CN116970335A - 一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料及其制备方法 - Google Patents
一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料及其制备方法。本发明的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料是由含氟硅水性聚氨酯分散体、水性紫外光引发剂、微纳米粒子/含氟硅烷偶联剂改性浆料、流平剂和消泡剂复配而成。该涂料具有无毒、使用安全,经涂装固化后的涂层具有超疏水、耐老化及耐腐蚀等优点,可用于风电叶片防冰、户外电线电缆防冰等场合。
Description
技术领域
本发明涉及水性聚氨酯涂料领域,特别涉及一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料及其制备方法。
背景技术
风能是一种清洁可再生能源,风力发电不仅是我国常规电力的一种补充,更是未来电力发展的一个趋势。由于较低温度下空气密度增加,可用风力比其他地方高,因此,风电场往往修建在寒冷的高山上,随着风力发电行业的大规模发展,风力发电风机叶片面临的覆冰问题也愈加突出,已成为制约结冰地区风电市场开发建设的重要因素,防冰、除冰问题也成为了风电领域亟待解决的难题。寒冷地区风机叶片的防冰、除冰技术对于风场及大型风力机的安全、经济、高效运行具有重要的意义。目前解决覆冰问题主要有主动式和被动式两种解决方案。主动式的解决方案主要是利用电、光、机械或化学方法解决覆冰问题。被动式的解决方案是在叶片表面覆盖超疏水涂料等以降低冰与叶片表面的黏附力,从而达到防冰或延迟结冰的效果。
现有技术中聚氨酯是一种常用的疏水涂层材料,油性聚氨酯材料因其成分含有有机溶剂而存在毒性较大、易燃、使用安全性差、污染环境等问题,使得水性聚氨酯涂料更受市场和消费者的青睐。从技术、适用和环境角度而言水性聚氨酯以其无毒、不燃、绿色环保、耐化学品、耐划伤、防湿透气以及与多种基材的粘接性好等优点广泛用于各种涂料。随着社会的发展、科技的进步,风电叶片防冰涂料不仅需要具有较好的防冰效果,还需要具有耐老化、耐腐蚀和长效除冰等性能。因此开发一种具有较好的防冰效果,同时具有耐老化、耐腐蚀和长效除冰等功能于一体的风电叶片防冰涂料成为发展趋势。
发明内容
本发明的目的是针对现有技术中存在的上述问题,提出一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,本发明的另一目的还提供了上述含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法。
为了实现上述目标,本发明采用如下的技术方案:
一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,所述含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料由100质量份含氟硅水性聚氨酯分散体、0.5-1.5质量份水性紫外光引发剂、15-35质量份微纳米粒子/含氟硅烷偶联剂改性浆料、1.0-2.0质量份流平剂和0.5-1.0质量份消泡剂复配而成。
优选地,所述水性紫外光引发剂为2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮、蒽醌-2-磺酸钠、2-羧基甲氧基硫杂蒽酮钠盐、2-羟基-3-(2-硫杂蒽酮氧基)丙基三甲基氯化铵、4-[N-(2-甲基丙烯酰氧基乙基)二甲基溴化铵甲基]二苯甲酮、3-烯丙基-1-[2-羟基-3-(2-硫杂蒽酮基)丙氧基]咪唑氯中的一种。
优选地,所述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。
优选地,所述消泡剂为水性有机硅消泡剂。
一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,包括以下制备步骤:
(1)含氟硅水性聚氨酯分散体的制备:
在容器中首先加入100质量份含氟硅聚醚多元醇,105-115℃下抽真空脱水1-2h,降至室温加入32-69质量份脂肪族或脂环族二异氰酸酯中的一种或几种,在75-95℃下反应1-3h,然后加入4-8质量份含有羧酸根基团的全氟端羟基二元醇化合物、3-5质量份低分子全氟二元醇扩链剂,前述所有原料混合后-NCO和-OH官能团物质的量之比为1.1-1.3,反应温度75-85℃,反应时间2-4h,加入过量-NCO物质的量的100%的含氟羟基丙烯酸酯单体,继续反应1-3h,制得羧基质量含量为1.0-2.5%的聚氨酯预聚物;
将所述的聚氨酯预聚物降至室温,加入3-10质量份中和剂将其中的羧酸根中和成盐,中和度80-110%;
将中和过的聚氨酯预聚物出料至分散器中,在搅拌下加入去离子水进行分散,即制得固含量为40-50%的含氟硅水性聚氨酯分散体;
(2)微纳米粒子/含氟硅烷偶联剂改性浆料的制备:
在装有搅拌装置、温度计和冷凝管的四口烧瓶中加入5质量份微纳米粒子,50质量份甲醇和0.5-1.5质量份含氟硅烷偶联剂的混合溶液,加热到50-70℃,回流12-24h,冷却到室温后,转移至旋转蒸发器,通过加热蒸馏除去甲醇,然后加入15-31质量份乙醇,超声分散1-2h即制得固含量为15-30%的微纳米粒子/含氟硅烷偶联剂改性浆料;
(3)含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备:
将所述含氟硅水性聚氨酯分散体100质量份,加入0.5-1.5质量份水性紫外光引发剂、15-35质量份微纳米粒子/含氟硅烷偶联剂改性浆料、1.0-2.0质量份流平剂和0.5-1.0质量份消泡剂,搅拌至混合均匀,即制得含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料。
优选地,所述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、4,4'-二环己基甲烷二异氰酸酯。
优选地,所述含有羧酸根基团的全氟端羟基二元醇化合物结构式如下:
其中n选自1-3中的一种。
优选地,所述低分子全氟二元醇扩链剂结构式如下:
其中n选自1-3中的一种。
优选地,所述含氟羟基丙烯酸酯单体结构式如下:
其中n选自1-3中的一种。
优选地,所述中和剂为三乙胺、三乙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、N-丙基二乙醇胺、N-丁基二乙醇胺中的一种。
优选地,所述微纳米粒子为微纳米二氧化钛、微纳米二氧化硅、微纳米高岭土中的一种。
优选地,所述含氟硅烷偶联剂为十七氟癸基三甲氧基硅烷、十三氟辛基三乙氧基硅烷中的一种。
本发明的有益之处在于:
(1)与目前市场上使用的溶剂型风电叶片表面防护涂料相比,本发明的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料具有无毒、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风电叶片表面防护涂料相比,本发明的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料具有耐老化性好、超疏水、耐腐蚀等优点。
(3)本发明的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料性能优异,体系的相容性良好,在紫外光照射下固化速度快,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。
具体实施方式
以下结合具体实施例对本发明作进一步详细说明。下述实施例中的实验方法,如无特殊说明,均为常规方法。下述实施例中所用的试验材料,如无特殊说明,均为从商业渠道购买得到的。
实施例1
(1)含氟硅水性聚氨酯分散体的制备
在容器中首先加入100质量份含氟硅聚醚多元醇,105℃下抽真空脱水2h,降至室温加入25质量份异氟尔酮二异氰酸酯、16质量份六亚甲基二异氰酸酯,在75℃下反应3h,然后加入含有羧酸根基团的4质量份全氟端羟基二元醇化合物(式4)、3质量份低分子全氟二元醇扩链剂(式5),在75℃下继续反应时间4h,加入48质量份含氟羟基丙烯酸酯单体(式6),继续反应3h,制得聚氨酯预聚物;
将上述制得的聚氨酯预聚物降至室温,加入3质量份三乙醇胺将其中的羧酸根中和成盐;
预聚物出料至分散器中,在搅拌下加入299质量份去离子水进行分散,即制得含氟硅水性聚氨酯分散体。
(2)微纳米粒子/含氟硅烷偶联剂改性浆料的制备
在装有搅拌装置、温度计和冷凝管的四口烧瓶中加入5质量份微纳米二氧化钛粒子,50质量份甲醇和0.5质量份十七氟癸基三甲氧基硅烷的混合溶液,加热到50℃,回流24h。冷却到室温后,产物转移至旋转蒸发器,通过加热蒸馏除去甲醇。加入31质量份乙醇,超声分散1h即制得固含量为15%的微纳米粒子/含氟硅烷偶联剂改性浆料。
(3)含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备
将上述制得的含氟硅水性聚氨酯分散体100质量份,加入0.5质量份2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮、35质量份上述制得的微纳米粒子/含氟硅烷偶联剂改性浆料、1.0质量份聚有机硅氧烷流平剂和0.5质量份水性有机硅消泡剂,搅拌,使各种助剂混合均匀,即制得含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料。
实施例2
(1)含氟硅水性聚氨酯分散体的制备
在容器中首先加入100质量份含氟硅聚醚多元醇,110℃下抽真空脱水1.5h,降至室温加入32质量份苯二亚甲基二异氰酸酯,在85℃下反应2h,然后加入6质量份含有羧酸根基团的全氟端羟基二元醇化合物(式7)、5质量份低分子全氟二元醇扩链剂(式8),85℃下继续反应时间3h,加入26质量份含氟羟基丙烯酸酯单体(式9),继续反应2h,制得聚氨酯预聚物;
将上述制得的聚氨酯预聚物降至室温,加入5质量份N-甲基二乙醇胺将其中的羧酸根中和成盐;
预聚物出料至分散器中,在搅拌下加入212质量份去离子水进行分散,即制得含氟硅水性聚氨酯分散体。
(2)微纳米粒子/含氟硅烷偶联剂改性浆料的制备
在装有搅拌装置、温度计和冷凝管的四口烧瓶中加入5质量份微纳米二氧化硅粒子,50质量份甲醇和1.0质量份十三氟辛基三乙氧基硅烷的混合溶液,加热到60℃,回流18h。冷却到室温后,产物转移至旋转蒸发器,通过加热蒸馏除去甲醇。加入24质量份乙醇,超声分散1.5h即制得固含量为20%的微纳米粒子/含氟硅烷偶联剂改性浆料。
(3)含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备
将上述制得的含氟硅水性聚氨酯分散体100质量份,加入1.0质量份2-羟基-3-(2-硫杂蒽酮氧基)丙基三甲基氯化铵、25质量份上述制得的微纳米粒子/含氟硅烷偶联剂改性浆料、1.5质量份聚醚改性的聚有机硅氧烷流平剂和0.7质量份水性有机消泡剂,搅拌,使各种助剂混合均匀,即制得含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料。
实施例3
(1)含氟硅水性聚氨酯分散体的制备
在容器中首先加入100质量份含氟硅聚醚多元醇,115℃下抽真空脱水1h,降至室温加入69质量份4,4'-二环己基甲烷二异氰酸酯,在95℃下反应1h,然后加入8质量份含有羧酸根基团的全氟端羟基二元醇化合物(式10)、4质量份低分子全氟二元醇扩链剂(式11),85℃下继续反应时间2h,加入43质量份含氟羟基丙烯酸酯单体(式12),继续反应1h,制得聚氨酯预聚物;
将上述制得的聚氨酯预聚物降至室温,加入10质量份N-丙基二乙醇胺将其中的羧酸根中和成盐;
预聚物出料至分散器中,在搅拌下加入234质量份去离子水进行分散,即制得含氟硅水性聚氨酯分散体。
(2)微纳米粒子/含氟硅烷偶联剂改性浆料的制备
在装有搅拌装置、温度计和冷凝管的四口烧瓶中加入5质量份微纳米高岭土粒子,50质量份甲醇和1.5质量份十七氟癸基三甲氧基硅烷的混合溶液,加热到70℃,回流12h。冷却到室温后,产物转移至旋转蒸发器,通过加热蒸馏除去甲醇。加入15质量份乙醇,超声分散1h即制得固含量为30%的微纳米粒子/含氟硅烷偶联剂改性浆料。
(3)含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备
将上述制得的含氟硅水性聚氨酯分散体100质量份,加入1.5质量份4-[N-(2-甲基丙烯酰氧基乙基)二甲基溴化铵甲基]二苯甲酮、15质量份上述制得的微纳米粒子/含氟硅烷偶联剂改性浆料、2.0质量份含氟表面活性剂流平剂和1.0质量份水性有机硅消泡剂,搅拌,使各种助剂混合均匀,即制得含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料。
对比例1
(1)水性聚氨酯分散体的制备
在容器中首先加入100质量份聚醚多元醇,105℃下抽真空脱水2h,降至室温加入25质量份异氟尔酮二异氰酸酯、16质量份六亚甲基二异氰酸酯,在75℃下反应3h,然后加入4质量份二羟甲基丙酸、3质量份丁二醇,在75℃下继续反应时间4h,加入48质量份丙烯酸羟丙酯,继续反应3h,制得聚氨酯预聚物;
将上述制得的聚氨酯预聚物降至室温,加入3质量份三乙醇胺将其中的羧酸根中和成盐;
预聚物出料至分散器中,在搅拌下加入299质量份去离子水进行分散,即制得水性聚氨酯分散体。
(2)水性聚氨酯基风电叶片表面防护涂料的制备
将上述制得的水性聚氨酯分散体100质量份,加入0.5质量份2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮、35质量份固含量为15%的微纳米二氧化钛粒子乙醇分散浆料、1.0质量份聚有机硅氧烷流平剂和0.5质量份水性有机硅消泡剂,搅拌,使各种助剂混合均匀,即制得水性聚氨酯基风电叶片表面防护涂料。
性能测试:将实施例1-3和对比例1制得的涂料涂膜后在50℃烘箱中烘干,然后在紫外光下30s完成固化,进行性能测试,得到结果如下:
由上表可知,涂料经过烘干、光固化后,实施例1-3耐老化及耐腐蚀性能、防冰性能及接触角相比对比例1提升效果明显,是因为通过紫外光固化的固化作用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;在含氟硅水性聚氨酯与含氟硅烷偶联剂改性的微纳米粒子的共同作用下使涂层呈现类似荷叶的乳突结构,使得光固化后的涂膜接触角得到提高,达到150°以上,使得风电叶片与冰附着力大幅度减小,满足需要风电叶片防冰的需要。
本发明综合考虑了含氟硅水性聚氨酯基超疏水风电叶片防冰涂料用于风电叶片表面的要求,通过含氟硅烷偶联剂改性微纳米粒子,改善了微纳米粒子的分散性与稳定性;加入流平剂、消泡剂,改善了含氟硅水性聚氨酯基超疏水风电叶片防冰涂料的施工性能;含氟硅水性聚氨酯分散体的制备、微纳米粒子/含氟硅烷偶联剂改性浆料的引入降低了固化后涂料涂膜的表面能;在氟硅烷偶联剂改性的微纳米粒子的作用下使含氟硅水性聚氨酯基超疏水风电叶片防冰涂料涂层呈现类似荷叶的乳突结构,使涂层达到超疏水效果;通过使用紫外光固化,提高涂层的交联度,从而提高含氟硅水性聚氨酯基超疏水风电叶片防冰涂料涂层的耐老化及耐腐蚀性能、防冰性能及接触角等性能。
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解,上述实施例不以任何形式限制本发明,凡采用等同替换或等效变换的方式所获得的技术方案,均落在本发明的保护范围内。
Claims (10)
1.一种含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,其特征在于,所述含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料由100质量份含氟硅水性聚氨酯分散体、0.5-1.5质量份水性紫外光引发剂、15-35质量份微纳米粒子/含氟硅烷偶联剂改性浆料、1.0-2.0质量份流平剂和0.5-1.0质量份消泡剂复配而成。
2.根据权利要求1所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,其特征在于,所述水性紫外光引发剂为2-羟基-4'-(2-羟乙氧基)-2-甲基苯丙酮、蒽醌-2-磺酸钠、2-羧基甲氧基硫杂蒽酮钠盐、2-羟基-3-(2-硫杂蒽酮氧基)丙基三甲基氯化铵、4-[N-(2-甲基丙烯酰氧基乙基)二甲基溴化铵甲基]二苯甲酮、3-烯丙基-1-[2-羟基-3-(2-硫杂蒽酮基)丙氧基]咪唑氯中的一种。
3.根据权利要求1所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,其特征在于,所述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。
4.根据权利要求1所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料,其特征在于,所述消泡剂为水性有机硅消泡剂。
5.根据权利要求1所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,包括以下制备步骤:
(1)含氟硅水性聚氨酯分散体的制备:
在容器中首先加入100质量份含氟硅聚醚多元醇,105-115℃下抽真空脱水1-2h,降至室温加入32-69质量份脂肪族或脂环族二异氰酸酯中的一种或几种,在75-95℃下反应1-3h,然后加入4-8质量份含有羧酸根基团的全氟端羟基二元醇化合物、3-5质量份低分子全氟二元醇扩链剂,前述所有原料混合后-NCO和-OH官能团物质的量之比为1.1-1.3,反应温度75-85℃,反应时间2-4h,加入过量-NCO物质的量的100%的含氟羟基丙烯酸酯单体,继续反应1-3h,制得羧基质量含量为1.0-2.5%的聚氨酯预聚物;
将所述的聚氨酯预聚物降至室温,加入3-10质量份中和剂将其中的羧酸根中和成盐,中和度80-110%;
将中和过的聚氨酯预聚物出料至分散器中,在搅拌下加入去离子水进行分散,即制得固含量为40-50%的含氟硅水性聚氨酯分散体;
(2)微纳米粒子/含氟硅烷偶联剂改性浆料的制备:
在装有搅拌装置、温度计和冷凝管的四口烧瓶中加入5质量份微纳米粒子,50质量份甲醇和0.5-1.5质量份含氟硅烷偶联剂的混合溶液,加热到50-70℃,回流12-24h,冷却到室温后,转移至旋转蒸发器,通过加热蒸馏除去甲醇,然后加入15-31质量份乙醇,超声分散1-2h即制得固含量为15-30%的微纳米粒子/含氟硅烷偶联剂改性浆料;
(3)含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备:
将所述含氟硅水性聚氨酯分散体100质量份,加入0.5-1.5质量份水性紫外光引发剂、15-35质量份微纳米粒子/含氟硅烷偶联剂改性浆料、1.0-2.0质量份流平剂和0.5-1.0质量份消泡剂,搅拌至混合均匀,即制得含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料。
6.根据权利要求5所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,所述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、4,4'-二环己基甲烷二异氰酸酯。
7.根据权利要求5所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,所述含有羧酸根基团的全氟端羟基二元醇化合物结构式如下:
其中n选自1-3中的一种。
8.根据权利要求5所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,所述低分子全氟二元醇扩链剂结构式如下:
其中n选自1-3中的一种。
9.根据权利要求5所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,所述含氟羟基丙烯酸酯单体结构式如下:
其中n选自1-3中的一种。
10.根据权利要求5所述的含氟硅水性聚氨酯基超疏水风电叶片表面防护涂料的制备方法,其特征在于,所述中和剂为三乙胺、三乙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、N-丙基二乙醇胺、N-丁基二乙醇胺中的一种;所述微纳米粒子为微纳米二氧化钛、微纳米二氧化硅、微纳米高岭土中的一种;所述含氟硅烷偶联剂为十七氟癸基三甲氧基硅烷、十三氟辛基三乙氧基硅烷中的一种。
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