CN1756809A - 用无铅电沉积涂料组合物进行涂布的方法及经涂覆的制品 - Google Patents
用无铅电沉积涂料组合物进行涂布的方法及经涂覆的制品 Download PDFInfo
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- CN1756809A CN1756809A CNA2004800056497A CN200480005649A CN1756809A CN 1756809 A CN1756809 A CN 1756809A CN A2004800056497 A CNA2004800056497 A CN A2004800056497A CN 200480005649 A CN200480005649 A CN 200480005649A CN 1756809 A CN1756809 A CN 1756809A
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- pigment
- acid
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- coating
- paint composition
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- 238000000034 method Methods 0.000 title claims abstract description 25
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- 239000008199 coating composition Substances 0.000 title abstract description 9
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- 239000000049 pigment Substances 0.000 claims abstract description 53
- 125000002091 cationic group Chemical group 0.000 claims abstract description 15
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- 239000005995 Aluminium silicate Substances 0.000 description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 description 3
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- 239000000839 emulsion Substances 0.000 description 3
- 239000008393 encapsulating agent Substances 0.000 description 3
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- ZTFZSHLWORMEHO-UHFFFAOYSA-A pentaaluminum;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O.[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O.[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O ZTFZSHLWORMEHO-UHFFFAOYSA-A 0.000 description 3
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Classifications
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- C09D7/40—Additives
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- C09D7/61—Additives non-macromolecular inorganic
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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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
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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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4488—Cathodic paints
- C09D5/4492—Cathodic paints containing special additives, e.g. grinding agents
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/10—Electrophoretic coating characterised by the process characterised by the additives used
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
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Abstract
本发明涉及基本上不含铅化合物的阳离子电沉积涂料组合物，以及更具体地涉及用该组合物涂布合金化热浸镀锌钢板的方法以及通过该方法得到的经涂覆的制品，其边缘部分及一般表面具有优良的耐腐蚀性。本发明提供了一种用包含防锈颜料的无铅阳离子电沉积涂料组合物涂布合金化热浸镀锌钢板以形成耐腐蚀性优良的电沉积涂层的方法，及通过该电沉积得到的经涂覆的制品。
Description
技术领域
本发明涉及基本上不含铅化合物的阳离子电沉积涂料组合物，以及更具体地涉及用该组合物涂布合金化热浸镀锌钢板的方法，其能够形成耐腐蚀性优良的边缘部分以及一般表面，以及通过该方法得到的经涂覆的(包膜)制品。
发明简述
阳离子电沉积涂料已经用于机动车的车体和零部件涂底漆，并且需要形成具有高抗腐蚀能力的涂膜。然而，从环境的观点来看，已被用作高度抗腐蚀的防锈颜料的铅化合物不是首选的。因此，各种无毒或低毒的、无铅防锈颜料已被开发并在JP-A-2000-309730等文献中进行了披露。JP-A-2000-309730中公开的是一种作为防锈颜料的包含具有1.1/1到2.5/1的锌/硅摩尔比的碱性硅酸锌的阳离子电沉积涂料组合物。
发明内容
本发明的目的是提供一种用包含防锈颜料的无铅电沉积涂料组合物涂布合金化热浸镀锌钢板以形成抗腐蚀性优良的电沉积涂膜的方法，以及通过该电沉积涂覆得到的经涂覆的制品。
作为考虑上述目的的认真研究的结果，本发明已经通过下面的
具体实施例加以完成。
因而，本发明的方法是用于使用包含粘合树脂和多种颜料的无铅阳离子电沉积涂料组合物涂布合金化热浸镀锌钢板，其包括：将无铅阳离子电沉积涂料组合物电沉积到合金化热浸镀锌钢板上的步骤，其中该粘合树脂包括阳离子基础树脂和交联剂，而该颜料包括质量比5到30％的磷酸铝颜料和质量比5到30％的氧化硅颜料，氧化硅颜料具有0.44到1.8ml/g的孔体积及10μm或更小的平均粒度。该无铅阳离子电沉积涂料组合物可以进一步包括质量比0.1到10％的单烷基锡化合物，其基于粘合树脂的固体含量的质量。
本发明的经涂覆的制品是一种例如汽车车体这样的制品，其包括通过上述方法涂布以无铅阳离子电沉积涂膜的合金化热浸镀锌钢板。该经涂覆的制品可以包括多层膜，如果必要，其在该无铅阳离子电沉积涂膜上具有底涂层(底漆)、中间涂层、外涂层(面漆)等。
发明详述
本发明详细说明如下。
在本发明的方法中使用的无铅阳离子电沉积涂料组合物中，术语“无铅”意味着该组合物基本上不包含铅(包括铅化合物中的铅)。随着分析仪器的进步，铅的检测极限逐年降低，而在本发明中，术语“无铅”具体指组合物的铅含量是10ppm或者更少。
磷酸铝颜料被加到本发明的方法中所用的无铅阳离子电沉积涂料组合物中。磷酸铝颜料的例子包括三聚二氢磷酸铝、偏磷酸铝、及焦磷酸铝。磷酸铝颜料可以单独或互相联合使用。磷酸铝颜料与组合物中所有颜料的质量比是质量比5到30％，优选10到20％(质量)。当质量比小于5％(质量)时，组合物不能显示出足够的防锈特性。另一方面，当质量比大于30％(质量)时，电沉积涂膜的光滑度则降低。
在本发明中，氧化硅颜料与磷酸铝颜料一起用作防锈颜料。氧化硅颜料的孔体积是0.44到1.8ml/g，优选0.7到1.6ml/g，且氧化硅颜料的平均粒度是10μm或更小，优选1到8μm。氧化硅颜料可以是任何包含二氧化硅作为主要成分且孔体积和平均微粒尺寸在上述范围内的细粒，如硅胶或气相法二氧化硅的细粒。当氧化硅颜料的孔体积小于0.44ml/g时，无铅阳离子电沉积涂料组合物不能展示出足够的抗侵蚀能力。另一方面，当孔体积大于1.8ml/g时，组合物的稳定性降低。而且，当平均微粒尺寸大于10μm时，电沉积涂膜的外观变差。
氧化硅颜料与在无铅阳离子电沉积涂料组合物中的所有颜料的质量比是5到30质量％，优选10到20质量％。当质量比小于5％时，该组合物有时不能显示出足够的防锈特性。另一方面，当质量比大于30质量％时，会发生电沉积涂膜的光滑度降低的情况。
本发明的方法所用的无铅阳离子电沉积涂料组合物优选包括单烷基锡化合物作为固化催化剂(或者用于封闭聚异氰酸酯化合物的离解催化剂)。单烷基锡化合物具有较低的挥发性，因此，在该组合物的电沉积涂膜在电沉积涂层之后通过湿碰湿涂覆抗破裂底漆(chipping primer)或中间涂层然后烘烤的情况下，或在烘烤电沉积涂膜后涂覆抗破裂底漆或中间涂层并烘烤的情况下，(单烷基锡化合物)几乎不能转移到上涂膜。这样，由于催化剂是不挥发的，使用单烷基锡化合物形成的电沉积涂膜极好地粘附到上涂膜，并且几乎不破坏上涂膜的表面从而展示极好的膜性能。虽然这里没有特别的限制，但单烷基锡化合物是优选的单丁基锡氧化物。单烷基锡化合物的例子包括三辛酸单丁基锡、三乙酸单丁基锡、三苯甲酸单丁基锡、三辛酸单丁基锡、三月桂酸单丁基锡、三肉豆蔻酸单丁基锡、三甲酸单甲基锡、三醋酸单甲基锡、三辛酸单甲基锡、三醋酸单辛基锡、三辛酸单辛基锡、三月桂酸单辛基锡、三醋酸单月桂基锡、三辛酸单月桂基锡、及三月桂酸单月桂基锡。这些单烷基锡化合物可以单独或以两种或更多化合物联合使用。而且，将在下文描述的其它离解催化剂只要其不降低本发明的有益效果就可以和单烷基锡化合物一起使用。
把单丁基锡化合物引入无铅阳离子电沉积涂料组合物的方法并不受到特别限制。在单丁基锡化合物是固体的情况下，单丁基锡化合物优选用分散树脂以及颜料分散。此外，在单丁基锡化合物是液体的情况下，它可以溶解于粘合树脂或与粘合树脂混合然后作为粘合组分的一部分被引入。
单丁基锡化合物与粘合树脂的固体含量的质量优选为0.1至10质量％，更优选为0.5到7.0质量％。当单丁基锡化合物的质量比小于0.1质量％时，单丁基锡化合物在催化活性方面有时会不足。另一方面，当质量比提高到大于10质量％时，催化活性不能相应提高，而且，会发生电沉积涂膜因为过分烘烤而分解的情况。
在本发明的方法中所使用的无铅阳离子电沉积涂料组合物除了单丁基锡化合物外还可以包含锌离子以提高固化效率。无机锌化合物如氧化锌及氢氧化锌或有机锌化合物可以用来维持锌离子的浓度在预定的水平。锌化合物可以单用或以两种或更多种化合物联用。
有机锌化合物的例子包括有机一元酸或二酸的锌盐，这些酸例如蚁酸、乙酸、丁酸、己酸、辛酸、十二烷酸、十四烷酸、十六烷酸、十八烷酸、二十二烷酸、新癸酸、丙烯酸、巴豆酸、异巴豆酸、十一碳烯酸、油酸、芥酸、山梨酸、亚油酸、亚麻酸、二苯乙酸、二苯丁酸、二苯丙酸、二环戊烷羧酸、二乙酰乙酸、苯甲酸、甲基苯甲酸、二甲氧苯甲酸、二(叔丁基)苯甲酸、二羟基苯甲酸、邻苯二甲酸酐、对苯二酸、琥珀酸、马来酸、马来酸酐、及富马酸。
无铅阳离子电沉积涂料组合物的锌离子含量优选为100到2000ppm，更好为300到1000ppm。当锌离子含量小于100ppm时，会发生这样的情形：其中将在下文中描述的离解催化剂不能显示出足够的活性，从而导致电沉积涂膜的固化不足。另一方面，当锌离子含量大于2000ppm时，电沉积涂膜外观和电沉积涂层可加工性有时会被损害。
优选阳离子基础树脂能使电沉积涂膜具有高度抗侵蚀能力。这样的阳离子基础树脂的例子包括氨基-环氧树脂、包含氨基的丙烯酸树脂、包含氨基的聚酯树脂等。其中，优选的是氨基-环氧树脂。氨基-环氧树脂能够这样得到以致环氧树脂的环氧环被氨基化合物打开，及被阳离子化，该氨基化合物如伯胺、仲胺、或叔胺的酸式盐。
作为阳离子基础树脂的起始材料的环氧树脂可以是多酚-多缩水甘油醚型环氧树脂，其是表氯醇和多环酚化合物之间的反应产物，多环酚化合物如双酚A、双酚F、双酚S、酚醛树脂、及甲酚酚醛树脂，或具有噁唑烷酮环的改性环氧树脂。环氧树脂优选为具有噁唑烷酮环的改性环氧树脂。该改性环氧树脂可以通过环氧树脂与通过二异氰酸盐化合物与一个活性氢化合物之间的反应制备的双氨基甲酸乙酯(双尿烷)化合物或与通过二异氰酸盐化合物与两个或更多个活性氢化合物之间的反应制备的杂氨基甲酸乙酯化合物的脱醇反应得到。在使用具有噁唑烷酮环的改性环氧树脂作为基础树脂的情况下，电沉积涂膜具有极好的耐腐蚀性。
阳离子基础树脂的胺值优选为30到130，更优选为40到80，而数均分子量优选为1,000到20,000。当胺值小于30时，难以乳化阳离子基础树脂。当胺值大于130时，树脂的电导率可能会增加，从而减弱气针孔性能(gas pin property)、降低库仑效率、或对包括再溶解性等的电沉积涂层可操作性不利。
用于中和阳离子基础树脂的酸的例子包括水溶性的有机酸如蚁酸、乙酸、丙酸、乳酸、柠檬酸、苹果酸、酒石酸、和丙烯酸；及无机酸如盐酸、磷酸、和氨基磺酸。其中，优选的是乙酸、乳酸、丙酸、蚁酸、和氨基磺酸。
优选可用作交联剂的是封闭的聚异氰酸酯化合物及醚化的三聚氰胺树脂。这些封闭的聚异氰酸酯化合物是这样的以致聚异氰酸酯化合物的异氰酸酯基团被封闭剂完全或部分封闭。在封闭聚异氰酸酯化合物中的封闭剂在电沉积后并在烘烤过程中被热分解，且产生的异氰酸酯基团和阳离子基础树脂的官能团起反应，从而硬化树脂。醚化的三聚氰胺树脂是通过用醇如甲醇及丁醇醚化三聚氰胺而得到。与封闭的聚异氰酸酯化合物一样，醚化的三聚氰胺树脂经受与阳离子基础树脂的醚交换以促进电沉积后烘烤过程中的交联反应。
作为封闭的聚异氰酸酯化合物的材料的聚异氰酸酯化合物的例子包括脂肪族二异氰酸酯化合物如三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、五亚甲基二异氰酸酯、六亚甲基二异氰酸酯、1，2-亚丙基二异氰酸酯、1，2-亚丁基二异氰酸酯、2，3-亚丁基二异氰酸酯、1，3-亚丁基二异氰酸酯、亚乙基二异氰酸酯、及亚丁基二异氰酸酯；脂肪族的、环状的二异氰酸酯化合物如1，3-环戊烷二异氰酸酯、1，4-环己烷二异氰酸酯、1，2-环己烷二异氰酸酯、异佛尔酮二异氰酸酯、及降冰片烷(norbornane)二异氰酸酯；脂肪族-芳香族的异氰酸酯化合物如间亚苯基二异氰酸酯、对亚苯基二异氰酸酯、4，4’-二苯基二异氰酸酯、1，5-萘二异氰酸酯、1，4-萘二异氰酸酯、4，4’-二苯基甲烷二异氰酸酯、2，4-或2，6-甲苯二异氰酸酯或其混合物、4，4’-甲苯胺二异氰酸酯、及1，4-二甲苯二异氰酸酯；芳香族二异氰酸酯化合物如联二茴香胺二异氰酸酯、4，4’-二苯基醚二异氰酸酯、及氯二苯基二异氰酸酯；三异氰酸酯化合物如三苯甲烷-4，4’，4”-三异氰酸酯、1，3，5-三异氰酸酯苯、及2，4，6-三异氰酸酯甲苯；四异氰酸酯化合物如4，4’-二苯基-二甲基甲烷-2，2’，5，5’-四异氰酸酯；及聚合的聚异氰酸酯化合物如甲苯二异氰酸酯二聚物和甲苯二异氰酸酯三聚物。其中，优选的聚异氰酸酯化合物是异佛尔酮二异氰酸酯、降冰片烷二异氰酸酯、及4，4’-二苯基甲烷二异氰酸酯。
用于封闭异氰酸酯基团的封闭剂的例子包括卤代烃如1-氯-2-丙醇和氯乙醇；脂肪族的或杂环的醇类如正丙醇、糖醇、及烷基取代的糖醇；酚化合物如苯酚、间甲氧甲酚、对硝基酚、对氯酚、及壬基酚；肟化合物如甲基乙基酮肟、甲基异丁基酮肟、丙酮肟、及环己酮肟；活性亚甲基化合物如乙酰丙酮、乙酰乙酸乙脂、及丙二酸二乙酯；脂肪族醇如ε-己内酰胺、甲醇、乙醇、及异丙醇；芳香族醇如苯甲醇；乙二醇醚如乙二醇单甲醚、乙二醇单***、乙二醇单丁醚、及二乙二醇单甲醚；等。其中，优选的是甲基乙基酮肟和ε-己内酰胺。
在无铅阳离子电沉积涂料组合物中，阳离子基础树脂/交联剂的固体含量比率优选为50/50到90/10，更优选60/40到80/20。当比率不在50/50到90/10的范围内时，固化效率通常不足。
在无铅阳离子电沉积涂料组合物中有机溶剂可以和水一起使用。有机溶剂的例子包括水溶性的有机溶剂，如甲氧基丙醇、乙基溶纤剂、丙基溶纤剂、丁基溶纤剂、2-乙基己基溶纤剂、正己基溶纤剂、甲醇、乙醇、异丙醇、正丁醇、异丁醇、乙二醇二甲基醚、双丙酮醇、丙酮、甲基乙基甲酮、甲氧基丁醇、二氧杂环乙烷、及乙二醇单***乙酸酯；及非水溶性的有机溶剂如二甲苯、甲苯、甲基异丁基甲酮、己烷、四氯化碳、2-乙基己醇、异佛尔酮、环己烷、及苯。其中，优选的有机溶剂是丁基溶纤剂、2-乙基己基溶纤剂、及正己基溶纤剂，它们具有极好的成膜性能。有机溶剂的量优选为每100质量份的阳离子基础树脂和交联剂的固体含量有0.1到10质量份。
在本发明中，虽然单烷基锡化合物被推荐作为离解封闭剂的离解催化剂，但其它的离解催化剂也可以使用。其它离解催化剂的例子包括有机锡化合物如月桂酸二丁基锡、***、及氧化二辛基锡；胺化合物如N-甲基吗啉；及金属盐如锶、钴、及铜。离解催化剂与粘合树脂的固体含量的质量比优选为0.1到10质量％，更优选1.0到7.0质量％。当质量比小于0.1质量％时，催化活性通常不足。另一方面，当质量比增加到大于10质量％时，催化活性不能相应提高，而且，会发生这样的情况，其中电沉积涂膜因为过度烘烤而被分解。
另外，如果必要，交联树脂微粒、颜料、及各种添加物可以加入到无铅阳离子电沉积涂料组合物中。保持经涂覆的制品的边缘部分的厚度的效率可以通过加入交联树脂微粒而提高。这些交联树脂微粒可以产生自丙烯酸树脂、环氧树脂、酚醛树脂、三聚氰胺树脂等。从容易生产的角度来看，交联树脂微粒是特别优选的如使用丙烯酸树脂。交联树脂微粒的数均微粒大小优选为0.02到30μm。
与磷酸铝颜料和氧化硅颜料结合使用的颜料的例子包括彩色颜料如氧化钛、氧化铁红、及碳黑；增量剂型颜料(体质颜料)如硅酸铝和沉淀的硫酸钡；及防锈颜料，其包括磷钼酸盐，其是磷钼酸与二价或三价金属，如铝、铁、钛、锆、锰、钴、镍、铜、锌、和硅的盐。在无铅阳离子电沉积涂料组合物包含这样的颜料的情况下，该组合物可以进一步包含用于分散颜料的树脂。
磷酸铝颜料、氧化硅颜料和其它颜料的总量，基于粘合树脂的固体含量，是0.2到100质量份，优选为0.5到50质量份。
无铅阳离子电沉积涂料组合物可以通过将上述组分分散在有机溶剂和水的水性介质中加以制备，其中水性介质包含水溶性的有机酸或无机酸作为中和剂。
在本发明的方法中，无铅阳离子电沉积涂料组合物可以施加于合金化热浸镀锌钢板。在本方法的优选具体实施例中，无铅阳离子电沉积涂料组合物用去离子水稀释以达到5到40质量％的固体浓度，优选15到25质量％，且组合物的pH值被调节到5.5到8.5，然后该组合物被引入电沉积槽。电沉积涂布优选在电沉积槽温度为20到35℃、100到450V的涂布电压、及1到5分钟的涂布时间的条件下进行。电沉积后烘烤电沉积涂膜的过程中，基质(substrate)温度是100到250℃，优选140到180℃，并且固化时间是5到60分钟，优选10到30分钟。电沉积涂膜的干燥厚度适宜为5到40μm，更好为10到30μm。上述电沉积涂布条件可以加以控制以得到该干燥厚度。
本发明的经涂覆的制品是通过本发明的方法得到的，其中合金化热浸镀锌钢板涂布以无铅阳离子电沉积涂料组合物。该经涂覆的制品可以适用于机动车车体、机动车部件等。抗破裂底漆涂膜和中间涂膜可以在电沉积涂膜上形成，然后，如果有必要，面漆(上涂层)如包含增亮剂的膜和透明膜可以在其上形成。虽然电沉积涂膜可以如上所述单独烘烤，但它也可以在固化组合物之前通过湿碰湿工艺涂布以抗破裂底漆涂膜或中间涂膜以便同时烘烤那些膜。抗破裂底漆涂膜、中间涂膜、及面漆可以在已知的条件下通过使用已知的组合物来形成以便涂布机动车外板等。
下面将参照制备实施例、实施例、和比较实施例对本发明进行更详细的描述。应该注意到，实施例中的“份”指的是“按质量计算的份”。
[制备实施例1]
固化剂的制备
把723份异佛尔酮二异氰酸酯、333份甲基异丁基酮、及0.01份二月桂酸二丁基锡加入到装备有搅拌器、冷凝器、氮气入口管、温度计、及滴液漏斗的烧瓶中，并加热到70℃。在内容物均匀溶解后，经两小时滴入610份甲基乙基酮肟，然后进行反应同时保持反应温度在70℃。反应期间测量反应混合物的红外光谱，并且继续反应直到异氰酸酯基团的吸收峰消失，以得到固化剂。
[制备实施例2]
环氧改性的阳离子基础树脂的制备
把92份2，4-/2，6-甲苯基二异氰酸酯(质量比8/2)、95份甲基异丁基甲酮(MIBK)、及0.5份二月桂酸二丁基锡加入到装备有搅拌器、冷凝器、氮气入口管、温度计、及滴液漏斗的烧瓶中，然后向其中滴加21份甲醇同时搅拌。反应在室温下开始，然后反应混合物的温度由生成的热提高到60℃。反应30分钟后，把57份乙二醇单-2-乙基己基醚从滴液漏斗滴加到反应混合物中，然后进一步加入42份双酚-A-氧化丙稀5-摩尔加合物。反应主要在60到65℃的温度范围内进行，同时测量红外光谱直到异氰酸酯基团的吸收峰消失。
在这样得到的封闭的聚异氰酸酯中加入365份环氧当量为188的环氧树脂，其由双酚A和表氯醇合成，然后混合物的温度被提高到125℃。接着，1.0份苯甲基二甲胺被加入到混合物中，在130℃反应直到环氧当量变成410。87份双酚A被加入到烧瓶中并在120℃反应，因此，环氧当量变成1190。冷却形成的混合物后，11份二乙醇胺、24份N-甲基乙醇胺、及25份79质量％的氨基乙基乙醇胺酮亚胺化合物的MIBK溶液被加入到混合物中且在110℃反应2小时。接着，混合物用MIBK稀释以致非挥发的成分的比率是80％，以得到具有阳离子基团的环氧改性的基础树脂。
[制备实施例3]
主乳剂的制备
均匀混合在生产实施例2中获得的672份(固体含量)基础树脂和在生产实施例1中制备的209.1份(固体含量)固化剂，然后在形成的混合物中加入3质量％的乙二醇单-2-乙基己基醚(基于固体内含物的质量)。蚁酸被加入到形成的混合物中以致中和比率(中和树脂的阳离子基团的比率)是41.7％，然后加入25质量％的醋酸锌和离子交换水的25％水溶液以稀释混合物从而使固体含量的质量比是30.0质量％。接着，在减压下除去MIBK直到固体含量的质量比变成36.0质量％，以制备主乳剂。
[制备实施例4]
颜料分散清漆的制备
环氧当量为450的双酚型环氧树脂与2-乙基己醇-半封闭的异佛尔酮二异氰酸酯反应。形成物用1-(2-羟基乙硫基)-2-丙醇和二羟甲基丙酸转变为叔锍，以制备用于分散颜料的树脂清漆，其具有70.6质量％的叔锍转变比率和60质量％的固体树脂含量。
[实施例1]
<无铅电沉积涂料组合物的制备>
50.0份在生产实例4中产生的用于分散颜料的树脂清漆、100.0份离子交换水、及100.0份下面的粒状混合物通过砂研磨机加以分散，然后进一步研磨直到微粒大小变成10μm或更小，以得到包含52.0质量％固体含量的分散浆料，其包含40质量％的氧化单丁基锡和颜料，及12质量％的固体树脂。氧化硅颜料的孔体积是1.6ml/g，并且其平均粒度是3.9μm。结果显示在表1中。
表1
| 粒状混合物 | 质量比 | 基于全部颜料的质量比质量比 |
| 氧化单丁基锡 | 3 | - |
| 三聚磷酸铝 | 20 | 20.6 |
| 氧化硅 | 20 | 20.6 |
| 二氧化钛 | 26 | 26.8 |
| 碳黑 | 1 | 1 |
| 高岭土 | 30 | 31 |
接着，混合2,000份去离子水、2,000份生产实施例3中的主乳化液、及500.0份分散浆料以得到固体含量为20.0质量％的无铅电沉积涂料组合物。氧化单丁基锡与粘合树脂的固体含量的质量比是0.5质量％，而组合物的锌离子含量是700ppm。
<电沉积涂层>
分别制备冷轧的未处理钢板样品和镀锌钢板样品。对每个样品进行脱脂并用磷酸锌基的化学处理剂(商品名SURFDYNE 5000，Nippon Paint有限公司制造)进行预处理以用作负电极，然后上述电沉积涂料组合物在150到250V外加电压和30℃槽温条件下被电沉积以获得具有25μm干厚度的电沉积涂膜。电沉积涂膜用水清洗然后在170℃烘烤20分钟。分析每个电沉积涂膜的耐腐蚀性。结果显示在表2中。
表2
| 项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 比较实施例1 | 比较实施例2 | 比较实施例3 | |
| 单丁基锡氧化物 | 1.0 | 0.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| 基于全部颜料的质量比 | 三聚磷酸铝 | 20.6 | 20.6 | 5.2 | 30.0 | 15.4 | 30.0 | 0.0 | 41.2 |
| 氧化硅 | 20.6 | 20.6 | 30.0 | 5.2 | 15.7 | 0.0 | 30.9 | 41.2 | |
| 二氧化钛 | 26.8 | 26.8 | 26.8 | 26.8 | 26.8 | 26.8 | 26.8 | 16.6 | |
| 碳黑 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | |
| 高岭土 | 31.0 | 31.0 | 37.0 | 37.0 | 41.1 | 42.2 | 41.3 | 0.0 | |
| 锌离子含量(ppm) | 700 | 700 | 680 | 720 | 700 | 720 | 640 | 730 | |
| 评估 | 光滑度(Ra；μm) | 0.18 | 0.23 | 0.18 | 0.19 | 0.20 | 0.19 | 0.19 | 0.41 |
| 耐腐蚀性试验(冷轧钢板；切割部分) | 1.5 | 1.7 | 1.4 | 1.4 | 1.5 | 1.7 | 2.4 | 1.9 | |
| 耐腐蚀性试验(冷轧钢板；边缘部分) | 1.3 | 1.4 | 1.2 | 1.2 | 1.2 | 1.5 | 2.0 | 1.6 | |
| 耐腐蚀性试验(镀锌钢板；切割部分) | 2.8 | 3.0 | 3.1 | 3.1 | 2.9 | 4.8 | 4.8 | 3.3 | |
| 耐腐蚀性试验(镀锌钢板；边缘部分) | 2.5 | 2.7 | 2.7 | 2.8 | 2.7 | 4.5 | 3.7 | 3.0 | |
单丁基锡氧化物的数量以与粘合树脂的固体含量的质量比(按质量计算的％)表示；每种颜料的数量以质量百分比表示；以及锌离子含量(ppm)是通过以12,000转每分钟离心每个组合物一小时得到的上清液的锌化合物的浓度。
<光滑度测试>
涂膜的表面粗糙度(Ra)是依据JIS-B0601测试。
<耐腐蚀性试验>
得到的经涂覆的制品经受包括16小时喷盐雾、2小时干燥、4小时盐水浸泡、及2小时干燥的腐蚀试验。腐蚀试验重复15次，然后测量切割部分的一侧的溶胀宽度。
[实施例2到6及比较实施例1到3]
用与实施例1同样的方式，制备无铅电沉积涂料组合物，电沉积到样品，然后按照耐腐蚀性进行评估，不同之处在于：改变三聚磷酸铝颜料、氧化硅颜料、及其它颜料的数量。结果显示在表2中。
从上述结果可以清楚地看到，包含特定数量三聚磷酸铝颜料和特定数量氧化硅颜料的无铅阳离子电沉积涂料组合物显示出，在使用冷轧钢板或镀锌钢板的情况下可提高耐腐蚀性而没有降低光滑度。
在本发明的方法中，合金化热浸镀锌钢板涂布以包含特定形态的磷酸铝颜料和氧化硅颜料的无铅阳离子电沉积涂料组合物，从而本发明的这样得到的经涂覆的制品具有耐腐蚀性极好的边缘部分和一般表面。更进一步，在使用包含单烷基锡化合物的无铅阳离子电沉积涂料组合物的情况下，形成的涂膜极好地粘附到上涂膜且几乎不破坏上涂膜的表面从而展示极好的膜性能。而且，从环境和工业健康的角度考虑，非挥发性的催化剂是优选的。本发明的经涂覆的制品具有上述特点，因此可以适用于需要较高耐腐蚀性的产品如机动车车体、机动车部件、及家用电器。
Claims (4)
1.一种用包含粘合树脂和多种颜料的无铅阳离子电沉积涂料组合物涂布合金化热浸镀锌钢板的方法，所述方法包括以下步骤：
将所述无铅阳离子电沉积涂料组合物电沉积到所述合金化热浸镀锌钢板上，其中所述粘合树脂包括阳离子基础树脂和交联剂，而所述颜料包括质量比5到30％的磷酸铝颜料和质量比5到30％的氧化硅颜料，所述氧化硅颜料具有0.44到1.8ml/g的孔体积和10μm或更小的平均粒度。
2.根据权利要求1所述的方法，其中所述无铅阳离子电沉积涂料组合物，基于所述粘合树脂的固体含量的质量，包括质量比0.1到10％的单烷基锡化合物。
3.一种经涂覆的制品，包括通过根据权利要求1或2所述的方法以所述无铅阳离子电沉积涂料组合物涂布的合金化热浸镀锌钢板。
4.根据权利要求3所述的经涂覆的制品，其中所述经涂覆的制品是机动车车体。
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| TW200712152A (en) * | 2005-08-05 | 2007-04-01 | Nippon Paint Co Ltd | Cationic electrodeposition coating composition and coated article therewith |
| CN104806334A (zh) * | 2015-04-13 | 2015-07-29 | 成都陵川特种工业有限责任公司 | 一种用于汽车排气管消音器的表面处理工艺 |
| CN107687015B (zh) * | 2017-08-18 | 2019-02-22 | 重庆市环岛机械制造有限公司 | 汽车配件涂装方法 |
| US11976210B2 (en) * | 2019-10-11 | 2024-05-07 | Axalta Coating Systems Ip Co., Llc | Edge protection for electrocoat |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719038A (en) * | 1983-12-27 | 1988-01-12 | Nippon Paint Co., Ltd. | Corrosion resistant, coated metal laminate, its preparation and coating materials |
| KR950014243A (ko) * | 1993-11-02 | 1995-06-15 | 후지이 히로시 | 양이온성 전착 피복 조성물 |
| TWI221861B (en) * | 1998-04-22 | 2004-10-11 | Toyo Boseki | Agent for treating metallic surface, surface-treated metal material and coated metal material |
| JP2000309730A (ja) | 1999-04-27 | 2000-11-07 | Kansai Paint Co Ltd | カチオン電着塗料 |
| KR100403466B1 (ko) * | 1999-12-20 | 2003-11-01 | 주식회사 포스코 | 박막수지코팅강판 하지용으로 사용되는 도포형크로메이트용액 |
| JP4693207B2 (ja) * | 2000-05-23 | 2011-06-01 | 関西ペイント株式会社 | カチオン電着塗料 |
| JP4060620B2 (ja) * | 2002-03-26 | 2008-03-12 | 日本ペイント株式会社 | 無鉛性カチオン電着塗料を用いる電着塗装方法 |
-
2003
- 2003-03-05 JP JP2003059026A patent/JP4204353B2/ja not_active Expired - Fee Related
-
2004
- 2004-03-03 CA CA2519855A patent/CA2519855C/en not_active Expired - Fee Related
- 2004-03-03 GB GB0518600A patent/GB2414481B/en not_active Expired - Fee Related
- 2004-03-03 US US10/547,909 patent/US7294410B2/en not_active Expired - Fee Related
- 2004-03-03 CN CNB2004800056497A patent/CN1318524C/zh not_active Expired - Fee Related
- 2004-03-03 WO PCT/JP2004/002682 patent/WO2004078857A1/en active Application Filing
- 2004-03-05 TW TW93105884A patent/TWI354691B/zh not_active IP Right Cessation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106922151A (zh) * | 2014-10-31 | 2017-07-04 | 威士伯采购公司 | 高边缘阴极环氧电泳涂料组合物 |
| US10676837B2 (en) | 2014-10-31 | 2020-06-09 | Swimc Llc | High edge cathodic epoxy electrocoat composition |
| CN106922151B (zh) * | 2014-10-31 | 2020-11-06 | 宣伟投资管理有限公司 | 高边缘阴极环氧电泳涂料组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| TW200502339A (en) | 2005-01-16 |
| GB0518600D0 (en) | 2005-10-19 |
| GB2414481A8 (en) | 2005-12-05 |
| WO2004078857A1 (en) | 2004-09-16 |
| CA2519855A1 (en) | 2004-09-16 |
| TWI354691B (en) | 2011-12-21 |
| CN1318524C (zh) | 2007-05-30 |
| US20060124462A1 (en) | 2006-06-15 |
| JP4204353B2 (ja) | 2009-01-07 |
| US7294410B2 (en) | 2007-11-13 |
| GB2414481B (en) | 2007-01-31 |
| CA2519855C (en) | 2011-06-14 |
| GB2414481A (en) | 2005-11-30 |
| JP2004269581A (ja) | 2004-09-30 |
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