CN1073462A - 改进了光泽的颜料 - Google Patents

改进了光泽的颜料 Download PDF

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CN1073462A
CN1073462A CN92114085A CN92114085A CN1073462A CN 1073462 A CN1073462 A CN 1073462A CN 92114085 A CN92114085 A CN 92114085A CN 92114085 A CN92114085 A CN 92114085A CN 1073462 A CN1073462 A CN 1073462A
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C·普伦盖尔
K·伯恩哈德
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Merck Patent GmbH
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Abstract

本发明涉及作涂覆片状基质的方法得到的改进 了光泽度的颜料，该方法的特征是用水解法将由金属 盐以及金属氧化物和/或染料颗粒的水悬浮液以金 属氢氧化物层的形式沉淀在片状基质上，金属氢氧化 物层含金属氧化物和/或染料颗粒。

Description

本发明涉及用金属氧化物掺杂的并具有高遮盖力和改进光泽的片状颜料。
除高光泽度外还具有满意的光干涉作用和适当遮盖力的片状颜料常常是很难制备的。特别是有色的片状颜料，一般是用共沉淀法制备的，其光泽和/或遮盖力常常是不能满意的。与之类似，涂覆了一层或多层的金属氧化物的片状底质涂料具有干涉性的光泽，但由于材料有透明性，所以遮盖力不适合。虽然遮盖力可以用沉淀相对粗的金属氧化物层加以提高，但又大大地降低了其光泽度。用金属底质作为片状载体物质同样可以提高遮盖力，但产生的金属光泽对于多数的应用也是极不理想的。
因此极需具有高光泽和高遮盖力以及有美学感染力的片状涂剂，以扩大并补充现有的片状、特别是有色的颜料。
本发明的目的是提供性能好的、特别是能满足上述要求的并适于工业应用的新颜料。上述目的是按本发明的方法制备的片状颜料达到的。
现已惊人地发现，与常规共沉淀法制备的颜料相比较而具有高光泽和高遮盖力的片状颜料可用金属盐溶液在小颗粒金属氧化物和/或染料存在下经水解作用沉淀一层金属氧化物层制备的。
因此，本发明提供高光泽度和高遮盖力和片状颜料，它是由片状片载体材料组成的，载体材料上涂有含亚微米级的金属氧化物和/或染料颗粒的无机基质，涂层是高度均匀的。
本发明也提供制备具有改进的光泽度和遮盖力的片状颜料的方法，其中片状基质的水乳液用金属盐水解涂以金属氧化物或金属氧化物水合物层，然后分离，可用水洗涤，干燥和煅烧，其特征在于：
（a）水解是在金属氧化物和/或染料颗粒存在下进行的;
（b）颗粒的大小在亚微米级范围。
本发明也提供制备本发明颜料的修饰方法以及颜料的用途。
本发明的颜料由片状无机载体材料组成，例如玻璃、高岭土、白云母、钛铁矿或特别是云母。这种片状材料用沉淀法涂上一层金属氢氧化物层，其中包封着金属氧化物和/或有机染料颗粒，但是金属氧化物和/或有机染料颗粒是在氢氧化物层沉淀的过程中被带入的，而不是常规意义上的共沉淀。
片状基质的厚度最好在0.1-5μm之间，特别是0.2-4.5μm之间，其它二尺寸通常是1-250μm之间，特别是2-200μm之间。
适合的母体氧化物有：例如二氧化硅、硅酸盐、三氧化硼、硼酸盐、氧化铝、铝酸盐等，特别优先选择的是二氧化钛;母体氧化物还有已知的制备片状微粒和有色光泽颜料的其他物质。
它们一般是在适合的pH值下用水解法生产的，起始原料是适合的可溶性金属盐，优选的是卤化物、硫酸盐或硝酸盐，特别优选的是氯化物。
包封在母体内的金属氧化物和/或有机染料颗粒的大小为10-40nm，因此它们明显地小于用共沉淀法生产的片状颜料或金属氧化物，并在母体氧化物的沉淀过程中被带入而包藏于母体堆集体的空隙之中，因此产生了高的堆积密度，以及由此产生了高遮盖力和高光泽度。
金属氧化物和/或有机染料颗粒的包封一般是无规排列的，最好是无定形或球形。
适合的金属氧化物颗粒是已知的在本发明颜料的制备过程中不与母体的前体物质反应的所有稳定无机氧化物。金属氧化物颗粒可以是有色的或无色的，但最好以纯态的加入。但使用不同金属氧化物和/或有机染料的混合物也是可以想到的。一些特别适合的金属氧化物是二氧化钛（TiO2）、氧化铝（Al2O3）、二氧化硅（SiO2）、二氧化锡（SnO2）、氧化镁（MgO）、氧化锌（ZnO）、氧化铁（例如Fe2O3或Fe3O4）、氧化铬（Cr2O3）、二氧化锑（CeO2）、氧化钨（WO3）、氧化钼（MoO3）、二氧化锆（ZrO2）以及混合氧化物如Cr2FeO4、CoAl2O4或NiAl2O4。
除了无机颜料颗粒外，也可以使用有机颜料颗粒，此时最好使用热稳定性的有机颜料。在许多情况下，制备本发明颜料的条件是可以改变的。例如降低干燥温度和任选降低煅烧温度，同时延长干燥时间或煅烧时间，或者用其它方法，这样就可以使用较不稳定的有机颜料颗粒。再者，被母体包封的有机颜料颗粒的稳定性常见有所提高。
所用的有机颜料颗粒，最好是例如酞菁、碱性染料与杂多酸的色淀产物、蒽醌、吩嗪、吩噁嗪、二酮吡咯并吡咯或苝。
上列的颜料颗粒是已知的，它们的制备方法请见例如“H.Kittel，Wissenschaftliche    Verlagsgesellshaft，Stuttgart，1960，G.benzig，Pigmente    für    Anstrichmittel，Expert    Verlag    1988”，一般它们都有商品供应。但是，这些有机颜料颗粒之列举只是为了说明本发明，而无论如何不是对其加以限制。除了上面清楚说明之外，还有许多其他的颜料颗粒是可以使用的。
在许多情况下，为了颜料颗粒能够很好地分散，是将前体溶液与湿润剂在一起混合的，例如非离子型或离子型的市售各级湿润剂，如聚乙二醇和聚丙二醇是非常适合的。湿润剂的类型和量不是关键性的，但一般说明来其比例不大于分散体系的2%（重量）。
本发明颜料的优点之一是片状载体材料（最好是云母）是用钛盐溶液水解（最好是四氯化钛溶液）涂覆，它也含有金红石变体的TiO2。这些金红石颗粒是在沉淀过程中被夹带入并被包封在母体的空隙中，它们也起金红石化核的作用，使二氧化钛部分金红石化。金红石变体在母体中的质量比例一般为0.5-40%（重量）。金红石颗粒的平均直径为10-40nm之间。得到的是高光泽度和高遮盖力的片状颜料，其中的金红石变体比例在很大程度上决定于煅烧温度。煅烧最好在700-1000℃之间的温度下进行，特别是800-900℃之间。不采用金红石化异质层，例如SnO2层。
小颗粒金属氧化物（平均粒度10-40nm）包封在金属氧化物涂层的空隙内，与共沉淀法得到的颜料比较，明显地增加了遮盖力和光泽度，涂层还具有高的均匀性。
遮盖力和（在有色颜料颗粒的情况下）观察角-本发明颜料的独立吸收色可因变更包封颜料颗粒的浓度而在较大范围内变化。包封颜料颗粒相对于母体的质量比例一般是在0.5-30%之间。特别是2-20%之间。
优选的本发明的颜料含一种或多种包封的有机和/或特别是无机有色颜料;特别优选氧化铁、氧化铬、氧化钴和有色的尖晶石，例如氧化铝钴（CoAl2O4）。
本发明的颜料因而成为具有很好的光学性质结合的光学体系，而且它的相对突出之处可在特殊的应用方面在较宽范围内变化和最佳化。此最佳化可由本领域技术熟练者按常规方法进行，不需要有任何发明高度。
本发明的颜料因此对于工业应用的颜料范围是一个明显的补充，并且它们有明显的经济重要性。
本发明的颜料是用湿化学制备的，例如US    30    87    828，DE20    09    556，DE    22    14    545，DE    25    22    572，DE    25    22    573，DE    31    37    809，DE    31    51    354，DE    31    51    355，DE    32    11    602，或DE    33    35    017中所述，也可在用共沉淀的颜料制造过程中采用。
优选的方法是制备片状基质的水悬浮液，再于5-95℃的温度下进行热处理。然后在悬浮液中在粒径为超微米区域的金属氧化物和/或有机染料存在下加入金属盐溶液。金属氧化物和/有机染料颗粒是极细地分散于基质悬浮液中或金属盐溶液中，或作为水分散液在金属盐加入基质悬浮液时分别同时加入。基质悬浮液的pH用同时加入适合于特殊金属盐水解和实现金属氢氧化物相应沉淀范围的碱来保持。在沉淀过程中，所加入的金属氧化物和/或有机染料颗被带入并包封于沉淀出的含水氧化物层的空隙中。分离出涂覆的基质，水洗，干燥，然后在400-1200℃的温度间煅烧，优选600-1000℃。
然而，也可以通过加热和/或加碱的方法来制备含欲涂覆的基质、欲被包封的亚微米颗粒和金属盐的悬浮液，并实现金属盐的水解。
下面的实施例对本发明进行具体说明，但并非对本发明加以限制。本文前后所用的温度均以摄氏度℃表示。
实例1
将100克云母悬浮于2000毫升之水中，加热至75℃，在此反应悬浮液中加入用盐酸酸化的1.6克SnCl4·5H2O于50毫升水中的溶液。接着同时加入355毫升TiCl4水溶液（每升含280克TiCl4）和355毫升由6克Aercsil 200
Figure 921140851_IMG1
（Degussa。极细的火成岩二氧化硅，粒度10-20nm）与0.2克Texopon K12 （Henkel，以月桂基硫酸盐为基础的湿润剂）组成的分散剂，在加入过程中将其pH保持恒定在1.8。加入完毕后，将上述试剂与TiCl4溶液混合，直至达到所要求的涂覆终点（此例为银色终点），然后将混合物搅拌15分钟以完成反应。过滤出颜料。洗至不含氯化物，于120℃干燥16小时。干燥后的颜料于850℃煅烧30分钟。
颜料组成：云母51%，SnO221%;Aerosil 200
Figure 921140851_IMG3
6%;TiO2约42%
实例2
重复实例1的方法，但以12%的Aerosil 200
Figure 921140851_IMG4
沉淀入TiO2层中，而不是用6%.所及颜料的组成为：云母44%;SnO2l%;Aerosil 200 12%;TiO2约43%
实例3
将100克云母悬浮于2000毫升之水中，加热至75℃，此反应混合物然后缓慢与5克微二氧化钛MT 100-S
Figure 921140851_IMG6
（Micro Titanium Oxide100-S
Figure 921140851_IMG7
）（Teikoku Kaku，粒度10-30nm）于300毫升四氯化钛水溶液（每升280克TiCl4）的悬浮液相混合。在加入过程中，将pH保持恒定在1.8。加入完毕后，将反应混合物搅拌15分钟以完成反应。然后滤出颜料，洗至无氯化物，120℃干燥16小时。干燥完毕后，将颜料于800℃下煅烧30分钟。TiO2层由20%金红石和80%锐锥石（锐锥石型TiO2-译注）组成。
实例4
重复实例3的方法，但将最后的煅烧温度升至850℃。得到的片状颜料的TiO2涂层由40%金红石和60%锐锥石组成。
实例5
重复实例3，用沉淀法以TiO2层涂覆母云片。将干燥后的产品在900℃进行煅烧。得到的片状TiO2涂覆的颜料的TiO2层组成为30%的金红石和70%的锐锥石。

Claims (9)

1、以无机母体涂覆的片状载体材料组成的高光泽和高遮盖力的颜料，其特征在于母体含亚微米级的金属氧化物和/或有机染料颗粒。
2、权利要求1的颜料，其特征在于颜料的基质是云母。
3、权利要求1的颜料，其特征在于包封的金属氧化物和/或染料颗粒的平均粒度为10-40nm。
4、权利要求1的颜料，其特征在于加入的金属氧化物颗粒为金红石变体的TiO2。
5、制备改进了光泽和遮盖力的片状颜料的方法，其中片状颜料水悬浮液基质用金属盐水解涂覆一层金属氧化物或金属氧化物水合物层，然后分离出颜料，洗涤（任选），干燥，煅烧，其特征在于水解是在粒度为亚微米级范围内的金属氧化物和/或染料存在下进行的。
6、权利要求5的方法，其特征在于所用的片状基质是云母。
7、权利要求5的方法，其特征在于金属氧化物和/或染料颗粒的平均粒度为10-40nm。
8、权利要求5的方法，其特征在于加入的TiO2颗粒是金红石变体。
9、应用权利要求1至6的颜料于油漆、染料、塑料和化妆品之类的配方。
CN92114085A 1991-12-06 1992-12-04 改进了光泽的颜料 Pending CN1073462A (zh)

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US11802210B2 (en) 2016-12-21 2023-10-31 Viavi Solutions Inc. Hybrid colored metallic pigment
US11891524B2 (en) 2016-12-21 2024-02-06 Viavi Solutions Inc. Pigments having a vapor deposited colorant

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CN107001812A (zh) * 2014-12-12 2017-08-01 默克专利股份有限公司 具有金属性质的非金属颜料
CN107001812B (zh) * 2014-12-12 2019-11-12 默克专利股份有限公司 具有金属性质的非金属颜料
US11802210B2 (en) 2016-12-21 2023-10-31 Viavi Solutions Inc. Hybrid colored metallic pigment
US11891524B2 (en) 2016-12-21 2024-02-06 Viavi Solutions Inc. Pigments having a vapor deposited colorant

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