CN107177289A - 单组分涂料组合物及用其涂覆的基底 - Google Patents

单组分涂料组合物及用其涂覆的基底 Download PDF

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CN107177289A
CN107177289A CN201710444473.4A CN201710444473A CN107177289A CN 107177289 A CN107177289 A CN 107177289A CN 201710444473 A CN201710444473 A CN 201710444473A CN 107177289 A CN107177289 A CN 107177289A
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China
Prior art keywords
coating compositions
resin
component coating
acid
polyester resin
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CN201710444473.4A
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CN107177289B (zh
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刘文庆
王娟
宋立明
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PPG Coatings Tianjin Co Ltd
PPG Industries Ohio Inc
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PPG Industries Ohio Inc
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Priority to CN201710444473.4A priority Critical patent/CN107177289B/zh
Publication of CN107177289A publication Critical patent/CN107177289A/zh
Priority to US16/622,365 priority patent/US20200165483A1/en
Priority to MX2019014909A priority patent/MX2019014909A/es
Priority to CA3066860A priority patent/CA3066860A1/en
Priority to RU2020100062A priority patent/RU2020100062A/ru
Priority to EP18816921.3A priority patent/EP3638743A4/en
Priority to KR1020197034381A priority patent/KR20190142367A/ko
Priority to PCT/CN2018/090870 priority patent/WO2018228388A1/en
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Abstract

本发明提供一种单组分涂料组合物，其包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂，其中由所述单组分涂料组合物形成的涂层的甲醛含量低于10ppm。本发明还提供用所述单组分涂料组合物涂覆的基底。

Description

单组分涂料组合物及用其涂覆的基底
技术领域
本发明涉及一种基本不含甲醛的单组分涂料组合物，具体而言，涉及一种包含聚酯树脂、丙烯酸树脂和封端异氰酸酯的基本不含甲醛的单组分涂料组合物。
背景技术
在汽车水性3C2B(三涂二烘)体系中的色漆层中，通常采用主体树脂为丙烯酸树脂、聚酯树脂和聚氨酯树脂并加交联剂的体系。在此种体系中，交联剂多采用含甲醛的三聚氰胺甲醛树脂，其优势在于可以做成1K(单组分)涂料，在生产、储存和施工上比较简便而且成本较低；但缺点在于会引入甲醛，而且此合成用交联剂反应是可逆的，在水性体系中的逆反应会释放出更多甲醛。有些体系的甲醛含量甚至能达到1000-2000ppm。众所周知，甲醛对环境及人体健康会造成极大危害：长期接触低浓度甲醛会引起头痛、头晕、乏力、感觉障碍，免疫力降低，并可出现瞌睡、记忆力减退或神经衰弱、精神抑郁等症状；慢性中毒对呼吸系统的危害也是巨大的，长期接触甲醛可引发呼吸功能障碍和肝中毒性病变，表现为肝细胞损伤、肝辐射能异常等，而且长期接触甲醛增大了罹患霍奇金淋巴瘤、多发性骨髓瘤、骨髓性白血病等特殊癌症的几率。
另一种体系常用异氰酸酯作为交联剂，即2K(双组分)涂料。其优点是外观性能优异，也不会引入甲醛；但缺点在于2K涂料在生产、储存和施工上都需要更高的投入，成本较高。
本发明旨在开发一种单组分无甲醛汽车涂料组合物，其既能满足不含甲醛的环保需求，同时避免了2K双组分包装带来的储存和施工的不便，而且能够与普通水性3C2B体系共线喷涂，易于推广和实现。
发明内容
本发明提供一种单组分涂料组合物，其包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂，其中由所述单组分涂料组合物形成的涂层的甲醛含量低于10ppm。
本发明还提供一种经涂覆的基底，其包括(1)基底，和(2)涂覆在所述基底至少一部分上的单组分涂料组合物，其中所述单组分涂料组合物包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂，其中由所述单组分涂料组合物形成的涂层的甲醛含量低于10ppm。
发明详述
除了实施例中的或另外明确说明的，应当认为说明书和权利要求书中使用的所有代表成分的数量、反应条件等的数值在所有情况下均可按照术语“约”进行变化。因此，除非有相反的说明，否则以下的说明书和权利要求书中所列出的数值参重均为近似值，可以按照本发明想要获得的性能而变化。起码，而不是为了限制相当于权利要求范围的这一原则的实施，每个数值参数至少应当按照有效数字来解释并运用普通的舍入法。
尽管列出本发明宽范围的数值范围和参数是近似值，但具体实施例中列出的数值记录得尽可能准确。但是，任何一个数值本来就具有一定的误差。该误差是其相应的测量方法中得出的标准偏差的必然结果。
本文中所使用的聚合物的重均分子量是通过凝胶渗透色谱法采用适当的标准物，例如聚苯乙烯标准物测定的。
本文中所使用的术语“酸值”是指中和1克样品中的游离酸所需的氢氧化钾的毫克数，以mgKOH/g表示。
本文中所使用的术语“胺值”是指每克胺类固化剂中和所需的酸，以氢氧化钾(KOH)的毫克数mgKOH/g表示。
根据本发明的单组分涂料组合物包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂。
聚酯树脂可包括多元酸和多元醇的反应产物。所述聚酯树脂可以由任何合适的多元酸和任何合适的多元醇形成。
合适的多元酸的实例包括但不限于下列中的一种或多种：马来酸；富马酸；衣康酸；己二酸；壬二酸；琥珀酸；癸二酸；戊二酸；癸二酸；十二烷二酸；邻苯二甲酸；间苯二酸；5-叔丁基间苯二酸；四氯邻苯二甲酸；四氢邻苯二甲酸；偏苯三甲酸；萘二甲酸；萘四甲酸；对苯二酸；六氢邻苯二甲酸；甲基六氢邻苯二甲酸；对苯二酸二甲酯；环己烷二甲酸；氯菌酸酐；1,3-环己烷二甲酸；1,4-环己烷二甲酸；三环癸烷聚羧酸；内亚甲基四氢邻苯二甲酸；内亚乙基六氢邻苯二甲酸；环己烷四甲酸；环丁烷四甲酸；或所有上述酸的酸和酸酐以及其组合。
合适的多元醇的实例包括但不限于下列中的一种或多种：烷撑二醇，诸如乙二醇；丙二醇；二乙二醇；二丙二醇；三乙二醇；三丙二醇；己二醇；聚乙二醇；聚丙二醇和新戊二醇；氢化双酚A；环己二醇；丙二醇，其包括1,2-丙二醇；1,3-丙二醇；丁基乙基丙二醇；2-甲基-1,3-丙二醇；和2-乙基-2-丁基-1,3-丙二醇；丁二醇，其包括1,4-丁二醇；1,3-丁二醇；和2-乙基-1,4-丁二醇；戊二醇，其包括三甲基戊二醇和2-甲基戊二醇；环己烷二甲醇；己二醇，其包括1,6-己二醇；己内酯二醇(例如，ε-己内酯和乙二醇的反应产物)；羟烷基化双酚；聚醚二醇，例如聚四亚甲基醚二醇；三羟甲基丙烷；季戊四醇；二季戊四醇；三羟甲基乙烷；三羟甲基丁烷；二羟甲基环己烷；甘油等或其组合。
优选地，可用于本发明涂料组合物中的聚酯树脂可包括一种聚酯树脂或多于一种聚酯树脂的组合。更优选地，可用于本发明涂料组合物中的聚酯树脂可包括高分子量聚酯树脂(a)和低分子量聚酯树脂(b)。
所述高分子量聚酯树脂(a)具有约10,000-50,000范围内的重均分子量。此外，所述高分子量聚酯树脂具有较低的酸值，诸如位于5-20mgKOH/g范围内的酸值。较高的分子量有助于提高涂层的柔韧性和抗石击机械性能。酸值的高低对整个涂层也具有较大的影响。较低的酸值可导致在固化过程中的交联程度和交联密度相对较低，使得所得涂层的柔韧性相对较高，抗石击性能较佳。较高的酸值可使在固化过程中的交联程度和交联密度增加，因此所得涂层的柔韧性相对较低，但是整个涂层对底材的附着力会得以改善。基于聚酯树脂的分子量和酸值对涂层的上述影响，本发明的涂料组合物采用了具有高重均分子量和较低酸值范围的聚酯树脂类型和具有低重均分子量和较高酸值范围的聚酯树脂类型的组合。后者将在下文进行描述。
所述高分子量聚酯树脂可以基于涂料组合物的重量计以约10-25wt％的量存在于该涂料组合物中。当该聚酯树脂在涂料组合物中的含量低于10wt％时，所得涂层的抗石击性能和柔韧性能不佳；当该聚酯树脂在涂料组合物中的含量高于25wt％时，由于聚酯树脂通常在耐湿或耐水性方面会较弱，使得所得涂层的耐湿或耐水性能不佳。此类聚酯树脂可以商购获得，其实例例如可包括但不限于得自allnex的VSM6299W/42WA等。
所述低分子量聚酯树脂(b)具有约3,000-6,000范围内的重均分子量。在该涂料组合物中引入此聚酯的主要作用是代替三聚氰胺甲醛树脂用于铝粉浆的分散。发明人出乎意外地发现，采用此种低分子量聚酯树脂代替三聚氰胺甲醛树脂分散铝粉浆能够实现更好的铝粉浆分散。所述低分子量聚酯树脂具有较高的酸值，诸如位于30-60mgKOH/g范围内的酸值，位于该范围内的较高酸值可使在固化过程中的交联程度和交联密度增加，因此所得涂层的柔韧性相对较低，然而能够增强整个涂层对底材的附着力。该类型的聚酯树脂因此能够为体系提供更高的交联密度，增强其机械性能。
所述低分子量聚酯树脂可以基于涂料组合物的重量计以约0-15wt％、优选约1-15wt％的量存在于该涂料组合物中。当该聚酯树脂在涂料组合物中的含量高于15wt％时，所得涂层的抗石击性能会下降。此类聚酯树脂可以商购获得，其实例例如可包括但不限于得自纽佩斯的SETAL 6306SS 60等。
适用的丙烯酸树脂可为均聚物或共聚物，其可由选自下述的一种或多种单体聚合而成：丙烯酸、甲基丙烯酸、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸异丁酯、丙烯酸β－羟基乙基酯、丙烯酸异辛酯、丙烯酸异冰片酯，丙烯酸月桂酯、丙烯酸羟基丁酯、丙烯酸-2-羟基丙酯、丙烯酸十八醇酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、甲基丙烯酸异丁酯、甲基丙烯酸β－羟基乙基酯、苯乙烯、甲基丙烯酸异辛酯、甲基丙稀酸异冰片酯、甲基丙烯酸月桂酯、甲基丙烯酸-2-羟基丙酯和甲基丙烯酸十八醇酯。
优选地，可用于本发明涂料组合物中的丙烯酸树脂可包括一种丙烯酸树脂或多于一种丙烯酸树脂的组合。最优选地，可用于本发明涂料组合物中的丙烯酸树脂可包括丙烯酸树脂(a)和丙烯酸树脂(b)。
所述丙烯酸树脂(a)优选具有8-9的pH、5.5-8.5mgKOH/g之间的酸值和5.6-8.4mgKOH/g之间的胺值。此种类型的丙烯酸树脂能为体系提供良好的机械性能、耐老化性能以及耐化学品性能。
所述丙烯酸树脂(a)可以基于涂料组合物的重量计以约10-30wt％的量存在于该涂料组合物中。当该丙烯酸树脂在涂料组合物中的含量低于10wt％时，会不利地影响所得涂层的机械性能和耐老化性能。当该丙烯酸树脂在涂料组合物中的含量高于30wt％时，则会降低漆膜的柔韧性，使漆膜变脆。此类丙烯酸树脂可以商购获得，其实例例如可包括但不限于得自Nuplex的Setaqua 6802。
所述丙烯酸树脂(b)优选具有6-7的pH、2.5-6.0mgKOH/g之间的酸值和0.6-2.8mgKOH/g之间的胺值。此种类型的丙烯酸树脂能提供较好的触变性，对整体油漆的生产、运输和储存稳定方面具有非常好的作用。
所述丙烯酸树脂(b)可以基于涂料组合物的重量计以约10-30wt％的量存在于该涂料组合物中。可以根据不同颜色对触变性的要求，调整其在配方中的含量。较低的含量会使涂层的整体触变性降低，同时不利于储存稳定性；而过高的含量则会可能会带来非常高的触变性，随着储存时间的延长，整体粘度增加可能较快，为了降低到施工粘度，可能需要加入大量的水，从而降低整个油漆的固体分。此类丙烯酸树脂可以商购获得，其实例例如可包括但不限于得自Nuplex的SETAQUA 6803。
为基本消除或消除甲醛的生产，本发明采用封端异氰酸酯代替含有甲醛的三聚氰胺树脂作为交联剂。由于多异氰酸酯已被某种带有活性氢原子的化合物反应实现封闭，其内部形成的化学键相对较弱，因此不能与多羟基树脂体系反应交联，从而可以与该多羟基树脂体系形成单组分体系，而无需分开储存。单组分涂料组合物涂布之后经历高温烘烤时，封闭型的单官能物质和异氰酸酯键断裂，使封闭型异氰酸酯开环而释放出大量的-NCO官能团，该官能团与树脂的羟基-OH发生交联反应形成膜。
用作交联剂的封端异氰酸酯通常以基于涂料组合物的重量计约5-12wt％的量存在于涂料组合物中。优选地，封端异氰酸酯、聚酯树脂、丙烯酸树脂的重量比为15:85～40:60。
根据本发明单组分涂料组合物形成的涂层具有低于10ppm的甲醛含量。更进一步的，根据本发明单组分涂料组合物形成的涂层基本不含甲醛。
根据本发明的涂料组合物还包含基于该涂料组合物的重量计约10-20wt％的助溶剂组分。所采用的助溶剂为水性体系常用的助溶剂，包括但不限于乙二醇丁类、丙二醇甲醚类和丁醇等。根据体系的施工环境需要，会做适当的调整，以达到具有良好的施工性。所有溶剂得自如BASF、陶氏化学等。
根据本发明的涂料组合物还包含基于该涂料组合物的重量计约5-40wt％的色浆。不同类型的涂料，其色浆含量区别较大。例如，作为金属漆，其含有2-5％的珠光或者铝粉浆。因此，色浆量会较低，可在5-25wt％的范围内。而一些素色漆的色浆含量就会较高，如白色漆，其色浆含量通常在25-40wt％范围内。色浆的主要作用是提供颜色和遮盖效果。本发明涂料组合物所采用的色浆为水性汽车漆体系常用的色浆颜料，经研磨后以达到良好的着色效果。色浆中的颜料商业得自杜邦、卡博特等。
根据本发明的涂料组合物可以采用静电喷涂施工。静电喷涂是利用高压静电电场使带负电的涂料微粒沿着电场相反的方向定向运动，并将涂料微粒吸附在工件表面的一种喷涂方法。静电喷涂设备由喷枪、喷杯以及静电喷涂高压电源等组成。通过调整雾化器喷涂流量、整形空气和移动速度控制施工膜厚。目前市场上通用的静电喷涂设备均可应用于本产品的施工喷涂，雾化器如Durr的Ecobell2、ABB的RB1000等。
本发明还提供一种经涂覆的基材，其包括基材和沉积在至少一部分所述基材上的单组分涂料组合物。可以用本发明的单组分涂料组合物涂覆的基材可以是任何合适的基材，包括但不限于金属或塑料。优选地，所述基材为金属基材。特别地，所述基材为汽车车身等。
实施例
提供下述实施例进一步阐述本发明，但不应认为其将本发明限制在实施例所述的细节。除另外说明之外，下述实施例以及通篇说明书中所有的份数和百分数均以重量计。
涂料组合物的制备
实施例1
用于制备实施例1的单组分涂料组合物的各组分及其含量示于下表1中，根据下述步骤制备该涂料组合物：
利用溶剂和聚酯树脂2对铝粉浆进行预混，分散30分钟后备用；
混合聚酯树脂1、两种丙烯酸树脂和交联剂，然后调节pH到8.0以上，搅拌下加入底材润湿剂、流平剂、消泡剂等助剂部分，搅拌30分钟后，在搅拌下加入助溶剂部分，然后搅拌1h；
在搅拌下加入色浆部分，搅拌30分钟；和
加入先前混制好的铝粉浆，之后搅拌30分钟，制得本发明实施例的涂料组合物。
对比实例1
用于制备对比实例1的单组分涂料组合物的各组分及其含量示于下表1中，根据下述步骤制备该涂料组合物：
利用溶剂和氨基树脂做铝粉浆的预混，分散30分钟后备用；
混合聚酯树脂和丙烯酸树脂，然后调节pH到8.0以上，搅拌下加入底材润湿剂、流平剂、消泡剂等助剂部分；搅拌30分钟后，再在搅拌下加入助溶剂部分，然后搅拌1h；
最后在搅拌下加入色浆部分，搅拌30分钟；和
加入事先混制好的铝粉浆，然后再搅拌30分钟，制得对比实例。
表1.实施例和比较实例的涂料组合物的配制
*基于涂料组合物的总重量(g)：
1聚酯树脂VSM6299W/42WA，供应商allnex，
2聚酯树脂SETAL 6306SS 60，供应商Nuplex，
3丙烯酸树脂Setaqua 6802，供应商Nuplex，
4丙烯酸树脂Setaqua 6803，供应商Nuplex，
5氨基树脂RESIMENE 741，供应商INEOS，
6封闭异氰酸酯树脂BL2794，供应商Bayer
7铝粉浆STAPA IL HYDROLAN VP57510/G，供应商Eckart；水性黑色浆和水性蓝色浆，供应商PPG，
8底材润湿剂BYK349，供应商BYK；消泡剂Surfyl-tg，供应商气体化学，
9溶剂乙二醇丁类、丙二醇甲醚类和丁醇等。
涂层制备过程：
首先，将水性中涂(得自PPG的1225A水性浅灰中涂)涂覆在电泳板底材上，经过闪干和脱水后烘干制得中涂板，烘干条件通常为在150℃下烘烤30分钟。然后，将如上所制备的实施例1和对比实例1的水性色漆涂覆在中涂板上，经过闪干和脱水(80℃下5分钟)后，冷却至室温。最后，喷涂清漆(得自PPG的CC2000 1K溶剂型高技术罩光清漆)，闪干，然后在140℃下烤干30分钟，得到经涂覆的底材。将所述经涂覆的底材进行下述性能测试。
性能测试
1.湿漆甲醛含量测试结果对比
甲醛含量测试根据GB/T23993-2009水性涂料中甲醛含量的测定进行，应用的是乙酰丙酮分光光度法：采用蒸馏的方法将样品中的甲醛蒸出；在pH＝6的乙酸-乙酸铵缓冲溶液中，馏分中的甲醛与乙酰丙酮在加热的条件下反应生成稳定的黄色络合物，冷却后在412nm处进行吸光度测试；根据标准工作曲线，计算出样品中的甲醛含量。
表2.本发明实施例和对比实例的甲醛含量比较
根据上面的甲醛含量测试结果对比，可以看出，本发明实施例1的单组分涂料组合物所形成的涂层的甲醛含量远远低于对比实例1中以三聚氰胺甲醛作为交联剂的涂料组合物所得涂层的甲醛含量。
2.外观对比如下：
为进行外观对比，使用机器人旋杯雾化器喷涂的方式，模拟喷涂现场进行喷涂。外观数据是应用BYK wavescan进行测量所得到的。
表3.本发明实施例和对比实例的外观数据比较
备注：
H：代表水平面样板，在喷涂过程及烘烤过程都保持水平；
V：代表垂直面样板，在喷涂过程及烘烤过程都保持垂直；
DOI：表示图像在涂膜表面映像的清晰程度、鲜艳性；
LW和SW：分别代表长波和短波，在橘皮仪器中用来表示漆膜表面波纹状态的技术指标；
根据上面的外观数据比较，可以看出，本发明实施例1的单组分涂料组合物所形成的涂层与对比实例1的涂料组合物所形成的涂层外观数据基本一致。
3.本发明实施例1与对比实例1的其他性能测试对比
按照下表，对实施例1的涂料组合物和对比实例1的涂料组合物进行下述性能测试，结果示于下表4中。
表4.各项性能比较
从上表可以看出，本发明的单组分涂料组合物在各项性能上具与对比实例的涂料组合物相当，然而其甲醛含量远远低于该对比实例。
尽管已解释和描述了本发明的特定方面，对本领域技术人员来说很明显的是可做出多种其它改变和修饰而不会背离本发明的精神和范围。因此所附权利要求意图涵盖落入本发明范围内的所有这些改变和修饰。

Claims (11)

1.一种单组分涂料组合物，其包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂，其中由所述单组分涂料组合物形成的涂层的甲醛含量低于10ppm。
2.如权利要求1所述的单组分涂料组合物，其中所述封端异氰酸酯树脂、聚酯树脂、丙烯酸树脂的重量比为15:85～40:60。
3.如权利要求1所述的单组分涂料组合物，其中所述聚酯树脂包含聚酯树脂(a)和聚酯树脂(b)的混合物。
4.如权利要求3所述的单组分涂料组合物，其中所述聚酯树脂(a)具有5-20mgKOH/g之间的酸值,且其重均分子量为10,000-50,000。
5.如权利要求3所述的单组分涂料组合物，其中所述聚酯树脂(b)具有30-60mgKOH/g之间的酸值，且其重均分子量为3,000-6,000。
6.如权利要求1所述的单组分涂料组合物，其中所述丙烯酸树脂包含丙烯酸树脂(a)和丙烯酸树脂(b)的混合物。
7.如权利要求6所述的单组分涂料组合物，其中所述水性丙烯酸树脂(a)的pH值在8-9之间，酸值在5.5-8.5mgKOH/g之间，胺值在5.6-8.4mgKOH/g之间。
8.如权利要求6所述的单组分涂料组合物，其中所述水性丙烯酸树脂(b)的pH值在6-7之间，酸值在2.5-6.0mgKOH/g之间，胺值在0.6-2.8mgKOH/g之间。
9.如上述权利要求任一项所述的单组分涂料组合物，其中由所述单组分涂料组合物形成的涂层基本不含甲醛。
10.经涂覆的基材，其包括：
(i)基材，和
(ii)沉积在至少一部分所述基材上的单组分涂料组合物，所述单组分涂料组合物包含聚酯树脂、丙烯酸树脂和封端异氰酸酯树脂，其中由所述单组分涂料组合物形成的涂层的甲醛含量低于10ppm。
11.如权利要求10所述的经涂覆基材，其中所述基材为汽车车身。
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