JP2018172578A - 有機無機複合粒子、及び化粧料 - Google Patents
有機無機複合粒子、及び化粧料 Download PDFInfo
- Publication number
- JP2018172578A JP2018172578A JP2017072496A JP2017072496A JP2018172578A JP 2018172578 A JP2018172578 A JP 2018172578A JP 2017072496 A JP2017072496 A JP 2017072496A JP 2017072496 A JP2017072496 A JP 2017072496A JP 2018172578 A JP2018172578 A JP 2018172578A
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- JP
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- Prior art keywords
- organic
- inorganic composite
- composite particles
- silica
- particles
- 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.)
- Granted
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- 239000000377 silicon dioxide Substances 0.000 claims abstract description 61
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000005484 gravity Effects 0.000 claims abstract description 10
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- LOIYMIARKYCTBW-UHFFFAOYSA-N trans-urocanic acid Natural products OC(=O)C=CC1=CNC=N1 LOIYMIARKYCTBW-UHFFFAOYSA-N 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 230000014616 translation Effects 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
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Abstract
Description
<シリカ成分>
機無機複合粒子に含まれるシリカ成分として、珪酸バインダーやシリカ系粒子が挙げられる。珪酸バインダーとしては、アルカリ金属珪酸塩、有機塩基の珪酸塩等の珪酸塩水溶液を陽イオン交換樹脂で処理して脱アルカリ(Naイオンの除去等)したものを使用できる。珪酸塩としては、珪酸ナトリウム(水ガラス)、珪酸カリウム等のアルカリ金属珪酸塩、第4級アンモニウムシリケート等の有機塩基の珪酸塩などが挙げられる。
<生分解性プラスチック粒子>
有機無機複合粒子に含まれる生分解性プラスチックは、石油由来の物が工業的に多用されているが、生分解性があれば原料が何であるかは問わない。但し、持続可能社会の実現の観点では、生分解性プラスチックは、再生可能な有機資源であるバイオマスプラスチックであることが望ましく、化学合成で作られるポリ乳酸、ポリカプロラクトン、ポリブチレンサクシネート、ポリエチレンサクシネート、ポリビニルアルコール、ポリアスパラギン酸、微生物で作られるプルラン、ポリグルタミン酸、ポリヒドロキシアルカン酸、植物や動物由来のデンプン、セルロース、アミロース、キチン、キトサンが挙げられる。特に植物由来のセルロースが品質、価格、流通量、および安全性の観点で好適である。
<有機無機複合粒子の製造方法>
次に、本発明の有機無機複合粒子の製造方法について説明する。本発明の有機無機複合粒子の製造方法は、シリカ成分を含有した液体に、生分解性プラスチックを含有した液体を混合し分散液を調製する工程Aと、この分散液中の固形分を造粒して有機無機複合粒子を調製する工程Bを含んでいる。
<工程(A)>
シリカ成分としてシリカゾルを用いる場合には、シリカ系粒子を固形分換算で1〜30重量%含むシリカゾルを準備する。このシリカゾルに、固形分濃度1〜50重量%の生分解性プラスチック粒子の水分散液を加えて、スラリーを調製する。
<工程(B)>
造粒は、噴霧乾燥法、および乳化法を用いた従来公知の方法で行うことができる。
<化粧料>
以下に、有機無機複合粒子と各種化粧料成分とを配合して得られる化粧料について具体的に説明する。本発明は、これらの化粧料に限定されるものではない。
[実施例1]
市販のシリカゾル(日揮触媒化成(株)製:SS−160、平均粒子径160nm、シリカ濃度20質量%)2kgをロータリーエバポレーターで濃縮して、シリカ濃度40質量%のシリカゾル1kgとする。このシリカゾルに、陽イオン樹脂(三菱化成社製、SK−1B。以下同様)を一気に加えてpHを2.5とした後、陽イオン交換樹脂を分離する。これにより、脱アルカリ処理(Naイオンの除去等)がなされ、シリカ系微粒子濃度39.3質量%のスラリーaが得られる。スラリーaに、セルロース系粒子(旭化成(株)製セオラス(登録商標)RC−N30)0.4kgと純水1.3kgを混合した高分子分散液を添加し、スラリーbを調製する。
この有機無機複合粒子の粉体の物性を以下の方法で測定した。その結果を表2に示す。
(1)有機無機複合粒子、シリカ系粒子および生分解性プラスチック粒子の平均粒子径(d1)、(d2)、(d4)の測定方法
レーザー回折法を用いてそれぞれの粒度分布を測定し、この粒度分布からメジアン径で表わされる平均粒子径(d1)、シリカ系粒子の平均粒子径(d2)および生分解性プラスチック粒子の平均粒子径(d4)を求めた。レーザー回折法による粒度分布の測定は、レーザー回折/散乱式粒子径分布測定装置LA-950v2(株式会社堀場製作所製)を用いた。
(2)超音波分散有無による平均粒子径比
前記レーザー回折/散乱式粒子径分布測定装置LA-950v2にて有機無機複合粒子の平均粒子径を測定する際、該装置の分散条件を「超音波60分間」に設定し分散した後、粒度分布を測定し、この粒度分布からメジアン径で表わされる平均粒子径(d3)を求める。(d2)と(d1)の超音波分散有無の平均粒子径比(d2/d1)とする。
(3)有機無機複合粒子の粒子密度の測定方法
有機無機複合粒子を磁性ルツボ(B−2型)に約30ml採取し、105℃で2時間乾燥後、デシケーターに入れて室温まで冷却する。次に、サンプルを15ml採取し、全自動ピクノメーター(QUANTACHROME社製:Ultrapyc1200e)を用いて真比重を測定し、粒子密度とする。
(4)シリカ系粒子の変動係数の測定方法
走査型電子顕微鏡(日本電子社製JSM−7600F)により、倍率2万倍から25万倍で写真(SEM写真)を撮影する。この画像の250個の粒子について、画像解析装置(旭化成社製、IP−1000)を用いて、平均粒子径を測定し、粒子径分布に関する変動係数(CV値)を算出した。
(5)シリカ系粒子の真球度の測定方法
透過型電子顕微鏡(日立製作所製、H−8000)により、倍率2万倍から25万倍の倍率で写真撮影して得られる写真投影図から、任意の50個の粒子を選び、それぞれその最大径(DL)と、これに直交する短径(DS)との比(DS/DL)を測定し、それらの平均値を真球度とした。
(6)有機無機複合粒子の比表面積の測定方法
有機無機複合粒子の粉体を磁性ルツボ(B−2型)に約30ml採取し、105℃の温度で2時間乾燥後、デシケーターに入れて室温まで冷却する。次に、サンプルを1g取り、全自動表面積測定装置(湯浅アイオニクス社製、マルチソーブ12型)を用いて、比表面積(m2/g)をBET法にて測定し、有機無機複合粒子に配合したシリカと生分解性プラスチックの組成比(配合重量比)から換算される比重(例えばシリカ100%であれば2.2g/cm3、セルロースが100%であれば1.5g/cm3)で換算した単位体積当たりの比表面積とした。
(7)有機無機複合粒子の細孔容積、細孔径の測定方法
有機無機複合粒子の粉体10gをルツボに取り、300℃で1時間乾燥後、デシケーターに入れて室温まで冷却し、自動ポロシメーター(カウンタークローム・インスツルメンツ社製PoreMasterPM33GT)を使用して水銀圧入法により測定した。水銀を1.5kPa〜231MPaで圧入し、圧力と細孔径の関係から細孔径分布を求めた。この方法によれば、約7nmから約1000μm迄の細孔に水銀が圧入されるため、多孔質シリカ系粒子の内部に存在する小径の細孔と、多孔質シリカ系粒子の粒子間の大径の空隙(おおむね多孔質シリカ系粒子の平均粒子径に対して1/5〜1/2のサイズに計測される)の両方が計測される。大径を除く、小径の細孔の計測結果をもとに、細孔容積、最頻細孔径(Dm)、最小細孔径(D0)、および最大細孔径(D100)を算出する。このとき、必要に応じてピーク分離ソフト(自動ポロシメーターに付属)が用いられる。
(8)有機無機複合粒子の組成分析方法
有機無機複合粒子の粉体0.2gを白金皿で精秤し、硫酸10mlと弗化水素酸10mlを加えて、砂浴上で硫酸の白煙が出るまで加熱する。冷却後、水約50mlを加えて加温溶解する。冷却後、水200mlに希釈しこれを試験溶液とする。この試験溶液について誘導結合プラズマ発光分光分析装置(島津製作所(株)製、ICPS−8100、解析ソフトウェアICPS−8000)を使用し、有機無機複合粒子の組成を求める。
(9)接触角の測定方法
有機無機複合粒子1gを200℃で乾燥させた後、直径1cm、高さ5cmのセルに入れ、50kgfの荷重でプレスして成型物を得る。得られた成型物の表面に水を一滴たらして水に対する接触角を測定した。
(10)弾性率の測定方法
有機無機複合粒子の粉体から、平均粒子径±0.5μmの範囲にある粒子1個を試料として取り、微小圧縮試験機(島津製作所製、MCTM−200)を用いて、この試料に一定の負荷速度で荷重を負荷し、圧縮弾性率を測定した。さらに、この操作を4回繰り返し、5個の試料について圧縮強度を測定し、その平均値を粒子圧縮強度とする。
(11)多孔質シリカ系粒子の感触特性
多孔質シリカ系粒子の粉体について、20名の専門パネラーによる官能テストを行い、さらさら感、しっとり感、転がり感、均一な延び広がり性、肌への付着性、転がり感の持続性、およびソフト感の7つの評価項目に関して聞き取り調査を行う。その結果を以下の評価点基準(a)に基づき評価する。さらに、各人がつけた評価点を合計し、以下の評価基準(b)に基づき多孔質シリカ系粒子の感触に関する評価を行った。結果を表3に示す。
(12)パウダーファンデーションの使用感
多孔質シリカ系粒子の粉体を用いて表4に示す配合比率(重量%)となるようにパウダーファンデーションを作製した。すなわち、実施例1の粉体(成分(1))と成分(2)〜(9)をミキサーに入れて撹拌し、均一に混合した。次に、化粧料成分(10)〜(12)をこのミキサーに入れて撹拌し、さらに均一に混合した。次いで、得られたケーキ状物質を解砕処理した後、その中から約12gを取り出し、46mm×54mm×4mmの角金皿に入れてプレス成型した。この様にして得られたパウダーファンデーションについて、20名の専門パネラーによる官能テストを行い、(1)肌への塗布中の均一な延び、しっとり感、滑らかさ、および(2)肌に塗布後の化粧膜の均一性、しっとり感、やわらかさの6つの評価項目に関して聞き取り調査を行う。その結果を以下の評価点基準(a)に基づき評価する。また、各人がつけた評価点を合計し、以下の評価基準(b)に基づきファンデーションの使用感に関する評価を行った。結果を表5に示す。
評価点基準(a)
5点:非常に優れている。
評価基準(b)
◎:合計点が80点以上
○:合計点が60点以上80点未満
△:合計点が40点以上60点未満
▲:合計点が20点以上40点未満
×:合計点が20点未満
[実施例2]
市販のシリカゾル(日揮触媒化成(株)製:SS−300、平均粒子径300nm、シリカ濃度20質量%)50gをロータリーエバポレーターで濃縮して、シリカ濃度40質量%のシリカゾル25gとする。このシリカゾルに、陽イオン樹脂(三菱化成社製、SK−1B)を一気に加えてpHを2.5とした後、陽イオン交換樹脂を分離する。これにより、脱アルカリ処理(Naイオンの除去等)がなされ、シリカ系微粒子濃度39.3質量%のスラリーaが得られる。スラリーaに、セルロース系粒子(旭化成(株)製セオラス(登録商標)RC−N30)10gと純水30gを混合した高分子分散液を添加し、スラリーbを調製する。
[実施例3]
高分子分散液内のセルロース系粒子(旭化成(株)製セオラス(登録商標)RC−N30)の混合量を、0.17kgに変更した以外は実施例1と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
[実施例4]
高分子分散液内のセルロース系粒子(旭化成(株)製セオラス(登録商標)RC−N30)の混合量を、0.93kgに変更した以外は実施例1と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
[実施例5]
シリカゾルとして市販品(日揮触媒化成(株)製 SI−550、平均粒子径5nm、固形分濃度20質量%)0.02kgを使用し、エバポレーターによる濃縮を行わなかった以外は実施例3と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
[実施例6]
2流体ノズルの気体供給圧力を0.1MPaに変更した以外は実施例1と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
[比較例1]
高分子分散液内のセルロース系粒子(旭化成(株)製セオラス(登録商標)RC−N30)の混合量を、0.02kgに変更した以外は実施例1と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
[比較例2]
実施例1で得た有機無機複合粒子0.1kgにヘキサメチルジシラザン(信越化学工業(株)製:SZ−31、分子量:161.4)0.01kgとメタノール(特級試薬)0.37kgを加えた。この混合液を、ミキサー(日本コークス工業(株)製FM5C/I)を使用して出力5Hzにて10分間撹拌したのち、120℃で16時間加熱し、有機無機複合粒子を得た。これを実施例1と同様に測定した。
[比較例3]
シリカゾルとして市販品(日揮触媒化成(株)製 SI−550、平均粒子径5nm、固形分濃度20質量%)を使用し、エバポレーターによる濃縮を行わなかった以外は実施例3と同様に有機無機複合粒子を調製し、実施例1と同様に測定した。
各実施例と比較例により得られた粉体を用いて、実施例1と同様に感触特性を評価した。その結果を表3に示す。その結果、各実施例の粉体は、化粧料の感触改良材として極めて優れているが、比較例の粉体は、感触改良材として適していないことが分かった。
表4に示す配合比率(重量%)となるように、各実施例と比較例の粉体(成分(1))を、他の成分(2)〜(9)とともにミキサーに入れて撹拌し、均一に混合させた。次に、化粧料成分(10)〜(12)をこのミキサーに入れて撹拌し、均一に混合させた。得られたケーキ状物質を用いて実施例1と同様に化粧料を得た。
Claims (8)
- シリカ成分と生分解性プラスチックを含む球状の有機無機複合粒子であって、
平均粒子径(d1)が0.5〜25μm、真比重が1.0超〜2.0g/cm3、水に対する接触角が90°以下である有機無機複合粒子。 - BET法で求めた単位体積あたりの比表面積が5〜60m2/cm3未満であることを特徴とする請求項1に記載の有機無機複合粒子。
- 弾性率が2〜30GPaであることを特徴とする請求項1または2に記載の有機無機複合粒子。
- 前記有機無機複合粒子の分散液を、超音波分散機を用いて60分間分散させたとき、分散後の平均粒子径(d3)と、分散前の平均粒子径(d1)の比(d3/d1)が、±0.05以内であることを特徴とする請求項1〜3のいずれか一項に記載の有機無機複合粒子。
- 前記有機無機複合粒子には、シリカ成分が1〜80重量%、生分解性プラスチックが20〜99重量%の範囲で含まれることを特徴とする請求項1〜4のいずれか一項に記載の有機無機複合粒子。
- 前記シリカ成分が、5nm〜1μmの平均粒子径(d2)を持つシリカ系粒子であることを特徴とする請求項1〜5のいずれか一項に記載の有機無機複合粒子。
- 前記生分解性プラスチックの平均粒子径(d4)が、1nm〜1μmの範囲にあることを特徴とする請求項1〜6のいずれか一項に記載の有機無機複合粒子。
- 請求項1〜7のいずれか一項に記載の有機無機複合粒子が配合された化粧料。
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JP2019178257A (ja) * | 2018-03-30 | 2019-10-17 | 日揮触媒化成株式会社 | 有機無機複合粒子、及び化粧料 |
WO2020004604A1 (ja) * | 2018-06-29 | 2020-01-02 | 日揮触媒化成株式会社 | 多孔質セルロース粒子とその製造方法、および化粧料 |
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KR20180111669A (ko) | 2018-10-11 |
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