CN102712816B - 效果颜料 - Google Patents

效果颜料 Download PDF

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CN102712816B
CN102712816B CN201080061228.1A CN201080061228A CN102712816B CN 102712816 B CN102712816 B CN 102712816B CN 201080061228 A CN201080061228 A CN 201080061228A CN 102712816 B CN102712816 B CN 102712816B
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base material
coating
effect pigment
material according
pigment
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CN102712816A (zh
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H·B·克尼斯
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Merck Patent GmbH
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Merck Patent GmbH
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Abstract

本发明涉及具有基材的效果颜料，其具有包含铜、铁和锰的复合金属氧化物的涂层，以及用于制备所述效果颜料的方法，以及所述效果颜料在漆料、涂料、粉末涂料、印刷油墨、塑料、陶瓷材料、玻璃中的用途，在化妆品制剂中的用途，用于激光标记以及用于制备颜料制剂和干制剂的用途。

Description

效果颜料
技术领域
本发明涉及具有基材的效果颜料，其具有包含含铜、铁和锰的复合金属氧化物的涂层，并且涉及一种用于制备效果颜料的方法，所述效果颜料在漆料、涂料、粉末涂料、印刷油墨、塑料、陶瓷材料、玻璃中的用途，在化妆品制剂中的用途，用于激光标记以及用于制备颜料制剂和干制剂的用途。
背景技术
光泽颜料或效果颜料，例如从DE 2522572中已知的那些，用于很多技术领域，特别是汽车涂漆领域、装饰涂料、塑料、漆料、印刷油墨和化妆品制剂中。
具有深灰色的效果颜料，例如从WO 9319131、DE 19522267、EP0735115和EP 0601761中已知。然而，这些颜料的缺点在于由于含有还原的二氧化钛(低价氧化物)而总是带有一些蓝灰色。
另外，已知灰色的效果颜料，其的着色通过施加CuxMn3-xO4(x=1.4或1.5)到以二氧化钛涂覆的薄片状基材的表面上而进行(EP0719843)。这些颜料同样也不是中性黑或灰色的，而是常常带点蓝色至绿色的着色。
US2,811,463描述了由氧化锰、氧化铜和氧化铁构成的作为煅烧产品的黑色无基材颜料的制备。然而，这种颜料根本不具有光泽。
黑色效果颜料在很多情况下基于碳。这种类型的颜料从DE4227082A1、DE 3636076A1、DE 3617430A1和EP 0246523中已知。黑色的光泽颜料或者通过使用炭黑、通过有机化合物的分解过程制备或者通过烃的取决于温度的煅烧来制备。EP 1520883公开了具有可调色彩内容（Farbanteil），即具有金、绿、红或蓝色调的黑色光泽的干涉颜料。
从现有技术中已知的黑色颜料具有如下缺点：其具有阴暗的光泽以及灰黑色或棕黑色或显出非常强烈地取决于视角的干涉色，这在大多数应用中是不理想的。另外，这些颜料在某些情况下非常难以制备或可再现。
发明内容
因此本发明的目的是制备一种具有中性灰或中性灰至中性黑主色调的光泽效果颜料。
令人惊奇的是，目前已经发现新的中性色的光泽效果颜料，其同时以高遮盖力和良好的加工性为特征，其不具有显著的或不具有视角色度并且其易于制备。因此本发明涉及一种具有基材的效果颜料，其具有包含含铜、铁和锰的复合金属氧化物的涂层。
对本发明而言必要的涂层优选包含复合金属氧化物，所述复合金属氧化物由氧化铜、氧化铁和氧化锰的单相混晶构成。优选复合金属氧化物显出尖晶石结构。在所述尖晶石结构中，至少两种不同类型的阳离子(二价和三价或四价阳离子)占据不同类型的晶格位置，即相对于每个基本单元（Elementarzelle）八个四面体配位的点位和16个八面体配位的点位。在正常尖晶石情况下，所有16个三价阳离子或四价阳离子位于八面体晶格位置上，在反尖晶石的情况下，每八个三价阳离子或四价阳离子和八个二价阳离子以八面体配位。由于一定的自由度，尖晶石中的阳离子分布常常具有有序/无序状态。
在复合金属氧化物中铁和锰可以作为二价和三价形式存在。复合金属氧化物可另外包含其它的三价和/或二价阳离子，优选铝、钴和/或钛阳离子。在此优选氧化铝、氧化钴和/或氧化钛的量为基于复合金属氧化物计0-10重量%。
复合金属氧化物优选符合式CuxFeyMn3-x-yO4，其中x=1-1.4且y=0.1-1。特别优选所述复合金属氧化物为按照化学计量比的尖晶石。特别优选的是Cu(Fe,Mn)2O4形式的铜尖晶石。
复合金属氧化物的量基于基材计为2.5-60重量%，优选20-60重量%，特别是20-50重量%。在一个优选的方案中，除复合金属氧化物之外，本发明必要的涂层可部分包含二氧化钛。本发明必要的包含复合金属氧化物的涂层的厚度优选为1-350nm，特别是10nm-300nm，且非常特别优选20-200nm。
用于本发明效果颜料的合适的基材，例如为所有已知的薄片状载体材料，优选透明或半透明的薄片。优选的是经用一种或多种高折射率或低折射率、透明或半透明的金属氧化物层涂覆的那些薄片状载体材料。特别优选二氧化钛涂覆的云母。
合适的载体材料例如为层状硅酸盐，特别是合成或天然的云母、玻璃薄片、金属薄片、SiOx薄片(x=≤2.0，优选x=2)、Al2O3薄片、TiO2薄片、合成或天然的氧化铁薄片、石墨薄片、结构化颜料、合成的无载体薄片、液晶聚合物(LCP)、全息颜料、BiOCl薄片或所述薄片的混合物。优选薄片选自合成或天然的云母、玻璃薄片、SiO2薄片和Al2O3薄片，特别是云母薄片。
一般而言，薄片状载体材料的厚度为0.05-5μm，特别是0.1-4.5μm。优选玻璃薄片的厚度≤1μm，特别是≤900nm，非常特别优选≤500nm。载体材料的大小本身并不重要并可与各个应用目的相协调。粒度通常为1-350μm、优选2-200μm、特别是5-150μm。一般而言，具有粒度为10-200μm、优选40-200μm、特别是10-130μm的粗大薄片，以及具有粒度为1-60μm、优选5-60μm、特别是10-40μm的细小薄片均可使用。还可优选使用由具有不同粒度的薄片组成的混合物。
所述粒度使用本领域技术人员已知和市购可得的仪器(例如得自Malvern公司，Horiba公司的)借助于在粉末或颜料悬浮体上的激光衍射来确定。优选所述基材的形状因子(纵横比：直径/厚度比)为5-750、特别是10-300、非常特别优选20-200。另外，还可使用其它基材，例如，可用上述层覆盖的球形颗粒或针形基材。
在优选的实施方式中，载体材料可以用一种或多种包含金属氧化物、金属氧化物水合物、金属低价氧化物、金属、金属氟化物、金属氮化物、金属氮氧化物及或这些材料的混合物的透明、半透明和/或不透明的层涂覆。所述金属氧化物、金属氧化物水合物、金属低价氧化物、金属、金属氟化物、金属氮化物、金属氮氧化物的层及其混合物可具有低折射率(折射率<1.8)或高折射率(折射率≥1.8，优选≥2.0)。合适的金属氧化物和金属氧化物水合物为本领域技术人员已知的全部金属氧化物或金属氧化物水合物，例如，氧化铝、氧化铝水合物、氧化硅、氧化硅水合物、氧化铁、氧化锡、氧化铈、氧化锌、氧化锆、氧化铬、氧化钛，特别是二氧化钛、以金红石或锐钛矿变型的、氧化钛水合物及其混合物，例如，钛铁矿或铁板钛矿。作为金属低价氧化物使用例如钛低价氧化物。合适作为金属的例如为铬、铝、镍、银、金、钛、铜或合金，合适作为金属氟化物的例如为氟化镁。作为金属氮化物或金属氮氧化物可以使用例如金属钛、锆和/或钽的氮化物或氮氧化物。优选将金属氧化物、金属、金属氟化物和/或金属氧化物水合物的层以及非常特别优选金属氧化物和/或金属氧化物水合物的层施加到载体上。特别优选的是铝、硅、铁、锡和钛的氧化物和/或水合氧化物，特别是二氧化钛、以金红石或锐钛矿变型的、及这些化合物的混合物。另外还可存在由高折射率和低折射率的金属氧化物、金属氧化物水合物、金属或金属氟化物的层构成的多层结构，其中高折射率层和低折射率层优选是交替的。特别优选由高折射率层和低折射率层构成的层组件（Schichtpakete），其中可将该层组件的一个或多个施加到载体上。为将载体纳入多层结构中，在此所述高折射率层和低折射率层的顺序可与载体相匹配。
合适的基材特别为经用一种或多种高折射率或低折射率、透明或半透明的金属氧化物层涂覆的那些薄片状载体材料。优选的是用一种或多种金属氧化物层涂覆的载体。特别优选的是二氧化钛涂覆的云母或用TiO2/SnO2单次涂覆或多次涂覆的云母。
优选通过湿化学法施加由金属氧化物、金属氢氧化物和/或金属氧化物水合物组成的层。这种类型的方法为本领域技术人员已知，并且例如在DE 2522572中已知。上述材料和颜料结构的实例和实施方式还例如在Research Disclosures RD 471001和RD 472005中找到。在湿法涂覆的情况下，将基材悬浮于水中，并在适用于水解的pH值下加入一种或多种可水解的金属盐，如此选择pH使得金属氧化物或金属氧化物水合物直接沉淀到薄片上而不发生二次沉淀。所述pH通常通过同时计量加入碱或酸而保持恒定。如果需要，则可在施加单个涂层后将颜料分离、干燥并任选灼烧，以随后又将其再悬浮以沉淀其他的层。另外，也可通过气相涂覆在流化床反应器中进行所述涂覆。
载体材料上的涂层优选由简单或复合的金属氧化物、金属、氮化物或氮氧化物，例如TiO2、ZrO2、ZnO、SnO2、SiO2、SiO(OH)2、Al2O3、AlO(OH)、B2O3或其混合物或还有BiOCl或还有MgF2构成。特别优选的是TiO2。
金属氧化物、金属氧化物水合物、金属低价氧化物、金属、金属氟化物、金属氮化物、金属氮氧化物的层或其混合物的厚度通常为1-1000nm，优选1-800nm，特别是1-600nm。特别合适的层厚度为1-300nm，特别是1-100nm。优选金属层的厚度为4-60nm。
本发明必要的包含复合金属氧化物的涂层可作为外部氧化物涂层存在或用一种或多种高折射率或低折射率的、透明或半透明的金属氧化物层，优选用TiO2层来涂覆。优选包含复合金属氧化物的涂层在外面。
本发明必要的包含复合金属氧化物的涂层由此制备：通过在基材的含水悬浮液中加入水溶性铜、铁和锰盐使得在基材上产生含水氧化物（任选部分地与二氧化钛层混合）而在基材上形成复合金属氧化物，其中所述水溶性的铜、铁和锰盐可同时或连续地计量加入。
优选首先加入锰盐溶液，任选地同时加入钛盐溶液，然后计量加入铜盐溶液以及随后计量加入铁盐溶液。合适的金属盐特别是卤化物、硝酸盐和硫酸盐，特别是氯化物和硫酸盐。通过合适的pH和温度条件实现金属氧化物的沉淀。对期望的颜料组合物而言所需的待使用量和浓度可由本领域技术人员根据常规确定。
本发明的效果颜料在包含复合金属氧化物的涂层上，还可具有一个或多个由高折射率和/或低折射率、透明或半透明的金属氧化物，特别是由TiO2、ZrO2、ZnO、SnO2、SiO2、SiO(OH)2、Al2O3、AlO(OH)、B2O3或其混合物构成的层。
将通过所述方法制备的颜料分离，洗涤，优选在80-150℃下干燥并在400-850℃、优选500-700℃下在空气中煅烧30-60分钟，由此形成复合金属氧化物。
制备具有包含复合金属氧化物的本发明涂层的效果颜料的其它方法包括煅烧如下物质的混合物：a)TiO2/CuO-涂覆的云母，b)TiO2/FeO-涂覆的云母和c)TiO2/MnO-涂覆的云母。所述涂覆的云母通过上述方法单独涂覆、洗涤和干燥。然后制备混合物并将以这种方式涂覆的云母在400-850℃、优选500-700℃下在空气中共同煅烧30-60分钟，由此形成复合金属氧化物。
为提高光、水和气候稳定性，通常建议取决于使用领域使制成的颜料经历后涂覆或后处理。作为后涂覆或后处理考虑本领域技术人员已知的所有后涂覆。这种后涂覆进一步提高了化学稳定性或简化了颜料的操作，特别是掺入各种介质中。为改善润湿性、分散性和/或与使用介质的相容性，可施加其它常规的功能性涂层，例如用硅烷。
特别优选一种效果颜料，其以所述顺序由以下构成：云母基材、任选地二氧化锡涂层、二氧化钛涂层、由具有式Cu(Fe,Mn)2O4的尖晶石结构的复合金属氧化物构成的涂层（其中二氧化钛涂层和包含复合金属氧化物的涂层可部分地或完全、优选部分地混合）以及任选的后涂层。
对于各种应用目的，本发明的效果颜料还可有利地用作与填料、有机染料和/或颜料例如透明和不透明的白色、彩色和黑色颜料的混合物，以及与薄片状氧化铁、有机颜料、全息颜料、LCP(液晶聚合物)、干涉颜料和常规的基于金属氧化物涂覆的基于云母、玻璃、Al2O3、Fe2O3、SiO2等的薄片的透明、彩色和黑色光泽颜料的混合物。本发明的效果颜料可以任意比与市购颜料和填料混合。
作为填料可提及的例如为天然和合成的云母，尼龙粉末，纯的或填充的密胺(Melanin-)树脂，滑石，玻璃，高岭土，铝、锰、钙、锌的氧化物或氢氧化物，BiOCl，硫酸钡，硫酸钙，碳酸钙，碳酸镁，碳，以及这些物质的物理或化学的组合物。对于填料的颗粒形状没有限制。根据需要，其可以例如为薄片状、球形或针形。
本发明的效果颜料可用于涂料(汽车和工业涂料、溶剂基和水基的、粉末涂料)、塑料、印刷油墨、陶瓷釉或化妆品制剂。它们还可以制剂形式(丸剂、糊剂、膏剂(Anteigung))使用，例如用于印刷油墨或塑料中。
本发明的效果颜料另外适用于制备包含一种或多种本发明效果颜料、粘结剂和任选一种或多种添加剂的可流动颜料制剂和干制剂。干制剂也理解为包含0-8重量%、优选2-8重量%、特别是3-6重量%水和/或溶剂或溶剂混合物的制剂。优选所述干制剂作为丸粒、颗粒、碎屑、小肠状或饼团状存在，并且粒度为0.2-80mm。所述干制剂特别用于制备印刷油墨和用在化妆品制剂中。
本发明的效果原料与多种颜色***，优选来自涂料、漆料和印刷油墨领域的颜色***相容。为了制备印刷油墨，多种粘结剂、特别是水溶型粘结剂是合适的，例如由BASF、Marabu、Sericol、Hartmann、Gebr.Schmidt、Sicpa、Aarberg、Siegberg、GSB-Wahl、Follmann、Ruco或Coates Screen INKS GmbH公司所市售的。印刷油墨可构造为基于水或基于溶剂的。所述颜料另外还适用于纸和塑料的激光标记，以及用于农业领域，例如用于温室薄膜，和例如用于帐篷帆布的着色。
本发明另外还涉及效果颜料在制剂例如漆料、印刷油墨、防伪印刷油墨、涂料、粉末涂料、塑料、陶瓷材料、玻璃中的用途，在化妆品配制剂中的用途，作为纸和塑料的激光标记用的掺杂剂的用途，以及制备颜料制剂和干制剂的用途。
在此引用文献的公开内容也清楚地属于本申请的公开内容。以下实施例更详细地解释了本发明而不限制本发明的范围。
具体实施方式
实施例
实施例1
制备具有深灰色主色调并具有组成云母、二氧化锡、二氧化钛、Cu(Fe,Mn)2O4的半透明光泽效果颜料：
在1.5L软化水中将100g粒度为10-60μm的云母在搅拌下加热至75℃。然后使用5%盐酸将悬浮液的pH调节至1.8。随后计量加入四氯化锡溶液(由4.5g 50%的SnCl4溶液和12g在50g完全去离子水中的浓盐酸组成)，其中通过同时滴加20%氢氧化钠溶液使pH保持恒定。添加完成之后，继续搅拌15min。随后计量加入四氯化钛/二氯化锰溶液(34.8g MnCl2*2H2O，溶于含量为340g TiCl4/I的250ml TiCl4溶液中)，其中通过同时滴加32%的氢氧化钠溶液使pH保持恒定。添加完成后，继续搅拌15min。然后计量加入氯化铜溶液(29g CuCl2*2H2O，溶于150ml完全去离子水中)和随后硫酸铁溶液(36.8g FeSO4*7H2O，溶于100ml完全去离子水中)。添加完成时，继续搅拌15min。随后通过加入20%氢氧化钠溶液将pH缓慢调节至9.8，并且继续搅拌30min。将产物滤出、洗涤、干燥、在600-700℃下灼烧并通过100μm筛网过筛。得到具有银色光泽和中性色的深灰色主色调以及高遮盖力的颜料。
随后，在掺入硝基纤维涂料中后由所述效果颜料制成涂料卡，并且测量其色彩。
色度黑卡：7.42
色度白卡：1.58
比较例
制备具有深灰色主色调并具有组成云母、二氧化锡、二氧化钛、根据EP 0719843的CuxMn3-xO4（其中x=1.4）的半透明光泽效果颜料：
在1.5L软化水中将100g粒度为10-60μm的云母在搅拌下加热至75℃。然后使用5%盐酸将悬浮液的pH调节至1.8。随后计量加入四氯化锡溶液(由4.5g 50%的SnCl4溶液和12g在50g完全去离子水中的浓盐酸组成)，其中通过同时滴加20%氢氧化钠溶液使pH保持恒定。添加完成之后，继续搅拌15min。随后计量加入四氯化钛/二氯化锰溶液(34.8g MnCl2*2H2O，溶于含量为340g TiCl4/I的250ml TiCl4溶液中)，其中通过同时滴加32%氢氧化钠溶液使pH保持恒定。添加完成之后，继续搅拌15min。然后计量加入氯化铜溶液(30.0g CuCl2*2H2O，溶于150ml完全去离子水中)。添加完成之后，继续搅拌15min。随后通过加入20%氢氧化钠溶液将pH值缓慢调节至9.8，并且再搅拌30min。将产物滤出、洗涤、干燥、在600-700℃下灼烧并通过100μm筛网过筛。
得到具有银色光泽和蓝灰色主色调以及高遮盖力的颜料。
随后，在掺入硝基纤维漆中后由所述效果颜料制备涂料卡，并且将测量其颜色。
色度黑卡：13.30
色度白卡：1.81

Claims (17)

1.具有基材的效果颜料，其具有包含由铜、铁和锰构成的复合金属氧化物的涂层，
并且所述复合金属氧化物具有尖晶石结构。
2.根据权利要求1所述的具有基材的效果颜料，其特征在于所述复合金属氧化物的量基于所述基材为2.5-60重量％。
3.根据权利要求2所述的具有基材的效果颜料，其特征在于所述复合金属氧化物的量基于所述基材为20-50重量％。
4.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述复合金属氧化物符合式CuxFeyMn3-x-yO4，其中x＝1-1.4且y＝0.1-1。
5.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述复合金属氧化物是式Cu(Fe,Mn)2O4的铜尖晶石。
6.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述涂层部分包含二氧化钛。
7.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述涂层的厚度为1-350nm。
8.根据权利要求7所述的具有基材的效果颜料，其特征在于所述涂层的厚度为100-250nm。
9.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述基材为薄片状。
10.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述基材是天然或合成的云母、BiOCl薄片、玻璃薄片、Fe2O3薄片、石墨薄片、Al2O3薄片、SiO2薄片或TiO2薄片或这些薄片的混合物。
11.根据权利要求10所述的具有基材的效果颜料，其特征在于，所述基材是天然或合成的云母。
12.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于所述基材在包含复合金属氧化物的涂层之下或之上具有一个或多个由高折射率和/或低折射率的透明或半透明金属化合物构成的层。
13.根据权利要求12所述的具有基材的效果颜料，其特征在于所述金属化合物选自TiO2、ZrO2、ZnO、SnO2、SiO2、SiO(OH)2、Al2O3、AlO(OH)、B2O3及其混合物。
14.根据权利要求1-3中任一项所述的具有基材的效果颜料，其特征在于其具有无机或有机的后涂层。
15.制备根据权利要求1-14中任一项所述的具有基材的效果颜料的方法，其特征在于所述薄片状基材的涂覆通过湿化学法、通过CVD法或PVD法进行。
16.根据权利要求1-14中任一项所述的具有基材的效果颜料的用途，用在漆料、涂料、印刷油墨、塑料、陶瓷材料、玻璃中，在化妆品配制剂中，用于激光标记以及用于制备颜料制剂和干制剂。
17.根据权利要求1-14中任一项所述的具有基材的效果颜料的用途，用在粉末涂料中。
CN201080061228.1A 2010-01-15 2010-12-17 效果颜料 Expired - Fee Related CN102712816B (zh)

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