CN111499908A - 一种防覆冰贴膜及其制备方法 - Google Patents
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Abstract
本发明提供一种防覆冰贴膜及其制备方法,由基体膜层和交联固化在基体膜层上的疏水层组成,所述疏水层为聚二甲基硅氧烷与支化聚氨酯的互穿交联弹性体,可以降低外力损伤影响;通过添加具有铁磁性的纳米微粒,使其在磁场中发生磁取向诱导分布,构筑嵌于疏水层上的疏水微纳结构。所述制备方法简单,可以方便地制备高疏水性表面,具有良好的防冰除冰效果,可对户外运行设备与仪表进行防冰冻保护以及在冰雪冻雨侵袭后表面快速除冰。
Description
技术领域
本发明涉及保护膜技术领域,具体涉及一种防覆冰贴膜及其制备方法。
背景技术
覆冰是常见的自然现象,尤其在低温高湿地区,空气中的水蒸气接触到温度低于冰点温度的材料表面时,就会发生相变形成冰霜,冻雨、霜雪等冰雪灾害也容易造成覆冰,覆冰给人们的生产和生活造成诸多的不便和损失,如冷冻设备覆冰会导致设备传热效率降低甚至失效,覆冰还会导致一些户外特殊设备、精密仪表等的失灵,严重的覆冰还会大量破坏生态环境、交通、电力设施等。
目前的防冰技术主要有两大类,第一类是主动方法,包括机械除冰和电热、光热除冰,但机械除冰的成本高、效率低,加热除冰能耗大,工艺及设备仍需完善;第二类是被动方法,使用疏水性材料等,但疏水材料的耐久性较差,在受外力作用下,疏水表面容易发生形变,导致疏水层脱落,疏水结构受到破坏,失去疏水性,从而失去抗结冰特性;
在结冰过程中,水滴结冰后体积会膨胀,会破坏超疏水表面的微纳米结构,而在除冰过程中,冰的黏附力会使超疏水表面结构在冰的脱落过程中受到破坏,导致超疏水表面无法承受反复的结冰/除冰过程;水滴在超疏水表面结冰后,冰会因为黏附力作用而固定在超疏水表面,无法自动从超疏水表面脱离。
发明内容
针对上述问题,本发明提供一种防覆冰贴膜的制备方法。
本发明的目的采用以下技术方案来实现:
一种防覆冰贴膜的制备方法,包括以下步骤:
(1)聚氨酯预聚体制备
9.2g异佛尔酮二异氰酸酯中加入平均分子量500-600的聚乙二醇6g,5%的二月丁基二月桂酸锡1ml,在保护气氛下,在80℃水浴搅拌回流1h;
(2)预聚体混合
在制得的聚氨酯预聚体中加入三羟甲基丙烷1.4g,聚乙二醇二甲基丙烯酸酯2.3g,粘度小于50mPas的低聚端羟基聚二甲基硅氧烷18-24g,正硅酸乙酯8-9g,具有铁磁性的纳米微粒0.4-2g,超声分散处理使其混合均匀;
(3)交联固化
将混合均匀后的预聚体涂布在基体膜层上,置于磁场中热交联固化成型,固化温度120℃,制得所述防覆冰贴膜;
优选的,所述基体膜层为PET或PVC薄膜;
优选的,所述具有铁磁性的纳米微粒粒径在0.1-1μm之间;
优选的,所述具有铁磁性的纳米微粒为铁磁金属纳米颗粒、铁磁性复合金属微粒、磁性金属氧化物微粒或其组合,所述铁磁金属纳米颗粒包括铁、钴、镍的微粒,所述铁磁性复合金属微粒包括铁与稀土金属复合的微粒;
优选的,所述具有铁磁性的纳米微粒由溶胶-凝胶法、共沉淀法、水热法、溶剂热、离子热法合成,或利用球磨、砂磨和胶体磨技术将磁性颗粒粉碎得到;
优选的,所述具有铁磁性的纳米微粒为具有棒状、长方体、棱柱或纳米花形貌的四氧化三铁微粒;
优选的,所述防覆冰贴膜上表面还涂覆有聚电解质薄层,涂附量0.5-5ml/m2;
优选的,所述聚电解质为聚二烯丙基二甲基胺盐酸盐、聚丙烯胺盐酸盐、聚二烯丙基二甲基氯化铵、质子化的聚乙撑亚胺、聚苯乙烯磺酸钠、聚乙烯酸酯或聚L赖氨酸;
优选的,所述聚电解质薄层的涂覆方法为:配制浓度0.01~0.2mol·L-1的聚电解质溶液,调节溶液pH至6-12;等离子体处理使防覆冰贴膜上表面呈负电荷状态,再涂布聚电解质,干燥即得。
本发明的有益效果为:
本发明提供的一种防覆冰贴膜,通过支化聚氨酯与聚二甲基硅氧烷的互穿交联,使疏水层具有良好的弹韧性和一定的自修复能力,降低外力损伤对防冰性能的影响;通过添加具有铁磁性的纳米微粒,使其在磁场中发生磁取向诱导分布,构筑嵌于疏水层上的微纳结构,方便地制备了高疏水性表面,由于水滴在超疏水表面不能完全铺展,接触面积小,接触角大,有利于增大水凝固的势垒,延缓了水滴的凝固,而且,超疏水表面粗糙的微纳结构所具有的的气垫,使得液滴在超疏水表面形成固-液-气三相共存界面,具有良好的绝热作用,结冰速度大大减低,具有良好的防覆冰效果。
具体实施方式
结合以下实施例对本发明作进一步描述。
本发明的实施例涉及一种防覆冰贴膜的制备方法,包括以下步骤:
(1)聚氨酯预聚体制备
9.2g异佛尔酮二异氰酸酯中加入平均分子量500-600的聚乙二醇6g,5%的二月丁基二月桂酸锡1ml,在保护气氛下,在80℃水浴搅拌回流1h;
(2)预聚体混合
在制得的聚氨酯预聚体中加入三羟甲基丙烷1.4g,聚乙二醇二甲基丙烯酸酯2.3g,粘度小于50mPas的低聚端羟基聚二甲基硅氧烷18-24g,正硅酸乙酯8-9g,具有铁磁性的纳米微粒0.4-2g,超声分散处理使其混合均匀;
(3)交联固化
将混合均匀后的预聚体涂布在基体膜层上,置于磁场中热交联固化成型,固化温度120℃,制得所述防覆冰贴膜;
疏水涂层在外力作用或低温环境下容易出现微裂缝,不仅加速涂层脱落,且在潮湿空气中易吸收水分,当发生冰冻时,微裂缝中的水分凝固,不仅疏水作用失效,还会将冰牢固地植入涂层内,使得并的粘附性增强,更加难以去除;本发明基于聚二甲基硅氧烷的疏水作用,在聚二甲基硅氧烷中引入支化聚氨酯,形成聚二甲基硅氧烷与支化聚氨酯的互穿交联弹性体,使得涂层具有良好的弹韧性,以减少外力损伤,同时,支化聚氨基酯与聚二甲基硅氧烷具有分子间和分子内的氢键(羧基、氨基和羟基)相互作用,由于体系内多重的氢键作用,形成能够实现软涂层表面应用过程中微裂缝的自修复性,提高防冰性能;
具有铁磁性的纳米微粒在磁场中发生磁取向诱导分布,使得微粒迁移至涂层表面,构筑取向排列的微阵列,固化后则嵌于涂层表面上,形成粗糙的表面微纳结构,提高涂层的疏水力;
优选的,所述基体膜层为PET或PVC薄膜;
聚对苯二甲酸乙二酯与聚氯乙烯具有良好的耐高低温性能和柔韧性,以其作为基体膜层,与疏水涂层结合度较好;
优选的,所述具有铁磁性的纳米微粒粒径在0.1-1μm之间;
合适的磁性纳米微粒粒径是形成阵列的表面疏水微纳结构的关键,粒径过小则无法形成粗糙表面,粒径过大则形成过高的粗糙度,无法起到疏水作用;
优选的,所述具有铁磁性的纳米微粒为铁磁金属纳米颗粒、铁磁性复合金属微粒、磁性金属氧化物微粒或其组合,所述铁磁金属纳米颗粒包括铁、钴、镍的微粒,所述铁磁性复合金属微粒包括铁与稀土金属复合的微粒;
优选的,所述具有铁磁性的纳米微粒由溶胶-凝胶法、共沉淀法、水热法、溶剂热、离子热法合成,或利用球磨、砂磨和胶体磨技术将磁性颗粒粉碎得到;
优选的,所述具有铁磁性的纳米微粒为具有棒状、长方体、棱柱或纳米花形貌的四氧化三铁微粒;
棒状长方体、棱柱或纳米花形貌的微粒在磁场中的诱导分布容易实现在涂层中的均匀分布,在涂层面上形成具有无数的针状突起的微纳粗糙结构,提高涂层的疏水力;四氧化三铁具有良好的光热转换性能,可以将光能转化为热能,使得膜层表面温度升高,使靠近膜表面的冰雪融化,在疏水结构作用下加速冰雪滑落,减少覆冰。
本申请的实施例还涉及一种由前述制备方法制备的防覆冰贴膜;
优选的,所述防覆冰贴膜上表面还涂覆有聚电解质薄层,涂附量0.5-5ml/m2;
所述聚电解质为聚二烯丙基二甲基胺盐酸盐、聚丙烯胺盐酸盐、聚二烯丙基二甲基氯化铵、质子化的聚乙撑亚胺、聚苯乙烯磺酸钠、聚乙烯酸酯或聚L赖氨酸;
所述聚电解质薄层的涂覆方法为:配制浓度0.01~0.2mol·L-1的聚电解质溶液,调节溶液pH至6-12;等离子体处理使防覆冰贴膜上表面呈负电荷状态,再涂布聚电解质,干燥即得;
如果环境湿度较高时导致水蒸汽直接在固体表面凝结,会导致撞击到固体表面的过冷水滴得以进入微纳凸起结构之间原本由空气占据的孔隙,此时虽然水滴在固体上的接触角仍然较高,但水滴流动时的摩擦力却大大增加,因此当固体倾斜时,液滴也难以迅速流下,这样不仅很难起到防冰效果,而且由于粗糙不平的表面增加了冰和固体之间的黏附力,表面上的冰反而更加难以清除。本发明利用等离子体处理,在微纳凸起结构间空气占据的孔隙填充部分的聚电解质,当环境湿度较高时,聚电解质吸收环境水分,在微纳凸起结构间形成的毛细管效应作用下,聚电解质将水分锁持在微纳结构孔隙,且凝固点显著降低,在低温下仍然保持液态,当固体表面结冰时,冰层和涂层间隔了一层水膜,由于水膜的润滑作用,冰和涂层之间的黏附作用相当微弱,从而使冰层可以很容易地清除。
实施例1
一种防覆冰贴膜,其制备方法包括以下步骤:
(1)聚氨酯预聚体制备
9.2g异佛尔酮二异氰酸酯中加入平均分子量500-600的聚乙二醇6g,5%的二月丁基二月桂酸锡1ml,在保护气氛下,在80℃水浴搅拌回流1h;
(2)预聚体混合
在制得的聚氨酯预聚体中加入三羟甲基丙烷1.4g,聚乙二醇二甲基丙烯酸酯2.3g,粘度小于50mPas的低聚端羟基聚二甲基硅氧烷18-24g,正硅酸乙酯8-9g,具有棒状、长方体、棱柱或纳米花形貌的四氧化三铁微粒0.4-2g,超声分散处理使其混合均匀;
所述四氧化三铁微粒的粒径在0.1-1μm之间,所述具有特殊形貌的四氧化三铁微粒可以由溶胶-凝胶法、共沉淀法、水热法制备;
(3)交联固化
将混合均匀后的预聚体涂布在PET或PVC薄膜上,置于磁场中热交联固化成型,固化温度120℃,制得所述防覆冰贴膜。
实施例2
一种防覆冰贴膜,其制备方法包括以下步骤:
(1)聚氨酯预聚体制备
9.2g异佛尔酮二异氰酸酯中加入平均分子量500-600的聚乙二醇6g,5%的二月丁基二月桂酸锡1ml,在保护气氛下,在80℃水浴搅拌回流1h;
(2)预聚体混合
在制得的聚氨酯预聚体中加入三羟甲基丙烷1.4g,聚乙二醇二甲基丙烯酸酯2.3g,粘度小于50mPas的低聚端羟基聚二甲基硅氧烷18-24g,正硅酸乙酯8-9g,具有棒状、长方体、棱柱或纳米花形貌的四氧化三铁微粒0.4-2g,超声分散处理使其混合均匀;
所述四氧化三铁微粒的粒径在0.1-1μm之间,所述具有特殊形貌的四氧化三铁微粒可以由溶胶-凝胶法、共沉淀法、水热法制备;
(3)交联固化
将混合均匀后的预聚体涂布在PET或PVC薄膜上,置于磁场中热交联固化成型,固化温度120℃,制得防覆冰贴膜;
(4)涂覆聚电解质薄层
配制浓度0.01~0.2mol·L-1的聚电解质溶液,调节溶液pH至6-12;等离子体处理使防覆冰贴膜上表面呈负电荷状态,再涂布聚电解质,涂附量0.5-5ml/m2,干燥即得;
所述聚电解质为聚二烯丙基二甲基胺盐酸盐、聚丙烯胺盐酸盐、聚二烯丙基二甲基氯化铵、质子化的聚乙撑亚胺、聚苯乙烯磺酸钠、聚乙烯酸酯或聚L赖氨酸。
实验例:
(1)拉伸测试
以实施例1制备的交联弹性体为测试对象,以未与聚氨酯预聚体交联改性的PDMS为对照,进行拉伸测试,具体为:样品尺寸10mm×5mm×0.8mm(长×宽×厚),拉伸速率为20mm/min,夹具间的样品长3mm,PDMS的断裂伸长率为252.7%,断裂强度为0.82MPa,实施例1制备的交联弹性体的断裂伸长率为430%,断裂强度为4.0MPa。
(2)自修复测试:
样品尺寸10mm×5mm×0.8mm(长×宽×厚),用刀片将样品条从中间横向切成两半,切口整齐吻合,随即将两样条靠拢进行对接,指压维持10s后,室温(25℃)放置4h,光学显微镜下已无切口痕迹,以断裂样与原样的断裂伸长率之比作为修复率,其修复率达84%,24h修复率为95%。
(3)疏水与防冰测试:
接触角测定实验:使用DSA30型光学接触角分析仪观测膜表面水滴的接触角变化情况。将4μl去离子水滴于膜表面,通过分析仪实时记录水滴在薄膜表面的形状变化,以未添加铁磁性的纳米微粒的贴膜为对照,测得接触角和滚动角结果如下:
接触角/° | 滚动角/° | |
对照 | 108 | 12 |
实施例1 | 159 | 4 |
实施例2 | 154 | 5 |
(4)冰沾附强度测试:
采用微电子机械天平(DCAT-21)测试冰与贴膜表面之间的黏附力,将600μl的水与铜环一起放置到贴膜表面,冷冻后,水滴冷冻成冰,同时将铜环冷冻固定在结冰水滴内部,再将铜环垂直固定到微电子机械天平上,在软件程序控制下,挡板以2mm/s的速度向下运动,直到冰与贴膜完全分离,测定其沾附强度,测定实施例1和实施例2制备的贴膜的沾附强度分别为318.9Pa和176.8Pa。
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种防覆冰贴膜的制备方法,其特征在于,包括以下步骤:
(1)聚氨酯预聚体制备
9.2g异佛尔酮二异氰酸酯中加入平均分子量500-600的聚乙二醇6g,5%的二月丁基二月桂酸锡1ml,在保护气氛下,在80℃水浴搅拌回流1h;
(2)预聚体混合
在制得的聚氨酯预聚体中加入三羟甲基丙烷1.4g,聚乙二醇二甲基丙烯酸酯2.3g,粘度小于50mPas的低聚端羟基聚二甲基硅氧烷18-24g,正硅酸乙酯8-9g,具有铁磁性的纳米微粒0.4-2g,超声分散处理使其混合均匀;
(3)交联固化
将混合均匀后的预聚体涂布在基体膜层上,置于磁场中热交联固化成型,固化温度120℃,制得所述防覆冰贴膜。
2.根据权利要求1所述的一种防覆冰贴膜的制备方法,其特征在于,所述基体膜层为PET或PVC薄膜。
3.根据权利要求1所述的一种防覆冰贴膜的制备方法,其特征在于,所述具有铁磁性的纳米微粒粒径在0.1-1μm之间。
4.根据权利要求1所述的一种防覆冰贴膜的制备方法,其特征在于,所述具有铁磁性的纳米微粒为铁磁金属纳米颗粒、铁磁性复合金属微粒、磁性金属氧化物微粒或其组合,所述铁磁金属纳米颗粒包括铁、钴、镍的微粒,所述铁磁性复合金属微粒包括铁与稀土金属复合的微粒。
5.根据权利要求4所述的一种防覆冰贴膜的制备方法,其特征在于,所述具有铁磁性的纳米微粒由溶胶-凝胶法、共沉淀法、水热法、溶剂热、离子热法合成,或利用球磨、砂磨和胶体磨技术将磁性颗粒粉碎得到。
6.根据权利要求4所述的一种防覆冰贴膜的制备方法,其特征在于,所述具有铁磁性的纳米微粒为具有棒状、长方体、棱柱或纳米花形貌的四氧化三铁微粒。
7.权利要求1-6任一所述的制备方法制备的防覆冰贴膜。
8.根据权利要求7所述的防覆冰贴膜,其特征在于,所述防覆冰贴膜上表面还涂覆有聚电解质薄层,涂附量0.5-5ml/m2。
9.根据权利要求8所述的防覆冰贴膜,其特征在于,所述聚电解质为聚二烯丙基二甲基胺盐酸盐、聚丙烯胺盐酸盐、聚二烯丙基二甲基氯化铵、质子化的聚乙撑亚胺、聚苯乙烯磺酸钠、聚乙烯酸酯或聚L赖氨酸。
10.根据权利要求8所述的防覆冰贴膜,其特征在于,所述聚电解质薄层的涂覆方法为:配制浓度0.01~0.2mol·L-1的聚电解质溶液,调节溶液pH至6-12;等离子体处理使防覆冰贴膜上表面呈负电荷状态,再涂布聚电解质,干燥即得。
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CN116376430A (zh) * | 2023-03-27 | 2023-07-04 | 清华大学 | 一种基于油基磁化微针的抗冰涂层及其制备方法和应用 |
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CN115505330B (zh) * | 2021-06-07 | 2023-11-14 | 株式会社神户制钢所 | 铝制翅片材和结冰结霜抑制剂 |
CN116376430A (zh) * | 2023-03-27 | 2023-07-04 | 清华大学 | 一种基于油基磁化微针的抗冰涂层及其制备方法和应用 |
CN116376430B (zh) * | 2023-03-27 | 2024-01-30 | 清华大学 | 一种基于油基磁化微针的抗冰涂层及其制备方法和应用 |
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