CN118055982A - 聚合物包封的TiO2复合颗粒和有机消光剂的水性分散体 - Google Patents
聚合物包封的TiO2复合颗粒和有机消光剂的水性分散体 Download PDFInfo
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Abstract
本发明涉及一种组合物以及用于制备该组合物的方法，该组合物包含聚合物包封的TiO2复合颗粒和有机消光剂的水性分散体。本发明的组合物可用于涂料组合物以改善涂料的耐损伤性。
Description
背景技术
本发明涉及一种组合物以及用于制备该组合物的方法，该组合物包含聚合物-包封的TiO2复合颗粒和有机消光剂的水性分散体。
在零售点销售的涂料通常通过分批方法大批生产，该分批方法包括研磨颜料和增量剂颗粒以形成固体分散体，然后在所谓的稀释阶段中将该分散体与粘结剂、增稠剂和其它添加剂合并。分批方法生产不同浓度颜料和增量剂的涂料基料，将该涂料基料输送到零售点，在零售点将着色剂添加到涂料中以满足消费者的需求。这种涂料生产的基本系统模型需要大量库存，并且由于使用固定量的TiO2而进一步处于不利地位，在这种情况下，需要灵活调整TiO2水平。例如，在着色剂需要比未着色涂料中存在的量低的量的TiO2来实现所需色调的情况下，需要添加过量的着色剂来平衡过量的TiO2。与使用过量TiO2和着色剂相关的不必要的成本以及制备最终涂料所需的额外时间是需要解决的基础系统模型中效率低下的示例。
基础系统模型的替代方案是销售点模型，在销售点模型中通过将粘结剂、颜料和增量剂组分从单独的储罐同时分配到涂料容器中，然后混合容器的内容物来制造多罐涂料。(参见US2003/0110101，第[0027]和[0028]段)。尽管这种销售点模型是对基本系统模型的改进，但它仍然是一种既依赖于将材料分配到容器中的速度又依赖于在容器中混合材料并稳定最终涂料的粘度所花费的时间的劳动和成本密集的分批方法。
因此，通过更有效和通用的方法制造多罐涂料将是有利的。
发明内容
本发明通过提供包含聚合物包封的TiO2复合颗粒、有机消光剂和流变改性剂的组合物来满足本领域的需要。
附图说明
图1是用于通过本发明的方法制造涂料的设备的示意图。
具体实施方式
本发明是包含聚合物包封的TiO2复合颗粒、有机消光剂和流变改性剂的组合物。
图1说明了用于实施本发明方法的优选设备的示例。在用于制备本发明组合物的方法的第一示例中，将储存在预涂料储罐(1)中的聚合物包封的TiO2复合颗粒和流变改性剂的水性分散体以及储存在预涂料储罐(2)中的有机消光剂和流变改性剂的水性分散体分别通过阀(13)和阀(12)进料到装配有混合挡板(7)的混合室(6)中，并混合以形成聚合物包封的TiO2复合颗粒和有机消光剂的水性分散体。混合室(6)优选为在线连续流动混合器，更优选为在线静态混合器。将储罐(1)和储罐(2)中的预涂料各自与合适的流变改性剂共混。例如，预涂料储罐(1)有利地含有ICI助洗剂或碱溶胀性乳液(ASE)，并且预涂料储罐(2)有利地含有ASE)，其示例包括聚丙烯酸，或疏水改性的碱溶胀性乳液(HASE)或羟乙基纤维素(HEC)。ICI助洗剂的商业示例是ACRYSOLTMRM-2020NPR HEUR流变改性剂(陶氏化学公司或其分支机构的商标)。
在用于制备本发明组合物的方法的第二示例中，将储存在预涂料储罐(1)中的聚合物包封的TiO2复合颗粒和流变改性剂的水性分散体、储存在预涂料储罐(2)中的有机消光剂和流变改性剂的水性分散体、以及储存在预涂料储罐(3)中的乳浊颜料-粘结剂杂化颗粒和流变改性剂的水性分散体同时进料到混合室(6)中并混合以形成聚合物包封的TiO2复合颗粒、有机消光剂和乳浊颜料-粘结剂杂化颗粒的水性分散体。
优选地，乳浊颜料颗粒是TiO2颗粒。预涂料储罐(3)任选地包含水溶性分散剂，诸如包含磺酸单体或其盐的结构单元以及基于该分散剂的重量计小于30重量％的丙烯酸或甲基丙烯酸的结构单元的聚合物。更具体地，水溶性分散剂包含50重量％至80重量％的磺酸单体或其盐的结构单元，其中磺酸单体是2-丙烯酰胺基-2-甲基丙磺酸或其盐、乙烯基磺酸或其盐、丙烯酸2-磺乙基酯、甲基丙烯酸2-磺乙基酯、丙烯酸3-磺丙基酯、甲基丙烯酸3-磺丙基酯、苯乙烯磺酸钠或2-丙烯-1-磺酸或其盐。
附加的材料诸如表面活性剂、分散剂、消泡剂、聚结剂、附加的增稠剂、有机乳浊颜料、防粘连添加剂、光引发剂和溶剂可以从预涂料储罐(5)中的任一个或所有储罐通过阀(14)、阀(16)和阀(17)中的任一个或所有阀进料到混合室(6)中。另选地，可能希望在任何预涂料中包含消泡剂、表面活性剂和聚结剂中的一种或多种。
着色剂是一类特殊的添加剂，需要特别小心。对于着色的涂料，将来自着色剂添加系统(8)的着色剂的一种或多种水性溶液或分散体通过阀(19)进料到混合室(6)中，形成最终的涂料，然后导入涂料容器(9)中。
聚合物包封的TiO2复合颗粒的水性分散体可以通过本领域已知的方法制备，例如，US 7,579,081、US 8,283,404、US 9,234,084和US 9,371,466。如通过动态光散射测量的聚合物包封的TiO2复合颗粒的z-平均粒度通常在200nm至500nm的范围内。聚合物包封的TiO2复合颗粒中的聚合物与TiO2的重量比通常在0.4:1至3:1的范围内。
如本文所用，术语“乳浊颜料-粘结剂杂化颗粒的水性分散体”是指a)多级聚合物颗粒的水性分散体，该多级聚合物颗粒包括1)水吸留核，所述水吸留核包含20重量％至60重量％的羧酸单体的盐的结构单元和40重量％至80重量％的非离子单烯属不饱和单体的结构单元；2)聚合物外壳，所述聚合物外壳具有在60℃至120℃的范围内的Tg；和3)叠加在所述外壳上的聚合物粘结剂层，其中所述聚合物粘结剂层具有不大于35℃的Tg并且包含至少一种单烯属不饱和单体的结构单元。合适的聚合物粘结剂材料的示例包括丙烯酸类、苯乙烯-丙烯酸类、乙烯基酯诸如乙酸乙烯酯和新癸酸乙烯酯，以及乙烯基酯-乙烯聚合物粘结剂。包含甲基丙烯酸甲酯的结构单元和一种或多种丙烯酸酯诸如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯或丙烯酸2-乙基己酯的结构单元的丙烯酸类粘结剂是特别优选的，苯乙烯-丙烯酸类粘结剂也是如此。
通过动态光散射测量的乳浊颜料-粘结剂杂化颗粒的z-平均粒度通常在300nm、或400nm、或450nm至750nm、或至700nm、或至600nm、或至550nm的范围内。乳浊颜料-粘结剂杂化颗粒的水性分散体可如US 7,691,942中所述制备。
合适的乳浊颜料包括折射率大于1.90的无机乳浊颜料。TiO2和ZnO是无机乳浊颜料的示例，优选TiO2。其它乳浊颜料包括有机乳浊颜料，诸如不透明聚合物(除了乳浊颜料-粘结剂杂化颗粒之外)，其可以从预涂料进料到混合器中以与聚合物包封的TiO2复合颗粒特定地混合。尽管有机乳浊颜料可用作无机乳浊颜料的替代物，但更希望使用有机乳浊颜料作为补充剂以增强无机乳浊颜料的效率。有机乳浊颜料可以从单独的添加剂罐添加到混合室中。ROPAQUETMULTRA不透明聚合物和AQACell HIDE 6299不透明聚合物是不透明聚合物的商业示例。
如本文所用，术语“有机消光剂”是指非成膜聚合物微球，如使用盘式离心光沉积仪(DCP)所测量的，该非成膜聚合物微球的中值重均粒度(D50)在0.7μm、或1μm、和/或2μm、和/或4μm，至30μm、或至20μm、或至13μm的范围内。这些有机聚合物微球优选地具有交联低Tg核，即具有如通过Fox方程式计算的不大于25℃、或不大于15℃、或不大于10℃的Tg的交联核。
有机聚合物微球的交联核优选地包含一种或多种单烯属不饱和单体的结构单元，所述单烯属不饱和单体的均聚物的Tg不大于20℃(低Tg单体)，诸如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯和丙烯酸2-乙基己酯。优选地，交联低Tg核包含基于核的重量计50重量％、或70重量％、或80重量％、或90重量％，至99重量％、或至97.5重量％的低Tg单烯属不饱和单体的结构单元。丙烯酸正丁酯和丙烯酸2-乙基己酯是用于制备低Tg核的优选的低Tg单烯属不饱和单体。
交联核进一步包括多烯属不饱和单体的结构单元，这些多烯属不饱和单体的示例包括甲基丙烯酸烯丙酯、丙烯酸烯丙酯、二乙烯基苯、三羟甲基丙烷三甲基丙烯酸酯、三羟甲基丙烷三丙烯酸酯、丁二醇(1,3)二甲基丙烯酸酯、丁二醇(1,3)二丙烯酸酯、乙二醇二甲基丙烯酸酯和乙二醇二丙烯酸酯。基于核的重量计，交联微球中多烯属不饱和单体的结构单元的浓度通常在1重量％、或2重量％，至9重量％、或至8重量％、或至6重量％的范围内。
交联聚合核优选地包覆有高Tg壳，即Tg为至少50℃、或至少70℃、或至少90℃的壳。壳优选地包括单体的结构单元，所述单体的均聚物的Tg大于70℃(高Tg单体)，诸如甲基丙烯酸甲酯、苯乙烯、甲基丙烯酸异冰片酯、甲基丙烯酸环己酯和甲基丙烯酸叔丁酯。高Tg壳优选地包含至少90重量％的甲基丙烯酸甲酯的结构单元。
基于聚合物包封的TiO2复合颗粒和有机消光剂的重量计，聚合物包封的TiO2复合颗粒在组合物中的浓度通常在10重量％、或40重量％、或60重量％至85重量％、或至80重量％的范围内；并且有机消光剂的浓度通常在5重量％或10重量％至76重量％或至40重量％的范围内。
本发明的组合物还可包含无机消光剂，该无机消光剂可从一个或多个单独的储罐进料至混合器中。无机消光剂的示例包括滑石、粘土、云母和绢云母；CaCO3；霞石正长岩；长石；硅灰石；高岭石；磷酸二钙；和硅藻土。
本发明的组合物还可以进一步包含不包封TiO2颗粒的另外的成膜聚合物颗粒。这些通常具有通过动态光散射测得的在50nm至600nm范围内的z-平均粒度的聚合物颗粒可以从胶乳预涂料储罐进料到混合器中。合适的聚合物分散体的示例包括丙烯酸、苯乙烯-丙烯酸、氨基甲酸酯、醇酸树脂、乙烯基酯(例如乙酸乙烯酯和叔碳酸乙烯酯)以及乙酸乙烯酯-乙烯(VAE)聚合物分散体以及它们的组合。如使用动态光散射所测量的，丙烯酸和苯乙烯-丙烯酸聚合物分散体通常具有在70nm至300nm范围内的z-平均粒度，而乙烯基酯胶乳通常具有在200nm至550nm范围内的z-平均粒度。如果希望将多于一种胶乳进料到混合室中，则优选从单独的胶乳预涂料储罐添加胶乳。
容易地预先确定包含在每个预涂料储罐中的流变改性剂的浓度和类型，以实现最终涂料的所需Brookfield、KU和ICI粘度。合适流变改性剂的示例包括疏水改性的环氧乙烷氨基甲酸酯聚合物(HEUR)；疏水改性的碱溶胀性乳液(HASE)；碱溶胀性乳液(ASE)；和羟乙基纤维素(HEC)和疏水改性的羟乙基纤维素(HMHEC)；以及它们的组合。
本发明的组合物可通过上文所述的在线混合方法以及通过本领域熟知的标准混合方法制备。本发明的在线混合方法提供了一种快速制备多种涂料的方式，在两次操作之间清洁最少。值得注意的是，在线混合的预涂料被分配到涂料容器中之后不需要进一步混合。
实施例
基本上如US 7,579,081实施例1中所述制备TiO2包封的聚合物颗粒的水性分散体(复合颗粒的水性分散体)；基本上如EP 2 586 835 B1实施例12中所述制备有机消光剂的水性分散体。表1说明含有和不含本发明组合物(分别为实施例1至3和比较例1至3)的涂料配方。在该表中，复合物颜料是指复合颗粒的归因于Ti-Pure R-706TiO2的部分；复合物粘结剂是指复合颗粒的归因于粘结剂的部分；复合物总是指复合颗粒和水的总重量；TiO2浆料是指Ti-Pure R-746TiO2浆料；胶乳是指RHOPLEXTMVSR-1050丙烯酸胶乳(49.5重量％固体)；聚结剂是指Texanol聚结剂；HEUR是指ACRYSOL RM-8W流变改性剂；并且小珠是指如上制备的微球的水性分散体。(RHOPLEX和ACRYSOL是陶氏化学公司(The Dow Chemical Company)或其附属公司的商标。)所有重量均以kg计，并且每种涂料的总体积为100L。
表1-涂料配方
金属标记测试程序：
使用1.5密耳鸟型涂胶棒(Bird draw-down bar)在Leneta form 5C不透明卡片上制备每种涂料的刮涂物，然后使涂料干燥过夜。取出3.5cm×11cm的经涂覆的卡片样品并将其放置在摩擦牢度测试仪(型号421，Satra Footware Technology Centre)上。使用铝箔覆盖的Veslic垫(Ar N°701垫，Swissatest公司，St Gallen，CH)和0.5kg砝码摩擦涂层的表面持续1至2个循环。目视评价涂层表面转移到涂层上的金属转移，并给出1至10的等级，其中等级1表示Al大量转移到涂层上，并且等级10表示没有金属转移。表2示出了金属标记测试的结果。
表2-金属标记测试结果
该数据示出了用本发明组合物配制的涂料在耐损伤性方面的显著改善。
Claims (7)
1.一种组合物，包含聚合物包封的TiO2复合颗粒、有机消光剂和流变改性剂。
2.根据权利要求1所述的组合物，其中基于所述聚合物包封的TiO2复合颗粒和所述有机消光剂的重量，TiO2包封的聚合物复合颗粒的浓度在10重量％至85重量％的范围内，并且基于所述聚合物包封的TiO2复合颗粒和所述有机消光剂的重量，所述有机消光剂的浓度在5重量％至76重量％的范围内；其中所述流变改性剂是HEUR。
3.根据权利要求2所述的组合物，其中所述有机消光剂包含中值重均粒度(D50)在0.7μm至30μm范围内的非成膜聚合物微球。
4.根据权利要求3所述的组合物，其中所述聚合物包封的TiO2复合颗粒中的所述聚合物与所述TiO2的重量比在0.4:1至3:1的范围内；其中基于所述聚合物包封的TiO2复合颗粒和所述有机消光剂的重量，所述TiO2包封的聚合物复合颗粒的浓度为在60重量％至80重量％的范围内，并且基于所述聚合物包封的TiO2复合颗粒和所述有机消光剂的重量，所述有机消光剂的浓度在10重量％至40重量％的范围内。
5.根据权利要求4所述的组合物，所述组合物还包含z-平均粒度在300nm至750nm范围内的乳浊颜料-粘结剂杂化颗粒。
6.根据权利要求4所述的组合物，所述组合物还包含未包封TiO2颗粒的成膜聚合物颗粒，其中所述成膜聚合物颗粒具有在50nm至600nm范围内的z-平均粒度。
7.根据权利要求1所述的组合物，所述组合物还包含一种或多种选自由以下项组成的组的附加组分：表面活性剂、分散剂、消泡剂、聚结剂、防粘连添加剂和光引发剂。
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