CN101688067B - 基于珍珠岩薄片的干扰颜料 - Google Patents
基于珍珠岩薄片的干扰颜料 Download PDFInfo
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- CN101688067B CN101688067B CN2008800243913A CN200880024391A CN101688067B CN 101688067 B CN101688067 B CN 101688067B CN 2008800243913 A CN2008800243913 A CN 2008800243913A CN 200880024391 A CN200880024391 A CN 200880024391A CN 101688067 B CN101688067 B CN 101688067B
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- pearl
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Classifications
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- C08K9/02—Ingredients treated with inorganic substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D17/00—Pigment pastes, e.g. for mixing in paints
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- C09D17/007—Metal oxide
- C09D17/008—Titanium dioxide
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- A61K2800/65—Characterized by the composition of the particulate/core
- A61K2800/651—The particulate/core comprising inorganic material
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
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Abstract
本发明涉及包含片状珍珠岩基质,和(a)介电材料,尤其是具有高折光指数的金属氧化物,和/或(a)金属层,尤其是薄的半透明金属层的颜料;它们的制备方法和它们在漆料、喷墨印刷中,在用于染色织物中,在用于着色涂料(漆料)中、在印刷油墨、塑料、化妆品、用于陶瓷和玻璃的釉料中的用途。
Description
本发明涉及具有珍珠岩芯的(干扰)颜料,其包含具有高折光指数的金属氧化物或(薄半透明)金属层,一种制备(干扰)颜料的方法和它们在漆料、喷墨印刷中、在用于染色织物中、用于着色涂料中、在印刷油墨、塑料、化妆品中、在用于陶瓷和玻璃釉料中的用途。
具有由透明载体材料如天然或合成云母、SiO2,或玻璃组成的芯的干扰颜料为已知的。例如参考Gerhard Pfaff和Peter Reynders,Chem.Rev.99(1999)1963-1981。
在大多数情况下,天然透明云母用作基质。天然云母为生物惰性的且因此可接受用于广泛应用。基质云母由厚度为约300-600nm且具有指定粒度分布的薄微片组成。
基于涂覆有金属氧化物如铁氧化物、钛氧化物等的天然云母的珠光颜料的缺点在于它们由于铁氧化物杂质而在主色角或阴影侧发展对于云母而言特定的黄色,并且由于云母基质的大范围厚度分布和云母基质表面不平坦,干扰作用弱。
本发明的目的是开发基于天然基质的其它珠光颜料,其将显示云母颜料的熟知优点(例如在各种基料体系中的良好施涂性能和环境相容性并且处理简单),同时具有实现优秀光学效果的可能性,即提供基于天然基质的具有高色强度和/或色纯度的干扰颜料。
所述目的已通过包含片状珍珠岩基质和(a)介电材料,尤其是具有高折光指数的金属氧化物;和/或(a)金属层,尤其是薄半透明金属层的颜料解决。
颜料粒子的长度通常为2μm-5mm,宽度为2μm-2mm,平均厚度为<4μm,长度与厚度之比为至少5∶1,且含具有两个基本平行面的珍珠岩芯,面之间的距离为芯的最短轴。珍珠岩芯涂覆有介电材料,尤其是具有高折光指数的金属氧化物,或金属层,尤其是薄半透明金属层。所述层可以涂覆有其它层。
适于(半透明)金属层的金属例如为Cr、Ti、Mo、W、Al、Cu、Ag、Au或Ni。半透明金属层的厚度通常为5-25nm,尤其是5-15nm。
根据本发明,术语“铝”包括铝和铝的合金。铝合金例如描述于G.Wassermann in Ullmanns der lndustriellen Chemie,4.Aufiage,Verlag Chemie,Weinheim,Band 7,S.281-292中。尤其适合的有描述于WO00/12634第10-12页中的腐蚀稳定性的铝合金,其除铝外,还包含量小于20重量%,优选小于10重量%的硅、镁、锰、铜、锌、镍、钒、铅、锑、锡、镉、铋、钛、铬和/或铁。
金属层可通过湿化学涂覆或通过化学气相沉积,例如羰基金属的气相沉积而得到。基质在金属化合物的存在下悬浮于含介质的水性和/或有机溶剂中并通过加入还原剂沉积在基质上。金属化合物例如为硝酸银或乙酰丙酮镍(WO03/37993)。
根据US-B-3,536,520,氯化镍可用作金属化合物且次磷酸盐可用作还原剂。根据EP-A-353544,如下化合物可用作湿化学涂覆的还原剂:醛(甲醛、乙醛、苯甲醛),酮(丙酮),碳酸及其盐(酒石酸、抗坏血酸),还原酮(异抗坏血酸、丙糖还原酮、还原酸)和还原糖(葡萄糖)。然而,也可使用还原醇(烯丙醇)、多元醇和多酚、亚硫酸盐、亚硫酸氢盐、连二亚硫酸盐、次磷酸盐、肼、硼氮化合物、金属氢化物以及铝和硼的配位氢化物。金属层的沉积还可借助CVD方法进行。这种方法为已知的。为此,优选使用流化床反应器。EP-A-0741170描述了通过在惰性气体料流中使用烃还原烷基铝化合物而使铝层沉积。金属层还可通过相应羰基金属在可加热流化床反应器中气相分解而沉积,如EP-A-045851所述。关于此方法的其它详情在WO93/12182中给出。在此情况下可用于将金属层施用在基质上的沉积薄金属层的其它方法为对于金属在高真空中气相沉积已知的方法。它详细描述于Vakuum-Beschichtung[Vacuum Coating],第1-5卷;编者Frey、Kienel和 VDI-Verlag,1995中。在溅射方法中,气体排料(等离子体)在载体与片状(靶)涂料之间着火。涂料用来自等离子体的高能离子如氩离子冲击并因此除去或雾化(atomised)。雾化涂料的原子或分子沉淀在载体上并形成所需薄层。溅射方法描述于Vakuum-Beschichtung[Vacuum Coating], 第1-5卷;编者Frey、Kienel和 VDI-Verlag,1995中。就室外应用而言,特别是在车辆漆料中的应用中,颜料可具有其它气候稳定性保护层,所谓后涂层,其同时实现最适应于基料体系。这种后涂层已例如描述于EP-A-0268918和EP-A-0632109中。
如果需要具有金属外观的颜料,则金属层的厚度为>25nm至100nm,优选30-50nm。如果需要具有着色金属效果的颜料,则可使其它着色或无色金属氧化物、金属氮化物、金属硫化物和/或金属层沉积。这些层为透明或半透明的。优选具有高折光指数的层与具有低折光指数的层交替或存在一层,其中折光指数在该层内逐渐改变。耐气候性可通过其它涂层提高,其同时导致最佳适应于基料体系(EP-A-268918和EP-A-632109)。
如WO06/131472所述,可将涂覆有珍珠岩片的金属和/或金属氧化物用等离子炬处理。该处理例如促进均匀结晶度和/或涂料稠化。某些粒子快速熔融和固化可提供与金属和/或金属氧化物涂层相关的增强性能如隔离性能、粘合性能和晶体表面形成。在反应区中的短停留时间使得快速处理。另外,可调整加工条件以选择性熔融和再固化且使粒子表面和近表面结晶。此外,可实现表面变平,这产生具有最小缺陷的均匀表面。这尤其可有助于避免粒子附聚。
本方法包括:
(A)提供涂覆的珍珠岩片,
(B)将所述涂覆的珍珠岩片夹带到气体料流中以输送至等离子炬;
(C)在所述气体料流中产生等离子体以加热涂覆的珍珠岩片的外表面;
(D)使所述涂覆的珍珠岩片冷却;和
(E)收集所述涂覆的珍珠岩片。
等离子炬优选感应等离子炬。优选用于本发明方法中的感应等离子炬可由Tekna Plasma Systems,Inc.of Sherbrooke,Quebec,Canada.Boulos等,US-A-5,200,595得到,在此将其关于等离子感应炬的构造和操作的教导引入作为参考。
在本发明一个优选实施方案中,颜料在珍珠岩基质上包含:
(a)介电层,
(b)金属层,和
(c)介电层。这种颜料具有高红外反射率和高可见透射。
优选,金属银用作金属层,这是由于它提供对红外辐射的高反射率以及对太阳辐射的高透射,条件是使它的反射损失最小化。尽管优选高纯度金属银膜,但可容许某些杂质和/或合金金属,只要它们不显著降低红外反射率或显著提高可见光吸光系数。金属银层的厚度为3-20nm。
适于层(c)的材料为以所用厚度对太阳和红外辐射为透过的材料。另外,这些材料用作抗反射涂层以使银层对可见光的发射最小,且这些材料优选具有高折光指数。一些适于层(c)的材料包括,但不限于二氧化钛、二氧化硅、一氧化硅、铋氧化物、锡氧化物、铟氧化物、铬氧化物、硫化锌和氟化镁。由于二氧化钛的高折光指数以及由于已发现它具有与银的最小相互扩散,二氧化钛为优选的材料。
适于层(a)的材料为透明材料,其与层(b)合作以使银层对可见光反射的损失最小化。适于层(c)的透明材料也适于层(a),二氧化钛也为用于此层的优选材料。层(a)可由与层(c)相同的材料形成,或在它可能具有不同厚度的情况下由不同的材料形成。
选择层(c)和层(a)的厚度以使太阳光透射和红外反射率最大。已发现约15-约50nm的厚度适于层(c)。然后层(a)的厚度基于大量考虑而选择,例如是否需要实现最佳太阳光透射,透射与热反射率的最佳比或这些最佳值之间的一些组合。
在大多数情况下,所需光学性能可通过选择约15-约50nm的层厚度而实现。
在本发明一个优选实施方案中,干扰颜料包含具有“高”折光指数的材料,在这里“高”折光指数定义为大于约1.65的折光指数,和任选具有“低”折光指数的材料,这里“低”折光指数定义为约1.65或更小的折光指数。可使用的各种(介电)材料包括无机材料如金属氧化物、金属低氧化物、金属氟化物、金属卤氧化物、金属硫化物、金属硫属元素化物、金属氮化物、金属氧氮化物、金属碳化物、其组合等,以及有机介电材料。这 些材料可容易得到且易于通过物理或化学气相沉积方法,或通过湿化学涂覆方法施用。
任选SiO2层可放在珍珠岩基质与具有“高”折光指数的材料之间。通过将SiO2层施用在珍珠岩基质上,保护珍珠岩表面以防化学变化,例如珍珠岩组分溶胀或浸出。SiO2层的厚度为5-200nm,尤其是20-150nm。SiO2层优选通过使用有机硅烷化合物如四乙氧基硅烷(TEOS)制备。SiO2层可由薄(厚度1-20nm)Al2O3、Fe2O3或ZrO2层代替。
此外,如EP-A-0982376所述,SiO2涂覆或TiO2涂覆的珍珠岩片可涂覆有氮掺杂的碳层。EP-A-0982376所述方法包括如下步骤:
(a)将SiO2或TiO2涂覆的珍珠岩片悬浮在液体中,
(b)如果合适,加入表面改性剂和/或聚合催化剂,
(c)在步骤(b)以前或以后,加入一种或多种包含氮和碳原子的聚合物,或一种或多种能形成这种聚合物的单体,
(d)在该片的表面上形成聚合涂层,
(e)分离涂覆的片,和
(f)将涂覆的片在气体气氛中加热至100-600℃。
聚合物可以为聚吡咯、聚酰胺、聚苯胺、聚氨酯、丁腈橡胶或三聚氰胺-甲醛树脂,优选聚丙烯腈,或单体为吡咯衍生物、丙烯腈、甲基丙烯腈、巴豆腈、丙烯酰胺、甲基丙烯酰胺或巴豆酰胺,优选丙烯腈、甲基丙烯腈或巴豆腈,最优选丙烯腈。
优选在步骤(f)中将片首先在含氧气氛中加热至100-300℃,然后在惰性气体气氛中加热至200-600℃。
因此,本发明还涉及基于本发明珍珠岩片的颜料,其在硅氧化物或钛氧化物涂覆的珍珠岩片整个表面上包含由50-95重量%碳、5-25重量%氮和0-25重量%元素氢、氧和/或硫组成的层,其中重量百分数数据涉及该层(PAN)的总重量。
氮掺杂的碳层的厚度通常为10-150nm,优选30-70nm。在所述实施方案中,优选的颜料具有如下层结构:珍珠岩基质/TiO2/PAN、珍珠岩基质/TiO2/PAN/TiO2、珍珠岩基质/TiO2/PAN/SiO2/PAN。
在一个尤其优选的实施方案中,基于珍珠岩基质的干扰颜料包含具有“高”折光指数,即折光指数大于约1.65,优选大于约2.0,最优选大于约2.2的介电材料层,将其施用在珍珠岩基质整个表面上。这种介电材料的实例为硫化锌(ZnS)、氧化锌(ZnO)、氧化锆(ZrO2)、二氧化钛(TiO2)、碳、氧化铟(In2O3)、氧化铟锡(ITO)、五氧化钽(Ta2O5)、氧化铬(Cr2O3)、氧化铈(CeO2)、氧化钇(Y2O3)、氧化铕(Eu2O3)、铁氧化物如氧化铁(II)/铁(III)(Fe3O4)和氧化铁(III)(Fe2O3)、氮化铪(HfN)、碳化铪(HfC)、氧化铪(HfO2)、氧化镧(La2O3)、氧化镁(MgO)、氧化钕(Nd2O3)、氧化镨(Pr6O11)、氧化钐(Sm2O3)、三氧化锑(Sb2O3)、一氧化硅(SiO)、三氧化硒(Se2O3)、氧化锡(SnO2)、三氧化钨(WO3)或其组合。介电材料优选金属氧化物。金属氧化物可以为具有或不具有吸收性能的单一氧化物或氧化物的混合物,例如TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,其中尤其优选TiO2。
可通过在TiO2层顶上施用具有低折光指数的金属氧化物如SiO2、Al2O3、AlOOH、B2O3或其混合物,优选SiO2,并任选在后者层顶上施用另外TiO2层而得到色彩更强且更透明的颜料(EP-A-892832、EP-A-753545、WO93/08237、WO98/53011、WO9812266、WO9838254、WO99/20695、WO00/42111和EP-A-1213330)。可使用的适合的低折光指数介电材料的非限定性实例包括二氧化硅(SiO2)、氧化铝(Al2O3),和金属氟化物如氟化镁(MgF2)、氟化铝(AlF3)、氟化铈(CeF3)、氟化镧(LaF3)、氟化钠铝(如Na3AlF6或Na5Al3F14)、氟化钕(NdF3)、氟化钐(SmF3)、氟化钡(BaF2)、氟化钙(CaF2)、氟化锂(LiF)、其组合,或折光指数为约1.65或更小的任何其它低指数材料。例如,有机单体和聚合物可用作低指数材料,包括二烯或链烯如丙烯酸酯类(例如甲基丙烯酸酯)、全氟链烯的聚合物、聚四氟乙烯(TEFLON)、氟化乙烯丙烯聚合物(FEP)、聚对亚苯基二甲基、对二甲苯、其组合等。另外,上述材料包括蒸发、浓缩和交联的透明丙烯酸酯层,其可通过US-B-5,877,895所述方法沉积,在此将其公开内容引入作为参考。
因此,除(a)高折光指数的金属氧化物外,优选的干扰颜料另外包含(b)低折光指数的金属氧化物,其中折光指数差为至少0.1。
以指定顺序特别优选已通过湿化学方法涂覆的基于珍珠岩基质的颜 料:TiO2、(SnO2)TiO2(基质:珍珠岩;层:(SnO2)TiO2,优选金红石改性)、低氧化钛、TiO2/低氧化钛、Fe2O3、Fe3O4、TiFe2O5、Cr2O3、ZrO2、Sn(Sb)O2、BiOCl、Al2O3、Ce2S3、MoS2、Fe2O3·TiO2(基质:珍珠岩,Fe2O3和TiO2的混合层)、TiO2/Fe2O3(基质:珍珠岩;第一层:TiO2;第二层:Fe2O3)、TiO2/柏林蓝、TiO2/Cr2O3或TiO2/FeTiO3。通常,层厚度为1-1000nm,优选1-300nm。
在另一个特别优选实施方案中,本发明涉及含至少三层高与低折光指数的交替层如TiO2/SiO2/TiO2、(SnO2)TiO2/SiO2/TiO2、TiO2/SiO2/TiO2/SiO2/TiO2、Fe2O3/SiO2/TiO2或TiO2/SiO2/Fe2O3的干扰颜料。
优选层结构如下:
(a)折光指数为>1.65的涂层,
(b)折光指数为≤1.65的涂层,
(c)折光指数为>1.65的涂层,和
(d)任选外部保护层。
在基体基质上的各个具有高和低折光指数的层的厚度对于颜料的光学性能而言为重要的。各个层,尤其是金属氧化物层的厚度取决于使用领域,并且通常为10-1000nm,优选15-800nm,特别是20-600nm。
层(A)的厚度为10-550nm,优选15-400nm,特别是20-350nm。层(B)的厚度为10-1000nm,优选20-800nm,特别是30-600nm。层(C)的厚度为10-550nm,优选15-400nm,特别是20-350nm。
特别适于层(A)的材料为金属氧化物、金属硫化物或金属氧化物混合物,例如TiO2、Fe2O3、TiFe2O5、Fe3O4、BiOCl、CoO、Co3O4、Cr2O3、VO2、V2O3、Sn(Sb)O2、SnO2、ZrO2、钛酸铁,铁氧化物水合物、低氧化钛(氧化态为2至<4的还原钛属)、钒酸铋、铝酸钴,以及这些化合物相互之间的混合物或混合相或与其它金属氧化物的混合物或混合相。金属硫化物涂层优选选自锡、银、镧、稀土金属,优选铈、铬、钼、钨、铁、钴和/或镍的硫化物。
特别适于层(B)的材料为金属氧化物或相应的氧化物水合物,例如 SiO2、MgF2、Al2O3、AlOOH、B2O3或其混合物,优选SiO2。
特别适于层(C)的材料为为无色或有色金属氧化物如TiO2、Fe2O3、TiFe2O5、Fe3O4、BiOCl、CoO、Co3O4、Cr2O3、VO2、V2O3、Sn(Sb)O2、SnO2、ZrO2、钛酸铁,铁氧化物水合物、低氧化钛(氧化态为2至<4的还原钛属)、钒酸铋、铝酸钴,以及这些化合物相互之间的混合物或混合相或与其它金属氧化物的混合物或混合相。TiO2层可另外含吸收性材料如碳,选择性吸收性着色剂、选择性吸收性金属阳离子,可涂覆有吸收性材料或可被部分还原。
吸收性或非吸收性材料的夹层可存在于(A)、(B)、(C)和(D)层之间。夹层的厚度为1-50nm,优选1-40nm,特别是1-30nm。这种夹层可例如由SnO2组成。可通过加入少量SnO2强制形成金红石结构(例如见WO93/08237)。
在此实施方案中,优选的干扰颜料具有如下层结构:
珍珠岩 | TiO2 | SiO2 | TiO2 |
珍珠岩 | TiO2 | SiO2 | Fe2O3 |
珍珠岩 | TiO2 | SiO2 | TiO2·Fe2O3 |
珍珠岩 | TiO2 | SiO2 | (Sn,Sb)O2 |
珍珠岩 | (Sn,Sb)O2 | SiO2 | TiO2 |
珍珠岩 | Fe2O3 | SiO2 | (Sn,Sb)O2 |
珍珠岩 | TiO2·Fe2O3 | SiO2 | TiO2·Fe2O3 |
珍珠岩 | TiO2 | SiO2 | MoS2 |
珍珠岩 | TiO2 | SiO2 | Cr2O3 |
珍珠岩 | Cr2O3 | SiO2 | TiO2 |
珍珠岩 | Fe2O3 | SiO2 | TiO2 |
珍珠岩 | TiO2 | Al2O3 | TiO2 |
珍珠岩 | Fe2TiO5 | SiO2 | TiO2 |
珍珠岩 | TiO2 | SiO2 | Fe2TiO5/TiO2 |
珍珠岩 | TiO低氧化物 | SiO2 | TiO低氧化物 |
珍珠岩 | TiO2 | SiO2 | TiO2/SiO2/TiO2+普鲁士蓝 |
珍珠岩 | TiO2 | SiO2 | TiO2/SiO2/TiO2 |
珍珠岩 | TiO2/SiO2/TiO2 | SiO2 | TiO2/SiO2/TiO2 |
金属氧化物层可通过CVD(化学气相沉积)或通过湿化学涂覆而施涂。金属氧化物层可通过羰基金属在水蒸气的存在下分解得到(相对于低分子量金属氧化物如磁铁矿)或在氧气和如果合适水蒸气的存在下分解而得到(例如镍氧化物和钴氧化物)。金属氧化物层优选通过羰基金属(如五羰基铁、六羰基铬;EP-A-45851)氧化气相分解,通过金属醇化物(如四正-和-异丙醇钛和锆;DE-A-4140900)或金属卤化物(如四氯化钛;EP-A-338428水解气相分解,通过有机锡化合物(尤其是烷基锡化合物如四丁基锡和四甲基锡;DE-A-4403678)氧化分解或通过EP-A-668329所述有机硅化合物(尤其是二叔丁氧基乙酰氧基硅烷)气相水解而施用,其中涂覆操作可在流化床反应器中进行(EP-A-045851和EP-A-106235)。Al2O3层(B)可有利地通过在铝涂覆的颜料冷却期间的受控氧化而得到,其另外在惰性气体下进行(DE-A-19516181)。
含磷酸盐、含铬酸盐和/或含钒酸盐以及含磷酸盐和含SiO2的金属氧化物层可根据DE-A-4236332和EP-A-678561所述钝化方法通过金属氧化物-卤化物(例如CrO2Cl2,VOCl3),尤其是卤氧化磷(例如POCl3)、磷酸和磷酸酯(例如亚磷酸二-和三甲基和二-和三乙基酯),和含氨基的有机硅化合物(例如3-氨基丙基-三乙氧基-和-三甲氧基硅烷)的水解或氧化气相分解施涂。
金属锆、钛、铁和锌的氧化物,那些金属的氧化物水合物、钛酸铁、低氧化钛或其混合物的层优选通过湿化学方法沉淀而施用,其中如果合适,可将金属氧化物还原。在湿化学涂覆的情况下,可使用对于制备珠光颜料所开发的湿化学涂覆方法;这些例如描述于DE-A-1467468、DE-A-1959988、DE-A-2009566、DE-A-2214545、DE-A-2215191、DE-A-2244298、DE-A-2313331、DE-A-2522572、DE-A-3137808、DE-A-3137809、DE-A-3151343、DE-A-3151354、DE-A-3151355、DE-A-3211602和DE-A-3235017、DE 1959988、WO 93/08237、WO 98/53001和WO03/6558中。
高折光指数的金属氧化物优选TiO2和/或铁氧化物,低折光指数的金属氧化物优选SiO2。TiO2层可以为金红石或锐钛矿改性,其中优选金红石改性。TiO2层也可通过已知方式,例如通过氨、氢气、烃蒸气或其混合物,或通过金属粉末还原,如EP-A-735,114,DE-A-3433657,DE-A-4125134、EP-A-332071、EP-A-707,050、WO93/19131或WO06/131472所述。
就涂覆而言,将基质粒子悬浮于水中并在适于水解的pH下加入一种或多种可水解金属盐,其选择使得金属氧化物或金属氧化物水合物直接沉淀在粒子上而不发生辅助沉淀。pH通常通过同时计量加入碱而保持恒定。然后将颜料分离、洗涤、干燥并如果合适,煅烧,其中可相对于所述涂覆使煅烧温度最佳。如果需要,在已施涂各个涂层以后,可将颜料分离、干燥并如果合适,煅烧,然后再次再悬浮以沉淀其它层。
金属氧化物层也可例如以类似于DE-A-19501307所述方法,通过通过如果合适在有机溶剂和碱性催化剂的存在下受控水解一种或多种金属酸酯制备金属氧化物层,以溶胶-凝胶方法得到。适合的碱性催化剂例如为胺如三乙胺、乙二胺、三丁基胺、二甲基乙醇胺和甲氧基丙基胺。有机溶剂为水溶混性有机溶剂如C1-4醇,尤其例如异丙醇。
适合的金属酸酯选自钒、钛、锆、硅、铝和硼的烷基和芳基醇化物、羧酸酯,和羧基-或烷基-或芳基取代的烷基醇化物或羧酸酯。优选使用铝酸三异丙基酯、钛酸四异丙基酯、锆酸四异丙基酯、原硅酸四乙基酯和硼酸三乙基酯。另外,可使用上述金属的乙酰丙酮化物和乙酰乙酰丙酮化物。这种金属酸酯的优选实例为乙酰丙酮锆、乙酰丙酮铝、乙酰丙酮钛和乙酰乙酰铝酸二异丁基油基酯或乙酰乙酰丙酮二异丙基油基酯和金属酸酯的混合物,例如 (Hüls),混合铝/硅金属酸酯。
作为具有高折光指数的金属氧化物,优选使用二氧化钛,其中根据本发明实施方案,US-B-3,553,001所述方法用于施涂二氧化钛层。
将钛盐水溶液缓慢加入待涂覆材料的悬浮液中,其中已将悬浮液加热至约50-100℃,尤其是70-80℃,并通过同时计量加入碱如氨水溶液或碱金属氢氧化物水溶液保持约0.5-5,尤其是约1.2-2.5的基本恒定的pH值。一达到沉淀TiO2层的所需厚度,就停止加入钛盐溶液和碱。将Al2O3或 MgO前体加入起始溶液为改善TiO2层的形态的一种方式。
此方法,也称作“滴定法”的特征在于避免过量钛盐这一事实。这通过每单位时间供入恰好用水合TiO2均匀涂覆所需的且可通过被涂覆粒子可得表面每单位时间吸收的量用于水解而实现。原则上,TiO2的锐钛矿形式在起始颜料的表面上形成。然而,通过加入少量SnO2,可强制形成金红石结构。例如如WO 93/08237所述,二氧化锡可在二氧化钛沉淀以前沉积并且涂覆有二氧化钛的产物可在800-900℃下煅烧。
在尤其优选的本发明实施方案中,将珍珠岩片在密闭反应器中与蒸馏水混合并在约90℃下加热。将pH设定为约1.8-2.2,并缓慢加入包含TiOCl2、HCl、甘氨酸和蒸馏水的制剂,同时通过连续加入1M NaOH溶液将pH保持恒定(1.8-2.2)。参考欧洲专利申请PCT/EP2008/051910。通过在TiO2沉积期间加入氨基酸如甘氨酸,可改善待形成的TiO2涂层质量。有利的是,将包含TiOCl2、HCl和甘氨酸和蒸馏水的制剂加入在水中的基质片中。
TiO2可任选通过常用程序还原:US-B-4,948,631(NH3,750-850℃),WO93/19131(H2,>900℃)或DE-A-19843014(固体还原剂如硅,>600℃)。
如果合适,可将SiO2(保护)层施用在二氧化钛顶上,为此可使用如下方法:将苏打水玻璃溶液计量加入被涂覆的材料的悬浮液中,其中此悬浮液已经加热至约50-100℃,尤其是70-80℃。通过同时加入10%盐酸将pH保持在4-10,优选6.5-8.5。在加入水玻璃溶液以后,进行搅拌30分钟。
可通过在TiO2层顶上施涂“低”折光指数,即折光指数小于约1.65的金属氧化物如SiO2,Al2O3,AlOOH,B2O3或其混合物,优选SiO2,并将另外Fe2O3和/或TiO2层施用在后者层顶上而得到色彩更强且更透明的颜料,这种包含珍珠岩基质和交替的高和低折光指数的金属氧化层的多层涂覆的干扰颜料可类似于WO98/53011和WO99/20695所述方法制备。
另外,可通过施用其它层如有色金属氧化物或柏林蓝、过渡金属如Fe、Cu、Ni、Co、Cr的化合物,或有机化合物如染料或色淀改进颜料的粉末色彩。
另外,本发明颜料也可涂覆有溶解性弱的稳固粘附的无机或有机着色 剂。优选使用色淀,尤其是铝色淀。为此,将氢氧化铝层沉淀,其中在第二个步骤中通过使用色淀将其色淀(DE-A-2429762和DE-A-2928287)。
此外,本发明颜料也可具有有配盐颜料,尤其是具有有氰基高铁酸盐配合物的其它涂层(EP-A-141173和DE-A-2313332)。
为增强气候和光稳定性,可取决于应用领域使(多层)珍珠岩片经受表面处理。有用的表面处理例如描述于DE-A-2215191、DE-A-3151354、DE-A-3235017、DE-A-3334598、DE-A-4030727、EP-A-649886、WO97/29059、WO99/57204和US-A-5,759,255中。所述表明处理也可促进颜料的处理,尤其是将它掺入各种施用介质中。
在一个优选实施方案中,本发明涉及含珍珠岩芯且包含Al2O3/TiO2混合层的颜料。该混合层可含至多20摩尔%Al2O3。Al2O3/TiO2混合层通过将铝和钛盐水溶液缓慢加入被涂覆的材料的悬浮液中,其中该悬浮液已经加热至约50-100℃,尤其是70-80℃,并通过同时计量加入碱如氨水溶液或碱金属氢氧化物水溶液而保持约0.5-5,尤其是约1.2-2.5的基本恒定pH值。一达到沉淀的Al2O3/TiO2的所需层厚度,就停止加入钛和铝盐溶液和碱。
Al2O3/TiO2混合层的厚度通常为20-200nm,尤其是50-150nm。优选颜料包含在Al2O3/TiO2混合层顶上的厚度为1-50nm,尤其是10-20nm的TiO2层。通过改变Al2O3/TiO2混合层的厚度,可按照需要增强和控制颜色的随角异色性。
在另一个优选实施方案中,本发明涉及含珍珠岩芯且由随后的TiO2/SnO2/TiO2层组成的颜料,其中紧接于珍珠岩基质的TiO2层的厚度为1-20nm,且优选通过使用醇化钛,尤其是钛酸四异丙基酯制备。
本发明颜料的微片状基质(芯)由珍珠岩组成。
珍珠岩为通常含约72-75%SiO2、12-14%Al2O3、0.5-2%Fe2O3、3-5%Na2O、4-5%K2O、0.4-1.5%CaO(以重量计)和小浓度其它金属元素的水合天然玻璃。珍珠岩与其它天然玻璃的区别在于更高的化学结合水含量(2-10重量%),玻璃质珍珠光泽的存在和典型同心或弓形洋葱皮状(即珍珠状)纹理。珍珠岩片可通过WO02/11882公开的方法制备,其可包括研磨、筛分 和热膨胀。优选具有受控粒度分布、低漂浮物含量和高蓝光亮度的珍珠岩片。优选具有小于50微米的中值粒度的珍珠岩片。优选具有15-50微米的中值粒度的珍珠岩片,最优选具有20-40微米的中值粒度的珍珠岩片。珍珠岩片的漂浮物含量小于10体积%;尤其是漂浮物含量小于5体积%;非常尤其是漂浮物含量小于2体积%。珍珠岩片的蓝光亮度大于80;尤其是大于82,非常尤其是大于85。
用于本发明中的珍珠岩片不是均匀形状。然而,为了简便,将珍珠岩片称作具有“直径”。珍珠岩片的平均厚度为<2μm,尤其是200-1000nm,尤其是200-600nm。目前优选片的直径(中值粒度(d50))优选约15-50μm,更优选约20-40μm。如果TiO2层作为高折光指数的材料沉积,则TiO2层的厚度为20-300nm,尤其是20-100nm,更尤其是20-50nm。
珍珠岩的Fe2O3含量优选低于2%,尤其是0%。
目前最优选的珍珠岩为OptimatTM 2550(World Minerals)。若通过沉降或离心除去粒度低于10μm的粒子,则也可使用珍珠岩,如OptimatTM1735(World Minerals)。
如果使用本发明珍珠岩基质,则可得到具有极好亮度、清晰(clear)且强烈色彩、强色彩动感、改善的色强度和/或色纯度的干扰颜料。
金属或非金属无机微片型粒子或颜料为效果颜料(尤其是金属效果颜料或干扰颜料),即,除赋予应用介质色彩外,还赋予其它性能如色彩的角度相关性(随角异色性)、光泽(非表面光泽)或纹理的颜料。在金属效果颜料上,在定向取向颜料粒子发生基本定向反射。在干扰颜料的情况下,赋予色彩的效果是由于薄的高度折射层的光的干扰现象。
本发明(效果)颜料可用于所有常规目的,例如用于使整块聚合物、涂料(包括效果修饰,包括汽车领域的那些)和印刷油墨(包括胶版印刷、凹版印刷、擦金印刷和苯胺印刷)的着色,以及例如用于化妆品应用,喷墨印刷,染色织物,陶瓷和玻璃的釉料以及纸和塑料的激光标示。这种应用由参考著作获知,如“Industrielle Organische Pigmente”(W.Herbst和K.Hunger,VCH Verlagsgesellschaft mbH,Weinheim/New York,第2版,完整修订版,1995)。
当本发明颜料为干扰颜料(效果颜料)时,它们可以为角异色的的并产生明亮的高度饱和(灿烂的)色。因此,它们非常尤其适于与常规透明颜料,例如有机颜料如二酮基吡咯并吡咯、喹吖啶酮、二噁嗪、苝、异吲哚啉酮等组合,其中透明颜料可具有与效果颜料近似的色彩。然而,类似于例如EP-A-388932或EP-A-402943,当透明颜料的色彩与效果颜料的色彩互补时,得到尤其有意义的组合效果。
本发明颜料可以以极好结果用于使高分子量有机材料着色。
本发明颜料或颜料组合物可用于其染色的高分子量有机材料可以为天然或合成来源的。高分子量有机材料的分子量通常为103-108g/摩尔或甚至更高。它们可例如为天然树脂、干性油、橡胶或干酪素,或由其衍生的天然物质,例如氯化橡胶、油改性的醇酸树脂、粘胶、纤维素醚或酯,例如乙基纤维素、乙酸纤维素、丙酸纤维素、乙酰丁酸纤维素或硝化纤维,但尤其是全体合成的如通过聚合、缩聚或加聚得到的有机聚合物(热固性塑料和热塑性塑料)。聚合树脂类中可尤其提到聚烯烃如聚乙烯、聚丙烯或聚异丁烯,以及取代聚烯烃如氯乙烯、乙酸乙烯酯、苯乙烯、丙烯腈、丙烯酸酯、甲基丙烯酸酯或丁二烯的聚合产物,以及所述单体的共聚产物,尤其例如ABS或EVA。
在一系列加聚树脂和缩聚树脂中,可例如提到甲醛与酚的缩合产物,所谓酚醛塑料(phenoplasts),和甲醛与脲、硫脲或三聚氰胺的缩合产物,所谓氨基塑料,和用作表面涂覆树脂的聚酯,或饱和的,如醇酸树脂,或不饱和的,如马来酸酯树脂;以及线性聚酯和聚酰胺、聚氨酯或聚硅氧烷。
所述高分子量化合物可以单独或以混合物,以塑料块或熔体形式存在。它们也可以以它们的单体的形式或以聚合态以溶解形式作为涂料或印刷油墨的成膜剂或基料存在,例如煮沸亚麻籽油、硝化纤维、醇酸树脂、三聚氰胺树脂和脲-甲醛树脂或丙烯酸树脂。
取决于意欲目的,已证明有利的是作为调色剂或以制剂的形式使用本发明效果颜料或效果颜料组合物。取决于调节方法或意欲应用,可有利地将一定量纹理改善剂(texture-improving agent)在调节处理以前或以后加入效果颜料中,条件是这对效果颜料在使高分子量有机材料着色,尤其是使 聚乙烯着色中的使用不具有不利影响。适合的试剂尤其是含至少18个碳原子的脂肪酸如硬脂酸或山萮酸,或其酰胺或金属盐,尤其是镁盐,以及增塑剂、蜡、树脂酸如松香酸、松香皂,烷基酚或脂族醇,例如硬脂醇,或含8-22个碳原子的脂族1,2-二羟基化合物,例如1,2-十二烷二醇,以及改性松香马来酸酯树脂或富马酸松香树脂。纹理改善剂以基于最终产物优选0.1-30重量%,尤其是2-15重量%的量加入。
本发明(效果)颜料可以以任何着色有效量加入要染色的高分子有机材料中。包含高分子量有机材料和基于高分子量有机材料0.01-80重量%,优选0.1-30重量%本发明颜料的着色的物质组合物为有利的。实践中通常使用1-20重量%,尤其是约10重量%的浓度。
高浓度,例如高于30重量%的那些通常为浓缩物(“母料”)的形式,其可用作制备具有相对低颜料含量的着色的材料的着色剂,常规配制剂中本发明颜料具有格外低的粘度使得它们仍然可良好加工。
为使有机材料着色,可单独使用本发明效果颜料。然而,为实现不同色调或色彩效果,除本发明效果颜料外,也可将任何所需量的其它赋予色彩的组分,例如白色、彩色、黑色或效果颜料加入高分子量有机物质中。当彩色颜料以与本发明效果颜料的混合物使用时,总量基于高分子量有机材料优选为0.1-10重量%。尤其高角异色性由本发明效果颜料与其它颜色的,尤其是互补色的有色颜料的优选组合提供,其中使用效果颜料的着色和使用有色颜料的着色在10°的测量角下具有20-340,尤其是150-210的色调差(ΔH*)。
优选,本发明效果颜料与透明有色颜料组合,其中透明有色颜料可以与本发明效果颜料存在于相同的介质中或存在于邻近的介质中。效果颜料和有色颜料有利地存在于邻近介质中的安排的实例为多层效果涂料。
用本发明颜料使高分子量有机物质着色例如通过使用辊磨机或混合或研磨设备将这种颜料,如果合适以母料形式,与基质混合而进行。然后使用本身已知方法如砑光、压模、挤出、涂覆、铸型或注塑使着色的材料成为所需最终形式。可将塑料工业中任何常规添加剂如增塑剂、填料或稳定剂以常规量在掺入颜料之前或之后加入聚合物中。特别是,为制备非硬质 成型制品或降低它们的脆性,需要将增塑剂,例如磷酸、邻苯二甲酸或癸二酸的酯在成型以前加入高分子量化合物中。
为了使涂料和印刷油墨着色,将高分子量有机材料和本发明效果颜料,如果合适与常规添加剂如填料、其它颜料、摧干剂或增塑剂一起精细分散或溶于相同有机溶剂或溶剂混合物中,其中可以各个组分分别溶解或分散或可以大量组分一起溶解或分散,并且仅在此后将所有组分放在一起。
将本发明效果颜料分散在要着色的高分子量有机材料中和加工本发明颜料组合物优选在仅发生相对弱剪切力的条件下进行使得效果颜料不会分裂成更小部分。
塑料包含量为0.1-50重量%,特别是0.5-7重量%的本发明颜料。在涂料领域中,本发明颜料以0.1-10重量%的量使用。在基料体系的染色中,例如对于漆料和用于凹版、胶版或丝网印刷的印刷油墨,颜料以0.1-50重量%,优选5-30重量%,特别是8-15重量%的量掺入印刷油墨中。
例如在塑料、涂料或印刷油墨中,尤其是在涂料或印刷油墨中,更尤其是在涂料中,得到的着色的特征可在于极好的性能,尤其是极好的高饱和度、显著的牢固性能、高色纯度和高角异色性。
当要染色的高分子量材料是涂料时,它尤其是特种涂料,非常尤其是汽车涂饰剂。
本发明效果颜料还适于唇部或皮肤化妆以及头发或指甲着色。
因此,本发明还涉及基于化妆品制剂或配制剂包含0.0001-90重量%本发明颜料,尤其是本发明效果颜料和10-99.9999%化妆品适用的载体材料的化妆品制剂或配制剂。
这种化妆品制剂或配制剂例如为唇膏、胭脂、粉底、指甲油和洗发剂。
颜料可单独使用或以混合物的形式使用。另外,可与其它颜料和/或着色剂一起,例如以如前文所述或如化妆品制剂中已知的组合使用本发明颜料。
本发明化妆品制剂和配制剂基于该制剂总重量优选含0.005-50重量%的本发明颜料。
适于本发明化妆品制剂和配制剂的载体材料包括用于这种组合物中的 常规材料。
本发明化妆品制剂和配制剂可以例如为棒、膏、霜、乳液、悬浮液、分散体、粉末或溶液的形式。它们例如为唇膏、睫毛膏制剂、胭脂、眼影笔、粉底、眼线笔、粉或指甲油。如果制剂为棒的形式,例如唇膏、眼影笔、胭脂或粉底,则制剂相当大部分由脂肪组分组成,其可以由一种或多种蜡组成,例如地蜡、羊毛脂、羊毛脂醇、氢化羊毛脂、乙酰化羊毛脂、羊毛脂蜡、蜂蜡、小烛树蜡、微晶蜡、巴西棕榈蜡、鲸蜡醇、硬脂醇、可可油、羊毛脂脂肪酸、凡士林、矿脂,在25℃下为固体的单-、二-或三甘油酯或其脂肪酯,聚硅氧烷蜡如甲基十八烷-氧基聚硅氧烷和聚(二甲基甲硅烷氧基)-硬脂氧基硅氧烷,硬脂酸单乙醇胺,松香(colophane)及其衍生物如松香二醇酯和松香甘油酯,在25℃下为固体的氢化油,糖甘油酯和钙、镁、锆和铝的油酸盐、肉豆蔻酸盐、羊毛酸盐(lanolate)、硬脂酸盐和二羟基硬脂酸盐。
脂肪组分也可由至少一种蜡与至少一种油的混合物组成,此时,例如如下油为适合的:石蜡油、鸭子尾脂腺油(purcelline oil)、全氢鲨烯、甜杏仁油、鳄梨油、红厚壳油(calophyllum oil)、蓖麻油、芝麻油、霍霍巴油、沸点为约310-410℃的矿物油,硅油如二甲基聚硅氧烷、亚油基醇、亚麻基醇、油醇、禾谷类油如麦胚芽油、羊毛酸异丙酯(isopropyl lanolate)、棕榈酸异丙酯、肉豆蔻酸异丙酯、肉豆蔻酸丁酯、肉豆蔻酸鲸蜡酯、硬脂酸十六烷基酯、硬脂酸丁酯、油酸癸酯、乙酰基甘油酯、醇和多元醇如二醇和甘油的辛酸酯和癸酸酯、醇和多元醇如鲸蜡醇、异硬脂醇的蓖麻醇酸酯、羊毛酸异鲸蜡酯、己二酸异丙酯、月桂酸己酯和辛基十二烷醇。
这种棒形式的制剂中的脂肪组分可通常占制剂总重量的99.91重量%。
本发明化妆品制剂和配制剂可另外包含其它组分如二醇、聚乙二醇、聚丙二醇、单链烷醇酰胺、未着色的、聚合的、无机的或有机的填料、防腐剂、UV过滤剂或化妆品中常见的其它辅助剂和添加剂,例如天然或合成或部分合成的二-或三甘油酯、矿物油、硅油、蜡、脂肪醇、Guerbet醇或其酯,亲脂性功能化妆品活性成分,包括防晒过滤剂,或这些物质的混合物。
适于皮肤化妆品的亲脂性功能化妆品活性成分、活性成分组合物或活性成分提取物为允许皮肤或局部应用的成分或成分混合物,可例如提到如下:
-对皮肤表面和头发具有清洁作用的活性成分;这些包括用于清洁皮肤的所有物质,例如油、皂、合成清洁剂和固体物质;
-具有除臭和抑制排汗作用的活性成分:它们包括基于铝盐或锌盐的止汗药,包含杀菌或抑菌除臭物质如三氯生(triclosan)、六氯酚(hexachlorophene)、醇和阳离子物质如季铵盐的除臭剂,和气味吸收剂如 (蓖麻醇酸锡与各种添加剂的组合)或柠檬酸三乙酯(任选与抗氧化剂如丁基羟基甲苯组合)或离子交换树脂;
-提供保护以防日光的活性成分(UV过滤剂):适合的活性成分为能吸收日光的UV辐射并将它转化成热的过滤剂物质(防晒剂);取决于所需作用,优选如下光防护剂:选择性吸收约280-315nm的导致晒斑的高能UV辐射(UV-B吸收剂)并透射315-400nm(UV-A范围)的较长波长的光防护剂,以及仅吸收315-400nm的UV-A范围较长波长辐射的光防护剂(UV-A吸收剂);适合的光防护剂例如为如下类的有机UV吸收剂:对氨基苯甲酸衍生物、水杨酸衍生物、二苯甲酮衍生物、二苯甲酰基甲烷衍生物、丙烯酸二苯酯衍生物、苯并呋喃衍生物、包含一个或多个有机硅基团的聚合UV吸收剂、肉桂酸衍生物、樟脑衍生物、三苯胺基-s-三嗪衍生物、苯基-苯并咪唑磺酸及其盐、邻氨基苯甲酸薄荷酯、苯并三唑衍生物,和/或选自氧化铝或二氧化硅涂覆的TiO2、氧化锌或云母的无机微细颜料;
-对抗昆虫的活性成分(拒斥剂)为意欲防止昆虫接触皮肤且在该处变为活性的试剂;它们驱赶昆虫并缓慢蒸发;最通常使用的拒斥剂为二乙基甲苯甲酰胺(DEET);其它常规拒斥剂将例如在“Pflegekosmetik”(W.Raab和U.Kindl,Gustav-Fischer-Verlag Stuttgart/New York,1991),第161页中找到;
-用于保护以防化学和机械影响的活性成分:这些包括在皮肤与外部有害物质之间形成隔离的所有物质,例如用于保护以防水溶液的石蜡油、硅油、植物油、PCL产品和羊毛脂,用于保护以防有机溶剂作用的成膜剂如藻酸钠、三乙醇胺藻酸盐、聚丙烯酸酯、聚乙烯醇或纤维素醚,或基于矿物油、植物油或硅油作为“润滑剂”以保护以防皮肤上严重机械应力的物质;
-增湿物质:例如如下物质用作控水剂(润湿剂):乳酸钠、脲、醇、山梨糖醇、甘油、丙二醇、胶原蛋白、弹性蛋白和透明质酸;
-具有角质软化(keratoplastic)效果的活性成分:过氧化苯甲酰、视黄酸、胶态硫和间苯二酚;
-抗微生物剂,例如三氯生或季铵化合物;
-可皮肤施用的油质或油溶性维生素或维生素衍生物:例如维生素A(游离酸形式的视黄醇或其衍生物)、泛酰醇、泛酸、叶酸及其组合,维生素E(生育酚)、维生素F;必须脂肪酸;或烟酰胺(烟酸酰胺);
-基于维生素的胎盘提取物:尤其包含维生素A、C、E、B1、B2、B6、B12、叶酸和生物素、氨基酸和酶以及痕量元素镁、硅、磷、钙、锰、铁或铜的化合物的活性成分组合物;
-皮肤修复配合物:可由双叉杆菌组(bifidus group)细菌灭活和分裂培养而得到;
-植物和植物提取物:例如山金车花(arnica)、芦荟(aloe)、长松萝(beardlichen)、常春藤(ivy)、荨麻(stinging nettle)、人参(ginseng)、指甲花(henna)、甘菊(camomile)、金盏草(marigold)、迷迭香(rosemary)、鼠尾草(sage)、马尾草(horsetail)或百里香(thyme);
-动物提取物:例如王浆、蜂胶、蛋白质或胸腺提取物;
-可皮肤施用的化妆油:Miglyol 812类型的中性油、杏仁油(apricotkernel oil)、鳄梨油、巴巴苏油、棉籽油、琉璃苣油、蓟油、花生油、γ-米谷醇(gamma-oryzanol)、玫瑰果油(rosehip-seed oil)、大麻油、榛子油、黑茶藨子籽油、霍霍巴油、樱核油、鲑鱼油、亚麻籽油、玉米籽油、欧洲坚果油(macadamia nut oil)、杏仁油(almond oil)、月见草油、貂油、橄榄油、胡桃油、桃仁油、乳香黄连木油、菜油、稻籽油、蓖麻油、红花油、芝麻油、豆油、葵花油、茶树油、葡萄籽油或麦胚芽油。
棒形式的制剂优选无水的,但在一些情况下可包含一定量的水,然而, 水量通常基于化妆品制剂总重量不超过40重量%。
如果本发明化妆品制剂和配制剂为半固体产品形式,即为膏或霜形式,则它们同样可以为无水的或水性的。这种制剂和配制剂例如为睫毛膏、眼线笔、粉底、胭脂、眼影笔,或用于处理眼圈的组合物。
另一方面,如果这种膏或霜为水性的,则它们尤其是除颜料外,包含1-98.8重量%脂肪相、1-98.8重量%水相和0.2-30重量%乳化剂的油包水型或水包油型乳液。
这种膏和霜也可包含其它常规添加剂,例如香料、抗氧化剂、防腐剂、胶凝剂、UV过滤剂、着色剂、颜料、珠光剂、未着色的聚合物以及无机或有机填料。如果制剂为粉末形式,则它们基本上由矿物填料或无机或有机填料如滑石、高岭土、淀粉、聚乙烯粉末或聚酰胺粉末以及辅助剂如粘合剂、着色剂等组成。
同样,这种制剂可包含常规用于化妆品中的各种辅助剂,例如芳香剂、抗氧化剂、防腐剂等。
如果本发明化妆品制剂和配制剂为指甲油、则它们基本上由硝化纤维和在溶剂体系中的溶液形式的天然或合成聚合物组成,其中溶液可包含其它辅助剂如珠光剂。
在该实施方案中,着色的聚合物以约0.1-5重量%的量存在。
本发明化妆品制剂和配制剂也可用于头发着色,此时它们以由常规用于化妆品工业中的基础物质和本发明颜料组成的洗发剂、霜或凝胶的形式使用。本发明化妆品制剂和配制剂以常规方式,例如通过将组分一起混合或搅拌,任选同时加热使得混合物熔融而制备。
本发明的各个特征和方面在以下实施例中进一步阐明。虽然给出这些实施例以向本领域技术人员显示在本发明范围内如何操作,但是它们不用于限制本发明范围,其中本发明范围仅在权利要求中定义。除非另有说明,以下实施例中以及说明书和权利要求中的其它地方中,所有份和百分数以重量计,温度以摄氏度表示,压力在大气压下或接近大气压力下。
实施例
实施例1
将17g OptiMatTM 1735悬浮于去离子水中。使粒子在30分钟期间沉降。除去仍在悬浮液中的粒子。此操作重复5次。
然后将沉降物材料分散在300ml去离子水中并加热至90℃。将悬浮液的pH设定为1.5,并以0.4ml每分钟的速度加入20ml包含9g SnCl4/5H2O、5g 37%HCl、1.00g甘氨酸和100g蒸馏水的溶液,同时连续加入1摩尔(molar)NaOH保持pH恒定。然后将pH设定为1.8并以1ml每分钟的速度加入467ml包含34.00g TiOCl2、32g 37%HCl、5.22g甘氨酸和445g蒸馏水的溶液,同时用1M NaOH将pH保持在1.8。在过滤、干燥并在750℃下在空气中煅烧以后得到13.3g鲜蓝色粉末,其显示对于紫色的随角异色性。通过X射线光谱确定涂层由金红石TiO2组成。
Claims (16)
1.一种颜料,其包含含有珍珠岩芯的珍珠岩片基质,珍珠岩芯具有两个基本平行面,面之间的距离为芯的最短轴,和
(a)具有高折光指数的介电材料层,其中高折光指数定义为大于1.65的折光指数;和/或
(a)厚度为5-25nm的半透明金属层。
2.根据权利要求1的颜料,其中介电材料为金属氧化物。
3.根据权利要求1的颜料,其中所述珍珠岩基质的中值粒度小于50微米。
4.根据权利要求1的颜料,其中所述颜料另外包含(b)低折光指数的金属氧化物,其中折光指数差为至少0.1,其中低折光指数指1.65或更小的折光指数。
5.根据权利要求3的颜料,其中所述颜料另外包含(b)低折光指数的金属氧化物,其中折光指数差为至少0.1,其中低折光指数指1.65或更小的折光指数。
6.根据权利要求4的颜料,其中所述具有高折光指数的金属氧化物为TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3、ZnO或这些氧化物的混合物或钛酸铁、铁氧化物水合物、低氧化钛或这些化合物的混合物和/或混合相。
7.根据权利要求4-6中任一项的颜料,其中所述具有低折光指数的金属氧化物为SiO2、Al2O3、AlOOH、B2O3或其混合物,其中可作为另外组分含碱金属或碱土金属氧化物。
8.根据权利要求1-6中任一项的颜料,其中珍珠岩芯的Fe2O3含量小于2%。
9.根据权利要求1-6中任一项的颜料,其中珍珠岩芯的Fe2O3含量是0%。
10.根据权利要求1-3任一项的颜料,其包含Al2O3/TiO2或MgO/TiO2,或介电层/金属层/介电层的混合层。
11.根据权利要求1-6任一项的颜料,其中所述珍珠岩片的平均厚度为<2μm。
12.根据权利要求1-6任一项的颜料,其中所述珍珠岩片的平均厚度为200-1000nm。
13.根据权利要求1-6任一项的颜料,其中所述珍珠岩片的平均厚度为200-600nm。
14.一种制备根据权利要求1的干扰颜料的方法,其通过用一种或多种金属氧化物以湿方法通过相应水溶性金属化合物的水解涂覆珍珠岩片,通过分离、干燥并任选煅烧因此得到的颜料,或通过将珍珠岩片在金属化合物的存在下悬浮在水性和/或含有机溶剂的介质中并通过加入还原剂而使金属化合物沉积在珍珠岩片上。
15.根据权利要求1-6中任一项的颜料在漆料、喷墨印刷中,在用于染色织物中,在用于着色涂料中、在印刷油墨、塑料、化妆品、用于陶瓷和玻璃的釉料中的用途。
16.用根据权利要求1-6中任一项的颜料着色的漆料、印刷油墨、塑料、化妆品、陶瓷和玻璃。
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PCT/EP2008/058160 WO2009007248A1 (en) | 2007-07-12 | 2008-06-26 | Interference pigments on the basis of perlite flakes |
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2008
- 2008-06-26 EP EP08761385A patent/EP2167587B1/en active Active
- 2008-06-26 KR KR1020157012024A patent/KR20150059796A/ko not_active Application Discontinuation
- 2008-06-26 US US12/668,028 patent/US20100203093A1/en not_active Abandoned
- 2008-06-26 JP JP2010515459A patent/JP2010532808A/ja active Pending
- 2008-06-26 WO PCT/EP2008/058160 patent/WO2009007248A1/en active Application Filing
- 2008-06-26 KR KR1020187003651A patent/KR20180016636A/ko active IP Right Grant
- 2008-06-26 CN CN2008800243913A patent/CN101688067B/zh active Active
- 2008-06-26 AT AT08761385T patent/ATE497997T1/de not_active IP Right Cessation
- 2008-06-26 DE DE602008004913T patent/DE602008004913D1/de active Active
- 2008-06-26 KR KR1020107003115A patent/KR20100056459A/ko active Application Filing
-
2014
- 2014-10-02 JP JP2014204330A patent/JP2015052117A/ja active Pending
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2016
- 2016-06-04 US US15/173,640 patent/US9963593B2/en active Active
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Also Published As
Publication number | Publication date |
---|---|
JP2010532808A (ja) | 2010-10-14 |
ATE497997T1 (de) | 2011-02-15 |
US20160280926A1 (en) | 2016-09-29 |
EP2167587B1 (en) | 2011-02-09 |
US20100203093A1 (en) | 2010-08-12 |
KR20180016636A (ko) | 2018-02-14 |
KR20150059796A (ko) | 2015-06-02 |
KR20100056459A (ko) | 2010-05-27 |
JP2015052117A (ja) | 2015-03-19 |
CN101688067A (zh) | 2010-03-31 |
US9963593B2 (en) | 2018-05-08 |
DE602008004913D1 (de) | 2011-03-24 |
EP2167587A1 (en) | 2010-03-31 |
WO2009007248A1 (en) | 2009-01-15 |
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