CN114632016A - 一种防晒乳液组合物 - Google Patents

一种防晒乳液组合物 Download PDF

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CN114632016A
CN114632016A CN202111641010.XA CN202111641010A CN114632016A CN 114632016 A CN114632016 A CN 114632016A CN 202111641010 A CN202111641010 A CN 202111641010A CN 114632016 A CN114632016 A CN 114632016A
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唐新宜
黄思丽
曹高
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Guangdong Pharmaceutical University
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Abstract

本发明公开了一种防晒乳液组合物，其特征在于，按重量百分比计，包括以下组分：按重量百分比计，包括以下组分：防晒剂8‑30%；助溶剂 0.5‑1.5%；乳化剂1.0‑3.0%；成膜剂0.5‑2%；螯合剂0.5‑1%；增稠剂0.1‑0.7%；中和剂0.1‑2%防腐剂0.2‑1.0%水补充至100%；所述的乳化剂选自聚氧乙烯‑2(21)硬脂醇醚、硬脂酸甘油酯/PEG‑100 硬酯酸酯中的一种或两种；所述的成膜剂选自丙烯酸酯共聚物及其衍生物成膜剂、乙烯基吡咯烷酮衍生物类成膜剂、有机硅树脂成膜剂、纤维素衍生物成膜剂中的至少一种。本发明通过选取特殊成分的乳化剂和成膜剂，使得防晒乳液组合物在涂抹后能够形成特殊形状的保护膜，提升防晒性、防水性。

Description

一种防晒乳液组合物
技术领域
本发明涉及日化用品技术领域，特别是涉及一种防晒乳液组合物。
背景技术
近年来，臭氧层破坏问题得到社会各界的重视。臭氧层是阻隔紫外线至关重要的一道屏障，能阻隔、吸收大部分紫外线。人体长期暴露在紫外线下，皮肤表皮细胞会损坏，皮肤变得黝黑、干燥，会使肌肤发炎、灼伤，甚至诱发皮肤肿瘤和皮肤磷状上皮癌等问题。采取一些方法来阻隔或吸收紫外线，防止肌肤被晒黑、晒伤，这就是所谓的防晒。1944年本杰明格林制作的防晒油拉开了“化学防晒”的序幕。1962年，弗兰兹格瑞特提出了阳光防护系数(Sun Protection Factor，SPF)的概念，从此防晒能力可以用数值来衡量。
防晒产品的发展离不开防晒剂的作用，常见的防晒剂主要有两类，物理防晒剂和化学防晒剂。其中，物理防晒剂主要有二氧化钛、氧化锌、滑石粉等；化学防晒剂主要有甲氧基肉桂酸辛酯、水杨酸辛酯、2-羟基-4-甲氧基二苯甲酮等。物理防晒剂抗紫外线的原理以反射、散射为主，这主要与粒子的粒径有关。化学防晒剂抗紫外线的原理主要是吸收紫外线，并能将紫外线的能量转化为热能释放出来。
目前防晒产品的发展趋势主要有以下几个方面：提高防晒产品的防水性、改变乳液的体系、简化防晒产品防水测试的方法、开发新型的防晒剂、复合使用防晒剂即偏向于UVA和UVB全波段覆盖等。随着生活水平的提高，户外活动，游泳等日渐频繁。紫外线辐射可以穿透水，因此防晒产品在水中对皮肤的保护能力及其抗水性是非常重要的；防水能力较弱的防晒产品接触到汗水等液体时，防晒能力就会大打折扣。因此，提高防晒产品的防水防汗能力势在必行。
发明内容
本发明的目的在于，提供一种涂抹后形成特殊薄膜的防晒乳液，具有防晒性、防水性好的优点。
本发明是通过以下技术方案实现的：
一种防晒乳液组合物，按重量百分比计，包括以下组分：
Figure BDA0003442925050000011
Figure BDA0003442925050000021
所述的乳化剂选自聚氧乙烯-n硬脂醇醚、硬脂酸甘油酯/PEG-100硬酯酸酯(乳化剂A165)中的一种或两种；
所述的成膜剂选自丙烯酸酯共聚物及其衍生物成膜剂、乙烯基吡咯烷酮衍生物类成膜剂、有机硅树脂成膜剂、纤维素衍生物成膜剂中的至少一种。
优选的，助溶剂0.6-1％，乳化剂1.3-2.5％，成膜剂0.7-1.6％，增稠剂0.2-0.4％。
优选的，所述的成膜剂选自乙烯基吡咯烷酮衍生物类成膜剂中的至少一种。
具体的，所述的乙烯基吡咯烷酮衍生物类选自聚乙烯吡咯烷酮、乙烯基吡咯烷酮/醋酸乙烯共聚物中的至少一种；
具体的，丙烯酸酯共聚物及其衍生物成膜剂的商用牌号为陶氏EPITEX 66、赢创SP-13中的至少一种。
所述的乙烯基吡咯烷酮衍生物类成膜剂选自聚乙烯吡咯烷酮(PVP K30)、乙烯基吡咯烷酮/醋酸乙烯共聚物(PVP-VA)中的至少一种；所述的有机硅树脂成膜剂选自迈图Silform flexible Resin(SFR)有机硅树脂；所述的纤维素衍生物成膜剂选自陶氏化学乙基纤维素EC。
优选的，按重量百分比计，还包括0.15-0.6％的双十八烷基三甲基氯化铵(Varisoft TA100)。
所述的助溶剂选自十六十八醇、硬脂酸中的至少一种；优选的，所述的助溶剂选自十六十八醇。
优选的，所述的乳化剂选自聚氧乙烯-n硬脂醇醚；所述的聚氧乙烯-n硬脂醇醚选自聚氧乙烯-2(21)硬脂醇醚(乳化剂72/721)、聚氧乙烯-6(25)硬脂醇醚(乳化剂A6/A25)至少一种。
所述的防晒剂选自甲氧基肉桂酸辛酯(Parsol MCX)、奥克立林(Parsol 340)、二苯酮-3、二苯酮-4、胡莫柳酯、亚甲基双苯并三唑基四甲基丁基酚、乙基己基三嗪酮、聚硅氧烷-15、双-乙基己氧苯酚甲氧苯基三嗪、水杨酸辛酯、4-甲基亚苄基樟脑、二氧化钛中的至少一种。
所述的螯合剂选自乙二胺四乙酸二钠。
所述的增稠剂选自丙烯酸树脂增稠剂、聚丙烯酰胺类增稠剂、汉生胶中的至少一种；所述的丙烯酸树脂增稠剂选自路博润卡波U21、卡波940、卡波941、卡波U20中的至少一种。所述的聚丙烯酰胺类增稠剂选自SEPIGEL305。
优选的，所述的丙烯酸树脂增稠剂选自路博润卡波U21。
所述的中和剂选自三乙醇胺、氢氧化钠、氢氧化钾中的至少一种；
防腐剂可以选自舒美euxyl K350。
本发明防晒乳液组合物的制备方法：
1)分别准确称取A相，B相和C相后待用(A相包括助溶剂、防晒剂、乳化剂，B相包括部分水，增稠剂和螯合剂，C相包括部分水、中和剂)；
2)A相，B相分别加热到75～85℃，搅拌均匀后待用；
3)将B相迅速加入A相后均质(5000转/分，3分钟)，乳化过程注意保温在80℃；
4)乳化完成后降温至45℃，加入C相继续搅拌(3000转/分，3分钟)；
5)将D相防腐剂和E相成膜剂加入乳液中继续搅拌(3000转/分，1分钟)并降温至40℃停止搅拌。
与现有技术相比，本发明具有如下有益效果
对于防晒乳液涂抹后防晒性能的好坏、耐水性、持久性、涂抹后的舒适性的探索，现有技术主要集中在1.通过探索新型防晒剂、复配防晒剂等提高防晒性，2.通过乳化剂、增稠剂的选择与复配提升乳液稳定性，3.通过成膜剂的选择与复配提升耐水性和持久性，4.通过选取温和乳化剂、增稠剂的调配来改善涂抹后的舒适性。
经研究发现，防晒组合物防晒性能、耐水、持久性、涂抹后的舒适性的好坏，不仅与防晒剂的类型相关，也与防晒剂涂抹后成膜的特性有关。若防晒膜厚实，细微皱褶较多，则防晒性和防水性较好；若防晒膜脆薄，平整，则防晒性和防水性较差。防晒膜较厚实可减少紫外线的穿透，水洗后仍然有一定的保护作用；防晒膜上褶皱的结构可增加紫外线的散射，从而保护皮肤。而防晒膜的形成与特性，不仅与成膜剂(低分子类共聚物)有关，而且与溶剂、乳化剂等有关。当防晒乳液涂抹到皮肤表面后，溶剂等易挥发物质会逐渐蒸发掉，不易挥发或难挥发的成分与成膜剂收缩在皮肤表面形成薄膜。因此溶剂的蒸发、不挥发成分浓缩在成膜剂形成的网之前，都会影响薄膜的形成与薄膜的构造，进而影响防晒性与防水性等。本发明通过选取特殊成分的乳化剂、成膜剂、溶剂，使得防晒乳液组合物在涂抹后能够形成特殊形状的保护膜，提升防晒性、防水性。
附图说明
图1：实施例1防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜厚实，细微皱褶较多
图2：实施例2防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜厚实，细微皱褶较多
图3：实施例3防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜厚实，细微皱褶较多
图4：对比例1防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜脆薄，平整。
图5：对比例2防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜脆薄，平整。
图6：对比例3防晒乳液涂抹后形成的防晒膜电镜照片(放大100倍)，防晒膜脆薄，平整。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
本发明实施例和对比例所用原料来源于市售产品。
实施例和对比例防晒乳液组合物的制备方法：
1)分别准确称取A相，B相和C相后待用(A相包括助溶剂、防晒剂、乳化剂，B相包括部分水，增稠剂和螯合剂，C相包括部分水、中和剂)；
2)A相，B相分别加热到75～85℃，搅拌均匀后待用；
3)将B相迅速加入A相后均质(5000转/分，3分钟)，乳化过程注意保温在80℃；
4)乳化完成后降温至45℃，加入C相继续搅拌(3000转/分，3分钟)；
5)将D相防腐剂和E相成膜剂加入乳液中继续搅拌(3000转/分，1分钟)并降温至40℃停止搅拌。
各项性能测试方法：
(1)防晒膜电镜照片：在PMMA板(Ra＝5μm，Sa＝6μm，50.3mm×50.3mm)上均匀点上0.12g防晒乳，并用戴有乳胶指套的手指快速均匀地涂布，涂抹后有0.1g防晒乳液均匀分布于PMMA板上，将涂抹后的样品板放在温度为25℃，湿度为60％的环境中自然干燥30min，然后将样品板置于显微镜下观察防晒乳的成膜形态。
(2)SPF：采用美国Solar light公司生产的SPF-290AS防晒指数测试仪对防晒样品的SPF值进行体外测试，软件版本为WinSPF 4.2，测试具体方法如下。先测定载体的空白膜作为本底曲线，然后用1mL注射器吸取样品，并在Transpore MTR型透明胶带上均匀点加，用戴有乳胶指套的手指快速均匀地涂布在薄膜上，使膜表面样品以2mg/cm2分布。将涂抹后的样品板放在温度为25℃、湿度为60％的环境中自然干燥15min，然后将样品板放在相应位置进行测试。使用防晒系数分析仪SPF-290AS在透明胶带上选取9点测试，并计算SPF平均值。
测试方法基于ISO 24443。测试方法和参数见下表。
Figure BDA0003442925050000051
Figure BDA0003442925050000061
(3)防水性评价：参考许慧慧等人提出的抗水性能仪器测试法，并结合2015版化妆品安全技术规范中的抗水性能标准，设计了以下防水测试方法：
选取相应的防晒乳液，然后用1mL注射器吸取并在3M透明膜带上均匀点加样品(3M胶带贴在石英板上)，并用戴有乳胶指套的手指快速均匀地涂布，使防晒乳液以2mg/cm2均匀分布在3M透明膜带上，在温度为25℃、湿度为60％的环境中静置15min后，将涂抹防晒乳液的3M透明膜带及石英板浸入装满2L蒸馏水的大烧杯中，将大烧杯放置在37℃恒温振荡水浴槽中，振荡频率为100次/min，记录时间为20min振荡(每次振荡后更换杯中水)，20min静置，再20min振荡，20min静置，即样品浸水40min后取出自然干燥20min，然后用SPF-290AS测定SPF值。重复上述步骤，即80分钟后再次测定。
表1：实施例防晒乳液组合物各组分配比(重量百分比)
Figure BDA0003442925050000062
Figure BDA0003442925050000071
续表1：
Figure BDA0003442925050000072
Figure BDA0003442925050000081
续表1：
Figure BDA0003442925050000082
由实施例1与实施例5的对比可知，双十八烷基三甲基氯化铵的添加能够显著提升防水性。
由实施例1与实施例6的对比可知，助溶剂优选十六十八醇，不仅初始SPF更高，并且防水性也更好。
由实施例1与实施例7/8的对比可知，乳化剂优选聚氧乙烯-n硬脂醇醚。
由实施例1与实施例9-12的对比可知，成膜剂优选乙烯基吡咯烷酮衍生物类成膜剂。
由实施例1与实施例13-16的对比可知，优选的配比下不仅初始SPF更高，并且防水性也更好。
表2：对比例防晒乳液组合物各组分配比(重量百分比)
Figure BDA0003442925050000091
由实施例1与对比例1对比可知，添加助溶剂能够提升初始SPF，尤其是能够提升防水性。
由实施例1与对比例2/3可知，当助溶剂含量过高或过低时，也无法得到本发明的技术效果。
由实施例1与对比例4/5可知，当其他组分的含量不在本发明范围内时，成膜性不好使得防水性差。

Claims (10)

1.一种防晒乳液组合物，其特征在于，按重量百分比计，包括以下组分：
防晒剂 8-30%；
助溶剂 0.5-1.5%
乳化剂 1.0-3.0%；
成膜剂 0.5-2%；
螯合剂 0.5-1%；
增稠剂 0.1-0.7%；
中和剂 0.1-2%
防腐剂 0.2-1.0%
水 补充至100%；
所述的乳化剂选自聚氧乙烯-n硬脂醇醚、硬脂酸甘油酯/PEG-100硬酯酸酯中的一种或两种；
所述的成膜剂选自丙烯酸酯共聚物及其衍生物成膜剂、乙烯基吡咯烷酮衍生物类成膜剂、有机硅树脂成膜剂、纤维素衍生物成膜剂中的至少一种。
2.根据权利要求1所述的防晒乳液组合物，其特征在于，
助溶剂 0.6-1%，
乳化剂 1.3-2.5%，
成膜剂 0.7-1.6%，
增稠剂 0.2-0.4%。
3.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的成膜剂选自乙烯基吡咯烷酮衍生物类成膜剂中的至少一种；所述的乙烯基吡咯烷酮衍生物类成膜剂选自聚乙烯吡咯烷酮、乙烯基吡咯烷酮/醋酸乙烯共聚物中的至少一种。
4.根据权利要求1或2所述的防晒乳液组合物，其特征在于，按重量百分比计，还包括0.15-0.6%的双十八烷基三甲基氯化铵。
5.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的助溶剂选自十六十八醇、硬脂酸中的至少一种；优选的，所述的助溶剂选自十六十八醇。
6.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的乳化剂选自聚氧乙烯-n硬脂醇醚；所述的聚氧乙烯-n硬脂醇醚选自聚氧乙烯-2(21)硬脂醇醚、聚氧乙烯-6（25）硬脂醇醚至少一种。
7.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的防晒剂选自甲氧基肉桂酸辛酯、奥克立林、二苯酮-3、二苯酮-4、胡莫柳酯、亚甲基双苯并三唑基四甲基丁基酚、乙基己基三嗪酮、聚硅氧烷-15、双-乙基己氧苯酚甲氧苯基三嗪、水杨酸辛酯、4-甲基亚苄基樟脑、二氧化钛中的至少一种。
8.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的螯合剂选自乙二胺四乙酸二钠。
9.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的增稠剂选自聚丙烯酰胺类增稠剂、汉生胶中的至少一种；所述的聚丙烯酰胺类增稠剂选自SEPIGEL305。
10.根据权利要求1或2所述的防晒乳液组合物，其特征在于，所述的中和剂选自三乙醇胺、氢氧化钠、氢氧化钾中的至少一种。
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