CN116426212A - 一种哑光聚酰亚胺涂层及其制备方法 - Google Patents
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Abstract
本发明公开了一种哑光聚酰亚胺涂层及其制备方法,涉及聚酰亚胺涂层技术领域,是将聚酰胺酸、树脂、固化剂、流平剂、脱气剂,混合,粉碎,过筛,得到粉末涂料;所述聚酰胺酸的固化温度高于树脂的固化温度;采用静电喷涂将粉末涂料喷涂在基底上,固化,即得哑光聚酰亚胺涂层。本发明制得的哑光聚酰亚胺涂层光泽度可达到20%@60°以下实现哑光效果,也可根据实际需求调整涂层光泽度,且采用静电喷涂高温固化涂层吸附力提高。
Description
技术领域
本发明涉及聚酰亚胺涂层技术领域,尤其涉及一种哑光聚酰亚胺涂层及其制备方法。
背景技术
粉末涂料是现代涂料行业重要的组成部分,且随着人们环保意识的提升和环保方面法律的完善,其逐渐被社会认可。高光泽的涂膜因其具有色泽鲜艳明亮的特点,深受市场的欢迎。但是高光泽涂膜带来的强反光作用,会导致人视觉的快速疲劳。为了降低反光强度,减少光污染,满足人们对产品表面柔和舒适的视觉需求,就需要不同光泽度效果的粉末涂料。在制备粉末涂料过程中可通过多种手段降低涂膜光泽,其中添加消光剂或消光填料是得到低光泽度粉末涂料的有效方法,但添加消光剂或消光填料难以将光泽降低到20%@60°以下,且添加量过多会造成涂层吸附力减弱,涂层表面形貌改变等不利影响。
作为高性能工程聚合物的聚酰亚胺,具有突出的耐高低温性能、机械性能、化学稳定性,在汽车工业、塑料制品、家居用品等涂层领域具有巨大的应用价值。因此,利用聚酰亚胺制备哑光涂层具有现实社会价值,受到了越来越多的科研工作者的关注。
发明内容
基于背景技术存在的技术问题,本发明提出了一种哑光聚酰亚胺涂层及其制备方法,制得的涂层光泽度可达到20%@60°以下实现哑光效果。
本发明提出的一种哑光聚酰亚胺涂层的制备方法,包括以下步骤:
S1、取聚酰胺酸、树脂、固化剂、流平剂、脱气剂,混合,粉碎,过筛,得到粉末涂料;所述聚酰胺酸的固化温度高于树脂的固化温度;
S2、采用静电喷涂将粉末涂料喷涂在基底上,固化,即得哑光聚酰亚胺涂层。
优选地,S1中,聚酰胺酸和树脂的总量占原料总质量的80~95%,其中,聚酰胺酸和树脂的质量比为1~3:1。
优选地,聚酰胺酸的制备如下:将芳香族二胺溶于有机溶剂中,配制二胺溶液;在氮气保护下,将芳香族二酐分批加入到二胺溶液中进行缩聚反应,得到聚酰胺酸溶液;将聚酰胺酸溶液进行冷冻干燥去除有机溶剂,得到聚酰胺酸粉末。
优选地,所述芳香族二胺为对苯二胺或4,4'-二氨基二苯醚或其组合;芳香族二酐为均苯四甲酸二酐或3,3',4,4'-联苯四甲酸二酐或其组合;有机溶剂为N,N'-二甲基乙酰胺或N,N'-二甲基甲酰胺。
优选地,芳香族二酐分批加入到二胺溶液中,调节溶液粘度为60000~120000mpa·s,每次加料间隔1h~2h;优选地,缩聚反应的反应温度为10~30℃,反应时间为4~8h,控制聚酰胺酸溶液的固含量在10~20%。
优选地,S1中,树脂为丙烯酸树脂、环氧树脂、聚酯树脂中的任意一种;固化剂为TGIC或HAA;流平剂为聚硅氧烷聚醚、硅酮化合物、氟碳化合物中的任意一种;脱气剂为安息香或二苯氧基丙醇。
优选地,S1中,原料中聚酰胺酸、树脂、固化剂、流平剂、脱气剂的质量百分比为50~60%:30~40%:4~10%:0.8~4%:0.2~1%;粉碎后过150~200目:
优选地,S2中,控制静电喷涂的涂膜厚度在60~80μm。
优选地,S2中,固化分两阶段进行,第一阶段在200~250℃加热10~20min,第二阶段在300~350℃加热20~40min。
本发明还提出了一种采用上述方法制备的哑光聚酰亚胺涂层。
与现有技术相比,本发明的有益效果主要体现在以下几个方面:
1.本发明利用静电喷涂技术,在静电作用下,粉末均匀地吸附于工件表面,经过高温烘烤流平固化后涂层均匀、有良好的吸附力;涂料利用率高达90%以上,节省涂料;且与空气喷涂和高压无气喷涂相比,静电喷涂的颗粒流动速度慢、颗粒飞散的少,作业环境得到改善;静电喷涂的生产效率高,适合工业化大规模生产。
2.本发明提出一种新的消光工艺来制备哑光聚酰亚胺涂层,是在涂料配方中使用聚酰亚胺和树脂这两种不同反应活性体系,分阶段固化,反应活性较快的体系—固化温度低的树脂先部分交联成网状结构,降低了整个体系的流动性,限制了随后反应活性较低体系—固化温度高的聚酰亚胺的交联,两种不同反应的应力收缩形成微观粗糙表面散射光线从而达到消光效果。
本发明制备的哑光聚酰亚胺涂层吸附力强,涂层光泽度可达到20%@60°以下,实现哑光效果,也根据实际需求调整涂层光泽度。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
下述实施例和对比例中的聚酰胺酸的制备如下:取50g 4,4'-二氨基二苯醚(0.25mol),置于418mL N,N’-二甲基乙酰胺(DMAc)中,机械搅拌,得到二胺溶液;在氮气保护下,将54.4g均苯四甲酸二酐(0.25mol)分4批(第一次加入二酐总质量的75%、第二次加入二酐总质量的20%、第三次加入二酐总质量的3%、第四次加入剩余的,每次加料间隔1h)加入到二胺溶液,室温反应6h,得到固含量20%、粘度为1200000(mPa·s)的聚酰胺酸溶液;将聚酰胺酸溶液放入冻干机18h去除N,N’-二甲基乙酰胺(DMAc),得到去除溶剂的聚酰胺酸。
实施例1
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸60g(60%)、丙烯酸树脂30g(30%)、TGIC 7g(7%)、486CFL 2.5g(2.5%)、安息香0.5g(0.5%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末涂料均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段200℃、15min、第二阶段320℃、30min,最终得到哑光聚酰亚胺涂层。
实施例2
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸50g(50%)、丙烯酸树脂40g(40%)、TGIC 7g(7%)、486CFL 2.5g(2.5%)、安息香0.5g(0.5%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段200℃、15min、第二阶段320℃、30min,最终得到哑光聚酰亚胺涂层。
实施例3
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸60g(60%)、丙烯酸树脂30g(30%)、TGIC 9g(9%)、486CFL 0.8g(0.8%)、安息香0.2g(0.2%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段200℃15min、第二阶段320℃30min,最终得到哑光聚酰亚胺涂层。
实施例4
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸60g(60%)、丙烯酸树脂30g(30%)、TGIC 6g(6%)、486CFL 3g(3%)、安息香1g(1%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段200℃、15min、第二阶段320℃、30min,最终得到哑光聚酰亚胺涂层。
实施例5
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸60g(60%)、聚酯树脂BS-4057BG 30g(30%)、HAA 6g(6%)、486CFL 3g(3%)、安息香1g(1%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段220℃、15min、第二阶段320℃、30min,最终得到哑光聚酰亚胺涂层。
对比例1
一种制备哑光聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸70g(70%)、丙烯酸树脂20g(20%)、TGIC 7g(7%)、486CFL 2.5g(2.5%)、安息香0.5g(0.5%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,高温固化分两阶段进行,第一阶段200℃、15min、第二阶段320℃、30min,最终得到半哑光聚酰亚胺涂层。
对比例2
一种制备聚酰亚胺涂层的方法,包括以下步骤:
S1:取去除溶剂的聚酰胺酸90g(90%)、TGIC 7g(7%)、486CFL2.5g(2.5%)、安息香0.5g(0.5%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S2:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S3:将静电喷涂后的铁板放入烘箱中高温固化,320℃高温固化30min,最终得到聚酰亚胺涂层。
对比例3
一种静电喷涂制备涂层的方法,包括以下步骤:
S1:取丙烯酸树脂90g(90%)、TGIC 7g(7%)、486CFL 2.5g(2.5%)、安息香0.5g(0.5%)放入粉碎机粉碎,将粉碎后的细粉通过180目检验筛筛分成粒径细小的粉末作为静电喷涂的粉末涂料;
S5:利用静电喷涂设备将粉末均匀喷涂在铁板上,控制涂膜厚度为60μm;
S6:将静电喷涂后的铁板放入烘箱中高温固化,200℃高温固化15min,最终得到涂层。
对本发明实施例和对比例所得到的涂层进行性能测试,测试结果参照表1所示。
表1涂层测试结果
光泽(%@60°) | 涂层外观形貌 | |
实施例1 | 14 | 平整细腻,哑光 |
实施例2 | 9 | 平整细腻,哑光 |
实施例3 | 10 | 平整细腻,哑光 |
实施例4 | 10 | 平整细腻,哑光 |
实施例5 | 11 | 平整细腻,哑光 |
对比例1 | 23 | 平整细腻,半哑光 |
对比例2 | 70 | 平整,镜面反光 |
对比例3 | 35 | 平整,轻微橘皮 |
由表1可以看出,实施例1-4与对比例2-3对比,聚酰胺酸和丙烯酸树脂这两种不同体系配比的聚酰亚胺涂层光泽度远低于单组分聚酰亚胺或聚丙烯酸树脂体系的涂层光泽度。实施例1-2和对比例1对比,在固化剂、流平剂和脱气剂相同的情况下,聚酰胺酸与树脂两种不同体系的配比不同时,聚酰亚胺涂层光泽度不同,随着树脂含量的增加,聚酰亚胺涂层光泽度逐渐降低达到哑光的效果。在聚酰胺酸与树脂两种不同体系中,树脂的反应活性较快,在200℃第一阶段固化时先部分交联成网状结构,降低了整个反应体系的流动性,限制了后续聚酰胺酸的亚胺化反应,两种不同的反应应力相互影响收缩形成了微观粗糙的表面,散射光线达到哑光。实施例1与实施例3-4对比,聚酰胺酸与树脂配比相同的情况下,调整固化剂、流平剂和脱气剂配比对聚酰亚胺涂层光泽度影响不大。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种哑光聚酰亚胺涂层的制备方法,其特征在于,包括以下步骤:
S1、取聚酰胺酸、树脂、固化剂、流平剂、脱气剂,混合,粉碎,过筛,得到粉末涂料;所述聚酰胺酸的固化温度高于树脂的固化温度;
S2、采用静电喷涂将粉末涂料喷涂在基底上,固化,即得哑光聚酰亚胺涂层。
2.根据权利要求1所述的哑光聚酰亚胺涂层的制备方法,其特征在于,S1中,聚酰胺酸和树脂的总量占原料总质量的80~95%,其中,聚酰胺酸和树脂的质量比为1~3:1。
3.根据权利要求1或2所述的哑光聚酰亚胺涂层的制备方法,其特征在于,聚酰胺酸的制备如下:将芳香族二胺溶于有机溶剂中,配制二胺溶液;在氮气保护下,将芳香族二酐分批加入到二胺溶液中进行缩聚反应,得到聚酰胺酸溶液;将聚酰胺酸溶液进行冷冻干燥去除有机溶剂,得到聚酰胺酸粉末。
4.根据权利要求3所述的哑光聚酰亚胺涂层的制备方法,其特征在于,所述芳香族二胺为对苯二胺或4,4'-二氨基二苯醚或其组合;芳香族二酐为均苯四甲酸二酐或3,3',4,4'-联苯四甲酸二酐或其组合;有机溶剂为N,N'-二甲基乙酰胺或N,N'-二甲基甲酰胺。
5.根据权利要求3所述的哑光聚酰亚胺涂层的制备方法,其特征在于,芳香族二酐分批加入到二胺溶液中,调节溶液粘度为60000~120000mpa·s,每次加料间隔1h~2h;优选地,缩聚反应的反应温度为10~30℃,反应时间为4~8h,控制聚酰胺酸溶液的固含量在10~20%。
6.根据权利要求1-5任一项所述的哑光聚酰亚胺涂层的制备方法,其特征在于,S1中,树脂为丙烯酸树脂、环氧树脂、聚酯树脂中的任意一种;固化剂为TGIC或HAA;流平剂为聚硅氧烷聚醚、硅酮化合物、氟碳化合物中的任意一种;脱气剂为安息香或二苯氧基丙醇。
7.根据权利要求1-6任一项所述的哑光聚酰亚胺涂层的制备方法,其特征在于,S1中,原料中聚酰胺酸、树脂、固化剂、流平剂、脱气剂的质量百分比为50~60%:30~40%:4~10%:0.8~4%:0.2~1%;粉碎后过150~200目。
8.根据权利要求1-7任一项所述的哑光聚酰亚胺涂层的制备方法,其特征在于,S2中,控制静电喷涂的涂膜厚度在60~80μm。
9.根据权利要求1-8任一项所述的哑光聚酰亚胺涂层的制备方法,其特征在于,S2中,固化分两阶段进行,第一阶段在200~250℃加热10~20min,第二阶段在300~350℃加热20~40min。
10.如权利要求1-10任一项所述方法制备的哑光聚酰亚胺涂层。
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