CN1139688A - 彩色颜料 - Google Patents

彩色颜料 Download PDF

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CN1139688A
CN1139688A CN96104477A CN96104477A CN1139688A CN 1139688 A CN1139688 A CN 1139688A CN 96104477 A CN96104477 A CN 96104477A CN 96104477 A CN96104477 A CN 96104477A CN 1139688 A CN1139688 A CN 1139688A
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pigment
coloured pigment
matrix
iron
trivalent
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K·阿姆布罗希斯
M·施拉姆尔码斯
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Merck Patent GmbH
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Abstract

本发明涉及一种彩色颜料，该颜料基于用被涂覆的氧化铁(三价)层涂覆的基质，还涉及该颜料的制备方法及其用途，尤其是在水性涂料体系中的用途。

Description

彩色颜料
本发明涉及一种彩色颜料，该颜料基于被氧化铁(三价)掺杂层涂覆的基质，还涉及该颜料的制备方法及其用途，尤其是在水性涂料体系中的用途。
文献中已多次公开了含有氧化铁的颜料。由DE1467468可知：珠光颜料靠加入氧化铁来增强其金色。DE-P1959998中公开了一种制备添加了氧化铁的珠光颜料的专用方法。而且，其中含氧化铁的一层还涂有一层二氧化钛和/或二氧化锆。这些珠光颜料中的氧化铁(三价)在酸性范围内从铁(三价)盐溶液中沉淀下来。DE2244298公开了一种金色颜料，基于用二氧化钛涂覆、并用Fe2O3后涂覆的云母片状粉末，Fe2O3由氢氧化铁(二价)氧化制成。SU16999930A1公开了具有提高的珍珠母光泽的红色颜料，基于涂覆了Fe2O3和B-2O3的云母片晶。
DE4135742A1公开了涂覆B2O3的氧化铁颜料，该颜料表面特别光滑。通过硝基苯法制备的磁铁矿颜料，接着在空气中煅烧，就能转化成各种色调的红色颜料。US5273576公开了一种珠光颜料，其中云母上涂有SnO2、ZnO或ZrO2掺杂的氧化铁(三价)层，该颜料的特点在于它提高的色度。
已有技术中的氧化铁颜料在用于非水性涂料体积中时，其高色值及高耐候性是显然的。然而在水性涂料体系中，已知的氧化铁颜料都显示出这种缺点：这些颜料导致涂膜中形成微细的气泡，这点变得越来越严重，尤其在汽车工业中。这些气泡使光的散射增加，并因此给着色水性涂料体系的色彩和光泽带来不利影响。
另一个缺点在于着色涂料影像清晰度的降低以及再生能力的减弱。
因此本发明的目的是开发一种改进的含氧化铁颜料，该颜料能很容易地分散于水性涂料体系中而其性能不降低，并且不存在上述缺点。
如今已意外地发现：用经SiO2和ZrO2掺杂的氧化铁(三价)层涂覆的基质，其高色值及高光泽是显然的，并能毫不困难地混入水性涂料体系中。
因此本发明提供了一种彩色颜料，基于用氧化铁(三价)涂覆的基质，其特征在于该氧化铁层是用ZrO2和SiO2掺杂过的。
本发明还提供了一种制备本发明颜料的方法，该方法的特点在于：在能使相应的氢氧化物或氧化物沉淀的条件下，将铁(三价)盐水溶液、锆盐水溶液和水溶性硅化合物同时或依次加入水性基质悬浮液中，然后将颜料分离、洗涤、干燥，并在高于500℃的温度下煅烧。
适用于涂料的基本基质是不透明和透明的片晶状或非片晶状基质。优选的基质是叶硅酸盐和用金属氧化物涂覆的片晶状材料。特别适用的基质为云母、滑石粉、高岭土、氯氧化铋、玻璃、SiO2或陶瓷的片状粉末，合成的无载体片晶或其它类似材料。此外，适用的还有金属片状粉末如铝的片状粉末，或是片晶状金属氧化物如片晶状氧化铁，以及用彩色或无色金属氧化物涂覆的云母，所述的金属氧化物如TiO2、Fe2O3、SnO2、Cr2O3、ZnO和其它金属氧化物，可以单独或混合用于一层涂层中，或用于连续涂层中。这些颜料通称为珠光颜料，已公开于德国专利及专利申请1467468、1959998、2009566、2214545、2215191、2244298、2313331、2522572、3137808、3137809、3151343、3151354、3151355、3211602和3235017中。
片晶状基质的厚度一般在0.1到5μm之间，尤其是在0.2至4.5μm之间。另两个方向的尺寸范围通常在1至250μm之间，尤其是在2至200μm之间。
制备本发明的颜料时，首先要制备基质的水性悬浮液。再将铁(三价)盐水溶液、锆盐水溶液和硅酸盐水溶液同时或最好是依次量入上述悬浮液中，同时，通过加入酸或碱使反应混合物的pH值保持在能引起金属盐水解的范围内。在这种条件下，Fe2O3、ZrO2和SiO2或其相应的氢氧化物就会依次或同时沉淀在基质表面上。反应溶液的温度不是非常关键，通常是在20-80℃。一般，氧化物或氢氧化物在pH值为3至12之间时沉淀。通过加入酸，最好是无机酸，例如HCl、HNO3、H2SO4，以及加入碱，例如NaOH、KOH、Na2CO3、NH3，就能很容易地使pH值保持在一恒定值上。
涂覆的基质经分离、洗涤并干燥后，所得颜料在大于500℃、最好是800-850℃的温度下煅烧。煅烧时间一般取决于沉积层的厚度，可以从几分钟至若干小时，但最好在20-120分钟之间。
作为能沉淀出氢氧化物或氧化物的金属盐，可以用所有通常碱或酸能水解的水溶性盐。特别适用的铁(三价)盐是铁的卤化物、铁的硝酸盐和铁的硫酸盐，最好是氯化铁(三价)。
锆化合物最好以氯化物ZrCl4或碱式氯化物ZrOCl2的形式使用。
二氧化硅以水溶性无机硅化合物的形式加入悬浮液中。适用的制品是可从市场上买到的称为“水玻璃”的碱金属硅酸盐水溶液，例如钾水玻璃和钠水玻璃。
对氧化铁(三价)层掺杂时，ZrO2与Sio2的比例可以是所有可能的比例。可以看出，尤其当ZrO2与SiO2之比为10∶1至0.1∶1，最好为5∶1至0.5∶1时，对颜色强度和光泽起了积极作用。氧化铁(三价)层中掺杂剂的量为0.1-10％重量，最好为0.1-5％重量，尤其是0.1-3％重量。
用本发明的方法制备的彩色颜料，其高颜色强度、高光泽及高不透明度是显然的。这种颜料适合于宽范围的着色体系，最好是清漆、涂料和印刷油墨领域的着色体系。
由于这种颜料的高光稳定性和高耐候性，它们突出地适用于汽车面漆，尤其是那些基于水性体系的汽车面漆。
因此，本发明还提供了本发明的氧化铁颜料在以下配方中的用途：如涂料、清漆、印刷油墨、塑料和化妆制品。
颜料在配方中的用量一般不超过30％，最好是0.5-10％。
本发明还提供了含有本发明颜料的配方。
以下给出的实施例是用于解释而不是用于限制本发明的。
实施例1
将由10kg粒径为10-50μm的云母悬浮于150l水中而构成的悬浮液，在搅拌下加热至75℃。用5％的HCl将pH值调节至3。然后加入FeCl3水溶液(Fe重含量为3％)，用约为30％的NaOH使pH值保持在3.0。当有了红色干涉色时，停止加FeCl3溶液，并将混合物再搅拌15分钟。
用5％的NaOH将pH值调节至3.2后，在一小时之内加入一种由175gZrOCl2·8H2O溶于15l水中构成的溶液。持续搅拌15分钟，并用5％的NaOH将pH值调节至9。在一小时之内，将硅酸钠溶液〔180ml硅酸钠(27％重量份)溶于15l水中〕量入，用5％的HCl使pH值保持恒定。加入结束时，用5％的HCl将pH值调节至6.5，再将悬浮液搅拌15分钟。滤出产品、用水洗涤、干燥并在850℃下煅烧。
实施例2-对比例
将由10kg粒径为10-50μm的云母悬浮于150l水中而构成的悬浮液，在搅拌下加热至75℃。用5％的HCl将pH值调节至3.0。然后加入FeCl3水溶液(Fe重含量为3％)，同时加入30％的NaOH使pH值保持恒定。当有了红色干涉色时，停止加FeCl3溶液，并将混合物再搅拌15分钟。
用5％的NaOH将pH值调节至5.0，并将此悬浮液再搅拌15分钟。滤出产品、用水洗涤、干燥并在850℃下煅烧。
用冷凝水检测法评价所得的颜料。
分别将实施例1和对比例所得的颜料混入一种商业水性清漆中，将所得涂料喷涂于金属板上就制成了检测样品。
按DIN50017(冷凝水检测法-气候条件恒定)进行检测。
检测时间：40℃下240小时
对溶胀过程的评价按DIN53230用目视进行。在评价尺度中，O表示“无变化”，5表示“剧烈改变”。
起泡程度按DIN53209用目视评价。m表示每单位面积出现气泡的频率，g表示气泡的尺寸。
评价尺度范围从0(优秀)至5(极差)。
光泽度评价按DIN67530用反射计进行。
影像清晰度(DOI)按ASTM EU30-91测量。
检测结果列于表1：
                                              表1
  实施例    溶胀        起泡  划格法检测  20°光译度评价，％   影像清晰度，％
    12空白样品(无颜料)    1-241        mo/gom3-4/g0-1mo/g0     Gt0Gt0Gt1      949097       975994
表1显示出：本发明的颜料抑制了水性涂料中细微气泡的形成，提高了影像清晰度，对光泽度的影响比未处理的颜料小得多。

Claims (9)

1.基于用氧化铁(三价)涂覆的基质的彩色颜料，其特征在于氧化铁层是经二氧化锆和二氧化硅掺杂的。
2.权利要求1的彩色颜料，其特征在于氧化铁层中二氧化锆和二氧化硅的比例为0.1-10％重量份。
3.权利要求1或2的彩色颜料，其特征在于ZrO2与SiO2的比例为10∶1至0.1∶1。
4.权利要求1-3之一的彩色颜料，其特征在于被涂覆的基质呈片晶状。
5.权利要求4的彩色颜料，其特征在于所述的基质是云母片晶或是SiO2、玻璃或陶瓷的片状粉末。
6.制备权利要求1中彩色颜料的方法，其特征在于：在能使相应的氢氧化物或氧化物沉淀的条件下，将铁(三价)盐水溶液、锆盐水溶液和水溶性硅化合物同时或依次加入水性基质悬浮液中，然后将颜料分离、洗涤、干燥，并在高于500℃的温度下煅烧。
7.权利要求1的彩色颜料用于以下配方中的用途，如涂料、着色剂、塑料和化妆制品。
8.用权利要求1的彩色颜料对水性涂料体系着色的用途。
9.含有权利要求1中彩色颜料的配方。
CN96104477A 1995-05-12 1996-05-10 彩色颜料 Pending CN1139688A (zh)

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JP2000086943A (ja) * 1998-09-10 2000-03-28 Nippon Paint Co Ltd ２色性塗料組成物
JP2001031911A (ja) * 1999-07-21 2001-02-06 Nippon Paint Co Ltd 多色性塗料組成物、塗膜形成方法および塗装物
JP2002121492A (ja) * 2000-10-19 2002-04-23 Nippon Paint Co Ltd 光輝性塗料組成物、塗膜形成方法および塗装物
DE10137831A1 (de) 2001-08-02 2003-02-13 Merck Patent Gmbh Mehrschichtige Interferenzpigmente
KR100435812B1 (ko) * 2001-10-19 2004-06-12 주식회사 태평양 다공성 구상 실리카 표면에 나노크기의 지르코니아와실리카가 코팅된 기능성 복합 분체 및 이의 제조방법, 및이를 함유하는 화장료 조성물
DE10204336A1 (de) * 2002-02-01 2003-08-14 Merck Patent Gmbh Verwendung von Mehrschichtpigmenten im Lebensmittel- und Pharmabereich
EP3234025B1 (de) * 2014-12-19 2019-04-24 Eckart GmbH Rotfarbene effektpigmente mit hohem chroma und hoher brillanz, verfahren zu ihrer herstellung und verwendung derselben
EP3034562B2 (de) * 2014-12-19 2021-12-08 Eckart GmbH Absorbierende Effektpigmente mit hohem Chroma und hoher Brillanz, Verfahren zu ihrer Herstellung und Verwendung derselben
EP3034563B1 (de) 2014-12-19 2019-02-20 Eckart GmbH Goldfarbene Effektpigmente mit hohem Chroma und hoher Brillanz, Verfahren zu ihrer Herstellung und Verwendung derselben
PL3034564T3 (pl) * 2014-12-19 2018-07-31 Eckart Gmbh Pigmenty efektowe o wysokiej transparentności, wysokim nasyceniu i wysokiej czystości barwy, sposób ich wytwarzania i ich zastosowanie

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JPH08302236A (ja) 1996-11-19
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CZ132096A3 (en) 1997-02-12
EP0742271A3 (de) 1998-05-27
BR9602208A (pt) 1998-04-07
JP3568685B2 (ja) 2004-09-22
KR960041293A (ko) 1996-12-19
CA2176287A1 (en) 1996-11-13
US5759257A (en) 1998-06-02

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