CN112795307B - 一种耐候自清洁自分层涂料及其制备方法和应用 - Google Patents
一种耐候自清洁自分层涂料及其制备方法和应用 Download PDFInfo
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
本发明公开了一种耐候自清洁自分层涂料及其制备方法和应用,所述耐候自清洁自分层涂料包括如下制备原料:碳醇封端聚二甲基硅氧烷、羟基氟碳树脂、环氧树脂、固化剂。本发明在高温固化羟基氟碳树脂基础上引入高活性体碳醇封端聚二甲基硅氧烷和环氧树脂,在涂膜固化过程中由于环氧树脂、氟碳树脂与碳醇封端聚二甲基硅氧烷地有机硅链段三元间的互不相容性及表面能差异,环氧树脂在底层富集与金属基材相结合,氟碳树脂在中间层富集,碳醇封端聚二甲基硅氧烷的有机硅链段在表面富集形成表面有机硅层,形成三层微相分离的自分层涂层,具有高耐候、自清洁、自分层、低表面能、疏水疏油、耐沾污、附着力强等特性。
Description
技术领域
本发明属于功能涂料技术领域,尤其涉及一种耐候自清洁自分层涂料及其制备方法和应用。
背景技术
在涂料工业中,由于绝大多数的单层涂料不能达到良好的保护和装饰效果,通常被涂物体表面需要涂刷多层涂膜才能满足要求。然而每层需分别施工,施工工序多、时间长、费用高,不同层之间可能存在层间结合力弱、使用寿命短等缺点。1976年Funke等提出一个新概念—自分层涂料。自分层涂料油两种(或多种)不相容的高聚物组成,涂装一次施工在底材上之后,能自发地直接产生相分离,在成膜过程中分成两个(或多个)连续的不同功能的涂层,形成不同组成的复合涂层系统,每层显示出不同的特征。这种一次施工的多层涂膜,不仅降低了生产成本,更重要的是解决了多层涂装系统的层间附着力问题。
自1976年Funke等首先研制出粉末自分层涂料以来,自分层理论得到广泛关注。1987年苏联把自分层涂料应用于溶剂型涂料,开始生产溶剂型自分层涂料,用作具有底面两层的磁漆;1989-1993年,欧洲委员会和欧洲涂料聚合物公司共同对自分层涂料的理论和应用进行了大规模的研究,设计领域主要为溶剂型自分层涂料,研制出溶剂型环氧-丙烯酸、环氧-氯化橡胶、环氧-氟-氯共聚物等自分层涂料。
低表面能涂料由于具有较低的表面能(涂膜表面能<25mN/m),灰尘、油渍、污损生物等在涂层表面的结合力弱,难以附着上去,即便附着,也很容易通过雨水冲刷或者其它机械方式轻松去除,体现自清洁或易清洁效果。然而,由于常规低表面能涂料表面能低,与大部分基材的附着力也较低,如何通过自分层技术与低表面能涂料相结合,解决基材附着力以及层间附着力问题,同时实现耐候、自清洁等功能,是目前功能涂料工业上一个有待攻克的重大技术难题。
相关技术公开了一种氟硅改性丙烯酸树脂疏水防腐涂料,该涂料包括按重量配比计的A组分和B组分;A组分包括将疏水树脂45-70、颜填料5-40、溶剂6-30、抗老化剂1-3、分散剂1-5、防沉剂0.5-2经混合、研磨、搅拌制备而成;B组分包括固化剂5-8。该涂料具有疏水性好、附着力、抗光老化性及柔韧性强,且具有自清洁性、耐腐蚀性好、施工方便、可大面积涂刷、性能优良等特点。其中,疏水树脂为选自甲基丙烯酸甲酯、甲基丙烯酸酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸异丁酯或丙烯酸异丙酯、甲基丙烯酸羟丙酯、丙烯酸单体中的两种或两种以上的混合物与含硅丙烯酸酯、含氟丙烯酸酯单体的共聚物(氟硅改性丙烯酸树脂)。该技术方案中没有涉及氟硅改性丙烯酸树脂的具体合成,也没有对疏水树脂中单体比例以及含硅丙烯酸酯、含氟丙烯酸酯的结构、用量以及对改性树脂性能的影响做针对性研究,所选用的可交联固化单体甲基丙烯酸羟丙酯的活性羟基为仲羟基,存在位阻大,反应活性低等问题。并且仲羟基所在的仲碳上带有的C-H极易被过氧化物攻击,导致链段断裂,耐候性差。
有报道公开一种自分层梯度氟硅基超疏水材料,由A组分和B组分构成,所述A组分由氟硅树脂、稀释溶剂、分散溶剂、改性纳米SiO2粉体、改性纳米硅溶胶、偶联剂、消泡剂及流平剂组成,所述B组分为脂肪族聚异氰酸酯。能够解决现有技术中存在超疏水涂层制备工艺复杂、实干时间长、交联固化温度高以及底面双层等不足。该发明制备的超疏水涂层水接触角可达151°以上,滚动角3°左右,并且兼顾柔韧性与超疏水性。然而该技术方案制备的涂层缺乏刚性稳定性,并且成本高昂,难以大面积推广使用。
相关技术公开了一种静态抗污自分层有机硅涂料及其制备方法与应用。所述静态抗污自分层有机硅涂料包括A组分和B组分,A组分为硅醇封端聚二甲基硅氧烷50~90份、氟碳酯-抗污单体调聚物1~40份、催化剂0.1~10份和溶剂0~30份,B组分为5~20份硅酸酯;所述氟碳酯-抗污单体调聚物由(甲基)丙烯酸氟碳酯、(甲基)丙烯酸酯抗污单体、巯基硅烷偶联剂、引发剂和溶剂份制成。该发明所述涂料可形成自分层涂层,其防污官能团富集于涂层表面,赋予材料优异的污损阻抗性,同时有机硅使涂料具有良好污损脱附能力,该自分层材料可满足低航速的船舶以及海上采油平台等设施的防污要求,具有优良减阻性能。然而,该技术方案选用的硅醇封端聚二甲基硅氧烷由于活性官能团为硅羟基,其反应活性较差,并且其所用氟碳酯-抗污单体调聚物缺乏活性羟基,影响了涂层的交联密度以及基材附着力。
发明内容
本发明旨在至少解决现有技术中存在的技术问题之一。为此,本发明的第一个目的是提出一种耐候自清洁自分层涂料,该涂料具有高耐候、自清洁、自分层、低表面能(<25mN/m)、疏水疏油、耐沾污、附着力强等特性。
本发明另一目的在于提供上述耐候自清洁自分层涂料的制备方法。
本发明再一目的在于提供上述耐候自清洁自分层涂料的应用。
为了达到本发明目的,本发明的技术方案是:
本发明的第一方面是提供一种耐候自清洁自分层涂料,包括如下制备原料:碳醇封端聚二甲基硅氧烷、羟基氟碳树脂、环氧树脂、固化剂。
所述碳醇封端聚二甲基硅氧烷的化学结构为:
其中,所述R包括-(CH2)aCH3、-(CH2)bCH2OH中的至少一种,n=3~100,m=1~17,a=0~19,b=1~17。
所述羟基氟碳树脂的羟值为10mgKOH/g~100mgKOH/g,优选30mgKOH/g~60mgKOH/g。
所述环氧树脂包括双酚A环氧树脂、双酚F环氧树脂中的至少一种,优选环氧值为0.20mol/100g~0.51mol/100g,固含量为50%~70%的双酚A环氧树脂。
所述固化剂包括氨基树脂固化剂、异氰酸酯类固化剂中的至少一种,所述氨基树脂固化剂包括甲醚化三聚氰胺树脂、高亚胺基甲醚化三聚氰胺树脂、正丁基醚化三聚氰胺树脂、正丁基醚化苯代三聚氰胺树脂中的至少一种。当采用氨基树脂固化剂时,由于氨基树脂固化剂在常温下不反应,需要高温烘烤(200℃~250℃之间)才能固化,因此所述耐候自清洁自分层涂料可配成单组份涂料;当采用异氰酸酯类固化剂时,由于异氰酸酯反应活性很强,需要将耐候自清洁自分层涂料配成双组分涂料。
按重量分数计,所述耐候自清洁自分层涂料包括如下制备原料:
所述耐候自清洁自分层涂料的制备原料还包括助剂,所述助剂包括催化剂和溶剂。
所述催化剂为封闭型的酸催化剂,包括对甲苯磺酸、对十二烷基苯磺酸、二壬基萘二磺酸中至少一种。
所述溶剂包括苯类溶剂、酯类溶剂、酮类溶剂中的至少一种。更具体地,所述溶剂包括甲苯、二甲苯、醋酸丁酯、醋酸乙酯、丁酮、甲基异丁基酮、乙二醇丁醚醋酸酯、乙二醇二醋酸酯、丙二醇甲醚醋酸酯、丙二醇乙醚醋酸酯中的至少一种。
按重量分数计,所述耐候自清洁自分层涂料包括如下制备原料:
进一步优选地,按重量分数计,所述耐候自清洁自分层涂料包括如下制备原料:
本发明的第二方面是提供一种耐候自清洁自分层涂料的制备方法,包括如下步骤:将所述耐候自清洁自分层涂料的所有制备原料搅拌混合,得到耐候自清洁自分层涂料。
所述搅拌混合的转速为100r/min~500r/min。
所述搅拌混合的温度为10℃~40℃,优选常温。
所述搅拌混合的时间为10min~60min。
本发明的第三方面是提供所述耐候自清洁自分层涂料在建筑铝单板、海洋防腐防污损、轨道交通、家居涂装、市政工程、风力发电等行业的应用。
所述耐候自清洁自分层涂料的应用方法为:将所述耐候自清洁自分层涂料喷涂或者滚涂到基材上,于180℃~245℃下烘烤固化3min~30min。
与现有技术相比,本发明具有以下有益效果:
1、本发明在高温固化羟基氟碳树脂基础上引入高活性体碳醇封端聚二甲基硅氧烷和环氧树脂,在涂膜固化过程中由于环氧树脂、氟碳树脂与碳醇封端聚二甲基硅氧烷地有机硅链段三元间的互不相容性及表面能差异,环氧树脂在底层富集与金属基材相结合,氟碳树脂在中间层富集,碳醇封端聚二甲基硅氧烷的有机硅链段在表面富集形成表面有机硅层,形成三层微相分离的自分层涂层。
2、本发明构建的三层微相分离的自分层涂层,环氧树脂富集在底层与金属基材相结合,给涂层提供高附着力;富集在中间层的氟碳树脂给涂层提供了高机械性能和高耐候、高防腐蚀性;富集在表面的有机硅层给涂层提供了爽滑性、防水防油防污和自清洁功能。
3、本发明构建的三层微相分离的自分层涂层,通过使用氟碳树脂和有机硅链段的不相容性,进一步增强有机硅链段向涂层表面迁移,氟碳树脂和有机硅链段两个低表面能组分的协同作用,进一步降低涂层表面能,提高疏水疏油性能。
4、本发明采用的碳醇封端聚二甲基硅氧烷的两端含有烷基链段,相比于传统的硅醇封端聚二甲基硅氧烷,具有更高的反应活性和更好的体系相容性,在高温烘烤条件下可充分参与固化反应,得到致密、平整、结构刚性的漆膜,避免了硅醇封端聚二甲基硅氧烷由于反应活性低、体系相容性差,在固化反应过程中容易出现固化不完全导致小分子硅油渗出流失,并且出现缩孔、橘皮等漆膜弊病。
5、本发明提供的制备方法简单可行,一次涂装就可得到三层微相分离的不同功能的涂层,并且只需要进行一次烘烤固化,极大的节省了人力及能源消耗,提高了生产效率。
具体实施方式
为了更好的说明本发明,下面结合具体实施方式作进一步说明。本发明中所用试剂或仪器均可由市场购得,使用的检测方法等都是本领域所熟知的,在此不再赘述。
实施例1
将80g碳醇封端聚二甲基硅氧烷(R=-CH3,n=3,m=3)、120g羟基氟碳树脂(羟值45mgKOH/g)、80g环氧树脂E20、80g氰特CYMEL 1156固化剂、0.8g金氏NACURE 2500催化剂和439.2g二甲苯于室温300r/min转速下搅拌混合反应30分钟,得到耐候自清洁自分层涂料。
实施例2
将135g碳醇封端聚二甲基硅氧烷(R=-(CH2)6CH2OH,n=15,m=6)、225g羟基氟碳树脂(羟值60mgKOH/g)、72g环氧树脂E44、180g氰特CYMEL 325固化剂、4.5g金氏NACURE 2107催化剂和103.5g丙二醇甲醚醋酸酯、180g乙酸乙酯于室温100r/min转速下搅拌混合反应60分钟,得到耐候自清洁自分层涂料。
实施例3
将135g碳醇封端聚二甲基硅氧烷(R=-(CH2)19CH3,n=50,m=12)、270g羟基氟碳树脂(羟值30mgKOH/g)、45g环氧树脂E51、135g氰特CYMELXW3106固化剂、4.5g金氏NACURE 5414催化剂和310.5g乙酸丁酯于室温500r/min转速下搅拌混合反应10分钟,得到耐候自清洁自分层涂料。
实施例4
将180g碳醇封端聚二甲基硅氧烷(R=-(CH2)17CH2OH,n=100,m=17)、180g羟基氟碳树脂(羟值35mgKOH/g)、72g环氧树脂E44、135g氰特CYMEL 303LF固化剂、9g金氏NACURE 3525催化剂和144g二甲苯和180g甲基异丁基酮于室温250r/min转速下搅拌混合反应25分钟,得到耐候自清洁自分层涂料。
对比例1
将120g碳醇封端聚二甲基硅氧烷(R=-(CH2)6CH2OH,n=15,m=6)、64g环氧树脂E44、160CYMEL 325固化剂、4g金氏NACURE 2107催化剂和172丙二醇甲醚醋酸酯、280g乙酸乙酯于室温100r/min转速下搅拌混合反应60分钟,得到有机硅-环氧涂料。
对比例2
将200g羟基氟碳树脂(羟值70mgKOH/g)、64g环氧树脂E44、160g氰特CYMEL 325固化剂、4g金氏NACURE 2107催化剂和172g丙二醇甲醚醋酸酯、160g乙酸乙酯于室温下100r/min转速下搅拌混合反应60分钟,得到有机硅-环氧涂料。
对比例3
将135g硅醇封端聚二甲基硅氧烷(n=15)、225g羟基氟碳树脂(羟值60mgKOH/g)、72g环氧树脂E44、180g氰特CYMEL325固化剂、4.5g金氏NACURE 2107催化剂和103.5g丙二醇甲醚醋酸酯、180g乙酸乙酯于室温100r/min转速下搅拌混合反应60分钟,得到自分层涂料。
对比例4
将135g硅醇封端聚二甲基硅氧烷(n=360)、225g羟基氟碳树脂(羟值60mgKOH/g)、72g环氧树脂E44、180g氰特CYMEL325固化剂、4.5g金氏NACURE 2107催化剂和103.5g丙二醇甲醚醋酸酯、180g乙酸乙酯于室温100r/min转速下搅拌混合反应60分钟,得到分层涂料。
性能测试:
采用上述实施例1~4和对比例1~4的涂料,使用30#线棒在洁净的马口铁板上刮板制备湿膜,放入230℃烘箱中烘烤10min,冷却后对漆膜进行性能测试,结果见表1。
表1.涂料性能测试结果
从表1可以看出,由本发明实施例1~4制备的制备得到的耐候自清洁自分层涂料漆膜各项性能皆大幅优于对比例1~4。其中,
(1)实施例1~4的铅笔硬度、杯凸测试、拉开法附着力和耐冲击性结果表明:本发明制备的涂料在湿膜固化过程中发生了自分层作用,环氧树脂迁移到底层与金属基材相结合,提供了优异的基材附着力,羟基氟碳树脂和以有机硅链段往中间层及表层迁移,提供了优异的表面性能,使得涂膜具有优异的附着力、机械性能、耐冲击性及柔韧性能;而对比例3和对比例4虽然也发生了自分层效应,但是由于硅醇封端聚二甲基硅氧烷的低反应活性,使得大部分硅醇封端聚二甲基硅氧烷没有参与到固化反应中来,而是以助剂的形式游离在漆膜中间,极大的降低了漆膜的附着力和表面性能。
(2)实施例1~4的对水接触角测试、动摩擦系数Ud测试和耐污性测试结果明显优于对比例1~4,同时漆膜表面能都低于25mN/m,属于低表面能漆膜,也明显低于对比例1~4的漆膜表面能,这是由于涂料湿膜在固化过程中,羟基氟碳树脂和有机硅的表面张力差异以及不相容性,导致羟基氟碳树脂和以有机硅链段往中间层及表层迁移,氟硅协同作用,使得氟硅链段表面迁移更加明显,得到了低表面能、疏水疏油、滑爽和低粘附性能的涂层,体现了一定程度的自清洁效果。而对比例1和对比例2由于没有氟硅协同效应,相关性能明显低于本发明的耐候自清洁自分层涂料。
(3)从表1的除冰强度测试结果可以看出,实施例1~4的防结冰性能显著优于对比例1~4,这是由于实施例1~4采用高反应活性的碳醇封端聚二甲基硅氧烷和羟基氟碳树脂,两者协同作用构建具有高强度的低表面能漆膜,有机硅链段富集在涂层最表面,提供疏水、爽滑、低粘附性等功能,体现了较好的防结冰性和低的除冰强度。
(4)实施例1~4的耐液体介质、耐水性、MEK和耐盐雾性测试结果明显优于对比例1~4,说明本发明制备的涂料固化程度和交联密度高,加上氟硅协同作用形成低表面能外涂层,极大的阻挡水和氧气的透过,使得本发明的耐候自清洁自分层涂料具有优异的耐化学性、耐溶剂性、耐盐雾、耐腐蚀性及耐水性;
(5)实施例1~4的耐人工气候加速试验结果明显优于对比例1~4,这是由于高活性的碳醇封端聚二甲基硅氧烷和羟基氟碳树脂形成致密的外层涂层,避免了环氧树脂层受到紫外线和水的破坏导致降解的发生。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (8)
1.一种耐候自清洁自分层涂料,其特征在于:按重量份数计由如下制备原料制得:
碳醇封端聚二甲基硅氧烷 5~30份
羟基氟碳树脂 5~30份
环氧树脂 5~30份
固化剂 5~30份
催化剂 0.1~3份
溶剂 10~80份。
3.根据权利要求1所述耐候自清洁自分层涂料,其特征在于:所述羟基氟碳树脂的羟值为10 mgKOH/g~100 mgKOH/g。
4.根据权利要求1所述耐候自清洁自分层涂料,其特征在于:所述环氧树脂包括双酚A环氧树脂、双酚F环氧树脂中的至少一种。
5.根据权利要求4所述耐候自清洁自分层涂料,其特征在于:所述环氧树脂为环氧值为0.20 mol/100g~0.51 mol/100g,固含量为50%~70%的双酚A环氧树脂。
6.一种权利要求1~5任一项所述耐候自清洁自分层涂料的制备方法,其特征在于:包括如下步骤:将所述耐候自清洁自分层涂料的所有制备原料搅拌混合,得到耐候自清洁自分层涂料。
7.权利要求1~5任一项所述耐候自清洁自分层涂料在建筑铝单板、海洋防腐防污损、轨道交通、家居涂装、市政工程或风力发电中的应用。
8.一种权利要求1~5任一项所述耐候自清洁自分层涂料的使用方法,其特征在于:将所述耐候自清洁自分层涂料喷涂或者滚涂到基材上,于180℃~245℃下烘烤固化3 min~30 min。
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