CN106243988A - 高固含量水性紫外光固化透明隔热涂料及其制备方法 - Google Patents
高固含量水性紫外光固化透明隔热涂料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种高固含量水性紫外光固化透明隔热涂料及其制备方法,其特征在于其原料组分及各组分的质量份分别为:高固含量水性聚氨酯分散体100质量份、水溶性光引发剂0.2‑0.5质量份、纳米功能元1‑5质量份、流平剂0.05‑0.2质量份、消泡剂0.1‑0.2质量份;将使各种组分混合均匀,即制得高固含量水性紫外光固化透明隔热涂料,其主要性能指标为:质量固含量为48‑52%,粘度为20‑100mPa.s。该涂料具有无毒、不燃、使用安全、耐黄变、无毒、不燃、隔热、透光性能好等优点,可用于建筑物幕墙玻璃和汽车窗玻璃等场合。
Description
技术领域
本发明涉及一种隔热涂料及其制备方法,尤其涉及一种高固含量水性紫外光固化透明隔热涂料及其制备方法。
背景技术
纳米透明隔热涂料是一种近十几年发展起来的功能性涂料,因具有高的可见光透过率和良好的节能隔热效果,可应用于建筑物幕墙玻璃和汽车窗玻璃等场合,受到关注越来越多。锑掺杂二氧化锡,也叫氧化锡锑(ATO),是一种新型多功能纳米材料,由于独特的气敏性和光电性能,在催化剂、气敏组件、防辐射抗静电涂层和红外吸收阻隔材料等领域得到广泛应用。
水性UV涂料继承和发展了传统UV涂料和水性涂料的特点,具有安全环保、节能高效、黏度可调、可薄涂层涂布,固化膜收缩率低和施工方便等优点,已成为涂料发展的一个主要方向。但相对于油性涂料,水性UV涂料存在力学性能、耐水性、耐候性差等缺点,而通过添加无机纳米材料形成有机/无机杂化体系,可提高涂膜的机械性能和耐候性等。把纳米ATO与水性UV固化涂料有效复合,形成一种可UV固化的水性纳米透明隔热涂料,不仅可提高水性UV涂料的基本性能(如附着力、硬度和耐蚀性),而且具有良好的隔热功能。此功能涂料结合了紫外光固化技术、水性涂料和纳米透明隔热涂料三者的优势,并且固化速率快,可自动化流水线涂装,生产效率高,因此具有广阔的应用前景。
发明内容
本发明所要解决的技术问题是为了油性涂料毒性较大、易燃、使用安全性差、污染环境等问题及水性UV涂料固含量低、干燥速度慢、粘度高、力学性能差、耐候性差、耐水性差、流平性差、耐黄变性差等问题,而提出一种高固含量水性紫外光固化透明隔热涂料,本发明的另一目的还提供了上述高固含量水性紫外光固化透明隔热涂料的制备方法。
本发明的具体技术方案为:一种高固含量水性紫外光固化透明隔热涂料,其特征在于在于其原料组分及各组分的质量份分别为:高固含量水性聚氨酯分散体100质量份、水溶性光引发剂0.2-0.5质量份、纳米功能元1-5质量份、流平剂0.05-0.2质量份、消泡剂0.1-0.2质量份;高固含量水性聚氨酯分散体主要性能指标为:质量固含量为48-52%,粘度为20-100mPa.s。
优选上述的水溶性光引发剂为2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮(光引发剂2959);所述的纳米功能元为溶胶-凝胶法改性纳米氧化锡锑(ATO)水性浆料,ATO质量含量为15%;所述的流平剂为聚有机硅氧烷、聚醚改性的聚有机硅氧烷或含氟表面活性剂;所述的消泡剂为水性有机硅消泡剂。
本发明还提供了上述高固含量水性紫外光固化透明隔热涂料的制备方法,其具体步骤如下:
(1)、高固含量水性聚氨酯分散体的制备;
在容器中首先加入聚酯多元醇,100-110℃下抽真空脱水1-2h,降至室温加入脂肪族或脂环族二异氰酸酯,在70-80℃下反应1-2h,然后加入含有亲水基团的化合物、低分子多元醇扩链剂,以上原料按官能团物质的量之比-NCO/-OH=1.6-2.0,且在占预聚物质量0.05-0.3%催化剂存在下进行反应,反应温度70-80℃,反应时间2-4h,加入过量-NCO物质的量的30-50%含羟基多功能团丙烯酸酯单体,继续反应1-2h,制得羧基质量含量为0.7-2.0%的聚氨酯预聚物;
将上述制得的聚氨酯预聚物降至室温,加入三乙胺将其中的羧酸根中和成盐,中和度80-110%;
预聚物出料至分散器中,在搅拌下加入去离子水进行分散,加入过量-NCO物质的量的50-70%的低分子脂肪胺类扩链剂反应10-30分钟,即制得高固含量水性聚氨酯分散体;
(2)、将上述制得的高固含量水性聚氨酯分散体100质量份,加入0.2-0.5质量份水溶性光引发剂、1-5质量份纳米功能元、0.05-0.2质量份流平剂和0.1-0.2质量份消泡剂,搅拌,使各种助剂混合均匀,即制得高固含量水性紫外光固化透明隔热涂料。
优选上述的脂肪族或脂环族二异氰酸酯为六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯、苯二亚甲基二异氰酸酯或4,4'-二环己基甲烷二异氰酸酯中一种或几种的混合。
优选上述的含有亲水基团的化合物为二羟甲基丙酸或二羟甲基丁酸。
优选上述的低分子多元醇扩链剂为乙二醇、二甘醇或1,4-丁二醇。
优选上述的低分子脂肪胺类扩链剂为乙二胺、二亚乙基三胺、三亚乙基四胺或四亚乙基五胺。
优选上述的催化剂为二月桂酸二丁基锡或辛酸亚锡。
优选上述的含羟基多功能团丙烯酸酯单体为季戊四醇三丙烯酸酯、季戊四醇三甲基丙烯酸酯、二季戊四醇五丙烯酸酯或二季戊四醇五甲基丙烯酸酯。
上述所制备的高固含量水性聚氨酯分散体其主要性能指标为:质量固含量为48-52%,粘度为20-100mPa.s(按国标测)。本发明还需加入水溶性光引发剂,使得透明隔热涂料在水分挥发后在紫外光作用下实现固化;本发明加入流平剂主要作用是降低高固含量水性紫外光固化透明隔热涂料的表面张力,使其在基材上有好的流平性。
有益效果:
1、与目前市场上使用的溶剂型隔热涂料相比,本发明的高固含量水性紫外光固化透明隔热涂料具有耐黄变、无毒、不燃、使用安全、不污染环境等优点。
2、与目前市场上使用的水性隔热涂料相比,本发明的高固含量水性紫外光固化透明隔热涂料具有高固含量、低粘度、好的耐水性、流平性、耐黄变性等优点。
3、本发明综合考虑了高固含量水性紫外光固化透明隔热涂料用于玻璃基材的要求,通过扩链、溶胶-凝胶法改性纳米氧化锡锑ATO和加入流平剂、水性消泡剂,改善了ATO的分散性与稳定性;多功能团丙烯酸酯单体的引入提高了固化后涂料涂膜的硬度、附着力、耐水、耐候性,使得高固含量水性紫外光固化透明隔热涂料能满足不同条件下的使用要求。
具体实施方式
下面就本发明举例说明,但不是对本发明的限制。
实施例1
在装有搅拌器、温度计、回流冷凝器的反应器中,加入聚酯多元醇(江苏金坛力合胶粘剂厂,108-Ⅰ)40g,100℃下抽真空脱水1h,降温至室温加入异氟尔酮二异氰酸酯10g,六亚甲基二异氰酸酯6.4g,升温至70℃,反应1h,加入二羟甲基丁酸1.6g,乙二醇1.3g,二月桂酸二丁基锡0.03g,在搅拌下继续反应4h,加入18.6g季戊四醇三丙烯酸酯,继续反应1h,得到预聚体,然后降温至室温,加入0.75g三乙胺使预聚体中和成盐;出料至分散器中,在高速剪切下加入去离子水86g,加入0.74g乙二胺扩链反应30分钟,出料,得到高固含量水性聚氨酯分散体,主要性能指标为:固含量为48%,粘度为21mPa.s。
在装有超声分散装置的分散器中,加入100g由上述所制备的高固含量水性聚氨酯分散体、0.2g光引发剂2959、1g ATO浆料、0.05g含氟表面活性剂(广州市氟缘硅科技公司,FY-1535)、0.1g水性有机硅消泡剂(广州宣宁化工科技有限公司,CA-2011),超声分散均匀后得到高固含量水性紫外光固化透明隔热涂料。
实施例2
在装有搅拌器、温度计、回流冷凝器的反应器中,加入聚酯多元醇(山东华诚高科胶粘剂有限公司,AD-60)40g,105℃下抽真空脱水1.5h,降温至室温加入苯二亚甲基二异氰酸酯14.2g,升温至75℃,反应1.5h,加入二羟甲基丙酸2.3g,二甘醇0.5g,辛酸亚锡0.1g,在搅拌下继续反应3h,加入9.2季戊四醇三甲基丙烯酸酯,继续反应2h,得到预聚体,然后降温至室温,加入1.7g三乙胺使预聚体中和成盐;出料至分散器中,在高速剪切下加入去离子水70g,加入1.7g二亚乙基三胺扩链反应20分钟,得到高固含量水性聚氨酯分散体,主要性能指标为:固含量为50%,粘度为43mPa.s。
在装有超声分散装置的分散器中,加入100g由上述所制备的高固含量水性聚氨酯分散体、0.5g光引发剂2959、3g ATO浆料、0.12g聚有机硅氧烷表面活性剂(德国毕克化学公司,BYK-333)、0.13g水性有机硅消泡剂(广州宣宁化工科技有限公司,CA-2031),超声分散均匀后得到高固含量水性紫外光固化透明隔热涂料。
实施例3
在装有搅拌器、温度计、回流冷凝器的反应器中,加入聚酯多元醇(浙江华峰新材料股份有限公司,PA-1225T)40g,110℃下抽真空脱水2h,降温至室温加入4,4'-二环己基甲烷二异氰酸酯27.4g,升温至80℃,反应1h,加入二羟甲基丙酸3g,1,4-丁二醇0.9g,二月桂酸二丁基锡0.19g,在搅拌下继续反应2h,加入15.6g季戊四醇三丙烯酸酯,继续反应2h,得到预聚体,然后降温至室温,加入2.4g三乙胺使预聚体中和成盐;出料至分散器中,在高速剪切下加入去离子水87g,加入4.9g四亚乙基五胺扩链反应10分钟,得到高固含量水性聚氨酯分散体,主要性能指标为:固含量为52%,粘度为98mPa.s。
在装有超声分散装置的分散器中,加入100g由上述所制备的高固含量水性聚氨酯分散体、0.5g光引发剂2959、5g ATO浆料、0.2g聚醚改性的聚有机硅氧烷表面活性剂(德国毕克化学公司,BYK-9565)、0.2g水性有机硅消泡剂(广州宣宁化工科技有限公司,CA-2011),超声分散均匀后得到高固含量水性紫外光固化透明隔热涂料。
对比例1
在装有搅拌器、温度计、回流冷凝器的反应器中,加入聚酯多元醇(江苏金坛力合胶粘剂厂,108-Ⅰ)40g,100℃下抽真空脱水1h,降温至室温加入异氟尔酮二异氰酸酯10g,六亚甲基二异氰酸酯6.4g,升温至70℃,反应1h,加入二羟甲基丁酸1.6g,乙二醇1.3g,二月桂酸二丁基锡0.03g,在搅拌下继续反应4h,加入15g丙酮稀释,得到预聚体,然后降温至室温,加入0.75g三乙胺使预聚体中和成盐;出料至分散器中,在高速剪切下加入去离子水101g,加入1.85g乙二胺扩链反应30分钟,出料,得到高固含量水性聚氨酯分散体,主要性能指标为:固含量为38%,粘度为128mPa.s。
在装有超声分散装置的分散器中,加入100g由上述所制备的高固含量水性聚氨酯分散体、1g ATO浆料、0.05g含氟表面活性剂(广州市氟缘硅科技公司,FY-1535)、0.1g水性有机硅消泡剂(广州宣宁化工科技有限公司,CA-2011),超声分散均匀后得到透明隔热涂料。
性能测试:将涂料在50℃烘箱中烘干,实施例1-3涂料在紫外光下50s完成固化,进行性能测试,得到结果如下:
注:可见光波长为400nm-800nm,紫外线波长为200nm-400nm,红外线波长为800nm-2000nm。
涂料经过光固化后,实施例1-3隔热性能、耐老化性能及硬度相比对比例1提升效果明显,是因为含羟基多功能团丙烯酸酯交联结构加入使涂料的机械强度得到了加强,另外体系耐化学腐蚀能力、耐老化性能得到了改善;加入纳米功能元使紫外线透过率、红外线透过率得到了明显改善,且随着纳米功能元量的增加,隔热效果更好,但对于可见光透过率有一定程度的降低;本发明的可见光透过率大于80%,能满足建筑物幕墙玻璃和汽车窗玻璃等场合的透光需要。
本发明所生产的高固含量水性紫外光固化透明隔热涂料性能优异,体系的相容性良好,在紫外光照射下固化速度快,原料成本低廉,生产效率高,易于工业化,应用十分广泛,整个工艺过程无有毒溶剂释放,是一种无毒无污染的环境友好型涂料。
Claims (9)
1.一种高固含量水性紫外光固化透明隔热涂料,其特征在于在于其原料组分及各组分的质量份分别为:高固含量水性聚氨酯分散体100质量份、水溶性光引发剂0.2-0.5质量份、纳米功能元1-5质量份、流平剂0.05-0.2质量份、消泡剂0.1-0.2质量份;高固含量水性聚氨酯分散体主要性能指标为:质量固含量为48-52%,粘度为20-100mPa.s。
2.根据权利要求1所述的高固含量水性紫外光固化透明隔热涂料,其特征在于所述的水溶性光引发剂为2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮;所述的纳米功能元为溶胶-凝胶法改性纳米氧化锡锑水性浆料,ATO质量含量为15%;所述的流平剂为聚有机硅氧烷、聚醚改性的聚有机硅氧烷或含氟表面活性剂;所述的消泡剂为水性有机硅消泡剂。
3.一种制备如权利要求1所述高固含量水性紫外光固化透明隔热涂料的方法,其具体步骤如下:
(1)、高固含量水性聚氨酯分散体的制备;
在容器中首先加入聚酯多元醇,100-110℃下抽真空脱水1-2h,降温加入脂肪族或脂环族二异氰酸酯,在70-80℃下反应1-2h,然后加入含有亲水基团的化合物、低分子多元醇扩链剂,以上原料按官能团物质的量之比-NCO/-OH=1.6-2.0,且在占预聚物质量0.05-0.3%催化剂存在下进行反应,反应温度70-80℃,反应时间2-4h,加入过量-NCO物质的量的30-50%含羟基多功能团丙烯酸酯单体,继续反应1-2h,制得羧基质量含量为0.7-2.0%的聚氨酯预聚物;
将上述制得的聚氨酯预聚物降温,加入三乙胺将其中的羧酸根中和成盐,中和度80-110%;
预聚物出料至分散器中,在搅拌下加入去离子水进行分散,加入过量-NCO物质的量的50-70%的低分子脂肪胺类扩链剂反应10-30分钟,即制得高固含量水性聚氨酯分散体;
(2)、将上述制得的高固含量水性聚氨酯分散体100质量份,加入0.2-0.5质量份水溶性光引发剂、1-5质量份纳米功能元、0.05-0.2质量份流平剂和0.1-0.2质量份消泡剂,搅拌,使各种助剂混合均匀,即制得高固含量水性紫外光固化透明隔热涂料。
4.根据权利要求3所述的方法,其特征在于所述的脂肪族或脂环族二异氰酸酯为六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯、苯二亚甲基二异氰酸酯或4,4'-二环己基甲烷二异氰酸酯中一种或几种的混合。
5.根据权利要求3所述的方法,其特征在于所述的含有亲水基团的化合物为二羟甲基丙酸或二羟甲基丁酸。
6.根据权利要求3所述的方法,其特征在于所述的低分子多元醇扩链剂为乙二醇、二甘醇或1,4-丁二醇。
7.根据权利要求3所述的方法,其特征在于所述的低分子脂肪胺类扩链剂为乙二胺、二亚乙基三胺、三亚乙基四胺或四亚乙基五胺。
8.根据权利要求3所述的方法,其特征在于所述的催化剂为二月桂酸二丁基锡或辛酸亚锡。
9.根据权利要求3所述的方法,其特征在于所述的含羟基多功能团丙烯酸酯单体为季戊四醇三丙烯酸酯、季戊四醇三甲基丙烯酸酯、二季戊四醇五丙烯酸酯或二季戊四醇五甲基丙烯酸酯。
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