CN105874014B - 制备颜料糊的方法、水性电泳涂料、其用途、阳离子电泳涂覆方法和经涂覆的制品 - Google Patents
制备颜料糊的方法、水性电泳涂料、其用途、阳离子电泳涂覆方法和经涂覆的制品 Download PDFInfo
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- CN105874014B CN105874014B CN201380081298.7A CN201380081298A CN105874014B CN 105874014 B CN105874014 B CN 105874014B CN 201380081298 A CN201380081298 A CN 201380081298A CN 105874014 B CN105874014 B CN 105874014B
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
本发明涉及一种通过将至少一种由固体颗粒组成的颜料与研磨树脂在水和/或有机液体存在下混合而制备颜料糊的方法，其特征在于所述研磨树脂包含核‑壳颗粒在20℃下为液体的环氧预聚物中的分散体或者由该分散体组成，且所述核‑壳颗粒具有聚硅氧烷核和聚合物壳。本发明还涉及水性电泳涂料、其用途、阳离子电泳涂覆方法和经涂覆的制品。
Description
本发明涉及一种生产颜料糊的方法，包括将至少一种由固体颗粒组成的颜料与研磨树脂在水和/或有机液体存在下混合。本发明还涉及一种可由所述方法获得颜料糊、包含所述颜料糊的水性电泳涂料、所述电泳涂料的用途、阳离子电泳涂覆的方法和通过所述方法涂覆的制品。
颜料糊也称为研磨糊、研磨材料或漆浆。在漆和印刷油墨的制备期间，该漆浆包含含用于分散的颜料和填料，以及基料、溶剂和其分散所需添加剂的配制剂的一部分(Lexikon，Lacke und Druckfarben，Georg Thieme Verlag，第10版，1998)。因此，颜料糊用于包含可固化树脂体系的漆、清漆和印刷油墨的着色。
研磨树脂的作用是润湿颜料表面，且通过该润湿改善颜料颗粒在例如油墨和漆中的分散，更特别地改善在水基油墨和漆中的分散。此外，研磨树脂具有在油墨或漆的树脂体系固化时能与该树脂体系的组分反应且因此将颜料颗粒牢固地掺入完全固化的树脂中的反应性基团。就本发明而言，它们特别包含用于电泳涂料中的颜料糊。相对于优选应用领域中的典型标准研磨树脂，此处所述的研磨树脂的特征尤其在于如下事实：在铝表面的阴极电泳涂覆中，实现了漆缺陷(所谓的针孔)的减少。
通常处于载液中的分散体中的核-壳颗粒是用于提高树脂体系如胶粘剂、漆和涂料的强度和/或耐冲击性(所谓的增韧剂)的已知添加剂。
JP03-006296A公开了使用核-壳颗粒来制备消光的可阴极沉积电泳涂料组合物。所述颗粒由通过聚合疏水性单体、交联性单体和任选的“巧交联性(craft-crosslinking)”单体而获得且具有20-100％凝胶比例的疏水性聚合物核以及可通过聚合烯属不饱和羧酸和玻璃化转变温度低于30℃的单体而获得且具有10-35℃的Tg和“水分散性官能团”的亲水性聚合物壳组成。因此，该发明的目的是提供一种具有消光外观的阴极电泳涂料。
EP305060A2公开了一种制备核-壳颗粒的详细程序和基于多元醇树脂的可阳离子电泳沉积的树脂混合物，该混合物包含由此制得的核-壳颗粒。所述核-壳颗粒可通过聚合a)含羟基的α,β-烯属不饱和单体(权利要求2：具有其他聚醚或聚酯基团且具有端-OH的(甲基)丙烯酸酯)，b)多官能α,β-烯属不饱和单体，和c)不同于a)和b)的其他α,β-烯属不饱和单体而获得。所述核-壳颗粒通过首先仅聚合b)和c)，随后将剩余的b)和c)与a)一起聚合而获得。因此，核应由聚烯烃组成，而壳包含丙烯酸酯组分。
EP560189A2公开了选自包含核-壳聚合物的宽化学品范围的“合成树脂”。可额外存在交联剂、颜料和其他助剂。所述核-壳颗粒的其他细节在该文献的权利要求3和4给出：
根据权利要求3的方案：
所述核可通过聚合至少一种共轭二烯烃、至少一种乙烯基芳族单体和任选的具有至少一个非共轭双键的二-至多烯属不饱和单体而获得。所述壳可通过聚合至少一种乙烯基芳族单体、至少一种甲基丙烯酸烷基酯，和任选的其他丙烯酸酯和/或具有至少一个非共轭双键的二-至多烯属不饱和单体和/或“其他单体”而获得。因此，核应由聚烯烃组成，而壳包含丙烯酸酯组分。
根据权利要求4的方案：
所述核可通过聚合至少一种乙烯基芳族单体与(在每种情况下任选的)如下单体而获得：(甲基)丙烯酸烷基酯、具有至少一个非共轭双键的二-至多烯属不饱和单体和/或“其他单体”。第一壳可通过聚合至少一种共轭二烯烃、至少一种乙烯基芳族单体，和任选的具有至少一个非共轭双键的二-至多烯属不饱和单体，和/或“其他单体”而获得。第二壳可通过聚合至少一种乙烯基芳族单体、至少一种甲基丙烯酸烷基酯，和任选的其他丙烯酸酯和/或具有至少一个非共轭双键的二-至多烯属不饱和，和/或“其他单体”而获得。
因此，已知的是将具有聚烯烃核的核-壳颗粒用于漆(包括可阴极沉积的电泳涂料)中。然而，上述文献均未提及可能经常发生漆缺陷—所谓的针孔这一问题，尤其是在铝表面的阴极电泳涂覆中。针孔是漆饰面中的小孔，其导致腐蚀防护变劣。由于基于选择特定核-壳颗粒的本发明，该缺陷在很大程度上得以避免。本发明的另一优点是该特别选择的核-壳颗粒可易于掺入颜料糊中。
对比实验的目的是显示在以不同浓度使用具有不同核的核-壳颗粒下，涂料特性改善在多大程度上不同。更特别地，使用具有聚硅氧烷核的核-壳颗粒导致铝表面上的缺陷(所谓的针孔)显著减少，且腐蚀防护改善。
因此，本发明提供了一种开头所述类型的制备颜料糊的方法，其中所述研磨树脂包含核-壳颗粒在20℃下为液体的环氧预聚物中的分散体，或者由该分散体组成，且所述核-壳颗粒具有聚硅氧烷核和聚合物壳。
具有聚硅氧烷核和聚合物壳的核-壳颗粒可作为交易产品例如由Kaneka以KaneMX 960名称商购获得。所述产品包含颗粒于液体环氧树脂中的分散体。
有利地将通过本发明方法制得的混合物均化。在均化期间，颜料颗粒有利地通过引入机械能而粉碎至预先选择的粒度且分散。
所述核-壳颗粒的聚合物壳有利地包含聚(甲基)丙烯酸酯。
其中存在所述核-壳颗粒的液体环氧预聚物有利地具有150-300g/eq的环氧当量。
核-壳颗粒在20℃下为液体的环氧预聚物中的分散体有利地以使得完成的颜料糊包含1-6重量％核-壳颗粒的量使用，基于所述研磨树脂的总量。
本发明还涉及一种可通过权利要求1-6中一项或多项所述的方法获得的颜料糊。
本发明进一步涉及一种水性电泳涂料，其包含可阳离子电泳沉积的树脂体系和本发明的颜料糊。
所述的水性电泳涂料的树脂体系有利地包含环氧基单体或预聚物和至少一种用于环氧化物的固化剂。
在一个优选的实施方案中，本发明的电泳涂料呈微粒乳状液形式。
微粒乳状液是水、油相和一种或多种表面活性物质的分散体，其中存在于该分散体中的颗粒具有5-500nm的平均粒径。微粒乳状液被认为是亚稳定的(参见EmulsionPolymerization and Emulsion Polymers，Editors P.A.Lovell和Mohamed S.El-Aasser，John Wiley and Sons，Chichester，New York，Weinheim，1997，第700页及随后各页；Mohamed S.El-Aasser，Advances in Emulsion Polymerization and Latex Technology，30th Annual Short Course，第3卷，1999年6月7-11日，Emulsion Polymers Institute，Lehigh University，Bethlehem，Pennsylvania，U.S.A.)。正如其所称呼的那样，微粒乳状液广泛用于例如清洁产品、化妆品或身体护理产品的领域中，而且用于涂料组合物如电泳涂料中。
借助微粒乳状液聚合制备水性初分散体例如由国际专利申请WO82/00148和WO98/02466，或者德国专利申请DE19628143A1和DE19628142A2已知。在这些已知方法的情况下，单体可在各种低分子量、低聚或聚合疏水性物质或共稳定剂存在下共聚(参见DE19628142A2)。此外，可在微粒乳状液的单体液滴中引入在水中具有低溶解度的疏水性有机助剂如增塑剂，成膜助剂如聚结剂或其他有机添加剂(参见DE19628143A1)。WO82/00148描述了例如使用乳化剂来稳定其中所公开的乳液。
WO82/00148特别地公开了使用阳离子可调的乳化剂制备可阴极沉积的树脂乳液，所述乳化剂结合在颗粒的表面且赋予其正电荷，其在低于10的pH水平下稳定乳液。所述乳化剂可带有反应性基团，借此可将其在交联反应期间引入聚合物树脂体系中。对乳化剂明确给出的实例为脂肪族单胺和脂肪族二胺如牛油-和油基-伯胺的乙酸盐，或者牛油-和油基-二胺的乙酸盐。牛油-和油基-胺包含具有至少一个碳-碳双键的烃链。也可使用聚合物乳化剂，例如已与二乙醇胺反应且使用例如乙酸赋予阳离子性的环氧-酚醛加合物。WO82/00148的某些工作实施例中所用的辅助乳化剂为EthoduomeenTM T13，其为具有不饱和烃基的叔胺。根据生产商AkzoNobel的信息，所述化合物为N',N',N-三(2-羟基乙基)-N-牛油基-1,3-二氨基丙烷。根据WO82/00148的教导，所述阳离子配制的乳化剂是树脂体系的仅有阳离子组分。
在Grabs和Schmidt-Naake的研究(Macromol.Symp.2009，275-276，第133-141页)中，由甲基丙烯酸2-氨基乙酯盐酸盐和苯乙烯、丙烯酸丁酯和/或甲基丙烯酸丁酯出发且原位聚合，从而形成由于甲基丙烯酸氨基乙酯单体的正电荷而带有表面正电荷且因此稳定在分散体中的树脂颗粒而制备微粒乳状液。可用于制备所述分散体的阳离子辅助乳化剂为饱和鲸蜡基三甲基溴化铵，其具有季N原子且因此带有永久正电荷。在这两种情况下，正电荷被卤素阴离子补偿。
其他优点是本发明的电泳涂料包含至少30ppm，优选至少100ppm，更优选至少200ppm，更特别地至少250ppm呈溶解形式的铋，所述含量数据基于制剂整体且所述量以Bi计。
特别地，就所述涂料组合物中的铋总量而言，术语“铋”就本发明而言优选是指任选带电荷的—例如带正电荷的—各种价态的阳离子铋原子。此处，铋可以以三价形式(Bi(III))存在，或者替代或额外地可以以其他氧化态存在。铋的量在每种情况下以铋金属计。
以金属计的铋原子的量可借助电感耦合等离子体发射光谱法(ICP-OES)测定。
本发明的电泳涂料有利地包含总量为至少30ppm的铋，基于该电泳涂料的总重量；其中至少15ppm铋以溶解形式存在，基于该电泳涂料的总重量。
优选地，存在至少一部分三价铋。该铋可呈水合形式和/或呈至少一种溶解盐形式和/或呈配合物形式。
就本发明的涂料组合物而言，术语“存在于溶液中”优选意指在18-40℃的涂料组合物温度下，组分以溶解形式存在于涂料组合物中。
铋组分优选可由至少一种选自如下组的铋化合物获得：铋的氧化物、碱性氧化物、氢氧化物、碳酸盐、硝酸盐、碱式硝酸盐、水杨酸盐和碱式水杨酸盐，及其混合物。至少一种该铋化合物优选在水中在至少一种配位剂存在下至少部分反应。
本发明的电泳涂料有利地包含至少一种适于配位铋的至少双齿的配位剂。
本发明进一步涉及在权利要求8-10至少一项中所述的水性电泳涂料用于阳离子电泳涂覆金属表面，更特别地铝表面的用途。
本发明进一步涉及一种使用权利要求8-10任一项中所述的水性电泳涂料阳离子电泳涂覆金属表面，更特别地铝表面的方法。
所述方法有利地通过将金属表面，更特别地铝表面浸入本发明的水性电泳涂料中而在两个步骤中实施，且在第一步骤中施加1-50V的电压，在第二步骤中施加50-400V，但比第一步骤中所施加的电压高不小于10V的电压，且将各步骤中的电压分别在所述范围内保持至少10秒钟。
最后，本发明还涉及一种至少部分具有已通过本发明方法涂覆的金属表面，更特别地铝表面的制品。
适于制备所述经涂覆制品的导电基材是本领域技术人员已知且通常使用的所有该类基材。本发明所用的导电基材优选选自钢，优选选自冷轧钢、镀锌钢如浸镀锌钢、合金镀锌钢(如铝锌合金镀钢(Galvalume)、镀锌扩散处理钢(Galvannealed)或锌-5％铝-稀土合金镀钢(Galfan))的钢，和镀铝钢、铝和镁；铝是尤其合适的。其他合适的基材包括热轧钢、高强钢、Zn/Mg合金、Zn/Ni合金。特别合适的基材是用于生产的汽车车身部件或者整个车身。本发明的方法还可用于卷材涂覆。在使用所述导电基材之前，优选将基材清洁和/或脱脂。
本发明所用的导电基材可为用至少一种金属磷酸盐预处理的基材。本发明所用的导电基材或者可为铬酸盐化的基材。特别地，通常在基材已清洁之后且在浸涂之前实施的该磷酸盐化或铬酸盐化预处理是汽车工业中常用的预处理步骤。就此而言，尤其希望有利地从环境和/或经济角度设计任选实施的预处理。因此，例如可存在任选的预处理步骤，其中在用水性涂料组合物(A)涂覆之前，代替常规的三阳离子(trikation)磷酸盐化，省略镍组分，相反，在本发明所用的导电基材上实施二阳离子(dikation)磷酸盐化(包含锌和锰阳离子且不含镍阳离子)。
然而，有利的是可省略用金属磷酸盐如磷酸锌磷酸盐化或铬酸盐化而至少涂覆的该导电基材预处理。因此，在一个优选实施方案中，本发明所用的导电基材不是该磷酸盐化或铬酸盐化的基材。
在用本发明所用的水性电泳涂料涂覆之前，可用包含至少一种含至少一个Ti原子和/或至少一个Zr原子的水溶性化合物且包含至少一种作为氟离子源的含至少一个氟原子的水溶性化合物的含水预处理组合物，或者用包含可通过使至少一种含至少一个Ti原子和/或至少一个Zr原子的水溶性化合物与至少一种作为氟离子源的含至少一个氟原子的水溶性化合物反应而获得的水溶性化合物的含水预处理组合物预处理本发明所用的导电基材。
下文使用工作实施例更详细地阐述本发明。
工作实施例和对比实施例
对比实施例1：
●对比实施例：制备含水制剂以验证具有铋配合物的涂料性质
将42.60份40％阳离子电泳涂料分散体(520，获自BASFCoatings GmbH的市售产品)与49.94份DI水混合。然后，在搅拌下与1.34份L(+)-乳酸铋水溶液一起添加6.12份含水颜料制剂(520颜料糊，获自BASF CoatingsGmbH的市售产品)。
本发明的实施例2、3和4：
●实施例：改变颜料糊且制备含水制剂以验证具有铋配合物和含聚硅氧烷核的核-壳颗粒的涂料性质
制备基于用于电泳涂料的常规组合物(520颜料糊，获自BASFCoatings GmbH的市售产品)的配方的含水颜料糊。
在该颜料糊配制剂中，代替使用通常所用的基于固含量为1％、5％或10％的研磨树脂，且使用包含含聚硅氧烷核的核-壳颗粒的产品(KANE ACE MX 960)，且如上文所述制备含水颜料糊。在所述改进的颜料糊配制剂中，含核-壳颗粒的产品的比例为0.71％(实施例2)、3.54％(实施例3)和6.97％(实施例4)。
将42.60份40％阳离子电泳涂料分散体(520，获自BASFCoatings GmbH的市售产品)与49.94份DI水混合。
表1：测试浴的组成(所有数据以重量份计)
然后，在搅拌下与1.34份L(+)-乳酸铋水溶液一起添加6.12份上述含水颜料制剂。
结果：
表面质量/缺陷
通过测试使得特别地在铝表面上形成的灰色涂层中的缺陷变得可见。在该测试中，在根据规定涂覆和烘干的板上另外施加黑色电泳涂层。
在漂洗和烘干后，由于实际涂层在这些位置处具有孔，缺陷(针孔)呈黑色。通过对各测试板上1cm2内的缺陷计数而进行评价(表2)。
表2：所述测试板1cm2面积上的针孔数量
腐蚀控制
表3：在铝上进行10天CASS测试(根据DIN EN ISO 9227CASS的铜促进乙酸盐喷雾测试)后的腐蚀/层离结果
表4：在铝上42天丝状锈蚀测试(根据DIN EN 3665的丝状锈蚀)后的最长细丝
Claims (25)
1.一种通过将至少一种由固体颗粒组成的颜料与研磨树脂在水和/或有机液体存在下混合而制备颜料糊的方法，其中所述研磨树脂包含核-壳颗粒在20℃下为液体的环氧预聚物中的分散体或者由该分散体组成，且所述核-壳颗粒具有聚硅氧烷核和聚合物壳。
2.如权利要求1所述的方法，其中将所得混合物均化。
3.如权利要求2所述的方法，其中在均化期间，通过引入机械能将颜料颗粒粉碎至预先选定的粒度且分散。
4.如权利要求1所述的方法，其中所述核-壳颗粒的聚合物壳包含聚(甲基)丙烯酸酯。
5.如权利要求2所述的方法，其中所述核-壳颗粒的聚合物壳包含聚(甲基)丙烯酸酯。
6.如权利要求3所述的方法，其中所述核-壳颗粒的聚合物壳包含聚(甲基)丙烯酸酯。
7.如权利要求1-6中任一项所述的方法，其中在20℃下为液体的环氧预聚物具有150-300g/eq的环氧当量。
8.如权利要求1-6中任一项所述的方法，其中核-壳颗粒的分散体以使得完成的颜料糊包含基于研磨树脂总量为1-6重量％核-壳颗粒的量用于在20℃下为液体的环氧预聚物中。
9.一种通过如权利要求1-8中任一项所述的方法获得的颜料糊。
10.一种水性电泳涂料，其包含可阳离子电泳沉积的树脂体系和如权利要求9所述的颜料糊。
11.如权利要求10所述的水性电泳涂料，其中所述树脂体系包含基于环氧化物的单体或预聚物和至少一种用于环氧化物的固化剂。
12.如权利要求10所述的水性电泳涂料，其呈微粒乳状液的形式。
13.如权利要求11所述的水性电泳涂料，其呈微粒乳状液的形式。
14.如权利要求10-13中任一项所述的水性电泳涂料，其包含至少30ppm呈溶解形式的铋，基于全部制剂且以Bi计。
15.如权利要求14所述的水性电泳涂料，其包含至少100ppm呈溶解形式的铋，基于全部制剂且以Bi计。
16.如权利要求14所述的水性电泳涂料，其包含至少200ppm呈溶解形式的铋，基于全部制剂且以Bi计。
17.如权利要求14所述的水性电泳涂料，其包含至少250ppm呈溶解形式的铋，基于全部制剂且以Bi计。
18.如权利要求10-13中任一项所述的水性电泳涂料用于阳离子电泳涂覆金属表面的用途。
19.根据权利要求18的用途，其中所述金属表面为铝表面。
20.一种使用如权利要求10-13中任一项所述的水性电泳涂料阳离子电泳涂覆金属表面的方法。
21.根据权利要求20的方法，其中所述金属表面为铝表面。
22.如权利要求20所述的方法，其通过将金属表面浸入如权利要求11所述的水性电泳涂料中而在两个步骤中实施，且在第一步骤中施加1-50V的电压，在第二步骤中施加50-400V，但比第一步骤中高不小于10V的电压，且将各步骤中的电压分别在所述范围内保持至少10秒钟。
23.如权利要求22所述的方法，其中所述金属表面为铝表面。
24.一种制品，其具有至少部分通过权利要求20-23中任一项所述的方法涂覆的金属表面。
25.根据权利要求24的制品，其中所述金属表面为铝表面。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/EP2013/077808 WO2015090469A1 (de) | 2013-12-20 | 2013-12-20 | Verfahren zur herstellung einer pigmentpaste, wässriger elektrotauchlack, verwendung desselben, verfahren zur kataphoretischen elektrotauchlackierung und beschichteter gegenstand |
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| Publication Number | Publication Date |
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| CN105874014A CN105874014A (zh) | 2016-08-17 |
| CN105874014B true CN105874014B (zh) | 2018-05-25 |
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| CN201380081298.7A Expired - Fee Related CN105874014B (zh) | 2013-12-20 | 2013-12-20 | 制备颜料糊的方法、水性电泳涂料、其用途、阳离子电泳涂覆方法和经涂覆的制品 |
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| US (1) | US10174212B2 (zh) |
| EP (1) | EP3083836B1 (zh) |
| JP (1) | JP6325111B2 (zh) |
| CN (1) | CN105874014B (zh) |
| CA (1) | CA2931095A1 (zh) |
| MX (1) | MX2016008067A (zh) |
| WO (1) | WO2015090469A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015090442A1 (de) * | 2013-12-20 | 2015-06-25 | Basf Coatings Gmbh | Wässrige primärdispersionen, verfahren zu ihrer herstellung und ihre verwendung |
| JP7401214B2 (ja) * | 2019-07-11 | 2023-12-19 | 日本ペイント・オートモーティブコーティングス株式会社 | カチオン電着塗料組成物 |
| US11466175B2 (en) | 2019-12-30 | 2022-10-11 | Ppg Industries Ohio, Inc. | Silicone-based electrodepositable coating composition |
| WO2023117986A1 (en) | 2021-12-21 | 2023-06-29 | Basf Se | Environmental attributes for a curable composition |
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| JP3288185B2 (ja) * | 1994-10-07 | 2002-06-04 | 日立化成工業株式会社 | 電子部品封止用エポキシ樹脂成形材料及びそれを用いた半導体装置 |
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- 2013-12-20 JP JP2016541615A patent/JP6325111B2/ja not_active Expired - Fee Related
- 2013-12-20 EP EP13814147.8A patent/EP3083836B1/de not_active Not-in-force
- 2013-12-20 CN CN201380081298.7A patent/CN105874014B/zh not_active Expired - Fee Related
- 2013-12-20 US US15/106,574 patent/US10174212B2/en not_active Expired - Fee Related
- 2013-12-20 MX MX2016008067A patent/MX2016008067A/es unknown
- 2013-12-20 CA CA2931095A patent/CA2931095A1/en not_active Abandoned
- 2013-12-20 WO PCT/EP2013/077808 patent/WO2015090469A1/de active Application Filing
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| DE3942766A1 (de) * | 1989-12-23 | 1991-06-27 | Basf Lacke & Farben | Verfahren zum beschichten elektrisch leitfaehiger substrate, waessriger lack, epoxid-aminaddukt und verwendung des epoxid-aminadduktes als reibharz zur herstellung von pigmentpasten |
| WO2000003070A2 (en) * | 1998-07-10 | 2000-01-20 | Ppg Industries Ohio, Inc. | Electrodeposition baths containing calcium salts |
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Also Published As
| Publication number | Publication date |
|---|---|
| MX2016008067A (es) | 2017-02-27 |
| CN105874014A (zh) | 2016-08-17 |
| US20160333197A1 (en) | 2016-11-17 |
| CA2931095A1 (en) | 2015-06-25 |
| US10174212B2 (en) | 2019-01-08 |
| JP2017508025A (ja) | 2017-03-23 |
| EP3083836B1 (de) | 2017-12-13 |
| JP6325111B2 (ja) | 2018-05-16 |
| EP3083836A1 (de) | 2016-10-26 |
| WO2015090469A1 (de) | 2015-06-25 |
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