CN1145382A - 金粉颜料 - Google Patents

金粉颜料 Download PDF

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CN1145382A
CN1145382A CN96108367A CN96108367A CN1145382A CN 1145382 A CN1145382 A CN 1145382A CN 96108367 A CN96108367 A CN 96108367A CN 96108367 A CN96108367 A CN 96108367A CN 1145382 A CN1145382 A CN 1145382A
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pigment
matrix
layer
solution
gold
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R·沃特
K·比恩哈德
G·帕夫
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Merck Patent GmbH
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Abstract

本发明涉及高度不透明的金粉颜料及其制备方法和应用。

Description

金粉颜料
本发明涉及高度不透明的金粉颜料及其制备方法和应用。
以云母片晶为基础的珠光颜料，由于添加铁氧化物而使其金色调增强，这在文献中已多次作过介绍并连续使用了多年。本文介绍的颜料包括将氧化铁与另一种金属氧化物、特别是二氧化钛一起沉淀在云母片晶上以及连续进行沉淀的两种。
例如，DE-C 14 67 488，CS 21 12 30和CS 22 36 08所介绍的珠光颜料是将另外的氧化铁层施加到涂覆了二氧化钛的云母片晶上。
美国专利3,087,826公开了将Fe2O3层沉积在TiO2层上而产生金色的颜料，该颜料在煅烧时呈现出淡红色调。DE-C 19 59998申请保护的颜料具有在云母上首先覆盖氧化钛和氧化铁涂层，然后覆盖二氧化钛和/或二氧化锆涂层。
DE-C 22 44 298介绍了一种制备金色珠光颜料的方法，在该方法中，首先将已用TiO2和ZrO2涂覆的云母颜料涂覆氢氧化铁(II)，然后将其氧化成Fe2O3。
DE-C 27 23 871公开了几种云母颜料，该颜料在很薄的TiO2层或Al2O3层上载有厚的Fe2O3层。
在EP 0 211 351 B1中介绍了用钛和铁的金属氧化物层覆盖片晶样的基质。
已知由现有技术生产的金粉颜料具有的缺点是，当将其涂覆在无光泽的角钢上时，却显示出棕色色调。
因此，需要制备高光泽、不透明、无需很复杂的技术而又没有上述缺点的金粉颜料。
众所周知，将碳掺入颜料中可以得到特殊的颜色效果。例如DE 41 41 069介绍了以片晶状硅酸盐基质为基础的闪光颜料，该基质的第一层用包含高折射的金属氧化物涂覆，第二层基本上是由碳或金属组成的黑色层，第三层是高折射的金属氧化物层。
现已出乎意料地发现，如果先用掺杂碳的二氧化钛层覆盖基质，然后再覆以氧化铁层可得到具有特殊色彩效果的金粉颜料。
因此，本发明提供了以金属氧化物涂覆的基质为基础的金粉颜料，其特征在于该颜料具有多层结构，其中，第一层是用热分解有机胶体微粒而得到的碳掺杂的二氧化钛层，其后是氧化铁(III)层。
本发明还提供了一种制备权利要求1的金粉颜料的方法，其特征在于，在需要可水解的金属盐溶液时，制备水性基质溶液，同时但分别地加入钛盐溶液和含水的有机胶体溶液，通过同时添加碱或酸使基质悬浮液的pH保持在能产生金属盐水解的范围内，分离出制成的基质、洗涤、干燥并在无氧的情况下，于＞700℃的温度下煅烧，煅烧后，氧化铁层或氢氧化铁层沉淀在按上述方式在水溶液中涂覆的基质上，然后，分离出制成的颜料、洗涤、干燥，需要时，煅烧。
适合于涂覆的基质基料是不透明的和透明的非片晶状基质。优选的基质是涂以金属氧化物的页硅酸盐和片晶状的材料。特别适宜的材料是云母、滑石、高岭土、氯氧化铋、玻璃粉、BaSO4、SiO2或合成陶瓷粉或其它类似材料。金属薄片也是适宜的，例如铝薄片或片晶状的金属氧化物，例如片晶状的氧化铁和在单层或相继各层中单独或以混合物的形式涂以有色或无色的金属氧化物的云母。这些称为珠光颜料的颜料公开在例如德国专利和专利申请14 67468、19 59 998、20 09 566、22 14 545、22 15 191、22 44 298、23 13331、25 22 572、31 37 808、31 37 809、31 51 343、31 51 354、31 51355、32 11 602以及32 35 017。
片晶状的基质通常具有的厚度为0.1-5微米，特别是0.2-4.5微米。其两种其它尺寸的范围通常为1-250微米，特别是2-200微米。
金粉颜料按两个步骤制备。首先用TiO2和有机胶体微粒覆盖基质。通过热解处理后，在第二步骤中用Fe2O3进行涂覆。
为了制备本发明的颜料，首先制备基质的水悬浮液。需要时，可将至少一种金属盐的溶液加入该水悬浮液中。其后，同时但分别地添加钛盐溶液和有机胶体溶液，通过同时添加酸或碱使反应混合物的pH保持在能产生金属盐水解的范围内。在此过程中，金属氧化物的混合物与胶体微粒一起沉淀在基质的表面上。
分离后，洗涤和干燥按上述方式涂覆的基质，将该颜料在无氧情况下于＞700℃、优选800-850℃下煅烧，在此过程中，有机胶体微粒发生分解。煅烧温度通常取决于沉淀层的厚度；煅烧时间可以由几分钟至几小时，但优选20-120分钟。
然后将涂覆了TiO2的基质悬浮于水中并借助添加铁(III)盐水溶液的方式涂覆氢氧化铁或氧化铁。分离出涂覆后的颜料、洗涤、干燥，需要时，在100-300℃、优选150-250℃的温度下煅烧。
该金属盐可以采用任一种酸或碱沉淀。最佳的浓度和pH值可以通过例行试验确定。通常，在整个沉淀过程中要保持为沉淀所确定的pH，以获得均匀的颜料。
使用那些工业上容易得到的碱是便利的，例如NaOH、KOH或氨，至于酸，可用稀释的矿物酸例如HCl、H2SO4或HNO3。由于碱和酸仅供改变pH之用，因此，它们的性质并不是关键的，所以也可以使用其它的酸和碱。
至于可从其沉淀氢氧化物的金属盐，可以使用所有能被碱或酸水解的水溶性盐。通常优选碱性水解。
适宜的金属盐是钛和铁的卤化物、硝酸盐和硫酸盐、特别是氯化物。
各种涂覆和水解金属盐的工艺参数都是常规类型的，且在例如DE 25 57 796中作了详细叙述。所有其它的参数例如粒度、金属盐的浓度、温度和优选的实施方案同样可在DE 25 57 796中查到。在涂覆片晶状基质的情况下，通过改变掺杂二氧化铁层的厚度可以得到任一种所需的一级或较高级的干涉色。TiO2层或Fe2O3层的厚度本身不是关键的，通常为约1-400nm、优选5-200nm。
TiO2层优选金红石的变型。这可以根据现有技术的方法通过将外来离子、特别是锡(IV)掺入该层中实现。这些方法叙述在例如DE-C 22 14 545和25 22 572中。
需要时，本发明的金粉颜料也可以后涂覆。
覆盖的组合物的主要成分包含有机胶体微粒。所有已知的颗粒尺寸＜10-5cm的有机胶体均可以使用。优选使用易溶于水的胶体的有机颗粒，例如多糖类、淀粉、纤维素、糊精或明胶及其衍生物。基质表面上的胶体微粒的比例占颜料总重的0.01-20％、优选0.1-10％。
在惰性条件下热解时，该胶体在金属氧化物层中破裂而产生极细碎的尺寸小于5nm的碳。该碳可均匀地分布在二氧化钛层中。这样，就将金属氧化物之间的空隙充满，从而产生极致密的高度不透明的碳-金属氧化物层。
二氧化钛层中碳的含量可以通过与二氧化钛一起涂覆到基质表面上的胶体微粒的量加以控制。
本发明的颜料中碳的比例通常占颜料总重的0.01-10％、优选0.1-5％、且特别优选0.1-1％。
由于基质不同，碳的重量比可随之变化很大。当碳含量升高时，颜料越来越呈现出石墨样的光泽。
尚未观察到由于有机溶剂而渗出碳的现象。此外，本发明的颜料在增加了的光泽及其高度不透明性上是显著的。除此而外，该颜料耐候性稳定而且是绝缘的。
根据本发明制备的金粉颜料是耐磨的、非常不透明和易于分散的，因而它们能用于各种用途、特别是用于汽车面漆、印刷油墨以及化妆品。
本发明因此还提供了该金粉颜料在一些配方例如油漆、清漆、粉末涂料、印刷油墨、塑料和化妆品中的应用。
本发明还提供了包含本发明的金粉颜料的一些配方。
以下实施例旨在更详细地说明本发明，但对本发明绝无限制：实施例1
将100克粒度为10-60微米的云母悬浮在2升水中，并将该悬浮液加热至75℃。将由2.3克SnCl4×5H2O和40毫升水中的10毫升37％HCl组成的溶液计量加入该云母悬浮液中。当SnCl4溶液添加完毕时，将220毫升TiCl4溶液(400克TiCl4/水)和明胶溶液(4克溶于220毫升水中)同时但分别地计量加入该颜料悬浮液中。用32％的NaOH溶液将pH调节至6.0。然后，将该混合物搅拌15分钟。最后，过滤出制成的颜料，洗涤除去盐，在100℃下干燥并在氮气气氛中于850℃下煅烧0.5小时。
将按上述方式涂覆的100克云母颜料悬浮在2升水中并将该悬浮液加热至75℃。在计量加入650毫升FeCl3溶液(5克FeCl3/100毫升水)的过程中，通过添加32％的NaOH溶液将pH保持恒定为4。当覆盖操作完毕时，继续在75℃下搅拌15分钟。过滤出制成的颜料，洗涤除去盐，然后在200℃下干燥10小时。得到具有金黄干涉色和灰色主色的颜料。实施例2
将100克粒度为10-60微米的云母悬浮在2升水中，并将该悬浮液加热至75℃。将由2.3克SnCl4×5H2O和40毫升水中的10毫升37％HCl组成的溶液计量加入该云母悬浮液中。当SnCl4溶液添加完毕时，将320毫升TiCl4溶液(400克TiCl4/水)和明胶溶液(4克溶于320毫升水中)同时但分别地计量加入该颜料悬浮液中。用32％的NaOH溶液将pH调节至6.0。然后，将该混合物搅拌15分钟。最后，过滤出制成的颜料，洗涤除去盐，在100℃下干燥并在氮气气氛中于850℃下煅烧0.5小时。
将按上述方式涂覆的100克云母颜料悬浮在2升水中并将该悬浮液加热至75℃。在计量加入300毫升FeCl3溶液(5克FeCl3/100毫升水)的过程中，通过添加32％的NaOH溶液将pH保持恒定为4。当覆盖操作完毕时，继续在75℃下搅拌15分钟。分离出制成的颜料，洗涤除去盐，然后在200℃下干燥10小时。得到具有金黄干涉色和灰色主色的颜料。实施例3
将100克粒度为10-60微米的云母悬浮在2升水中，并将该悬浮液加热至75℃。将由2.3克SnCl4×5H2O和40毫升水中的10毫升37％HCl组成的溶液计量加入该云母悬浮液中。当SnCl4溶液添加完毕时，将400毫升TiCl4溶液(400克TiCl4/水)和明胶溶液(4克溶于400毫升水中)同时但分别地计量加入该颜料悬浮液中。用32％的NaOH溶液将pH调节至6.0。然后，将该混合物搅拌15分钟。最后，过滤出制成的颜料，洗涤除去盐，在100℃下干燥并在氮气气氛中于850℃下煅烧0.5小时。
将按上述方式涂覆的100克云母颜料悬浮在2升水中并将该悬浮液加热至75℃。在计量加入170毫升FeCl3溶液(5克FeCl3/100毫升水)的过程中，通过添加32％的NaOH溶液将pH保持恒定为4。当覆盖操作完毕时，继续在75℃下搅拌15分钟。过滤出颜料，洗涤除去盐，然后在200℃下干燥10小时。得到具有金黄干涉色和灰色主色的颜料。对比例1
将100克粒度为10-60微米的云母悬浮在2升水中，并将该悬浮液加热至75℃，并添加1550毫升FeCl3溶液(5克Fe溶于100毫升水中)。通过添加32％的NaOH溶液将pH保持恒定为4。添加完毕后，将该颜料悬浮液在75℃下搅拌15分钟。过滤出涂覆了云母的颜料，洗涤除去盐，然后在200℃下干燥10小时。
得到带有棕色主色的铜黄金色的干涉色颜料。对比例2
将100克粒度为10-60微米的云母悬浮在2升水中，并将该悬浮液加热至75℃。将由2.3克SnCl4×5H2O和40毫升水中的10毫升37％HCl组成的溶液计量加入该云母悬浮液中。在添加32％的NaOH溶液的过程中将pH保持恒定为4。当SnCl4溶液添加完毕时，将500毫升TiCl4溶液(400克TiCl4/水)和明胶溶液(4克溶于500毫升水中)同时但分别地计量加入该颜料悬浮液中。用32％的NaOH溶液将pH调节至6.0，然后，将该混合物搅拌15分钟。最后，过滤出制成的颜料，洗涤除去盐，在氮气气氛中于850℃下煅烧0.5小时。
得到黄色干涉色和灰色主色的颜料。

Claims (8)

1.以金属氧化物涂覆的基质为基础的金粉颜料，其特征在于该颜料具有多层结构，其中，第一层是用热分解有机胶体微粒而得到的碳掺杂的二氧化钛层，其后是氧化铁(III)层。
2.根据权利要求1的金粉颜料，其特征在于该基质是片晶状的。
3.根据权利要求2的金粉颜料，其特征在于该片晶状的基质是云母片晶、玻璃粉、BaSO4、SiO2或合成陶瓷粉或用一种或多种金属氧化物涂覆的云母片晶。
4.根据权利要求1-3中任一项的金粉颜料，其特征在于该胶体的有机颗粒是淀粉、纤维素、明胶、糊精或其衍生物。
5.根据权利要求1-4中任一项的金粉颜料，其特征在于该TiO2层是金红石的变型。
6.权利要求1的金粉颜料的制备方法，其特征在于在需要可水解的金属盐溶液时，制备水性基质溶液，同时但分别地加入钛盐溶液和含水的有机胶体溶液，通过同时添加碱或酸使基质悬浮液的pH保持在能产生金属盐水解的范围内，分离出制成的基质、洗涤、干燥并在无氧的情况下，于＞700℃的温度下煅烧，煅烧后，氧化铁层或氢氧化铁层沉淀在按上述方式在水溶液中涂覆的基质上，然后，分离出制成的颜料、洗涤、干燥，需要时，煅烧。
7.权利要求1的金粉颜料在油漆、清漆、粉末涂料、印刷油墨、塑料和化妆品配方中的应用。
8.包含权利要求1的金粉颜料的配方。
CN96108367A 1995-06-23 1996-06-20 金粉颜料 Pending CN1145382A (zh)

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