CN102414007A - 粉末涂料挤出方法 - Google Patents
粉末涂料挤出方法 Download PDFInfo
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- CN102414007A CN102414007A CN2010800185012A CN201080018501A CN102414007A CN 102414007 A CN102414007 A CN 102414007A CN 2010800185012 A CN2010800185012 A CN 2010800185012A CN 201080018501 A CN201080018501 A CN 201080018501A CN 102414007 A CN102414007 A CN 102414007A
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Classifications
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Abstract
本发明提供一种生产粉末涂料的方法,所述方法包括以下步骤:制备包含树脂和任选其交联剂的粉末涂料预混合料;将预混合料供入通过熔体挤出机,其中熔体挤出机条件包括100-200℃的温度和1-16巴的压力;将挤出材料冷却;和将它粉碎成细颗粒,所述方法的特征在于将1-25重量%(基于所述预混合料的重量)颗粒材料在水中的悬浮液或分散体加入熔体挤出机中,所述水与至少粉末涂料预混合料的树脂不溶混,且所述水作为过热的加压液体保留在熔体挤出机中,其仅当离开挤出机时从预混合料中蒸发,悬浮液或分散体的颗粒材料保留在挤出材料中。
Description
发明领域
本发明涉及一种制备粉末涂料组合物的方法,更特别地涉及一种粉末涂料挤出方法,其中将颗粒材料在水中的悬浮液或分散体注入挤出装置中。
发明背景
粉末涂料组合物为通常包含固体成膜树脂,通常具有一种或多种颜料和任选一种或多种性能添加剂如增塑剂、稳定剂、助流剂和增量剂的固体组合物。通常将树脂热固,掺入例如成膜聚合物和相应交联剂(其本身可以为另一成膜聚合物)。通常,树脂具有30℃以上的Tg,软化点或熔点。
通常,粉末涂料通过将组合物的组分一起干混合,然后将共混物在树脂的软化点以上,但在其固化温度以下的温度下挤出以生产配制成分的熔体混合料。挤出物被立即冷却并被压成固体薄片,其中将配制的涂料逐步粗磨并磨碎至明确的粒度分布以通过涂布器喷雾。
对于将含有颜料和添加剂的那些粉末涂料组合物,成膜树脂与这些组分完全干混合通常使用一系列两个高强度预混合混合机和低强度最后混合机实现。预混合混合机中高速旋转的叶片均匀分布少量颜料和添加剂并有助于树脂的分散。最后混合机-通常含有滚动和切刀叶片-接收来自预混合混合机的产物以及未通过预混合的原料。来自最后混合机或来自中间称量料斗的干混合材料然后进入挤出机的进料孔中。
尽管使用这类混合机,但对于颜料和添加剂而言仍平常的是无效“润湿”,以及因此不能均匀地分散在整个混合物和整个粉末基涂料组合物中。通常着色粉末产量的多达25%必须返回通过挤出机再加工以更完全地分散颜色并实现可重现的配色。
如果颜料不充分地分散,则可不发生粉末产物中最大色强度发展或该颜色发展可能是不一致的。这当产生浅粉色或灰色且其中有色颜料的实际使用可以为小于所产生的粉末总重量的1%时尤其真实。因此,为实现合适的色强度-就美学和功能而言-配方设计师通常需要将过量颜料与粉末基基料组合。但该过量颜料的使用可能是非常有问题的。颜料通常是粉末基涂料组合物的最昂贵组分,因此其过量使用抬高了涂料的成本。此外,过量颜料-和实际上其它添加剂-可导致在将粉末基涂料组合物应用于基质上中的困难以及直接导致固化膜的差外观。例如,太高的着色可导致表面缺陷如针孔和桔皮皱纹。
已开发了某些方法以设法解决颜色控制的问题和粉末涂料中功能添加剂非均匀分布的相关问题。
M.C.Meyer在“Modern Approach to the Pigmentation of PowderCoatings”(www.sunchemical.com)中描述了预分散颜料浓缩物或母料的开发,其中已将颜料预分散在与粉末涂料相容且通常具有低玻璃化转变温度(例如130°F)的树脂中。将这类颜料分散体以与干颜料相同的方式掺入粉末涂料配制剂中,即通过与树脂和粉末涂料配制剂的其它成分一起预混合,随后供入挤出机中。在挤出期间,载体树脂与其它组分一起熔融,从而分布颜料。
为完全实现颜料初级粒子中固有的峰值色强度,Meyer的方法要求将各个可得到的有色颜料最佳地预分散在固体载体树脂中。预分散方法包括多个阶段且以使用板框式压滤机过滤并洗涤初级颜料粒子而开始:颜料作为水润湿的“滤饼”排出,然后将其干燥、粉碎并与载体树脂混合。
WO 2006/047238(Degussa Corporation)描述了一种颜料预分散体,其中载体树脂为液体,该预分散体任选含有有机和无机溶剂、表面活性剂和抗氧化剂。预混合料通过在约1-120分钟期间将液体树脂中的颜料分散体加入以约100-6000rpm的速度旋转的分配器中的其它粉末涂料原料中,然后将预混合料装入挤出机中而制备。然后在升高的温度下加工预混合料直至当形成均匀的预混合料熔体时。
WO2005/103170(PPG Industries)提供一种生产热固性粉末涂料组合物的方法,其包括以下步骤:A)将原材料由初始位置供入挤出机中;B)在原材料进入挤出机中以后且在它离开挤出机以前,将至少一种难掺的添加剂引入原材料中;和C)使组合的原材料和难掺的添加剂通过挤出机的至少一部分以形成热固性粉末涂料组合物。在一个实施方案中,难掺的添加剂包含颜料,其优选为超分散的且可将其以液体颜料分散体或干液体颜料分散体的形式加入挤出机中。如该出版物中所用,术语液体颜料分散体意指分散在与原材料相容的加溶树脂中的颜料。
尽管这类颜料预分散体的使用是有利的,但存在相关的缺点。预分散体的制备要求明显的时间和能量投入。配方设计师还必须找到与最终粉末涂料制备中所用的基料体系相容的载体树脂。此外,颜料的有效分布取决于在引入挤出机筒中以后载体树脂尽可能早地熔融,或取决于在相同点的液体载体树脂的流动行为:这可强加对挤出机中温度和压力条件的要求,这对粉末涂料的基料体系而言不是最佳的。
发明陈述
根据本发明,提供一种生产粉末涂料的方法,所述方法包括以下步骤:
制备包含树脂和任选所述树脂的交联剂的粉末涂料预混合料;
将预混合料供入通过熔体挤出机,其中熔体挤出机条件包括100-200℃的温度和1-16巴的压力;
将挤出的材料冷却;和
将它粉碎成细颗粒,
其中所述方法的特征在于将1-25重量%(基于所述预混合料的重量)颗粒材料在水中的悬浮液或分散体加入熔体挤出机中,所述水与至少粉末涂料预混合料的树脂不溶混,且所述水作为过热的加压液体保留在熔体挤出机中,其仅当离开挤出机时从预混合料中蒸发,悬浮液或分散体的颗粒材料保留在挤出的材料中。
可将一部分含水悬浮液或分散体与预混合料进料组合加入熔体挤出机中,但优选将大部分-最佳地基本所有-含水悬浮液或分散体直接加入熔体挤出机内熔融状态的预混合料中。就这点而言,可将含水悬浮液或分散体在沿着熔体通过挤出机的路径一个或多个点上注入。
经由含水悬浮液或分散体所加入的水的量应对挤出机中保持预混合料为熔融状态所需要的温度具有最小骤冷效应。水应快速地与熔体挤出机在液体注入点的温度和压力平衡。因此优选将含水分散体或悬浮液以1-15重量%(基于预混合料的重量),优选3-14重量%,更优选4-7重量%的量加入。
设定熔体挤出机的温度和压力条件使得在注入以后,水以液态保留在挤出机中且不会达到超临界液态:与至少粉末涂料预混合料的树脂不溶混-优选呈惰性,水形成挤出机内的第二液相。水不会使树脂塑化或溶解,但所得两相体系降低挤出机内预混合料的粘度。
不受理论束缚,水相与树脂相之间的疏水相互作用具有将树脂定位在预混合料中的作用;预混合料物质的非极性聚合物组分与预混合料的更大极性组分一起呈给水相。在这些条件下,水相运载的颗粒材料可高度分布-甚至以纳米级-在整个熔融树脂中。
当它离开熔体挤出机,进入降低的压力环境中时,加入熔体挤出机中的水蒸发。水的蒸发首先用于冷却熔融挤出物。其次,蒸发将不连续物引入冷却、固化的挤出物中,这使挤出物更容易地分裂成具有特殊尺寸的颗粒。第三,水的蒸发提供分配力给加入含水悬浮液或分散体中的颗粒材料。
颗粒材料最终分布在挤出物中将至少部分地由含水悬浮液或分散体中该材料的量和材料的粒度决定。优选颗粒材料占分散体或悬浮液的0.1-60重量%。同样,优选颗粒材料具有0.001-5μm,优选0.01-2μm,更优选0.1-0.5μm的平均粒径。
本发明方法对于颗粒无机和有机颜料的分布具有特殊效用。这类有机颜料可任选被表面改性且可选自:偶氮颜料、酞菁颜料和多环/杂环颜料。类似地,合适的无机着色颜料可选自:金红石和锐钛矿型二氧化钛、炭黑、灯黑、石墨、生烧棕土(raw and burnt umber)、生烧黄土(raw and burntsienna)、碳酸钙、硫酸钡、高岭土、滑石、二氧化硅、云母铁矿、氧化铁棕、氧化铁红、薄铝片、铬酸锶和磷酸锌。这些颜料的分布可通过使基于颗粒颜料的总重量为0.01-20重量%的分散聚合物进一步悬浮或分散在水中而进一步改善。
为评估颜料在整个树脂上的分布,可显色测试挤出物或挤出机中的熔融预混合料。如果该测试可在要引入一批粉末涂料的时间表内进行,则本发明方法可包括反馈控制机制。例如,如果发现给定批料的初始载荷具有令人满意的颜色性能,则显色测试结果可用于改进如下至少一种:熔体挤出机的温度、熔体挤出机的压力、预混合料供入挤出机的速率、分散体或悬浮液加入挤出机的速率、和所述悬浮液或分散体中颗粒材料的量。与所谓批料控制相比,该反馈控制通过使不令人满意的挤出物的量最小化而使产物的损失最小化。此外,它排除了对于各个颜料或颜料组合对预测试树脂配制剂的需要。
预混合料的树脂不意欲限制本发明的特征且可包含任何已知用于粉末涂料组合物的热塑性或热固性树脂。例如,合适的热固性树脂包括羧基官能聚酯、羟基官能聚酯和选自环氧-丙烯酸、聚酯-丙烯酸和环氧-聚酯树脂体系的混杂体系。然而,在本发明的优选实施方案中,树脂选自具有45-120℃的软化点的热固性树脂。
根据本发明的第二方面,提供一种可通过如前文所定义的方法得到的粉末涂料组合物。
发现在通过本发明方法得到的粉末涂料组合物与通过常规方法制备的粉末涂料组合物之间发现有明显区别,所述常规方法即为其中粉末涂料组合物通过将预混合料供入通过熔体挤出机而不具有将颗粒材料在水中的悬浮液或分散体加入熔体挤出机中的步骤的方法。
根据本发明方法制备的材料的断裂表面的精密检查,例如通过使用电子显微镜,显示具有比通过常规方法制备的材料更少微孔的粉末的更光滑表面。
附图简述
将参考附图描述本发明,其中:
图1为适于进行本发明方法的熔体挤出机的第一实施方案的示意图。
图2为适于进行本发明方法的熔体挤出机的第二实施方案的示意图。
定义
为描述本发明组合物中组分的比例,术语“树脂”包括任何树脂或聚合物本身,以及固化剂。
如本文所用,术语“颗粒”意指由保持单独地分散在分散介质中的固体或液体物质的小离散物质组成。
当用于本文中时,任何聚合物的“玻璃化转变温度”或Tg可如Fox在Bull.Amer.Physics.Soc.,1,3第123页(1956)中所述计算。Tg也可使用差示扫描量热法(以20℃/分钟的加热速率,其中Tg在内弯的中点取得)实验测量。除非另有说明,如本文所用,指定的Tg指计算的Tg。
在水中的悬浮液或分散体
要悬浮或分散在水中的颗粒材料可选自在粉末涂料组合物中用作常规添加剂的颗粒组分。这类添加剂用于赋予或改善涂层的性能-例如耐腐蚀性-且就这点而言,当它们均匀地分散在整个粉末涂料组合物中时,添加剂的效率增强。根据本发明加入挤出机中的这类颗粒添加剂在水内的悬浮液或分散体提供这种均匀分布。
颗粒材料原则上可选自:颜料;填料;锌颗粒,包括锌粉;纳米粘土颗粒如(橡胶韧化)胶乳颗粒,特别是软胶乳颗粒;流动控制剂;除气剂;和防结块剂。然而,其它合适颗粒可包括:增粘剂;光稳定剂和UV吸收剂;流动和流平添加剂;光泽改进添加剂;缩孔剂;固化剂;组织形成剂;表面活性剂;抗氧化剂(特别是亚磷酸盐、受阻酚和丙酸盐);抗微生物剂;和有机增塑剂。
在本发明优选实施方案中,分散或悬浮在水中的颗粒材料包括有机着色颜料、无机着色颜料或其混合物。可任选表面改性的有机颜料颗粒应优选选自:偶氮颜料;酞菁颜料;和多环/杂环颜料。无机着色颜料应优选选自:金红石和锐钛矿型二氧化钛;炭黑如可由Engelhard Corporation(Obio)得到的9875 Black;灯黑;石墨;生烧棕土;生烧黄土;碳酸钙;硫酸钡;高岭土;滑石;二氧化硅;云母铁矿;氧化铁棕;氧化铁红;薄铝片;铬酸锶;和磷酸锌。
着色剂或颜料的量可以为至多45份每百重量份树脂(phr),优选0.1-40phr,更优选0.5-35phr。
特别适于经由悬浮液或分散体掺入的填料包括:硅溶胶;玻璃颗粒;玻璃纤维;金属纤维;金属薄片;云母颗粒;偏硅酸钙颗粒;及其混合物。
流动控制剂可以基于水的重量至多3重量%的量存在于所加入的悬浮液或分散体中。增强组合物熔体流动性能并有助于消除表面缺陷的这类流动控制剂通常包括丙烯酸和氟基聚合物。市售流动控制剂的实例包括:P-67、P-200和(均可由Estron Chemical Inc.,Calvert City,KY得到);来自BYK Chemie(Wallingford,CONN)的361和300;和来自Monsanto(St.Louis,MO)的2000。
除气剂也可以以基于水的重量0.1-5重量%的量存在于所加入的水中。这类除气剂促进固化方法期间气体的释放。市售除气剂的实例包括:可由Well Worth Medicines得到的Benzoin;和可由GCA Chemical Corporation(Brandenton,FLA)得到的B。
加入的水还可包含量基于水的重量为0.05-1.0重量%的防结块剂(干流动添加剂)。这类添加剂的实例包括热解法二氧化硅、沉淀二氧化硅、热解法氧化铝、粘土、滑石及其混合物。
认识到需要强大的力将颗粒固体引入并将它们分散在整个挤出机内的熔体中。该分散部分取决于固体可被周围介质润湿的容易性和对该介质的亲合性。为减少分散所需的力,优选使用促进颗粒固体掺入的分散剂。这些在大多数情况下为表面活性物质,也称作表面活性剂,其具有阴离子活性或阳离子活性或非离子结构。
在本发明中,分散剂可以以相对小的量-例如基于颗粒材料的总重量0.01-25重量%-加入颗粒材料分散于其中的水中。在其中悬浮或分散在水中的颗粒材料包含颜料的那些实施方案中,优选该颗粒材料进一步包含基于颗粒颜料的总重量为0.01-20重量%的分散聚合物。
合适的润湿分散剂例如描述于美国专利5,735,944;EP-A-154 678;EP-A-270 126;EP-A-318 999;DE-A-3 930 687;DE-A-1 157 326;和DE-A-1157 327中。
在水中的悬浮液或分散体还可含有至多50%的溶解材料,例如二氧化碳、一氧化二氮或氨,其可或不可与预混合料的组分反应,但影响树脂的极性响应和因此熔体挤出机中两相的尺寸和结构。
为形成悬浮液或分散体,通常进行预混合阶段,其中将所有所需添加剂材料均化。然后通过合适的研磨机如水平介质研磨机加工预混合料:一次或多次通过研磨机是通常的。所得分散体或悬浮液然后为如以下进一步描述可经由注射口加入熔体挤出机中的形式。
粉末涂料预混合料
本发明粉末涂料预混合料必然包含树脂和其交联剂。预混合料可明显包含如本领域所知且将在下文中讨论的其它组分。
1.树脂和交联剂
粉末组合物中的树脂和交联体系不意欲限制本发明的特征。因此,适于包含在粉末涂料预混合料中的树脂包括热塑性和热固性基础树脂。
当用于粉末涂料中时,热塑性树脂必须熔融并在120-300℃的烘干温度下在数分钟内流出成薄膜而没有显著的降解。因此,适用于本发明实践中的热塑性树脂包括聚酰胺、聚酯、纤维素酯、聚乙烯、聚丙烯、聚(氯乙烯)[PVC]、聚(偏二氟乙烯)[PVF2]、聚苯基砜和聚(四氟乙烯)[PTFE],其中聚苯基砜和PTFE是特别优选的。所有合适的热塑性树脂可容易由商业来源得到。
适于本发明的热固性树脂包括环氧树脂、聚氨酯、聚硅氧烷、结晶树脂、聚酯(包括不饱和聚酯)、丙烯酸系树脂,和混杂物如环氧-丙烯酸树脂、聚酯-丙烯酸树脂和环氧-聚酯。这些树脂的玻璃化转变温度(Tg)必须足够高使得颗粒在运输和储存期间可能遭遇的温度下不会稠合在一起或烧结。优选,Tg为45-120℃,其中大于55℃的Tg范围是更优选的。
1.1 环氧树脂
合适的环氧树脂为含具有环氧乙烷官能的脂族或芳族骨架的那些,例如:由表氯醇与双酚如双酚A和双酚F在碱性催化剂的存在下反应而产生的二缩水甘油醚缩聚物;和通过线型酚醛树脂与表氯醇在氢氧化钠作为催化剂存在下反应而合成的线型酚醛树脂的缩水甘油醚。
通常,环氧树脂应具有:600-2000的环氧当量(EEW);300-400的羟基当量;和在150℃下200-2000厘泊(cps),优选300-1000cps的熔体粘度。这类树脂的低熔体粘度可使它们能在小于200℃的温度下被挤出。
优选用于本发明的市售环氧树脂为在商标GT-7004、GT-7071、GT-7072、GT-6259(Huntsman LLC)1001和2042(ShellChemicals,Inc.)下出售的双酚A环氧树脂。
各种用于环氧树脂的固化剂可取决于所需方法和性能得到。双氰胺、改性和取代双氰胺、固体二羧酸和它们的酐是可用于环氧树脂固化的那些试剂的实例。为了方便环氧树脂基粉末的配制以及本发明其它树脂基粉末的配制,固体形式的固化剂是优选的。
1.2 有机硅树脂
用于本发明中的有机硅树脂应:在室温下为固体;具有大于55℃,优选大于60℃的Tg;和在150℃下约500至约10,000cps,优选2000-5000cps的粘度。对于熔融涂料粉末在涂料粉末稠合和固化的温度下适当熔体流动,要求这些粘度参数。上述Tg的下限是防止粉末涂料过度堵塞所需要的。理想地,有机硅树脂还应具有硅氧烷官能(Si-O-H),其特征应优选在于树脂的-OH含量为2.5-7.5重量%。
有机硅树脂的有机结构部分通常为芳基,特别是苯基,或短链(C1-C4)烷基。如果要求最终粉末涂料具有良好耐热性,则甲基和苯基是所选择的有机结构部分。在任何情况下,有机硅树脂应优选具有小于1.5的取代度,更优选1-1.5的取代度(其中取代度定义为每硅原子平均取代基数且为对于各个成分,摩尔百分数乘以取代基数的总和)。
适用于本发明中的有机硅树脂尤其描述于美国专利3,170,890;4,879,344;3,585,065和4,107,148中,通过引用将其公开内容并入本文中。合适的市售有机硅树脂的实例为苯基聚硅氧烷SY-430和甲基聚硅氧烷MK(均为Wacker Silicone,美国的产品)和甲基苯基聚硅氧烷6-2230(DowCorning)。
本发明有机硅树脂应优选含有小于0.2重量%的有机溶剂,优选小于0.1重量%。然而,由于有机硅树脂合成的方法,大多数商业有机硅树脂含有一些残余有机溶剂。这种有机溶剂倾向于被包裹在有机硅树脂内,且当有机硅树脂与其它组分熔体混合形成粉末涂料组合物时,通常不被除去。因此,可需要充分除去这种残余有机溶剂。这通过将有机硅树脂熔融并通过用惰性气体吹扫或通过真空从熔融树脂中除去溶剂而实现。
1.3 羟基官能聚酯树脂
适用于本发明方法中的羟基官能聚酯在官能性方面主要是羟基,且应特征优选在于具有:i)约25至约50的羟基数;ii)小于或等于15,但优选约1-2的酸值;和iii)高于50℃的Tg。
满足这些要求的羟基官能聚酯为作为107、3000/3016和3109市售的。然而,同样,这种聚酯可作为多元羧酸和多元醇的缩合产物形成。因而,用于制备这种聚酯树脂的羧酸包括邻苯二甲酸、四-和六氢邻苯二甲酸和它们的酐、己二酸、癸二酸、对苯二甲酸和间苯二甲酸、1,3-和1,4-环己烷-二羧酸,和偏苯三酸酐,这类酸的酯中一种或多种。另外,合适双官能醇包括乙二醇、二甘醇、丙二醇和三亚甲基二醇,合适二元醇包括己二醇、1,3-、1,2-和1,4-丁二醇、新戊二醇、2-丁基-2-乙基-1,3-丙二醇、2-甲基-1,3-丙二醇、1,4-环己二醇、三羟甲基丙烷及其混合物。技术人员知道进行酸和醇缩合的大量方法。
羟基官能聚酯可通过羟基与脂族和芳族异氰酸酯和与氨基塑料固化。异氰酸酯固化形成树脂,所述树脂在技术上为聚氨酯,但通常作为聚酯出售。氨基塑料为低聚物,所述低聚物为醛,特别是甲醛,与氨基-或带有氨基的物质,例如三聚氰胺、脲、双氰胺和苯胍胺的反应产物。在许多情况下优选使用氨基塑料的前体,例如六羟甲基三聚氰胺、二羟甲基脲和它们的醚化形式,即被具有1-4个碳原子的链烷醇改性。六甲氧基甲基三聚氰胺和四甲氧基甘脲例示了所述醚化形式。因此,多种市售氨基塑料和它们的前体可用于与本发明线性聚酯组合。特别优选可由American Cyanamid得到的氨基交联剂
氨基塑料固化剂通常以足以与聚酯的至少一半羟基反应的量,即羟基官能的至少一半化学计量当量提供。优选交联剂的量足以与聚酯的所有羟基官能充分完全反应,具有氮交联官能的交联剂以每当量聚酯的羟基官能约2-约12当量氮交联官能的量提供。
用氨基塑料将羟基官能聚酯固化在约120-200℃(约250-400°F)的温度下在约20-30分钟内进行。
可使用酸性催化剂通过降低所需温度或提高反应速率或二者而改进用氨基塑料树脂使聚酯固化。当需要在环境储存温度下降低速率时,酸性催化剂可用胺封住。当催化剂未通过热封端时可从固化膜中逸出的挥发性胺适于此目的。对于本发明而言,特别理想的是延迟组合物的完全固化直至涂覆的金属基质已移至固化炉长度的约四分之三。在具体实施方案中,在完全固化以前的停留时间为约33秒。1557,可由King Industries得到的氨基封端的二壬基萘磺酸是适用于本发明粉末涂料组合物的氨基塑料固化中的封闭酸催化剂的实例。固化也可通过加入游离酸如三乙醇胺延迟。
二异氰酸酯通过在羟基位置上在聚合物链之间形成氨基甲酸酯连接键而使羟基官能聚酯树脂固化。合适的脂族二异氰酸酯通过六亚甲基二异氰酸酯(HDI)、二异氰酸根合二环己基甲烷(作为DESMODUR由MllesChemical出售)和异佛尔酮二异氰酸酯(IPDI)例示。甲苯二异氰酸酯(TDI)为合适芳族二异氰酸酯的实例。游离二异氰酸酯的低温反应性可通过将它们与选自苯酚、甲酚、异壬酚、酰胺如ε-己内酰胺、肟如甲基乙基肟和丁酮肟、含亚甲基活性化合物如丙二酸二乙酯和丙二酸异亚丙基酯和乙酰乙酸酯和亚硫酸氢钠的封端剂加成而减弱。加合物具有在升高的温度下断裂以使封端剂和可以以所需方式与聚酯反应的游离二异氰酸酯再生的弱键。封端二异氰酸酯的实例包括己内酰胺封端的异佛尔酮二异氰酸酯和己内酰胺封端的六亚甲基二异氰酸酯。市售的这类固化剂的实例为在CARGILL商标下出售的24-2400、24-2430和24-2450产品。
可使用超过化学计量量约10-20重量%,优选5-10重量%过量的二异氰酸酯。聚酯与二异氰酸酯的反应在约80-约230℃的温度下在湿气不存在下进行,当使用封端二异氰酸酯时,温度优选为至少约120℃,更优选约200℃或更高。二月桂酸二丁锡和三亚乙基二胺为可用于促进二异氰酸酯固化的催化剂的实例。封端异氰酸酯在涂料固化中的使用描述于T.A.Potter等人在Water-Borne & Higher-Solids Coatings Symposium,New Orleans,1986年2月5-7日提出的文章中。
用于二异氰酸酯的其它可选择固化剂包括:Primids,例如PrimidXL552和QM1260,其为可由EMS-Primid得到的羟基烷基酰胺;可由CibaGeigy得到的Araldite PT910缩水甘油酯;和可由DSM得到的Uranox。
1.4 羧基官能聚酯树脂
羧基官能聚酯也适于本发明的目的。这些可由与羟基官能树脂相同的多官能酸和二醇,但用过量酸制备。酸值为约18-约55。优选的商品为:430、3010和7617(可由UCB得到);3400和3900;和可由Ems-Chemin AG得到的GRILESTA V7372。这些羧基官能聚酯的快速固化可用聚环氧化物固化剂如异氰脲酸三缩水甘油酯(TGIC)实现。
适用于本发明实践中的不饱和聚酯包括有机二-或多官能酸和二-或多官能醇的烯属不饱和反应产物。通常酸为不饱和的。这类聚酯树脂通常与可共聚第二树脂如邻苯二甲酸二烯丙酯组合最佳起作用。还可需要掺入引发剂。
1.5 丙烯酸树脂
优选用于粉末涂料的丙烯酸系树脂为丙烯酸和/或甲基丙烯酸烷基酯与甲基丙烯酸和/或丙烯酸缩水甘油酯和烯烃单体如苯乙烯的共聚物。缩水甘油基官能丙烯酸系树脂作为由Mitsui Toatsu Chemicals,Inc.出售,为此,羧基封端聚合物可用作交联剂。丙烯酸和甲基丙烯酸羟基烷基酯共聚物也适于本发明。
1.6 混杂树脂体系
混杂树脂体系如环氧-丙烯酸系和聚酯-丙烯酸系混合物也适于本发明。然而,如果使用这一体系,它优选为聚酯-环氧树脂混杂物。如本领域所知,聚酯-环氧树脂混杂物包含环氧树脂和羧基封端聚酯树脂,还可包含催化剂以驱动固化反应。通常,酸性树脂具有550-1100的当量,环氧树脂具有600-1000的当量。用于环氧-酸反应的催化剂包括季铵盐、季盐、膦、胺、咪唑和金属盐。例如,氧化锌(ZnO2)以每百重量份树脂1-5份作为催化剂有效地改进固化速率和产物的物理性能。
2.预混合料的其它组分
可另外或作为选择将如下文所述可分散在水内的那些颗粒材料加入预混合料中。例如,水可具有分散或悬浮在其中的颗粒颜料和任选分散剂,然而可将其它添加剂-例如填料、锌颗粒、纳米粘土颗粒、胶乳颗粒、流动控制剂、除气剂和防结块剂加入预混合料中。同样,这些单独的添加剂类型可部分地加入预混合料中且部分悬浮或分散在水中,而不是仅在一个或另一个中。本发明因此提供可如何将不同添加剂引入粉末涂料中的配置。
粉末涂料的生产方法
将参考图1描述本发明方法,所述图1描绘了适用于本发明中的熔体挤出机。
通常将预混合料的组分一起干混合。如果该干混合(和/或稍后挤出)可潜在地损害某些上列组合物组分,或同样如果某些磨损组分可能损害混合机和/或挤出机,则可需要将这类组分加入形成的粉末中而不是在预混合料本身中包含它们。例如通常更适当地将添加剂如热解法二氧化硅和氧化铝后混合。
参考图1,提供用于加工粉末涂料预混合料的熔体挤出机(10)。可将来自干混合机的预混合料料流在入口(12)处直接供入熔体挤出机中。
熔体挤出机(10)在本文中作为剖面图描述,其显示同步旋转双螺杆挤出机的一半。这包含管或筒,其中一对螺杆轴安装有大量不同的螺杆元件。这些元件以直线构型排列,使得当以同步旋转方式操作时每对螺杆相互啮合并将材料向出口模头(16)输送。螺杆元件构型的变化当然是可能的。这类变化与操作旋转速度一起使得在沿着挤出机(10)长度的不同点上控制预混合料的吞吐量并因此控制沿着筒的不同点上的压力。然而,不取决于该构型,优选螺杆连续操作并使熔融进料在熔体挤出机(10)的主要部分内经受高剪切混合。筒装配有加热和冷却装置以在沿着筒的不同点上根据需要控制熔体温度。通常将进料区(11a)冷却至20℃以下以防止进料喉中堵塞。通常将熔融区(11b)加热至树脂组分的Tg以上。分散区(11c)通常冷却以将熔体温度保持在操作加工温度下,高剪切螺杆构型和螺杆施加在熔体上的功起作用以通过粘性发热提高熔体温度。
熔体挤出机(10)还包含入口(14),分散体或悬浮液通过所述入口引入。尽管仅阐述一个这种入口(14),但应当理解如果需要的话,分散体或悬浮液可在沿着挤出机(10)的不同入口位置,包括进料喉(12)处加入。为确保分散体或悬浮液被挤出机(10)中的材料最大地吸收,优选将该液体直接注入挤出机(10)的筒部分。
入口或各个入口(14)经由进料管连接在添加剂注射器系统(114,图2)上,所述注射器系统包含压力源、一个或多个用于颗粒添加剂的悬浮液或分散体的加压容器,和压力计(未显示)。进料管包含流量计和控制阀结构(未显示)。压力源和控制阀可用于在操作员的直接管理下建立所述(或各个)含水悬浮液或分散体至熔体挤出机(10)中的流率。作为选择,含水悬浮液或分散体的流率和组成可以在如下所述反馈控制下。
概括地,使预混合料共混物沿着挤出机(10)的长度通过,并到达S部分,在那里将它用含水分散体或悬浮液处理。在S部分处,挤出机中的温度和压力条件必须使得混合的预混合料保持在熔融状态,且注入的水不蒸发或达到超临界状态。应注意到当悬浮液或分散体以这种小的相对量(重量%)加入时,它的加入对挤出机(10)的S部分中的熔体温度具有最小的影响且水温快速地与熔体平衡。因此,技术人员知道关于注入悬浮液或分散体可使用宽范围的温度和压力条件。然而,目前优选在注入挤出机中以前将悬浮液或分散体任选在注射器系统(114)中预热。如果使用预热,则水也不得达到超临界条件,因而优选注射下的水温保持在25-90℃。
对于大部分本发明研究的粉末涂料组合物,挤出机中的熔体温度通常为小于200℃,优选为110-140℃。对于这类温度条件,本发明中所用水蒸发的压力可例如通过咨询的蒸汽表找到,例如Thermodynamic andTransport Properties of Fluids G.Rogers和Y.R.Mayhew,Blackwell UK出版(ISBN0-631-19703-6)中那些。必须首先控制挤出机中在S部分处的压力以确保不会发生水的蒸发,其次不会通过水达到超临界条件。所述压力尤其随挤出机中的预混合料进料速率、螺杆元件的转速、挤出机温度和注入水的进料速率和压力而变。
通过阐述,为实现关于加入水的理想热条件,在200℃下S部分中所需的压力条件将小于16巴。类似地,当在110-140℃的温度下操作时,S部分中的压力应保持在约1.5-3.6巴。
当将悬浮液或分散体在高于挤出机内存在的压力的压力下泵入入口(14)中时,发现有利的效果。压力保持阀可用于提供恒定的泵负荷和工作条件,由此保持工艺稳定性。优选所述保持压力为5-30巴,更优选10-30巴,最优选12-18巴。注入分散体或悬浮液的压力可使用合适的泵控制。
在熔体挤出机(10)的S部分中,分散体或悬浮液与粉末涂料前体组合物中的材料混合。在本发明方法中加入的液体水的量确保加工材料的吞吐量保持在类似于不加入水的程度。此外,该重量确保水不使材料的粘度降至在熔体挤出机(10)内发生差混合或逆流的程度。
已在挤出机中混合并用注入的分散体或悬浮液处理的熔体预混合料-下文为粉末涂料前体-流入挤出机模头(16)中。如本领域中所知,模头(16)可具有为大量不同构型的多个孔。对于本发明没有优选的特殊构型。同样,技术阅读者知道模头(16)可被容许压降通过它们的其它装置置换;例如,这种压降可使用特殊螺杆构型实现。在任何情况下,共混物在熔体挤出机中的平均停留时间通常为小于2分钟,更通常为30-45秒。
应注意挤出机的S部分内的压力可不同于模头出口(16)处的。该出口压力取决于模头的几何形状、待挤出熔体的粘度(其也随温度而变)和流率。因此,通过改变挤出机中螺杆元件的构型和速度和分散体或悬浮液注入点处的材料流量,注射压力可以高于或低于出口压力。然而,在实践操作条件下,模头出口压力优选大于熔体挤出机(10)的S部分中的压力条件。
当熔融前体料流通过模头(16)时,必须将它释放至较低压力并收集。由于该释放,流动料流中的水快速地-优选瞬时气化-导致挤出物起泡。水的蒸发还用于冷却挤出物并将不连续物引入因此形成的固体中。在分散体或悬浮液添加的重量计范围的较高限度下,该冷却效果将使得在将它粉碎成颗粒以前仅需要挤出物的有限的进一步冷却。然而,在5重量%以下的分散体或悬浮液注入水平下可需要例如使用冷却辊二次冷却以防止起泡挤出物聚结。
水的蒸发确保它有效地从粉末涂料中除去。而水的使用对于冷却挤出物的结构具有有利影响,因此水将不会有害地影响得自该挤出物的粉末涂料的性能。此外,蒸发物(蒸汽)可被回收并通过冷凝器和/或分离器以使水再生。
粉末涂料优选以蒸汽的形式被回收,然后经受另外的加工步骤,其中将它粉碎至所需颗粒尺寸。这类步骤可包括研磨和筛分中至少一种。由于引入材料中的弱点,这些步骤可比对于未用分散体或悬浮液处理的挤出物更快速/或在更低的能量成本下进行。所得颗粒然后进入最终产物收集容器中用于随后的处理。
在将它研磨以后,但优选以前,可使用合适测量工具和方法测试挤出物的性能-特别是意欲通过加入熔体挤出机中的悬浮液或分散体内的颗粒赋予的那些性能。例如可使用光学测量传感器或电阻传感器测试挤出物。如果相对于“标准”,未实现所需性能,则对于随后的批料或如果实践可行的话相同批料,挤出机的操作员可通过改进以下至少一项校正这一点:熔体挤出机的温度、熔体挤出机的压力、预混合料供入挤出机中的速率、所述(或各个)分散体或悬浮液加入挤出机中的流率、所述(或各个)分散体或悬浮液加入挤出机中的温度、和所述或各个悬浮液或分散体的组成。挤出机的压力和温度,和悬浮液或分散体的温度应在不发生加入的水蒸发以及不通过该水获得超临界条件的约束条件下进行。
图2阐述本发明的第二实施方案,其中设备具有用于反馈控制的装置。将关于给定生产批料的挤出物的颜色的动态调整讨论该控制,但应认识到该控制也可适用于可以以类似方式测量的挤出物的其它性能。
将批料的预混合料以上文讨论的方式加入熔体挤出机(100)中。另外,制备一种或多种包含颜料的悬浮液或分散体(115a-d)-基于所需所得挤出物颜色-并装入注射器系统(114)中。
参考图2,熔体挤出机(100)的排料区具有连接在透光测量探针(119)上的分光计(118)。该探针(119)在测量点(120)处经由钻孔延伸至挤出机机筒中,它在那里观察熔融材料并产生产物着色的输出信号指征。适于该目的的探针包括Equitech International Corporation(USA)生产的衰减全反射(ATR)和反射聚合物熔体探针。
探针(119)在挤出机(100)的钻孔内安全地使用使得它不干扰其中的混合和捏合元件。还配置探针(119)和钻孔以防止来自挤出机的混合材料出现在测量点(120)的区域内。尽管存在实现这些效果的不同方法,但一种简单的方法要求一步形成钻孔并将制动器(未显示)安装在探针(119)上,其不可通过以下步骤:套管也可穿线地用于钻孔中以进一步保护其中的制动器。
测量探针(119)与分光计(118)组合定期地将光信号发送至基于在测量点(120)处存在的材料混合物的评估装置(121)。
光信号为待挤出混合物的真色强度(“进行中的颜色”)的尺度,并用作评估装置(121)中储存的所需色强度的比较测量。操作在评估装置(121)中进行,由此将标准的反射值与确定的挤出机中熔体的反射值对比。如果给定熔体挤出机(100)内的条件,则探针(119)应理想地进一步包含热电偶或红外线传感器以当探针(119)测量混合物的颜色时同时测量挤出机中熔体的温度。在该实施方案中,评估装置(121)应对温度传感器敏感以补偿所测量的进行中的颜色或作为选择“标准”颜色以得到所测量温度的效果。适于该目的的评估装置为Equitech International Corporation(USA)提供的在线颜色分析器。
如果存在任何与标准的偏差,则建立评估装置(121),优选将提供关于偏差和非偏差的相异的可听和/或可见记号给熔体挤出机(100)的操作员。评估装置(121)还运转地连接在控制器(122)上,所述控制器提供控制信号(123)以回馈到悬浮液或分散体的注射器系统(114)中。
如果建立在预定颜色设定点的外部的与颜色标准的偏差,则控制信号(123)携带指令以动态调整-即在批料加工期间-所述(或各个)分散体或悬浮液加入挤出机(100)中的流率。探针(119)和分光计(118)然后用于建立如何通过在合适时间延迟以后进行其测量而进行挤出物颜色的动态调整。重复该过程直至进行中的颜色与(补偿)颜色标准的偏差在预定的颜色设定点内。
在上述方法中,颜色标准可由预先存在的颜色数据文件得到。作为选择,它可通过直接测量得到,例如通过使用探针(119)和分光计(118)得到具有所需颜色,但小规模,例如在实验室中制备的着色粉末试样的测量。
对于给定的标准或目标产物颜色,通常将本发明反馈控制实施方案用标称组合物和含水分散体或悬浮液(115a-d)流率初始化,其中所述流率决定每单位重量给定预混合料的颜料加入量。初始条件将挤出机的操作点置于所需进行中的颜色越近,颜色将更快速地实现。因此优选使用合适软件使初始条件的选择自动化。
一旦具有预混合料、颗粒颜料和其它添加剂的初始标称组合,则评估装置(121)和/或控制器(122)还应优选包含软件组件以实现连续的着色剂添加剂调整以随后实现所需进行中的颜色。
如本领域所知,挤出物的目标颜色、所需进行中的颜色和给定照明体的测量颜色可分解成描述色空间的三维的三个信号值。色空间的背景可尤其在Judd和Wyszecki,Color in Business Science and Industry,JohnWiley & Sons,New York,1975;Billmeyer,J.和Saltzman,M.,Principlesof Color Technology,John Wiley & Sons,New York,1981;和Wyszecki和Stiles,Color Science:Concepts and Methods,定量数据和公式,第2版,John Wiley & Sons,New York,1982中找到。评估装置(121)和/或控制器(122)的软件和硬件组件应最佳地使三个参数或信号值各自独立地调整以影响颜色。因而,这些装置的软件组件倾向于基于Kubelka-Munk理论或其直线化近似值。
尽管该反馈控制和动态调整可导致给定批料的挤出物的凸出部分由于不正确的颜料添加而损失,但批料的其余部分应具有适当的颜色。此外,因为可经常监控挤出物的颜色,可根据需要调整它。因此,本发明提供当生产小批料着色粉末涂料时显著省时。
在以下实施例中进一步阐述本发明。然而,应当理解需要保护所有在本发明范围内的改变,因此应当理解本发明不受这些实施例限制。
实施例
在以下实施例中,粉末涂料通过在挤出期间加入颜料水分散体而制备。
实施例1
粉末涂料预混合料由下表1所示配制剂A制备。
表1
将该配制剂使用连接在过程控制器上的Brabender螺杆进料机以10kg/h的恒定速率供入Bierstorff Extruder ZE25UT中以精确地保持进料速率。挤出机安装有连接在两个连接在液体进料供应器上的定容计量泵上的液体注入口。接近挤出机的出口,但在通过挤塑螺杆搅拌的区安装有能测量挤出期间熔融材料的反射光谱的颜色探测器。将所述挤出机保持在120℃的加工温度和2巴的出口压力下。另外,所述挤出机装配有备有2个直径为3.5mm的孔的机头出口,(起泡的)产物从所述孔中挤出。
将含有60重量%颜料红(Pigment Red)101的Luconyl NG Red 3370(可由BASF得到)颜料水分散体与稀释水一起以表2所示速率泵入注射孔中。
表2
标称颜料含量(%) | 含水颜料进料速率(升/小时) | 稀释水进料速率(升/小时) |
1 | 0.06 | 0.585 |
6 | 0.36 | 0.51 |
8 | 0.48 | 0.48 |
在挤出期间,使用颜色探测器测量熔体的颜色。该测量的结果在表3中给出。
表3
标称颜料含量(%) | CIE L* | a* | b* |
1 | 61.77 | 12.07 | 1.56 |
6 | 64.17 | 3.05 | -3.74 |
8 | 73.31 | 9.39 | 3.17 |
实施例2
粉末涂料预混合料由配制剂A(如上所述)制备。再次将该配制剂使用连接在过程控制器上的Brabender螺杆进料机以10kg/h的恒定速率供入Bierstorff Extruder ZE25UT中以精确地保持进料速率。挤出机安装有备有连接在液体进料供应器上的定容计量泵的单独液体注入口。将所述挤出机保持在120℃的加工温度和2巴的出口压力下。另外,所述挤出机装配有备有2个直径为3.5mm的孔的机头出口,(起泡的)产物从所述孔中挤出。
将颜料分散体WIMS Hydrotinter 5G448(可由Akzo Nobel GmbH得到)用水稀释以得到7.56重量%颜料分散体。在预混合料A的挤出期间将水分散体以6升/小时的速率泵入注射孔中。
实施例3
粉末涂料预混合料由配制剂A制备并供入配置有如上所述Brabender螺杆进料机、过程控制器、机头出口和两个单独注射孔的Biestorff挤出机中。挤出机中的进料速率保持在10kg/hr的恒定速率。将挤出机保持在120℃的加工温度和巴的出口压力下。
将颜料分散体WIMS Hydrotinter 5b157(可由Akzo Nobel GmbH得到)用水稀释以得到9.18重量%颜料分散体。在预混合料A的挤出期间将水分散体以6升/小时的速率泵入注射孔中。
实施例4
粉末涂料预混合料由配制剂A制备并供入配置有如上所述Brabender螺杆进料机、过程控制器、机头出口和两个单独注射孔的Biestorff挤出机中。挤出机中的进料速率保持在10kg/hr的恒定速率。将挤出机保持在120℃的加工温度和2巴的出口压力下。
将颜料分散体WIMS Hydrotinter 5R852(可由Akzo Nobel GmbH得到)用水稀释以得到9.96重量%颜料分散体。在预混合料A的挤出期间将水分散体以6升/小时的速率泵入注射孔中。
实施例5
粉末涂料预混合料由配制剂A制备并供入配置有如上所述Brabender螺杆进料机、过程控制器、机头出口和两个单独注射孔的Biestorff挤出机中。挤出机中的进料速率保持在10kg/hr的恒定速率。将挤出机保持在120℃的加工温度和2巴的出口压力下。
将颜料分散体WIMS Hydrotinter 5T068(可由Akzo Nobel GmbH得到)用水稀释以得到15重量%颜料分散体。在预混合料A的挤出期间将水分散体以6升/小时的速率泵入注射孔中。
实施例6
将来自实施例1-5的起泡产物冷却以形成固体,干燥并精细研磨使得颗粒可使用106μm筛筛分。然后通过通常方法应用产生的细粉并固化以形成粉末涂覆的板。
通常,根据本发明制备的粉末涂料适于应用于广泛的基质材料上,包括金属和非金属基质。例如可将粉末涂料应用于对涂料为惰性的各种金属基质如铁、钢和铝上。合适的非金属基质可包括木和纸基基质,例如包括碎料板和卡片纸板、玻璃、陶瓷、塑料和橡胶。
Claims (15)
1.一种生产粉末涂料的方法,所述方法包括以下步骤:
-制备包含树脂和任选所述树脂的交联剂的粉末涂料预混合料;
-将预混合料供入通过熔体挤出机,其中熔体挤出机条件包括100-200℃的温度和1-16巴的压力;
-将挤出的材料冷却;和
-将它粉碎成细颗粒,
其中所述方法的特征在于将1-25重量%(基于所述预混合料的重量)颗粒材料在水中的悬浮液或分散体加入熔体挤出机中,所述水与至少粉末涂料预混合料的树脂不溶混,且所述水作为过热的加压液体保留在熔体挤出机中,其仅当离开挤出机时从预混合料中蒸发,悬浮液或分散体的颗粒材料保留在挤出的材料中。
2.根据权利要求1的方法,其中将至少一部分悬浮液或分散体与预混合料进料组合加入熔体挤出机中。
3.根据权利要求1或2的方法,其中所述树脂选自具有45-120℃的软化点的热固性树脂。
4.根据权利要求1-3中任一项的方法,其中所述悬浮液或分散体以1-15重量%,优选3-14重量%,更优选4-7重量%(基于预混合料的重量)的量加入。
5.根据权利要求1-4中任一项的方法,其中所述颗粒材料占分散体或悬浮液的0.1-60重量%。
6.根据权利要求1-5中任一项的方法,其中所述颗粒材料具有0.001-5μm,优选0.01-2μm,更优选0.1-0.5μm的平均粒径。
7.根据权利要求1-6中任一项的方法,其中分散或悬浮于水中的所述颗粒材料包含有机着色颜料、无机着色颜料或其混合物。
8.根据权利要求7的方法,其中所述有机颜料颗粒被表面改性。
9.根据权利要求7或8的方法,其中所述有机着色颜料选自:偶氮颜料、酞菁颜料和多环/杂环颜料。
10.根据权利要求7的方法,其中所述无机着色颜料选自:金红石和锐钛矿型二氧化钛、炭黑、灯黑、石墨、生烧棕土、生烧黄土、碳酸钙、硫酸钡、高岭土、滑石、二氧化硅、云母铁矿、氧化铁棕、氧化铁红、薄铝片、铬酸锶和磷酸锌。
11.根据权利要求7-10中任一项的方法,其中悬浮或分散在水中的颗粒材料进一步包含基于颗粒颜料的总重量为0.01-20重量%的分散聚合物。
12.根据权利要求1-11中任一项的方法,其进一步包括显色测试挤出物的步骤。
13.根据权利要求1-12中任一项的方法,其进一步包括显色测试挤出机中熔融预混合料的步骤。
14.根据权利要求12或13的方法,其中所述显色测试的结果用于改进如下至少一种:熔体挤出机的温度、熔体挤出机的压力、预混合料供入挤出机的速率、分散体或悬浮液加入挤出机的速率、和所述悬浮液或分散体中颗粒材料的量。
15.可通过如权利要求1-14中任一项所定义的方法得到的粉末涂料组合物。
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CN106378919A (zh) * | 2016-08-31 | 2017-02-08 | 玉石塑粉有限公司 | 粉末涂料邦定挤出机及其操作方法 |
CN112917871A (zh) * | 2019-12-06 | 2021-06-08 | 科倍隆有限公司 | 用于生产粉末涂料熔体的方法和装置 |
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