CN112876988A - 一种油水分离易清洁无机纳米涂层及其制备方法 - Google Patents
一种油水分离易清洁无机纳米涂层及其制备方法 Download PDFInfo
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Abstract
本发明提供一种油水分离易清洁无机纳米涂层及其制备方法，按重量份数计，包括氟硅树脂1.0～1.5份、氟代有机物55.4～60份、丙二醇甲醚40.6～42份、乙二醇2.0～2.5份、乙二醇丁醚0.1～0.5份、硅酸酯1.0～5.0份和无机纳米粒子0.1～60份。本发明采用氟硅树脂和全氟丁基甲醚作为基底材料，不仅对环境友好成本低，且无毒无污染，可实现油水分离，同时具备自清洁功能。
Description
技术领域
本发明涉及化工涂料技术领域，涉及一种油水分离易清洁无机纳米涂层及其制备方法。
背景技术
石油开采、石油化工、化工、交通运输、机械加工、纺织、皮革、医药、食品制造等行业每天都在排放出大量的含油污水。据报道，每年世界上约有500～1000万吨油类通过各种途径流入海洋。由于含油污水的化学耗氧量(COD)高，含油量大，对环境污染严重，特别是近几年发生的漏油事件，更是对我们赖以生存的环境和人类健康造成了巨大危害。对含油污水进行有效的分离和处理既有科学价值，又有社会意义。
超疏水表面一般指水滴在其接触角大于150°，滚动角小于10°的表面。它具有自清洁、抗粘附、防雾抑菌、防水等优良特性，因而超疏水材料在防水衣物、外墙涂料、电子元器件、管道微流、油水分离、生物医用等领域展现出了十分广泛的应用前景。具有超疏水超亲油特性的油水分离涂层具有分离过程简洁、分离效率高的特点，与传统油水分离技术相比拥有更好的发展前景。然而，目前超疏水表面的制备方法不仅工艺复杂、成本高昂，而且超疏水涂层表面的微纳结构极易被破坏，在油水分离过程中会导致涂层表面失去其超疏水特性，从而影响油水分离的效果。
再加之近年来，研究者通过研究具有自清洁功能的荷叶的表面拓扑结构，发现荷叶微观表面非常粗糙，且由超疏水性物质组成，于是，人们开始制备具有特殊浸润性和粗糙表面的油水分离涂层，并利用这种特殊分离涂层进行油水分离。
因此，发明一种油水分离易清洁无机纳米涂层以及该涂层的简单易行的制备方法势在必行。
发明内容
本发明目的在于提供一种油水分离易清洁无机纳米涂层及其制备方法，采用氟硅树脂和全氟丁基甲醚作为基底材料，不仅对环境友好成本低，且无毒无污染，可实现油水分离，同时具备自清洁功能。
本发明的技术方案是这样实现的：
一方面，本发明提供一种油水分离易清洁无机纳米涂层，包括氟硅树脂、氟代有机物、丙二醇甲醚、乙二醇、乙二醇丁醚、硅酸乙酯和无机纳米粒子。
进一步地，按重量份数计，氟硅树脂1.0～1.5份、氟代有机物55.4～60份、丙二醇甲醚40.6～42份、乙二醇2.0～2.5份、乙二醇丁醚0.1～0.5份、硅酸酯1.0～5.0份和无机纳米粒子0.1～60份。
进一步地，按重量份数计，氟硅树脂1.0～1.4份、氟代有机物55.4～55.8份、丙二醇甲醚40.6～41.0份、乙二醇2.0～2.4份、乙二醇丁醚0.1～0.3份、硅酸酯1.0～5.0份和无机纳米粒子0.1～60份。
进一步地，所述氟代有机物为全氟三丙胺或全氟丁基甲醚，其中氟代有机物中氟的强吸电子能力，具有优越的热稳定性，独特的低表面自由能和较低的粘度，对本发明制备的无机纳米涂层性能具有较优的改善作用。
进一步地，所述无机纳米粒子包括二氧化硅纳米粒子、二氧化钛纳米粒子、氧化铝纳米粒子、氧化锌纳米粒子、氧化石墨烯纳米粒子中的一种或多种的组合。所述无机纳米粒子的粒径为10～200nm。
进一步地，所述硅酸酯包括正硅酸甲酯、正硅酸乙酯、正硅酸丙酯、正硅酸异丙酯、正硅酸丁酯中的一种或多种的组合。
进一步地，本发明所制备的油水分离易清洁无机纳米涂层中样品的固含量在1.0～1.4％，固含量测试条件为样品在160摄氏度烘箱内烘4小时。
另一方面，本发明提供一种油水分离易清洁无机纳米涂层的制备方法，包括以下步骤：
1)将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30～90℃反应得到无机纳米材料；
2)将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后喷涂在基材表面，水平放置20～60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到油水分离易清洁无机纳米涂层。
进一步地，所述喷涂采用喷枪喷涂，喷涂压力为4～5bar。
进一步地，所述基材为玻璃板、木材、塑料板、钢板、纸板、布料或石材，具体可根据材料进行变化。
进一步地，所述涂层厚度为2～5微米。
有益效果：
本发明提供的油水分离易清洁无机纳米涂层具有高致密性、好的耐污性，在常温即可固化，使用工艺简单，寿命长。本发明通过采用氟代有机物提高涂层表面活性，能有效降低水的表面张力，提高疏水性。本发明采用氟硅树脂作为基材之一，其本身具有超疏水性，与水的接触角大于130°，最大可达到155°。制备过程中，以氟硅树脂的Si-R和氟代有机物的O-R的缩合反应为起始，官能团释放出活性氢和反应过程中释放的热量进行交联聚合，使得体系中的硅氧键Si-OR相互结合，Si-OR接触到空气中的水分后生成硅氧氢键Si-OH+-R，在基材表面形成致密的膜层；氟代有机物中的F与无机纳米粒子表面的氢键相结合形成网状结构的纳米尺寸粗糙表面，使得涂层表面具有疏水性和自清洁功能，测试水滴接触角在142～167°，涂层对油的接触角为0°，因此本发明涂层能有效分离油水。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1实施例1中制备涂层烘干样的TGS测试结果图。
图2实施例1制备涂层烘干样的DSC测试结果图。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员所获得的所有其他实施例，都属于本发明保护的范围。
除非另有定义，下文中所使用的所有专业术语与本领域技术人员通常理解的含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的，并不是旨在限制本发明的保护范围。
除有特别说明，本发明中用到的各种试剂、原料均为可以从市场上购买的商品或者可以通过公知的方法制得的产品。
实施例1
一种油水分离易清洁无机纳米涂层，按重量份数计，包括氟硅树脂1.0份、氟代有机物55.8份、丙二醇甲醚40.6份、乙二醇2.4份、乙二醇丁醚0.1份、硅酸酯5.0份和无机纳米粒子0.1份。
所述氟代有机物为全氟丁基甲醚；
所述无机纳米粒子包括二氧化硅纳米粒子、二氧化钛纳米粒子、氧化铝纳米粒子的组合，三者重量比例为1:1:1；所述无机纳米粒子的粒径为150～200nm；
所述硅酸酯包括正硅酸乙酯。
一种油水分离易清洁无机纳米涂层的制备方法，包括以下步骤：
1)将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30～90℃反应得到无机纳米材料；
2)将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后采用喷枪喷涂在基材表面，喷涂压力为4～5bar，喷涂完后将基材水平放置20～60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到厚度为2～5微米的油水分离易清洁无机纳米涂层；
所述基材为玻璃板。
本发明所制备的油水分离易清洁无机纳米涂层中样品的固含量在1.0～1.4％，固含量测试条件为样品在160摄氏度烘箱内烘4小时。
实施例2
一种油水分离易清洁无机纳米涂层，按重量份数计，包括氟硅树脂1.4份、氟代有机物55.4份、丙二醇甲醚41.0份、乙二醇2.0份、乙二醇丁醚0.3份、硅酸酯5.0份和无机纳米粒子60份。
所述氟代有机物为全氟三丙胺或全氟丁基甲醚；
所述无机纳米粒子包括氧化铝纳米粒子、氧化石墨烯纳米粒子的组合，二者质量比为1:2；所述无机纳米粒子的粒径为10～50nm；
所述硅酸酯包括正硅酸甲酯。
一种油水分离易清洁无机纳米涂层的制备方法，包括以下步骤：
1)将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30～90℃反应得到无机纳米材料；
2)将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后采用喷枪喷涂在基材表面，喷涂压力为4～5bar，喷涂完后将基材水平放置20～60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到厚度为2～5微米的油水分离易清洁无机纳米涂层；
所述基材为纸板。
实施例3
一种油水分离易清洁无机纳米涂层，按重量份数计，包括氟硅树脂1.2份、氟代有机物55.5份、丙二醇甲醚40.7份、乙二醇2.1份、乙二醇丁醚0.2份、硅酸酯3.0份和无机纳米粒子30份。
所述氟代有机物为全氟丁基甲醚；
所述无机纳米粒子包括二氧化硅纳米粒子、二氧化钛纳米粒子、氧化铝纳米粒子、氧化锌纳米粒子、氧化石墨烯纳米粒子的组合，质量比为1:1:1:1:1；所述无机纳米粒子的粒径为50～100nm；
所述硅酸酯包括正硅酸乙酯。
一种油水分离易清洁无机纳米涂层的制备方法，包括以下步骤：
1)将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30～90℃反应得到无机纳米材料；
2)将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后采用喷枪喷涂在基材表面，喷涂压力为4～5bar，喷涂完后将基材水平放置20～60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到厚度为2～5微米的油水分离易清洁无机纳米涂层；
所述基材为塑料板。
实施例4
一种油水分离易清洁无机纳米涂层，按重量份数计，包括氟硅树脂1.5份、氟代有机物60份、丙二醇甲醚42份、乙二醇2.5份、乙二醇丁醚0.5份、硅酸酯4.0份和无机纳米粒子46份。
所述氟代有机物为全氟丁基甲醚；
所述无机纳米粒子包括二氧化硅纳米粒子、二氧化钛纳米粒子、氧化铝纳米粒子、氧化锌纳米粒子、氧化石墨烯纳米粒子的组合，质量比为1:1:1:1:1；所述无机纳米粒子的粒径为100～150nm；
所述硅酸酯包括正硅酸乙酯。
一种油水分离易清洁无机纳米涂层的制备方法，包括以下步骤：
1)将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30～90℃反应得到无机纳米材料；
2)将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后采用喷枪喷涂在基材表面，喷涂压力为4～5bar，喷涂完后将基材水平放置20～60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到厚度为2～5微米的油水分离易清洁无机纳米涂层；
所述基材为布料。
实施例5
对本发明实施例制备的涂层进行检测，具体测试方法如下：
测试结果如下：
ND＝未被检出。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种油水分离易清洁无机纳米涂层，其特征在于，包括氟硅树脂、氟代有机物、丙二醇甲醚、乙二醇、乙二醇丁醚、硅酸乙酯和无机纳米粒子。
2.根据权利要求1所述油水分离易清洁无机纳米涂层，其特征在于，按重量份数计，包括氟硅树脂1.0~1.5份、氟代有机物55.4~60份、丙二醇甲醚40.6~42份、乙二醇2.0~2.5份、乙二醇丁醚0.1~0.5份、硅酸酯1.0~5.0份和无机纳米粒子0.1~60份。
3.根据权利要求2所述油水分离易清洁无机纳米涂层，其特征在于，按重量份数计，包括氟硅树脂1.0~1.4份、氟代有机物55.4~55.8份、丙二醇甲醚40.6~41.0份、乙二醇2.0~2.4份、乙二醇丁醚0.1~0.3份、硅酸酯1.0~5.0份和无机纳米粒子0.1~60份。
4.根据权利要求1所述油水分离易清洁无机纳米涂层，其特征在于，所述氟代有机物为全氟三丙胺或全氟丁基甲醚。
5.根据权利要求1所述油水分离易清洁无机纳米涂层，其特征在于，所述无机纳米粒子包括二氧化硅纳米粒子、二氧化钛纳米粒子、氧化铝纳米粒子、氧化锌纳米粒子、氧化石墨烯纳米粒子中的一种或多种的组合；所述无机纳米粒子的粒径为10~200nm。
6.根据权利要求1所述油水分离易清洁无机纳米涂层，其特征在于，所述硅酸酯包括正硅酸甲酯、正硅酸乙酯、正硅酸丙酯、正硅酸异丙酯、正硅酸丁酯中的一种或多种的组合。
7.一种权利要求1~6任一项所述油水分离易清洁无机纳米涂层的制备方法，其特征在于，包括以下步骤：
将无机纳米粒子在惰性气体氛围下超声分散在丙二醇甲醚和乙二醇中，得到无机纳米粒子分散液；将硅酸酯加入无机纳米粒子分散液中在30~90℃反应得到无机纳米材料；
将氟硅树脂、氟代有机物溶解在乙二醇丁醚中在惰性气体氛围下超声分散后喷涂在基材表面，水平放置20~60分钟，再将无机纳米材料分散喷涂在基材表面膜上，室温干燥，得到油水分离易清洁无机纳米涂层。
8.根据权利要求7所述油水分离易清洁无机纳米涂层的制备方法，其特征在于，所述喷涂采用喷枪喷涂，喷涂压力为4~5bar。
9.根据权利要求7所述油水分离易清洁无机纳米涂层的制备方法，其特征在于，所述基材为玻璃板、木材、塑料板、钢板、纸板、布料或石材。
10.根据权利要求7所述油水分离易清洁无机纳米涂层的制备方法，其特征在于，所述涂层厚度为2~5微米。
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