CN115006311A - 一种透明双相防晒组合物及其制备方法 - Google Patents
一种透明双相防晒组合物及其制备方法 Download PDFInfo
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- CN115006311A CN115006311A CN202210798001.XA CN202210798001A CN115006311A CN 115006311 A CN115006311 A CN 115006311A CN 202210798001 A CN202210798001 A CN 202210798001A CN 115006311 A CN115006311 A CN 115006311A
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Abstract
本发明公开了一种透明双相防晒组合物及其制备方法,所述防晒组合物,包括澄清透明的呈连续相的水相和澄清透明的呈非连续相的油相,其中油相以颗粒形式均匀分布于水相,所述水相包括水相增稠剂,所述油相包括油溶性紫外防御剂、润肤剂和油相增稠剂。本发明制得的防晒组合物具有稳定性好、肤感清爽、涂抹均匀、防晒能力强的特点。
Description
技术领域
本发明涉及一种防晒组合物,特别是一种透明双相防晒组合物及其制备方法。
背景技术
长期暴露于紫外辐射下,会使皮肤发生非保护性的持续的黑化,并且加速皮肤老化,同时也会引起红斑,甚至引发皮肤癌等严重病症。因此,对皮肤采取光保护措施非常重要。目前通常会采用防晒类化妆品来对皮肤进行保护。
防晒类化妆品是指具有屏蔽或吸收紫外线作用的化妆品,是抵御紫外线的重要途径之一。防晒组合物对紫外线的防护程度与所含紫外防御剂的含量和种类相关,为达到较高的防晒能力,需要添加高含量的紫外防御剂,而大量紫外防御剂的混配,往往带来较为粘腻的肤感。现有防晒产品大多为油包水、水包油或者无水体系。油包水型防晒组合物,油相比例高于水相比例,水相比例通常不能过高,否则体系稳定性较差,而且涂布于皮肤表面,往往会感到发粘、油腻。水包油型防晒组合物,油相比例低于水相比例,虽然肤感较为清爽,但其抗迁移能力较弱,防水性能较差。而无水体系防晒组合物一般为全油体系,如透明防晒棒状,油膜感较重,且硬度高,不易涂抹,肤感不易接受。
除此之外,还有一部分防晒产品为双相形式。目前常见的双相防晒组合物,其静置时水相和油相各自为连续相,具有两个不同的层,使用时需要摇匀后涂抹到皮肤表面,非常容易出现涂抹混合不均匀的情况,导致实际防晒功效减弱,且无法精准控制用量的问题。
公开号为CN111991246A,公开日为2020年11月27日的中国发明公开了一种泡泡水粉底及其制备方法,其水粉底包括水、保湿剂、水相增稠剂、油相增稠剂,得到将修颜成分完整包裹于微囊之中,均匀分散在精化水啫喱中的保湿精华水粉底。但是上述粉底的成分中不含紫外线吸收剂,其水相含量超过75%,含量高,油相少,且粘度低,制备工艺要求转速8000rpm。此方法制备工艺要求高,水相和油相的比例有一定先置,若加入10%油溶性紫外线防晒剂,不能达到SPF50的防晒效果,且因其粘度低难以长期稳定。
因此,目前还未研究出一种稳定的、肤感舒适、容易涂抹、防晒能力强的双相分布均匀的防晒组合物。
发明内容
本发明的目的在于,提供一种透明双相防晒组合物及其制备方法。本发明制得的防晒组合物具有稳定性好、肤感清爽、涂抹均匀、防晒能力强的特点。
本发明的技术方案:一种透明双相防晒组合物,所述防晒组合物,包括澄清透明的呈连续相的水相和澄清透明的呈非连续相的油相,其中油相以颗粒形式均匀分布于水相,所述水相包括水相增稠剂,所述油相包括油溶性紫外防御剂、润肤剂和油相增稠剂。
前述的一种透明双相防晒组合物中,水相增稠剂的质量占水相总质量的1~4%;油溶性紫外防御剂的质量占防晒组合物总质量的1~25%;润肤剂的质量占防晒组合物总质量的2~30%;油相增稠剂的质量占油相总质量的1.3~5%。
前述的一种透明双相防晒组合物中,所述水相和油相的质量比为0.6:1~10:1。
前述的一种透明双相防晒组合物中,所述水相增稠剂包括丙烯酸(酯)类交联聚合物-2钠、聚丙烯酰基二甲基牛磺酸钠和丙烯酰二甲基牛磺酸铵/VP共聚物中的任意两种或三种组合。
前述的一种透明双相防晒组合物中,所述水相增稠剂还包括柠檬果皮粉、透明质酸钠、汉生胶、丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物、卡波姆、纤维素中的任意一种或多种。
前述的一种透明双相防晒组合物中,所述油相增稠剂包括二丁基月桂酰谷氨酰胺和二丁基乙基己酰基谷氨酰胺。
前述的一种透明双相防晒组合物中,所述油相还包括助溶剂,所述助溶剂为多元醇或者异构醇。
所述油溶性紫外防御剂采用具有UV全波段防护功效的紫外防御剂。
前述的一种透明双相防晒组合物中,所述油溶性紫外防御剂采用具有UV全波段防护功效的紫外防御剂。
前述的一种透明双相防晒组合物中,所述润肤剂包括己二酸二丁酯、丁基辛醇水杨酸酯、月桂酸己酯中的任意一种或多种组合。
上述的明双相防晒组合物的制备方法,包括以下操作步骤:
a、将水相增稠剂分散于水相中,加热至60~100℃,保温10~15min,低速均质15~30min,得均一透明液体,为水相;
b、将油溶性紫外防御剂与润肤剂混合,加热至60~100℃,搅拌混合均匀,得透明均一液体,为A品;
c、向A品中加入油相增稠剂,加热至60~90℃,再加入助溶剂,保温10~15min,搅拌混合至透明均一,得油相;
d、将油相加入水相中,加热融解后搅拌降温至室温,得透明双相防晒组合物。
前述的制备方法中,加热速度为0.5~1℃/min,降温速度为1~2℃/min,步骤a中的均质速度为1800~2200rpm,步骤b和步骤c中的搅拌速度为450~550rpm,步骤d中的搅拌速度为80~120rpm。
与现有技术相比,本发明的有益效果为:
本发明防晒组合物包含水相和油相两相,水相由水溶性、亲水性或水分散性等物质组成,油相由油溶性、亲油性或油分散性等物质组成。在油相增稠剂和水相增稠剂的作用下,油相以颗粒形式稳定均匀分布于水相中,形成水相为连续相,油相为非连续相,且水、油两相外观均澄清透明。静置时该组合物并不会出现分层现象,具备较高粘度,其中的水相粘度为40000~100000cp。
由于油相以颗粒形式稳定均匀分布于水相中,因此组合物中的水、油两相比例没有过多限制。即使油相的比例远高于水相的比例,组合物整体依旧具备良好的稳定性和相对清爽的肤感,为原料的选择和调整提供更大的空间。
水相增稠剂采用具备高增稠效果、澄清透明外观、肤感清爽等特点的水溶性物质,采用丙烯酸(酯)类交联聚合物-2钠、聚丙烯酰基二甲基牛磺酸钠和丙烯酰二甲基牛磺酸铵/VP共聚物中的任意两种或者三者复配,可在达到良好的增稠效率的同时保持透明外观和肤感舒适度。
油相增稠剂采用二丁基月桂酰谷氨酰胺与二丁基乙基己酰基谷氨酰胺搭配,两者各自的单体通过氢键作用自聚、纤维化、最终形成稳定的网状结构,将油分固定于该结构中,形成油凝胶。两者协同作用可使油相达到较高的透明度外观和较高硬度;而采用的蓖麻油/IPDI共聚物可进一步促进油相的凝胶化。
利用凝胶化技术将油溶性紫外防御剂固定于油相网状结构中,可减少防晒剂引发的刺激性反应,降低油溶性紫外防御剂的化学降解性能从而提高体系的稳定性。同时该结构可通过散射紫外线从而提高防晒效果,对防晒起到协同增效的作用。
采用的助溶剂与二丁基月桂酰谷氨酰胺、二丁基乙基己酰基谷氨酰胺在结构上具有相似相溶相应,可以进一步降低其融化温度,使得组合物在油相可于较低的温度60~90℃下进行制备融化,避免过高温度加热破坏组合物中有效物质的功效,还起到安全性高和节约能源的作用。
油溶性紫外防御剂采用多种防晒剂复配,可以对UV全波段进行防护。
润肤剂的选配,既可以与油溶性紫外防御剂溶解性好,而且可以较好地兼容油相中的其他成分,使得油相均一;还有利于油相增稠剂中二丁基月桂酰谷氨酰胺和二丁基乙基己酰基谷氨酰胺的凝胶化。
因此,本发明的双相组合物不通过乳化剂将水、油两相进行混合,不属于传统的水包油或者油包水体系,而是油相在油相增稠剂作用下凝固,并在水相增稠剂的作用下,以透明颗粒的形式稳定均匀悬浮于水相中,最终呈透明的双相外观。而且组合物对油溶性紫外防御剂包容性好,油溶性紫外防御剂在油相和水相中的溶解性、稳定性高,使用时无需摇匀,即可均匀涂抹于皮肤表面,具有高SPF值,肤感清爽不油腻。该防晒组合物长期储存外观无变化,稳定性好,肤感清爽,涂抹均匀、防晒能力强。
在制备方法中,对加热温度、加热速度、搅拌速度等参数的限制,使得最终料体中油相的粒径大小均一稳定,容易涂抹,油相最终凝固所形成的颗粒的粒径直径为0.2~0.5mm。
具体实施方式
下面结合实施例对本发明作进一步的说明,但并不作为对本发明限制的依据。
一种透明双相防晒组合物,所述防晒组合物,包括澄清透明的呈连续相的水相和澄清透明的呈非连续相的油相,其中油相以颗粒形式均匀分布于水相,所述水相包括水相增稠剂,所述油相包括油溶性紫外防御剂、润肤剂和油相增稠剂。
所述水相增稠剂的质量占水相总质量1~4%;油溶性紫外防御剂的质量占防晒组合物总质量的1~25%;润肤剂的质量占防晒组合物总质量的2~30%;油相增稠剂的质量占油相总质量的1.3~5%。
所述水相和油相的质量比为0.6:1~10:1。
所述水相增稠剂包括丙烯酸(酯)类交联聚合物-2钠、聚丙烯酰基二甲基牛磺酸钠和丙烯酰二甲基牛磺酸铵/VP共聚物中的的任意两种或三种组合;还包括柠檬果皮粉、透明质酸钠、汉生胶、丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物、卡波姆、纤维素中的任意一种或多种组合。
所述油相增稠剂包括二丁基月桂酰谷氨酰胺和二丁基乙基己酰基谷氨酰胺。还包括蓖麻油/IPDI共聚物、C30-45烷基二甲硅烷基聚丙基倍半硅氧烷中的任意一种或者两种组合。采用熔点为66℃的烷基有机硅蜡:C30-45烷基二甲硅烷基聚丙基倍半硅氧烷,该成分结合了硅蜡与硅树脂的特点,加入后可提高油相的涂抹顺滑感、柔软感以及产品的耐转移性。
所述油相还包括助溶剂,所述助溶剂为多元醇或者异构醇。
所述油溶性紫外防御剂采用具有UV全波段防护功效的紫外防御剂。所述油溶性紫外防御剂采用UVA(320~400nm)波段的紫外防御剂和UVB(275~320nm)波段的紫外防御剂。
UVA波段的紫外防御剂采用二乙氨羟苯甲酰基苯甲酸己酯和丁基甲氧基二苯甲酰基甲烷中的任意一种或两种组合;UVB(275~320nm)波段的紫外防御剂采用乙基己基三嗪酮、阿魏酸、阿魏酸乙基己酯、阿魏酸乙酯、聚硅氧烷-15、对甲氧基肉桂酸异戊酯、甲基肉桂酸乙基己酯、奥克立林、胡莫柳酯、水杨酸乙基己酯中的任意一种或多种组合。
所述油溶性紫外防御剂还可以采用覆盖UVA与UVB波段的紫外防御剂:双-乙基己氧苯酚甲氧苯基三嗪和三联苯基三嗪中的一种或两种组合。
所述润肤剂包括己二酸二丁酯、丁基辛醇水杨酸酯、月桂酸己酯中的任意一种或多种组合。
所述润肤剂还包括牛油果树果脂,水黄皮籽油、辛基聚甲基硅氧烷和肉豆蔻酸异丙酯中的任意一种或多种组合。
实施例1:
一种透明双相防晒组合物,所述防晒组合物,包括澄清透明的呈连续相的水相和澄清透明的呈非连续相的油相,其中油相以颗粒形式均匀分布于水相;
所述水相包括以下质量含量的组分:甘油4%、乙醇4%、水45.8%、丙烯酸(酯)类交联聚合物-2钠0.5%、聚丙烯酰基二甲基牛磺酸钠0.3%、柠檬果皮粉0.3。
所述油相包括油溶性紫外防御剂、润肤剂、油相增稠剂和助溶剂。
油溶性紫外防御剂采用以下质量含量的组分:二乙氨羟苯甲酰基苯甲酸己酯5%、双-乙基己氧苯酚甲氧苯基三嗪3%和乙基己基三嗪酮5%。
润肤剂采用以下质量含量的组分:己二酸二丁酯15%、丁基辛醇水杨酸酯10%和肉豆蔻酸异丙酯4%。
油相增稠剂采用以下质量含量的组分:二丁基月桂酰谷氨酰胺0.5%、二丁基乙基己酰基谷氨酰胺0.2%、蓖麻油/IPDI共聚物0.1%、C30-45烷基二甲硅烷基聚丙基倍半硅氧烷0.3%。
助溶剂采用以下质量含量的组分:1,2-戊二醇2%。
上述的一种透明双相防晒组合物的制备方法:包括以下操作步骤:
a、将水相增稠剂分散于水相中,以0.5~1℃/min的速度加热至80℃,保温10~15min,后经Primix均质机,以2000rpm的速度低速均质15~30min,得均一透明液体,得水相;
b、将油溶性紫外防御剂与润肤剂混合,以1℃/min的速度加热至80℃,以500rpm的速度搅拌,混合均匀,得透明均一液体,为A品;
c、向A品中加入油相增稠剂,以1℃/min的速度加热至70℃,保温10min,以500rpm的速度搅拌,混合至透明均一,得油相;
d、将油相加入水相中,加热融解后以1000rpm的速度搅拌,以1℃/min的速度降温至室温,得透明双相防晒组合物。其中,油相以颗粒形式均匀分布于水相,静置时该组合物并不分层。
按照实施例1的透明双相防晒组合物的制备方法,根据成分表1的配方,分别制成实施例2~3和对比例1~2的防晒组合物。
表1防晒组合物配方表
将实施例1~3和对比例1~2制得的成品分别进行性能测试,测试方法为:
1)膜均匀性
将样品均匀涂布在聚丙烯片材上,然后将该片材暴露于UV灯并拍照。基于涂覆片材的视觉外观以1~5分评价膜均匀性。如果外观为均匀的黑色,则为5分;若外观为非均匀半透明,则评为1分。
2)SPF值
在5cm×5cm的聚甲基丙烯酸甲酯(PMMA)板上,将样品以2mg/cm2的方式均匀涂布1分钟,在25℃下干燥15分钟。通过SPF分析仪测定波长307nm处的SPF值。
3)防水性
在5cm×5cm的聚甲基丙烯酸甲酯(PMMA)板上,将样品以2mg/cm2的方式均匀涂布1分钟,在25℃下干燥15分钟。将PMMA板在水中以中等程度搅动20分钟,然后出水20分钟(不擦拭PMMA板)。再入水中以中等程度搅动20分钟,出水自然晾干(不擦拭PMMA板),用SPF测定仪测定SPF值。根据前后SPF值差异,对样品的防水性进行打分,1~5分,其中5分为防水效果极佳,1分为几乎没有防水效果。
4)稳定性
在室温下观察组合物从制造起1小时后的状态,未发现明显沉降,进一步在~18℃、4℃、25℃、40℃、45℃下保存3个月,观察稳定性。三个月后所有温度条件下稳定性均极佳,则为“√”,其中一个或多个温度条件下稳定性未通过,则为“×”,其中组合物中出现颗粒沉降、料体变浑浊,则表示稳定性未通过。
5)肤感
由10名专业人员对防晒组合物涂抹后的粘腻感进行打分,1~5分,其中完全不粘腻为5分,特别粘腻为1分。
测试结果见表2。
对比例1相较于实施例,水相增稠剂加量较低导致体系稳定性不佳,油相颗粒发生沉降。油相增稠剂加量较高导致涂布均匀性不佳,肤感偏重。
对比例2相较于实施例,水相增稠剂加量较高造成涂抹肤感较为粘腻。油相增稠剂加量较低,酯类油脂加量偏低,对防水性造成一定影响,同时使得油相颗粒稳定性弱,料体容易浑浊。
表2防晒组合物性能测试表
性能指标 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 |
膜均匀性 | 5 | 5 | 5 | 4 | 4.5 |
SPF值 | 50 | 50 | 50 | 45 | 50 |
防水性 | 3.5 | 3.5 | 3.5 | 4 | 3 |
稳定性 | √ | √ | √ | × | × |
粘腻感 | 4.6 | 4.5 | 4.5 | 4 | 3 |
Claims (10)
1.一种透明双相防晒组合物,其特征在于:所述防晒组合物,包括澄清透明的呈连续相的水相和澄清透明的呈非连续相的油相,其中油相以颗粒形式均匀分布于水相,所述水相包括水相增稠剂,所述油相包括油溶性紫外防御剂、润肤剂和油相增稠剂。
2.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:水相增稠剂的质量占水相总质量的1~4%;油溶性紫外防御剂的质量占防晒组合物总质量的1~25%;润肤剂的质量占防晒组合物总质量的2~30%;油相增稠剂的质量占油相总质量的1.3~5%。
3.根据权利要求2所述的一种透明双相防晒组合物,其特征在于:所述水相和油相的质量比为0.6:1~10:1。
4.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:所述水相增稠剂包括丙烯酸(酯)类交联聚合物-2钠、聚丙烯酰基二甲基牛磺酸钠和丙烯酰二甲基牛磺酸铵/VP共聚物中的任意两种或三种组合。
5.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:所述油相增稠剂包括二丁基月桂酰谷氨酰胺和二丁基乙基己酰基谷氨酰胺。
6.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:所述油相还包括助溶剂,所述助溶剂为多元醇或者异构醇。
7.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:所述油溶性紫外防御剂采用具有UV全波段防护功效的紫外防御剂。
8.根据权利要求1所述的一种透明双相防晒组合物,其特征在于:所述润肤剂包括己二酸二丁酯、丁基辛醇水杨酸酯、月桂酸己酯中的任意一种或多种组合。
9.根据权利要求1~8任意一项所述的透明双相防晒组合物的制备方法,其特征在于:包括以下操作步骤:
a、将水相增稠剂分散于水相中,加热至60~100℃,保温10~15min,低速均质15~30min,得均一透明液体,为水相;
b、将油溶性紫外防御剂与润肤剂混合,加热至60~100℃,搅拌混合均匀,得透明均一液体,为A品;
c、向A品中加入油相增稠剂,加热至60~90℃,再加入助溶剂,保温10~15min,搅拌混合至透明均一,得油相;
d、将油相加入水相中,加热融解后搅拌降温至室温,得透明双相防晒组合物。
10.根据权利要求9所述的一种透明双相防晒组合物的制备方法,其特征在于:加热速度为0.5~1℃/min,降温速度为1~2℃/min,步骤a中的均质速度为1800~2200rpm,步骤b和步骤c中的搅拌速度为450~550rpm,步骤d中的搅拌速度为80~120rpm。
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