CN116323819A - 用于产生浅色导电底漆涂层的底漆组合物 - Google Patents
用于产生浅色导电底漆涂层的底漆组合物 Download PDFInfo
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- CN116323819A CN116323819A CN202180069739.6A CN202180069739A CN116323819A CN 116323819 A CN116323819 A CN 116323819A CN 202180069739 A CN202180069739 A CN 202180069739A CN 116323819 A CN116323819 A CN 116323819A
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- primer
- primer formulation
- coating
- walled
- carbon nanotubes
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Abstract
本发明涉及导电涂层,特别是在它们经历静电喷涂之前的部件的导电底漆涂层,以及用于产生这种涂层(底漆涂层)的底漆组合物。本发明提出一种用于在静电喷涂之前在部件上产生浅色导电底漆涂层的底漆组合物,所述底漆组合物包含大于0.005wt%且小于0.1wt%的浓度的单壁和/或双壁碳纳米管,并且具有不大于20微米的底漆组合物的研磨度。施加这种底漆组合物的技术结果是具有小于109Ω/sq的比表面电阻和至少60%的光反射系数(LRV)的浅色导电底漆涂层。本发明还提出一种用于制备底漆组合物的方法和浅色导电底漆涂层。
Description
技术领域
本发明涉及导电涂层,更具体地涉及在部件的静电喷涂(electrostaticpainting,静电喷漆)之前用于它们的导电底漆涂层(conductive priming coating,导电底涂层),以及涉及产生这种涂层(底漆)的底漆配制品(priming formulation,底漆配方,底漆制剂)。
背景技术
静电喷涂是工程中广泛使用的生产喷涂的涂层(painted coating,喷漆涂层,着色涂层)的方法,其中在将其应用于部件表面之前,涂料流被分成带电的小液滴。这种喷涂方法的优点,即实现薄而均匀的涂层并允许过程自动化,确保了它的广泛应用。该过程要求待被喷涂的部件或至少其表面具有足以排出带电涂料液滴带来的电荷的电导率,即导电。部件应具有小于109Ohm/sq(Ohm/□)、更优选小于107Ohm/□、最优选小于105Ohm/□的表面电阻(surface resistance)。如果待被喷涂的部件由导电材料(诸如金属)制成,则很容易满足该条件。然而,许多行业使用需要喷涂的部件,但它们是由电导率不足的聚合物材料制成的。因此,车身的很多部件的特征在于大于1012Ohm/□的表面电阻,这使其无法静电喷涂。必须在这种部件上预先形成导电底漆涂层。
本行业广泛使用的形成导电底漆涂层的方法是通过在部件上施加以大于3wt.%的量包含炭黑(CB)的悬浮液进行的。在干燥这种悬浮液之后,获得包含大于10wt.%的炭黑的涂层。该方法的显著缺点是涂层的深灰色(直至黑色)。这给随后的静电喷涂成白色或浅色色调带来严重困难:为获得高光反射率值(LRV),需要加厚施加的涂层,这降低了生产涂喷线的生产量,增加了涂料消耗,并且还可能不利地影响涂层使用寿命。
已知公开[CN110591483A,FUDAN Univ.,20.12.2019,C09D133/04C09D175/04C09D5/24C09D7/46C09D7/61]提供了8-12份的成膜树脂、35-45份的水基助粘剂和润湿剂、6.5-7.0份的水基增稠剂、14-20份的水、0.6-1.0份的水基分散剂、0.6-1.0份的水基消泡剂、15-25份的钛白、0.1-0.8份的颜料炭黑、0.1-6份的导电功能粉体的混合物的使用。从公开中可以看出,使用术语“导电功能粉体”,作者是指导电石墨烯或导电炭黑。使用该悬浮液作为底漆产生导电涂层:例如,0.36wt.%的CB N311和0.22wt.%的导电石墨烯XF178的存在提供了3.4·105Ohm/□的涂层表面电阻;为了将涂层表面电阻降低到小于3·104Ohm/□,导电石墨烯的浓度应提高到大于1.8wt.%。本申请没有提供有关包含较少量导电功能粉体和CB的涂层的数据。发明申请CN110591483A中提供的底漆的明显缺点是高浓度的碳添加剂,即0.2至6.8wt.份(颜料CB和导电CB或石墨烯),这总是大于0.17wt.%。这种高浓度的碳添加剂导致生产的底漆涂层颜色较深。
已知专利公开[CN104403397B,DONGFENG MOTOR,2017年7月28日,C09D5/24,C09D163/00,C09D133/00,B05D7/26,B05D3/02]提供了具有碳纳米管的复合底漆配制品,该配制品具有0.1-1.5wt.%的均匀分散在车底漆配制品中的碳纳米管含量,并且通过将碳纳米管引入车底漆配制品,随后分散所得混合物而获得。通过施加该底漆配制品产生的涂层的表面电阻为103-109Ohm/□。在底漆配制品中碳纳米管的重量浓度为0.8wt.%时,通过施加这种底漆配制品产生的涂层的表面电阻为5·106Ohm/□。使用本公开提供的这种底漆配制品的前提是底漆配制品的颜色比车顶漆层的颜色浅。
提供的方法的缺点是获得的底漆涂层颜色深。从讨论的公开中提供的数据可以看出(讨论的公开CN104403397B的图1),即使引入本公开中要求保护的最小量,即0.1wt.%的碳纳米管,涂层也具有LRV约50%的深灰色。这极大地限制了该底漆配制品到深色喷涂的汽车部件的可能应用范围。提供的方法的另一个缺点是需要将碳纳米管分散在已经含有所有其他组分的底漆配制品中,即,在具有复杂组成的相当粘稠的分散体中。没有碳纳米管的预先分散,获得的底漆配制品可能是不均匀的,即,它可能含有相当大的肉眼看作黑点的纳米管团聚物。
从上述描述可以看出,形成具有小于109Ohm/□的表面电阻以及至少60%的光反射率值(LRV)的导电浅色底漆涂层存在工程问题。发明申请[CN110591483A]和公开[CN104403397B]没有解决该问题。本发明采用专利公开[CN104403397B,东风汽车(DONGFENG MOTOR),2017年7月28日,C09D5/24,C09D163/00,C09D133/00,B05D7/26,B05D3/02]作为原型(Prototype)。
发明内容
本发明提供了一种底漆配制品,用于在静电喷涂之前产生部件的浅色(light-colored)导电底漆涂层,其中配制品包含大于0.005wt.%且小于0.1wt.%的浓度的单壁和/或双壁碳纳米管,底漆配制品的研磨度(degree of grinding)不大于20μm。
使用这种导电底漆配制品的技术结果是产生具有小于109Ohm/□的表面电阻和至少60%的光反射率值(LRV)的浅色导电底漆涂层。这允许随后将部件喷涂成浅色或白色。
术语“底漆配制品”是指具有复杂组成(complex composition,复杂组合物)的悬浮液,其包含溶剂、成膜剂、分散剂、颜料、流变学和粘度改性剂、改善底漆对待喷涂的部件和顶漆层材料的粘附性的试剂以及导电添加剂。除导电添加剂外,底漆配制品的化学性质和组分含量可基于喷涂部件的材料、用于在特定设备上喷涂的工艺特征、经济参数,基于现有技术,而不是本发明的特征。例如,底漆配制品可以是水基的(水作为溶剂),或者溶剂可以是有机溶剂,包括但不限于二甲苯、乙酸丁酯、甲基乙基酮、乙酸甲氧基丙酯、甲苯、环己酮等。成膜剂可以选自但不限于已知的丙烯酸类(acrylic)、环氧树脂、聚氨酯、聚酯或其他成膜剂,但不限于提供的实例。
术语“研磨度”是指根据标准[GOST 6589-74油漆和清漆(Paints andVarnishes),使用“Klin”仪器测定研磨度的方法(Method for Determination of theGrinding Degree using a“Klin”Instrument)刮板细度仪(Grindometer)]和[ISO 1524:2020(en)油漆、清漆和喷涂油墨-研磨细度的测定(Paints,Varnishes and PrintingInks-Determination of Fineness of Grind)]测定的底漆配制品中碳纳米管的颗粒和团聚物的尺寸。该参数表征了在底漆配制品中碳纳米管团聚物根据尺寸分布的上限。
实现的技术结果是由于在底漆配制品中使用具有大于0.005wt.%且小于0.10wt.%的浓度的单壁和/或双壁碳纳米管作为导电组分引起的,该碳纳米管分散良好至小于20μm的团聚物尺寸。
提供该技术结果所需的显著特征是使用单壁和/或双壁碳纳米管而不是多壁碳纳米管作为导电组分。单壁和双壁碳纳米管以及多壁碳纳米管结合了高电导率和管状形态。然而,单壁和双壁碳纳米管的关键区别在于它们优选通过范德华力(π-π相互作用)结合,团聚成六角形紧密堆积的管束。为此,在碳纳米管分散至20μm或更小的研磨度时,悬浮液中不会残留线圈状的团聚物,而是仅有束。另一方面,多壁碳纳米管不易成束,它们的团聚物通常具有线圈形态,即使尺寸为几微米。
已知渗流阈值(percolation threshold),即分布在分散介质中的分散颗粒形成连接簇的最小浓度,它越低,这些颗粒的长度L与直径d的比率越高。对于球形颗粒,随机分布颗粒的渗流阈值约为30%v/v。对于L/d比率较高的颗粒,渗流阈值明显较低,比率越高,阈值越低。为此,与包含线圈状团聚物的底漆相比,包含单壁和/或双壁碳纳米管的线性团聚物(束)的底漆配制品具有明显更高的电导率,并且与线圈状团聚物相比,需要单壁和/或双壁碳纳米管的线性团聚物(束)的浓度显著更低以实现给定的电导率,例如体积电阻率小于108Ohm·cm。
因此,为了实现技术结果,底漆配制品必须包含单壁和/或双壁碳纳米管,这些纳米管必须分散到最大尺寸20μm,以确保单壁和/或双壁碳纳米管的团聚物的主要线性形态,并且单壁和/或双壁碳纳米管的浓度必须小于0.1wt.%。同时满足这三个要求确保高电导率和高光反射率值(LRV至少为60%)。
优选的是,根据其流变学,底漆配制品应为非牛顿假塑性流体,即其粘度取决于剪切速率,粘度越低,剪切速率越大,增加10倍剪切速率降低粘度大于2倍。在使用奥斯特瓦尔德-德沃尔(Ostwald-de Waele)幂律关系描述流体粘度时,这意味着流动特性指数低于0.7。这将降低单壁和/或双壁碳纳米管在底漆配制品的储存和准备使用期间的团聚速率,然而,来自理想(牛顿)的较小偏差的流变学的底漆配制品也可以实现技术结果。
为了优化底漆配制品的流变学参数,即其粘度和所谓的触变性指数,或不同剪切速率下的粘度比率,该配制品优选包含流变改性剂(rheology modifier)。这种改性剂可以选自但不限于膨润土、层状硅酸盐、层状铝硅酸盐、高分子量聚合物或其他已知的增稠剂,或稀释剂,或增塑剂,或胶凝剂,或它们的组合。流变改性剂及其含量主要通过对底漆流变学所选的喷涂工艺要求来选择。
底漆还优选包含5至40wt.%的白色颜料,其将增加产生的底漆涂层的光反射率值(LRV)。所述白色颜料优选为二氧化钛(钛白)。最优选地,底漆中二氧化钛的含量大于20wt.%。然而,当使用较低浓度的二氧化钛或当使用不同的白色颜料时,包括但不限于氧化锌、氧化镁、碳酸钙、硫酸钡,当使用不同颜色的颜料时,也可以实现技术结果。
优选底漆还包含0.1至2wt.%的分散剂以便以较低能源成本和以较短时间实现单壁和/或双壁碳纳米管和颜料所需的分散度,即不存在具有尺寸超过20μm的多团聚物。根据其化学性质,分散剂可包括但不限于高分子量共聚物的烷基铵盐、或具有极性基团的线性聚合物、或具有极性基团的嵌段共聚物。可以使用的一些可商购的分散剂包括但不限于Disperbyk 118、Disperbyk 161、Disperbyk 180、Disperbyk 2155、BYK 9076等。注意在某些情况下,技术结果也可以在没有分散剂的情况下实现。
本发明还提供了生产底漆配制品的方法,其特征在于包括以下顺序的步骤:(A)将单壁和/或双壁碳纳米管的浓缩物引入到至少包含溶剂的混合物中,所述浓缩物是包含至少1wt.%的单壁和/或双壁碳纳米管的分散体系,所述分散体系通过将碳纳米管和分散介质的混合物机械加工至不超过50μm的研磨度获得;和(B)混合所得混合物以形成具有不大于20μm的研磨度的均匀悬浮液。
提供的方法可以使用来自公开[RU2654959C2,MSD Technologies S.AR.L.,2018年5月23日,C01B 32/174,B82B 1/00,B82B 3/00,B82Y 40/00]的超浓缩物,即单壁和/或双壁碳纳米管的浓缩物,所述浓缩物包含至少2wt%的单壁和/或双壁碳纳米管,碳纳米管团聚物的最大尺寸不大于50μm,作为单壁和/或双壁碳纳米管的所述浓缩物。单壁和/或双壁碳纳米管的浓缩物可以包括但不限于可商购的单壁TUBALL碳纳米管TUBALL MATRIXTM 204、TUBALL MATRIXTM 302等的浓缩物。然而,当在分散介质中使用较低浓度的单壁和/或双壁碳纳米管分散体时,例如包含1.5wt.%或甚至1wt.%的单壁和/或双壁碳纳米管,也可以实现技术结果。
单壁和/或双壁碳纳米管的浓缩物可以与底漆配制品的一种或几种其他组分的引入同时引入。方法还可以包括一个或几个引入底漆配制品的其他组分和额外混合的另外的步骤。提供的方法的实施方式是一种方法,其中在步骤(A)之前将底漆配制品的所有其他组分引入溶剂并混合,并且步骤(A)和(B)的顺序完成底漆配制品的生产。提供的方法的另一个可能的实施方式是一种方法,其中在步骤(A)之前将分散剂和成膜剂引入到溶剂中,而在步骤(A)中,单壁和/或双壁碳纳米管的浓缩物与白色颜料一起引入,所述白色颜料在完成底漆配制品的生产的步骤(B)中与混合单壁和/或双壁碳纳米管的浓缩物同时分散。
提供技术结果的用于生产底漆配制品的方法的显著特征是底漆配制品的生产包括引入单壁和/或双壁碳纳米管的预分散浓缩物的步骤。预分散至不大于50μm的研磨度是必要的,以在底漆配制品中在随后的它们机械混合的步骤期间分散纳米管,以产生具有不大于20μm的研磨度的均匀悬浮液,所述悬浮液在表面的应用和随后干燥产生具有高电导率(表面电阻小于109Ohm/□)和高光反射率值(LRV至少为60%)的膜。
在步骤(B)中,在步骤(A)中获得的混合物以产生具有不大于20μm的研磨度的均匀悬浮液的混合可以通过任何已知的混合方法和使用混合设备进行,所述设备包括但不限于立式搅拌器(也称为溶解器)、行星式混合器、转子-定子型混合器(rotor-stator typemixer)、双螺杆混合器,以及用于分散的单元,例如胶体磨、珠磨机、行星式磨机、球磨机等。在一些应用中,优选使用盘式溶解器,即具有盘式叶轮,优选具有齿状盘式叶轮的立式搅拌器进行混合。在一些应用中,优选使用珠磨机在大于10W.h/kg的输入能量下进行混合,珠子直径优选大于0.4mm且小于1.8mm且珠子体积与悬浮液体积比率大于0.5且小于2。
在一些应用中,除单壁和/或双壁碳纳米管的浓缩物外,底漆配制品的所有组分优选在步骤(A)之前引入溶剂并混合,并且步骤(A)和(B)的顺序完成了底漆配制品的生产。
在一些应用中,优选在步骤(A)之前将分散剂和成膜剂引入溶剂中,而在步骤(A)中,将单壁和/或双壁碳纳米管的浓缩物和白色颜料引入到包含溶剂、分散剂和成膜剂的混合物中,并且在完成底漆配制品生产的步骤(B)中进行白色颜料的分散。
将单壁和/或双壁碳纳米管在它们没有预分散的情况下直接引入底漆配制品中无法实现技术效果,因为获得的悬浮液的分散度不足,因此存在许多尺寸超过20μm的线圈状团聚物。以单壁和/或双壁碳纳米管小于0.1wt.%的浓度,将单壁和/或双壁碳纳米管直接引入底漆配制品中,获得的底漆涂层的表面电阻高于109Ohm/□,以及通过将单壁和/或双壁碳纳米管的浓度增加到高于0.1wt.%来实现所需电阻的任何尝试都会使底漆涂层成为不可接受的深色(LRV小于60%)。此外,单壁和/或双壁碳纳米管的大团聚物的存在会损害底漆配制品的质量,即其表面包含肉眼可见的黑点。
本发明提供了通过将所述底漆配制品施加到部件表面上并随后干燥而生产的浅色导电底漆涂层。
干燥是指从施加在部件表面的底漆配制品中部分除去溶剂。这可以通过加热或不加热部件、用气流吹或通过自然对流来实现。对于一些应用,优选干燥进行至底漆层中小于20wt.%或甚至小于1wt.%的溶剂含量。对于一些应用,优选较高含量的溶剂留在底漆层中,如30wt.%。干燥程度、干燥条件和干燥时间的选择取决于顶漆层的化学组成,以及具体的工艺实施。
底漆涂层可以通过将提供的底漆配制品施加到由具有大于1010Ohm/sq的表面电阻的聚合物材料制成的部件上来生产;例如,喷涂部件可以由聚合物制成,所述聚合物包括但不限于聚丙烯,聚酰胺,聚碳酸酯,丙烯腈、丁二烯和苯乙烯的共聚物或它们的混合物。
底漆涂层可以通过将提供的底漆配制品施加到由具有大于1010Ohm/sq的表面电阻的复合材料制成的部件上来生产;例如,喷涂部件可以由滑石填充聚丙烯、玻璃填充聚酰胺、碳填充聚酰胺或聚酯片材压制材料(polyester sheet press-material)(SMC复合材料)制成。
本发明通过以下提供的实例和附图进行说明。在以下说明本发明的实施方式的实例中,表面电阻率根据ANSI/ESD STM 11.11-2015测量。在生产的底漆配制品中的研磨度根据ISO 1524:2020测量。用于施加的底漆涂层的光反射率值(LRV)使用具有d8几何结构的BYK spectro2guide分光光度计测量。底漆配制品的粘度使用具有RV-04轴的BrookfieldDV3T粘度计在25℃下对于100ml样品测量。
提供实例和附图是为了更好地说明本发明提供的技术问题的解决方案,并且不穷尽本发明所有可能的实施方式。
附图说明
图1
[图1]实施例1-3中使用的单壁碳纳米管的透射电子显微照片。
图2
[图2]与粘度计轴的转速ω,rpm相对的实施例1-9的底漆配制品的动态粘度η,mPa·s。
图3
[图3]与底漆配制品中单壁和/或双壁碳纳米管的浓度相对的底漆涂层的表面电阻Rs,Ohm/□,和底漆涂层的光反射率值LRV,%。点旁边的数字表示实施例数字。
图4
[图4]实施例6中使用的单壁和双壁碳纳米管的透射电子显微照片。
[表1]
具体实施方式
实施例
本发明的优选实施方式
实施例1
底漆配制品是使用可商购的碳纳米管浓缩物TUBALLTM MATRIX 302生产的,所述浓缩物包含10wt.%的TUBALLTM单壁碳纳米管(SWCNT)和90wt.%的丙烷-1,2-二醇与2,2'-[(1,1'-联苯基)-4,4'-二基二-2,1-亚乙基二基]双-(苯磺酸钠)(sodium 2,2’-[(1,1’-biphenyl)-4,4’-diyldi-2,1-ethylene diyl]bis-(benzene sulphonate))的混合物并且通过将碳纳米管和分散介质的混合物机械加工至40μm的混合物的研磨度生产。在使用的浓缩物中单壁碳纳米管的透射电子显微照片如图1所示。在1.5l金属容器中,将100.0g二氧化钛DuPont R706和9.9g碳纳米管浓缩物TUBALLTM MATRIX 302同时引入到预混混合物,所述预混混合物包含546.1g可商购的丙烯酸树脂(acryl resin,丙烯酰基树脂)Lacryl 8810(不挥发物含量44wt.%)的水性乳液(aqueous emulsion,含水乳液)、327.0g蒸馏水、14.0g丙烯酸类聚合物基分散剂(acrylic polymer-based dispersing agent)KusumotoDisparlon AQ D-400、2g植物油基脱气剂WS 360和1.0g基于改性层状硅酸盐Laponite-RD的流变改性剂。将获得的混合物使用转子-定子型混合器IKA T50数字(digital)ULTRA-TURRAX以10000rpm的转速混合40分钟直至形成均匀悬浮液。在生产的底漆配制品中的SWCNT含量为0.099wt.%。底漆配制品的体积电阻率为3.5·103Ohm·cm,底漆配制品的研磨度为19μm。由图2中所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.43。使用喷枪将获得的底漆配制品施加在由聚丙烯制成的聚合物基材上并在室温下干燥24小时。底漆涂层的干燥后厚度为17μm。底漆涂层的表面电阻为7.2·104Ohm/□。测量的底漆涂层的光反射率值(LRV)为60%。本实施例及以下实施例2-9获得的涂层的光反射率值和表面电阻数据如图3所示。
本发明实施方式
实施例2
如实施例1,使用可商购的碳纳米管浓缩物TUBALLTM MATRIX 302制备底漆配制品。在1.5l金属容器中,将124.0g硫酸钡“Barit”、124.0g碳酸钙“Microcaltsit KM-2”、248.0g二氧化钛DuPont R706和8.5g碳纳米管浓缩物TUBALLTM MATRIX 302同时引入混合物中,所述混合物包含389.7g可商购的丙烯酸树脂Lacryl 8810(不挥发物含量44wt.%)的水性乳液、96.7g蒸馏水、24.2g丙烯酸类聚合物基分散剂Kusumoto Disparlon AQ D-400和3g植物油基脱气剂WS 360。使用具有磨室TML1、外叶轮直径40mm、内盘直径60mm、锆珠直径在1.2mm至1.7mm范围内、磨室中氧化锆珠与混合物体积比率8:13的珠磨机Dispermat CN 20来将混合物混合。以10.7m/s(3,400rpm)的叶轮转速混合30分钟直至形成均匀的悬浮液;总输入能量为46.8W·h/kg。之后,将60.0g获得的混合物与包含31.8g可商购的Lacryl 8810(不挥发物含量44wt.%)的水性乳液、7.8g蒸馏水、0.014g植物油基脱气剂WS 360和0.01g基于改性层状硅酸盐Laponite-RD的流变改性剂的混合物混合。使用顶置式搅拌器进行混合15分钟,转速为1.9m/s(1,500rpm,叶轮直径20mm)。在生产的底漆配制品中的SWCNT含量为0.05wt.%。底漆配制品的体积电阻率为3.4·103Ohm·cm,底漆配制品的研磨度为17.5μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.32。使用喷枪将制备的底漆配制品施加在由聚丙烯、ABS共聚物、聚碳酸酯、聚酰胺、滑石填充聚丙烯、玻璃填充聚酰胺、碳填充聚酰胺制成的聚合物基材上并在室温下干燥24小时。表1提供了底漆涂层干燥后的厚度、它们的表面电阻率和光反射率值(LRV),以及在施加底漆涂层之前基材的表面电阻率和光反射率值。
实施例3
如实施例1中所提供,使用可商购的碳纳米管浓缩物TUBALLTM MATRIX 302制备底漆配制品。在1.5l金属容器中,将124.0g硫酸钡“Barit”、124.0g碳酸钙“Microcaltsit KM-2”、248.0g二氧化钛DuPont R706和17.0g碳纳米管浓缩物TUBALLTM MATRIX 302同时引入预混混合物中,所述预混混合物包含389.7g可商购的丙烯酸树脂Lacryl 8810(不挥发物含量44wt.%)的水性乳液、96.7g蒸馏水、24.2g丙烯酸类聚合物基分散剂Kusumoto DisparlonAQ D-400和3g植物油基脱气剂WS 360。使用转子-定子型混合器IKA T50数字ULTRA-TURRAX,以10000rpm的转速混合混合物40分钟,直至获得均匀的悬浮液。之后,将60.0g获得的混合物与包含31.8g可商购的Lacryl 8810(不挥发物含量44wt.%)的水性乳液、7.8g蒸馏水、0.014g植物油基脱气剂WS 360和0.01g基于改性层状硅酸盐Laponite-RD的流变改性剂的混合物混合。使用顶置式搅拌器进行混合15分钟,转速为3.4m/s(1,500rpm,叶轮直径40mm),直至形成均匀的悬浮液。生产的底漆配制品包含0.099wt.%SWCNT。底漆配制品的体积电阻率为7.8·102Ohm·cm,底漆配制品的研磨度为19μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.41。使用喷枪将制备的底漆配制品施加到由聚丙烯制成的聚合物基材上并在室温下干燥24小时。底漆涂层的干燥后厚度为17μm。底漆涂层的表面电阻为1.3·104Ohm/□。测量的底漆涂层的光反射率值(LRV)为62%。
实施例4
底漆配制品是使用碳纳米管浓缩物制备的,所述浓缩物包含5wt.%的单壁碳纳米管和95wt.%的三甘醇二甲基丙烯酸酯和高分子量共聚物的烷基铵盐的混合物,并且通过机械加工碳纳米管和分散介质的混合物至该混合物的研磨度为35μm来生产。在500ml金属容器中,将36.6g二氧化钛DuPont R706和2.0g碳纳米管浓缩物同时引入到108.2g的20wt.%的可商购的粘合促进剂Superchlon 822S的二甲苯溶液、1.0g分散剂Disperbyk118、1.8g基于改性硅酸盐Claytone HY的流变改性剂、17.2g二甲苯和1.3g甲苯的预混混合物中。使用具有附加模块APS-500、直径60mm的聚酰胺盘、氧化锆珠与混合物体积比率1:1的珠磨机Dispermat CN 20,以8.5m/s(2,700rpm)的转速混合混合物30分钟,直至形成均匀的悬浮液。将包含5.5g的20wt.%的可商购的粘合促进剂Superchlon822S的二甲苯溶液、7.2g甲苯和3.0g二甲苯的混合物添加到84.2g获得的混合物中,并且使用顶置式搅拌器以3.1m/s(1,500rpm,叶轮直径40mm)的转速混合15分钟。生产的底漆配制品包含0.099wt.%SWCNT。生产的底漆配制品的体积电阻率为6.0·104Ohm·cm,底漆配制品的研磨度为15μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.42。使用喷枪将获得的底漆配制品施加在由聚丙烯制成的聚合物基材上并在室温下干燥20分钟。底漆涂层的干燥后厚度为12μm。底漆涂层的表面电阻为7.9·105Ohm/□。测量的底漆配制品的光反射率值(LRV)为74%。
实施例5
使用碳纳米管浓缩物制备底漆配制品,所述浓缩物包含2wt.%的单壁碳纳米管和98wt.%的三甘醇二甲基丙烯酸酯和高分子量共聚物的烷基铵盐的混合物,并且通过机械加工碳纳米管和分散介质的混合物至混合物的研磨度为20μm来生产。在1.5l金属容器中,将214.0g硫酸钡“Barit”和2.5g碳纳米管浓缩物同时引入到172.0g可商购的丙烯酸树脂Degalan LP 64/12、600.5g乙酸丁酯、6.0g分散剂Disperbyk 118和5.0g基于改性硅酸盐Claytone HY的流变改性剂的预混混合物中。使用具有磨室TML1、外叶轮直径20mm、内盘直径60mm、锆珠直径在0.8mm至1.0mm范围内、磨室中氧化锆珠与混合物体积的比率8:13的珠磨机Dispermat CN 20来混合混合物。以10.7m/s(3,400rpm)的叶轮转速进行混合30分钟,直至形成均匀的悬浮液;总输入能量为46.8W·h/kg。产生的底漆配制品包含0.005wt.%SWCNT。底漆配制品的体积电阻率为3.4·108Ohm·cm,底漆配制品的研磨度为12μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.35。使用喷枪将制备的底漆配制品施加到由聚丙烯制成的聚合物基材上并在室温下干燥24小时。底漆涂层的干燥后厚度为12μm。底漆涂层的表面电阻为9.8·108Ohm/□。测量的底漆涂层的光反射率值(LRV)为77%。
实施例6
使用碳纳米管浓缩物制备底漆配制品,所述浓缩物包含1wt.%的单壁和双壁碳纳米管和99wt.%的三甘醇二甲基丙烯酸酯、具有高极性颜料亲和(pigment-affine)基团的线性聚合物和高分子量共聚物的烷基铵盐的混合物,并且通过机械加工碳纳米管和分散介质的混合物至混合物的研磨度为23μm来生产。在使用的浓缩物中单壁和双壁碳纳米管的透射电子显微照片如图4所示。在1.5l金属容器中,将50g碳纳米管浓缩物引入到172.0g可商购的丙烯酸树脂Degalan LP 64/12、553.0g乙酸丁酯、6.0g分散剂Disperbyk 118和5.0g基于改性硅酸盐Claytone HY的流变改性剂的预混混合物中。使用顶置式搅拌器以6.3m/s(2000rpm,叶轮直径60mm)的转速混合获得的混合物,直至形成均匀的悬浮液。之后,将214.0g二氧化钛DuPont R706另外引入到混合物中并且使用具有磨室TML1、外叶轮直径40mm、内盘直径60mm、锆珠直径在0.8mm至1.0mm的范围内、磨室中氧化锆珠与混合物体积比率8:13的珠磨机Dispermat CN 20来混合。以叶轮转速10.7m/s(3,400rpm)进行混合30分钟。总输入能量为46.8W·h/kg。生产的底漆配制品包含0.05wt.%的单壁和双壁碳纳米管。底漆配制品的体积电阻率为5.6·104Ohm·cm,底漆配制品的研磨度为14μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.40。使用喷枪将制备的底漆配制品施加到由聚丙烯制成的聚合物基材上并在室温下干燥24小时。底漆涂层的干燥后厚度为14μm。生产的底漆涂层的表面电阻(surface resistivity,表面电阻率)为3.7·105Ohm/□。测得的底漆涂层的光反射率值(LRV)为73%。
实施例7
使用可商购的碳纳米管浓缩物TUBALLTM MATRIX 204制备底漆配制品,所述浓缩物包含10wt.%的单壁碳纳米管和90wt.%的三甘醇二甲基丙烯酸酯和高分子量共聚物的烷基铵盐的混合物并且通过机械加工碳纳米管和分散介质的混合物至混合物的研磨度为40μm来生产。在150ml玻璃容器中,将0.5g碳纳米管浓缩物TUBALLTM MATRIX 204引入预混底漆混合物中,所述预混底漆混合物包含13g可商购的丙烯酸树脂Dianal BR-116(40wt.%的甲苯溶液)、25.7g可商购的丙烯酸树脂Superchlone 930S(20wt.%的二甲苯溶液)、23.7g二甲苯、11.9g乙酸丁酯、24.0g二氧化钛DuPont R706、0.5g基于改性硅酸盐Claytone 40的流变改性剂和0.6g分散剂Disperbyk 118。使用顶置式搅拌器将混合物混合20分钟,直至形成均匀的悬浮液,转速为4.2m/s(2000rpm,叶轮直径40mm)。生产的底漆配制品包含0.05wt.%SWCNT。生产的底漆配制品的体积电阻率为5.0·104Ohm·cm,底漆配制品的研磨度为15μm。由图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.31。使用喷枪将制备的底漆配制品施加在由聚丙烯制成的聚合物基材上并在室温下干燥10分钟。底漆涂层的干燥后厚度为17μm。生产的底漆涂层的表面电阻为6.3·105Ohm/□。测量的底漆涂层的光反射率值(LRV)为67%。
实施例8
如实施例7中所提供,使用可商购的碳纳米管浓缩物TUBALLTM MATRIX 204制备底漆配制品。在500ml金属容器中,将48.0g二氧化钛DuPont R706和1.0g可商购的碳纳米管浓缩物TUBALLTM MATRIX 204同时引入到26.0g可商购的丙烯酸树脂Dianal BR-116(40wt.%甲苯溶液)、51.4g可商购的丙烯酸树脂Superchlone 930S(20wt.%二甲苯溶液)、47.2g二甲苯、24.0g乙酸丁酯、1.0g基于改性硅酸盐Claytone 40的流变改性剂和1.2g分散剂Disperbyk 118的预混混合物中。使用具有附加模块APS-500、直径60mm的聚酰胺盘、氧化锆珠与混合物体积比率1:1的珠磨机Dispermat CN 20,以8.5m/s(2,700rpm)的转速混合混合物30分钟,直至形成均匀的悬浮液;总输入能量为37.2W·h/kg。生产的底漆配制品包含0.05wt.%SWCNT。底漆配制品的体积电阻率为4.8·105Ohm·cm,底漆配制品的研磨度为14μm。从图2所示的与粘度计轴转速相对的底漆配制品的动态粘度可知,底漆配制品满足奥斯特瓦尔德-德沃尔幂律关系,流动特性指数为0.41。使用喷枪将获得的底漆配制品施加在由聚丙烯制成的聚合物基材上并在室温下干燥30分钟。底漆涂层的干燥后厚度为14μm。底漆涂层的表面电阻为2.5·105Ohm/□。测量的底漆涂层的光反射率值(LRV)为72%。
实施例9(比较)
尽管引入20.0g碳纳米管浓缩物,但与实施例4类似地制备底漆配制品。生产的底漆配制品包含0.5wt.%。生产的底漆配制品的体积电阻率为1.2·102Ohm·cm及其研磨度为26μm。从图2可以看出,生产的底漆配制品具有极高的粘度,这限制了其在基材上施加的可能方法。使用喷枪将底漆配制品施加到由聚丙烯制成的聚合物基材上并在室温下干燥24小时。底漆涂层的干燥后厚度为34μm。生产的底漆涂层的表面电阻为7.6·102Ohm/□。测量的光反射率值(LRV)的值为54%。因此,生产的底漆配制品的颜色不够浅。
工业适用性
本发明可用于在静电喷涂前在由具有大于1010Ohm/sq的表面电阻的聚合物或复合材料制成的部件上产生具有至少60%的光反射率值的导电底漆涂层,以及生产这种涂层的底漆配制品的生产。
Claims (18)
1.一种底漆配制品,用于在静电喷涂之前产生部件的浅色导电底漆涂层,其特征在于,所述底漆配制品包含大于0.005wt.%且小于0.1wt.%的浓度的单壁和/或双壁碳纳米管,并且所述底漆配制品的研磨度不大于20μm。
2.根据权利要求1所述的底漆配制品,其特征在于,所述底漆配制品还包含5至40wt.%的一种或几种白色颜料,所述白色颜料选自由氧化镁、氧化锌、二氧化钛、碳酸钙、硫酸钡组成的组。
3.根据权利要求1所述的底漆配制品,其特征在于,所述底漆配制品还包含0.1至2wt.%的一种或几种分散剂,所述分散剂选自高分子量共聚物的烷基铵盐、和/或具有极性基团的线性聚合物、和/或具有极性基团的嵌段共聚物。
4.根据权利要求1所述的底漆配制品,其特征在于,所述底漆配制品的体积电阻率小于108Ohm·cm。
5.根据权利要求1所述的底漆配制品,其特征在于,所述底漆配制品是在奥斯特瓦尔德-德沃尔幂律关系中具有小于0.7的流动特性指数的假塑性非牛顿流体。
6.根据权利要求1所述的底漆配制品,其特征在于,所述底漆配制品还包含0.1至5wt.%的一种或几种流变改性剂,所述流变改性剂选自由膨润土、层状硅酸盐、改性层状硅酸盐和高分子量聚合物组成的组。
7.一种用于生产根据权利要求1所述的底漆配制品的方法,其特征在于,所述方法包括以下顺序的步骤:(A)将单壁和/或双壁碳纳米管的浓缩物引入到至少包含溶剂的混合物中,所述浓缩物是分散体系,所述分散体系包含至少1wt.%的单壁和/或双壁碳纳米管并且通过将碳纳米管和分散介质的混合物机械加工至不大于50μm的所得混合物的研磨度获得;以及(B)混合所得混合物以形成具有不大于20μm的研磨度的均匀悬浮液。
8.根据权利要求7所述的方法,其特征在于,使用具有盘式叶轮的顶置式搅拌器进行步骤(B)中的混合。
9.根据权利要求7所述的方法,其特征在于,使用转子-定子型混合器进行步骤(B)中的混合。
10.根据权利要求7所述的方法,其特征在于,使用珠磨机在大于10W·h/kg的输入能量下进行步骤(B)中的混合,所述珠磨机具有大于0.4mm且小于1.8mm的珠子直径和大于0.5且小于2的珠子体积与悬浮液体积的比率。
11.根据权利要求7所述的方法,其特征在于,在步骤(A)之前将所述底漆配制品的所有其他组分引入到所述溶剂中并混合,并且步骤(A)和(B)的顺序完成所述底漆配制品的生产。
12.根据权利要求10所述的方法,其特征在于,在步骤(A)之前将分散剂和成膜剂引入到所述溶剂中,并且在步骤(A)中,将所述单壁和/或双壁碳纳米管的浓缩物和白色颜料引入到包含溶剂、分散剂和成膜剂的所述混合物中,并且在完成所述底漆配制品的生产的步骤(B)中进行所述白色颜料的分散。
13.一种浅色导电底漆涂层,其特征在于,所述涂层通过下述产生:在所述部件的表面上施加权利要求1所述的底漆配制品,然后进行干燥。
14.根据权利要求13所述的浅色导电底漆涂层,其特征在于,所述涂层的干燥进行直至残留溶剂浓度不大于20wt.%。
15.根据权利要求13所述的浅色导电底漆涂层,其特征在于,待喷涂的所述部件由具有大于1010Ohm/sq的表面电阻的聚合物材料制成。
16.根据权利要求13所述的浅色导电底漆涂层,其特征在于,待喷涂的所述部件由具有大于1010Ohm/sq的表面电阻的复合材料制成。
17.根据权利要求15所述的浅色导电底漆涂层,其特征在于,待喷涂的所述部件由下述制成:聚丙烯;或聚酰胺;或聚碳酸酯;或丙烯腈、丁二烯和苯乙烯的共聚物;或它们的混合物。
18.根据权利要求16所述的浅色导电底漆涂层,其特征在于,待喷涂的所述部件由下述制成:滑石填充聚丙烯、或玻璃填充聚酰胺、或碳填充聚酰胺、或聚酯片材压制材料。
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