CN1102948C - 多层干涉颜料 - Google Patents

多层干涉颜料 Download PDF

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CN1102948C
CN1102948C CN97196619A CN97196619A CN1102948C CN 1102948 C CN1102948 C CN 1102948C CN 97196619 A CN97196619 A CN 97196619A CN 97196619 A CN97196619 A CN 97196619A CN 1102948 C CN1102948 C CN 1102948C
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pigment
metal oxide
refractive index
coating
high refractive
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CN1225657A (zh
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H-D·布鲁克内
A·海兰德
C·施米特
C·萨克
C·斯比尔
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Merck Patent GmbH
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Merck Patent GmbH
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Abstract

由一种透明载体材料交替涂敷低折射率的金属氧化物层和高折射率的金属氧化物层组成的多层干涉颜料,所说的折射率的差值为至少0.1,可以通过下列过程获得:用湿法通过相应的水溶性金属化合物的水解交替用高折射率的金属氧化物水合物和低折射率的水合物涂敷所说的透明载体材料,分离,干燥所得的颜料,如果有必要,可以煅烧所得的颜料。

Description

多层干涉颜料
本发明涉及由交替涂敷低折射率的金属氧化物和高折射率的金属氧化物涂层的透明载体材料组成的多层干涉颜料。
具有低透明度并具有类似的层状结构的多层颜料是已知的。所说的金属氧化物层或者用湿法通过从金属盐溶液向载体材料上沉淀金属氧化物的水合物,或者通过真空中的气相沉积或溅射制备。一般来说,气相沉积法太复杂并且用于大批量生产颜料时成本高。因此,US 4,434,010描述了多层干涉颜料,由一种反射材料(铝)的中心层和在所说的中心铝层的两个面上交替涂敷的两种透明的高折射率和低折射率的介电材料,如二氧化钛和二氧化硅的涂层组成。这种颜料用于印刷证券。
特公平7-759描述了一种具有金属光泽的干涉颜料。它由一种交替涂敷二氧化钛和二氧化硅涂层的基质组成。所说的基质用铝、金和银的碎片形成或者用涂敷金属的云母和玻璃片状颗粒形成。因此,它是一种典型的金属颜料。这种颜料具有高度的不透明性。对于需要高度透明性的颜料的用途,如农用薄膜,该颜料是不合适的。此外,它还有不能产生干涉颜料具有的深度效果的缺点,因为,由于光在形成所说的核的金属层上的高度反射,在应用的介质中较深的颜料颗粒不能对光学外观有所贡献。因此,所说的干涉效果局限于位于所说的金属层上的涂层。
本发明的目的是提供一种基本透明的干涉颜料,具有强烈的干涉色和/或所说的干涉色的角依赖性。此外,本发明的目的是提供在可见光区和红外光区中具有特定的光谱特性的颜料。
根据本发明,通过由交替涂敷低折射率的和高折射率的金属氧化物涂层的透明载体材料组成的多层干涉颜料达到了这个目的,所说的折射率的差值至少为0.1,所说的多层颜料通过用高折射率的金属氧化物和低折射率的金属氧化物通过相应的水溶性金属化合物的水解用湿法交替涂敷所说的透明载体,然后分离、干燥而得,如果有必要,煅烧所说的颜料。
所说的透明载体材料是云母、一种不同于云母的层状硅酸盐、玻璃碎片、片状颗粒形式的PbCO3·Pb(OH)2(碱式碳酸铅)和BiOCl,或通过WO 93/08237描述的方法制备的片状二氧化硅。
高折射率的金属氧化物可以是一种氧化物或者具有或不具有光吸收性质的氧化物的混合物,例如TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,或者是高折射率的化合物,例如钛酸铁、氧化铁水合物和钛的低价氧化物,或者是这些化合物相互之间的或者与其它金属氧化物的混合物和/或混合相。
低折射率的金属氧化物是SiO2、Al2O3、AlOOH、B2O3或其混合物,类似地,可以具有吸光或不吸光的性质。如果希望,所说的低折射率的金属氧化物层可以包括碱金属氧化物和碱土金属氧化物作为组分。
另外,根据本发明,通过一种制备所说的新型颜料的方法达到了这个目的,其中,把所说的透明载体材料悬浮在水中,并通过加入相应的水溶性金属化合物并使之水解从而交替用高折射率的金属氧化物水合物和低折射率的金属氧化物水合物涂敷载体材料,设定各种金属氧化物的沉淀所需的pH值并通过同时加入酸或碱保持恒定,然后,把所涂敷的载体材料从所说的水悬浮液中分离出来,干燥,如果有必要,进行煅烧。
另外,本发明涉及所说的新型颜料用于颜料涂料、印刷油墨、塑料、陶瓷和玻璃釉料、化妆品、尤其是农用薄膜的生产中的应用。
为此,它们可以以与传统的商业颜料,如无机和有机吸光颜料、金属颜料和LCP颜料的混合物的形式使用。
高折射率和低折射率的金属氧化物的涂层的厚度对于所说的颜料的光学性能是至关重要的。由于希望一种具有强干涉颜色的产品,所说的涂层的厚度必须相互之间相对调整。如果n是一个涂层的折射率,d是其厚度,一个薄涂层中呈现的颜色是n和d的乘积,即光学厚度。这样一种薄膜的颜色,如用反射光中的垂直入射光所产生的,来自波长为λ=(4/2N-1)·nd的光的相长和波长为λ=(2/N)·nd的光的相消,这里,N是正整数。随着所说的薄膜厚度的增大发生的颜色变化分别来自特定波长的光通过干涉产生的相长或相消。例如,115nm厚的折射率为1.94的二氧化钛薄膜的光学厚度为115×1.94=223nm,在反射过程中,波长为2×223nm=446nm(蓝色)的光相消,导致反射光为黄色。在多层颜料的情况下,干涉色由特定波长的光的相长确定,如果在一种多层颜料中的两个或多个层具有相同的光学厚度,反射光的颜色随着层数的增加变得更强,更饱满。而且,通过适当选择层厚,有可能得到与观察角度相关的颜色的特别显著的变化。产生一种明显的色彩跳动,这可能是根据本发明的颜料所希望的。所以,各个金属氧化物层的厚度与其折射率无关,为20~500nm,优选的是50~300nm。
所说的层数和层厚取决于要求的效果和所用的基质。在云母上,如果产生TiO2/SiO2/TiO2 3层体系并且各层的厚度在光学上相互匹配,可以取得要求的效果。例如,在使用光学上较薄的TiO2和SiO2涂层时(层厚<100nm),有可能产生蓝色干涉色的颜料,这种颜料用较小的TiO2含量,产生比纯TiO2-云母颜料更强的颜色并且更透明。TiO2的节约量最高可达50wt%。
通过沉淀厚的SiO2涂层(层厚>100nm),获得了具有干涉色的强烈的显著的角相关性的颜料。
通过进一步沉淀SiO2和TiO2涂层,也可能获得5层或更高的体系,但是,所说的层数受所说的颜料的经济效益的限制。
但是,如果使用具有均匀层厚的SiO2片状颗粒代替云母作为基质,那么可以获得特别良好确定的干涉效果。
在这种情况下,例如,用3层上述结构产生一种包括7个精确确定厚度的薄层的干涉体系。这样一种颜料的反射或发射光谱表现出比基于云母等具有宽厚度分布的基质的相应颜料的光谱更精细的并且更精确匹配的结构。
即使用极薄的TiO2层(层厚<40nm),这些颜料也表现出强烈的干涉色,所说的干涉色的角相关性也是特别明显的。用传统的金属氧化物-云母颜料没有观察到这种非常的颜色跳动。
例如,根据国际专利申请WO 93/08237,通过一种碱金属硅酸盐溶液的水解和固化,在一个连续带上制备所说的SiO2片状颗粒。
所说的金属氧化物层优选的是通过一种湿化学法涂敷,所说的湿化学法可以是为制备珍珠光泽的颜料而开发的湿化学涂敷法中的一种,例如,在DE 14 67 468,DE 19 59 988,DE 20 09 566,DE 22 14 545,DE 22 15 191,DE 22 44 298,DE 23 13 331,DE 25 22 572,DE 3137 808,DE 31 37 809,DE 31 51 343,DE 31 51 354,DE 31 51355,DE 32 11 602,DE 32 35 017或另外的专利文献和其它出版物中描述了这类技术。
对于所说的涂敷,把所说的基质颗粒悬浮在水中,在适合于水解的pH值下加入一种或多种可水解的金属盐,选择所说的pH值使所说的金属氧化物和/或金属氧化物水合物直接沉淀在所说的片状颗粒上而没有任何二次沉淀产生。通常通过同时定量加入一种碱保持pH值恒定。然后把所说的颜料分离,洗涤并干燥,如果有必要,可以煅烧,有可能对于特定的涂层优化所说的煅烧温度。如果有必要,可以分离涂敷了每个涂层的颜料并干燥,如果有必要,在为了通过沉淀涂敷下一个涂层而重新悬浮之前煅烧。
此外,涂敷也可以在流化床反应器中通过气相涂敷进行,其中,例如可以使用在EP 0 045 851和EP 0 106 235中提出的制备珍珠光泽颜料的相应技术。
所用的高折射率的金属氧化物优选的是二氧化钛,所用的低折射率的金属氧化物优选的是二氧化硅。
对于涂敷所说的二氧化钛涂层,在US 3,553,001中描述的方法是优选的。
向一种待涂敷的材料的悬浮液中缓慢加入一种钛盐水溶液,加热到约50~100℃,优选的是70~80℃,通过同时定量加入一种碱,如氨水或碱金属氢氧化物水溶液保持基本恒定的pH值约为0.5~5,优选的是约1.5~2.5。一旦达到TiO2沉淀的要求的涂层厚度,停止加入所说的钛盐溶液和碱溶液。
这种方法也称为滴定法,可以显著地避免过量的钛盐。通过仅向水解提供单位时间的钛盐量可以做到这一点,所说的单位时间钛盐量是均匀涂敷所说的水合TiO2所必需的,并且是由待涂敷的颗粒的可得的表面积单位时间内可以吸附的钛盐量。因此没有产生不沉淀在待涂敷的表面上的水合二氧化钛颗粒。
对于涂敷所说的二氧化硅涂层,可以使用下列方法:向待涂敷的材料的悬浮液中定量加入一种硅酸钠溶液,加热到50~100℃,优选的是70~80℃。通过同时加入10%的盐酸保持pH值恒定为4~10,优选的是6.5~8.5。在硅酸盐溶液的加入后,搅拌30分钟。
也有可能通过涂敷另外的涂层改变所说的颜料的粉末颜色,例如涂敷着色金属氧化物或普鲁士蓝、过渡金属化合物,如Fe、Cu、Ni、Co或Cr的化合物,或者有机化合物,如染料或彩色沉淀颜料。
到目前为止,还没有提出在细分散的片状颗粒基质上在含水介质中使用纯无机原料用湿化学法产生两个或多个具有精确确定的厚度的不同折射率的干涉层的方法。
此外,可以使所说的颜料经过后涂层或后处理过程,以进一步增大光稳定性、耐候性和化学稳定性的或者促进所说的颜料的加工处理,尤其是其混入不同介质中的加工处理。合适的后涂层技术是在DE-C 22 15191、DE-A 31 51 354、DE-A 32 35 017或DE-A 33 34 598中所描述的那些技术。
所说的另外涂覆的物质仅占全部颜料的约0.1~5wt%,优选的是约为0.5~3wt%。
另外,所说的新型颜料可以涂敷热结合的低溶解度的无机或有机着色剂。优选的是使用彩色沉淀颜料,具体的是铝沉淀色料。为此,通过沉淀涂敷一种氢氧化铝涂层,并在第二个步骤中用彩色沉淀色料上色。在DE 24 29 762和DE 29 28 287中更详细地描述了该过程。
如EP 0 141 173和DE 23 13 332中所述,同样优选的是用络合盐颜料的另一个涂层,尤其是铁氰络合物,如普鲁士蓝和Turnbull蓝。
根据DE 40 09 567,所说的新型颜料也可以涂敷有机染料,尤其是涂覆酞菁或金属酞菁和/或阴丹士林染料。为此,制备一种在染料溶液中的颜料悬浮液,然后把这种悬浮液与一种溶剂混合,所说的染料在所说的溶剂中溶解度很低或者为零。
此外,对于一种另外的涂层,也可以使用金属的硫属化物或金属的硫属化物水合物和碳黑。
所说的颜料可以以传统方式用于彩色涂料、印刷油墨、塑料、化妆品和用于陶瓷和玻璃的釉料。优选的是用于彩色农用薄膜。
为了阻止太阳的红外辐射,从而防止例如温室中的过热,农用薄膜通常用颜料进行处理。
到目前为止,几乎所有的用于农用薄膜中的颜料是彩色颜料。所以,它们吸收大部分可见光,但是,这些可见光是在所说的薄膜下的植物生长所需要的。因此,至今为止在农用薄膜中所用的颜料对植物的生长有不利的影响。
因此,本发明得的一个目的是提供一种在可见光区域具有高透明度并且在NIR区具有高反射率的颜料。也可以调整这样的颜料的性质使得他们具有其它的或附加的功能,例如,以控制的方式影响植物的形态。
下面给出的实施例用于说明本发明但不限制本发明。
实施例1
具有薄SiO2层的3层体系
1)第一个TiO2涂层
把150g的云母(颗粒尺寸10~40μm)悬浮在2l的去离子水中,并把该悬浮液加热到75℃。在60分钟的过程中,向这种悬浮液中定量加入175ml的TiCl4水溶液(400g的TiCl4)。在整个添加过程中,用32%的NaOH溶液使pH保持恒定为2.2。在添加结束时,为了完成所说的沉淀,在75℃进行30分钟的搅拌。
2)SiO2层:
用NaOH溶液把所说的悬浮液的pH值提高到7.5。在90分钟的过程中,在75℃向这种悬浮液中定量加入250ml的硅酸钠溶液(125gSiO2/l)。在该过程中,用10%的盐酸使pH值保持恒定。在添加结束后,为了完成所说的沉淀,在75℃再搅拌30分钟。
3)第二个TiO2层:
再用10%的盐酸把所说的pH值降低到2.2,如步骤1)中所述,用另外的175ml的TiCl4溶液通过沉淀再次涂敷TiO2
然后,使所说的混合物冷却到室温,过滤出所得的颜料,用去离子水水洗至不合盐并在110℃干燥。然后把所说的颜料在850℃煅烧30分钟。
值得注意的是这样获得的颜料比对比的纯TiO2-云母颜料更强的蓝干涉色和更高的透明度。
实施例2
具有厚SiO2层的3层体系
1)第一个TiO2涂层
把150g的云母(颗粒尺寸10~40μm)悬浮在2l的去离子水中,并把该悬浮液加热到75℃。在100分钟的过程中,向这种悬浮液中定量加入300ml的TiCl4水溶液(400g的TiCl4/l)。在整个添加过程中,用32%的NaOH溶液使pH保持恒定为2.2。在添加结束时,为了完成所说的沉淀,在75℃进行30分钟的搅拌。
2)SiO2层:
用NaOH溶液把所说的悬浮液的pH值提高到7.5。在7.5小时的过程中,在75℃定量加入1350ml的硅酸钠溶液(125g SiO2/l)。在该过程中,用10%的盐酸使pH值保持恒定。在添加结束后,为了完成所说的沉淀,在75℃再搅拌30分钟。
3)第二个TiO2层:
再把所说的pH值降低到2.2,如步骤1)中所述,用另外的250ml的TiCl4溶液通过沉淀再次涂敷TiO2
然后,使所说的混合物冷却到室温,过滤出所得的颜料,用去离子水水洗至不含盐并在110℃干燥。然后把所说的颜料在850℃煅烧30分钟。
在垂直观察时,这样获得的颜料表现出强烈的蓝-绿干涉色,当所说的颜料倾斜时,所说的干涉色通过紫色变成红色。
实施例3
具有Fe2O3层的3层体系
本实施例描述一种其中的第三层不再是TiO2而是Fe2O3的层状结构。
1)TiO2
如实施例1所述。
2)SiO2
如实施例1所述。
3)Fe2O3
用10%的盐酸把涂敷了TiO2和SiO2的云母的悬浮液的pH值调节至3.0。然后在5小时的过程中,定量加入1750ml的FeCl3水溶液(35gFe/l)并通过同时加入32%的NaOH保持pH值恒定。然后,为了完成所说的沉淀,在75℃进行45分钟的搅拌。
把所说的混合物冷却到室温,过滤出所得的红-棕色颜料,用去离子水水洗至不含盐并在110℃干燥。然后把所说的颜料在850℃煅烧30分钟。获得一种具有类似铜的干涉色的橙色-棕色珍珠光泽的颜料。
实施例4
包括5个交替的TiO2和SiO2层的多层体系
如实施例1所述,用TiO2、SiO2和TiO2涂敷云母。再涂敷另一个SiO2层和一个TiO2外层。涂敷过程如上所述。
所得的颜料比实施例1的颜料具有更清澈的蓝干涉色并具有更高的透明度。
实施例5
在可见光区具有高透明度,在近红外区具有高反射率的3层体系
把100g的云母(颗粒尺寸10~60μm)悬浮在2l的去离子水中,并把该悬浮液在强烈搅拌的条件下加热到80℃。在pH为2.0下和以4ml/min的速度向这种混合物中定量加入一种在90ml的去离子水中的3g的SnCl4×5H2O和10ml的盐酸(37%)的溶液。然后,在1.8的pH下,以2ml/min的速度定量加入480ml的TiCl4水溶液(400g的TiCl4/l)。然后用NaOH溶液(32%)把所说的悬浮液的pH值提高到7.5,在该pH下,以2ml/min的速度定量加入一种在314ml的去离子水中的230ml的硅酸钠(来自Merck;Order No.5621)的溶液。用盐酸(10%)保持该过程中的pH值恒定。然后,在2.0的pH值下,以4ml/min的速度定量加入一种在90ml去离子水中的3g的SnCl4×5H2O和10ml的盐酸(32%)的溶液。然后,在1.8的pH值下,以2ml/min的速度定量加入481ml的TiCl4溶液(400g的TiCl4/L)。
在加入SnCl4×5H2O溶液和TiCl4溶液过程中,在每种情况下用NaOH溶液(32%)保持pH值恒定。
完成后,过滤出所说的颜料,用20l去离子水洗涤,在110℃干燥并在850℃煅烧30分钟。
这种颜料用于生产涂料薄膜,其透射光谱复制于图1中。值得注意的是所说的颜料在可见光区有非常好的透明度,在近红外区有非常高的反射率,即用传统的干涉颜料不能获得的性能。因此,这种颜料特别适用于农用薄膜。
实施例6
具有高的颜色角相关性的颜料
把100g的TiO2-云母颜料(颗粒尺寸10~60μm,35%的TiO2)悬浮在2l的去离子水中,并把该悬浮液在强烈搅拌的条件下加热到80℃。然后用氢氧化钠溶液(32%)把pH值调节到7.5,在该pH值下,以2ml/min的速度向这种混合物中定量加入一种在300ml的去离子水中的296ml的硅酸钠(来自Merch;Order NO.5621)溶液。在该加入过程中,用盐酸(10%)保持pH值恒定。然后,在2.0的pH值下,以4ml/min的速度向这种混合物中定量加入一种在90ml的去离子水中的3g的SnCl4×5H2O和10ml的盐酸(37%)的溶液。然后,在1.8的pH下,以2ml/min的速度定量加入238ml的TiCl4水溶液(400g的TiCl4/l)。
在加入SnCl4×5H2O溶液和TiCl4溶液过程中,在每种情况下用NaOH溶液(32%)保持pH值恒定。
完成后,过滤出所说的颜料,用20l去离子水洗涤,在110℃干燥并在850℃煅烧30分钟。
把所煅烧的颜料搅拌到一种透明涂料(浓度1.7%)中,这种涂料涂敷到黑/白卡片上。
所说的颜料的干涉色是非常明显的,尤其是在黑色的卡片上。当所说的卡片从垂直向水平的视角倾斜时,所说的反射色从强烈的蓝色向强烈的紫色变化。在各种垂直(80°/100°)和水平的(25°/155°)观察角下测定所说的黑卡的反射光谱。图2中复制了所说的反射曲线。
实施例7
用SiO2片状颗粒作为载体的3层体系
1)第一个TiO2涂层
把100g的SiO2片状颗粒(颗粒尺寸20~70μm)悬浮在1.5l的去离子水中,并把该悬浮液加热到75℃。在90分钟的过程中,向这种悬浮液中定量加入160ml的TiCl4水溶液(400g的TiCl4/l)。在整个添加过程中,用32%的NaOH溶液使pH保持恒定为2.2。在添加结束时,为了完成所说的沉淀,在75℃进行30分钟的搅拌。
2)SiO2层:
用NaOH溶液把所说的悬浮液的pH值提高到7.5。在3.5小时的过程中,在75℃定量加入720ml的硅酸钠溶液(125g SiO2/l)。在该过程中,用10%的盐酸使pH值保持恒定。在添加结束后,为了完成所说的沉淀,在75℃再搅拌30分钟。
3)第二个TiO2层:
再把所说的pH值降低到2.2,如步骤1)中所述,用另外的235ml的TiCl4溶液通过沉淀再次涂敷TiO2
然后,使所说的混合物冷却到室温,过滤出所得的颜料,用去离子水水洗至不含盐并在110℃干燥。然后把所说的颜料在850℃煅烧30分钟。这样得到的颜料在垂直观察时,表现出明亮的黄-绿干涉色,当所说的颜料倾斜时,所说的颜色通过蓝-绿向暗紫变化。

Claims (2)

1、一种制备多层干涉颜料的方法,所述多层干涉颜料由一种透明载体材料交替涂敷高折射率的化合物层和低折射率的金属氧化物层组成,所述高折射率的化合物选自TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3、ZnO,或这些氧化物的混合物或者钛酸铁、氧化铁水合物和钛的低价氧化物,或者是这些化合物之间的或者与其它金属氧化物的混合物和/或混合相,所述低折射率的金属氧化物选自SiO2、Al2O3、AlOOH、B2O3或其混合物,如果有必要,碱金属氧化物和碱土金属氧化物可以作为附加组分,所述高折射率层和低折射率层的折射率差值为至少0.1,所述方法包括:把所说的透明载体材料悬浮在水中,通过加入相应的水溶性无机金属化合物并使之水解而交替涂敷高折射率的化合物的水合物和低折射率的金属氧化物水合物,确定所述高折射率的化合物的水合物和低折射率的金属氧化物水合物沉淀所需的pH值并通过加入酸或碱使其保持恒定,然后,把所涂敷的载体材料从水悬浮液中分离出来,干燥,如果有必要,进行煅烧。
2、根据权利要求1的方法,特点在于所说的透明载体材料是云母、不同于云母的层状硅酸盐、玻璃碎片、PbCO3·Pb(OH)2、BiOCl或片状SiO2
CN97196619A 1996-05-09 1997-05-23 多层干涉颜料 Expired - Fee Related CN1102948C (zh)

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US7169222B2 (en) 2007-01-30
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US6689205B1 (en) 2004-02-10
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