CN116376324A - 二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料 - Google Patents

二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料 Download PDF

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CN116376324A
CN116376324A CN202211677462.8A CN202211677462A CN116376324A CN 116376324 A CN116376324 A CN 116376324A CN 202211677462 A CN202211677462 A CN 202211677462A CN 116376324 A CN116376324 A CN 116376324A
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titanium dioxide
composite pigment
dioxide composite
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tio
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赵显垈
金鐘根
权玟廷
金尾书
黄俊弼
李艺瑟
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Cosmecca Korea Co Ltd
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Abstract

本发明公开了二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料。根据本发明的二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料，通过在高屈折率的无机复合颜料上涂布被膜形成剂的工艺，可以对颜料的表面进行改性来提高效能，可以实现提高无机复合颜料在水包油剂型中的分散力、附着力及耐久性等的效果，可以提供满足消费者的使用体验，外观的水润感提升了的凝胶状的二氧化钛复合颜料。并且，光滑柔顺的性状突出、涂抹性佳，皮肤涂抹时的感受舒适且清爽，且随着剂型的分散度和稳定性提高，可以提高SPF和PA数值来实现有效的紫外线屏蔽。

Description

二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧 化钛复合颜料
技术领域
本发明涉及一种二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料。更详细地说，本发明涉及分散力、附着力及耐久性得以提高，通过涂布处理工艺对颜料表面进行改性来实现光滑柔顺的性状，从而能够增强涂抹性和使用体验来得到清爽感，且提高了SPF和PA数值的紫外线屏蔽性能优异的二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料。
背景技术
女性追求美的本能与生俱来，但目前为了使自身显得更隽美的体形管理、对于美容或化妆品关注的趋势愈发明显。
并且，不局限于女性，随着男性出于皮肤管理的目的开始关注化妆品，化妆品市场持续扩大，市场上出现了多种化妆品。
通常，化妆品大致可分为基础化妆品、粧前底霜和彩妆化妆品等，被调制成固态、液态或凝胶状的化妆料并采用多种化妆品容器来保管这些化妆品。
最近，能够展现保湿、美白、祛纹、防紫外线、淡化粉刺、缓解过敏性皮炎、消炎和角质溶解等多种功能的功能性化妆品也得到了广大消费者的青睐。
另一方面，颜料在通常意义上是指使物质发色的色素。相对于染料是作为溶于水的色素渗入并固着在纤维或纸中，颜料作为不溶于水或油等中的微粉状的固体掺混到塗料、绘画材料、印刷油墨、塑料、橡胶等中来进行使用。
颜料分为无机颜料和有机颜料，无机颜料具有在热、日照条件下稳定不变色的特点，有机颜料是将染料调制成不溶于水的形态，色彩鲜明、品种繁多。这种颜料多用于彩妆化妆品，其主要目的恰当地覆盖并将色彩赋予给皮肤，即在遮掩老年斑、雀斑等使皮肤呈现心仪的色彩的同时，吸收皮脂等的皮肤分泌物来抑制脸部出油的问题，展现健康的魅力焕发的容貌。
然而，使用颜料时需通盘考虑作为化妆品的卫生性、感觉性要素。因此，作为化妆品用颜料所需的条件，除了对于皮肤无害以外，需具有符合法律规定的品目、规格、试验方法、使用标准的品质。
彩妆化妆品是在多种基材中分散由有机颜料、无机颜料(体质颜料、美白颜料、彩妆颜料、珠光颜料)等形成的混合粉体而成。作为制作基材的原料，可以列举油脂、蜡、碳化氢、脂肪酸、高级醇、合成酯油等的油性原料，多元醇、水溶性高分子等的水性原料及表面活性剂(乳化剂、分散剂)等。通过调配这些原料，可以制作多种性状的化妆品。
就颜料在彩妆化妆品中的功能而言，有机颜料、无机颜料用于调整产品的色调，美白颜料除了色调以外，还用于被覆力的调控。体质颜料及其他粉末在作为颜料的稀释剂用来调整色调的同时，还用于确保产品的延展性、附着性、光泽或维持该产品的形态的目的。
另一方面，作为功能性化妆品之一的防紫外线化妆品包括通过吸收、发散及反射等的方式屏蔽紫外线的无机紫外线屏蔽剂、有机紫外线屏蔽剂。
有机紫外线屏蔽剂以吸收紫外线来减少到达皮肤的紫外线量的方式屏蔽光，无机紫外线屏蔽剂则采用了反射、发散紫外线来保护皮肤的方式。
作为无机紫外线屏蔽剂的例子，可以列举氧化锌(ZnO)、二氧化钛(TiO2)。这类无机紫外线屏蔽剂虽有白浊现象且皮肤涂抹性不佳，但对于包括紫外线在内的太阳光线的惰性大、稳定性优异。此外，不被皮肤吸收或在皮肤蓄积，不会导致皮肤刺激或过敏的问题。
本发明人经潜心研究开发了具有紫外线屏蔽效果的二氧化钛复合颜料的制造方法，由此可以提供分散力、附着力及耐久性得以提高，通过涂布处理工艺对颜料表面进行改性来实现光滑柔顺的性状，增强涂抹性和使用体验来得到清爽感，且提高了SPF和PA数值的紫外线屏蔽性能优异的二氧化钛复合颜料。
发明内容
发明要解决的问题
本发明的目的在于，通过在高屈折率的无机复合颜料上涂布被膜形成剂的工艺，对颜料的表面进行改性来提高效能。
并且，本发明的目的还在于，得到无机复合颜料在水包油剂型中的分散力、附着力及耐久性等提高的效果。
并且，本发明的目的还在于，提供满足消费者的使用感受，外观的水润感提升的凝胶状的二氧化钛复合颜料。
并且，本发明的目的还在于，提供光滑柔顺的性状突出、涂抹性佳，皮肤涂抹时的感受舒适且清爽的二氧化钛复合颜料。
并且，本发明的目的还在于，提高剂型的分散度和稳定性，进而提高SPF和PA数值来实现有效的紫外线屏蔽。
技术方案
本发明的一个方面，可以提供一种二氧化钛复合颜料的制造方法，该制造方法包括：步骤(a)在蒸馏水中添加二氧化钛，进行搅拌来使之分散，步骤(b)将四氯化钛水溶液和浓度为10重量％～30重量％的氢氧化钠水溶液添加到上述分散的二氧化钛中，进行搅拌来实施氢氧化钛涂布，步骤(c)静置上述氢氧化钛涂布后的溶液，用蒸馏水洗涤生成的白色沉积物并进行过滤，步骤(d)干燥上述过滤得到的粉体，以及步骤(e)将上述的氢氧化钛复合粉体在700℃～950℃的温度范围进行烧制来形成二氧化钛复合颜料。
其中，上述步骤(a)～步骤(d)的处理工艺的反应式可以为TiO2+TiOCl2+2NaOH→TiO(OH)2/TiO2+Na+Cl-，上述步骤(e)的处理工艺的反应式可以为TiO(OH)2/TiO2→TiO2+H2O。
根据本发明的二氧化钛复合颜料的制造方法，还可以包括将上述二氧化钛复合颜料90重量％～98重量％和水溶性聚合物或有机硅、硅烷、有机硅共聚物2重量％～10重量％加入到亨舍尔混合机中进行分散处理的步骤。
根据本发明的二氧化钛复合颜料的制造方法，还可以包括干燥上述分散处理的粉体的步骤。
根据本发明的二氧化钛复合颜料的制造方法，还可以包括进一步分散处理上述干燥的粉体来获得亲水性或疏水性的步骤。
并且，本发明的另一个方面可以提供利用上述的制造方法制造的二氧化钛复合颜料。
发明效果
根据本发明，通过在高屈折率的无机复合颜料上涂布被膜形成剂的工艺，可以对颜料的表面进行改性来提高效能。
并且，可以得到无机复合颜料在水包油剂型中的分散力、附着力及耐久性等提高的效果。
并且，可以提供满足消费者的使用体验，外观的水润感提升的凝胶状的二氧化钛复合颜料。
并且，可以提供光滑柔顺的性状突出、涂抹性佳、皮肤涂抹时的感受舒适且清爽的二氧化钛复合颜料。
并且，随着剂型的分散度和稳定性提高，可以实现提高了SPF和PA数值的有效的紫外线屏蔽。
附图说明
图1为表示本发明的一个实施例的二氧化钛复合颜料的制造方法的工艺流程图。
图2为表示比较例1(对照A)的分散程度的图像。
图3为表示比较例2(对照B)的分散程度的图像。
图4为表示试验例1(试验A)的分散程度的图像。
图5为表示试验例2(试验B)的分散程度的图像。
图6为表示比较例1、比较例2、试验例1及试验例2的SPF和PA数值的图。
具体实施方式
以下，参照附图来详细说明本发明的优选实施例。但本发明不局限于以下说明的实施例，也可以通过其他方式来实施本法发明。以下说明的实施例用于完整全面地体现本发明的内容，并力求能够将本发明的思想充分地传达给本领域技术人员。本说明书中，对于相同的构成要素赋予相同的符号，省略重复的说明。
图1为表示本发明的一个实施例的二氧化钛复合颜料的制造方法的工艺流程图，图2为表示比较例1(对照A)的分散程度的图像，图3为表示比较例2(对照B)的分散程度的图像。图4为表示试验例1(试验A)的分散程度的图像，图5为表示试验例2(试验B)的分散程度图像，图6为表示比较例1、比较例2、试验例1及试验例2的SPF和PA数值的图。
参照图1～图6，作为本发明的一个实施例的二氧化钛复合颜料的制造方法，大致包括在蒸馏水中添加二氧化钛，进行搅拌来使之分散的步骤(a)(S100)，将四氯化钛水溶液和浓度为10重量％～30重量％的氢氧化钠水溶液添加到上述分散的二氧化钛中，进行搅拌来实施氢氧化钛涂布的步骤(b)(S200)，静置上述氢氧化钛涂布后的溶液，用蒸馏水洗涤生成的白色沉积物并进行过滤的步骤(c)(S300)，干燥上述过滤得到的粉体的步骤(d)(S400)，以及将上述的氢氧化钛复合粉体在700℃～950℃的温度范围进行烧制来形成二氧化钛复合颜料的步骤(e)(S500)。以下，具体说明步骤(a)～步骤(e)的处理工艺。
首先，S100，在蒸馏水中添加二氧化钛后在70℃～90℃的温度范围进行搅拌。其次，S200，将四氯化钛水溶液、作为碱源的浓度为10重量％～30重量％的氢氧化钠水溶液添加到上述分散的二氧化钛中，在70℃～90℃的温度范围进行搅拌来实施氢氧化钛涂布。
随后，S300，静置上述氢氧化钛涂布后的溶液，用蒸馏水洗涤生成的白色沉积物并进行过滤。随后，S400，将上述过滤得到的粉体置于干燥装置中，在60℃～100℃的温度范围干燥18小时。
随后，S500，将上述的氢氧化钛复合粉体在700℃～950℃的温度范围进行烧制来形成氧化物，由此得到二氧化钛复合颜料。
此时，上述S100步骤～S400步骤的处理工艺的反应式为TiO2+TiOCl2+2NaOH→TiO(OH)2/TiO2+Na+Cl-，上述S500步骤的处理工艺的反应式为TiO(OH)2/TiO2→TiO2+H2O。
另一方面，按照以下方式实施表面处理的工艺，从而将亲水性及疏水性的特性赋予给按照上述方式得到的二氧化钛复合颜料。即，以下的过程相当于在上述二氧化钛复合颜料上涂布被膜形成剂的处理工艺。
首先，S600，将上述二氧化钛复合颜料90重量％～98重量％和水溶性聚合物或有机硅、硅烷、有机硅共聚物2重量％～10重量％加入到亨舍尔混合机中，通过5秒、3次的分散处理来实施涂布。
随后，S700，将上述涂布的粉体在60℃～100℃的温度范围干燥18小时。干燥后，S800，进一步粉碎因所涂布的水溶性聚合物或有机硅、硅烷、有机硅共聚物的影响凝集的粉体，从而将亲水性、疏水性赋予给所述粉体。
以下，说明通常的无机颜料和本发明的一个实施例的二氧化钛复合颜料、及对实施了被膜涂布的情形进行对比的试验结果。
首先，试验样品如以下所示。
表1
说明
空白 空白对照
对照A 纳米尺寸的无机颜料(CR-50)
对照B SH 52
试验A SH 52_250nm&被膜形成剂涂布5％
试验B SH 52_160nm&被膜形成剂涂布5％
再者，以上试验样品各自的试验配方如以下所示。
表2
Figure BDA0004017562070000061
试验样品中，空白为没有加入颜料的试验样品，对照A(比较例1)为采用通常的无机颜料(CR-50)的情形。对照B(比较例2)为本发明的二氧化钛复合颜料没有经表面处理的例子，试验A(试验例1)为250nm尺寸的二氧化钛复合颜料经5％的被膜形成剂处理的情形，试验B(试验例2)为160nm尺寸的二氧化钛复合颜料经5％的被膜形成剂处理的情形。
图2～图5中示出了以上样品的分散程度对比试验的图像。图2为比较例1、即采用标准的无机颜料(CR-50)的情形，可以确认到表面起伏和凝结成块的现象。
然而，自图3的比较例2开始、即在采用二氧化钛复合颜料的情形，可以确认上述提到的起伏和凝结成块的现象得到了显著的改善。尤其是，在经表面处理的试验例1(图4)和试验例2(图5)的情形，分散更为充分，几乎没有起伏和凝结成块的现象。
另一方面，为了比较紫外线屏蔽能力，测定了上述同一试验样品的日光防护指数(Sun Protection Factor,SPF)及紫外线防护指数(Protection Factor of UVA,PA)，图6中示出了测定结果。
如图6所示，与采用通常的颜料(对照A、空白对照)的情形相比，可以确认采用本发明的一个实施例的二氧化钛复合颜料(对照B、试验A及试验B)时的SPF及PA数值得到了极大的提升。
尤其是，采用经表面处理且小尺寸的二氧化钛复合颜料时，这些数值的提升效果更为明显。
根据以上说明的本发明的实施例的二氧化钛复合颜料的制造方法，通过在高屈折率的无机复合颜料上涂布被膜形成剂的工艺，可以对颜料的表面进行改性来提高效能，可以实现无机性复合颜料在水包油剂型中的分散力、附着力及耐久性等提高了的效果，可以提供满足消费者的使用体验且外观的水润感提升了的凝胶状的二氧化钛复合颜料。
并且，光滑柔顺的性状突出、涂抹性佳，皮肤涂抹时的感受舒适且清爽，且随着剂型的分散度和稳定性提高，可以提高SPF和PA数值来实现有效的紫外线屏蔽。
以上，参照本发明的一个实施例进行了说明。本领域的技术人员知晓，在不脱离本发明的权利要求书记载的本发明的思想及范围的前提下，可以对本发明进行多种改进和改良，且只要基本包含本发明的权利要求书的构成要素，这些改进和改良均包含在本发明的技术范畴内。

Claims (7)

1.一种二氧化钛复合颜料的制造方法，其特征在于，该制造方法包括
步骤(a)，在蒸馏水中添加二氧化钛，进行搅拌来使之分散，
步骤(b)，将四氯化钛水溶液和浓度为10重量％～30重量％的氢氧化钠水溶液添加到上述分散的二氧化钛中，进行搅拌来实施氢氧化钛涂布，
步骤(c)，静置上述氢氧化钛涂布后的溶液，用蒸馏水洗涤生成的白色沉积物并进行过滤，
步骤(d)，干燥上述过滤得到的粉体，以及
步骤(e)，将上述的氢氧化钛复合粉体在700℃～950℃的温度范围进行烧制来形成二氧化钛复合颜料。
2.如权利要求1所述的二氧化钛复合颜料的制造方法，其中，上述步骤(a)～步骤(d)的处理工艺的反应式为TiO2+TiOCl2+2NaOH→TiO(OH)2/TiO2+Na+Cl-。
3.如权利要求1所述的二氧化钛复合颜料的制造方法，其中，上述步骤(e)的处理工艺的反应式为TiO(OH)2/TiO2→TiO2+H2O。
4.如权利要求1所述的二氧化钛复合颜料的制造方法，其中，还包括将上述二氧化钛复合颜料90重量％～98重量％和水溶性聚合物或有机硅、硅烷、有机硅共聚物2重量％～10重量％加入到亨舍尔混合机中进行分散处理的步骤。
5.如权利要求4所述的二氧化钛复合颜料的制造方法，其中，还包括干燥上述分散处理的粉体的步骤。
6.如权利要求5所述的二氧化钛复合颜料的制造方法，其中，还包括进一步分散处理上述干燥的粉体来获得亲水性或疏水性的步骤。
7.一种二氧化钛复合颜料，其特征在于，该二氧化钛复合颜料是用权利要求1～6中任意一项所述的二氧化钛复合颜料的制造方法制得。
CN202211677462.8A 2021-12-30 2022-12-26 二氧化钛复合颜料的制造方法及利用该制造方法制造的二氧化钛复合颜料 Pending CN116376324A (zh)

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