CN1662594A - 紫外稳定化粒子 - Google Patents

紫外稳定化粒子 Download PDF

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Publication number
CN1662594A
CN1662594A CN038148897A CN03814889A CN1662594A CN 1662594 A CN1662594 A CN 1662594A CN 038148897 A CN038148897 A CN 038148897A CN 03814889 A CN03814889 A CN 03814889A CN 1662594 A CN1662594 A CN 1662594A
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Prior art keywords
pigment
particle
polymkeric substance
stable
stabilizer
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CN038148897A
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CN100475895C (zh
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A·胡贝尔
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Merck Patent GmbH
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Merck Patent GmbH
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    • 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
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20—Halogens; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/496—Triazoles or their condensed derivatives, e.g. benzotriazoles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
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    • C04B14/30—Oxides other than silica
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  • Inorganic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Paints Or Removers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Cosmetics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

本发明涉及紫外稳定化粒子，其特征在于，它们反射或吸收具有波长为290－500nm的光。本发明另外涉及一种生产根据本发明的粒子的方法以及该粒子用于表面涂料、水性涂料、粉末涂料、油漆、印刷油墨、安全印刷油墨、塑料、混凝土中，用于化妆品配方中，用于农业覆膜和帐篷帆布中，用于纸和塑料的激光标记，用作光保护，和用于制备颜料组合物和干制剂的用途。

Description

紫外稳定化粒子
本发明涉及紫外稳定化粒子，其特征在于它们反射或吸收具有波长为290-500nm的光。
表面涂料一般提供有紫外过滤器，其以粉末或液体形式添加到涂料中。在塑料或粉末涂料的情况下，通过将这些过滤器添加到待挤出的批料中而实现保护。经常可建议另外向表面涂料或粉末涂料中添加叔胺，例如2，2，6，6-四甲基哌啶。表面涂料、粉末涂料或塑料的紫外保护也经常是必需的，因为其中存在的颜料或粒子具有不足够的紫外稳定性。例如，在用光，特别是紫外光照射BiOCl颜料时出现变灰色。因此，一般对以溶液或以组合物形式的BiOCl颜料提供有紫外吸收剂。但是，这种类型的溶液或组合物具有的缺点是，紫外吸收剂必须以相对于颜料为相对高的浓度加以应用，这导致在施涂介质中有多种缺陷。
本发明的目的因此是提供紫外稳定化粒子，其可以容易且无问题地引入施涂介质中并同时可以简单的方式生产。
令人惊奇地，现在已经发现，如果这些粒子的表面直接用紫外稳定剂涂覆，则粒子，例如BiOCl的光稳定性可以很大地提高。紫外吸收剂在此应该反射或吸收具有波长为250-500nm的光。紫外稳定剂向粒子表面上或在粒子表面上的施涂和固定与由粒子和紫外稳定剂组成的混合物相比，导致显著更大的紫外保护效率。同时，直接的紫外保护剂/粒子表面接触与直接用于表面涂料、粉末涂料和塑料中相比，导致明显更低的紫外保护剂浓度。此外，抑制了紫外保护剂在施涂介质中的扩散，这种扩散是导致表面涂料、粉末涂料和塑料方面多种缺陷的原因。与现有技术相反，这些耐紫外的粒子可以纯粉状应用于施涂介质中而不是作为溶液或组合物形式。
本发明因此涉及紫外稳定化粒子，其特征在于它们反射或吸收具有波长为290-500nm的光。
本发明另外涉及根据本发明的粒子的生产方法并涉及其用途，特别是在表面涂料、水性涂料、粉末涂料、油漆、印刷油墨、安全印刷油墨、塑料中和在化妆品配方中的用途。根据本发明的粒子另外还适用于制备颜料组合物和用于制备干制剂。
本领域技术人员已知的所有紫外光敏感的有机或无机粒子都可以通过根据本发明的方法加以稳定化。这些粒子可以是球形、针形或薄片状。粒子的尺寸本身不是关键的并可以匹配于特别的应用场合。一般，球形粒子具有直径为0.02-100μm，特别是0.03-20μm，并特别是0.05-1μm。针形的粒子具有长度为0.05-10μm，优选为0.05-5μm，特别是0.05-1μm。特别优选的底材是薄片状底材。合适的薄片状底材具有厚度为0.02-5μm，特别是0.1-4.5μm。在另外两个量程内的延伸通常为1-500μm，优选2-200μm，并特别是5-60μm。
合适的粒子是无机和有机颜料以及其混合物。
合适的无机粒子，例如未经涂覆或经一种或多种金属氧化物涂覆的并是填料的SiO2珠粒，荧光颜料，白色颜料，例如二氧化钛、锌白、油漆级氧化锌、铅白、硫化锌、锌钡白，黑色颜料，例如铁-锰黑、尖晶石黑和氧化铁黑，彩色颜料，例如氧化铬、氧化铬水合物绿、铬绿、钴绿、群青绿、钴蓝、群青蓝、铁蓝、锰蓝、群青紫、钴紫和锰紫、氧化铁红、硫硒化镉、钼酸盐红、群青红、氧化铁棕、混合棕、尖晶石和刚玉相、铬橙、氧化铁黄、镍-钛黄、铬-钛黄、镉-锌硫化物、铬黄、锌黄、碱土金属铬酸盐、拿浦黄和钒酸铋，磁性颜料，例如CrO2、Fe2O3、Fe3O4、Co改性铁氧化物、铁酸钡和纯铁颜料，石墨薄片，效应颜料，全息颜料和BiOCl。
所用的效应颜料优选是可商购的金属效应颜料，例如购自Flex的ChromaFair颜料，经涂覆或未经涂覆的铝薄片，金-青铜颜料，例如购自Eckart，经涂覆的氧化铁薄片，例如购自BASF的Paliochrom颜料，购自BASF的Sicopearl颜料和购自BASF的角异色性颜料，如例如在EP 0 753 545 A2中所述，以及珠光颜料和光干涉颜料-金属氧化物涂覆的云母薄片颜料-可例如得自Merck，Darmstadt，以商品名Iriodin。后者例如公开于德国专利和专利申请14 67 468、19 59998、20 09 566、22 14 545、22 15 191、22 44 298、23 13 331、25 22 572、31 37 808、31 37 809、31 51 343、31 51 354、31 51355、32 11 602、32 35 017、DE 38 42 330、DE 41 37 764、EP 0 608388、DE 196 14 637、DE 196 18 569。优选使用珠光颜料。特别地，应用TiO2和/或Fe2O3涂覆的云母颜料，SiO2薄片，Al2O3薄片，玻璃薄片，陶瓷薄片或无合成载体的薄片。
特别优选的无机颜料是BiOCl薄片，TiO2粒子，荧光颜料、全息颜料，导电和磁性颜料，金属效应颜料，例如基于铝薄片，和效应颜料，例如珠光颜料，光干涉颜料，角异色性颜料，基于薄片状底材，例如天然或合成云母、Al2O3、TiO2、SiO2、Fe2O3、玻璃或石墨薄片的多层颜料。优选的效应颜料是涂覆有TiO2(金红石或锐钛矿)的底材，例如TiO2涂覆的天然或合成云母，TiO2涂覆的SiO2、Al2O3、石墨、玻璃、Fe2O3，或金属薄片，特别是铝薄片。另外优选具有两个、三个或更多个层的多层颜料，其包含一个或多个TiO2层，和球形SiO2粒子，该SiO2粒子可以涂覆有一种或多种金属氧化物。
合适的源自染料索引(Colour Index)列表的有机颜料例如有单偶氮颜料C.I.颜料棕25，C.I.颜料橙5、13、36、67，C.I.颜料红1、2、3、5、8、9、12、17、22、23、31、48:1、48:2、48:3、48:4、49、49:1、52:1、52:2、53、53:1、53:3、57:1、251、112、146、170、184、210和245，C.I.颜料黄1、3、73、65、97、151和183；重氮颜料C.I.颜料橙16、34和44，C.I.颜料红144、166、214和242，C.I.颜料黄12、13、14、16、17、81、106、113、126、127、155、174、176和188；二苯并[cd，jk]芘-5，10-二酮颜料C.I.颜料红168，蒽醌颜料C.I.颜料黄147和177，C.I.颜料紫31；蒽素嘧啶颜料C.I.颜料红122、202和206，C.I.颜料紫19；喹啉酮颜料C.I.颜料黄138；二噁嗪颜料C.I.颜料黄138；二噁嗪颜料C.I.颜料紫23和37；黄烷士酮颜料C.I.颜料蓝60和64；异吲哚啉颜料C.I.颜料橙69，C.I.颜料红260，C.I.颜料黄139和185；异吲哚啉酮颜料C.I.颜料橙61，C.I.颜料红257和260，C.I.颜料黄109、110、173和185；异宜和蓝酮颜料C.I.颜料紫31，金属配合物颜料C.I.颜料黄117和153，C.I.颜料绿8；萘环酮(Perinone)颜料C.I.颜料橙43，C.I.颜料红194；苝颜料C.I.颜料黑31和32，C.I.颜料红123、149、178、17j9、190和224，C.I.颜料紫29；酞菁颜料C.I.颜料蓝15、15:1、15:2、15:3、15:4、15:6和16，C.I.颜料绿7和36；皮蒽酮颜料C.I.颜料橙51，C.I.颜料红216；硫靛颜料C.I.颜料红88和181，C.I.颜料紫38；三芳基碳鎓颜料C.I.颜料蓝1、61和62，C.I.颜料绿1，C.I.颜料红81、81:1和169，C.I.颜料紫1、2、3和27；苯胺黑(C.I.颜料黑1)；醛连氮黄(C.I.颜料黄101)以及C.I.颜料棕22和液晶聚合物(LCP颜料)。
特别优选有机颜料是偶氮颜料、液晶聚合物和荧光颜料。
还可以将不同种粒子/颜料的混合物通过根据本发明的方法加以稳定化。
上述粒子的耐紫外性通过向粒子表面施涂紫外保护剂或紫外稳定剂而显著提高。紫外保护剂/稳定剂向粒子表面上的固定优选通过结合聚合物或聚合物混合物将保护剂施涂到表面而实现。
粒子表面上的紫外保护剂/稳定剂的比例取决于待保护的粒子而定。粒子优选包含0.001-1000重量％，特别优选0.01-500重量％，并特别为0.1-100重量％，基于粒子。
根据本发明的BiOCl薄片在表面上包含例如5-70重量％，特别是10-50重量％的紫外稳定剂。
合适的紫外稳定剂是本领域技术人员已知的并可以商购，例如紫外吸收剂、紫外反射剂、紫外散射剂、抗氧剂、染料、炭黑粒子、自由基捕获剂、超微细钛。
合适的紫外吸收剂是例如苯并三唑、三嗪、草酰替苯胺、二苯甲酮、芳基化氰基丙烯酸酯，特别是羟基苯并三唑，如2-(3’，5’-双(1，1-二甲基苄基)-2’-羟基-苯基)苯并三唑，2-(2’-羟基-5’-(叔辛基)苯基)苯并三唑，2-(2’-羟基-3’-(2-丁基)-5’-(叔丁基)苯基)苯并三唑，双(3-2H-苯并三唑基)-2-羟基-5-叔辛基)甲烷，2-(4-己氧基-2-羟基-苯基)-4，6-二苯基-1，3，5-三嗪，和二苯甲酮2，4-二羟基二苯甲酮。
此外，合适的紫外吸收剂为炭黑，和紫外散射剂，例如cyanaralic酸衍生物。
可以应用的紫外保护剂同样还有自由基捕获剂。合适的自由基捕获剂为例如有机和无机硝基化合物，酚，例如对苯二酚，稠合的芳族化合物，位阻胺(HALS)。
特别合适的紫外反射保护剂是金属，纳米粒子，例如二氧化钛或氧化铁，二氧化钛和硫酸钡。这里术语纳米粒子用于意指具有尺寸＜300纳米，优选＜150纳米的有机、无机、金属粒子。
另外，也可以应用不同种紫外保护剂的混合物，其中不限制混合比例。特别优选为由自由基捕获剂和炭黑粒子组成的混合物。
特别优选的紫外稳定剂为2-羟基二苯甲酮，2-羟基苯基苯并三唑，2-羟基苯基三嗪，草酰替苯胺，三唑，三嗪，二氧化钛纳米粒子，氧化铁纳米粒子，炭黑，位阻胺(HALS)，和所述紫外稳定剂的混合物。
也可以为防止通过皮肤吸收而将紫外保护剂共聚，这是在化妆品产品方面特别期望的。
根据本发明的粒子可容易地生产。向待保护的粒子表面固定紫外保护剂是通过预先或同时沉淀一种适合的聚合物而进行，或者如果保护剂本身就是聚合物，则由其自身沉淀。
特别优选的方法是将紫外保护剂固定到具有LCST和/或UCST聚合物的粒子表面上。
LCST聚合物和UCST聚合物是在低温或升高的温度下可溶于溶剂中，而在升高温度或降低温度并达到所谓的LCST或UCST(分别是最低临界共溶温度或最高临界共溶温度)时作为分离相从溶液中沉积出来的聚合物。这种类型的聚合物例如描述于文献“Polymere”[聚合物]，H.-G.Elias，Hüthig und Wepf-出版社，Zug，1996，在第183页及后面几页上。
适用于本发明的LCST聚合物例如是WO01/60926A1中描述的那些。
特别合适的LCST聚合物是聚氧化乙烯(PEO)衍生物、聚氧化丙烯(PPO)衍生物，特别是丙烯酸酯改性的PEO-PPO-PEO三嵌段共聚物，聚甲基乙烯基醚、聚-N-乙烯基己内酰胺、乙基羟乙基纤维素、聚-N-异丙基丙烯酰胺和烯属硅氧烷聚合物。
合适的UCST聚合物特别有聚苯乙烯、聚苯乙烯共聚物和聚氧化乙烯共聚物。
基于最终产物，聚合物的含量是0.1-80重量％，优选1-30重量％，特别是1-20重量％。
紫外保护剂或其混合物可以直接施涂到待保护的表面并用LCST和/或UCST聚合物固定，或在一步中以与LCST和/或UCST聚合物的混合物形式施涂到表面并固定。
优选将紫外保护剂与可固定的聚合物或聚合物混合物，优选LCST和/或UCST聚合物混合，如需要，在溶剂存在下混合。将LCST聚合物/保护剂混合物在低于LCST的温度下溶解，而将UCST聚合物/保护剂溶液在高于UCST下溶解。一般，LCST温度是0.5-90℃，优选是35-80℃，而UCST温度是5-90℃，特别是35-60℃。然后，添加待稳定的粒子。随后，升高温度，一般为高于LCST或低于UCST约5℃，在此期间聚合物与紫外保护剂一起沉淀并沉积在粒子表面上。最后，以聚合物在粒子表面上交联的形式进行固定，其中聚合物不可逆地固定到粒子表面上。固定过程可以借助自由基、阳离子、阴离子方式或通过缩合反应进行。LCST或UCST聚合物优选借助自由基或通过缩合反应而加以交联。
为进行沉积层在水中的自由基交联(固定)，优选使用浓度为1-100重量％的过氧二硫酸钾或过氧二硫酸铵，基于用于涂层的烯属LCST或UCST聚合物。取决于聚合物的LCST或UCST温度，交联是在0-35℃下使用催化剂例如Fe(II)盐进行，或在40-100℃下通过自由基引发剂的直接热分解而进行。
优选将粒子与LCST或UCST聚合物的溶液掺混为分散体形式，其中优选使用与聚合物溶液相同的溶剂并将分散体的温度降低到低于LCST或UCST。但是，也可以进行粒子在LCST或UCST溶液中的直接分散。
如果在根据本发明的方法中需要溶剂，则溶剂的选择取决于所用聚合物的溶解性。溶剂优选是水或水混溶性有机溶剂。水混溶性溶剂也包括与水具有混溶性差距的溶剂。在这些情况下，混合比例以一定方式选择，使得发生可混溶。合适的溶剂的例子是一元醇和多元醇，例如甲醇、乙醇、正丙醇、异丙醇、二醇、甘油、丙二醇、聚乙二醇、聚丁二醇，和聚亚烷基二醇与甲醇、乙醇、丙醇和丁醇的单醚和二醚；醚，例如四氢呋喃、二噁烷、1，2-丙二醇丙基醚，1，2-丁烷-1-甲基醚，乙二醇单甲醚，二甘醇单甲醚；酯，例如乙酸甲酯，乙二醇或丙二醇与乙酸的单酯，丁内酯；酮，例如丙酮或甲乙酮；酰胺，例如甲酰胺，二甲基甲酰胺，二甲基乙酰胺，N-甲基吡咯烷酮和六甲基磷酸三酰胺；亚砜和砜，例如二甲亚砜和环丁砜，烷羧酸，例如甲酸或乙酸。
合适的溶剂特别是水，此外还有有机溶剂，例如醇和二醇。
LCST和/或UCST聚合物涂层特别优选完成为完全包覆粒子。
根据本发明的后处理进一步增加了粒子的化学稳定性并同时简化了粒子的操作，特别是引入各种施涂介质中。根据本发明的粒子具有增加的对在水性涂料中的絮凝的稳定性和对在有机涂料体系的情况下形成结构的稳定性。
紫外稳定化粒子另外具有非常好的气候稳定性，非常好的分散行为，并由于它们的稳定性而是非常适于非常宽变化范围的应用体系，特别是适于水性涂料和有机涂料。
紫外稳定化粒子与多种多样的配色体系相容，优选选自表面涂料，水性涂料，粉末涂料，油漆，印刷油墨，安全印刷油墨，塑料和化妆品配方的领域。根据本发明的粒子另外还适于纸和塑料的激光标记，如光保护，适于将混凝土着色和适于在农业领域中应用，例如用于温室覆膜(sheeting)，并例如适于将帐篷帆布着色。
不言而喻的是，根据本发明的粒子也可以有利地以与有机染料、有机颜料或其它颜料，例如透明和不透明的白色、彩色和黑色颜料的共混物形式，和与薄片状氧化铁，有机颜料，全息颜料，LCP(液晶聚合物)，和基于金属氧化物涂覆的云母、玻璃、Al2O3、石墨和SiO2薄片的常规的透明的彩色的和黑色的光泽颜料等的共混物形式而用于各种应用。根据本发明加以稳定化的粒子可以任何比例与可商购的颜料和填料混合。
根据本发明的粒子另外适于制备可流动的颜料组合物，和干制剂，例如粒剂、团块、香肠状物和丸剂等。颜料组合物和干制剂特征在于它们包含至少一种或多种根据本发明的粒子，粘结剂和非必要的一种或多种添加剂。
本发明还涉及该紫外稳定化粒子用于表面涂料、水性涂料、粉末涂料、油漆、印刷油墨、安全油墨、塑料、混凝土，另外用于化妆品配方中，用于纸和塑料的激光标记，用作防腐蚀方面的颜料，用于农业覆膜和帐篷帆布和用于制备颜料组合物和干制剂的用途。
本发明因此还涉及包含根据本发明的颜料制剂的配方。
下面的实施例意于更详细地解释本发明，但是不对本发明加以限制。
                         实施例
实施例1
实施例1a：BiOCl颜料的紫外稳定化
将0.25g苯并三唑衍生物(购自Ciba-Geigy的紫外吸收剂)与1.0g改性的LCST聚合物(基于聚氧化丙烯、聚氧化乙烯的三嵌段共聚物)混合并溶解在20ml 23℃下的蒸馏水中。随后，在200rpm下的溶解器中将20gBi-Flair83S糊剂(在分散体形式下的具有粒度为10-30μm的薄片状BiOCl颜料，购自Merck KGaA，德国的产品)搅拌入上述混合物中。将混合物在23℃下搅拌5分钟并加热到40℃。在40℃下另外搅拌混合物10分钟后，将1.0g过氧二硫酸钾加入，并将混合物加热到65℃并经过2h交联。将混合物冷却到室温，加入20ml水，并通过离心将颜料与液体分离。将此紫外稳定化的粒子用水洗涤并离心分离。然后向得到的颜料滤饼中加入足够的水直到在颜料糊剂中的固体浓度为约50％。
实施例1b：着色的水性涂料的制备
在每种情况下，用由实施例1a得到的经紫外稳定化的BiOCl颜料着色的水性涂料和用未经处理的BiOCl颜料着色的水性涂料通过将5g颜料糊剂(相应于2.5g颜料)搅拌加入15g丙烯酸酯/蜜胺基水性涂料中而制备。水性涂料由如下物质组成：
147.2g        Viacryl SC323 w/70SBB，Vianova
49.1g         Maprenal MF 501w/63EDGM，Clariant
14.3g         三乙胺
489.4g        蒸馏水
实施例1c：色彩测量
用于经各种着色的涂层样品的底材是玻璃试样载玻片。在125℃下的风扇辅助的炉中烘烤操作0.5h之久后，施涂到玻璃试样载玻片上的不透明的涂层的干层厚度为100μm。
在Xenotest(氙灯试验)中进行紫外曝光24h和45h。对颜料的损坏通过测量明度值L*的变化而用比色法确定。色彩测量使用45°测量几何学和Datacolor仪器进行。色彩测量的结果如表1中所示。
表1：涂层样品在紫外曝光24h和45h后的以％计的L*值降低
试验编号 着色涂层 24h 45h
1 用BiOCl颜料着色的涂层 -17.0％ -25.0％
2 用BiOCl颜料着色并有紫外保护剂在涂层中的涂层 -7.0％ -10.0％
3 用根据实施例1的经紫外稳定化的BiOCl颜料着色的涂层 -2.5％ -3.0％
BiOCl颜料在水性涂料中的耐紫外性的研究表明，借助使用LCST聚合物的包含紫外保护剂的涂层实现耐紫外性方面的显著改进。
实施例2
实施例2a：用炭黑对BiOCl颜料的紫外稳定化
将0.1g炭黑(特种黑350，Degussa-Hüls AG)与2.0g改性的LCST聚合物(聚氧化丙烯二丙烯酸酯)混合。随后，将混合物在Scandex中分散0.5h，并向其中加入40ml蒸馏水。将得到的颜料组合物简短地摇荡，并取出20ml，冷却到0.5℃并在溶解器中搅拌直到形成均匀的混合物。然后，将20gBi-Flair83S糊剂搅拌入上述混合物中。将混合物在0.5℃下搅拌15分钟并加热到23℃。另外将混合物搅拌1小时后，将溶解在20ml蒸馏水中的1g丙烯酸酯改性的PEO-PPO-PEO聚合物加入，并将混合物加热到50℃。然后添加在10ml水中的0.3g过氧二硫酸钾。将混合物加热到65℃并在此温度下经过2h交联。将混合物冷却到室温之后，加入20ml水，并通过离心将颜料与液体分离。将此紫外稳定化的颜料用水洗涤并离心分离。然后向通过离心得到的颜料滤饼中加入足够的水直到固体浓度为约50％。
实施例2b：着色的水性涂料的制备
类似于实施例1b，通过将5g颜料糊剂(相应于2.5g颜料)搅拌加入15g丙烯酸酯/蜜胺基水性涂料中而制备。
实施例2c：色彩测量
将经炭黑稳定化的BiOCl颜料的色彩变化与未改性的颜料在各自的涂层中进行比较。色彩测量的结果如表2中所示。
表2：涂层样品在紫外曝光12h后的以％计的L*值降低
试验编号 着色涂层 12h
1 用BiOCl颜料着色的涂层 -14.7％
2 用根据实施例2的经紫外稳定化的BiOCl颜料着色的涂层 -6.3％
与未稳定化的BiOCl颜料相比，经炭黑稳定化的BiOCl颜料具有明显更高的耐紫外性。

Claims (13)

1.紫外稳定化粒子，其特征在于，它们反射或吸收具有波长为290-500nm的光。
2.根据权利要求1的紫外稳定化粒子，其特征在于，该粒子在表面上用可固定的聚合物或聚合物混合物包覆，其中聚合物层包含或包括一种或多种紫外保护剂或紫外稳定剂。
3.根据权利要求1或2的紫外稳定化粒子，其特征在于，紫外保护剂或紫外稳定剂选自紫外吸收剂、紫外反射剂、紫外散射剂、抗氧剂、染料、炭黑粒子、自由基捕获剂、超微细钛及其混合物。
4.根据权利要求3的紫外稳定化粒子，其特征在于，紫外保护剂或紫外稳定剂选自二苯甲酮、三唑、三嗪、二氧化钛纳米粒子、氧化铁纳米粒子、炭黑、位阻胺(HALS)及其混合物。
5.根据权利要求1-4中任一项的紫外稳定化粒子，其特征在于该粒子包含0.001-1000重量％紫外保护剂或紫外稳定剂，基于粒子。
6.根据权利要求2的紫外稳定化粒子，其特征在于，通过在水和/或有机溶剂中沉淀而将聚合物施涂到粒子表面上。
7.根据权利要求1-6中任一项的紫外稳定化粒子，其特征在于，该粒子为薄片状、球形或针形。
8.根据权利要求1-7中任一项的紫外稳定化粒子，其特征在于，该粒子选自BiOCl薄片、TiO2粒子、荧光颜料、全息颜料、珠光颜料、光干涉颜料、多层颜料、金属效应颜料、角异色性颜料、导电和磁性颜料、有机颜料和偶氮颜料。
9.根据权利要求8的紫外稳定化粒子，其特征在于，所述珠光颜料、光干涉颜料、多层颜料和角异色性颜料基于天然或合成云母、Al2O3、TiO2、SiO2、Fe2O3、玻璃或石墨薄片。
10.一种生产根据权利要求1的紫外稳定化粒子的方法，其特征在于，将一种或多种紫外保护剂或紫外稳定剂直接施涂到待保护的粒子表面上并用随后施涂的聚合物或聚合物混合物固定，或在一步中以与一种或多种聚合物的混合物形式施涂到表面上并不可逆地固定。
11.根据权利要求10的方法，其特征在于，聚合物是LCST和/或UCST聚合物，或LCST和/或UCST聚合物的聚合物混合物。
12.根据权利要求1的紫外稳定化颜料用于表面涂料、水性涂料、粉末涂料、油漆、印刷油墨、安全印刷油墨、塑料、混凝土中，用于化妆品配方中，用于农业覆膜和帐篷帆布中，用于纸和塑料的激光标记，用作光保护，和用于制备颜料组合物和干制剂的用途。
13.包含根据权利要求1的紫外稳定化颜料的配方。
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CN112375400B (zh) * 2016-08-24 2022-09-09 东丽株式会社 黑色颜料及其制造方法、颜料分散液、感光性组合物及其固化物
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CN100475895C (zh) 2009-04-08
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AU2003293294A1 (en) 2004-04-19
DE10228186A1 (de) 2004-01-22
WO2004029144A2 (de) 2004-04-08
US20060155007A1 (en) 2006-07-13
AU2003293294A8 (en) 2004-04-19
EP1517951A2 (de) 2005-03-30
WO2004029144A3 (de) 2004-05-06

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