CN113416434B - 植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法及其应用 - Google Patents
植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法及其应用，该方法首先将有机颜料分子与凹土混合均匀，通过高温烘焙法制备出类玛雅蓝有机/无机杂化颜料；随后通过水热法在类玛雅蓝表面包覆一层二氧化钛，得到二氧化钛/类玛雅蓝复合颜料；最后通过表面改性法用天然植物油对复合颜料进行表面改性，制备出环保型彩妆颜料。本发明中所述的类玛雅蓝杂化颜料为安全环保、具有抗炎作用、颜色可配的凹土基颜料，二氧化钛层赋予彩妆防紫外线即防晒功能；天然植物油改善了颜料的表面性能，使其与皮肤具有良好的相容性，且赋予彩妆抗衰老性能，适用于粉底霜、眼影等彩妆领域。
Description
技术领域
本发明涉及日用化妆品技术领域，具体涉及一种环保型抗衰老防晒彩妆颜料的制备方法，尤其涉及一种植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法及其应用。
背景技术
色素也称着色剂或色料，是彩妆的主要成分之一。根据彩妆类化妆品的性能和作用，对彩妆类化妆品色素的主要要求为：（1）颜料鲜艳、美观、色感好；（2）着色力强，透明性好或遮盖力强；（3）与其他组分相容性好，分散性好；（4）耐光性、耐热性、耐酸性、耐碱性和耐有机溶剂性强；（4）安全性高，在我国《化妆品卫生规范》允许使用范围及限制条件下，无毒、无刺激、无过敏性。
粉底霜和眼影一般使用耐光性强、不易引起过敏现象，使用安全系数大的无机颜料为色素，例如氧化铁红、氧化铁黄、群青、氧化铬绿、氢氧化铬绿等。但它们具有以下缺点：氧化铁需要在严格控制的条件下制备；群青对酸敏感，易褪色，产生硫化氢气体；而氧化铬绿、氢氧化铬绿含有重金属铅和砷。另外，无机色素色谱不全、产品单调、很多颜色需通过配色得到；色调的丰富性不强，且与皮肤相容性差。针对以上问题，本发明提供了一种无毒、无刺激、与皮肤相容性好、抗衰老防晒彩妆颜料的制备方法。
发明内容
发明目的：本发明提供了一种植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法及其应用，本发明中所述的类玛雅蓝杂化颜料为安全环保、具有抗炎作用、颜色可配的凹土基颜料，包覆的二氧化钛层赋予彩妆防紫外线即防晒性能；植物油改善了颜料的表面性能，使其与皮肤具有良好的相容性，且赋予彩妆抗衰老性能；适用于粉底霜、眼影等彩妆领域。
技术方案：一种环保型抗衰老防晒彩妆颜料的制备方法，包括以下步骤：S1：将有机颜料分子与凹土混合均匀后，放入100～200 ℃烘箱中烘焙24～48 h，在乙醇溶液中浸泡6～12 h，离心、干燥、研磨至无颗粒，制备出类玛雅蓝有机/无机杂化颜料；S2：称取类玛雅蓝有机/无机杂化颜料到无水乙醇中，超声分散15～30 min,加入氨水，搅拌10～30 min，再加入钛酸四丁酯，在40～50 ℃水浴下恒温搅拌8～12 h，离心、干燥、研磨至无颗粒，制备出二氧化钛/类玛雅蓝复合颜料；S3：称取天然植物油分散于无水乙醇中，加入二氧化钛/类玛雅蓝复合颜料，混合均匀后，60～80 ℃水浴下恒温搅拌2～5 h，离心、干燥、研磨至无颗粒，制备出植物油改性的二氧化钛/类玛雅蓝复合颜料。
优选地，S1中所述的有机颜料分子为靛红、靛蓝、甲基紫、亚甲基蓝、刚果红、茜素黄或市售彩妆有机颜料。
优选地，S1中所述的凹土为过200目筛的纯化凹土，其直径为20～100 nm。
优选地，S1中所述的有机颜料分子与纯化凹土的质量比为1～15：100。
优选地，S2中所述的原料质量配比为：类玛雅蓝有机/无机杂化颜料：无水乙醇：氨水：钛酸四丁酯 = 1～10：50～100：0.1～1：0.2～2。
优选地，S3中所述的天然植物油种类为具有美容抗衰老作用的橄榄油、椰子油、摩洛哥坚果油、鳄梨油、葡萄籽油、棕榈油、荷荷巴油、甜杏仁油、月见草油、金盏花油的任意一种或其组合。
优选地，S3中所述的原料质量配比为：植物油：二氧化钛/类玛雅蓝复合颜料：无水乙醇 = 0.2～0.5：10：100～200。
优选地，S1、S2、S3中所述的离心过程中离心转速为1000～5000 r/min，离心时间为30～60 min,。
优选地，S1、S2、S3中所述的烘干过程中温度为60～100 ℃，干燥时间为6～24 h。
本发明还提供了一种植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法制备出的复合颜料在环保型抗衰老防晒彩妆颜料中的应用。
有益效果：本发明通过高温烘焙法制备出类玛雅蓝杂化颜料；随后通过水热法在类玛雅蓝颜料表面包覆一层二氧化钛；最后通过表面改性法用天然植物油对复合颜料进行表面改性，制备出植物油改性的二氧化钛/类玛雅蓝复合颜料，该复合颜料可以应用在环保型防晒彩妆颜料中。
与现有技术相比，本发明具有如下优势：
本发明所用颜料主体为类玛雅蓝有机/无机杂化颜料，有机颜料分子在高温下通过分子热运动进入凹土孔道，且通过乙醇浸泡，洗除游离的有机分子，颜料载体为对人体无害、安全健康且具有抗炎作用的凹土。
本发明通过水热法在类玛雅蓝颜料表面沉积一层二氧化钛，一方面对凹土孔道进行了封堵，因此增强了颜料的耐光性，另一方面二氧化钛对紫外线阻隔能力强，赋予彩妆颜料防紫外线即防晒功能。
本发明通过天然植物油对二氧化钛/类玛雅蓝复合颜料进行改性，植物油中不饱和脂肪酸中羧基与复合颜料凹土表面的羟基发生酯化反应，一方面降低了颜料的表面能，使其用在彩妆颜料中时，与皮肤具有良好的相容性；另一方面天然不饱和脂肪酸的存在，赋予彩妆颜料抗衰老性能。
具体实施方式
下面结合具体实施方式对本发明进一步阐述，但并不限制本发明。
实施方式1：
一种环保型抗衰老防晒彩妆颜料的制备方法，包括以下步骤：
S1：将2 g有机颜料靛红与20 g纯化凹土混合均匀后，放入150 ℃烘箱中烘焙48h，在乙醇溶液中浸泡12 h，离心、干燥、研磨至无颗粒，制备出类玛雅蓝-靛红有机/无机杂化颜料；
S2：称取5 g类玛雅蓝-靛红有机/无机杂化颜料到50 ml无水乙醇中，超声分散30min，加入0.2 ml氨水，搅拌30 min，再加入0.4 ml钛酸四丁酯，在45 ℃水浴下恒温搅拌12h，离心、干燥、研磨至无颗粒，制备出二氧化钛/类玛雅蓝-靛红复合颜料；
S3：称取0.10 g橄榄油分散于50 ml无水乙醇中，加入2 g二氧化钛/类玛雅蓝-靛红复合颜料，混合均匀后，75 ℃水浴下恒温搅拌4 h，离心、干燥、研磨至无颗粒，制备出橄榄油改性的二氧化钛/类玛雅蓝-靛红复合颜料。
实施方式2：
S1：将2 g市售彩妆有机颜料果绿与20 g纯化凹土混合均匀后，放入150 ℃烘箱中烘焙48 h，在乙醇溶液中浸泡12 h，离心、干燥、研磨至无颗粒，制备出类玛雅蓝-果绿有机/无机杂化颜料；
S2：称取5 g类玛雅蓝-果绿有机/无机杂化颜料到50 ml无水乙醇中，超声分散30min，加入0.2 ml氨水，搅拌30 min，再加入0.4 ml钛酸四丁酯，在45 ℃水浴下恒温搅拌12h，离心、干燥、研磨至无颗粒，制备出二氧化钛/类玛雅蓝-果绿复合颜料；
S3：称取0.10 g椰子油分散于50 ml无水乙醇中，加入2 g二氧化钛/类玛雅蓝-靛红复合颜料，混合均匀后，75 ℃水浴下恒温搅拌4 h，离心、干燥、研磨至无颗粒，制备出的椰子油改性的二氧化钛/类玛雅蓝-果绿复合颜料。
实施方式3：
S1：将3 g有机颜料甲基紫与20 g纯化凹土混合均匀后，放入180 ℃烘箱中烘焙48h，在乙醇溶液中浸泡6 h，离心、干燥、研磨至无颗粒，制备出类玛雅蓝-甲基紫有机/无机杂化颜料；
S2：称取5 g类玛雅蓝-甲基紫有机/无机杂化颜料到50 ml无水乙醇中，超声分散30 min，加入0.3 ml氨水，搅拌30 min，再加入0.6 ml钛酸四丁酯，在45 ℃水浴下恒温搅拌12 h，离心、干燥、研磨至无颗粒，制备出二氧化钛/类玛雅蓝-甲基紫复合颜料；
S3：称取0.20 g荷荷巴油分散于50 ml无水乙醇中，加入2 g二氧化钛/类玛雅蓝-靛红复合颜料，混合均匀后，80 ℃水浴下恒温搅拌3 h，离心、干燥、研磨至无颗粒，制备出荷荷巴油改性的二氧化钛/类玛雅蓝-甲基紫复合颜料。
通过上述各实施例1制备的植物油改性的二氧化钛/类玛雅蓝复合颜料，将其应用在市售粉底霜中，其性能指标如表1所示。
表1 粉底霜性能指标
防晒性能评价：
采用SPF（防晒指数）-290s分析***，，在SPF-290s分析***上先描绘出一条载体的空白本底曲线，用点样器在透明膜上均匀点上2mg/cm2的样品，晾干后，随机检测10个点，描绘出相应光波长，计算样品检测结果，得到SPF值以及标准差，每个样品检测5次，结果如表2所示，其中对比例为市售粉底霜：
表2 对比例与实施例的SPF（防晒指数）检测结果
| 组别 | 对比例 | 实施例1 | 实施例2 | 实施例3 |
| SPF值 | 5±0.56 | 25±0.35 | 26±0.21 | 25±0.48 |
由表1、2可以看出，利用本发明中植物油改性的二氧化钛-类玛雅蓝复合颜料制备的粉底霜符合常规粉底霜的指标要求，不含有汞、砷和铅等重金属物质，使用安全健康且具有防晒效果。上述实施方式只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰，都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于，包括以下步骤：
S1：将有机颜料分子与凹土混合均匀后，放入100～200 ℃烘箱中烘焙24～48 h，在乙醇溶液中浸泡6～12 h，离心、干燥、研磨至无颗粒，制备出类玛雅蓝有机/无机杂化颜料；
S2：称取类玛雅蓝有机/无机杂化颜料到无水乙醇中，超声分散15～30 min,加入氨水，搅拌10～30 min，再加入钛酸四丁酯，在40～50 ℃水浴下恒温搅拌8～12 h，离心、干燥、研磨至无颗粒，制备出二氧化钛/类玛雅蓝复合颜料；
S3：称取天然植物油分散于无水乙醇中，加入二氧化钛/类玛雅蓝复合颜料，混合均匀后，60～80 ℃水浴下恒温搅拌2～5 h，离心、干燥、研磨至无颗粒，制备出植物油改性的二氧化钛/类玛雅蓝复合颜料。
2.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S1中所述的有机颜料分子为靛红、靛蓝、甲基紫、亚甲基蓝、刚果红或茜素黄。
3.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备
方法，其特征在于：S1中所述的凹土为过200目筛的纯化凹土，其直径为20～100 nm。
4.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备
方法，其特征在于：S1中所述的有机颜料分子与凹土的质量比为1～15：100。
5.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S2中所述的原料质量配比为：类玛雅蓝有机/无机杂化颜料：无水乙醇：氨水：钛酸四丁酯 = 1～10：50～100：0.1～1：0.2～2。
6.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S3中所述的天然植物油种类为具有美容抗衰老作用的橄榄油、椰子油、摩洛哥坚果油、鳄梨油、葡萄籽油、棕榈油、荷荷巴油、甜杏仁油、月见草油、金盏花油的任意一种或其组合。
7.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S3中所述的原料质量比为：天然植物油：二氧化钛/类玛雅蓝复合颜料：无水乙醇=0.2～0.5：10：100～200。
8.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S1、S2、S3中所述的离心过程中离心转速为1000～5000 r/min，离心时间为30～60min。
9.根据权利要求1所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法，其特征在于：S1、S2、S3中所述的干燥过程中温度为60～100 ℃，干燥时间为6～24 h。
10.一种如权利要求1至9中任一项所述的植物油改性的二氧化钛/类玛雅蓝复合颜料的制备方法制备出的复合颜料在环保型抗衰老防晒彩妆颜料中的应用。
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| CN112079973A (zh) * | 2020-09-01 | 2020-12-15 | 淮阴工学院 | 高耐候性类玛雅蓝染料的制备方法 |
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