料の重量(グラム/m2)として計算することができる。面積は試料の外縁部に対して垂直な平面への投影面積として計算される。試料は10cm×10cmの正方形に切断されているので、面積は既知である。次いで、このような正方形の各々を秤量し、次いで、得られた重量を100cm2の既知の面積で除して、対応する坪量を決定する。
多孔質溶解性固体構造体の密度は、次の等式によって求めることができる:密度計算値=多孔質固体の坪量/(多孔質固体の厚さ×1,000)。多孔質溶解性固体構造体の坪量及び厚さは、上述の方法に従って求めることができる。
多孔質溶解性固形構造体の比表面積は、ガス吸着技術を介して測定することができる。表面積は、分子規模の固体試料の露出した表面の測定値である。BET(Brunauer、Emmet、及びTeller)理論は、表面積を決定するのに使用される最もよく知られているモデルであり、ガス吸着等温線に基づいている。ガス吸着は、物理的な吸着及び毛管凝縮を使用してガス吸着等温線を測定するものである。この技術は、以下の工程によって要約される。試料を試料管に入れ、真空下又はガス流下で熱して試料の表面上の汚染物を除去する。試料重量は、脱ガスされた試料及び試料管の混合重量から空の試料管重量を差し引いて得られる。次に試料管を分析ポート上に置き、分析を開始する。この分析プロセスの最初の工程は、試料管を排気し、次に液体窒素温度でヘリウムガスを使用して試料管内の自由空間体積を測定する。次に試料を再度排気し、ヘリウムガスを除去する。計器は次に、要求される圧力測定値が達成されるまで、ユーザが特定する間隔でクリプトンガスを投与することによって吸着等温線を収集し始める。次に試料を、クリプトンガス吸着を備えるASAP2420を使用して分析してもよい。これらの測定は、Micromeritics Analytical Services,Inc.(One Micromeritics Dr,Suite 200,Norcross,GA 30093)により行うことが推奨される。この技術に関する更なる情報は、Micromeritics Analytical Servicesのウェブサイト(www.particletesting.com又はwww.micromeritics.com)上で入手可能であり、又はClyde Orr及びPaul Webbによる「Analytical Methods in Fine particle Technology」という書籍において公開されている。
2粘度21~26cps及び加水分解%86~89%を有するBP-17、CAS:9002-89-5、供給元:Liwei Chemical Company LTD(China)
3JORDAPON SCI、CAS:61789-32-0、供給元:BASF
4ISELUX、CAS:928663-45-0、供給元:Innospec Active Chemicals
5MIRANOL ULTRA L-32、CAS:68608-66-2、供給元:McIntyre Group Ltd(University Park, IL)
6AMPHOSOL HCA-B、供給元:Stepan Company(Northfield, IL)
7MACKAM DAB-ULS、CAS:4292-10-8、供給元:McIntyre Group Ltd(University Park, IL)
8EVERSOFT UCS-50 SG、CAS:68187-30-4、供給元:Sino Lion(New Jersey)
9MACKANATE EL P、CAS:68815-56-5、供給元:Solvay
10Citric Acid Anhydrous Fine Granular 51N、供給元:S.A. Citrique Belge N.V.(Pastorijstraat 249, B-3300 Tienen, Belgium)
Claims (15)
- 多孔質溶解性固体構造体であって、
a.前記多孔質溶解性固体の約20重量%~約50重量%、好ましくは約22重量%~約50重量%、より好ましくは約28重量%~約45重量%、更により好ましくは約34重量%~約41重量%のイセチオネート界面活性剤、好ましくはココイルイセチオン酸ナトリウム、ラウロイルメチルイセチオン酸ナトリウム、又はこれらの組み合わせと、
b.前記多孔質溶解性固体の約4重量%~約25重量%、好ましくは約6重量%~約18重量%、より好ましくは約8重量%~約16重量%、更により好ましくは約10重量%~約16重量%の非サルフェートアニオン性界面活性剤、好ましくはココイルグルタミン酸ナトリウム、ラウロイルグルタミン酸ナトリウム、ラウレススルホコハク酸二ナトリウム、又はこれらの組み合わせと、
c.前記固体構造体の約5重量%~約28重量%、好ましくは約7重量%~約26重量%、より好ましくは約9重量%~約24重量%、更により好ましくは約11重量%~約22重量%の両性界面活性剤、双性イオン性界面活性剤、又はこれらの組み合わせ、好ましくはラウラミドプロピルベタイン、コカミドプロピルベタイン、ラウロアンホ酢酸ナトリウム、又はこれらの組み合わせと、
d.前記多孔質溶解性固体構造体の約18重量%~約38重量%、好ましくは約20重量%~約36重量%、より好ましくは約22重量%~約34重量%、更により好ましくは約24重量%~約32重量%のポリビニルアルコールと、
e.約4.5%~約20%、好ましくは約5.5%~約17%、より好ましくは約6.5%~約14%、更により好ましくは約7.5%~約11%のグリセリンと、
を含み、
前記多孔質溶解性固体構造体が、約0.05g/cm3~約0.20g/cm3、好ましくは約0.07g/cm3~約0.18g/cm3、より好ましくは約0.09g/cm3~約0.16g/cm3、又は更により好ましくは約0.11g/cm3~約0.14g/cm3の密度を有する、多孔質溶解性固体構造体。 - 破断点歪みが、20mm以上、好ましくは25mm以上、より好ましくは30mm以上、又は更により好ましくは35mm以上である、請求項1又は2に記載の多孔質溶解性固体構造体。
- イセチオネートのレベルが、約20重量%~約30重量%であり、非サルフェートアニオン性界面活性剤のレベルが、約15重量%~約25重量%であり、両性及び/又は双性イオン性界面活性剤のレベルが、約15重量%~約25重量%である、請求項1又は2に記載の多孔質溶解性固体構造体。
- イセチオネートのレベルが、約31重量%~約41重量%であり、非サルフェートアニオン性界面活性剤のレベルが、約7重量%~約18重量%であり、両性及び/又は双性イオン性界面活性剤のレベルが、約7重量%~約18重量%である、請求項1又は2に記載の多孔質溶解性固体構造体。
- イセチオネートのレベルが、約38重量%~約41重量%であり、非サルフェートアニオン性界面活性剤のレベルが、約7重量%~約17重量%であり、両性及び/又は双性イオン性界面活性剤のレベルが、約7重量%~約17重量%である、請求項1又は2に記載の多孔質溶解性固体構造体。
- 前記イセチオネートが、ココイルイセチオン酸ナトリウムを含み、前記非サルフェートアニオン性界面活性剤が、ココイルグルタミン酸ナトリウムを含み、前記双性イオン性界面活性剤が、ラウラミドプロピルベタインを含む、請求項5に記載の多孔質溶解性固体構造体。
- 前記イセチオネートが、約15重量%~約32重量%のラウロイルメチルイセチオン酸ナトリウム、及び約7重量%~約25重量%のココイルイセチオン酸ナトリウムを含み、前記非サルフェートアニオン性界面活性剤が、ココイルグルタミン酸ナトリウムを含み、前記双性イオン性界面活性剤が、ラウラミドプロピルベタインを含む、請求項5に記載の多孔質溶解性固体構造体。
- イセチオネートのレベルが、約21重量%~約25重量%であり、非サルフェートアニオン性界面活性剤のレベルが、約14重量%~約17重量%であり、両性及び/又は双性イオン性界面活性剤のレベルが、約22重量%~約25重量%である、請求項1又は2に記載の多孔質溶解性固体構造体。
- イセチオネートのレベルが、約21重量%~約25重量%であり、非サルフェートアニオン性界面活性剤のレベルが、約22重量%~約25重量%であり、両性及び/又は双性イオン性界面活性剤のレベルが、約14重量%~約17重量%である、請求項1又は2に記載の多孔質溶解性固体構造体。
- 前記イセチオネートが、ココイルイセチオン酸ナトリウムを含み、前記非サルフェートアニオン性界面活性剤が、ココイルグルタミン酸ナトリウム及びラウレススルホコハク酸二ナトリウムを含み、前記双性イオン性界面活性剤が、ラウラミドプロピルベタインを含む、請求項8又は9に記載の多孔質溶解性固体構造体。
- 前記イセチオネートが、ココイルイセチオン酸ナトリウムを含み、前記非サルフェートアニオン性界面活性剤が、ココイルグルタミン酸ナトリウムを含み、前記双性イオン性界面活性剤が、ラウラミドプロピルベタインを含む、請求項8又は9に記載の多孔質溶解性固体構造体。
- 前記多孔質溶解性固体構造体が、複数の層を有する、請求項1~11のいずれか一項に記載の多孔質溶解性固体構造体。
- 総界面活性剤量が、前記多孔質溶解性構造体の約40重量%~約70重量%である、請求項1~12のいずれか一項に記載の多孔質溶解性固体の構造体。
- 水溶性ポリマーがポリビニルアルコールを含み、可塑剤がグリセリンを含む、請求項1~13のいずれか一項に記載の多孔質溶解性固体構造体。
- 前記多孔質溶解性固体構造体が、連続気泡発泡体である、請求項1~14のいずれか一項に記載の多孔質溶解性固体構造体。
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US20210147763A1 (en) | 2021-05-20 |
BR112022008432A2 (pt) | 2022-07-19 |
US20230059551A1 (en) | 2023-02-23 |
CN114727933B (zh) | 2024-03-08 |
US11525104B2 (en) | 2022-12-13 |
EP4061320A1 (en) | 2022-09-28 |
CN114727933A (zh) | 2022-07-08 |
JP7359958B2 (ja) | 2023-10-11 |
CA3157576A1 (en) | 2021-05-27 |
WO2021097691A1 (en) | 2021-05-27 |
MX2022003979A (es) | 2022-04-26 |
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