CN115461039B - 微乳液组合物以及含有该微乳液组合物的化妆品 - Google Patents
微乳液组合物以及含有该微乳液组合物的化妆品 Download PDFInfo
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- CN115461039B CN115461039B CN202180029578.8A CN202180029578A CN115461039B CN 115461039 B CN115461039 B CN 115461039B CN 202180029578 A CN202180029578 A CN 202180029578A CN 115461039 B CN115461039 B CN 115461039B
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Abstract
本发明为一种微乳液组合物,其含有:(A)下述通式(1)所表示的由格里芬法计算出的HLB为8.0以上的聚醚改性有机聚硅氧烷;(B)下述通式(7)所表示的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷;(C)下述通式(8)所表示的甘油衍生物;Gly‑{O‑(PO)f(EO)g(BO)hH}3 (8)(D)除所述(C)以外的多元醇;(E)25℃下的运动粘度为20mm2/s以下的硅油;(F)水,所述(A)的质量与所述(B)的质量之比(A)/(B)满足1.0~15.0,所述微乳液组合物的25℃下的外观为透明至半透明。由此可提供一种外观为透明至半透明的微乳液组合物。
Description
技术领域
本发明涉及一种含有硅油的微乳液组合物,以及含有该微乳液组合物的化妆品。
背景技术
近年来,流行一种为了防止掉妆而不易被汗或皮脂等脱除的粉底或耐水功能的睫毛膏。由于这些产品含有以硅树脂为代表的覆膜形成剂,因此通常的洁面剂难以将其脱除。在脱除这些时,需要使洁面剂在皮肤上充分延展并融合,但具有因与底妆融合而延展厚重的倾向。因此,寻求一种可轻盈延展的制剂。此外,大量报道了具有双连续结构的微乳液组合物能够得到改善了功能性或使用感的化妆品,从以湿润的手即可简单使用的角度出发,可应用于洁面剂(专利文献1~7)。
与水分散型乳液或油分散型乳液相比,双连续微乳液组合物虽然需要使用大量的表面活性剂,但在用作化妆品时会残留活性剂带来的粘腻或油腻的感觉,因此为了保持轻盈的触感而优选减少表面活性剂的使用量(专利文献8),或优选使用有机硅类表面活性剂、硅油。在专利文献9中,通过使用有机硅类表面活性剂、硅油,获得了双连续微乳液组合物,但活性剂的使用量大,有可能会导致粘腻。
通过使用作为天然表面活性剂的表面活性素(Surfactin),能够制作含有硅油的微乳液组合物。专利文献10中报告了一种由表面活性素、氨基改性有机硅、水性溶剂组成的乳化组合物。其特征在于乳化力高、少量表面活性剂即可,但由于活性剂为阴离子型,因此与非离子型的表面活性剂相比,会残留较强的活性剂带来的粘腻感。
另外还研究了将甘油衍生物用作助剂而改善延展性的洁面剂。专利文献11~12中,虽然通过使用特定的甘油衍生物得到了延展不厚重的洁面剂,但油剂需要同时使用硅油与酯油,没有单独使用硅油的案例。专利文献13中,通过使用特定的甘油衍生物而得到了单独掺合硅油的微乳液,但必须使用高HLB(亲水亲油平衡值,Hydrophilic-LipophilicBalance)的非有机硅类表面活性剂。
现有技术文献
专利文献
专利文献1:日本特开2009-196909号公报
专利文献2:日本特开2015-105255号公报
专利文献3:日本特开2017-66085号公报
专利文献4:日本特开2004-217640号公报
专利文献5:日本特开2013-32348号公报
专利文献6:日本特开2014-224061号公报
专利文献7:日本特开2010-222324号公报
专利文献8:日本特开2011-178769号公报
专利文献9:日本特开2019-99469号公报
专利文献10:国际公开第2018/008653号
专利文献11:日本特开2012-017305号公报
专利文献12:日本特开2016-013975号公报
专利文献13:日本特开2007-015972号公报
发明内容
本发明要解决的技术问题
本发明是鉴于上述情况而完成的,其目的在于提高一种微乳液组合物以及含有水中油型微乳液组合物的化妆品,所述微乳液组合物即使仅使用有机硅类的表面活性剂,也能在将25℃下的运动粘度为20mm2/s以下的硅油用于油相时,外观为透明至半透明。
解决技术问题的技术手段
为了解决上述技术问题,本发明提供一种微乳液组合物,其含有:
(A)下述通式(1)所表示的由格里芬法(Griffin法)计算出的HLB(亲水亲油平衡值,Hydrophilic-Lipophilic Balance)为8.0以上的聚醚改性有机聚硅氧烷,
[化学式1]
式(1)中,R1为同种或不同种的碳原子数为1~30的烷基、芳基、芳烷基、或这些基团的卤素取代基、氨基取代基或羧基取代基,
R2为同种或不同种的下述通式(2)所表示的聚氧化烯基,
[化学式2]
-(CH2)2-C1H21-O-(C2H4O)b(C3H6O)cR5 (2)
式(2)中,R5为未取代或取代的一价烃基或氢原子,l、b及c为满足0≤l≤15、2≤b≤200、0≤c≤200、3≤b+c≤200的整数,
R3为同种或不同种的下述通式(3)~(6)中任一通式所表示的基团,
[化学式3]
-(CH2)2-CmH2m-(SiOR1 2)d-SiR1 3 (3)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 3)3-e1 (4)
-(CH2)2-CmH2m-SiR1 c1-(OSiR1 e2(OSiR1 3)3-c2)3-e1 (5)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 e3(OSiR1 3)3-e3)3-e2)3-e1 (6)
式(3)~(6)中,R1与上述R1相同,m、d及e1~e3为满足0≤m≤5、0≤d≤500、0≤e1≤2、0≤e2≤2、0≤e3≤2的整数,
R4相互独立地为R1、R2或R3,a1为满足0≤a1≤100、a2为满足0≤a2≤50、a3为满足0≤a3≤50的数,其中,a2为0时R4中的至少一个为R2;
(B)下述通式(7)所表示的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷,
[化学式4]
式(7)中,R1、R2、R3、R4与上述对R1、R2、R3、R4的定义相同,a4为满足0≤a4≤100、a5为满足0≤a5≤50、a6为满足0≤a6≤50的数,其中,a5为0时R4中的至少一个为R2;
(C)下述通式(8)所表示的甘油衍生物,
[化学式5]
Gly-{O-(PO)f(EO)g(BO)hH}3 (8)
式(8)中,Gly为自甘油中去除了羟基的残基,PO为氧化丙烯基,EO为氧化乙烯基,f及g分别为PO及EO的平均加成摩尔数,f+g表示1~30的值,PO与EO的质量比(PO/EO)为1/5~5/1,BO表示碳原子数为4的氧化烯基,h为BO的平均加成摩尔数,表示1~5的值;
(D)除所述(C)以外的多元醇;
(E)25℃下的运动粘度为20mm2/s以下的硅油;
(F)水,
所述(A)的质量与所述(B)的质量之比(A)/(B)满足1.0~15.0,所述微乳液组合物的25℃下的外观为透明至半透明。
若为这样的微乳液组合物,则能够制作成外观为透明至半透明的微乳液组合物。此外,由于使用有机硅类表面活性剂作为活性剂、使用硅油作为油剂,因此其具有活性剂带来的粘腻或油腻的感觉少的特征。
此时,所述微乳液组合物中的所述(A)聚醚改性有机聚硅氧烷的质量与所述(B)聚醚改性有机聚硅氧烷的质量之比(A)/(B)为1.0~15.0。
若为这样的质量比,则能够易于得到稳定且外观为透明至半透明的微乳液组合物。
此时,优选所述(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.0以上且13.0以下。
此外,此时,优选所述(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.5以上且10.5以下。
由此,能够易于得到外观为透明至半透明的微乳液组合物。特别是若HLB为8.5以上且10.5以下,则能够易于得到外观为透明的微乳液组合物。
此时,所述(A)聚醚改性有机聚硅氧烷优选为在化妆品显示名称中记为PEG-9聚二甲基硅氧烷的化合物。
若为这样的聚醚改性有机聚硅氧烷,则易于获得原料,从而能够更容易地得到微乳液组合物。
此时,所述微乳液组合物优选为将所述微乳液组合物添加于水中时能够分散的组合物。
若为这样的微乳液组合物,则能够适用于化妆品等用途。
此时,相对于所述微乳液组合物,含有0.1~10wt%的所述(A)聚醚改性有机聚硅氧烷。
若(A)聚醚改性有机聚硅氧烷在上述范围内,则易于形成D相。
此时,优选所述(D)多元醇为甘油或甘油的衍生物。
若为这样的化合物,则能够在更大的浓度范围内形成D相。
此时,优选所述(E)为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。
这样的硅油为在1气压下的沸点为260℃以下的挥发性硅油,能够适用于本发明的微乳液组合物。
此外,本发明还能够提供一种含有上述微乳液组合物的化妆品。
由此通过以上述的微乳液组合物为基础而制作化妆品,能够制成涂布时的易延展度良好、触感清爽、清洁效果高、清洗性及经时稳定性优异的化妆品。
发明效果
如上所述,本发明的微乳液组合物通过以特定的比例将特定的甘油衍生物、多元醇进行组合并使用两种不同HLB的聚醚改性有机聚硅氧烷作为表面活性剂,从而在将25℃下的运动粘度为20mm2/s以下的硅油用作油相时,无需使用阴离子型或阳离子型的表面活性剂,即能够制作外观为透明至半透明的微乳液组合物。掺合了该微乳液组合物的清洁化妆品是一种涂布时的易延展度良好、触感清爽、清洁效果高、清洗性优异的化妆品。
具体实施方式
以下,对本发明进行详细说明,但本发明并不受此限定。
如上所述,寻求提供下述微乳液组合物以及寻求开发含有水中油型微乳液组合物的化妆品,所述微乳液组合物即使不使用阴离子型或阳离子型的表面活性剂而仅使用有机硅类的表面活性剂,即可在将25℃下的运动粘度为20mm2/s以下的硅油用作油相时,使其外观为透明至半透明。
本申请的发明人为了实现上述目的进行了深入研究,结果发现,通过将特定的甘油衍生物、多元醇进行组合并使用两种不同HLB的聚醚改性有机聚硅氧烷作为表面活性剂,从而在将25℃下的运动粘度为20mm2/s以下的硅油用作油相时,可得到外观为透明至半透明且热力学稳定的微乳液组合物。
此外,确认可得到涂布时的易延展度良好、触感清爽、清洁效果高、清洗性优异的洁面剂,进而完成了本发明。
即,本发明为一种微乳液组合物,其含有:
(A)下述通式(1)所表示的由格里芬法计算出的HLB(亲水亲油平衡值,Hydrophilic-Lipophilic Balance)为8.0以上的聚醚改性有机聚硅氧烷,
[化学式6]
式(1)中,R1为同种或不同种的碳原子数为1~30的烷基、芳基、芳烷基、或这些基团的卤素取代基、氨基取代基或羧基取代基,
R2为同种或不同种的下述通式(2)所表示的聚氧化烯基,
[化学式7]
-(CH2)2-C1H21-O-(C2H4O)b(C3H6O)cR5 (2)
式(2)中,R5为未取代或取代的一价烃基或氢原子,l、b及c为满足0≤l≤15、2≤b≤200、0≤c≤200、3≤b+c≤200的整数,
R3为同种或不同种的下述通式(3)~(6)中任一通式所表示的基团,
[化学式8]
-(CH2)2-CmH2m-(SiOR1 2)d-SiR1 3 (3)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 3)3-e1 (4)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 3)3-e2)3-e1 (5)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 e3(OSiR1 3)3-e3)3-e2)3-e1 (6)
式(3)~(6)中,R1与上述R1相同,m、d及e1~e3为满足0≤m≤5、0≤d≤500、0≤e1≤2、0≤e2≤2、0≤e3≤2的整数,
R4相互独立地为R1、R2或R3,a1为满足0≤a1≤100、a2为满足0≤a2≤50、a3为满足0≤a3≤50的数,其中,a2为0时R4中的至少一个为R2;
(B)下述通式(7)所表示的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷,
[化学式9]
式(7)中,R1、R2、R3、R4与上述对R1、R2、R3、R4的定义相同,a4为满足0≤a4≤100、a5为满足0≤a5≤50、a6为满足0≤a6≤50的数,其中,a5为0时R4中的至少一个为R2;
(C)下述通式(8)所表示的甘油衍生物,
[化学式10]
Gly-{O-(PO)f(EO)g(BO)hH}3 (8)
式(8)中,Gly为自甘油中去除了羟基的残基,PO为氧化丙烯基,EO为氧化乙烯基,f及g分别为PO及EO的平均加成摩尔数,f+g表示1~30的值,PO与EO的质量比(PO/EO)为1/5~5/1,BO表示碳原子数为4的氧化烯基,h为BO的平均加成摩尔数,表示1~5的值;
(D)除所述(C)以外的多元醇;
(E)25℃下的运动粘度为20mm2/s以下的硅油;
(F)水,
所述(A)的质量与所述(B)的质量之比(A)/(B)满足1.0~15.0,所述微乳液组合物的25℃下的外观为透明至半透明。
[A成分]
本发明中所使用的(A)由格里芬法计算出的HLB为8.0以上的聚醚改性有机聚硅氧烷如下述通式(1)所示。
[化学式11]
在上述式(1)中,R1为同种或不同种的碳原子数为1~30的烷基、芳基、芳烷基、或这些基团的卤素取代、氨基取代或羧基取代基。其中,优选碳原子数为1~10的烷基、芳基、芳烷基、氟取代烷基、氯取代烷基、氨基取代烷基、羧基取代烷基。更具体而言,可列举出甲基、乙基、丙基、丁基、戊基、环戊基、环己基、苯基、甲苯基等、三氟丙基、十七氟癸基、氯丙基、氯苯基等。进一步优选碳原子数为1~5的烷基、苯基或三氟丙基。
R2为同种或不同种的下述通式(2)所表示的聚氧化烯基。
[化学式12]
-(CH2)2-C1H21-O-(C2H4O)b(C3H6O)cR5 (2)
式(2)中,R5为未取代或取代的一价烃基或氢原子,l、b及c为满足0≤l≤15、2≤b≤200、0≤c≤200、3≤b+c≤200的整数。
在上述式(2)中,R5为未取代或取代的一价烃基或氢原子。l为0≤l≤15,优选0≤l≤2。b为2≤b≤200,优选2≤b≤100,进一步优选2≤b≤50。若b大于200,则由于亲水性过高而导致缺乏稳定性。c为0≤c≤200,优选0≤c≤100,进一步优选0≤c≤50。若c大于200,则由于亲水性过高而导致缺乏稳定性。b+c为3≤b+c≤200,优选3≤b+c≤100,进一步优选3≤b+c≤50。若b+c小于3,则由于缺乏亲水性从而导致乳化性变弱而缺乏稳定性。为了赋予充分的亲水性以便得到油中水型乳化物,期望b/c≥1,且为了赋予充分的疏水性以便得到水中油型乳化物,期望b/c≤1。当聚氧化烯基部分由环氧乙烷单元与环氧丙烷单元这两者构成时,可以是这两个单元的嵌段共聚物或无规共聚物中的任一种。
R3为同种或不同种的下述通式(3)~(6)中任一通式所表示的基团。
[化学式13]
-(CH2)2-CmH2m-(SiOR1 2)d-SiR1 3 (3)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 3)3-e1 (4)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 3)3-e2)3-e1 (5)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 e3(OSiR1 3)3-e3)3-e2)3-e1 (6)
式(3)~(6)中,R1与上述R1相同,m、d及e1~e3为满足0≤m≤5、0≤d≤500、0≤e1≤2、0≤e2≤2、0≤e3≤2的整数。
对于这些通式中的R1,其例示及优选的范围与上述R1相同,m为0≤m≤5,优选0≤m≤2,d为0≤d≤500,优选1≤d≤100,更优选1≤d≤50。若d大于500,则由于缺乏亲水性而导致缺乏稳定性。
R4相互独立地为R1、R2或R3。此外,a1为0≤a1≤100,优选1≤a1≤50,进一步优选1≤a1≤30。若a1大于100,则由于缺乏亲水性而导致难以得到稳定的乳化物。a2为0≤a2≤50,优选1≤a2≤30,进一步优选1≤a2≤10。若a2大于50,则由于亲水性过高而导致缺乏稳定性。a3为0≤a3≤50,优选0≤a3≤30,进一步优选0≤a3≤10。若a3大于50,则由于缺乏亲水性而导致同样缺乏稳定性。其中,a2为0时R4中的至少一个为R2。
当作为乳化剂来看时,通式(1)所表示的聚醚改性有机聚硅氧烷的重均分子量没有特别限定,但优选为500~200,000,特别优选为1,000~100,000。
本发明的通式(1)所表示的聚醚改性有机聚硅氧烷能够通过在铂催化剂或铑催化剂的存在下,使有机氢聚硅氧烷、下述通式(2’)所表示的聚氧化烯化合物、下述通式(3’)~(6’)中任一通式所表示的有机硅化合物、以及根据情况而进一步添加的末端含有不饱和基团的烯化合物进行加成反应而容易地进行合成。其中,作为有机氢聚硅氧烷,为直链状或环状均可,从可顺利进行加成反应的角度出发,优选主要为直链状。
[化学式14]
式(2’)中,R5、l、b及c与上述R5、l、b及c相同。
[化学式15]
式(3’)~(6’)中,R1、m、d及e1~e3与上述R1、m、d及e1~e3相同。
例如以末端不饱和基团相对于1摩尔的SiH基的摩尔比计,有机氢聚硅氧烷与上述通式(2’)所表示的聚氧化烯化合物、上述通式(3’)~(6’)中任一通式所表示的有机硅化合物、以及末端含有不饱和基团的烯化合物的合计的混合比例为0.5~2.0,优选为0.8~1.2。
此外,期望在铂催化剂或铑催化剂的存在下进行上述加成反应,具体而言,适合使用氯铂酸、醇改性氯铂酸、氯铂酸-乙烯基硅氧烷络合物等催化剂。另外,可将催化剂的用量设为催化剂量,但特别是以铂或铑的量计为50ppm以下,优选为20ppm以下。
可以根据需要在有机溶剂中进行上述加成反应。作为有机溶剂,例如可列举出甲醇、乙醇、2-丙醇、丁醇等脂肪醇;甲苯、二甲苯等芳香族烃;正戊烷、正己烷、环己烷等脂肪族或脂环式烃;二氯甲烷、三氯甲烷、四氯化碳等卤代烃等,特别是在用作化妆品用途时适合为乙醇、2-丙醇(异丙醇)。加成反应条件没有特别限定,优选在回流下反应1~10小时。
(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.0以上。格里芬法定义为HLB值=20×(亲水部的分子量的总和/整体的分子量)。此外,HLB值是表示表面活性剂的相对于水和油剂的亲和性的数值。当HLB小于8.0时,可能会使所得到的微乳液组合物的外观受损。
此时,优选(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.0以上且13.0以下。由此,能够容易得到外观为透明至半透明的微乳液组合物。
此外,此时,优选(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.5以上且10.5以下。由此,能够容易得到外观为透明的微乳液组合物。
此外,期望由格里芬法计算出的HLB为8.5以上且10.5以下的(A)聚醚改性有机聚硅氧烷为化妆品显示名称中的PEG-9聚二甲基硅氧烷。这样的物质并不限定于以下的实例,但例如可以使用Shin-Etsu Chemical Co.,Ltd.制造的“KF-6013”。若为这样的聚醚改性有机聚硅氧烷,则易于获得原料,且更易于得到微乳液组合物。
[B成分]
作为本发明中所使用的(B)成分的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷如下述通式(7)所示。
[化学式16]
式(7)中,R1、R2、R3、R4与上述对R1、R2、R3、R4的定义相同。a4为满足0≤a4≤100、a5为满足0≤a5≤50、a6为满足0≤a6≤50的数。其中,a5为0时R4中的至少一个为R2。
a4为0≤a4≤100,优选1≤a4≤50,进一步优选1≤a4≤30。若a4大于100,则由于缺乏亲水性而导致难以得到稳定的乳化物。a5为0≤a5≤50,优选1≤a5≤30,进一步优选1≤a5≤10。若a5大于50,则由于亲水性过高而导致缺乏稳定性。a6为0≤a6≤50,优选0≤a6≤30,进一步优选0≤a6≤10。若a6大于50,则由于缺乏亲水性而导致同样缺乏稳定性。
(B)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为5.0以下。当HLB大于5.0时,由于相对于(E)成分的相容性会下降,故而不优选。
这样的物质并不限定于以下的实例,但例如可以使用Shin-Etsu Chemical Co.,Ltd.制造的“KF-6015”、“KF-6017”、“KF-6017P”、“KF-6028”、“KF-6028P”。
通过同时使用(A)成分与(B)成分,相对于后述的作为(E)成分的在25℃下的运动粘度为20mm2/s以下的硅油的相容能力得到提高,因此外观的透明性得到提高。若仅为(A)成分,则其与(C)成分相容但不与(E)成分相容。因此,通过同时使用(B)成分,可起到相对于(E)成分的相容剂的作用。
在本发明的微乳液组合物中,(A)聚醚改性有机聚硅氧烷的质量与(B)聚醚改性有机聚硅氧烷的质量之比(A)/(B)为1.0~15.0。优选(A)/(B)为2.0~10.0。若(A)/(B)不为1.0以上,则微乳液组合物不稳定,若(A)/(B)不为15.0以下,则会使微乳液组合物的外观受损。
[C成分]
本发明中所使用的甘油衍生物如下述通式(8)所示。
[化学式7]
Gly-{O-(PO)f(EO)g(BO)hH}3 (8)
式(8)中,Gly为自甘油中去除了羟基的残基,PO为氧化丙烯基,EO为氧化乙烯基,f及g分别为PO及EO的平均加成摩尔数,f+g表示1~30的值,PO与EO的质量比(PO/EO)为1/5~5/1,BO表示碳原子数为4的氧化烯基,h为BO的平均加成摩尔数,表示1~5的值。
上述甘油衍生物通过以3~150摩尔当量的比例相对于1摩尔的甘油加成环氧丙烷、环氧乙烷后,以3~15摩尔当量的比例加成环氧丁烷而得到。总而言之,通过在相对于甘油合成PO与EO的加成物后,以嵌段状加成环氧丁烷而得到。
从提高清洁效果的角度出发,环氧丙烷(PO)与环氧乙烷(EO)的质量比(PO/EO)为1/5以上,从提高洗涤性效果的角度出发,环氧丙烷(PO)与环氧乙烷(EO)的质量比(PO/EO)为5/1以下。
环氧丙烷(PO)与环氧乙烷(EO)的平均加成摩尔数合计为3~90摩尔,即f+g在1~30的范围内。若PO及EO的平均加成摩尔数合计小于3摩尔、即f+g小于1,则洗涤性变差。若平均加成摩尔数合计大于90摩尔、即f+g大于30,则清洁效果变差,进一步使用时的延展性变差,皮肤有粘腻感,洗涤性变差。
碳原子数为4的环氧烷(BO)的平均加成摩尔数为3~15摩尔,即h在1~5的范围内。若BO的平均加成摩尔数小于3摩尔、即h小于1,则清洁效果变弱,皮肤残留粘腻感。若平均加成摩尔数大于15摩尔、即h大于5,则使用时的延展性或洗涤性变差。
作为碳原子数为4的环氧烷(BO),可列举出1,2-环氧丁烷、2,3-环氧丁烷、四亚甲基氧化物(四氢呋喃)等。其中,从容易获得、容易控制反应等角度出发,优选1,2-环氧丁烷。
对甘油加成这些环氧烷时,可使用碱催化剂、相转移催化剂、路易斯酸催化剂等进行加成反应。通常,优选使用氢氧化钾等碱催化剂。
作为(C)甘油衍生物,具体而言,可列举出(EO)的平均加成摩尔数为8、(PO)的平均加成摩尔数为5、(BO)的平均加成摩尔数为3的甘油衍生物,从降低涂布时的油光感、打滑感的角度出发,优选聚氧丁烯聚氧乙烯聚氧丙烯甘油基醚(3BO)(8EO)(5PO)。作为市售产品,例如可使用Wilbride S-753(NOF CORPORATION制造)。该甘油衍生物发挥后述的诱发共连续结构的重要作用。
[D成分]
本发明中所使用的(D)成分为除(C)成分以外的多元醇。对于D成分,作为通常所使用的多元醇,具体可列举出赤藓糖醇、麦芽糖醇、木糖醇、山梨糖醇等糖醇,1,3-BG、甘油、PG、DPG等多元醇,可单独使用一种或适宜地组合使用两种以上。特别优选使用水溶性的甘油或除(C)成分以外的甘油衍生物。
作为多元醇,优选使用碳原子数为5~10的1,2-烷烃二醇与除其以外的多元醇中的一种、或组合使用碳原子数为5~10的1,2-烷烃二醇与除其以外的多元醇中的两种以上。对于多元醇的使用,可通过与作为(A)成分的通式(1)所表示的由格里芬法计算出的HLB为8.0以上的聚醚改性有机聚硅氧烷、作为(B)成分的通式(7)所表示的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷进行组合而调整HLB,从而易于形成作为表面活性剂相的一种的D相。
具体而言,碳原子数为5~10的1,2-烷烃二醇为1,2-戊二醇、1,2-己二醇、1,2-庚二醇、1,2-辛二醇、1,2-壬二醇、1,2-癸二醇。其中,优选使用1,2-己二醇、1,2-庚二醇及1,2-辛二醇中的一种以上。
作为除碳原子数为5~10的1,2-烷烃二醇以外的多元醇,只要可用作化妆品原料则没有特别限定,例如可例示出乙二醇、二乙二醇、聚乙二醇、丙二醇、二丙二醇、聚丙二醇、甘油、二甘油、聚甘油、1,3-丁二醇、异丁二醇、山梨糖醇、甘露糖醇、葡醇(glycol)等。
此时,作为(D)成分的多元醇优选为甘油或甘油的衍生物。特别优选二丙二醇、甘油、1,3-丁二醇。进一步,当使用甘油时,由于其能够在更大的浓度范围内形成D相故而特别优选。
在化妆品中,(D)成分的多元醇的总掺合量优选设为1.0~70质量%,更优选设为5~50质量%。若为1.0质量%以上的掺合量,则能够充分得到微乳液。
[E成分]
本发明中的(E)成分为在25℃下的运动粘度为20mm2/s以下的硅油。
运动粘度为依据JIS Z 8809:2011中所记载的使用坎农-芬斯克粘度计(Cannon-Fenske viscometer)的方法而测定的在25℃下的运动粘度。
在25℃下的运动粘度为20mm2/s以下的硅油,可以为直链状、支链状、环状中任一种,作为具体实例,其为二甲基聚硅氧烷、甲基苯基聚硅氧烷、部分甲基被碳原子数为2~20的烷基取代的二甲基聚硅氧烷,其可以具有或不具有挥发性,但优选挥发性油剂且1气压下的沸点为260℃以下。
挥发性硅油可以为直链状、支链状、环状中的任一种,作为其具体实例,可列举出六甲基二硅氧烷、八甲基三硅氧烷、十甲基四硅氧烷、十二甲基五硅氧烷、七甲基乙基三硅氧烷、八甲基二乙基四硅氧烷等直链状硅油,甲基三(三甲基硅氧烷基)硅烷、四(三甲基硅氧烷基)硅烷等支链状硅油,八甲基环四硅氧烷、十甲基环五硅氧烷、十二甲基环六硅氧烷、四甲基四乙基环四硅氧烷等环状硅油。优选八甲基三硅氧烷、十甲基四硅氧烷、十二甲基五硅氧烷、甲基三(三甲基硅氧烷基)硅烷、四(三甲基硅氧烷基)硅烷、十甲基环五硅氧烷、十二甲基环六硅氧烷。
此时,(E)成分优选为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。这些化合物适用于本发明的微乳液组合物。
[F成分]
本发明中所使用的(F)成分为水。
[微乳液的制备方法]
进行乳化时,没有特别限定,但使用通常的乳化分散机即可,作为其实例可列举出均质分散器(homodisper)等高速旋转离心放散型搅拌机、高速搅拌机等高速旋转剪切型搅拌机、均化器等高压喷射式乳化分散机、胶体磨、超声波乳化机等。
在混合(A)~(F)这六种成分时,例如可使用相转变温度乳化法或D相乳化法等(乳化工序)。
相转变温度乳化法是指在HLB所相称的相转变温度(PIT)附近进行搅拌之后,通过快速冷却而生成微细乳液的方法。在PIT附近,由于油/水之间的表面张力显著下降,因此容易生成微细的乳化颗粒。
D相乳化法是指通过向表面活性剂添加水溶性的多元醇从而调整表面活性剂的HLB,在形成D相之后,添加油,经由O/D乳液,通过添加水而生成微细的乳液的方法。
本发明的微乳液期望历经过通过D相乳化法而形成的双连续结构。具体而言,通过在(A)HLB为8.0以上的聚醚改性有机聚硅氧烷、(B)HLB为5.0以下的聚醚改性有机聚硅氧烷、(C)甘油衍生物及作为(D)成分的多元醇的混合物中,在利用均质分散器施加剪切的条件下,缓慢掺合作为(E)成分的在25℃下的运动粘度为20mm2/s以下的硅油,从而形成D相。然后,通过缓慢添加规定量的(F)水,得到透明至半透明的微乳液。
微乳液具有油可溶于水中的胶束水溶液相、水可溶于油中的逆胶束油溶液相、水-油均呈连续结构的双连续相这三种类型,微乳液属于其中任一种相。
可通过下述方法确认微乳液组合物为水性还是油性。在将数滴微乳液组合物滴加至大量过量的水中其迅速均匀地分散,而滴加至大量过量的油中不分散时,其为水性,相反,将其滴加至大量过量的油中其迅速均匀地分散,而滴加至大量过量的水中不分散时,其为油性。油可溶于水中的胶束水溶液由于在添加至水中时迅速分散而添加至油中时不分散,因此其为水性。水可溶于油中的逆胶束油溶液相由于其添加至水中时不分散而添加至油中时迅速分散,因此其为油性。水-油均呈连续结构的双连续相,为水性或油性中的任一种。
此时,本发明的微乳液组合物优选添加至水中时会分散。即,优选油可溶于水中的胶束水溶液、水-油均呈连续结构的双连续相中的任一种。若为这样的微乳液组合物,则可适用于化妆品等用途。
进一步,可通过以下方法确认微乳液组合物为胶束水溶液相还是双连续相。
本发明的微乳液组合物优选为形成胶束水溶液相的组合物。具有胶束水溶液相可利用公知的冷冻断裂复型法通过观察电子显微镜照片进行确认。可更简单地通过色素的分散试验进行确认。色素的分散试验是通过分别添加水性色素与油性色素,当迅速混合于水及油这两者时,所得到的微乳液组合物为双连续相,当仅水性色素分散时,其为胶束水溶液相。
本发明的微乳液组合物的外观为透明至半透明。该微乳液的平均粒径或结构周期优选为200nm以下。在向由(A)~(E)构成的白色的D相凝胶中添加(F)水的阶段中,经由外观为透明的具有双连续结构的微乳液,在添加了全部(F)水时可得到外观为透明至半透明的水中油型微乳液。
在本发明的微乳液组合物中,优选含有0.1~10wt%的(A)聚醚改性有机聚硅氧烷,更优选含有1~10wt%。若(A)聚醚改性有机聚硅氧烷在上述范围内,则易于形成D相。
在本发明的微乳液组合物中,(C)、(D)、(E)、(F)各成分的含有比例没有特别限定,优选相对于10质量份的作为(A)成分的HLB为8.0以上的聚醚改性有机聚硅氧烷,作为(C)成分的甘油衍生物为0.1~10质量份,作为(D)成分的多元醇为5~100质量份,作为(E)成分的硅油为1~50质量份、(F)水为10~800质量份。
[微乳液组合物的物性]
本发明的微乳液组合物由于使用有机硅类表面活性剂作为活性剂、使用硅油作为油剂,因此无需使用阴离子型或阳离子型的表面活性剂,即具有来自活性剂的粘腻感或油腻感少、即使与底妆融合也能够保持轻薄的触感的特征。因此,通过以上述的微乳液组合物为基础而制成洁面剂,从而可得到涂布时易延展度良好、触感清爽、清洁效果高、清洗性及经时稳定性优异的洁面剂。
[化妆品]
本发明的微乳液组合物能够用于各种用途,特别是适合用作皮肤或毛发的所有外用化妆品的原料,进一步适用于清洁用途。此时,上述微乳液组合物的掺合量优选在化妆品整体的0.1~40质量%的范围内,更优选在0.1~10质量%的范围内。若为0.1质量%以上,则可得到充分的触感,若为40质量%以下,则使用感及清洁效果良好。
[其他成分]
在本发明的微乳液组合物及含有该微乳液组合物的化妆品中,还可以掺合作为其他成分的通常可用于化妆品中的各种成分。作为其他成分,例如可以含有作为(G)成分的除(E)成分以外的油剂、作为(H)成分的粉体、作为(I)成分的除(A)及(B)成分以外的表面活性剂、作为(J)成分的交联型有机聚硅氧烷、作为(K)成分的覆膜剂、作为(L)成分的其他添加剂。这些成分可以单独使用一种、或适宜地组合使用两种以上。这些成分,可根据化妆品的种类等进行适当选择而使用,此外其掺合量也可以根据化妆品的种类等而设为公知的掺合量。
(G)成分:除(E)成分以外的油剂
在本发明的化妆品中,可以根据其目的掺合作为(G)成分的选自除(E)成分以外的油剂中的一种或两种以上的油剂。只要是通常的用于化妆品的油剂,则可以使用固体、半固体、液状中的任一种,例如可以使用天然动植物油脂类及半合成油脂、烃油、高级醇、酯油、氟类油剂、紫外线吸收剂等。当掺合油剂时,油剂的掺合量没有特别限定,但优选为化妆品整体的1~95质量%,更优选为1~30质量%。进一步,(E)/(G)优选为10/0~5/5,进一步优选为10/0~8/2。当(E)/(G)为5/5以上时,微乳液的外观良好。
·天然动植物油脂类及半合成油脂
作为天然动植物油脂类及半合成油脂,例如可列举出鳄梨油、亚麻籽油、杏仁油、虫白蜡、紫苏油、橄榄油、可可脂、木棉蜡、榧子油、巴西棕榈蜡、鱼肝油、小烛树蜡、提纯小烛树蜡、牛脂、牛脚脂、牛骨脂、氢化牛脂、杏仁籽油、鲸蜡、氢化油、小麦胚芽油、芝麻油、稻米胚芽油、稻糠油、甘蔗蜡、山茶花油、红花油、乳木果油、中国桐油、肉桂油、荷荷巴蜡、角鲨烷、角鲨烯、紫虫胶蜡、海龟油、大豆油、茶籽油、山茶油、月见草油、玉米油、猪脂、菜籽油、日本桐油、米糠蜡、胚芽油、马脂、杏油、棕榈油、棕榈仁油、蓖麻油、氢化蓖麻油、蓖麻油脂肪酸甲酯、葵花油、葡萄籽油、月桂蜡、霍霍巴油、澳洲坚果油、蜂蜡、貂油、白池花籽油、棉籽油、棉蜡、木蜡、日本蜡仁油、蒙旦蜡、椰子油、氢化椰子油、椰子油脂肪酸三甘油酯、羊脂、落花生油、羊毛脂、液状羊毛脂、还原羊毛脂、羊毛脂醇、硬质羊毛脂、乙酸羊毛脂、乙酰化羊毛脂醇、羊毛脂脂肪酸异丙酯、POE羊毛脂醇醚、POE羊毛脂醇乙酸酯、羊毛脂脂肪酸聚乙二醇酯、POE氢化羊毛脂醇醚、卵黄油等。其中,POE表示聚氧乙烯。
·烃油
作为烃油,可列举出直链状、支链状及挥发性的烃油等,具体而言,可列举出地蜡(ozokerite)、α-烯烃低聚物、轻质异链烷烃、异十二烷、异十六烷、轻质液体异链烷烃、角鲨烷、合成角鲨烷、植物性角鲨烷、角鲨烯、纯地蜡(ceresin)、石蜡(paraffin)、固体石蜡(paraffin wax)、聚乙烯蜡、聚乙烯-聚丙烯蜡、(乙烯/丙烯/苯乙烯)共聚物、(丁烯/丙烯/苯乙烯)共聚物、流动石蜡、流动异构石蜡、姥鲛烷、聚异丁烯、氢化聚异丁烯、微晶蜡、凡士林、高级脂肪酸等。作为高级脂肪酸,可列举出月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山嵛酸、十一烯酸、油酸、亚油酸、亚麻酸、花生四烯酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)、异硬脂酸、12-羟基硬脂酸等。
·高级醇
作为高级醇,可列举出月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六烷基醇、油醇、异硬脂醇、己基十二醇、辛基十二醇、十六十八醇、2-癸基十四醇、胆固醇、植物甾醇、POE胆固醇醚、单硬脂甘油醚(鲨肝醇)、单油烯基甘油醚(鲨油醇)等。
·酯油
作为酯油,可列举出己二酸二异丁酯、己二酸2-己基癸酯、己二酸二-2-庚基十一烷基酯、单异硬脂酸N-烷基二酯、异硬脂酸异鲸蜡酯、三异硬脂酸三羟甲基丙烷、二-2-乙基己酸乙二醇酯、2-乙基己酸鲸蜡酯、三-2-乙基己酸三羟甲基丙烷、四-2-乙基己酸季戊四醇酯、辛酸鲸蜡酯、辛基十二烷基胶酯、油酸油醇酯、油酸辛基十二烷基酯、油酸癸酯、二辛酸新戊二醇、二癸酸新戊二醇、柠檬酸三乙酯、琥珀酸2-乙基己酯、乙酸戊酯、乙酸乙酯、乙酸丁酯、硬脂酸异鲸蜡酯、硬脂酸丁酯、癸二酸二异丙酯、癸二酸二-2-乙基己酯、乳酸鲸蜡酯、乳酸肉豆蔻酯、异壬酸异壬酯、异壬酸异十三烷基酯、棕榈酸异丙酯、棕榈酸2-乙基己酯、棕榈酸2-己基癸酯、棕榈酸2-庚基十一烷基酯、12-羟基硬脂酸胆固醇酯、二季戊四醇脂肪酸酯、肉豆蔻酸异丙酯、肉豆蔻酸辛基十二烷基酯、肉豆蔻酸2-己基癸酯、肉豆蔻酸肉豆蔻酯、二甲基辛酸己基癸酯、月桂酸乙酯、月桂酸己酯、N-月桂酰-L-谷氨酸-2-辛基十二烷基酯、月桂酰肌氨酸异丙酯、苹果酸二异硬脂酯、甘油酯油等。作为甘油酯油,可列举出乙酰甘油酯、三异辛酸甘油酯、三异硬脂酸甘油酯、三异棕榈酸甘油酯、三山嵛酸甘油酯、单硬脂酸甘油酯、二-2-庚基十一酸甘油酯、三肉豆蔻酸甘油酯、肉豆蔻酸异硬脂酸二甘油酯等。
·氟类油剂
作为氟类油剂,可列举出全氟聚醚、全氟萘烷、全氟辛烷等。
·紫外线吸收剂
作为紫外线吸收剂,例如可列举出对氨基苯甲酸等苯甲酸类紫外线吸收剂、邻氨基苯甲酸甲酯等邻氨基苯甲酸类紫外线吸收剂、水杨酸甲酯、水杨酸辛酯、水杨酸三甲基环己酯等水杨酸类紫外线吸收剂、对甲氧基肉桂酸辛酯等肉桂酸类紫外线吸收剂、2,4-二羟基二苯甲酮等二苯甲酮类紫外线吸收剂、尿刊酸乙酯等尿刊酸类紫外线吸收剂、4-叔丁基-4’-甲氧基-二苯甲酰基甲烷等二苯甲酰基甲烷类紫外线吸收剂、苯基苯并咪唑磺酸、三嗪衍生物等。紫外线吸收剂可含有紫外线吸收散射剂。作为紫外线吸收散射剂,例如可列举出微粒氧化钛、微粒含铁氧化钛、微粒氧化锌、微粒氧化铈及它们的复合物等对紫外线进行吸收散射的粉体,也可使用将这些对紫外线进行吸收散射的粉体预先分散在油剂中而成的分散物。
(H)成分:粉体
粉体只要是通常可掺合于化妆品中的原料则没有特别限定,例如,可列举出颜料、有机硅球状粉体等。当掺合粉体时,粉体的掺合量没有特别限定,但期望掺合化妆品整体的0.1~90质量%,进一步优选掺合1~35质量%。
作为颜料,只要是通常可用于彩妆化妆品的颜料则没有特别限制。例如可列举出滑石、云母、绢云母、合成金云母、硫酸钡、氧化铝、高岭土、二氧化硅、碳酸钙、氧化锌、氧化钛、红氧化铁、黄氧化铁、黑氧化铁、群青、普鲁士蓝、碳黑、低级氧化钛、钴紫、氧化铬、氢氧化铬、钛酸钴、氯氧化铋、钛-云母类珠光颜料等无机颜料,红色201号、红色202号、红色204号、红色205号、红色220号、红色226号、红色228号、红色405号、橙色203号、黄色205号、黄色4号、黄色5号、蓝色1号、蓝色404号、绿色3号等的锆、钡或铝色淀等有机颜料,叶绿素、β-胡萝卜素等天然色素,染料等。
另外,上述粉体也可以使用对颗粒表面进行了处理的粉体。此外,出于不损失制剂的耐水性的目的,其表面处理剂优选可赋予其疏水性的化合物,只要是能够赋予其疏水性则没有特别限定,可列举出有机硅处理剂、蜡类、石蜡类、全氟烷基与磷酸盐等的有机氟化合物、表面活性剂、N-酰基谷氨酸等氨基酸、硬脂酸铝、肉豆蔻酸镁等金属皂等处理剂。更优选作为有机硅处理剂的辛基硅烷(Shin-Etsu Chemical Co.,Ltd.制造:AES-3083)或三甲氧基甲硅烷基聚二甲基硅氧烷等硅烷类或甲硅烷基化剂、二甲基有机硅(Shin-EtsuChemical Co.,Ltd.制造:KF-96A系列)、甲基氢型聚硅氧烷(Shin-Etsu Chemical Co.,Ltd.制造:KF-99P、KF-9901等)、有机硅支链型有机硅处理剂(Shin-Etsu Chemical Co.,Ltd.制造:KF-9908、KF-9909等)等硅油、丙烯酸有机硅(Shin-Etsu Chemical Co.,Ltd.制造:KP-574、KP-541)等。进一步,上述表面疏水化处理剂可以单独使用一种或组合使用两种以上。作为实施了表面处理的着色颜料的具体实例,可列举出Shin-Etsu Chemical Co.,Ltd.制造:KTP-09系列、特别是KTP-09W、09R、09Y、09B等。作为含有疏水化处理微粒二氧化钛或疏水化处理微粒氧化锌的分散体的具体实例,可列举出Shin-Etsu Chemical Co.,Ltd.制造:SPD-T5、T6、T7、T5L、Z5、Z6、Z5L等。当掺合这些成分时,优选掺合为化妆品中的0.01~95质量%。
作为有机硅球状粉体,可列举出交联型有机硅粉末(即,由具有二有机硅氧烷单元的重复链进行交联而成的结构的有机聚硅氧烷形成的所谓有机硅橡胶粉末)、有机硅树脂颗粒(三维网状结构的聚有机倍半硅氧烷树脂颗粒)、有机硅树脂包覆有机硅橡胶粉末等。作为交联型有机硅粉末、有机硅树脂颗粒的具体实例,有以(聚二甲基硅氧烷/乙烯基聚二甲基硅氧烷)交联聚合物、聚甲基倍半硅氧烷等等名称而周知的化合物。这些成分以粉体或以含有硅油的溶胀物形式而进行市售,例如以KMP-598、590、591、KSG-016F等(均为Shin-Etsu Chemical Co.,Ltd.制造)的产品名称而进行市售。这些粉体,因球状粉体特有的滚动效应而赋予化妆品光滑性,改善使用感。这些粉体可使用一种或组合使用两种以上。
特别是在提高防止粘腻等触感的效果或修补皱纹或毛孔等凹凸效果等方面,优选有机硅树脂包覆硅橡胶粉末。作为有机硅树脂包覆硅橡胶粉末的具体实例,已知有以化妆品显示名称而定义的(乙烯基聚二甲基硅氧烷/聚甲基硅氧烷倍半硅氧烷)交联聚合物、(二苯基聚二甲基硅氧烷/乙烯基二苯基聚二甲基硅氧烷/倍半硅氧烷)交联聚合物、聚有机硅-22、聚有机硅-1交联聚合物等。这些有机硅树脂包覆硅橡胶粉末以KSP-100、101、102、105、300、411、441等(均为Shin-Etsu Chemical Co.,Ltd.制造)的产品名称而在进行市售。这些粉体可以使用一种或两种以上。当掺合该成分时,优选为化妆品中的0.01~95质量%。
(I)成分:除(A)·(B)成分以外的表面活性剂
作为除(A)·(B)成分以外的表面活性剂,有不含有机硅骨架的非离子型表面活性剂、阴离子型表面活性剂、阳离子型表面活性剂及两性表面活性剂、由格里芬法计算出的HLB为5.0~8.0的聚醚改性有机聚硅氧烷、聚甘油改性有机硅、交联型聚醚改性有机硅、及交联型聚甘油改性有机硅,但没有特别限制,只要是通常可用于化妆品中的化合物则均可使用,这些表面活性剂可以单独使用一种或适当组合使用两种以上。在这些表面活性剂中,就与(A)·(B)成分的相容性的角度而言,优选含有有机硅骨架的表面活性剂。
在这些表面活性剂中,优选亲水性的聚氧乙烯基、聚氧乙烯聚氧丙烯或聚甘油残基的含量占分子中的10~70%。作为这样的表面活性剂的具体实例,可列举出Shin-EtsuChemical Co.,Ltd.制造的KSG-210、240、310、320、330、340、320Z、350Z、710、810、820、830、840、820Z、850Z;KF-6012、6100、6104、6105、6106等。
掺合(I)成分时的掺合量优选为化妆品中的0.01~15质量%。
(J)成分:交联型有机聚硅氧烷
作为交联型有机聚硅氧烷,只要是可用于通常的化妆品中的化合物则没有特别限定,其可单独使用一种或适当组合使用两种以上。
该交联型有机聚硅氧烷与在上述(H)成分中所说明的有机硅球状粉体不同,其不具有球状形状。
此外,(J)成分与作为上述(I)成分的除(A)·(B)成分以外的表面活性剂不同,其优选为在其分子结构中不具有聚醚或聚甘油结构的化合物。此外,优选为通过以油剂进行溶胀而具有结构粘性的弹性体。作为具体实例,可列举出以化妆品显示名称而定义的(聚二甲基硅氧烷/乙烯基聚二甲基硅氧烷)交联聚合物、(聚二甲基硅氧烷/苯基乙烯基聚二甲基硅氧烷)交联聚合物、(乙烯基聚二甲基硅氧烷/月桂基聚二甲基硅氧烷)交联聚合物、(月桂基聚二甲基硅氧烷基乙基聚二甲基硅氧烷/双乙烯基聚二甲基硅氧烷)交联聚合物等。这些聚合物以包含在室温为液状的油的膨胀物的形式而市售,作为具体实例,可列举出Shin-Etsu Chemical Co.,Ltd.制造的KSG-15、1510、16、1610、18A、19、41A、42A、43、44、042Z、045Z、048Z等。
以固体成分计,掺合(J)成分时的掺合量优选为化妆品中的0.01~30质量%。
(K)成分:覆膜剂
作为覆膜剂,可同时使用现有的覆膜形成剂。作为现有的覆膜剂,只要是通常可掺合于化妆品中的原料则没有特别限定,具体而言,可使用聚乙烯醇、聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚丙烯酸烷基酯等乳胶类,糊精、烷基纤维素或硝基纤维素等纤维素衍生物,三(三甲基硅氧烷基)甲硅烷基丙基氨基甲酰支链淀粉等有机硅化多糖化合物,(丙烯酸烷基酯/聚二甲基硅氧烷)共聚物等丙烯酸-有机硅类接枝共聚物,三甲基硅氧烷基硅酸等有机硅树脂,有机硅改性聚降冰片烯、氟改性有机硅树脂等有机硅类树脂,氟树脂,芳香族类烃树脂,聚合物乳液树脂,萜烯树脂,聚丁烯,聚异戊二烯,醇酸树脂,聚乙烯吡咯烷酮改性聚合物,松香改性树脂,聚氨酯等。
其中,特别优选有机硅类覆膜剂,其中可使用三(三甲基硅氧烷基)甲硅烷基丙基氨基甲酰支链淀粉(作为溶解在溶剂中的市售产品,Shin-Etsu Chemical Co.,Ltd.制造:TSPL-30-D5、ID)、(丙烯酸烷基酯/聚二甲基硅氧烷)共聚物(作为溶解在溶剂中的市售产品,Shin-Etsu Chemical Co.,Ltd.制造:KP-543、545、549、550、545L等)、三甲基硅氧烷基硅酸(作为溶解在溶剂中的市售品,Shin-Etsu Chemical Co.,Ltd.制造:KF-7312J、X-21-5250等)、有机硅改性聚降冰片烯(作为溶解在溶剂中的市售品,Shin-Etsu Chemical Co.,Ltd.制造:NBN-30-ID等)、及有机硅氧烷接枝聚乙烯醇类聚合物等,但并不限于这些。
掺合(K)成分时的掺合量优选为化妆品中的0.1~20质量%。
(L)成分:其他添加剂
作为其他添加剂,可列举出油溶性凝胶剂、水溶性增粘剂、抑汗剂、杀菌防腐剂、香料、盐类、抗氧化剂、pH调节剂、螯合剂、清凉剂、消炎剂、美肤用成分(美白剂、细胞赋活剂、皮肤粗糙改善剂、血液循环促进剂、皮肤收敛剂、抗脂溢剂等)、维生素类、氨基酸类、核酸、激素、包合物等。这些(L)成分可以单独使用一种或适当组合使用两种以上。掺合(L)成分时的掺合量优选为化妆品中的0.1~20质量%。
·油溶性凝胶剂
作为油溶性凝胶剂,可列举出硬脂酸铝、硬脂酸镁、肉豆蔻酸锌等金属皂,N-月桂酰-L-谷氨酸、α,γ-二正丁胺等氨基酸衍生物,糊精棕榈酸酯、糊精硬脂酸酯、糊精2-乙基己酸棕榈酸酯等糊精脂肪酸酯,蔗糖棕榈酸酯、蔗糖硬脂酸酯等蔗糖脂肪酸酯,低聚果糖硬脂酸酯、低聚果糖2-乙基己酸酯等低聚果糖脂肪酸酯,单苯亚甲基山梨糖醇、二苯亚甲基山梨糖醇等山梨糖醇的苯亚甲基衍生物,二硬脂二甲铵锂蒙脱石、司拉氯铵水辉石、锂蒙脱石的有机改性粘土矿物等。
·水溶性增粘剂
作为水溶性增粘剂,可列举出阿拉伯树胶、黄芪胶、半乳聚糖、角豆树胶、胍尔豆胶、卡拉亚树胶、角叉菜胶、果胶、琼脂、榅桲籽(marmelo)、淀粉(稻米、玉米、马铃薯、小麦等)、海藻胶(algae colloid)、特兰特胶、刺槐豆胶等植物类高分子,黄原胶、葡聚糖、琥珀酰聚糖、普鲁兰多糖等微生物类高分子,胶原蛋白、酪蛋白、白蛋白、明胶等动物类高分子,羧甲基淀粉、甲基羟丙基淀粉等淀粉类高分子,甲基纤维素、乙基纤维素、甲基羟丙基纤维素、羧甲基纤维素、羟甲基纤维素、羟丙基纤维素、硝基纤维素、纤维素硫酸钠、羧甲基纤维素钠、结晶纤维素、阳离子化纤维素、纤维素粉等纤维素类高分子,海藻酸钠、海藻酸丙二醇酯等海藻酸类高分子,聚乙烯基甲醚、羧乙烯基聚合物等乙烯类高分子,聚氧乙烯类高分子,聚氧乙烯聚氧丙烯共聚物类高分子,聚丙烯酸钠、聚丙烯酸乙酯、聚丙烯酰胺、丙烯酰基二甲基牛磺酸盐共聚物等丙烯酸类高分子,聚乙烯亚胺,阳离子聚合物等其他合成水溶性高分子,膨润土、硅酸铝镁、蒙脱石、贝德石、绿脱石、皂石、水辉石、硅酸酐等无机类水溶性高分子等。
其中,优选使用选自植物类高分子、微生物类高分子、动物类高分子、淀粉类高分子、纤维素类高分子、海藻酸类高分子、聚氧乙烯聚氧丙烯共聚物类高分子、丙烯酸类高分子及无机类水溶性高分子中的一种或组合了两种以上的水溶性增粘剂。
·抑汗剂
作为抑汗剂,可列举出氯化羟铝、尿囊素氯羟基铝等羟基卤化铝、氯化铝等卤化铝、尿囊素铝盐、丹宁酸、柿子单宁、硫酸铝钾、氧化锌、对苯酚磺酸锌、烧明矾、四氯(Al/锆)水合物、三氯水合甘氨酸(Al/锆)等。作为表现出高效果的成分,特别优选羟基卤化铝、卤化铝及它们的氧卤化锆及羟卤化锆的络合物或混合物(例如、四氯(Al/锆)水合物、三氯水合甘氨酸(Al/锆))等。
·杀菌防腐剂
作为杀菌防腐剂,可列举出对羟基苯甲酸烷基酯、苯甲酸、苯甲酸钠、山梨酸、山梨酸钾、苯氧乙醇、咪唑烷基脲、水杨酸、异丙基甲基苯酚、苯酚、对氯间甲酚、六氯酚、苯扎氯铵、氯己定、三氯卡班、碘丙炔醇丁基氨甲酸酯、聚赖氨酸、感光素、银、植物提取物等。
·香料
作为香料有天然香料及合成香料。作为天然香料有从花、叶、木材、果皮等中分离的植物性香料,麝香、麝猫等动物性香料。作为合成香料,可列举出单萜等烃类,脂肪族醇、芳香族醇等醇类,萜醛、芳香族醛等醛类,脂环酮等酮类,萜烯酯等酯类,内酯类,酚类,氧化物类,含氮化合物类,缩醛类等。
·盐类
作为盐类,可列举出无机盐、有机酸盐、胺盐及氨基酸盐。作为无机盐,例如可列举出盐酸、硫酸、碳酸、硝酸等无机酸的钠盐、钾盐、镁盐、钙盐、铝盐、锆盐、锌盐等。作为有机酸盐,例如可列举出乙酸、脱氢乙酸、柠檬酸、苹果酸、琥珀酸、抗坏血酸、硬脂酸等有机酸类的盐。作为胺盐及氨基酸盐,例如可列举出三乙醇胺等胺类的盐、谷氨酸等氨基酸类的盐等。除此以外,还可使用透明质酸、硫酸软骨素等的盐、或进一步也可使用制剂处方中使用的酸-碱的中和盐等。
·抗氧化剂
作为抗氧化剂,没有特别限定,例如可列举出类胡萝卜素、抗坏血酸及其盐、抗坏血酸硬脂酸酯、乙酸生育酚、生育酚、对叔丁基苯酚、丁基羟基苯甲醚、二丁基羟基甲苯、植酸、阿魏酸、硫代牛磺酸、亚牛磺酸、亚硫酸盐、异抗坏血酸及其盐、绿原酸、表儿茶素、表没食子儿茶素、表没食子儿茶素没食子酸酯、芹菜素、山萘酚、杨梅素、槲皮素等。
·pH调节剂
作为pH调节剂,可列举出乳酸、柠檬酸、乙醇酸、琥珀酸、酒石酸、dl-苹果酸、碳酸钾、碳酸氢钠、碳酸氢铵等。
·螯合剂
作为螯合剂,可列举出丙氨酸、依地酸钠盐、聚磷酸钠、偏磷酸钠、磷酸等。
·清凉剂
作为清凉剂,可列举出L-薄荷脑、樟脑、薄荷醇乳酸酯等。
·消炎剂
作为消炎剂,可列举出尿囊素、甘草酸及其盐、甘草次酸及甘草次酸十八醇酯、氨甲环酸、薁等。
·美肤用成分
作为美肤用成分,可列举出胎盘提取液、熊果苷、谷胱甘肽、虎耳草提取物等美白剂,蜂王浆、感光素、胆固醇衍生物、小牛血液提取液等细胞活化剂,皮肤粗糙改善剂,壬酸香草酰胺、烟酸苄酯、烟酸β-丁氧基乙酯、辣椒素、姜酮、斑蝥酊、鱼石脂、咖啡因、丹宁酸、α-龙脑、生育酚烟酸酯、肌醇烟酸酯、环扁桃酯、桂利嗪、妥拉苏林、乙酰胆碱、维拉帕米、千金藤素、γ-谷维素等血液循环促进剂,皮肤收敛剂,硫、二甲噻蒽等抗脂溢剂等。
·维生素类
作为维生素类,可列举出维生素A油、视黄醇、乙酸视黄醇、棕榈酸视黄醇等维生素A类,核黄素、核黄素四丁酸酯、黄素腺嘌呤二核苷酸等维生素B2类,吡多醇盐酸盐、吡哆醇二辛酸酯、吡哆醇三棕榈酸酯等维生素B6类,维生素B12及其衍生物、维生素B15及其衍生物等维生素B类,L-抗坏血酸、L-抗坏血酸二棕榈酸酯、L-抗坏血酸-2-硫酸钠、L-抗坏血酸磷酸二酯二钾等维生素C类,麦角钙化醇、胆钙化醇等维生素D类,α-生育酚、β-生育酚、γ-生育酚、dl-α-生育酚乙酸酯、dl-α-生育酚烟酸酯、dl-α-生育酚琥珀酸酯等维生素E类,烟酸、烟酸苄酯、烟酰胺等烟酸类,维生素H、维生素P、泛酸钙、D-泛醇、泛酸醇乙基醚、乙酰基泛酸醇乙基醚等泛酸类,生物素等。
·氨基酸类
作为氨基酸类,可列举出甘氨酸、缬氨酸、亮氨酸、异亮氨酸、丝氨酸、苏氨酸、苯丙氨酸、精氨酸、赖氨酸、天冬氨酸、谷氨酸、胱氨酸、半胱氨酸、蛋氨酸、色氨酸等。
·核酸
作为核酸,可列举出脱氧核糖核酸等。
·激素
作为激素,可列举出雌二醇、乙烯基雌二醇等。
·包合物
作为包合物,可列举出环糊精等。
本发明中的化妆品没有特别限定,优选应用于洁面剂、护肤化妆品、护发化妆品、彩妆化妆品、防晒化妆品等。
作为本发明的化妆品的性状,可选择液状、霜状、固体状、膏状、凝胶状、慕斯状、喷雾状、粘土状、粉末状、棒状等各种性状。
实施例
以下,使用实施例对本发明进行具体说明,但本发明并不受下述实施例限定。
(实施例1~12、比较例1~10)
按照表1~2所示的组成制备乳液。以质量%表示掺合量。
[(A)成分]
作为(A)由格里芬法计算出的HLB为8.0以上的聚醚改性有机聚硅氧烷,使用KF-6013(HLB=10.0、Shin-Etsu Chemical Co.,Ltd.)。
[(B)成分]
作为(B)由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷,使用KF-6017(HLB=4.5、Shin-Etsu Chemical Co.,Ltd.)、KF-6028(HLB=3.5、Shin-EtsuChemical Co.,Ltd.)。
[(C)成分]
作为(C)甘油衍生物,使用Wilbride S-753(NOF CORPORATION)。
[(D)成分]
作为(D)成分,将作为除(C)成分以外的多元醇的甘油、乙基己基甘油加入到200mL的玻璃烧杯中并在室温下使用分散器搅拌而将其溶解。
[(E)成分]
将(D)成分搅拌溶解后,作为(E)成分的在25℃下的运动粘度为20mm2/s以下的硅油,使用作为运动粘度为4mm2/s的环状有机聚硅氧烷的十甲基环五硅氧烷(KF-995)、作为运动粘度为6mm2/s的直链二甲基聚硅氧烷的KF-96A-6cs、作为苯基改性有机聚硅氧烷的KF-56A(均为Shin-Etsu Chemical Co.,Ltd.)。
在室温下缓慢掺合上述(A)~(E)成分从而形成D相。
[(F)成分]
然后,在室温下缓慢添加规定量的(F)水,由此制备乳液。以质量%表示掺合量。
[(G)成分]
在实施例8~12中,按照表1所示的组成掺合角鲨烷、异十二烷、棕榈酸2-乙基己酯。
关于水分散性,即向10ml的水中添加1滴实施例1~12、比较例1~10中制备的乳液考察分散性(水分散性试验)。同样地,关于油分散性,向10ml的十甲基环五硅氧烷溶液中添加1滴微乳液考察分散性(油分散性试验)。将结果与25℃下的乳液的外观评价一同示于表1~2中。
对所得到的无色透明或半透明的微乳液(实施例1~12)进行色素溶解试验。作为试验方法,关于水溶性,通过向所得到的微乳液中添加水溶性色素(蓝色一号)的水溶液(浓度0.1质量%)而考察溶解性。此外,关于油溶性,与上述相同,向所得到的微乳液中添加油溶性色素(β胡萝卜素)的十甲基环五硅氧烷溶液(浓度1.0质量%)而考察溶解性。将结果与25℃下的乳液的外观评价一同示于表1中。
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[表2]
如上述表1所示,在实施例1~12中得到了外观为透明至半透明的微乳液。向水中滴加微乳液时,结果均得到均匀分散,因此确认到了在水中的分散性。
对依据上述表1所得到的微乳液实施色素溶解试验。由于仅水溶性色素溶解,因此确认到了微乳液为水溶性胶束结构(水中油型微乳液)。
如上述表2所示,在比较例1~10中得到了外观为白色浑浊的乳液或分离状态的液体。向水中滴加白色浑浊的乳液,结果均得到均匀分散,因此确认到了在水中的分散性。在比较例1中,没有同时使用作为相容剂的(B)而仅使用了(A)进行乳化,因此其相对于(E)的相容性变低而外观白色浑浊。比较例2~3由于不含作为D相的引发剂的(C),因此没有经由D相而白色浑浊。比较例4由于不含作为活性剂的(A),因此难以乳化而发生分离。比较例5~7由于未使用与(A)及(B)相容性高的(E)而单独使用了(G),因此未相容而发生了分离。在比较例8~10中,由于(A)/(B)的质量比不在1.0~15.0的范围内,因此乳液的外观发生了分离并白色浑浊。
使用以上述表1配比制备的实施例1、4、6、7、10、比较例1、3,对洁面剂进行性能评价(“涂布时的触感”、“清洁效果”、“清洗后的触感”、“保存稳定性”)。将结果示于表3。
[涂布时的触感]
由10名专业测试员,将2g上述制备的洁面剂涂布在左手腕上,用右手食指以6cm/秒的速度在3cm的距离内推揉1分钟。1分钟后按照下述标准(5~1)评价易延展度,以10名专业测试员的总分数进行表示。
<评价标准>
5:感觉到对皮肤的延展性非常好
4:感觉到对皮肤的延展性良好
3:感觉到对皮肤的延展性稍好
2:感觉到对皮肤的延展性稍差
1:感觉到对皮肤的延展性差
<基于总评分的5个评价等级>
S:总评分为40~50分
A:总评分小于30~40分
B:总评分小于20~30分
C:总评分小于10~20分
D:总评分小于10分
[清洁效果]
由10名专业测试员10,将2g上述制备的洁面剂涂布在涂了底妆的左手腕上,用右手食指以6cm/秒的速度在3cm的距离内推揉1分钟。然后,用水冲洗10秒后,按照下述标准(5~1)评价清洁效果,以10名专业测试员的总分数进行表示。
<评价标准>
5:底妆脱落得非常良好,切实感觉到了充分的清洁效果
4:底妆脱落得良好,切实感觉到了清洁效果
3:底妆脱落得稍好,略感觉到了清洁效果
2:底妆脱落得稍差,几乎未感觉到清洁效果
1:底妆脱落得差,未感觉到清洁效果
<基于总评分的5个评价等级>
S:总评分为40~50分
A:总评分小于30~40分
B:总评分小于20~30分
C:总评分小于10~20分
D:总评分小于10分
[清洗后的触感]
由10名专业测试员,将2g上述制备的洁面剂涂布在涂了底妆的左手腕上,用右手食指以6cm/秒的速度在3cm的距离内推揉1分钟。然后,用水冲洗10秒后,按照下述标准(5~1)评价包括皮肤上的残留感在内的触感,以10名专业测试员的总分数进行表示。
<评价标准>
5:明显没有残留感,感觉到了充分的清爽感
4:没有残留感,感觉到了清爽感
3:几乎没有残留感,略感觉到了清爽感
2:稍有残留感,几乎未感觉到清爽感
1:有残留感,未感觉到清爽感
<基于总评分的5个评价等级>
S:总评分为40~50分
A:总评分小于30~40分
B:总评分小于20~30分
C:总评分小于10~20分
D:总评分小于10分
[保存稳定性]
10g洁面剂填充于玻璃瓶中并密封,然后在50度及5度的恒温槽内保存一个月。对保存后的样本的外观进行确认,并按照下述标准评价保存稳定性。
<评价标准>
○:在任一温度条件下均未发现外观变化
×:在某一温度条件下发现了外观变化
[表3]
实施例1 | 实施例4 | 实施例6 | 实施例7 | 实施例10 | 比较例1 | 比较例3 | |
涂布时的触感 | S | S | S | A | A | C | D |
清洁效果 | S | A | S | S | S | B | C |
清洗后的触感 | A | A | S | A | A | C | D |
保存稳定性 | ○ | ○ | ○ | ○ | ○ | ○ | × |
在比较例1、3中没有得到充分的性能。在比较例1、3中,得到了外观白色浑浊、粒径大的水中油型乳液,其在皮肤上的延展性、清洁效果、清洗后的触感均不充分。特别是比较例3由于不含(C)成分而保存稳定性低且发生了分离。
另一方面,可知作为本发明的实施例的实施例1、4、6、7、10的微乳液组合物均可用作涂布时的易延展度良好、触感清爽、清洁效果高、清洗性优异且保存稳定性良好的洁面剂。
另外,本发明并不受上述实施方案的限定。上述实施方案为例示,与本发明的权利要求书所记载的技术构思具有实质相同的组成并发挥相同作用效果的技术方案均包含在本发明的保护范围内。
Claims (16)
1.一种微乳液组合物,其特征在于,其含有:
(A)下述通式(1)所表示的由格里芬法计算出的HLB为8.0以上的聚醚改性有机聚硅氧烷,
[化学式1]
式(1)中,R1为同种或不同种的碳原子数为1~30的烷基、芳基、芳烷基、或这些基团的卤素取代基、氨基取代基或羧基取代基,
R2为同种或不同种的下述通式(2)所表示的聚氧化烯基,
[化学式2]
-(CH2)2-C1H21-O-(C2H4O)b(C3H6O)cR5 (2)
式(2)中,R5为未取代或取代的一价烃基或氢原子,l、b及c为满足0≤l≤15、2≤b≤200、0≤c≤200、3≤b+c≤200的整数,
R3为同种或不同种的下述通式(3)~(6)中任一通式所表示的基团,
[化学式3]
-(CH2)2-CmH2m-(SiOR1 2)d-SiR1 3 (3)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 3)3-e1 (4)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 3)3-e2)3-e1 (5)
-(CH2)2-CmH2m-SiR1 e1-(OSiR1 e2(OSiR1 e3(OSiR1 3)3-e3)3-e2)3-e1 (6)
式(3)~(6)中,R1与上述R1相同,m、d及e1~e3为满足0≤m≤5、0≤d≤500、0≤e1≤2、0≤e2≤2、0≤e3≤2的整数,
R4相互独立地为R1、R2或R3,a1为满足0≤a1≤100、a2为满足0≤a2≤50、a3为满足0≤a3≤50的数,其中,a2为0时R4中的至少一个为R2;
(B)下述通式(7)所表示的由格里芬法计算出的HLB为5.0以下的聚醚改性有机聚硅氧烷,
[化学式4]
式(7)中,R1、R2、R3、R4与上述对R1、R2、R3、R4的定义相同,a4为满足0≤a4≤100、a5为满足0≤a5≤50、a6为满足0≤a6≤50的数,其中,a5为0时R4中的至少一个为R2;
(C)下述通式(8)所表示的甘油衍生物,
[化学式5]
Gly-{O-(PO)f(EO)g(BO)hH}3 (8)
式(8)中,Gly为自甘油中去除了羟基的残基,PO为氧化丙烯基,EO氧化乙烯基,f及g分别为PO及EO的平均加成摩尔数,f+g表示1~30的值,PO与EO的质量比(PO/EO)为1/5~5/1,BO表示碳原子数为4的氧化烯基,h为BO的平均加成摩尔数,表示1~5的值;
(D)除所述(C)以外的多元醇;
(E)25℃下的运动粘度为20mm2/s以下的硅油;
(F)水,
所述(A)的质量与所述(B)的质量之比(A)/(B)满足1.0~15.0,所述微乳液组合物的25℃下的外观为透明至半透明。
2.根据权利要求1所述的微乳液组合物,其特征在于,
所述(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.0以上且13.0以下。
3.根据权利要求2所述的微乳液组合物,其特征在于,
所述(A)聚醚改性有机聚硅氧烷的由格里芬法计算出的HLB为8.5以上且10.5以下。
4.根据权利要求3所述的微乳液组合物,其特征在于,
所述(A)聚醚改性有机聚硅氧烷为在化妆品显示名称中记为PEG-9聚二甲基硅氧烷的化合物。
5.根据权利要求1所述的微乳液组合物,其特征在于,
其为将所述微乳液组合物添加至水中时能够分散的组合物。
6.根据权利要求2所述的微乳液组合物,其特征在于,
其为将所述微乳液组合物添加至水中时能够分散的组合物。
7.根据权利要求3所述的微乳液组合物,其特征在于,
其为将所述微乳液组合物添加至水中时能够分散的组合物。
8.根据权利要求4所述的微乳液组合物,其特征在于,
其为将所述微乳液组合物添加至水中时能够分散的组合物。
9.根据权利要求1~8中任一项所述的微乳液组合物,其特征在于,
相对于所述微乳液组合物,含有0.1~10wt%的所述(A)聚醚改性有机聚硅氧烷。
10.根据权利要求1~8中任一项所述的微乳液组合物,其特征在于,所述(D)多元醇为甘油或甘油的衍生物。
11.根据权利要求9所述的微乳液组合物,其特征在于,
所述(D)多元醇为甘油或甘油的衍生物。
12.根据权利要求1~8中任一项所述的微乳液组合物,其特征在于,
所述(E)为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。
13.根据权利要求9所述的微乳液组合物,其特征在于,
所述(E)为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。
14.根据权利要求10所述的微乳液组合物,其特征在于,
所述(E)为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。
15.根据权利要求11所述的微乳液组合物,其特征在于,
所述(E)为选自十甲基环五硅氧烷、二甲基聚硅氧烷、甲基苯基聚硅氧烷中的一种以上。
16.一种化妆品,其中,该化妆品含有权利要求1~15中任一项所述的微乳液组合物。
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