CN112654682A - 香槟色调的金属效应颜料 - Google Patents

香槟色调的金属效应颜料 Download PDF

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CN112654682A
CN112654682A CN201980052376.8A CN201980052376A CN112654682A CN 112654682 A CN112654682 A CN 112654682A CN 201980052376 A CN201980052376 A CN 201980052376A CN 112654682 A CN112654682 A CN 112654682A
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layer
metallic effect
coating
thickness
pigment
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CN112654682B (zh
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伊冯娜·宾德尔
阿达贝尔特·胡贝尔
丹尼尔·格拉泽尔
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Schlenk Metallic Pigments GmbH
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Abstract

本发明涉及金属效应颜料，其具有高遮盖力和薄氧化铁涂层，以产生香槟色调。

Description

香槟色调的金属效应颜料
技术领域
本发明涉及金属效应颜料，其具有高遮盖力和薄氧化铁层，以产生香槟色色调。
背景技术
迄今为止，还没有具有高遮盖力和淡黄-米黄(yellowish-beige)色调的已知的类似金属效应颜料或珠光颜料，该淡黄-米黄色调的色调角(huv)的范围为50～65(香槟色调)且饱和度(Suv)的范围为0.2～0.3(对于△E45°≤3)。当前市场上有具有相似色调的颜料(例如，Eckart公司的
Figure BDA0002935814120000011
或来自Merck公司的Iriodin 9602)的遮盖力有时不令人满意和/或具有明显偏离的色调和色彩饱和度值。
EP2999752B1公开了一种基于来自VMP工艺的薄Al基底薄片的金属效应颜料，其具有高遮盖力且以Fe2O3作为着色层。WO2013/175339公开了一种具有至少一层金属氧化物层的基于铝的金属效应颜料。EP2303969B1公开了一种铁铝混合物的效应颜料的生产。WO2015/040537A1公开了一种不可磁化的效应颜料，其由具有一个或多个钝化层和掺杂铝的氧化铁层的铝或铝合金芯组成。WO2007/093334A1公开了一种生产色彩效应颜料的方法及其在化妆品中的用途。这些有色效应颜料由着色层包围的含铝芯组成的颜料和/或具有至少一种金属氧化物层的效应颜料，该着色层通过Al芯的湿化学(wet-chemical)氧化产生，该金属氧化物层包括至少一种着色颜料。CA2,496,126公开了一种用于化妆品的基于金属(银、金、铜、铝、锌、钛及其合金)的效应颜料，其在湿化学方法中通过溶胶-凝胶法(sol-gelprocess)涂覆另外的金属氧化物层。US7,828,890B2公开了一种具有铝或铝合金芯的效应颜料，且在铝或铝合金芯的周围包覆含有氧化铝的层或含有氧化铝/氢氧化物的层，该层可通过对薄片状铝或铝合金颜料进行湿化学氧化获得，其中，铝或铝合金芯中金属铝的含量不超过90wt％(基于颜料的总重量)，被氧化的铝或铝合金颜料具有至少一种具有高折射率(折射率>1.95)的金属硫属化物层，其在具有高折射率的金属硫属化物层和包覆含氧化铝或含氧化铝/氢氧化物的层(混合层)之间形成。EP0950693A1公开了一种基于非金属基底的多层珠光颜料。WO2011/085780A1公开了一种基于非金属基底的多层效应颜料。WO96/22336A1公开了一种基于薄片状铝基底的有色颜料，其涂覆有金属氧化物层，金属氧化物层中具有着色颜料。专业书籍“金属效应颜料”(第二修订版，作者：彼得·威斯林等，文森茨出版社)在第三部分“特种铝颜料”的第二章“彩色铝颜料”(第70-76页)中记载了具有“香槟色”外观(商品名
Figure BDA0002935814120000021
)的氧化铝颜料的生产及其与着色颜料结合的用途。与此类似，DE19520312B4公开了一种通过铝薄片的湿化学氧化生产彩色效应颜料。
EP3345974A1和EP3081601A1确实描述了金属效应颜料或珠光颜料，但是没有描述那些淡黄-米黄色调的颜料，该该淡黄-米黄色调的色调角(hue angle)(huv)的范围为50～65(香槟色调)且饱和度(Suv)的范围为0.2～0.3(对于△E45°≤3)。
发明内容
因此，本发明的目的是提供一种具有高遮盖力和淡黄-米黄色调的金属效应颜料，该淡黄-米黄色调的色调角(huv)的范围为50～65(香槟色调)且饱和度(Suv)的范围为0.2～0.3(对于△E45°≤3)。
该目的通过权利要求描述的实施方式实现。
更特别地，提供了一种基于经涂覆的铝基底薄片的金属效应颜料，其中，铝基底薄片的厚度为5～35nm(优选地为15～25nm)、具有整体结构且被小于10nm(通常为2～5，通常为2～3nm)的Al2O3“自然”(native)钝化层(即生产过程中产生的钝化层，但未在单独的处理步骤中应用)包围，这些铝基底薄片被至少一层层厚为10～100nm(优选地，20～80nm)的SiO2涂层A包裹，并支撑一层另外施加的Fe2O3涂层B，该涂层B包裹了具有SiO2涂层A的基底薄片，其层厚为5～45nm(优选地为10～45nm，更优选地为20～45nm，特别优选地为20～40nm)，其特点是，色素沉着(pigmentation)不大于7％时△E45≤3，特别地，色素沉着小于7％时△E45°≤1，饱和度(Suv)的范围为0.2～0.3，色调角(huv)的值为50～65，随角异色/Alman指数的值大于26，Gdiff(粒度)值不大于6。
可选地，还包括依次包裹涂层B的外层C，例如是1～30nm厚的SiO2层，其还可选地渗透(penetrate)下方的Fe2O3。此外，可对层B或层C(如果存在)进行有机或有机-无机表面改性(surface modification)。
可以被认为是实际钝化层的SiO2层A通过溶胶-凝胶法(sol-gel process)湿化学地(wet-chemically)进行施加。层B由通过沉淀反应湿化学地施加的Fe2O3组成，其层厚为5～45nm，优选地为10～45nm，更优选地为20～45nm，更特别地为20～40nm。氧化铁层也可以是混合层，该混合层包括一种或两种选自Al2O3或TiO2的金属氧化物，基于层B，其含量大于0～20wt％。
铝基底薄片是多晶态的(polycrystalline)且平均厚度为5～35nm，优选地为15～25nm。优选地，每个基底薄片具有非常均匀的厚度。然而，由于生产过程，薄片内的厚度可能存在波动。基于所讨论的薄片的平均厚度，这些波动应优选地不大于±25％，更优选最多为±10％。这里的平均厚度是指最大和最小厚度的数值平均值。通过基于经涂覆的基底薄片的透射和扫描电子显微照片(TEM和SEM)的测量确定最小和最大的层厚。
所使用的铝薄片优选地是那些已知的真空金属化颜料(VMP)。VMP可以通过从金属化(metallized)的薄膜上剥离铝来获得。它们以特别低的基底薄片厚度和特别光滑的表面而出名，该特别光滑的表面具有增强的反射率。在本发明的上下文中，片状物或薄片是厚度/长度比至少为1:100(优选地，更高)的那些薄片。
这里提及的涂层或铝基板薄片的“厚度”应理解为指定的平均厚度，除非在相关点定义了某些不同之处。
铝基底薄片在构造上是整体的(monolithic)。虽然基底薄片内的微观结构可能发生改变，“整体”在这方面是指由单个独立的无断裂、分层或夹杂物的单元组成。铝基底薄片优选地在结构上是均匀的(homogeneous)，其意味着薄片中不会有浓度梯度(concentration gradient)。特别地，铝基底薄片在构造上不是层状的(在本文中，不考虑由生产工艺产生但未在单独的工艺步骤中施加的“自然”Al2O3钝化层)且没有任何颗粒分布其中。特别地，它们不具有核-壳结构，其中，壳例如由适合于基底薄片的材料组成，且核由不同的材料(例如，氧化硅)组成。与此相反，在一部分基底薄片的更复杂的、非整体的结构意味着生产过程更复杂、耗时且昂贵。
除非另有说明，否则后续部分中的百分比数字应记为wt％。
当用△E45°≤1进行刀涂布(knife-coated)(遮盖地)时，本发明的金属效应颜料的饱和度(Suv)的值为0.2～0.3，色调角(huv)的值为50～65，随角异色/Alman指数的值大于26，且Gdiff(粒度)的值不大于6。本发明金属效应颜料的非常好的遮盖力从事实上证明了对于刀涂布的遮盖涂层，此处限定ΔE45°≤1，需要色素沉着不超过7％。特别地，对于7％的色素沉着，ΔE45°的值低于3.0。通过金属效应颜料与有机和/或无机颜料的混合，不能获得具有相应遮盖力和随角异色的这种色调。此外，就色调设置的再现(reproduction)而言，颜料混合不太精确。
与基于铝颜料的颜料混合物相反，本发明的金属效应颜料不易燃，因此例如出于运输的目的，不必归类为危险品。
相反，例如，即使在高水平的色素沉着下，市售的颜料Merck Iriodin 9602的非创新的实例也无法获得如上所述的ΔE45°遮盖力值。即使在非常高的20％的色素沉着下(这里，ΔE45°为5.1)，也无法获得ΔE45°<3的遮盖力。从算术上讲，直到色素沉着大于30％时，才能预期具有ΔE45°≤1的刀涂布遮盖涂层。
如果将色素沉着为20％的市售颜料Iriodin 9602与黄色颜料Helio Beit UN210(4.5％；黄色颜料的初始质量，除非另有说明，是基于所用颜料的干质量(dry mass))混合，为了模仿香槟色调，该混合物的ΔE45°遮盖力值位于本发明的金属效应颜料所达到的范围的上部，但是在此必须牢记色素沉着明显更高。尽管这种组合物不能获得本发明的金属效应颜料所达到的色调角(huv)或者规定的随角异色值(此处，相对于纯颜料，添加黄色糊状物增加了遮盖力，但损害了随角异色/Alman指数)，但是混合物的饱和度值在本发明的金属效应颜料所达到的0.2～0.3的范围内。
也可以将市售的来自舒伦克金属颜料公司的商品名为“Alustar 10200”的银元颜料(色素沉着为4％)与4.5％的(黄色颜料的初始质量，除非另有说明，是基于所使用的颜料的干质量)市售的来自赫利奥拜特颜料膏公司的黄色颜料(Helio Beit UN120)混合，以获得本发明颜料范围中的色调。实际上，对于两者而言，以这种方式获得的混合物的ΔE45°遮盖力在本发明的金属效应颜料所达到的范围内。混合物的随角异色和Gdiff同样在本发明的金属效应颜料的范围内。然而，饱和度(Suv)的值约为0.5，色调角(huv)的值约为70，无法获得本发明的金属效应颜料所达到的范围。
如果将上述混合物中黄色颜料的比例从4.5％增加到10％，那么确实有可能满足本发明金属效应颜料的色调角(huv)的范围，但这导致更高的饱和度，其明显超出本发明的金属效应颜料的范围。
通过珠光颜料和/或金属效应颜料彼此混合或通过添加炭黑或染料的这种组合方式，无法产生淡黄-米黄色香槟色调，其色调角(huv)为50～65，饱和度(Suv)为0.2～0.3且具有极高的遮盖力。在色调大致相等的情况下，随角异色也会有所不同。通常必须添加炭黑以提高遮盖力。
基于银元的银色颜料与有机染料(如，有机黄色颜料)的混合物的其它缺点如下：UV稳定性和温度稳定性较低，需要额外的混合程序，且在某些情况下，有必要添加稳定剂或乳化剂。用UV稳定性更高的无机(黄色)颜料对Al颜料进行着色不会达到具有相应氧化铁层的Al颜料的相应亮度(关于有机颜料的光化学分解的文献：丽莎·盖拉迪、伊拉里亚·德加诺、玛丽亚·佩拉·科隆比尼、乔伊·马祖雷克、迈克尔·席林、赫兰特·汉坚、汤姆·勒纳，“合成有机颜料的光化学降解的多重分析研究”，《染料和颜料》，第123卷，2015年，第396-403页)。
通过将金色铝颜料(示例性地选择颜料21YY(来自舒伦克金属颜料公司的ZenexoGoldenshine 21YY)，其具有以下颜料结构：基底＝Decomet(VMP铝薄片)，层厚为～25nm，其上有厚度为～60nm的SiO2层，且最后是厚度为～100nm的Fe2O3层，还有层厚为～10nm的SiO2涂层)与炭黑、TiO2或珠光颜料(在此示例中为来自默克(Merck)公司的Iriodin 119PolarWhite)混合，也无法获得饱和度(Suv)为0.2～0.3的所需色调。这些配方确实具有良好的遮盖力和良好的随角异色性，但是不能通过相应的混合达到上述饱和度(Suv)值。
通过改变涂料混合物的色素沉着并确定在预定湿膜厚度下用刀涂布遮盖涂层所需的色素沉着来确定遮盖力。此处的色素沉着(％)是指纯颜料的质量占涂料混合物的总质量的比例，该涂料混合物是溶剂型硝化纤维/聚环己酮/聚丙烯酸酯清漆(SC～10％)中的涂料混合物。为了进行此测定，使用来自Zehnter的薄膜解冻(film-thawing)设备，将至少四种不同的着色剂以38μm的湿膜厚度施加到TQC的黑白卡片上，且干燥后，使用来自Byk公司的Byk-mac I仪器记录△E45°。将获得的△E45°值进行曲线拟合并确定ΔE45°＝1时的色素沉着值。如果在38μm的预定湿膜厚度下，△E45°≤1，则该层定义为遮盖层(hiding layer)。达到该值所需的色素沉着越低，遮盖力越高。
一般而言，薄片的平均最大直径为约2～200μm，更特别地为约5～100μm。本发明的颜料的d50(Al基底+SiO2+Fe2O3层)通常为15～30μm。除非另有说明，否则本文的d50值是通过使用具有Quixel湿分散的Sympatec Helos仪器测定。
通常，涂覆的基底薄片的部分表面的涂层足以获得光泽颜料。例如，仅可涂覆薄片的上侧和/或下侧，而侧面被排除在外。然而，根据本发明，任选钝化的基底薄片的整个表面(包括侧面)被涂层A和B覆盖。因此，基底薄片被涂层A和B完全包裹。这改善了本发明的颜料的光学性能并提高了经涂覆的基底薄片的机械和化学稳定性。
本发明的用于生产金属光泽颜料的方法包括以下步骤：提供铝基底薄片(通常是钝化的铝基底薄片)；通过溶胶-凝胶法将SiO2层A湿化学地施加到预先提供的一种这样的铝基底薄片上；随后通过一种或多种铁(III)盐的湿化学沉淀施加Fe2O3层B；且随后进行煅烧。
为了产生涂层A，有机硅化合物在基底薄片的存在下被有效地水解，在所述有机硅化合物中，有机基团经由氧原子与金属键合。有机硅化合物的优选实例是正硅酸乙酯(原硅酸四乙酯，TEOS)。水解优选在碱(例如KOH，NaOH，Ca(OH)2或NH3)或酸(例如磷酸和有机酸(如乙酸))作为催化剂的存在下进行。尽管优选地水的量为2～100倍，更特别地为5～20倍，但是水必须至少以水解所需的化学计量的量存在。基于用水量，通常的做法是添加1～40vol％(优选地为1～10vol％)的浓度为25wt％的水性碱(例如KOH，NaOH，Ca(OH)2或NH3)。对于温度范围，已经证明有利的是在40～80℃(优选地为50～70℃)下加热反应混合物1～12小时(优选地为2～8小时)。
在工艺方面，用涂层A对基底薄片进行涂覆的方法如下：
引入铝基底薄片、有机溶剂、水和催化剂之后，将用于水解的含硅化合物以纯物质形式或以溶液形式(例如，以在有机溶剂中的30～70vol％，优选地为40～60vol％的浓度)添加至经预热的反应混合物中。可替代地，可在升高的温度下连续地计量含硅化合物，在这种情况下，可以先加入水和水性碱，也可以连续地计量加入。涂覆结束后，将反应混合物冷却回到室温。
为防止在涂覆过程中发生团聚，可对悬浮液施加强大的机械应力，例如泵送、剧烈搅拌或采用超声波。
涂覆步骤可以可选地重复一次或多次。如果母液(mother liquor)的外观呈乳白色浑浊(milkily cloudy)，建议在进一步涂覆之前，先将其更换。
覆盖有涂层A的铝基底薄片可通过简单的方式分离，如过滤、用有机溶剂洗涤，优选地醇类也通常用作溶剂，然后干燥(通常在20～200℃下进行2～24小时)。
可通过将铁(III)盐(如，氯化铁(III))和硫酸盐的水解分解来施加层B，随后通过煅烧将所得的含氢氧化物层转化成氧化物层。持续加热(优选地在250～550℃的温度下)5～360分钟，优选地，在300～450℃的温度下持续进行30～120分钟。
如果将氧化铁层用作混合层，该混合层包括一种或两种金属氧化物，基于所述层B，含量大于0～20wt％，且所述金属氧化物选自Al2O3或TiO2，则除了铁(III)盐之外，例如，AlCl3和/或TiOCl2可分别用作Al2O3和TiO2的前体化合物。
借助于本发明的生产方法，可以以简单的方式可重复地大量生产经涂覆的基底薄片。获得了完全包裹的颜料颗粒，并具有高质量的单个涂层(均匀、薄膜状)。
本发明的金属效应颜料可有利地用于化妆品中，只要它们在毒理学/微生物学上是可以接受的即可。在这里可以广谱(broad-spectrum)使用：主要是指甲油、唇彩、眼影、口红。其它可能的用途包括例如香波和粉末。
为了增强效果，本发明的颜料可以与有机或无机染料混合。
附图说明
图1图示了本发明的金属效应颜料的一般层结构(未按比例)；
图2图示了本发明的金属效应颜料的SEM截面，即创新颜料(该颜料的构造：基底＝Decomet(VMP铝薄片)，层厚为～25nm，其上有～60nm的SiO2层，且最后是～45nm的Fe2O3层，没有另外的涂层，例如另外的SiO2涂层，且没有表面改性)。
具体实施方式
下面的实施例用作对本发明的进一步说明，但不限于此。
实施例
创新颜料＝Decomet(VMP铝)作为基底，层A＝SiO2，其层厚在创新范围内，层B＝Fe2O3，其层厚在创新范围内。
创新实例
(1)创新颜料+约1.6％的Al2O3
(2)创新颜料
(3)具有约6％的TiO2的创新颜料
(4)具有约1.6％的Al2O3+SiO2的创新颜料(层C，算术厚度为16.5nm)
(5)具有约1.6％的Al2O3+SiO2的创新颜料(层C，算术厚度为26.5nm)
非创新实例
(6)含4.5％的黄色颜料Helio Beit UN 210的Merck Iriodin 9602
(7)Merck Iriodin 9602
(8)具有4％的黄色颜料Helio Beit UN 210的Alustar 10200
(9)具有10％的黄色颜料Helio Beit UN 210的Alustar 10200
(10)颜料21YY(Zenexo GoldenShine，舒伦克金属颜料公司)
(11)具有1％的Helio Beit Carbon Black(炭黑分散体)的颜料21YY
(12)具有10％的Iriodin 119的颜料21YY
(13)具有20％的Iriodin 119的颜料21YY
(14)具有50％的Iriodin 119的颜料21YY
(15)具有1.5％的TiO2的颜料21YY
创新实例的生产
首先，使用正硅酸乙脂(TEOS)通过溶胶-凝胶法用SiO2涂覆Al薄片(参见例如WO2015/014484A1)。
随后，向2L烧杯中加入铝含量为15g的悬浮液。该悬浮液用自来水补足至900克。在合成开始时，进行轻微的酸化。随后开始添加FeCl3溶液。通过加入碱性溶液(如，KOH、NaOH、Ca(OH)2或NH3)使pH保持恒定。在合成结束时，随着搅拌，pH升高。随后，在沉淀之后，通过过滤、干燥和随后的煅烧分离出产生的颜料。
下表列出了上述创新实例和非创新实例的层厚和色彩数据(coloristic data)：
Figure BDA0002935814120000081
·分别用Zeiss Auriga 40扫描电子显微镜记录SEM显微照片。
·色度数据通过测量颜料(除非另有说明，否则在溶剂型硝化纤维/聚环己酮/聚丙烯酸酯清漆中的色素沉着为7％，SC～10％)的刀涂布涂层获得，该涂层通过在来自Zehntner的自动成膜设备上使用38μm的线绕刮涂刀施加到TQC的DIN A5黑/白卡上。
·使用来自Byk公司的Byk-mac I测量色彩数据。

Claims (11)

1.一种基于经涂覆的铝基底薄片的金属效应颜料，其中，所述铝基底薄片的厚度为5～35nm、具有整体结构且被小于10nm的Al2O3自然钝化层包围，这些铝基底薄片被至少一层层厚为10～100nm的SiO2涂层A包裹，还有施加的Fe2O3涂层B，所述涂层B包裹具有SiO2涂层A的基底薄片且层厚为5～45nm，其特征在于，色素沉着不大于7％时△E45≤3，特别地，色素沉着小于7％时△E45°≤1，饱和度(Suv)的范围为0.2～0.3，色调角(huv)的值为50～65，随角异色/Alman指数的值大于26，Gdiff(粒度)值不大于6。
2.根据权利要求1所述的金属效应颜料，其特征在于，所述铝基底薄片的厚度为15～25nm。
3.根据权利要求1或2所述的金属效应颜料，其特征在于，SiO2涂层A的层厚为20～80nm。
4.根据权利要求1-3中任一项所述的金属效应颜料，其特征在于，Fe2O3涂层B的层厚为10～45nm。
5.根据权利要求1-4中任一项所述的金属效应颜料，其特征在于，氧化铁层是混合层，所述混合层包括一种或两种金属氧化物，基于所述层B，含量大于0～20wt％，且所述金属氧化物选自Al2O3或TiO2。
6.根据权利要求1-5中任一项所述的金属效应颜料，其特征在于，还包括依次包裹所述涂层B的外层C，更具体地是1～30nm厚的SiO2层，其还可选地渗透下方的Fe2O3。
7.根据权利要求1-6中任一项所述的金属效应颜料，其特征在于，对所述层B或如果存在的所述层C进行有机或有机-无机表面改性。
8.一种制备权利要求1-5中任一项所述的金属效应颜料的方法，其特征在于，包括通过溶胶-凝胶法将SiO2层A湿化学地施加到预先提供的铝基底薄片上，随后通过一种或多种铁(III)盐的湿化学沉淀施加Fe2O3层B，以及随后煅烧。
9.根据权利要求8所述的方法，其特征在于，还包括施加依次包裹所述涂层B的另外的外层C，更具体地是1～30nm厚的SiO2层，其还可选地渗透下方的Fe2O3。
10.根据权利要求8或9所述的方法，其特征在于，还包括对所述层B或如果存在的所述层C进行有机或有机-无机表面改性。
11.一种权利要求1-7中任一项所述的金属效应颜料在着色性涂料、印刷油墨、液体油墨、塑料、玻璃、陶瓷制品和装饰性化妆品制剂中的用途，特别是在指甲油、唇彩、眼影、口红、香波和/或粉末中的用途，其中，所述金属效应颜料可单独使用或与有机和/或无机颜料混合使用。
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