CN114376926B - 一种基于六方氮化硼粉体的防晒控油粉饼及其制备方法 - Google Patents
一种基于六方氮化硼粉体的防晒控油粉饼及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于六方氮化硼粉体的防晒控油粉饼及其制备方法,涉及彩妆技术领域。本发明的技术要点是以六方氮化硼作为主要的辅助防晒剂和填充剂,在添加少量的物理防晒剂二氧化钛时,可达到较好的防晒效果。粉饼由以下重量份的原料制成:六方氮化硼、改性滑石粉、改性高岭土、二氧化钛、二氧化硅、氧化锌、硬脂酸镁、丁基甲氧基二苯甲酰基甲烷、淀粉、尿囊素、烟酰胺、角鲨烷、蚕丝油、聚二甲基硅氧烷、戊二醇、去离子水、苯氧乙醇。本发明的粉饼具有良好的防晒、控油和柔焦优点。防晒指数SPF值最终在25~30范围内。
Description
技术领域
本发明涉及化妆品的彩妆技术领域,具体涉及一种基于六方氮化硼粉体的防晒控油粉饼及其制备方法。
技术背景
六方氮化硼粉体具有高化学惰性和热稳定性,由于其2Gpa的莫氏强度、扁平的片层结构、接近人体皮肤的折光指数以及0.16的摩擦系数决定了它不仅具有优良的抗氧化性和优异的润滑性,同时具备适当的遮盖力和附着力,并且添加了六方氮化硼的彩妆类化妆品在视觉上会呈现出自然、轻薄的裸妆感。而目前粉饼用无机粉体大多是天然矿石,在使用性及稳定性等方面并不总是令人满意——例如滑石、云母等无机材料具有催化活性,会引起香料和油等的氧化,被认为是导致异味的原因。
粉饼是彩妆类化妆品中底妆的一种,专业名称为定妆粉饼,它能吸走皮肤表面过多油脂,令妆容保持柔光,光滑的效果。在底妆上妆时它主要的作用为:修补面部瑕疵以均匀肤色,同时便于后期上妆中的其余彩妆品与肌肤贴合,延长妆容的持久度。在补妆时它的主要作用为:吸收面部分泌的过多油脂,修补因外力因素而脱落的底妆部分。然而它仍然存在以下问题:大多粉饼用途仅为遮瑕定妆,并未兼有防晒功效;市面所售的粉饼大多控油效果一般,且并不防水。
发明内容
为解决相关技术中存在的问题,本发明提供一种基于六方氮化硼粉体的防晒控油粉饼及其制备方法,所提供的粉饼具有多重功效,所提供的制备方法简单易实现。针对粉饼的防晒功效,由于六方氮化硼纳米粉体的颗粒尺寸可控,使它在防晒类化妆品中有明显优势,它允许在不同的形成阶段对纳米粉体进行调控,从而控制尺寸和表面积;六方氮化硼与二氧化钛组合作为防晒剂时,不仅可以增强二氧化钛对紫外线的屏蔽效果,同时,粒径4~6μm的六方氮化硼可以有效的屏蔽红外辐射,更好的预防皮肤“光老化”;针对粉饼的控油功效,全氟辛基三乙氧基硅烷具有13个低表面能惰性基团,将全氟辛基三乙氧基硅烷的惰性基团引入粉体表面,将使被改性的粉体具有极低的表面能从而使粉体达到疏水疏油的性能。
作为本发明的一个方面,提供一种基于六方氮化硼粉体的防晒控油粉饼,以下组分按重量份计,包含:六方氮化硼10~20份、改性滑石粉15~20份、改性高岭土2~8份、二氧化钛10~15份、二氧化硅2~5份、氧化锌5~15份、氧化铁黑1~4份,氧化铁红0.1~1份,氧化铁黄5~10份、硬质酸钠2~5份、丁基甲氧基二苯甲酰基甲烷2~5份、淀粉5~10份、尿囊素1~5份、烟酰胺1~5份、角鲨烷1~5份、蚕丝油1~5份、聚二甲基硅氧烷2~4份、戊二醇1~4份、水1~3份。
作为一种优选实施方案,所述防晒控油粉饼还可以包含0.01~0.1份苯氧乙醇和/或苯甲酸钠。
在本发明的实施案例中,所述改性滑石粉或改性高岭土是通过以下具体方法得到:
S1、取10~20份滑石粉或高岭土在乙醇中超声扩散,得到混合物A;
S2、将全氟辛基三乙氧基硅烷加入S1中所述混合物A超声并搅拌5h,得到混合物B;
S3、将S2中所述混合物B固液分离,并冷冻干燥固相,得到粉末状固体;
S4、将S3中所述粉末状固体以球磨,得到改性滑石粉或改性高岭土。
在本发明的实施案例中,所述全氟辛基三乙氧基硅烷具有以下结构:
作为本发明的又一个方面,提供一种基于六方氮化硼粉体的防晒控油粉饼的制造方法,以下组分均按重量份计,包括以下步骤:
步骤1:将改性滑石粉15~20份、改性高岭土2~8份、六方氮化硼10~20份,二氧化钛10~15份、二氧化硅2~5份、氧化锌5~15份、硬质酸钠2~5份、丁基甲氧基二苯甲酰基甲烷2~5份、淀粉5~10份、尿囊素1~5份、烟酰胺1~5份混合,球磨,得到混合物Ⅰ;
步骤2:再将氧化铁黑1~4份,氧化铁红0.1~1份,氧化铁黄5~10份混合,加入所述混合物Ⅰ中,在固体打粉机内,得到混合物Ⅱ;
步骤3:称取角鲨烷1~5份、蚕丝油1~5份、聚二甲基硅氧烷2~4份、戊二醇1~4份、水1~3份、苯氧乙醇和/或苯甲酸钠0.01~0.1份在40~50℃恒温水浴混合,得到混合物Ⅲ;
步骤4:使用喷雾混合法将所述混合物Ⅲ与所述混合物Ⅱ混合至显色均匀,得到混合物IV;
步骤5:将所述混合物IV置于固体打粉机中以3500r/min混合3~5分钟,重复2~3次,得到混合物Ⅴ;
步骤6:将所述混合物Ⅴ压盘制得粉饼坯体。
在本发明的实施案例中,所述六方氮化硼由粒径为2~5um的六方氮化硼和粒径为5~7um的六方氮化硼组成。
在本发明的实施案例中,所述二氧化硅为多孔球形,所述二氧化硅的平均粒径为3μm,且其吸油量可达130ml/100g。
在本发明的实施案例中,所述二氧化钛与六方氮化硼掺杂构成防晒剂。
本发明至少包含如下有益效果:通过采用全氟辛基三乙氧基硅烷对高岭土和滑石粉进行改性,可使高岭土、滑石粉这类填充粉体在水中的接触角大大提升。由于粉饼中填充粉占比较大,当填充粉与水接触时接触角较小,处于被润湿状态,这使得大多粉饼无法达到防水效果,控油通过二氧化硅实现。由于全氟辛基三乙氧基硅烷具有13个惰性低表面能基团,可使被改性的粉体具有极低的表面能从而使粉体达到疏水疏油的性能。通过上述技术方案改进后,可明显看出填充粉体与水的接触角增大,从而达到很好的防水性;改善了传统粉饼不防水的缺陷,使得粉饼的用途更加广泛。使用六方氮化硼充当主要填充粉体克服了相关技术中以高岭土作为主要填充粉体时,粉质僵硬厚重的缺陷;同时使用六方氮化硼时,产品亲肤感更温和。通过六方氮化硼与二氧化钛掺杂构成防晒剂,提升防晒剂的紫外屏蔽效果并降低二氧化钛在皮肤中可能存在的潜在光学毒性,同时屏蔽红外辐射。
附图说明
图1为实施例1疏水疏油改性后高岭土的接触角示意图,(a)为未改性的高岭土与水的接触角示意图(b)为改性后高岭土与水的接触角(c)为未改性的高岭土与角鲨烷的接触角示意图(d)为改性后高岭土与角鲨烷的接触角。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
本发明中所涉及的六方氮化硼与二氧化钛掺杂构成防晒剂是指:将六方氮化硼与二氧化钛掺杂均匀后作为物理防晒剂在产品中使用,使产品更高效的屏蔽紫外光线对皮肤的辐射,同时也可屏蔽红外光线对皮肤的辐射。
本发明实施案例中的二氧化硅为联锴粉体提供的二氧化硅,粒径为3um,产品编码107121,吸油量为100~130ml/100g;色粉由纳璐科技有限公司提供,型号为77491RED、77492YELLOW、77499BLACK;高岭土由联锴粉体提供,粒径2um,产品编码106324;滑石粉由联锴粉体提供,粒径为8um,产品编码106138;2~5um六方氮化硼由联合微粉提供,产品编码608101SM;5~7um六方氮化硼由广州萨科提供;聚二甲基硅氧烷由陶氏提供,型号规格分别为DOW2501、DOW593、DOW319;香精由科莱恩提供。如无特殊说明,均为常用试剂,均可以通过市售获得。
实施例1改性滑石粉或改性高岭土的制备
S1、取10g滑石粉在50ml乙醇中超声扩散,得到混合物A;
S2、将4mL全氟辛基三乙氧基硅烷分别加入S1中所述混合物A中超声并搅拌5h,得到混合物B;
S3、将S2中所述混合物B固液分离,并冷冻干燥固相,得到粉末状固体;
S4、将S3中所述粉末状固体以球磨,以3000r/min球磨6min,得疏水疏油改性滑石粉。
采用上述同样的方法,制备改性高岭土。
本实施例中所制备的改性滑石粉和改性高岭土应用于本发明的其它实施例中。
实施例2
步骤1:将4g二氧化硅、2g尿囊素、2g烟酰胺、4g平均粒径为2μm的六方氮化硼、11g平均粒径为5μm的六方氮化硼、4g丁基甲氧基二苯甲酰基甲烷、12g二氧化钛、10g氧化锌、7g改性高岭土、4g硬脂酸钠、10g淀粉、20g改性滑石粉,混合,加入球磨机,在3500r/min条件下,球磨6分钟使混合物充分混合后,过1000目筛,制备成预混合粉,标记为混合物Ⅰ;
步骤2:称取1g氧化铁红77491RED、10g氧化铁黄77492YELLOW、2g氧化铁黑77499BLACK混合,加入混合物Ⅰ中,在固体打粉机中,以3500r/min混合3分钟,得到混合物Ⅱ;
步骤3:称取1g蚕丝油、1g角鲨烷、1.9g聚二甲基硅氧烷DOW2501、0.6g聚二甲基硅氧烷DOW593、0.5g聚二甲基硅氧烷DOW3196、2g戊二醇、2.5g水、0.05g苯氧乙醇、0.05g苯甲酸钠、0.3g香精,于45℃恒温水浴混合,得到混合物Ⅲ;
步骤4:使用喷雾混合法将所述混合物Ⅲ与所述混合物Ⅱ混合至显色均匀,得到混合物IV;
步骤5:将所述混合物IV置于固体打粉机中,以3500r/min混合3分钟,重复2~3次得到混合物Ⅴ;
步骤6:将所述混合物Ⅴ压盘制得粉饼坯体。
实施例3
步骤1:将4g二氧化硅、2g尿囊素、2g烟酰胺、4g平均粒径为2μm的六方氮化硼、11g平均粒径为5μm的六方氮化硼、4g丁基甲氧基二苯甲酰基甲烷、12g二氧化钛、10g氧化锌、7g改性高岭土、4g硬脂酸钠、10g淀粉、20g改性滑石粉,混合,加入球磨机,在3500r/min条件下,球磨6分钟使混合物充分混合后,过1000目筛,制备成预混合粉,标记为混合物Ⅰ;
步骤2:称取1g氧化铁红77491RED、3g氧化铁黄77492YELLOW、1.5g氧化铁黑77499BLACK混合,加入混合物Ⅰ中,固体打粉机中,以3500r/min混合3分钟,得到混合物Ⅱ;
步骤3:称取1g蚕丝油、1g角鲨烷、1.9g聚二甲基硅氧烷DOW2501、0.6g聚二甲基硅氧烷DOW593、0.5g聚二甲基硅氧烷DOW3196、2g戊二醇、2.5g水、0.05g苯氧乙醇、0.05g苯甲酸钠、0.3g香精,于45℃恒温水浴混合,得到混合物Ⅲ;
步骤4:使用喷雾混合法将所述混合物Ⅲ与所述混合物Ⅱ混合至显色均匀,得到混合物IV;
步骤5:将所述混合物IV置于固体打粉机中,以3500r/min混合3分钟,重复2~3次得到混合物Ⅴ;
步骤6:将所述混合物Ⅴ压盘制得粉饼坯体。
实施例4
步骤1:将4g二氧化硅、2g尿囊素、2g烟酰胺、4g平均粒径为2μm的六方氮化硼、11g平均粒径为5μm的六方氮化硼、4g丁基甲氧基二苯甲酰基甲烷、12g二氧化钛、10g氧化锌、7g改性高岭土、4g硬脂酸钠、10g淀粉、20g改性滑石粉,混合,加入球磨机,在3500r/min条件下,球磨6分钟使混合物充分混合后,过1000目筛,制备成预混合粉,标记为混合物Ⅰ;
步骤2:称取1g氧化铁红77491RED、3g氧化铁黄77492YELLOW、1.5g氧化铁黑77499BLACK混合,加入混合物Ⅰ中,固体打粉机中,以3500r/min混合3分钟,重复3次,得到混合物Ⅱ;
步骤3:称取1g蚕丝油、1g角鲨烷、1.9g聚二甲基硅氧烷DOW2501、0.6g聚二甲基硅氧烷DOW593、0.5g聚二甲基硅氧烷DOW3196、2g戊二醇、2.5g水、0.05g苯氧乙醇、0.05g苯甲酸钠、0.3g香精,于45℃恒温水浴混合,得到混合物Ⅲ;
步骤4:使用喷雾混合法将所述混合物Ⅲ与所述混合物Ⅱ混合至显色均匀,得到混合物IV;
步骤5:将所述混合物IV置于固体打粉机中,以3500r/min混合3分钟,并重复2次,得到混合物Ⅴ;
步骤6:将所述混合物Ⅴ压盘制得粉饼坯体。
对比例1采用市面所购买的:1号美宝莲纽约fitme粉饼;
对比例2采用市面所购买的:2号橘朵eevan花园系列柔焦粉饼;
对比例3采用市面所购买的:3号花西子蚕丝蜜粉饼;
对比例4采用市面所购买的:4号蜜丝佛陀粉饼;
对比例5采用市面所购买的:5号纪梵希绒雾柔雾哑光定妆粉饼。
实施例5功效测试实验
检测项目1:粉饼的防晒效果测试
步骤1:征集30名志愿者,志愿者年龄集中在23~26岁之间,将30名志愿者随机分为6组,每组5人;
步骤2:为6组志愿者分别提供粉扑和实施例2~4以及对比例1~5的粉饼,并指定粉饼肤感测评表,见表1.粉饼肤感测评指标。
步骤3:志愿者分别用食指推开步骤2中所提供粉饼,观察粉饼的细腻度,并按表1粉饼肤感测评指标进行打分,结果见表2;
步骤4:志愿者分别使用洁面乳(妮维雅氨基酸洗面奶)清洗手臂内侧,并在手臂内侧涂抹化妆水(妮维雅丝柔美白爽肤水)、面霜(妮维雅晶纯皙白美白补水凝露)、bb霜(薇诺娜极润保湿bb霜)后,志愿者使用粉扑蘸取步骤2中粉饼,均匀薄涂于手臂内侧,完成定妆。
步骤5:志愿者将手臂置于阳光下曝晒,每间隔30min于室内观察,观察四次。
步骤6:将步骤2中粉体分别称取25mg于玻璃片上,并滴加1滴甘油,将粉体与甘油的混合物涂匀在玻璃片上,阴干10min成膜后,将样品置于UV~2000S SPF测试仪上检测样品的SPF值,结果见表1。
表1粉饼SPF值测评结果
检测项目2:接触角测试实验
采用压片机对实施例1中制备的疏水疏油改性样品进行压片,制备样品2~3个。压片时每片样品质量为10g,压片压力为24.5MPa,压片直径为20mm,压片表面光滑平整。采用湿润角测量仪,于室温下,按接触角测量步骤,小心滴加液体于固体表面,形成液滴,取10次接触角读数平均值做为测量结果。分别测量水、甘油三酯、胆固醇与改性后的高岭土、改性后的滑石粉的接触角。实验结果表面,经全氟辛基三乙氧基硅烷改性后的高岭土和改性后的滑石粉与水以及油脂的接触角均大于90°,其图(b)改性后高岭土与水的接触角;其中接触角为127°;图(d)改性后高岭土与角鲨烷的接触角,其接触角为135°,均处于不润湿状态,参见附图1。表明改性后的高岭土具有优异的疏水疏油性。
检测项目3:粉饼的持妆效果测试
按照表2中的测评指标对本发明实施例2~4以及对比例所涉及的粉饼进行测评:
表2.粉饼肤感测评指标
步骤1:征集30名志愿者,志愿者年龄集中在23~26岁之间,各志愿者的肤质均为油性皮肤,将30名志愿者随机分为6组,每组5人;
步骤2:为6组志愿者分别提供粉扑和实施例2~4以及对比例1~5的粉饼,并指定粉饼肤感测评表,见表1.粉饼肤感测评指标。
步骤2:志愿者分别用食指推开步骤2中所提供粉饼,观察粉饼的细腻度,并按表1粉饼肤感测评指标进行打分,结果见表2;
步骤4:志愿者分别使用洁面乳(妮维雅氨基酸洗面奶)洁面,涂抹化妆水(妮维雅丝柔美白爽肤水)、面霜(妮维雅晶纯皙白美白补水凝露)、bb霜(薇诺娜极润保湿bb霜)后,志愿者使用粉扑蘸取步骤2中粉饼,均匀薄涂于左脸,完成定妆。
步骤5:定妆完成后,步骤四中志愿者可进行正常外出作息,每间隔4h在社交距离下进行一次观察,共观察两次后对粉体控油力按表1粉饼肤感测评指标进行打分,结果见表2;
步骤6:定妆完成后,步骤四中志愿者可进行正常外出作息,每间隔4h在社交距离下进行一次观察,共观察两次后对粉体持妆力按表1粉饼肤感测评指标进行打分,结果见表2;
步骤7:定妆完成后,对志愿者们在社交距离下进行面部观察;并使用步骤二中粉体均匀薄涂于柠檬表面,以同样距离进行观察,粉饼的遮瑕力按表1粉饼肤感测评指标进行打分,结果见表2;
步骤:8:志愿者们素颜正常外出作息,于下午16:30面部普遍开始大量泛油时分别试用步骤2中粉饼,并在完成试用后用吸油纸检测。粉饼的吸油力按表2粉饼肤感测评指标进行打分,结果见表3。
表3.粉饼功效测评结果
通过本发明提供的实施例及对比例可以看出,从粉饼功效测评结果看,本发明提供的基于六方氮化硼粉体的防晒控油粉饼,SPF值呈倍数增加,参见表1;控油力和吸油力都有很大提升,参见表3。
本具体实施例仅仅是对本发明的解释,其并不是对本发明的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本发明的权利要求范围内都受到专利法的保护。
Claims (6)
1.一种基于六方氮化硼粉体的防晒控油粉饼,其特征在于,以下组分按重量份计,包含:六方氮化硼10~20份、改性滑石粉15~20份、改性高岭土2~8份、二氧化钛10~15份、二氧化硅2~5份、氧化锌5~15份、氧化铁黑1~4份,氧化铁红0.1~1份,氧化铁黄5~10份、硬质酸钠2~5份、丁基甲氧基二苯甲酰基甲烷2~5份、淀粉5~10份、尿囊素1~5份、烟酰胺1~5份、角鲨烷1~5份、蚕丝油1~5份、聚二甲基硅氧烷2~4份、戊二醇1~4份、水1~3份;
所述六方氮化硼由平均粒径为2~5um的六方氮化硼和平均粒径为5~7um的六方氮化硼组成;
所述改性滑石粉或所述改性高岭土是通过以下具体方法得到:
S1、取10~20g滑石粉或高岭土在乙醇中超声扩散,得到混合物A;
S2、将全氟辛基三乙氧基硅烷加入S1中所述混合物A超声并搅拌5h,得到混合物B;
S3、将S2中所述混合物B固液分离,并冷冻干燥固相,得到粉末状固体;
S4、将S3中所述粉末状固体以球磨,得到改性滑石粉或改性高岭土。
2.根据权利要求1所述的基于六方氮化硼粉体的防晒控油粉饼,其特征在于,以下组分按重量份计,还包含:0.01~0.1份苯氧乙醇和/或苯甲酸钠。
3.根据权利要求2所述基于六方氮化硼粉体的防晒控油粉饼,其特征在于,所述全氟辛基三乙氧基硅烷具有以下结构:
。
4.一种根据权利要求1所述的基于六方氮化硼粉体的防晒控油粉饼的制造方法,其特征在于,以下组分均按重量份计,包括以下步骤:
步骤1:将改性滑石粉15~20份、改性高岭土2~8份、六方氮化硼10~20份,二氧化钛10~15份、二氧化硅2~5份、氧化锌5~15份、硬质酸钠2~5份、丁基甲氧基二苯甲酰基甲烷2~5份、淀粉5~10份、尿囊素1~5份、烟酰胺1~5份混合,球磨,得到混合物Ⅰ;
步骤2:再将氧化铁黑1~4份,氧化铁红0.1~1份,氧化铁黄5~10份混合,加入所述混合物Ⅰ中,在固体打粉机内,得到混合物Ⅱ;
步骤3:称取角鲨烷1~5份、蚕丝油1~5份、聚二甲基硅氧烷2~4份、戊二醇1~4份、水1~3份、苯氧乙醇和/或苯甲酸钠0.01~0.1份在40~50℃恒温水浴混合,得到混合物Ⅲ;
步骤4:使用喷雾混合法将所述混合物Ⅲ与所述混合物Ⅱ混合至显色均匀,得到混合物Ⅳ;
步骤5:将步所述混合物Ⅳ置于固体打粉机中以3500r/min混合3~5分钟,重复2~3次,得到混合物Ⅴ;
步骤6:将所述混合物Ⅴ压盘制得粉饼坯体。
5.根据权利要求1所述的基于六方氮化硼粉体的防晒控油粉饼或权利要求3所述的基于六方氮化硼粉体的防晒控油粉饼的制造方法,其特征在于,所述二氧化硅为多孔球形,所述二氧化硅的平均粒径为3µm,且其吸油量可达130ml/100g。
6.根据权利要求1所述的基于六方氮化硼粉体的防晒控油粉饼或权利要求3所述的基于六方氮化硼粉体的防晒控油粉饼的制造方法,其特征在于,所述二氧化钛与六方氮化硼掺杂构成防晒剂。
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