JP2015189698A - セルロース系水溶性増粘剤 - Google Patents
セルロース系水溶性増粘剤 Download PDFInfo
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- JP2015189698A JP2015189698A JP2014067659A JP2014067659A JP2015189698A JP 2015189698 A JP2015189698 A JP 2015189698A JP 2014067659 A JP2014067659 A JP 2014067659A JP 2014067659 A JP2014067659 A JP 2014067659A JP 2015189698 A JP2015189698 A JP 2015189698A
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- cellulose
- acid
- fine
- fine fibrous
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- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Landscapes
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
(1)1000nm以下の繊維幅を有し、かつ繊維を構成するセルロースのヒドロキシ基の一部がリンオキソ酸基で置換された微細繊維状セルロースを含む増粘剤。
(2)微細繊維状セルロースの数平均繊維径が2〜150nmである、(1)に記載の増粘剤。
(3)微細繊維状セルロースが、セルロースのヒドロキシ基の一部が、下記構造式(1):
a、b、m、nは自然数であり(ただし、a=b×mである)、
α1、α2、・・・、αn及びα’のうちの少なくとも1つはO−であり、残りはR又はORであり、
Rは、各々独立して、水素原子、飽和−直鎖状炭化水素基、飽和−分岐鎖状炭化水素基、飽和−環状炭化水素基、不飽和−直鎖状炭化水素基、不飽和−分岐鎖状炭化水素基、芳香族基又はこれらの誘導基であり、
βは有機物又は無機物からなる1価以上の陽イオンである]
で表されるリンオキソ酸基で置換されたものである、(1)又は(2)に記載の増粘剤。
(4)リンオキソ酸基がリン酸基である、(1)〜(3)のいずれかに記載の増粘剤。
(5)(1)〜(4)のいずれかに記載の増粘剤と水とを含む、組成物。
(6)pH調整剤、無機塩類、界面活性剤、オイル類、保湿剤、防腐剤、有機微粒子、無機微粒子、消臭剤、香料、有機溶媒及び機能成分からなる群から選択される機能性添加剤をさらに含む、(5)に記載の組成物。
(7)pHが2〜6である、(5)又は(6)記載の組成物。
(8)化粧料組成物である、(5)〜(7)のいずれかに記載の組成物。
(9)クリーム状、ゲル状又は乳液状の剤形を有する(8)に記載の組成物。
本発明の増粘剤は、1000nm以下の繊維幅を有し、かつ繊維を構成するセルロースのヒドロキシ基の一部がリンオキソ酸基で置換された微細繊維状セルロースを含む。微細繊維状セルロースは、通常製紙用途で用いるパルプ繊維よりもはるかに細いセルロース繊維又は棒状粒子をさす。
(2)同じ画像内で該直線と垂直に交差する直線Yを引き、該直線Yに対し、20本以上の繊維が交差する。
上記の微細繊維状セルロースは、セルロースを含む繊維原料を、リンのオキソ酸又はその塩から選ばれる少なくとも1種の化合物(以下、「化合物A」という)により処理して、セルロースにリンオキソ酸基を導入するリンオキソ酸基導入工程(a)と、該工程(a)終了後に、リンオキソ酸基を導入したセルロース(以下、「リンオキソ酸基導入セルロース」という)を解繊処理する解繊処理工程(b)により製造できる。
繊維原料を化合物Aにより処理する方法としては、乾燥状態又は湿潤状態の繊維原料に化合物Aの粉末や水溶液を混合する方法、繊維原料のスラリーに化合物Aの粉末や水溶液を添加する方法等が挙げられる。これらのうち、反応の均一性が高いことから、乾燥状態の繊維原料(パルプ)に化合物Aの水溶液を添加する方法、又は湿潤状態の繊維原料(パルプ)に化合物Aの粉末や水溶液を添加する方法が好ましい。
解繊処理工程(b)では、通常、解繊処理装置を用いて、リンオキソ酸基導入セルロースを解繊処理して、微細繊維状セルロース含有スラリーを得る。解繊処理の際には、リンオキソ酸基導入セルロースを水と有機溶媒を単独又は組み合わせて希釈してスラリー状にすることが好ましい。希釈後のリンオキソ酸基導入セルロースの固形分濃度は0.1〜20質量%であることが好ましく、0.5〜10質量%であることがより好ましい。希釈後のリンオキソ酸基導入セルロースの固形分濃度が前記下限値以上であれば、解繊処理の効率が向上し、前記上限値以下であれば、解繊処理装置内での閉塞を防止できる。
上記微細繊維状セルロースの製造方法において、工程(a)と工程(b)の間にアルカリ処理工程を有すると、微細繊維状セルロースの収率が向上するため、好ましい。また、該アルカリ処理によって、セルロースに導入されたリンオキソ酸基に陽イオンを供給して、容易に塩にすることができる。
本発明はまた、1000nm以下の繊維幅を有し、かつ繊維を構成するセルロースのヒドロキシ基の一部がリンオキソ酸基で置換された微細繊維状セルロースと水とを含む組成物に関する。本発明の組成物は、さらに、機能性添加剤を含んでいてもよい。機能性添加剤としては、例えば、pH調整剤、無機塩類、有機塩類、界面活性剤、オイル類、保湿剤、防腐剤、有機微粒子、無機微粒子、消臭剤、香料、有機溶媒、機能成分等が挙げられる。これらは単独で用いてもよく、二種以上併せて用いてもよい。
一実施形態において本発明の組成物は、化粧料組成物である。本発明の化粧料組成物は、好ましくは300mPa・s以上、より好ましくは400〜50000mPa・sの粘度を有する。本発明の化粧料組成物は、例えば、クリーム状、ゲル状、乳液状の剤形を有する。本発明の微細繊維状セルロースを化粧料組成物に配合することにより、少ない量で粘度の調整を容易に実施でき、使用感に優れた化粧料組成物を得ることができる。また、皮膚に塗布した際のべとつき感や、ざらつき感がない使用感を得ることができる。
リン酸化微細セルロース(微細セルロース1)の調製:
尿素100g、リン酸二水素ナトリウム二水和物55.3g、リン酸水素二ナトリウム41.3gを109gの水に溶解させてリン酸化試薬を調製した。
カルボキシル化微細セルロース(微細セルロース2)の調製:
乾燥質量200g相当分の未乾燥の針葉樹晒クラフトパルプとTEMPO2.5gと、臭化ナトリウム25gとを水1500mlに分散させた後、13質量%次亜塩素酸ナトリウム水溶液を、1.0gのパルプに対して次亜塩素酸ナトリウムの量が5.4mmolになるように加えて反応を開始した。反応中は0.5Mの水酸化ナトリウム水溶液を滴下してpHを10〜11に保ち、pHに変化が見られなくなった時点で反応終了と見なした。
その後、このパルプスラリーを脱水し、脱水シートを得た後、10Lのイオン交換水を注ぎ、攪拌して均一に分散させた後、濾過脱水して、脱水シートを得る工程を2回繰り返した。
セルロース表面のリン酸基量測定:
製造例1にて作製した微細セルロース1のリン酸基量を測定した。絶乾質量で0.04g程度の固形分を含む微細セルロース繊維含有スラリーを分取し、イオン交換水を用いて50g程度に希釈した。この溶液を、マグネチックスターラーを用いて撹拌しながら、0.01Nの水酸化ナトリウム水溶液を加えていったときの電気伝導度の値の変化を測定し、その値が極小となる時の0.01N水酸化ナトリウム水溶液の滴下量を滴定終点における滴下量とした。
製造例2にて作製した微細セルロース2のカルボキシル基量を測定した。絶乾質量で0.04g程度の固形分を含む微細セルロース繊維含有スラリーを分取し、イオン交換水を用いて50g程度に希釈した。この溶液を、マグネチックスターラーを用いて撹拌しながら、0.01Nの水酸化ナトリウム水溶液を加えていったときの電気伝導度の値の変化を測定し、その値が極小となる時の0.01N水酸化ナトリウム水溶液の滴下量を滴定終点における滴下量とした。
得られた各試料を25℃にてB型粘度計(No.2及びNo.3ローター)(BLOOKFIELD社製、アナログ粘度計T−LVT)を用いて回転数60rpm(3分)で粘度を測定した。100mM塩酸水溶液を調製し、1mL(0.1mM)ずつ加えては粘度を測定した。測定結果を表1に示す。
解繊パルプスラリーの上澄み液を濃度0.01〜0.1質量%に水で希釈し、親水化処理したカーボングリッド膜に滴下した。乾燥後、酢酸ウラニルで染色し、透過型電子顕微鏡(日本電子社製、JEOL−2000EX)により観察し、幅4nm程度の微細繊維状セルロースになっていることを確認した。
微細セルロース1と水と塩化ナトリウムを用いた組成物を調製した。微細セルロースを0.3質量%、塩化ナトリウム(機能性添加剤)を0.1質量%添加してスラリーとし、IKA社T25URTRA TURRAXホモジナイザーを用いて回転数10,000rpmで5分間攪拌して試料を得た。結果を表2に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例1と同様に行った。結果を表2に示す。
塩化ナトリウムの代わりにドデシルベンゼンスルホン酸ナトリウムを1.0質量%添加した以外は実施例1と同様に行った。結果を表3に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例2と同様に行った。結果を表3に示す。
塩化ナトリウムの代わりにスクワランを10質量%添加した以外は実施例1と同様に行った。結果を表4に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例3と同様に行った。結果を表4に示す。
塩化ナトリウムの代わりにグリセリンを10質量%添加した以外は実施例1と同様に行った。結果を表5に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例4と同様に行った。結果を表5に示す。
塩化ナトリウムの代わりにメチルパラベンを0.3質量%添加した以外は実施例1と同様に行った。結果を表6に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例5と同様に行った。結果を表6に示す。
塩化ナトリウムの代わりに疎水化酸化チタン(STV−455、チタン工業株式会社製)を1.0質量%添加した以外は実施例1と同様に行った。結果を表7に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例6と同様に行った。結果を表7に示す。
塩化ナトリウムの代わりにアニオン性ポリエチレンエマルション(商品名:「E−2213」(平均粒子径:0.07μm)、東邦化学工業社製)を1.0質量%添加した以外は実施例1と同様に行った。結果を表8に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例7と同様に行った。結果を表8に示す。
塩化ナトリウムの代わりにエタノールを10質量%添加した以外は実施例1と同様に行った。結果を表9に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例8と同様に行った。結果を表9に示す。
塩化ナトリウムの代わりにヒノキチオールを1.0質量%添加した以外は実施例1と同様に行った。結果を表10に示す。
微細セルロース1の代わりに微細セルロース2を用いた以外は実施例9と同様に行った。結果を表10に示す。
表11に微細セルロース1又は微細セルロース2を用いた酸性染毛料の処方を示す。調製法は常法に従った。得られた各試料のpHは「表11」のとおりであり、ほぼ同程度であった。次に各試料の安定性及び使用感を評価した結果、実施例10は良好であった。これに対し、比較例10では粘度が低く、使用感に劣るものであった。
表12に微細セルロース1を使用したヘアジェルの処方を示す。常法により調製された実施例11はたれ落ちがない良好な使用感を示すヘアジェルであった。
Claims (9)
- 1000nm以下の繊維幅を有し、かつ繊維を構成するセルロースのヒドロキシ基の一部がリンオキソ酸基で置換された微細繊維状セルロースを含む増粘剤。
- 微細繊維状セルロースの数平均繊維径が2〜150nmである、請求項1に記載の増粘剤。
- リンオキソ酸基がリン酸基である、請求項1〜3のいずれかに記載の増粘剤。
- 請求項1〜4のいずれかに記載の増粘剤と水とを含む、組成物。
- pH調整剤、無機塩類、界面活性剤、オイル類、保湿剤、防腐剤、有機微粒子、無機微粒子、消臭剤、香料、有機溶媒及び機能成分からなる群から選択される機能性添加剤をさらに含む、請求項5に記載の組成物。
- pHが2〜6である、請求項5又は6記載の組成物。
- 化粧料組成物である、請求項5〜7のいずれかに記載の組成物。
- クリーム状、ゲル状又は乳液状の剤形を有する請求項8に記載の組成物。
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US11441243B2 (en) | 2017-05-15 | 2022-09-13 | Daio Paper Corporation | Fine cellulose fiber and method for producing same |
JP2019023296A (ja) * | 2017-07-24 | 2019-02-14 | 大王製紙株式会社 | セルロース微細繊維含有物及びその製造方法、並びにセルロース微細繊維分散液 |
CN110959016B (zh) * | 2017-07-24 | 2022-04-01 | 大王制纸株式会社 | 纤维素微细纤维含有物及其制造方法以及纤维素微细纤维分散液 |
US11220787B2 (en) | 2017-07-24 | 2022-01-11 | Daio Paper Corporation | Fine cellulose fiber-containing substance, method for manufacturing the same, and fine cellulose fiber dispersion |
EP3660055A4 (en) * | 2017-07-24 | 2021-04-28 | Daio Paper Corporation | SUBSTANCE CONTAINING FINE CELLULOSE FIBERS, METHOD OF PRODUCING IT AND FINE CELLULOSE FIBER DISPERSION |
CN110959016A (zh) * | 2017-07-24 | 2020-04-03 | 大王制纸株式会社 | 纤维素微细纤维含有物及其制造方法以及纤维素微细纤维分散液 |
WO2021107147A1 (ja) * | 2019-11-29 | 2021-06-03 | 王子ホールディングス株式会社 | 繊維状セルロース、繊維状セルロース分散液及びシート |
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