CN105246982B - 经涂布的珍珠岩片 - Google Patents
经涂布的珍珠岩片 Download PDFInfo
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- CN105246982B CN105246982B CN201380074550.1A CN201380074550A CN105246982B CN 105246982 B CN105246982 B CN 105246982B CN 201380074550 A CN201380074550 A CN 201380074550A CN 105246982 B CN105246982 B CN 105246982B
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- coated
- pearl sliver
- sliver
- weight
- pearl
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Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- 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
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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
- C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- 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
- C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
- C09C1/003—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer
- C09C1/0039—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/42—Clays
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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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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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/62—L* (lightness axis)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/66—Hue (H*)
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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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- C09C2200/10—Interference pigments characterized by the core material
- C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
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Abstract
本公开涉及一种制备经涂布的珍珠岩片的方法,其包括:(i)提供珍珠岩片;(ii)在所述珍珠岩片上涂覆氧化锡层以获得氧化锡涂布的珍珠岩片;(iii)在步骤(ii)中获得的所述氧化锡涂布的珍珠岩片上涂覆二氧化钛层以获得二氧化钛和氧化锡涂布的珍珠岩片;及(iv)在所述二氧化钛和氧化锡涂布的珍珠岩片上涂覆氧化铁层以获得所述经涂布的珍珠岩片。本公开还涉及经涂布的珍珠岩片,其包含:具有氧化锡层,再是二氧化钛层,然后是氧化铁层的珍珠岩片。
Description
发明领域
本发明涉及为经涂布的珍珠岩片的效果颜料,其包含带氧化锡层,再是二氧化钛层,然后是氧化铁层的珍珠岩片。
发明背景
效果颜料基于层状基材(例如已经涂有金属氧化物层的云母或珍珠岩片)的用途。这些颜料由于光的反射与折射可以展现珍珠般的光泽,并且根据金属氧化物层的厚度,其还可展现出干涉色效果。
DE102005025609公开了具高金属亮度,用于(例如)化妆品、漆和颜色中的非金属颜料混合物,其包含金色干涉颜料并且还包含银白色、银灰色和黑灰色干涉颜料。
EP1469042公开了一种颜料混合物,其包含含有基于玻璃片的效果颜料的组分A和含有有机和/或无机片状、针形、球形或晶状着色剂和/或填料的组分B。一种或多种着色剂与经涂布的玻璃片混合使得能够为涂覆系统赋予彩虹效应,增加颜色效果并且获得新的颜色效果。
WO2006110359涉及一种效果颜料,其包含涂有半透明金属氧化膜的合成片晶,所述合成片晶具有特征在于至少9.5μm的D10,介于约20和小于40μm之间的D50,及大于35至小于85μm的D90的尺寸分布。金属氧化膜可包含二氧化钛或氧化铁。合成片晶选自氧化铝、二氧化硅、氯氧化铋、氮化硼和玻璃。WO2006110359讲授了如何改变颜料的粒度分布以便优化闪烁效果。
本领域中目前已知的制备氧化铁涂布的珍珠岩片的方法和用氧化铁涂布云母和玻璃片的标准方法无效,因为氧化铁层易于从基材上剥离,使得产品不合需要。
因此,在本领域中仍然需要具有高闪烁效果(即,氧化铁不从基材剥离),仍然生产经济的效果颜料。
因此本发明的一个目的是提供色度和闪烁改善的效果颜料。本发明的另一目的是在天然基材(即,珍珠岩片)的基础上开发会表现出诸如以下优点的效果颜料:在各种组合物中的良好应用性能、环境相容性和处理简单以及实现优异光学效果,即高闪烁效果。
发明概述
根据本发明的一个实施方案,本文提供一种制备经涂布的珍珠岩片的方法,其包括:(i)提供珍珠岩片;(ii)在所述珍珠岩片上涂覆氧化锡层以获得氧化锡涂布的珍珠岩片;(iii)在步骤(ii)中获得的所述氧化锡涂布的珍珠岩片上涂覆二氧化钛层以获得二氧化钛和氧化锡涂布的珍珠岩片;及(iv)在所述二氧化钛和氧化锡涂布的珍珠岩片上涂覆氧化铁层以获得所述经涂布的珍珠岩片。
根据本发明的另一个实施方案,本文还提供经涂布的珍珠岩片,其包含:具有氧化锡层,再是二氧化钛层,然后是氧化铁层的珍珠岩片。
根据本发明的再一个实施方案,本文提供一种制备经涂布的珍珠岩片的方法,其包括:(i)制备水和D50在10μm至50μm范围内的珍珠岩片的浆料;(ii)将步骤(i)中获得的所述浆料加热至约70℃至约100℃的温度并将所述浆料的pH调节至介于约1和3之间;(iii)在步骤(ii)后,向所述浆料中添加锡盐溶液,同时将pH维持在介于约1和4之间;(iv)在步骤(iii)后,搅拌所述浆料至少30分钟;(v)在步骤(iv)后,向所述浆料中添加钛盐溶液,同时将pH维持在介于约1和4之间;(vi)在步骤(v)后,向所述浆料中添加铁盐溶液,同时将pH维持在介于约1和4之间;及(vii)在步骤(vi)后,过滤,然后洗涤,并且再在约500℃至约1000℃下煅烧所述浆料以获得所述经涂布的珍珠岩片。
本发明的这些和其它目的和优点应从附图及其描述显而易见。
附图简述
图1为示出实施例1的经良好涂布的珍珠岩片的光学显微照片。
图2为示出实施例2的经良好涂布的珍珠岩片的光学显微照片。
图3为示出实施例3的经良好涂布的珍珠岩片的光学显微照片。
图4为示出比较例4的经不良涂布的珍珠岩片的光学显微照片。
图5为示出比较例5的经不良涂布的珍珠岩片的光学显微照片。
图6为示出比较例6的未使用TiO2层,导致涂层开裂和剥落的珍珠岩片的光学显微照片。
图7为示出实施例8的经良好涂布的珍珠岩片的光学显微照片。
发明详述
在过去,已经以描述性方式在严重依赖主观性的同时描述了效果颜料的闪烁。效果颜料“闪烁”的主观性分级由于闪烁效果的定量描述并不清楚。为解决这个问题,在过去几年中已经开发了测量装置以实际测量效果颜料的“闪烁”。此类测量装置的一个实例为来自于Byk-Gardner GmbH的Byk-mac(Lausitzer Straβe 8,82538Geretsried,Germany)。这种装置允许测量用于薄片表征的闪烁和粒度。闪烁等级(S_G)是以下两个参数的函数:闪烁面积(S_a)与指定测量中的光反射次数相对应;并且闪烁强度(S_i)对应于光反射的强度。
最常见的闪烁效果颜料基于涂有金属氧化物的云母或平均粒度大于40μm的合成云母,以及涂有金属氧化物的玻璃片或涂有金属氧化物的氧化铝片。此类效果颜料通常提供了所需闪烁效果。
如本文中所用,珍珠岩片是通常含约72-75%SiO2、12-14%Al2O3、0.5-2%Fe2O3、3-5%Na2O、4-5%K2O、0.4-1.5%CaO(按重量计)和低浓度的其它金属元素的水合天然玻璃片。珍珠岩片与天然玻璃的区别在于化学结合水含量更高(按重量计2-10%),存在玻璃质、珍珠般光泽和特有的同心或弧形洋葱皮样(即,珍珠岩)断裂。珍珠岩片可通过WO02/11882中公开的方法制备,所述方法可包括碾磨、过筛和热膨胀。优选具有控制的粒度分布、低漂浮物含量和高蓝光亮度的珍珠岩片。
优选中值粒度小于约50μm的珍珠岩片。优选中值粒度为约15至约50μm的珍珠岩片并且最优选中值粒度为约20至约40μm的珍珠岩片。
本发明中使用的珍珠岩片的形状不均一。然而,为了简洁起见,珍珠岩片将被称为具有“直径”。珍珠岩片具有<约2μm,特别是约200至约1000nm,特别是约200至约600nm的平均厚度。当前优选所述片的直径(中值粒度(d50))在约15-50μm的优选范围内,更优选约20-40μm的范围。
珍珠岩片具有小于10体积%的漂浮物含量;特别是小于5体积%的漂浮物含量;尤其是小于2体积%的漂浮物含量。珍珠岩片具有高于80;特别是高于82;尤其是高于85的蓝光亮度。
优选的珍珠岩为OPTIMATTM2550(World Minerals生产的消光剂)。如果(例如)通过沉降或离心去除了粒度低于10μm的颗粒,则珍珠岩,如OPTIMATTM1735(World Minerals生产的消光剂)也可使用。
本文提供一种制备经涂布的珍珠岩片的方法,其包括:(i)提供珍珠岩片;(ii)在所述珍珠岩片上涂覆氧化锡层以获得氧化锡涂布的珍珠岩片;(iii)在步骤(ii)中获得的所述氧化锡涂布的珍珠岩片上涂覆二氧化钛层以获得二氧化钛和氧化锡涂布的珍珠岩片;及(iv)在所述二氧化钛和氧化锡涂布的珍珠岩片上涂覆氧化铁层以获得所述经涂布的珍珠岩片。
在上述方法中提供珍珠岩片的步骤(i)包括:选择平均粒径D50在约1μm至约1000μm,优选约10μm至约500μm,更优选约10μm至约100μm,甚至更优选约15μm至约50μm,且最优选约20μm至约40μm的范围内的珍珠岩片。
步骤(ii)中涂覆的所述氧化锡的量按所述经涂布的珍珠岩片的总重量计为约0.5重量%至约5重量%。步骤(iii)中涂覆的所述二氧化钛的量按所述经涂布的珍珠岩片的总重量计为约0.5重量%至约50重量%。步骤(iv)中涂覆的所述氧化铁的量按所述经涂布的珍珠岩片的总重量计为约0.5重量%至约50重量%。
步骤(ii)中涂覆的所述氧化锡层的厚度为约1nm至约10nm。步骤(iii)中涂覆的所述二氧化钛层的厚度为约1nm至约150nm。步骤(iv)中涂覆的所述氧化铁层的厚度为约1nm至约150nm。
本文提供了经涂布的珍珠岩片。经涂布的珍珠岩片包含带氧化锡层,再是二氧化钛层,然后是氧化铁层的珍珠岩片。
本文所述经涂布的珍珠岩片可用于(i)油漆、(ii)喷墨印刷、(iii)织物染色、(iv)涂层着色、(v)印刷油墨、(vi)塑料、(vii)化妆品或(viii)陶瓷和玻璃用釉料中。
经BYK-mac测量,本文所述经涂布的珍珠岩片具有至少约3.9,更优选介于约3.9和约10之间,且最优选介于约3.9和约7之间的闪烁等级(S_G)。
经BYK-mac测量,对于本发明的目的而言所需的闪烁效果为至少约3.9的闪烁等级(S_G)。
本文使用的珍珠岩可以例如OPTIMATTM2550(World Minerals生产的消光剂)商购获得。然后可将珍珠岩片分级为所需闪烁效果的最佳粒度,再涂覆氧化锡、二氧化钛和氧化铁。珍珠岩片的这种分级包括选择平均粒径D50在约1μm至约1000μm,优选约10μm至约500μm,更优选约10μm至约100μm,甚至更优选约15μm至约50μm,且最优选约20μm至约40μm的范围内的珍珠岩片。可于水浆中通过重力分离进行分级。在实验室环境中,可通过沉淀进行分级并且在生产设施中可用离心机进行分级。其它分级方法例如过筛和风力分级也可使用。
在一个实施方案中,通过以下方法制备经涂布的珍珠岩片。将具有约10-50μm(优选约30μm)平均粒度的珍珠岩片与水混合的浆料加热至约70℃至约100℃(优选约80℃至约85℃)的温度并用酸例如HCl将pH调节至约1.5。然后随碱例如NaOH一起添加锡盐(例如,SnCl4)溶液以便维持pH。搅拌约60分钟后,随碱例如NaOH一起添加钛盐(例如,TiCl4)溶液以维持pH。然后用碱例如NaOH将pH升高至约3.0,之后随碱例如NaOH一起添加铁盐(例如,FeCl3)溶液以维持pH。铁盐(例如,FeCl3)添加之后,过滤、洗涤浆料并且在约500℃至约1000℃,更优选约700℃至约900℃,并且最优选约850℃下煅烧以获得本发明经涂布的珍珠岩片。
直接向云母上涂布氧化铁的常规方法不可用于珍珠岩,因为氧化铁无法沉积到珍珠岩表面上。
已经意外地发现氧化锡层有助于氧化铁沉积到珍珠岩上。还已发现氧化铁涂层易于从珍珠岩片上剥离。据信由于在氧化铁和珍珠岩片表面之间形成的弱键,氧化铁涂层易于剥离。生产期间的煅烧温度使这些弱键处于热应力下,这样将氧化铁剥离珍珠岩片。已经发现在改变加工条件,包括使用更低的煅烧温度后,实现了剥离问题最低限度的解决。然而,已经发现一旦在珍珠岩片上涂布氧化锡,再涂布二氧化钛,然后涂布氧化铁,剥离问题就会得以解决。
根据所用二氧化钛和氧化铁的量,可产生从金色到青铜色、铜色和赤褐色的一系列颜色(参见实施例)。
本发明具金属样颜色和闪烁效果的经涂布的珍珠岩片可用于装饰性涂层中以产生仿古效果的涂层。金属样颜色意味着颜料提供了看起来像金属的颜色效果,例如金色、青铜色和铜色。
在一些实施方案中,可通过CVD(化学气相沉积)或通过湿化学涂布涂覆金属氧化物层。可通过在水蒸气的存在下(相对低分子量的金属氧化物例如磁铁矿)或在氧气和(适当时)水蒸气(例如,氧化镍和氧化钴)的存在下分解羰络金属获得金属氧化物层。特别地借助于羰络金属(例如,五羰基铁、六羰基铬;EP-A-45851)的氧化气相分解,借助于金属醇化物(例如,四正和异丙醇钛和锆;DE-A-4140900)或金属卤化物(例如,四氯化钛;EP-A-338428)的水解气相分解,借助于有机基锡化合物(特别是烷基锡化合物例如四丁基锡和四甲基锡;DE-A-4403678)的氧化分解或借助于如EP-A-668329中所述的有机基硅化合物(特别是二-叔丁氧基乙酰氧基硅烷)的气相水解来涂覆金属氧化物层,对于在流化床反应器中进行的涂层操作而言是可能的(EP-A-045851和EP-A-106235)。有利地在惰性气体下以另外的方式进行的涂有铝的颜料冷却期间,可通过控制氧化获得Al2O3层(B)(DE-A-19516181)。
优选通过湿化学法通过沉淀来涂覆钛、铁和锡的氧化物层,在适当情况下,对于要还原的金属氧化物而言可能。在湿化学涂布的情况下,可使用为生产珠光颜料开发的湿化学涂布法;这些(例如)在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、DE1959988、WO93/08237、WO98/53001和WO03/6558中有描述。
TiO2层可处于金红石或锐钛矿改性,其中优选金红石改性。也可通过已知方式,如EP-A-735,114、DE-A-3433657、DE-A-4125134、EP-A-332071、EP-A-707,050、WO93/19131或WO06/131472中所述,例如氨水、氢气、烃蒸气或其混合物或金属粉末还原TiO2层。
为了涂布,使基材颗粒(即,珍珠岩片)悬浮于水中并且在适合水解的pH下添加一种或多种可水解的金属盐,如此选择pH以使金属氧化物或水合金属氧化物直接沉淀到颗粒上,而无副沉淀发生。通常通过同时计量加入碱来保持pH恒定。然后将颜料(即,经涂布的珍珠岩片)分离、洗涤、干燥并且在适当情况下煅烧,可根据谈论的涂层优化煅烧温度。若需要,在已经涂覆各个涂层之后,可将颜料分离、干燥并且,在适当情况下煅烧,然后再次重新悬浮以沉淀其它层。
金属氧化物层也可例如类似于DE-A-19501307中所述的方法,通过一种或多种金属酸酯的受控水解来获得,在适当情况下在有机溶剂和碱性催化剂的存在下,通过溶胶-凝胶工艺生成金属氧化物层。适合的碱性催化剂为(例如)胺,例如三乙胺、乙二胺、三丁胺、二甲基乙醇胺和甲氧基丙胺。有机溶剂为可与水混溶的有机溶剂例如C1-4醇,特别是异丙醇。
适合的金属酸酯选自钛、铁和锡的烷基和芳基醇化物、羧酸酯和经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酯、钛酸四异丙酯、锆酸四异丙酯、原硅酸四乙酯和硼酸三乙酯。另外,可使用前述金属的乙酰丙酮化物和乙酰乙酰丙酮化物。该类型的金属酸酯的优选实例为乙酰丙酮合钛和二异丁基油烯基乙酰乙酰铝酸酯或二异丁基油烯基乙酸乙酰丙酮化物及金属酸酯的混合物。
珍珠岩片上的氧化物层可任选地通过常见工序还原:US-B-4,948,631(NH3,750-850℃)、W093/19131(H2,>900℃)或DE-A-19843014(固体还原剂,例如硅,>600℃)。
也可通过涂覆另外的层,例如有色金属氧化物或柏林蓝(Berlin Blue)、过渡金属(例如Fe、Cu、Ni、Co、Cr)的化合物或有机化合物(例如染料或色淀),来改变颜料的粉末颜色。
为增强耐候性和光稳定性,可根据应用的领域,使(多层)珍珠岩片经受表面处理。例如在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中描述了有用的表面处理。表面处理可促进处理颜料,特别是将其掺入用于各种应用的各种组合物中。
根据调节方法或预期应用,可有利的是在调节过程之前或之后向效果颜料添加一定量的质地改进剂,条件是这对效果颜料用于为各种应用的各种组合物上色的用途无不良影响。具体地,适合的试剂为含有至少18个碳原子的脂肪酸(例如硬脂酸或山萮酸),或其酰胺或金属盐,特别是镁盐,还有增塑剂、蜡、树脂酸(例如枞酸、松香皂)、烷基苯酚或脂肪醇(例如硬脂醇),或含8-22个碳原子的脂肪族1,2-二羟基化合物(例如1,2-十二烷二醇),还有改性马来酸松香树脂或富马酸松香树脂。按终产物计,按优选0.1-30重量%,特别是2-15重量%的量添加质地改进剂。
可按任何染色有效量向被着色的物质添加效果颜料(即,经涂布的珍珠岩片)。按着色物质组合物的总重量计,着色物质组合物可包含0.01-80重量%或优选0.1-30重量%的效果颜料。高浓度,例如高于30重量%的浓度,通常呈浓缩剂(“母料”)形式,其可作为着色剂用于生产具有相对较低颜料含量的着色材料,根据本发明所述的颜料在传统配制剂中具有极低粘度,以致其仍可良好加工。
根据应用,除根据本发明所述的效果颜料外可添加任何所需量的其它赋色组成部分,例如白色、彩色、黑色或效果颜料以便获得不同的色调或颜色效果。当彩色颜料与根据本发明所述的效果颜料混合使用时,总量按着色组合物的总重量计优选为0.1-10重量%。通过根据本发明所述的效果颜料与另一种颜色,特别是互补色的彩色颜料的优选组合提供了特别高的随角异色(goniochromicity),由使用效果颜料产生的着色和使用彩色颜料产生的着色,在10°的测量角下色调之差(ΔΗ*)为约20至约340,特别是约150至约210。
优选地,根据本发明所述的效果颜料与透明的彩色颜料组合,所述透明的彩色颜料可以存在于与根据本发明所述的效果颜料相同的介质中或存在于邻近介质中。效果颜料与彩色颜料有利地存在于邻近介质中的排列的一个实例为多层效果涂层。
用根据本发明所述的效果颜料对组合物着色是例如通过用滚轧机或混合或研磨装置将这种颜料,在适当的情况下以母料的形式,与基材混合进行的。然后使用本身巳知的方法如压延、压力成型、挤出、涂覆、浇注或注塑成型使着色的材料形成所需最终形态。在掺入所述颜料之前或之后,可以按通常的量向聚合物中添加塑料工业中常用的任何添加剂,例如增塑剂、填料或稳定剂。
为了对组合物例如涂层和印刷墨水着色,根据本发明所述的效果颜料,在适当的情况下连同常用添加剂例如填料、其它颜料、催干剂或增塑剂一起,被精细地分散或溶解在相同有机溶剂或溶剂混合物中,可能各个组分单独溶解或分散或许多组分一起溶解或分散,之后才将所有组分放在一起。
将根据本发明所述的效果颜料分散在被着色的组合物中和加工根据本发明所述的颜料组合物,优选地在经受只发生较弱剪切力从而所述效果颜料不会破碎成更小的部分的条件下进行。
塑料中本发明颜料的含量为0.1-50重量%,尤其是0.5-7重量%。在涂层部分,本发明的颜料的用量为0.1-10重量%。在粘合剂体系,例如用于油漆和凹板印刷、胶印或丝网印刷的印刷墨水的粘合剂体系的着色中,按0.1-50重量%,优选5-30重量%且尤其是8-15重量%的量向印刷墨水中掺入所述颜料。
本发明经涂布的珍珠岩片可用于此前已经使用了效果颜料的任何应用中。因此,本发明的产品在所有类型的汽车和工业油漆应用,特别是在需要深色强度的有机彩色涂层和油墨领域中的使用不受限制。例如,这些颜料可用于主色调中或作为定型剂为所有类型的汽车和非汽车交通工具喷漆。类似地,本发明经涂布的珍珠岩片也可用于所有粘土/胶木/木材/玻璃/金属/瓷釉/陶瓷及无孔或多孔表面。
当用本发明经涂布的珍珠岩片着色的组合物为涂层时,其特别地为特种涂层,非常特别地为汽车末道漆。
本发明经涂布的珍珠岩片也可用于粉末涂层组合物中。其可掺入面向玩具行业或家庭的塑料颗粒中。这些效果颜料可浸入纤维中以赋予服装和地毯新的美观色彩。本发明经涂布的珍珠岩片可用于改善鞋、橡胶和乙烯基/大理石地板、乙烯基壁板和所有其它乙烯基产品的外观。
本发明经涂布的珍珠岩片可用于各种组合物,例如印刷油墨、指甲油、漆、热塑性和热固性材料、天然树脂和合成树脂中。一些非限制性实例包括聚苯乙烯及其混合聚合物、聚烯烃(尤其是聚乙烯和聚丙烯)、聚丙烯酸化合物、聚乙烯基化合物(例如聚氯乙烯和聚乙酸乙烯酯)、聚酯和橡胶,还有由纤维胶和纤维素醚制成的细丝、纤维素酯、聚酰胺、聚氨酯、聚酯(例如聚对苯二甲酸二醇酯和聚丙烯腈)。
关于各种颜料应用较为全面的讨论,参见Temple C.Patton编辑,The PigmentHandbook,第II卷,Applications and Markets,John Wiley and Sons,New York(1973)。另外,参见例如,关于油墨:R.H.Leach编辑,The Printing Ink Manual,第4版,VanNostrand Reinhold(International)Co.Ltd.,London(1988),特别是第282-591页;关于油漆:C.H.Hare,Protective Coatings,Technology Publishing Co.,Pittsburgh(1994),特别是第63-288页。前述参考文献据此通过引用并入本文,其讲授油墨、油漆和塑料组合物、配制剂及于其中本发明组合物可用的包括一定量的着色剂的媒介物。例如,本发明经涂布的珍珠岩片可按10-15%的水平用于平版胶印油墨中,其余是含有胶化和未胶化烃树脂、醇酸树脂、蜡化合物和脂肪族溶剂的媒介物。本发明经涂布的珍珠岩片也可按例如1-10%的水平连同可包括二氧化钛、丙烯酸晶格、成膜助剂、水或溶剂的其它颜料一起用于汽车油漆配制剂中。本发明经涂布的珍珠岩片也可按例如20-30%的水平用于聚乙烯中的塑料色母粒中。
根据本发明所述的效果颜料也适合嘴唇和皮肤化妆及为头发或指甲上色。因此本发明还涉及化妆品制剂或配制剂,其按化妆品制剂或配制剂的总重量计包含0.0001-90重量%的颜料,特别是根据本发明所述的效果颜料和10-99.9999%的适合化妆的载体材料。此类化妆品制剂或配制剂为,例如唇膏、腮红、粉底、指甲油和洗发剂。化妆品制剂或配制剂中的颜料可单独或呈混合物形式使用。另外,可能连同其它颜料和/或着色剂一起使用根据本发明所述的颜料,例如呈上文所述的或化妆品制剂中已知的组合使用。根据本发明所述的化妆品制剂和配制剂优选地含有按所述制剂的总重量计,量为0.005-50重量%的根据本发明所述的颜料。适合根据本发明所述的化妆品制剂和配制剂的载体材料包括此类组合物中使用的常用材料。
根据本发明所述的化妆品制剂和配制剂可呈(例如)棒状、膏、霜、乳液、悬浮液、分散体、粉末或溶液形式。其为,例如唇膏、睫毛膏、腮红、眼影、粉底、眼线笔、粉或指甲油。如果所述制剂呈棒状形式,例如唇膏、眼影、腮红或粉底,则所述制剂由很大一部分的脂肪组分组成,所述脂肪组分可由一种或多种蜡,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、凡士林油、甘油一酸酯、甘油二酯或甘油三酯或其在25℃下为固体的脂肪酸酯、硅酮蜡(例如甲基十八烷-氧基聚硅氧烷和聚(二甲基硅氧基)硬脂氧基硅氧烷)、硬脂酸单乙醇胺、松香及其衍生物(例如松香酸二甘醇酯和松香甘油酯)、在25℃下为固体的氢化油、糖甘油酯及钙、镁、锆和铝的油酸盐、肉豆蔻酸盐、羊毛脂酸盐、硬脂酸盐和二羟基硬脂酸盐组成。脂肪组分也可由至少一种蜡和至少一种油的混合物组成,在这种情况下下列油适合,例如:石蜡油、鸭子尾脂腺油(purcelline oil)、全氢鲨烯、甜杏仁油、鳄梨油、海棠油(calophyllum oil)、蓖麻油、芝麻油、荷荷巴油(jojoba oil)、沸点为约310℃至约410℃的矿物油、硅油(例如二甲基聚硅氧烷)、亚油基醇、亚麻基醇、油醇、禾谷类油(例如小麦胚芽油)、羊毛酸异丙酯(isopropyl lanolate)、棕榈酸异丙酯、肉豆蘧酸异丙酯、肉豆蘧酸丁酯、肉豆蘧酸鲸蜡酯、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。这种棒状形式的制剂中的脂肪组分通常可占制剂总重量的99.91重量%。
根据本发明所述的化妆品制剂和配制剂可另外包含其它组成部分,例如二醇、聚乙二醇、聚丙二醇、单链烷醇酰胺、未上色的聚合、无机或有机填料、防腐剂、UV过滤剂或化妆品中常见的其它佐剂和添加剂,例如天然或合成或部分合成的甘油二酯或三酯、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,或此类物质的混合物。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。举例而言,可提到如下:
·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例如三氯生(triclosan)、六氯酚(hexachlorophene)、醇和阳离子物质(例如季铵盐)的除臭剂,和气味吸收剂例如(蓖麻醇酸锌与各种添加剂的组合)或柠檬酸三乙酯(任选与抗氧化剂例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够吸收日光的UV辐射并将它转化成热量的过滤剂物质(遮光剂);根据所需作用,优选如下光防护剂:选择性吸收在约280-315nm范围内的导致晒斑的高能UV辐射(UV-B吸收剂)并发射在例如315-400nm范围(UV-A范围)的较长波长的光防护剂,以及仅吸收在315-400nm的UV-A范围内的较长波长辐射的光防护剂(UV-A吸收剂);
·适合的光防护剂为,例如来自以下类别的有机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/或选自涂有氧化铝或二氧化硅的TiO2、氧化锌或云母的无机微细颜料;
·对抗昆虫的活性成分(驱虫剂),是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;最常使用的驱虫剂为二乙基甲苯酰胺(DEET);其它常见驱虫剂将例如在"Pflegekosmeti k"(W.Raab和U.Kindl,Gustav-Fischer-VerlagStuttgart/New York,1991),第161页中找到;
·用于防御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屏障的所有物质,例如用于防御水溶液的石蜡油、硅油、植物油、PCL产品和羊毛脂,用于防御有机溶剂作用的成膜剂例如藻酸钠、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”用于防御皮肤上严重机械应力的物质;
·保湿物质:例如以下物质用作湿度控制剂(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、氨基酸和酶以及微量元素镁、硅、磷、钙、锰、铁或铜的化合物的活性成分组合物;
·皮肤修复复合物:可由双歧杆菌类(bifidus group)细菌的灭活和分解培养物得到;
·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)、金盖草(marigold)、迷迭香(rosemary)、鼠尾草(sage)、马尾草(horsetail)或百里香(thyme);
·动物提取物:例如蜂王浆、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(apricot kerneloil)、鳄梨油、巴巴苏油、棉籽油、琉璃苣油、蓟油、花生油、γ-谷维醇、玫瑰果油、大麻油、榛子油、黑醋栗籽油、荷荷巴油、樱核油、鲑鱼油、亚麻籽油、玉米籽油、澳洲坚果油(macadamianut oil)、杏仁油、月见草油、貂油、橄榄油、美洲山核桃油、桃仁油、开心果油、菜油、稻籽油、蓖麻油、红花油、芝麻油、豆油、葵花油、茶树油、葡萄籽油或小麦胚芽油。
呈棒状形式的制剂优选无水,但在某些情况下可包含一定量的水,然而,水量通常按化妆品制剂的总重量计不超过40重量%。如果根据本发明所述的化妆品制剂和配制剂呈半固体产品形式,即呈膏或霜形式,则它们同样可以无水或含水。这种制剂和配制剂为,例如睫毛膏、眼线笔、粉底、腮红、眼影笔,或用于处理眼圈的组合物。另一方面,如果这种膏或霜含水,则它们尤其是除颜料外,还包含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。此类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、未上色的聚合物以及无机或有机填料。如果制剂呈粉末形式,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佐剂如粘合剂、着色剂等组成。同样,此类制剂可包含常规用于化妆品中的各种佐剂,例如芳香剂、抗氧化剂、防腐剂等。如果根据本发明所述的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呈溶液形式的天然或合成聚合物组成,其中溶液可包含其它佐剂,例如珠光剂。在该实施方案中,有色聚合物以约0.1-5重量%的量存在。根据本发明所述的化妆品制剂和配制剂也可用于头发上色,在这种情况下它们以由常规用于化妆品工业中的基础物质和根据本发明所述的颜料组成的洗发剂、霜或凝胶的形式使用。根据本发明所述的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中的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,其中此范围仅在权利要求中定义。除非以下实施例中以及说明书和权利要求中的其它地方另有说明,所有份数和百分数按重量计,温度按摄氏度计并且压力在大气压下或接近大气压力下。
实施例
实施例1
将215g珍珠岩(平均粒度30μm)于1785mL蒸馏水中的浆料加热至83℃并且用HCl将pH调至1.4。然后按3.2g/min添加50g的20%SnCl4溶液,用NaOH维持pH。搅拌60分钟后,按3g/min添加36g的40%TiCl4溶液,用NaOH维持pH。然后用NaOH将pH升高至3.0,之后按1.2g/min添加39%FeCl3溶液,用NaOH维持pH。添加320g的FeCl3后,浆料经过滤、洗涤并在850℃下煅烧。如图1所示,所得产物具有青铜色。
实施例2
除添加335g的FeCl3外,像实施例1一样进行该实施例。如图2所示,所得产物具有铜干涉色。
实施例3
除添加360g的FeCl3外,像实施例1一样进行该实施例。如图3所示,所得产物具有赤褐色干涉色。
比较例4
将125g珍珠岩(平均粒度30μm)于2606mL蒸馏水中的浆料加热至80℃并且用HCl将pH调至3.0。然后按1.6mL/min添加206g的39%FeCl3溶液,用NaOH维持pH。浆料经过滤、洗涤并在650℃下煅烧。所得产物具有青铜色,但是Fe2O3主要沉淀在珍珠岩片旁边,而不是作为珍珠岩上的涂层。这于图4中示出。
比较例5
与实施例4一样进行该实施例,但是添加240g的39%FeCl3。所得产物具有赤褐色,但是Fe2O3主要沉淀在珍珠岩片旁边,而不是作为珍珠岩上的涂层。这于图5中示出。
比较例6
将183g珍珠岩(平均粒度30μm)于1817mL蒸馏水中的浆料加热至74℃并且用HCl将pH调至1.5。然后按0.8g/min添加51g的20%SnCl4溶液,用NaOH维持pH。搅拌30分钟后,用NaOH将pH升高至3.2,之后按0.56g/min添加39%FeCl3溶液,用NaOH维持pH。添加466g的FeCl3后,浆料经过滤、洗涤并在850℃下煅烧。所得产物具有赤褐色。当配制成装饰性涂层时,许多Fe2O3涂层开裂并且从珍珠岩表面剥落。这于图6中示出。
实施例7
将125g珍珠岩(平均粒度30μm)于1250mL蒸馏水中的浆料加热至80℃并且用HCl将pH调至1.4。然后按1.77mL/min添加58.75g的20%SnCl4溶液,用NaOH维持pH。搅拌30分钟后,按1.6mL/min添加209g的40%TiCl4溶液,用NaOH维持pH。然后用NaOH将pH升高至3.2,之后按1.0g/min添加10g的39%FeCl3溶液,用NaOH维持pH。一小份浆料样品经过滤、洗涤并在850℃下煅烧。再重复添加10g和取样7次。产生一系列具有范围从浅砂色到金橙色的颜色的产物。
实施例8
将180g珍珠岩(平均粒度30μm)于1820mL蒸馏水中的浆料加热至80℃并且用HCl将pH调至1.4。然后按2.57mL/min添加40g的20%SnCl4溶液,用NaOH维持pH。搅拌30分钟后,按2.44mL/min添加300g的40%TiCl4溶液,用NaOH维持pH。然后用NaOH将pH升高至3.2,之后按1.28mL/min添加55g的39%FeCl3溶液,用NaOH维持pH。浆料经过滤、洗涤并在850℃下煅烧。如图7所示,所得产物具有金色。
结果
对于颜色数据而言:
L*=亮度;
C*=色度;
H°=色调;以及
S_G=闪烁等级。
全部在15°下经BYK-mac测量。
下面在表1中提供了上文所讨论的所有样品的L*、C*、H°和S_G值。
表1
实施例 | L* | C* | H° | S_G |
1 | 81.4 | 42.6 | 61.6 | 6.29 |
2 | 65.9 | 40.7 | 46.3 | 5.84 |
3 | 63.1 | 32.0 | 24.5 | 3.98 |
比较例4 | N/A<sup>1</sup> | N/A<sup>1</sup> | N/A<sup>1</sup> | N/A<sup>1</sup> |
比较例5 | N/A<sup>1</sup> | N/A<sup>1</sup> | N/A<sup>1</sup> | N/A<sup>1</sup> |
比较例6 | 71.8 | 30.2 | 23.3 | 3.4 |
7 | 参见下表2 | 参见下表2 | 参见下表2 | 参见下表2 |
8 | 92.27 | 48.48 | 79.55 | 5.30 |
1因为珍珠岩片未形成良好的涂层,所以对于比较例4和5而言,未获得颜色测量数据。
下面在表2中提供了实施例7中样品系列的颜色数据。
表2
样品 | L* | C* | H° | S_G |
a | 86.60 | 16.88 | 100.15 | 4.87 |
b | 86.00 | 22.94 | 96.70 | 5.09 |
c | 84.64 | 29.32 | 93.27 | 4.97 |
d | 82.57 | 33.92 | 90.02 | 5.17 |
e | 81.38 | 38.33 | 86.34 | 4.90 |
f | 78.74 | 39.28 | 81.74 | 4.71 |
g | 74.81 | 37.55 | 75.70 | 4.57 |
h | 72.50 | 34.59 | 67.47 | 4.09 |
如上文所示,本发明的经涂布的珍珠岩片(参见实施例1-3、7和8)当与本领域中已知的(参见比较例4-6)比较时提供了非常可取的L、C、H和S_G值。更具体地,本发明可取的经涂布的珍珠岩片的S_G值为至少3.9。
Claims (27)
1.一种制备经涂布的珍珠岩片的方法,其包括:
(i)提供珍珠岩片;
(ii)在所述珍珠岩片上涂覆氧化锡层以获得氧化锡涂布的珍珠岩片;
(iii)在步骤(ii)中获得的所述氧化锡涂布的珍珠岩片上涂覆二氧化钛层以获得二氧化钛和氧化锡涂布的珍珠岩片;及
(iv)在所述二氧化钛和氧化锡涂布的珍珠岩片上涂覆氧化铁层以获得所述经涂布的珍珠岩片。
2.根据权利要求1所述的方法,其中提供珍珠岩片的步骤(i)包括:
选择平均粒径D50在1μm至1000μm范围内的珍珠岩片。
3.根据权利要求1所述的方法,其中步骤(ii)中涂覆的所述氧化锡的量按所述经涂布的珍珠岩片的总重量计为0.5重量%至5重量%。
4.根据权利要求1所述的方法,其中步骤(iii)中涂覆的所述二氧化钛的量按所述经涂布的珍珠岩片的总重量计为0.5重量%至50重量%。
5.根据权利要求1所述的方法,其中步骤(iv)中涂覆的所述氧化铁的量按所述经涂布的珍珠岩片的总重量计为0.5重量%至50重量%。
6.根据权利要求1所述的方法,其中步骤(ii)中涂覆的所述氧化锡层的厚度为1nm至10nm。
7.根据权利要求1所述的方法,其中步骤(iii)中涂覆的所述二氧化钛层的厚度为1nm至150nm。
8.根据权利要求1所述的方法,其中步骤(iv)中涂覆的所述氧化铁层的厚度为1nm至150nm。
9.经涂布的珍珠岩片,其由根据权利要求1所述的方法获得。
10.一种组合物,其包含根据权利要求9所述的经涂布的珍珠岩片。
11.一种将根据权利要求9所述的经涂布的珍珠岩片用于(i)油漆、(ii)喷墨印刷、(iii)织物染色、(iv)涂层着色、(v)印刷油墨、(vi)塑料、(vii)化妆品或(viii)陶瓷和玻璃用釉料中的方法。
12.油漆、印刷油墨、塑料、化妆品、陶瓷和玻璃,其用根据权利要求9所述的经涂布的珍珠岩片着色。
13.经涂布的珍珠岩片,其包含:
具有氧化锡层,再是二氧化钛层,然后是氧化铁层的珍珠岩片。
14.根据权利要求13所述的经涂布的珍珠岩片,其中所述珍珠岩片具有在1μm至1000μm范围内的平均粒径D50。
15.根据权利要求13所述的经涂布的珍珠岩片,其中在所述珍珠岩片上的所述氧化锡的量为0.5重量%至5重量%。
16.根据权利要求13所述的经涂布的珍珠岩片,其中在所述珍珠岩片上的所述二氧化钛的量按所述经涂布的珍珠岩片的总重量计为0.5重量%至50重量%。
17.根据权利要求13所述的经涂布的珍珠岩片,其中在所述珍珠岩片上的所述氧化铁的量按所述经涂布的珍珠岩片的总重量计为0.5重量%至50重量%。
18.根据权利要求13所述的经涂布的珍珠岩片,其中所述氧化锡层的厚度为1nm至10nm。
19.根据权利要求13所述的经涂布的珍珠岩片,其中所述二氧化钛层的厚度为1nm至150nm。
20.根据权利要求13所述的经涂布的珍珠岩片,其中所述氧化铁层的厚度为1nm至150nm。
21.根据权利要求13所述的经涂布的珍珠岩片,其经BYK-mac测量,具有至少3.9的闪烁等级(S_G)。
22.根据权利要求21所述的经涂布的珍珠岩片,其经BYK-mac测量,具有3.9至7的闪烁等级(S_G)。
23.一种组合物,其包含根据权利要求13所述的经涂布的珍珠岩片。
24.一种制备经涂布的珍珠岩片的方法,其包括:
(i)制备水和D50在10μm至50μm范围内的珍珠岩片的浆料;
(ii)将步骤(i)中获得的所述浆料加热至70℃至100℃的温度并将所述浆料的pH调节至介于1和3之间;
(iii)在步骤(ii)后,向所述浆料中添加锡盐溶液,同时将pH维持在介于1和4之间;
(iv)在步骤(iii)后,搅拌所述浆料至少30分钟;
(v)在步骤(iv)后,向所述浆料中添加钛盐溶液,同时将pH维持在介于1和4之间;
(vi)在步骤(v)后,向所述浆料中添加铁盐溶液,同时将pH维持在介于1和4之间;及
(vii)在步骤(vi)后,过滤,然后洗涤,并且再在500℃至1000℃下煅烧所述浆料以获得所述经涂布的珍珠岩片。
25.经涂布的珍珠岩片,其由根据权利要求24所述的方法获得。
26.一种组合物,其包含根据权利要求25所述的经涂布的珍珠岩片。
27.根据权利要求26所述的组合物,其为(i)油漆组合物、(ii)喷墨印刷组合物、(iii)织物染色组合物、(iv)涂层组合物、(v)印刷油墨组合物、(vi)塑料组合物、(vii)化妆品组合物或(viii)陶瓷和玻璃用釉料组合物。
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SI3034563T1 (sl) * | 2014-12-19 | 2019-06-28 | Eckart Gmbh | Zlato obarvani efektni pigmenti z visoko kromo in visokim sijajem, postopek za njihovo pripravo in njihova uporaba |
SI3034566T1 (sl) * | 2014-12-19 | 2019-05-31 | Eckart Gmbh | Pigmenti s kovinskim efektom, ki imajo visoko kromo in visok sijaj, postopek za njihovo pripravo in njihova uporaba |
ES2662134T3 (es) * | 2014-12-19 | 2018-04-05 | Eckart Gmbh | Pigmentos de efecto de gran transparencia, gran cromatismo y gran brillantez, procedimiento para su preparación y uso de los mismos |
SI3034562T2 (sl) * | 2014-12-19 | 2022-04-29 | Eckart Gmbh | Absorbirni efektni pigmenti z visoko kromatičnostjo in visokim sijajem, postopek za njihovo pripravo in njihova uporaba |
FR3065641B1 (fr) * | 2017-04-26 | 2019-07-05 | L'oreal | Composition cosmetique conferant un teint naturel et un effet bonne mine |
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KR102246416B1 (ko) | 2019-08-02 | 2021-04-29 | 충남대학교산학협력단 | 도축 혈액을 이용한 다공성 소재 개질방법 및 이에 의해 개질된 다공성 소재 |
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- 2013-03-14 BR BR112015022544A patent/BR112015022544A2/pt not_active Application Discontinuation
- 2013-03-14 ES ES13877502.8T patent/ES2657234T3/es active Active
- 2013-03-14 MX MX2015012962A patent/MX2015012962A/es unknown
- 2013-03-14 WO PCT/US2013/031390 patent/WO2014142884A1/en active Application Filing
- 2013-03-14 KR KR1020157024946A patent/KR102049310B1/ko active IP Right Grant
- 2013-03-14 CA CA2904192A patent/CA2904192C/en active Active
- 2013-03-14 JP JP2016500042A patent/JP6223537B2/ja active Active
- 2013-03-14 EP EP13877502.8A patent/EP2970680B1/en active Active
- 2013-03-14 RU RU2015143693A patent/RU2619686C2/ru active
- 2013-03-14 CN CN201380074550.1A patent/CN105246982B/zh active Active
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Also Published As
Publication number | Publication date |
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EP2970680B1 (en) | 2017-11-08 |
BR112015022544A2 (pt) | 2017-08-22 |
EP2970680A1 (en) | 2016-01-20 |
JP2016513746A (ja) | 2016-05-16 |
CN105246982A (zh) | 2016-01-13 |
KR102049310B1 (ko) | 2019-11-28 |
CA2904192A1 (en) | 2014-09-18 |
KR20150127093A (ko) | 2015-11-16 |
JP6223537B2 (ja) | 2017-11-01 |
EP2970680A4 (en) | 2016-11-02 |
MX2015012962A (es) | 2015-12-01 |
RU2619686C2 (ru) | 2017-05-17 |
CA2904192C (en) | 2020-07-14 |
WO2014142884A1 (en) | 2014-09-18 |
RU2015143693A (ru) | 2017-04-19 |
ES2657234T3 (es) | 2018-03-02 |
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