CN101568601A - 新的棒状形式的c.i.颜料紫37 - Google Patents
新的棒状形式的c.i.颜料紫37 Download PDFInfo
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- CN101568601A CN101568601A CNA2007800462687A CN200780046268A CN101568601A CN 101568601 A CN101568601 A CN 101568601A CN A2007800462687 A CNA2007800462687 A CN A2007800462687A CN 200780046268 A CN200780046268 A CN 200780046268A CN 101568601 A CN101568601 A CN 101568601A
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- pigment
- oil
- pigment violet
- bar
- shaped form
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
本发明涉及新的棒状形式的C.I.颜料紫37，其制备方法和其用于着色高分子量有机材料的用途。棒状形式的C.I.颜料紫37的长度为0.5－30μm，宽度为0.05－1μm，特别是0.100－0.500μm，平均厚度为0.01－0.200μm，特别是0.03－0.100μm。
Description
本发明涉及新的棒状形式的C.I.颜料紫37
其制备方法和其用于着色高分子量有机材料的用途。
US 5,298,076公开了一种用于着色高分子量有机材料的方法，其包括将有效着色量的咔唑二噁嗪粗颜料(crude pigment)，即C.I.颜料紫23，比表面积为约2-20m2/g，平均粒度为0.5-20μm，结合到高分子量有机材料。该方法特别可用于产生多色效应和伪装效应并且用于汽车涂层。
DE102005008659涉及一种制备透明二噁嗪颜料如C.I.颜料紫37的方法，其包括在偏心振动研磨机中研磨粗二噁嗪颜料，所述偏心振动研磨机具有至少在振动元件处存储的研磨容器以及具有刚性地紧扣到研磨容器的激励器单元。
EP1199309A1涉及一种用于具有通式
的组成为C22H12Cl2N6O4的甲基取代的、苯并咪唑酮稠合的二噁嗪颜料或者其异构体或互变体的相转化方法，其包括用一定的有机溶剂处理式(1)的颜料。在这种相转化的过程中，形成4种新的结晶多晶型物，其被称为相II、IV、V和VI并且通过其X射线粉末衍射图表征。
WO9845757涉及通过辐照由辐射感光前体结构化的黑色-着色的高分子量有机材料，该材料的着色由着色的有机颜料(在辐照前其至少之一是潜在形式的)组成。
在WO9845757的实施例5中，描述了以下化合物
的合成，即C.I.颜料紫37的辐射感光前体，其用于着色高分子量有机材料。也就是说，通过旋涂玻璃板获得了包括前体的薄膜。薄膜被干燥并且前体通过UV光被转化为C.I.颜料紫37。
US3,472,844涉及式
的2，6-苯甲酰基氨基-3，7-二乙氧基-9，10-二乙酰氨基-三苯基二噁嗪的新的红紫色晶形(“β-变体”)。其可以通过以下方式获得：在由碱和/或水组成的添加剂的存在下在硝基苯中在高于150℃加热2，5-二乙酰氨基-3，6-二(2′，5′-二乙氧基-4′-苯甲酰基氨基)-1，4-苯醌达一段延长期间，或者在硝基苯中在高于160℃加热2，6-苯甲酰基氨基-3，7-二乙氧基-9，10-二乙酰氨基-三苯基二噁嗪的“α-变体”达一段延长期间。
JP56135556描述了一种制备式
的二噁嗪化合物，例如式
的化合物的方法，包括在极性非质子溶剂中在100-200℃加热式I
的二酰亚胺化合物[其中Ar是(被取代的)芳族残基；Y是卤素、酰氨基或酰氧基]。相比于传统的颜料，通过细分所述二噁嗪化合物获得的颜料在抗渗移性方面是更优良的。
根据应用实施例3，通过在喹啉中在150-160℃在对甲苯磺酰氯的存在下加热
获得了C.I.颜料紫37的绿色晶体。
现在令人惊讶地发现，粗C.I.颜料紫37，已知以颗粒尺寸为0.5-1μm的同分异构的(isometric)颗粒形式存在，可以容易且有效地通过在极性溶剂中在高温下再结晶粗C.I.颜料紫37而转化为具有棒状形式的“效果”颜料。
因此，本发明涉及棒状形式的C.I.颜料紫37。棒状形式的C.I.颜料紫37的长度为0.5-30μm，尤其1-30μm，宽度为0.05-1μm，尤其0.100-0.500μm，和平均厚度为0.01-0.200μm，尤其0.03-0.100μm。新的色彩性能由C.I.颜料紫37获得，例如，在松弛(remission)和透光(transmission)中的不同颜色或者取决于视角而显现不同颜色。因此，其注定用作效果颜料，例如在安全应用中。
与这种颜料的常规的应用范围(颗粒尺寸～50nm)不同，新的颜料仅仅在其新的且非常大的结晶尺寸中是令人感兴趣的。
另外，本发明涉及一种制备棒状形式的C.I.颜料紫37的方法，其包括
(a)在高温在极性溶剂中分散和部分溶解粗C.I.颜料紫37达规定的一段时间。
通常，将混合物的温度降低到20-40℃以抑制进一步的结晶。
如果以1mm辊轧的PVC薄片的形式结合，如应用实施例1中举例说明的，根据本发明可获得的棒状形式的C.I.颜料紫37(1.0％颜料)的特征在于：
-在透光(transmission)中的颜色是紫色，
-在松弛(remisson)中的颜色从绿色变化到褐色和然后黑色，这取决于晶体长度。
这意味着，通过改变颜料在NMP中的停留时间(从1分钟到12小时)，获得了新的色彩性能，即，在松弛(remisson)中的颜色从绿色变化到褐色和然后黑色，这取决于晶体长度。在所有情况中，在透光(transmission)中的颜色是紫色。
图1是本申请的实施例1中获得的并且在透光(transmission)中具有紫色颜色和在松弛(remission)中具有绿色颜色的棒状形式的C.I.颜料紫37的显微照片。
图2是本申请的实施例1中获得的并且在透光(transmission)中具有紫色颜色和在松弛(remission)中具有褐色颜色的棒状形式的C.I.颜料紫37的显微照片。
通过在高温在极性溶剂中分散和部分溶解粗C.I.颜料紫37进行了制备棒状形式的C.I.颜料紫37的新方法。高温是指从100℃到溶剂回流温度的温度，尤其是从120℃到溶剂回流温度的温度。
所期望的棒状形式的C.I.颜料紫37是完全通过将温度维持在某一水平达规定的时间(优选地120℃至回流和1分钟至12小时)获得的。然后，将温度降低，优选地至0-50℃，尤其至20-40℃，借此抑制了进一步的结晶。然后冷却悬浮液至室温，过滤，用水洗涤滤液并且干燥颜料。
原料粗C.I.颜料紫37是常规的市售可得的同分异构的(isometric)粗C.I.颜料紫37，其颗粒尺寸为0.5-1μm。
合适的极性溶剂是N，N，N′，N′-四甲基脲，N，N-二甲基乙酰胺，N-甲基甲酰胺和N，N-二甲基甲酰胺(DMF)和N-甲基-吡咯烷酮(NMP)。N，N-二甲基甲酰胺和N-甲基-吡咯烷酮是优选的并且N-甲基-吡咯烷酮是最优选的。
粗C.I.颜料紫37与溶剂的摩尔比是1∶270-1∶27，尤其1∶133-1∶33。
溶剂的量取决于溶剂的极性，即C.I.颜料紫37在溶剂中的溶解度。
如果溶剂是NMP，基于每份颜料，NMP的含量为3-30重量份，尤其4-20重量份。
制备棒状形式的C.I.颜料紫37的新方法更详细地相对于NMP作为溶剂来举例说明，但不局限于此。
加热NMP和粗C.I.颜料紫37的混合物至约170℃-NMP的回流温度的温度并且在所述温度搅拌1分钟至12小时。将混合物的温度降低到20-40℃以抑制进一步的结晶。然后冷却悬浮液至室温，过滤，用水洗涤滤液而除去NMP并且干燥颜料。
通过改变颜料在NMP中的停留时间(从1分钟到12小时)，获得了新的色彩性能，即，在松弛(remisison)中的颜色从绿色变化到褐色和然后黑色，这取决于晶体长度。在所有情况中，在透光(transmission)中的颜色保持强紫色。
本发明的生产方法使以简单方式可再生产地生产棒状形式的C.I.颜料紫37成为可能。本发明的棒状形式的C.I.颜料紫37显示出特定的形态，异色效果(color flop effect)和/或在松弛(remission)/透光(transmission)中的不同颜色，当在塑料、油漆、印刷油墨等中结合时，并且易于分散。
本发明的棒状形式的C.I.颜料紫37非常可用于许多目的，如着色塑料，玻璃，陶瓷产品，装饰化妆品制剂，尤其是涂层和油墨，包括印刷油墨，包括安全印刷油墨。所有的工业常用的印刷方法是合适的，例如，丝网印刷(screen printing)，凹版印刷(intaglio printing)，金粉印刷(bronzeprinting)，胶版印刷(flexographic printing)和胶印(offset printing)。有可能仅仅使用一种颜料，将两种颜色(紫色/绿色)或(紫色/褐色)结合在应用介质的基质中，该效果被认为是独特的。
对于这些应用，本发明的颜料也有利地可用于与透明和遮盖性(hiding)白色、彩色和黑色颜料和此外常规的发光颜料(基于金属氧化物涂层的云母)和金属颜料和已知的(视角闪色(goniochromatic))发光颜料混合。
根据本发明的颜料可用于所有的常规目的，例如用于着色聚合物本体，表面涂层(包括效果罩面漆，包括用于汽车领域的那些)和印刷油墨，和另外，例如，用于化妆品。这样的应用从参考著作中已知，例如：″Industrielle Organische Pigmente″(W.Herbst and K.Hunger，VCHVerlagsgesellschaft mbH，Weinheim/New York，2nd，完全修订版，1995).
可以使用按照本发明的颜料或颜料组合物的着色用高分子量有机材料可以是天然或合成来源的。高分子量有机材料通常具有分子量约103-108g/mol或甚至更高。它们可以是，例如，天然树脂，干燥油，橡胶或酪蛋白，或由其衍生的天然物质，如氯化橡胶，油改性的醇酸树脂，粘胶，纤维素醚或酯，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，但尤其例如其通过聚合、缩聚或加聚得到的完全合成的有机聚合物(热固性塑料和热塑性塑料)。从聚合树脂的种类来看，可以提及尤其是聚烯烃，如聚乙烯，聚丙烯或聚异丁烯，以及取代的聚烯烃，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合反应产物，如尤其ABS或EVA。
从一系列的加聚树脂和缩聚树脂来看，可以提及甲醛与酚类的缩合产物(所谓的酚醛塑料)，和甲醛与脲，硫脲或蜜胺的缩合产物(所谓的氨基塑料)，和用作表面涂层树脂的聚酯(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，聚氨酯或硅酮。
所述高分子量化合物可单独或作为混合物以塑料本体或熔体的形式存在。它们也可以其单体形式或在聚合态下以溶解形式作为用于表面涂层或印刷油墨的成膜剂或基料，例如，熟亚麻仁油(boiledlinseedoil)，硝化纤维，醇酸树脂，蜜胺树脂和脲-甲醛树脂或丙烯酸树脂存在。
根据预期用途，已经证实有利的是使用按照本发明的颜料或颜料组合物作为调色剂或制剂。根据调理方法或预期用途，可以有利地在调理工艺之前或之后将一定量的纹理改进剂加入颜料中，前提是这对(效果)颜料用于着色高分子量有机材料，尤其聚乙烯没有不利影响。合适的试剂尤其是，包含至少18个碳原子的脂肪酸，例如硬脂酸或山萮酸(behenic acid)，或其酰胺或金属盐，尤其镁盐，以及增塑剂，蜡，树脂酸，如松香酸，松香皂，烷基酚类或脂族醇，如硬脂基醇，或包含8-22个碳原子的脂族1，2-二羟基化合物，如1，2-十二烷二醇，以及改性的松香马来酸酯树脂或富马酸松香树脂。纹理改进剂的加入量基于最终产物优选为0.1-30重量％，尤其2-15重量％。
按照本发明的颜料可以任何着色(tinctorially)有效量加入到被着色的高分子量有机材料中。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％的根据本发明的颜料的着色物质组合物是有利的。通常可以使用的浓度是1-20重量％，尤其约10重量％。
高浓度，例如超过30重量％的浓度通常是可用作着色剂用于生产具有相对低颜料含量的着色材料的浓缩物(″母料″)形式，其中按照本发明的颜料在常规配方中具有特别低的粘度使得它们仍可很好地被处理。
为了着色有机材料，按照本发明的颜料可单独使用。但为了实现不同的色调或颜色效果，除了根据本发明的(效果)颜料，也可将任何所需量的其它颜色-赋予成分，如白色，着色，黑色或效果颜料加入高分子量有机物。当着色的颜料用于与按照本发明的(效果)颜料混合时，总量优选为0.1-10重量％，基于高分子量有机材料。
用按照本发明的颜料对高分子量有机物的着色，例如，通过将这种颜料(如果合适，为母料形式)与基材使用辊磨机或混合或研磨装置混合而进行。着色材料随后使用本身已知的方法，如压光(calendering)，压塑，挤塑，涂覆，倾倒或注塑而成为所需最终形式。常用于塑料工业的任何添加剂，如增塑剂，填料或稳定剂可在结合颜料之前或之后以常规量被加入聚合物中。尤其是，为了生产非刚性成型制品或降低其脆性，令人期望的是在成型之前将增塑剂，例如磷酸，邻苯二甲酸或癸二酸的酯加入高分子量化合物(compounds)。
对于着色表面涂层和印刷油墨，高分子量有机材料和按照本发明的颜料，如果合适与常规添加剂，例如，填料，其它颜料，干燥剂或增塑剂一起，细分散或溶解在相同的有机溶剂或溶剂混合物中，其中各个组分可单独溶解或分散或多个组分在一起溶解或分散，和仅在此之后将所有的组分结合在一起。
按照本发明的颜料在被着色的高分子量有机材料中的分散以及对按照本发明的颜料组合物的处理优选在这样的条件下进行：仅出现相对弱的剪切力，这样效果颜料不会破碎成较小部分。
例如在塑料，表面涂层或印刷油墨中，尤其在表面涂层或印刷油墨中，更尤其在表面涂层中获得的着色以优异的性能而著称，尤其是非常高的饱和度，突出的牢固性能，依赖于角度的变色(色移)和在松弛(remission)和透光(transmission)中的不同颜色，当用于塑料中时。
当被着色的高分子量材料是表面涂层时，它尤其是一种特殊性表面涂层，非常特别是汽车罩面漆。
由于其不可复制的光学效果，按照本发明的颜料有利地用于从纸和塑料来生产防假冒的材料。术语由纸制造的防假冒的材料是指，例如，有价证券，如钞票，支票，印花，邮票，铁路运输与空运票券，彩票，礼券，进门卡，表格和股票。术语由塑料制造的防假冒的材料是指，例如，支票卡，***，电话卡和身份证。为了获得最佳的光学效果，在处理期间应当确保棒状形态的颜料良好取向，即尽可能与相应介质的表面平行排列。颜料颗粒的这种平行取向最佳地由流水作业来实施，通常在所有已知的塑性加工，涂漆，涂覆和印刷的方法中完成。
按照本发明的颜料还适用于化妆嘴唇或皮肤和用于着色毛发或指甲。
本发明因此还涉及一种化妆品制剂或配方，其包含0.0001-90重量％的根据本发明的颜料和10-99.9999％的化妆品合适的载体材料，基于化妆品制剂或配方总重。
这样的化妆品制剂或配方是，例如，唇膏，腮红(blushers)，粉底(foundations)，指甲油和洗发剂。
颜料可单独或以混合物形式使用。另外，可以将按照本发明的颜料与其它颜料和/或着色剂一起，例如按照以上描述或在化妆品制剂中已知的组合使用。
按照本发明的化妆品制剂或配方优选包含基于制剂总重0.005-50重量％的根据本发明的颜料。
适用于按照本发明的化妆品制剂或配方的载体材料包括常用于这些组合物的材料。
按照本发明的化妆品制剂或配方可以是例如，棒，软膏，乳膏，乳液，悬浮液，分散体，粉末或溶液的形式。它们是，例如，唇膏，染眉毛油制剂，腮红，眼影，粉底，眼线膏，粉末或指甲油的形式。
如果制剂是棒，例如唇膏，眼影，腮红或粉底的形式，该制剂由显著部分的脂肪组分组成，可由以下构成：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，鲸蜡基醇，硬脂基醇，可可脂，羊毛脂脂肪酸，矿脂，石油膏，单-，二-或三-甘油酯或其脂肪酯(在25℃下是固体)，硅酮蜡，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，松脂萜烷(colophane)和其衍生物，如二醇松香酸酯和甘油松香酸酯，在25℃下是固体的氢化油，糖甘油酯和油酸酯，肉豆蔻酸酯，羊毛酸酯(lanolates)，硬脂酸酯和钙，镁，锆和铝的二羟基硬脂酸盐。
脂肪组分也可由至少一种蜡和至少一种油的混合物组成，在这种情况下以下油，例如，是合适的：石蜡油，purcelline油，全氢角鲨烯(perhydrosqualene)，甜杏仁油，鳄梨油，胡桐油(calophyllum oil)，蓖麻油，芝麻油，霍霍巴油(jojoba oil)，具有沸点约310-410℃的矿物油，硅酮油，如二甲基聚硅氧烷，亚油基(linoleyl)醇，亚麻醇，油醇，谷粒油，如麦胚油，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，硬脂酸丁基酯，油酸癸基酯，乙酰基甘油酯，醇和多醇，例如二醇和甘油的辛酸酯和癸酸酯，醇和多醇，例如鲸蜡醇的蓖麻油酸酯，异硬脂基醇(isostearyl alcohol)，羊毛酸异鲸蜡基酯(isocetyl lanolate)，己二酸异丙基酯，月桂酸己基酯和辛基十二醇。
脂肪组分在棒形式的这些制剂中一般可占制剂总重的最高99.91重量％。
按照本发明的化妆品制剂和配方可以另外包含进一步的组分，例如二醇，聚乙二醇，聚丙二醇，单链烷醇酰胺，非着色聚合无机或有机填料，防腐剂，UV滤光剂或其它助剂和在化妆品中常见的添加剂，例如，天然或合成或部分合成二-或三-甘油酯，矿物油，硅酮油，蜡，脂肪醇，Guerbet醇或其酯，亲油官能化妆品活性成分，包括防晒滤光剂，或这些物质的混合物。
适用于皮肤化妆品的亲油官能化妆品活性成分，活性成分组合物或活性成分提取物是被批准用于皮肤或局部用途的成分或成分的混合物。例如可以提及以下物质：
-在皮肤表面和毛发上具有清洁作用的活性成分；这些包括用于清洁皮肤的所有的物质，如油，皂，合成洗涤剂和固体物质；
-具有除臭和出汗抑制作用的活性成分：它们包括基于铝盐或锌盐的抗出汗剂，包含杀菌或抑菌除臭物质，例如三氯生，六氯酚，醇和阳离子物质，如，例如，季铵盐，和气味吸收剂，例如
(蓖麻油酸锌和各种添加剂的组合)或柠檬酸三乙酯(任选地与抗氧化剂，如，例如，丁基羟基甲苯结合)或离子交换树脂的防臭剂；
-提供针对日光保护的活性成分(UV滤光剂)：合适的活性成分是能够吸收日光的UV辐射并将它转化成热的滤光剂物质(防晒剂)；根据所需作用，以下的光保护剂是优选的：选择性地吸收在约280-315nm范围内的引起晒伤的高能UV辐射(UV-B吸收剂)和传输较长波长范围，例如，315-400nm(UV-A范围)的光保护剂，以及仅吸收UV-A范围315-400nm的较长波长辐射的光保护剂(UV-A吸收剂)；
合适的光保护剂是，例如，选自p-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物UV吸收剂，肉桂酸衍生物，樟脑衍生物，三苯氨基-s-三嗪衍生物，苯基苯并咪唑磺酸和其盐，氨基苯甲酸薄荷基酯，苯并***衍生物的有机UV吸收剂，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颜料；
-针对昆虫的活性成分(驱虫剂)是用于防止昆虫接触皮肤和在此变得活性的试剂；它们驱走昆虫和慢慢蒸发；最常用的驱虫剂是二乙基甲苯酰胺(DEET)；其它常见驱虫剂，例如，会见于以下文献中：″Pflegekosmetik″(W.Raab和U.Kindl，Gustav-Fischer-VerlagStuttgart/New York，1991)第161页；
-针对化学和机械影响进行保护的活性成分：这些包括在皮肤和外部有害物质之间形成隔绝层的所有物质，如，例如，用于针对水溶液进行保护的石蜡油，硅油，植物油，PCL产品和羊毛脂，用于保护不受有机溶剂影响的成膜剂，如藻酸钠，三乙醇胺藻酸酯，聚丙烯酸酯，聚乙烯基醇或纤维素醚，或作为″润滑剂″针对皮肤上的严重机械应力进行保护的基于矿物油，植物油或硅油的物质；
-润湿物质：以下物质，例如用作湿度控制剂(润湿剂)：乳酸钠，脲，醇，山梨醇，甘油，丙二醇，胶原，弹性蛋白和透明质酸；
-具有角质增生(keratoplastic)作用的活性成分：过氧化苯甲酰，视黄酸，胶体硫和间苯二酚；
-抗微生物剂，例如，三氯生或季铵化合物；
-可涂皮肤的油状或油溶性维生素或维生素衍生物：例如维生素A(游离酸或其衍生物形式的视黄醇)，泛醇，泛酸，叶酸，和其组合，维生素E(生育酚)，维生素F；必需脂肪酸；或烟酸胺(烟酰胺)；
-维生素基胞衣提取物：包含尤其维生素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：可得自双歧乳杆族菌(bifilar group bacteria)的灭活和分解的培养物；
-植物和植物提取物：例如山金车油，芦荟，内腔苔癣(beardlichen)，常春藤，小荨麻，人参，指甲花，白花母菊，万寿菊，迷迭香，鼠尾草，马尾或百里香；
-动物提取物：例如王浆，蜂胶，蛋白质或胸腺提取物；
-可涂皮肤的化妆品油：Miglyol 812型中性油，杏仁油，鳄梨油，巴巴苏油，棉子油，琉璃苣籽油，蓟油，花生油，γ-谷维素，玫瑰实种子油(rosehip-seed oil)，***籽油，榛子油，黑醋果子油，霍霍巴油(jojoba oil)，樱核油，鲑鱼油，亚麻子油，谷子油(cornseed oil)，昆士兰果油，杏仁油，月见草油，貂油，橄榄油，山核桃油，桃油，乳香黄连木油，菜油，稻种子油，蓖麻油，红花油，芝麻油，豆油，向日葵油，茶树油，葡萄子油或麦胚油。
棒形式的制剂优选为无水的但可在某些情况下包含一定量的水，但一般来说不超过基于化妆品制剂总重的40重量％。
如果按照本发明的化妆品制剂和配方是半固体产物形式，也就是说软膏或乳膏的形式，它们也可是无水或含水的。这样的制剂和配方是，例如，染眉毛油，眼线膏，粉底，腮红，眼影，或用于处理眼袋的组合物。
另一方面，如果这样的软膏或乳膏是含水的，它们尤其是油包水型或水包油型乳液，除了颜料，它包含1-98.8重量％的脂肪相，1-98.8重量％的水相和0.2-30重量％的乳化剂。
这样的软膏和乳膏也可包含其它的常规添加剂，例如，香水，抗氧化剂，防腐剂，胶凝剂，UV滤光剂，着色剂，颜料，珠化剂，非着色聚合物以及无机或有机填料。
如果制剂是粉末形式，它们基本上由矿物或无机或有机填料例如，滑石，高岭土，淀粉，聚乙烯粉末或聚酰胺粉末，以及助剂如粘结剂，着色剂等等组成。
这样的制剂也可包含各种常用于化妆品的助剂，如香料，抗氧化剂，防腐剂等等。
如果按照本发明的化妆品制剂和配方是指甲油，它们基本上由硝化纤维和天然或合成聚合物组成，其形式为在溶剂体系中的溶液，对于溶液来说可能包含其它助剂，例如珠化剂。
在该实施方案中，着色聚合物的存在量是约0.1-5重量％。
按照本发明的化妆品制剂和配方也可用于着色毛发，在这种情况下以洗发剂，乳膏或凝胶的形式使用，后者由常用于化妆品工业的基础物质(base substances)和根据本发明的颜料组成。按照本发明的化妆品制剂和配方按照常规方式，例如通过将组分混合或搅拌在一起，任选地加热使得混合物熔化而制成。
本发明的各种特征和方面进一步在以下实施例中举例说明。虽然这些实施例的给出是为了显示给本领域技术人员如何在本发明范围内进行操作，但是它们不应视为对本发明的范围的限制，其中这样的范围仅仅在权利要求中限定。除非另有陈述，在以下实施例中和在说明书和权利要求的其它地方，全部份数和百分数是按照重量计的，温度是摄氏度，压力为大气压或近似大气压。
实施例
按照DIN 53 775第7部分，使用受压PVC板(1mm厚)，含有1.0wt％的棒状形式的C.I.颜料紫37，制备分析样品，来测量色调值h和饱和度C*以及遮盖力ΔE*S/W。
使用Minolta CM 3610d分光光度计(d/8几何结构，包括光泽，发光体D65，观察器10°)和B&W Leneta卡，进行在松弛(remission)和透光(transmission)中的所有颜色测量。使用Datacolor FX 10和B&WLeneta卡进行全部“依赖于角度”的测量。
实施例
实施例1
在室温下将10g的粗C.I.颜料紫37分散在100ml的N-甲基-吡咯烷酮(NMP)中。然后使用油浴将混合物加热至190℃并且保持该温度15分钟。将反应冷却至30℃并且通过过滤分离新形成的晶体。使用100ml的水，通过洗涤滤饼除去保留在颜料中的NMP。然后，在60℃在真空烘箱中干燥颜料。
通过经由温热压光(160℃；参照应用实施例1)将1％的干燥粉末分散在99％的PVC中，在松弛(remission)中观察到绿色颜色，在透光(transmission)中效果是紫色。
通过在高温下改变颜料的停留时间，观察到其它颜色。
| 停留时间 | 在松弛中的颜色 | 在透光中的颜色 |
| 1分钟 | 淡绿色 | 紫色 |
| 15分钟 | 暗绿色 | 紫色 |
| 3小时 | 褐色 | 紫色 |
| 12小时 | 黑色 | 紫色 |
应用实施例1
测量0.35mm辊轧的PVC薄片的颜色：
-预混：
0.4g颜料与14.0g的基础混合物混合30分钟，然后与26.0g的聚氯乙烯(PVC)(
SH 7020，EVC GmbH)慢慢地搅拌。基础混合物由以下组成：增塑剂(12.9g
10P(邻苯二甲酸二-2-丙基庚基酯，BASF)，0.6g
39(过氧化的大豆油，Witco VinylAdditives GmbH)和0.5g Mark BZ 561(Crompton Vinyl AdditivesGmbH)。
-生产辊轧的薄片：
根据以下所述，在160℃的辊温度(各个辊)下，在2辊研磨机(Collin型，D-85560 Ebersberg)中辊轧以上获得的PVC和颜料/基础混合物的混合物：
a)热辊轧6分钟(每分钟转动辊轧薄板，辊夹口(roll nip)0.35mm)。
Claims (10)
1.一种棒状形式的C.I.颜料紫37。
2.一种棒状形式的C.I.颜料紫37，其长度为0.5-30μm，宽度为0.05-1μm，特别是0.100-0.500μm，和平均厚度为0.01-0.200μm，特别是0.03-0.100μm。
3.一种制备权利要求1的棒状形式的C.I.颜料紫37的方法，其包括
(a)在高温下在极性溶剂中将粗C.I.颜料紫37分散和部分溶解达规定的一段时间，其中所述极性溶剂选自N，N，N′，N′-四甲基脲、N，N-二甲基乙酰胺、N-甲基甲酰胺、N，N-二甲基甲酰胺(DMF)和N-甲基-吡咯烷酮(NMP)，和其中高温是指100℃至溶剂的回流温度的温度。
4.权利要求3的方法，其中溶剂是N-甲基-吡咯烷酮。
5.权利要求4的方法，其中在步骤(a)中颜料被加热到120℃至回流温度。
6.权利要求3的方法，其中粗C.I.颜料紫37与溶剂的摩尔比是1∶133-1∶33。
7.棒状形式的C.I.颜料紫37，其可根据权利要求3-6中任一项的方法获得。
8.高分子量有机材料，其包含有效着色量的权利要求1、2或7中任一项的棒状形式的C.I.颜料紫37。
9.一种用于着色高分子量有机材料的方法，其包括将有效着色量的权利要求1、2或7中任一项的棒状形式的C.I.颜料紫37结合到所述有机材料中。
10.一种防假冒的材料，其包括权利要求1、2或7中任一项的棒状形式的C.I.颜料紫37。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| EP06126131.9 | 2006-12-14 | ||
| EP06126131 | 2006-12-14 |
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| Country | Link |
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| US (1) | US20110009536A1 (zh) |
| EP (1) | EP2092020A2 (zh) |
| JP (1) | JP2010513579A (zh) |
| KR (1) | KR20090099564A (zh) |
| CN (1) | CN101568601A (zh) |
| WO (1) | WO2008071585A2 (zh) |
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| CN102863818B (zh) * | 2012-09-18 | 2014-05-14 | 杭州红妍颜料化工有限公司 | 一种颜料紫3的制备方法 |
| IN2013MU01990A (zh) | 2013-06-11 | 2015-05-29 | Keki Hormusji Gharda |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3472844A (en) * | 1965-10-28 | 1969-10-14 | Ciba Ltd | Modification of 2:6-dibenzoylamino-3:7 - diethoxy - 9:10 - diacetylamino-triphendioxazine |
| JPS5950260B2 (ja) * | 1980-03-27 | 1984-12-07 | 住友化学工業株式会社 | ジオキサジン化合物の製法 |
| US4481358A (en) * | 1981-04-10 | 1984-11-06 | Sumitomo Chemical Company, Limited | Process for producing dioxazine violet pigment |
| US4801702A (en) * | 1985-11-06 | 1989-01-31 | Ciba-Geigy Corporation | Process for the preparation and conditioning or organic pigments |
| EP0968250B1 (en) * | 1997-01-27 | 2001-04-18 | Ciba SC Holding AG | Soluble chromophores having improved solubilising groups |
| AU7211498A (en) * | 1997-04-09 | 1998-10-30 | Ciba Specialty Chemicals Holding Inc. | Black-pigmented structured high molecular weight material |
| US6027866A (en) * | 1997-11-07 | 2000-02-22 | Fuji Photo Film Co., Ltd. | Silver halide photographic element |
| DE10052221A1 (de) * | 2000-10-21 | 2002-05-02 | Clariant Gmbh | Verfahren zur Herstellung neuer Kristallmodifikationen eines methylsubstituierten Benzimidazolon-Dioxazin-Pigmentes |
| DE102005008659A1 (de) * | 2005-02-25 | 2006-08-31 | Clariant Produkte (Deutschland) Gmbh | Verfahren zur Herstellung transparenter Dioxazinpigmente |
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2007
- 2007-12-04 JP JP2009540712A patent/JP2010513579A/ja not_active Withdrawn
- 2007-12-04 CN CNA2007800462687A patent/CN101568601A/zh active Pending
- 2007-12-04 KR KR1020097014704A patent/KR20090099564A/ko not_active Application Discontinuation
- 2007-12-04 WO PCT/EP2007/063208 patent/WO2008071585A2/en active Application Filing
- 2007-12-04 US US12/517,888 patent/US20110009536A1/en not_active Abandoned
- 2007-12-04 EP EP07847718A patent/EP2092020A2/en not_active Withdrawn
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| Publication number | Publication date |
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| US20110009536A1 (en) | 2011-01-13 |
| KR20090099564A (ko) | 2009-09-22 |
| EP2092020A2 (en) | 2009-08-26 |
| WO2008071585A3 (en) | 2008-07-31 |
| JP2010513579A (ja) | 2010-04-30 |
| WO2008071585A2 (en) | 2008-06-19 |
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