CN1175073C - 耐气候老化的粉末涂料的制备方法 - Google Patents
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Abstract
一种通过将粉末涂料组合物施涂在金属或非金属表面上,然后再熔融和固化来制备耐气候老化粉末涂层的方法,其中所施涂的粉末涂料组合物含有聚酯树脂和作为交联剂的多官能度低分子量环氧化物,其中聚酯树脂中酸结构单元只基于或主要基于芳族二羧酸、它们的酸酐和/或酯,然后熔融并用NIR辐射进行固化。
Description
本发明提供了一种制备金属和非金属基材上的外部耐气候老化粉末涂料的方法。
已经发现在涂布金属时粉末涂料的装饰性或功能性表面涂层具有广泛的应用,因为此方法具有较高的经济可行性并且从保护环境的观点考虑评价较好。已经开发出了许多粉末涂料配方以用于不同的领域。对于经受紫外线辐射的涂层,例如那些暴露于室外条件下(建筑油漆、窗框、车库门、金属门、庭园家具、汽车部件等)的涂层来说,已经开发出了稳定的粉末涂料体系,例如基于具有末端羧基的聚酯树脂的涂料体系。通常这些聚酯树脂用低分子量、高官能度的交联剂如多官能度的环氧化物或羟烷基酰胺来固化。
基于以芳族羧酸如对苯二甲酸或间苯二甲酸为基的聚酯的外部耐气候老化粉末涂料已经广为人知并且已经使用了一段时间。制备基于这些聚酯树脂的粉末涂料是成本效果合算的,并且涂层具有良好的机械性能和耐侯性,足以用于许多领域,特别是在气候条件温和的地方。这类粉末涂料体系用已知的传统方法固化在基材上。
粉末涂料体系耐气候老化性能的提高已经有诸多尝试了。例如已经有人尝试通过使用只由或主要由脂肪族和/或脂环族组分构成的聚酯树脂来改进粉末涂料的耐气候老化性。这些聚酯树脂描述于,例如美国专利US-PS 5486988和欧洲专利0 561 102。尽管由这些树脂制备的粉末涂料表现出改进的耐气候老化性,但它们的机械性能基本上都较差,并且与上述基于芳族羧酸的体系相比原材料成本较高。
因此本发明的目的是提供成本效果合算的没有上述不足的粉末涂料涂层。具体地说,该粉末涂料应当满足提高耐气候老化性的要求,这样它们才可以用于,例如气候条件极端的地方而不会损伤涂层。
此目的可以通过下面的方法实现:将基于含有芳族二羧酸、它们的酸酐和/或酯作为基本成分,并且用低分子量、多官能度环氧树脂交联的聚酯树脂的粉末涂料涂层,利用近红外区域内(NIR)的辐射来固化。
此粉末涂料组合物可以含有,例如40-95重量%的聚酯和1-20重量%的低分子量多官能度环氧树脂,其中其它传统成分也可以传统的用量存在,以使所有成分的总量达到100重量%。
聚酯的数均分子量Mn为,例如500-10000,玻璃化转变温度为,例如30-80℃。
聚酯可以含有羟基和/或羧基官能团,其中如果存在此种官能化作用,则羟值可以是,例如10-200,而酸值可以是,例如10-200。
根据本发明所使用的NIR辐射是短波红外辐射,其最大强度的波长范围是约760-约1500纳米,优选780-1200纳米。利用NIR辐射来使漆料干燥是普遍已知的(Kai Br,JOT2/98)。按照此方法,在高强度NIR辐射的协助下粉末涂料可以在短时间内固化,而不会对基材产生任何实质上的加热。
令人惊讶的是发现基于含有芳族二羧酸如对苯二甲酸或间苯二甲酸、它们的酸酐和/或酯作为基本结构单元,同时含有低分子量、多官能度的环氧化物作为交联剂的聚酯树脂的粉末涂料在用NIR辐射固化时,具有比通常用这类树脂体系以传统方法,例如在循环空气加热炉中进行固化所产生的耐候性要好地多的耐气候老化性。涂层的机械性能如柔韧性至少与用传统固化方法所产生的柔韧性处于同一水平。此外,NIR固化与传统的加热炉固化相比,能够实质性地缩短固化时间。
可以用于本发明方法的粉末涂料配方中含有羟基和/或羧基官能化的聚酯作为基料的基础,该聚酯含有芳族二羧酸、它们的酸酐和/或酯例如对苯二甲酸或间苯二甲酸作为酸结构单元的唯一或主要成分,它们与传统的脂肪族二醇例如新戊二醇、乙二醇、丁二醇、己二醇或二甘醇或环己烷二甲醇反应。其它芳族二羧酸的例子是萘-2,6-二羧酸、萘-1,5-二羧酸和苯二甲酸。优选使用基于对苯二甲酸和间苯二甲酸或它们的酸酐的羧基官能化聚酯。
相对于聚酯中的二羧酸部分,优选芳族二羧酸大于50%的酸组成,特别优选对苯二甲酸和/或间苯二甲酸或者它们的酸酐和/或酯大于50重量%的酸组成。
任选地脂肪族和/或脂环族二羧酸,例如己二酸或环己烷二羧酸被用作次要组分,其中脂肪族和/或脂环族二羧酸部分不超过50%,相对于聚酯中的二羧酸部分。至于其它组分,聚酯树脂中可以含有少量的多官能度支化剂如甘油或三羟甲基丙烷,以及添加剂如加速剂。还可能使用不同聚酯的混合物。根据本发明可以使用的聚酯可以通过传统的将二羧酸、它们的酸酐和/或酯与二醇反应来制备,例如参见D.A.Bates,“The Science of Powder Coatings(粉末涂料科学)”,1和2卷,Gardiner House,London,1990。
适用于本发明方法中的粉末涂料配方含有一定量的低分子量、多官能度环氧化物作为交联组分以用于固化。用量通常是1-20重量%,相对于聚酯/环氧化物体系。可以用作交联剂的有,例如异氰酸三缩水甘油酯(TGIC)、基于对苯二甲酸/苯偏三酸的多缩水甘油基酯(例如可购于汽巴精化公司,商标名为AralditePT 910)、多官能度脂肪族环氧乙烷化合物如DSM树脂公司提供的商标名为Uranox的化合物、或缩水甘油基官能化的(甲基)丙烯酸酯共聚物。
含有聚酯和环氧化物交联剂的粉末涂料配方可以任选地含有其它传统组分,例如颜料和/或填料,以及任选地其它传统添加剂如流动控制剂、脱气剂和/或加速剂。它们以本领域内技术人员所熟知的用量加入,例如使用0-50重量%的颜料和/或填料以及0.02-3重量%的传统添加剂。
本发明的粉末涂料是通过已知的挤出/碾磨法来制备的,该方法对于本领域内技术人员而言是熟知的。也可以使用其它方法,例如用超临界溶液喷雾法或非水性分散法来制备粉末。
在本发明的方法中,上述粉末涂料用已知的粉末施涂工艺施涂到要涂布的基材上,例如用静电喷涂法,然后熔融并用NIR辐射照射来固化,此NIR辐射的最大强度分布区域在,例如800-1200纳米,照射时间为,例如1-200秒,优选1-30秒。适用于本发明涂布方法的辐射元件是市售的,例如购于SerVis工业公司(Industrie SerVisCo.);例如可以使用辐射元件温度达到3500K的卤素灯。也可以使用传统热源(红外辐射、对流加热炉)和任选地与其它反射镜/透镜系统的组合。
优选使用没有其它组合的NIR辐射来进行固化。
与基于相同树脂的传统固化粉末涂料涂层相比,根据本发明方法得到的涂层具有特别的流动特性、良好的机械性能和大大改善的耐气候老化性能。
粉末涂层所需的光泽度可以通过改变粉末涂料配方来调节。可能会生成高光泽度或丝光(Silk-finish)或无光泽的涂层。
根据本发明方法得到的粉末涂料可以用在所有需要耐气候老化性的领域。金属如铝、铁或其它木基材料如中等密度纤维板(MDF)或不同材料的混合物都可以用作基材。由于所得到的涂层的良好机械性能,特别是柔韧性,该方法也特别适用于涂布线圈或预涂布的金属(PCM)。
根据本发明的方法,通过使用成本效果合算的原材料可以经济可行地制备具有优越性能的外部耐气候老化粉末涂层,并且明显减少了固化时间。
下列实施例用来解释本发明:
制备粉末涂料
列于表中的粉末涂料配方用传统用来制备粉末涂料的方法,通过各组分的剧烈混合,挤出和碾磨转化为涂料粉末。
使用电晕喷涂枪将粉末以相同的层厚静电施涂到铝测试板上。使用根据本发明的方法,在购于SerVis工业公司(Industrie SerVisCo.)的500W NIR辐射元件提供的strip unit中进行固化,功率/单位面积为120kW/m2。固化时间分别为:实施例1为5秒,实施例2为12.5秒,实施例3为15秒,实施例4为8秒。在辐射元件与基材之间的距离为50毫米的条件下进行固化。
至于对比例的情况,样品在循环空气加热炉中200℃固化10分钟。
表1:粉末涂料组合物
实施例编号 | 1 | 2 | 3 | 4 |
颜色 | 黑色 | 红色 | 白色 | 灰色 |
树脂Alftalat AN03640 | 57% | 57% | 57% | 57% |
硬化剂Araldite PT 910 | 5.2% | 5.2% | 5.2% | 5.2% |
颜料 | 1%炭黑 | 2%有机红颜料 | 25%二氧化钛 | 19.8%无机颜料 |
填料 | 32.3% | 31.3% | 8.3% | 13.5% |
*一种聚酯,其中酸组分含有对苯二甲酸和间苯二甲酸作为主要成分。
所有配方都含有4.2%的市售流动控制剂和0.3%的脱气辅助物。
耐气候老化试验
在耐气候老化测试之前和之后均检测机械性能,所有样品的结果如下:
落球冲击试验(ASTM D 2794):20英寸磅,
棒轴柔韧性试验(DIN EN ISO 1519)4毫米
Erichsen试验(DIN EN ISO 1520)7毫米
划格法附着力试验(DIN EN ISO 2094)GtOA
所有样品都进行快速老化试验QUV(B)313纳米。表2给出了剩余光泽度(在60°测量)下降到老化测试前起始数值的50%之后的时间。
表2:老化试验后的测试结果
对应于实施例号码的样品 | 1 | 1* | 2 | 2* | 3 | 3* | 4 | 4* |
剩余光泽度<50%后的时间(小时) | 450 | 350 | 500 | 400 | 500 | 400 | 500 | 350 |
*非本发明的样品,在循环空气加热炉中固化。
Claims (7)
1.一种通过将粉末涂料组合物施涂在金属或非金属表面上,然后再熔融和固化来制备耐气候老化粉末涂层的方法,其特征在于施涂一种含有聚酯树脂和作为交联剂的多官能度低分子量环氧化物的粉末涂料组合物,所述环氧化物选自异氰酸三缩水甘油酯、基于对苯二甲酸的多缩水甘油基酯、多官能度脂肪族环氧乙烷化合物、缩水甘油基官能化的(甲基)丙烯酸酯共聚物,并且其中聚酯树脂中酸结构单元含有多于50重量%的芳族二羧酸、它们的酸酐和/或酯,然后熔融并用近红外区域内辐射进行固化。
2.按照权利要求1的方法,其特征在于所使用的粉末涂料组合物含有40-95重量%的聚酯树脂。
3.按照权利要求2的方法,其特征在于聚酯是羧基官能化的。
4.按照权利要求1的方法,其特征在于聚酯树脂基于对苯二甲酸和/或间苯二甲酸、它们的酸酐和/或酯。
5.按照权利要求4的方法,其特征在于多于50重量%的对苯二甲酸和/或间苯二甲酸或者它们的酸酐和/或酯被用作聚酯树脂中的酸成分。
6.按照权利要求1的方法,其特征在于固化时间的范围是1-30秒。
7.按照权利要求1的方法,其特征在于使用最大强度分布为0.8-1.2微米的近红外区域内辐射元件。
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DE19935539A DE19935539A1 (de) | 1999-07-30 | 1999-07-30 | Verfahren zur Herstellung witterungsstabiler Pulverbeschichtungen |
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CN1175073C true CN1175073C (zh) | 2004-11-10 |
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EP (1) | EP1208176B1 (zh) |
JP (1) | JP2003506517A (zh) |
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CO (1) | CO5160381A1 (zh) |
CZ (1) | CZ2002357A3 (zh) |
DE (2) | DE19935539A1 (zh) |
ES (1) | ES2223567T3 (zh) |
HU (1) | HUP0201979A3 (zh) |
MX (1) | MXPA02001079A (zh) |
MY (1) | MY122733A (zh) |
NO (1) | NO20020401L (zh) |
PL (1) | PL353200A1 (zh) |
PT (1) | PT1208176E (zh) |
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DE10120011B4 (de) * | 2001-04-24 | 2005-07-14 | Advanced Photonics Technologies Ag | Verfahren zum Beschichten eines dünnen Flächenkörpers mit einem Substrat |
JP2007522329A (ja) * | 2004-02-11 | 2007-08-09 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | 向上された流動特性を有する近赤外線硬化粉体塗料組成物 |
EP1798267A1 (en) * | 2005-12-15 | 2007-06-20 | Dupont Powder Coatings France S.A.S. | Powder coating composition suitable for coil coating |
DE102006062041A1 (de) * | 2006-12-29 | 2008-07-03 | Evonik Degussa Gmbh | Verfahren zur Beschichtung von Metallbändern |
KR101415412B1 (ko) * | 2007-10-16 | 2014-07-04 | 주식회사 케이씨씨 | 근적외선 경화 가능한 분체도료 조성물 |
CN106700697A (zh) * | 2008-11-07 | 2017-05-24 | 帝斯曼知识产权资产管理有限公司 | 可热固化的粉末涂料组合物 |
EP2424919B1 (en) * | 2009-04-29 | 2012-09-19 | DSM IP Assets B.V. | Powder coating composition comprising a polyester and a crosslinker with oxirane groups providing improved corrosion resistance to a substrate coated therewith |
WO2011096841A1 (ru) * | 2010-02-08 | 2011-08-11 | Trofimov Aleksej Vital Evich | Облицовочный элемент |
ES2595082T3 (es) * | 2011-03-25 | 2016-12-27 | Dsm Ip Assets B.V. | Composiciones de resina para composiciones de revestimiento en polvo termoendurecibles |
JP5883576B2 (ja) * | 2011-05-20 | 2016-03-15 | 株式会社Uacj | 樹脂被覆アルミニウム板の製造方法 |
KR20160099637A (ko) * | 2013-12-17 | 2016-08-22 | 닛산 가가쿠 고교 가부시키 가이샤 | 투명 도전막용 보호막 형성 조성물 |
RU2689745C2 (ru) * | 2014-09-08 | 2019-05-28 | Йотун А/С | Порошковое покрытие |
CN107011774B (zh) * | 2017-04-10 | 2020-10-02 | 立邦涂料(天津)有限公司 | 一种高硬度粉末涂料组合物及其制备方法和用途 |
CN112724725B (zh) * | 2020-12-16 | 2022-05-06 | 艾勒可新材料(佛山)有限公司 | 一种具有金属效果的粉末涂料及其制备方法 |
CN113736349B (zh) * | 2021-09-14 | 2022-05-17 | 安徽华辉塑业科技股份有限公司 | 一种耐腐蚀环氧树脂涂料及其制备方法 |
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JPS5916571A (ja) * | 1982-07-19 | 1984-01-27 | Nippon Paint Co Ltd | 粉体塗料の硬化方法 |
US5198962A (en) | 1989-08-03 | 1993-03-30 | Tyson Glenn M | Lighting system |
JPH0592172A (ja) * | 1991-05-20 | 1993-04-16 | Tawada:Kk | 線材の着色方法 |
EP0561102B1 (fr) * | 1992-03-16 | 1997-10-15 | U C B, S.A. | Polyesters cycloaliphatiques contenant des groupes carboxyle terminaux pour la préparation de peintures en poudre |
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DE4330404A1 (de) * | 1993-09-08 | 1995-03-09 | Basf Lacke & Farben | Pulverlacke, Verfahren zu deren Herstellung sowie Verwendung der Pulverlacke zur Beschichtung von Metallblechen |
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JPH10212434A (ja) * | 1997-01-31 | 1998-08-11 | Kansai Paint Co Ltd | エポキシ硬化型ポリエステル樹脂粉体塗料 |
JPH11166154A (ja) * | 1997-12-02 | 1999-06-22 | Nippon Ester Co Ltd | 粉体塗料用ポリエステル樹脂組成物 |
KR20010040921A (ko) | 1998-02-17 | 2001-05-15 | 메리 이. 보울러 | 분말 코팅의 생산 방법 |
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Publication number | Publication date |
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AU6826200A (en) | 2001-02-19 |
DE50007928D1 (de) | 2004-10-28 |
AU779890B2 (en) | 2005-02-17 |
CZ2002357A3 (cs) | 2002-08-14 |
ATE277137T1 (de) | 2004-10-15 |
KR20020031162A (ko) | 2002-04-26 |
PL353200A1 (en) | 2003-11-03 |
EP1208176A1 (de) | 2002-05-29 |
JP2003506517A (ja) | 2003-02-18 |
PT1208176E (pt) | 2004-11-30 |
ES2223567T3 (es) | 2005-03-01 |
HUP0201979A2 (en) | 2002-10-28 |
MY122733A (en) | 2006-05-31 |
WO2001009258A1 (de) | 2001-02-08 |
DE19935539A1 (de) | 2001-02-08 |
CA2379807C (en) | 2007-09-11 |
EP1208176B1 (de) | 2004-09-22 |
NO20020401D0 (no) | 2002-01-25 |
NO20020401L (no) | 2002-01-25 |
CO5160381A1 (es) | 2002-05-30 |
MXPA02001079A (es) | 2002-08-20 |
RU2219207C2 (ru) | 2003-12-20 |
CA2379807A1 (en) | 2001-02-08 |
US6537620B1 (en) | 2003-03-25 |
HUP0201979A3 (en) | 2003-08-28 |
CN1382194A (zh) | 2002-11-27 |
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