CN114469779A - 一种添加凹凸棒石的清爽防晒乳液及制备方法 - Google Patents
一种添加凹凸棒石的清爽防晒乳液及制备方法 Download PDFInfo
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Abstract
本发明涉及一种添加凹凸棒石的清爽防晒乳液及制备方法,其添加凹凸棒石和使用纳米TiO2空心球对BEMT的紫外屏蔽性能协同增效,能在不过量增加有机紫外线过滤剂的量的情况下增强防晒霜紫外线防护能力,解决紫外线防护能力强的防晒霜,油相含量过高造成防晒乳液油腻感严重和易致痘的技术问题。
Description
技术领域
本发明属于涉及化妆品技术领域,具体涉及一种添加凹凸棒石的清爽防晒乳液及制备方法。
背景技术
过量的紫外辐射会对人体健康造成严重损害,紫外线按照其波长可分为长波紫外线UVA(320~400nm),中波紫外线UVB(280~320nm)和短波紫外线UVC(200~280nm)。UVA有很强的穿透力,可以直达肌肤的真皮层,使色素沉积、皮肤晒黑,严重的会引起皮肤癌。UVB可以穿透大气层到达皮肤的表皮层,使皮肤出现红斑、炎症等现象,是皮肤晒伤的因素。UVC基本上会被大气层阻留,所以不会对人体皮肤造成损害。近年来,环境污染、气候变暖,大气臭氧层遭到破坏,这导致更多的紫外线到达地球表面。因此,加强对紫外线的防护成为了当下热点。紫外线辐射可能通过破坏人体皮肤细胞的DNA导致皮肤癌,使用防晒霜可以最大限度地减少患皮肤癌的可能性。随着公众对紫外线辐射对皮肤造成的有害影响的认识不断提高,人们对可提供光保护的防晒霜产品越来越感兴趣,防晒霜也早已成为当下日化行业中的热点话题之一。近年来,传统的紫外吸收剂已无法满足消费者日益增长的紫外防护需求,在这种环境下催生了一系列新型的高效紫外线吸收剂。
双-乙基己氧基苯酚甲氧苯基三嗪(Bis-Ethylhexyloxyphenol MethoxyphenylTriazine,BEMT)是一种新型的油溶性的有机紫外吸收剂,可用于防晒配方中制备乳液,是一种广谱的紫外线吸收剂,能吸收UVB和UVA,它的吸收顶峰有两个,分别位于波长310及340nm处,BEMT与一些UVB有机防晒剂和无机防晒剂复配使用有协同作用。其光稳定性极高,与其他防晒剂例如阿伏苯宗混合还能抑制它们产生光分解反应。与无机防晒剂相比,有机防晒剂存在的安全隐患更多一些,比如对皮肤刺激大、导致皮肤过敏等,因此在不增加有机紫外线过滤剂的量的情况下增强紫外线防护的防晒制剂是非常必要的。
在防晒配方中,油相含量过高往往会造成防晒霜油腻感严重和易致痘的问题。粉体填充剂也是化妆品中常用的原料之一,填充剂又称为体质颜料,不仅起着填充作用,还能起到降低油相含量、增稠、悬浮、保湿和润滑的功效。凹凸棒石(Attapulgite;ATP)又名坡缕缟石、坡缕石,分子式
Mg5Si20(OH2)(H2O)4·nH2O,是海泡石族的一种矿石,由蒙脱石转化而成,由含水的层链状镁质硅酸盐组成。其微观结构为纤维状晶体结构且具有纳米级孔穴通道,有良好的吸附性、悬浮性、分散性、离子交换性。
发明内容
针对背景技术中需要在不过量增加有机紫外线过滤剂的量的情况下增强防晒霜紫外线防护能力和油相含量过高造成防晒配方油腻感严重和易致痘的问题,本发明的目的在于提供一种添加凹凸棒石的清爽防晒乳液及其制备方法,该清爽防晒乳液能在增强防晒霜紫外线防护能力的同时不增加油腻感,且制备方法简单易行、成本低廉。
本发明解决其技术问题采用的技术方案是:一种添加凹凸棒石的清爽防晒乳液,其原料按质量份计包括以下各组分:
A相:C12-15醇苯甲酸酯10.00~15.00份、丙基辛基庚酯8.00~12.00份、纳米TiO2空心球5.00~10.00份、鲸蜡硬脂醇0.50~2.00份和BEMT 2.00~6.00份;
B相:凹凸棒石水分散液35.00~65.00份、甘油2.00~10.00份、硬脂酰谷氨酸钠0.50~2.00份、硬脂醇聚醚-21 0.10~1.00份和黄原胶0.10~0.50份;
C相:苯氧乙醇0.50~3.00份。
C12-15醇苯甲酸酯和丙基辛基庚酯为润肤剂,二者均能为BEMT提供良好的油溶性;TiO2为UVB紫外线过滤剂,BEMT为全波段紫外屏蔽剂;鲸蜡硬脂醇为助乳化剂;甘油为保湿剂;硬脂酰谷氨酸钠和硬脂醇聚醚-21为乳化剂(O/W);凹凸棒石为填充剂和保湿剂;EDTA二钠为螯合剂;黄原胶为流变调节剂;苯氧乙醇为防腐剂。清爽防晒乳液添加凹凸棒石和使用纳米TiO2空心球对BEMT的紫外屏蔽性能协同增效。
为进一步提高防晒效果:所述的纳米TiO2空心球为正辛基三乙氧基硅烷改性的金红石型纳米TiO2空心球,改性剂正辛基三乙氧基硅烷的用量为TiO2的质量的2~8%。
进一步地:所述的凹凸棒石水分散液包括以下组分:凹凸棒石、EDTA二钠和去离子水;凹凸棒石的固含量为0.5~4.5%,EDTA二钠与去离子水的质量比为0.001:1~0.005:1。EDTA二钠起螯合剂的作用,与凹凸棒石粉体中可能携带的金属离子络合,防止可溶性金属离子对配方稳定性带来的危害。
上述添加凹凸棒石的清爽防晒乳液的制备方法,包括如下步骤:将A相和B相分别加热至75~85℃,然后将B相加入A相,3000~5000rpm转速下均质5~10min;均质完成后冷却至45℃以下,将C相加入均质后的A、B二相混合液中,于1500~3000rpm下均质1~3min,冷却至室温后,真空脱泡,得到清爽防晒乳液。
进一步地,所述的脱泡方法为减压物理脱泡,将均质后的A、B、C三相混合液转移至样品罐中,将样品罐放置于SPEEDMIXER DAC600高速混合机中抽真空,在600~1200rpm转速下5~10min。
本发明的有益效果是:
1.凹凸棒石是一种天然一维水合镁铝硅酸盐矿物,有良好的吸附性、悬浮性和分散性,吸油值大,价格便宜。本发明通过在在防晒配方中添加凹凸棒石,达到降低油相含量,抗痘、减轻配方油腻感、获得清爽的肤感、降低成本的作用。凹凸棒石是一种水合硅酸镁铝矿物,棒晶束带有大量的结合水,防晒配方中添加凹凸棒石可以达到长效补水保湿的作用。
2.一些有机紫外屏蔽剂可能会导致人类和动物的生物蓄积产生不良反应如过敏性皮炎和接触性皮炎等,因此,在不增加有机紫外线过滤剂的量的情况下增强紫外线防护的防晒制剂是非常必要的。BEMT与部分UVB紫外屏蔽剂复配会表现出十分优异的协同效应,本发明通过BEMT和TiO2的协同效应使防晒配方的紫外防护能力大幅提高。同时,无机防晒剂的引入使配方的成本得到了有效的控制。
3.本发明添加的无机防晒剂是纳米TiO2空心球,纳米TiO2空心球相较于纳米TiO2粉体更容易与BEMT发生协同增强效应,BEMT分子可以进入TiO2微球内部,TiO2这种半导体氧化物可以吸收紫外辐射使低能价带电子跃迁到高能导带变成光生电子,BEMT分子捕获光生电子的能量使分子热运动加剧,空心球内部的BEMT分子更容易对TiO2光生电子能量进行捕获,促进BEMT分子发生快速互变异构,进而增强紫外线吸收能力。
附图说明
图1为实施例2、对比例2、对比例3和对比例4的稳定性试验乳液粘度变化图;
图2为实施例2、对比例2、对比例3和对比例4的稳定性试验乳液离心上层清液高度变化图。
具体实施方式
本发明不局限于下列具体实施方式,本领域一般技术人员根据本发明公开的内容,可以采用其他多种具体实施方式实施本发明的,或者凡是采用本发明的设计结构和思路,做简单变化或更改的,都落入本发明的保护范围。需要说明的是,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。
以下结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。
防晒指数(SPF值)测试方法:采用UV–2000S型抗紫外透过性能测试仪(美国蓝菲公司)来测量评估乳液的防晒性能。参照欧盟Colipa标准,在5cm*5cm PMMA有机板上称取32.5mg的防晒乳液,用一次性乳胶手套快速涂抹均匀且控制板上的残量为29.0mg,重复实验三次,记录三次测量平均值记为SPF值。
稳定性试验测试方法:测试通过本发明配方制备的乳液的稳定性,将每种乳液在阳光照射下储存6个月。在乳化后的不同时间(0、30、60、90和180天)进行分析取样,通过Brookfield DV2T粘度计测量乳液粘度,安信TG16G离心机离心一定量的防晒乳液,通过粘度变化和乳液离心后上层清液高度来评价乳液稳定性。
实施例1
一种添加凹凸棒石的清爽防晒乳液,其原料按质量份计包括以下各组分:
A相:C12-15醇苯甲酸酯10.00份、丙基辛基庚酯8.00份、纳米TiO2空心球5.00份(3%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇0.50份、BEMT 4.00份;
B相:凹凸棒石水分散液69.30份(凹凸棒石的固含量为0.5%,EDTA二钠与去离子水的质量比为0.001:1。)、甘油2.00份、硬脂酰谷氨酸钠0.50份、硬脂醇聚醚-21 0.10份、黄原胶0.10份;C相:苯氧乙醇0.50份;
A相和B相分别加热至85℃,将B相加入A相,3000rpm转速下均质5min。均质完成后冷却至43℃,将C相加入均质后的AB相,于1500rpm下均质1min,冷却至室温后,使用SPEEDMIXER DAC600高速混合机在600rpm旋转10min,真空脱泡,得到清爽防晒乳液F1。
参照欧盟Colipa标准,测得实施例1制得的清爽防晒乳液F1的SPF值为31。
实施例2
一种添加凹凸棒石的清爽防晒乳液,其原料按质量份计包括以下各组分:A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、纳米TiO2空心球10.00份(5%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.50份、BEMT 5.00份;
B相:凹凸棒石水分散液56.10份(凹凸棒石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-21 0.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,使用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡,8min,得到清爽防晒乳液F2。
参照欧盟Colipa标准,测得实施例2制得的清爽防晒乳液F2的SPF值为37。
实施例3
一种添加凹凸棒石的清爽防晒乳液,其原料按质量份计包括以下各组分:
A相:C12-15醇苯甲酸酯13.00份、丙基辛基庚酯8.00份、纳米TiO2空心球8.00份(2%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.00份、BEMT 3.00份;
B相:凹凸棒石水分散液58.10份(凹凸棒石的固含量为3%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油5.00份、硬脂酰谷氨酸钠1.50份、硬脂醇聚醚-21 0.60份、黄原胶0.30份;C相:苯氧乙醇1.50份;
A相和B相加热至85℃和75℃,将B相加入A相,4000rpm转速下均质8min,均质完成后冷却至40℃。
将C相加入均质后的AB相,于2500rpm下均质2min,冷却至室温后,使用SPEEDMIXERDAC600高速混合机在1000rpm转速下真空脱泡7min,得到清爽防晒乳液F3。
参照欧盟Colipa标准,测得实施例3制得的清爽防晒乳液F3的SPF值为33。
实施例4
一种添加凹凸棒石的清爽防晒乳液,其原料按质量份计包括以下各组分:
A相:C12-15醇苯甲酸酯15.00份、丙基辛基庚酯12.00份、纳米TiO2空心球6.00份(8%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇2.00份、BEMT 6.00份;
B相:凹凸棒石水分散液42.5份(凹凸棒石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油10.00份、硬脂酰谷氨酸钠2.00份、硬脂醇聚醚-21 1.00份、黄原胶0.50份;C相:苯氧乙醇3.00份;
A相和B相分别加热至75℃,将B相加入A相,5000rpm转速下均质10min,均质完成后冷却至41℃。
将C相加入均质后的AB相,于3000rpm下均质3min,冷却至室温后,使用SPEEDMIXERDAC600高速混合机在1200rpm转速下真空脱泡5min,得到清爽防晒乳液F4。
参照欧盟Colipa标准,测得实施例4制得的清爽防晒乳液F4的SPF值为35。
对比例1
一种防晒乳液的原料按质量份计包含以下各组分:
A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、鲸蜡硬脂醇1.50份、BEMT5.00份;
B相:凹凸棒石水分散液66.10份(凹凸棒石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-21 0.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,使用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡8min,得到防晒乳液F5。
参照欧盟Colipa标准,测得对比例1制得的防晒乳液F5的SPF值为13。
对比例2
一种防晒乳液的原料按质量份计包含以下各组分:
A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、纳米TiO2空心球10.00份(5%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.50份、BEMT 5.00份;
B相:滑石水分散液56.10份(滑石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-210.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡8min,得到防晒乳液F6。
参照欧盟Colipa标准,测得对比例2制得的滑石防晒乳液F6的SPF值为32。
对比例3
一种防晒乳液的原料按质量份计包含以下各组分:
A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、纳米TiO2空心球10.00份(5%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.50份、BEMT 5.00份;
B相:蒙脱石水分散液56.10份(蒙脱石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-21 0.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡8min,得到防晒乳液F7。
参照欧盟Colipa标准,测得对比例3制得的蒙脱石防晒乳液F7的SPF值为31。
对比例4
一种防晒乳液的原料按质量份计包含以下各组分:
A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、纳米TiO2空心球10.00份(5%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.50份、BEMT 5.00份;
B相:去离子水56.10份、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-210.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡8min,得到防晒乳液F8。
参照欧盟Colipa标准,测得对比例4制得的防晒乳液F8的SPF值为30。
对比例5
一种防晒乳液的原料按质量份计包含以下各组分:
A相:C12-15醇苯甲酸酯12.00份、丙基辛基庚酯10.00份、纳米TiO2空心球10.00份(5%正辛基三乙氧基硅烷改性)、鲸蜡硬脂醇1.50份;
B相:凹凸棒石水分散液61.10份(凹凸棒石的固含量为4.5%,EDTA二钠与去离子水的质量比为0.005:1。)、甘油3.00份、硬脂酰谷氨酸钠0.70份、硬脂醇聚醚-21 0.50份、黄原胶0.20份;C相:苯氧乙醇1.00份;
A相和B相加热至80℃和82℃,将B相加入A相,3500rpm转速下均质5min,均质完成后冷却至45℃。
将C相加入均质后的AB相,于2000rpm下均质2min,冷却至室温后,用SPEEDMIXERDAC600高速混合机在800rpm转速下真空脱泡8min,得到防晒乳液F9。
参照欧盟Colipa标准,测得对比例5制得的防晒乳液F9的SPF值为16。
对比例6
将实施例2中的纳米TiO2空心球替换为同质量的相同改性方法的改性金红石型二氧化钛粉末,其他条件不变,得到防晒乳液F10。
参照欧盟Colipa标准,测得对比例5制得的防晒乳液F10的SPF值为33不同实施例、对比例防晒乳液防晒指数测试结果如下表:
表1.不同实施例对比例防晒乳液防晒指数对比
结合对比例1、对比例5和实施例2可知,只添加5%BEMT(对比例1)和10%纳米TiO2球(对比例5)的防晒乳液的SPF值分别为13和16,而同时添加5%BEMT和10%纳米TiO2球(实施例2)的防晒乳液由于二者的协同效应(TiO2促进BEMT对紫外辐射的吸收进而导致单重态激发,在分子内氢键的作用下,H原子发生快速互变异构转移到相邻的O原子或N原子,通过振动弛豫将吸收的紫外线能量释放为无害的热能)使得防晒指数大幅提升至37,防晒指数增幅达28%。
结合实施例2和对比例6可知,纳米TiO2空心球相较于纳米TiO2粉体更容易与BEMT发生协同增强效应,BEMT可以进入TiO2空心球内部,纳米二氧化钛空心球内部的BEMT更容易对TiO2光生电子能量捕获,所以具有更高的SPF值。
实施例2、对比例2、对比例3和对比例4的稳定性试验结果如下表所示
表2.实施例2、对比例2、对比例3和对比例4的稳定性试验乳液粘度变化表
(Brookfield;DV2T;S05;20rpm;25℃)
(粘度变化越小越好)
表3.实施例2、对比例2、对比例3和对比例4的稳定性试验乳液离心上清液高度
(安信TG16G离心机;3000rpm;5min,结果越小越好)
结合实施例2和对比例4的乳液粘度变化结果和乳液离心上清液高度变化可知,添加凹凸棒石的配方较未添加凹凸棒石的配方要更稳定,凹凸棒石具有良好的悬浮性、分散性和较大的吸油值,添加配方中可以是乳液稳定性大幅提升。
结合实施例2、对比例2和对比例3的乳液粘度变化结果和乳液离心上清液高度变化可知,在配方中添加凹凸棒石的乳液的稳定性要优于添加滑石和蒙脱石的乳液,滑石和蒙脱石在乳液中可能发生片层的叠合导致乳液稳定性下降。
根据热力学第二定律,乳液是一种非均相体系,生来就是不稳定的,最终会分为两相,但是采取一些适合的配方可以是乳液稳定的保存很长时间。结合实施例2、对比例2、对比例3和对比例4可知,添加凹凸棒石的乳液在180天后无论是粘度变化还是乳液离心后上层清液的变化都是明显小于其他对比例,说明添加凹凸棒石可以大幅提升乳液的稳定性。
Claims (5)
1.一种添加凹凸棒石的清爽防晒乳液,其特征在于其原料按质量份计包括以下各组分:
A相:C12-15醇苯甲酸酯10.00~15.00份、丙基辛基庚酯8.00~12.00份、纳米TiO2空心球5.00~10.00份、鲸蜡硬脂醇0.50~2.00份和BEMT 2.00~6.00份;
B相:凹凸棒石水分散液35.00~65.00份、甘油2.00~10.00份、硬脂酰谷氨酸钠0.50~2.00份、硬脂醇聚醚-21 0.10~1.00份和黄原胶0.10~0.50份;
C相:苯氧乙醇0.50~3.00份。
2.根据权利要求1所述的添加凹凸棒石的清爽防晒乳液,其特征在于:所述的纳米TiO2空心球为正辛基三乙氧基硅烷改性的金红石型纳米TiO2空心球,改性剂正辛基三乙氧基硅烷的用量为TiO2的质量的2~8%。
3.根据权利要求1所述的添加凹凸棒石的清爽防晒乳液,其特征在于:所述的凹凸棒石水分散液包括以下组分:凹凸棒石、EDTA二钠和去离子水;凹凸棒石的固含量为0.5-4.5%,EDTA二钠与去离子水的质量比为0.001:1~0.005:1。
4.根据权利要求1~3任一项所述的添加凹凸棒石的清爽防晒乳液的制备方法,其特征在于包括如下步骤:将A相和B相分别加热至75℃~85℃,然后将B相加入A相,3000~5000rpm转速下均质5~10min;均质完成后冷却至45℃以下,将C相加入均质后的A、B二相混合液中,于1500~3000rpm下均质1~3min,冷却至室温后,真空脱泡,得到防晒乳液。
5.根据权利要求4所述的添加凹凸棒石的清爽防晒乳液的制备方法,其特征在于:所述的脱泡方法为将均质后的A、B、C三相混合液转移至样品罐中,将样品罐放置于SPEEDMIXERDAC600高速混合机中抽真空,在600~1200rpm转速下5~10min。
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