CN105346146B - 滚动角可控的高密度聚乙烯超疏水片材/容器及其制备方法 - Google Patents
滚动角可控的高密度聚乙烯超疏水片材/容器及其制备方法 Download PDFInfo
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Abstract
本发明属于超疏水材料制备技术领域,涉及滚动角可控的高密度聚乙烯超疏水片材/容器及其制备方法,先通过平板硫化机将高密度聚乙烯粒料模压成10微米至2厘米的高密度聚乙烯片材,再使用平板硫化机在模具中将2~4片高密度聚乙烯片材叠压在一起,然后将叠压在一起的高密度聚乙烯片材冷却至室温,或移至曲面模具上并使与曲面模具贴合后冷却至室温,最后用手、铁钳或万能试验机将叠压在一起的高密度聚乙烯片材进行剥离,得到滚动角可控的高密度聚乙烯超疏水片材或容器;其方法简单易行,原理科学,操作简便,制备成本低,环境友好,制备的超疏水片材/容器具有很高的水接触角,并且滚动角可控。
Description
技术领域:
本发明属于超疏水材料制备技术领域,涉及滚动角可控的高密度聚乙烯超疏水片材/容器及其制备方法。
背景技术:
疏水性是材料表面的重要特征之一,它是由表面的化学组成和微观几何结构共同决定的。当液滴与材料表面接触,它仍保持液滴形状或者在表面铺展形成液膜,这一性质通常用水接触角(WCA)来衡量。通常将接触角大于150°,滚动角小于10°的表面称为超疏水表面。超疏水材料独特的表面特性使其广泛应用于防水、防污、防雾、自清洁、流体减阻、微流体芯片和抑菌等领域。与金属材料相比,高聚物材料的表面超疏水化研究显得更为广泛和重要。聚合物本身具有较低的自由能和良好的热成型加工性能,在制备工艺上方便简洁,方式多样,适合大批量快速生产,且成本低廉。制备超疏水表面,主要从两个方面着手:一方面是在疏水材料(接触角大于90°)表面构建粗糙结构;另一方面是在粗糙表面上用低表面能物质进行修饰。常用于表面修饰的低表面能材料大多是含氟、硅基团的物质,如:氟化烷基硅烷、氟高聚物、氟化合物等。近十几年来,源源不断的加工技术被用来制备超疏水表面,如光刻工艺、模板法、刻蚀法、自组装法、电化学沉积法、电纺丝法、等离子体法、溶胶凝胶法和相分离法等。采用这些方法制备超疏水表面的思想是构建微观尺度上微米和纳米级的分层复杂几何结构,增加表面粗糙度(参考文献:Xinjian Feng,Jiang Lei.Adv.Mater.2006,18,3063-3078;Ye Tian,Bin Su,Lei Jiang,Adv.Mater.2014,26,6872–6897;Paul Roach,Neil J.Shirtcliffe,Michael I.Newton,Soft Matter,2008,4,224-240)。
高密度聚乙烯(HDPE)是一种常见的热塑性塑料,广泛用于生产生活的各个方面,关于高密度聚乙烯的超疏水化研究一直备受关注(参考文献:焦志达,陈刚,吉海燕,塑料科技,2012,40(3):64-66;Lie Shen,Hongliang Ding,QinghuaCao,Weican Jia,Wen Wang,Qipeng Guo,Carbon,2012,50:4284-4290;刘建平,钟铧均,杨小敏,李霜,蓝芳,广州化工,2010,38(9):67-69;郑建勇,冯杰,钟明强,高分子学报,2010,10:1186-1192;Zhiqing Yuan,Hong Chen,Jianxin Tang,Dejian Zhao,Journal of Applied Polymer Science,2009,113:1626–1632;Yuwon Lee,Kuk-Youn Ju,Jin-Kyu Lee,Langmuir,2010:26(17):14103–14110;刘建平,杨小敏,钟铧均,赵永刚胡林,化学通报,2010,11:1041-1044;Qianfeng Xu,Yang Liu,Fang-Ju Lin,Bikash Mondal,Alan M.Lyons,ACS Appl.Mater.Interfaces,2013,5:8915-8924;JonghoLee,Ronald S.Fearing,Langmuir,2012,28:15372-15377;袁志庆,一种超疏水高密度聚乙烯薄膜的制备方法,中国专利CN101157768B;Zhen-Xiu Zhang,Yanan Li,Ming Ye,Kanoktip Boonkerd,Zhenxiang Xin,Doris Vollmer,JinKuk Kim,Xu Deng,J.Mater.Chem.A,2014,2:1268–1271),但实际应用方面却进展不大,主要原因在于:一是现有制备方法涉及到特定的设备、专门的带有微纳米结构的模板、苛刻的条件和较长的周期,难以进行超疏水表面的大面积制备;二是现有方法需要大量的化学试剂和有机溶剂,涉及环境和污染问题;三是现有的一些方法需要用低表面能物质进行化学修饰,如含氟或硅的化合物,这些化合物价格昂贵,增加了产品成本;四是关于滚动角可控的超疏水高密度聚乙烯报道非常少。
滚动角可控的超疏水高密度聚乙烯是指通过制备条件来调节超疏水表面的滚动角,滚动角不同,其用途也不同。高密度聚乙烯表面的滚动角由表面黏附力决定,水滴在低黏附性超疏水表面,即使有轻微的倾斜(<10°)也极易滚动滑落,在水滴与高黏附性超疏水表面的接触角大于150°的情况下,将表面倾斜90°甚至180°,水滴仍然黏附在表面上,这种性质被用来在微米尺度上操纵液滴,可以在微流体系统、液体无损转移和生物技术等方面发挥重大作用。韩建梅等(Journal of Colloid and Interface Science,2008,326:360–365)报道了通过本体光聚合的方法在砂纸打磨过的高密度聚乙烯表面接枝丙烯酸,控制好光聚合的时间,能得到超疏水表面,且在不同的条件下,该表面的黏附性有很大差别,该方法需采用挥发性较大的单体丙烯酸进行化学光聚合,需要配置光刻胶,涉及到光聚合的均匀性,产品的稳定性,及环境污染和成本问题,难以大面积制备;Xianliang Sheng与Jihua Zhang(Langmuir,2009,25(12):6916-6922)报道了通过阳极氧化铝模板挤出的方法制备高密度聚乙烯纳米纤维表面,调节氧化铝模板的孔径和挤出压力,滚动角能在10°和90°左右进行调节,该方法需专门的纳米氧化铝模板,聚合物挤出后需要用高浓度氢氧化钠溶液将模板刻蚀去除,步骤繁琐,实验要求高,成本高,难以产业化。另外,关于曲面型高密度聚乙烯超疏水容器的绿色、简便、低成本制备方法也未见报道。
综上所述,可控滚动角(从水滴几乎无法稳定的超小滚动角到水滴在表面倾转90°或180°也不发生滚动的超大滚动角)的超疏水高密度聚乙烯已有报道,但目前的方法存在过程繁琐、难以控制、周期较长、成本较高和环境污染等问题。因此,寻求一种易于工业化生产、绿色环保、低成本、快速的方法来制备滚动角可控的超疏水高密度聚乙烯片材/容器显得尤为重要。
发明内容:
本发明的目的在于克服现有技术存在的缺点,提供滚动角可控的高密度聚乙烯超疏水片材/容器及其制备方法。
为了实现上述目的,本发明所述滚动角可控的高密度聚乙烯超疏水片材的厚度为10微米至2厘米,其外观根据厚度和尺寸包含薄膜、片材和块材三种形式;制备滚动角可控的高密度聚乙烯超疏水曲面容器所需片材的厚度为10微米至2厘米,制得的曲面容器高度为0.1~50厘米,开口直径为0.5~100厘米;高密度聚乙烯超疏水片材/容器的表面为层压或热压剥离产生的多层次微纳米结构,多层次微纳米结构包括有不规则多边形或类环形凹槽结构;高黏附高密度聚乙烯超疏水片材/容器的表面微纳米结构特征为:不规则多边形或类环形凹槽结构的平均直径为0.1~2微米,高度为0.1~8微米,凹槽底部为片层结构,凹槽周围为齿状、带状、丝状聚合物结构,齿状和带状结构的尺寸小于1微米,齿状和带状结构中有直径2~50纳米的纤维状结构,丝状结构的直径小于20纳米;低黏附高密度聚乙烯超疏水片材/容器的表面微纳米结构特征为:不规则多边形或类环形凹槽结构的平均直径为2~60微米,高度为2~150微米,凹槽底部和周围为齿状、带状、丝状聚合物微纳米结构,齿状和带状结构的尺寸小于200微米,齿状和带状结构中有直径2~50纳米的纤维状结构,丝状结构的直径小于30纳米;高密度聚乙烯超疏水表面与水的接触角均大于150°,滚动角大于0°,小于180°;高密度聚乙烯超疏水片材/容器根据制备条件处于超疏水低黏附状态或超疏水高黏附状态。
本发明制备滚动角可控的高密度聚乙烯超疏水片/容器的具体步骤如下:
(1)压片:在110~170℃温度和1~10MPa压强下通过平板硫化机将高密度聚乙烯粒料模压成10微米至2厘米的高密度聚乙烯片材;
(2)叠压:高黏附高密度聚乙烯超疏水表面的叠压条件:设定温度为122~126℃,预热2~10min,保压压力为1~5MPa,保压时间为1~5min,使用平板硫化机在模具中将步骤(1)制得的2~4片高密度聚乙烯片材叠压在一起;低黏附高密度聚乙烯超疏水表面的叠压条件:设定温度为127~129℃,预热2~10min,保压压力为1~5MPa,保压时间为1~5min,使用平板硫化机在模具中将步骤(1)制得的2~4片高密度聚乙烯片材叠压在一起;
(3)层间剥离:将步骤(2)叠压在一起的高密度聚乙烯片材冷却至室温,用手、铁钳或万能试验机将叠压在一起的高密度聚乙烯片材进行剥离,得到滚动角可控的高密度聚乙烯超疏水片材;将步骤(2)叠压在一起的高密度聚乙烯片材迅速转移至曲面模具上并使其与曲面模具贴合,冷却至室温,用手、铁钳或万能试验机将叠压在一起的高密度聚乙烯片材进行剥离,得到曲面型高密度聚乙烯超疏水容器。
本发明所述方法将传统的聚合物加工技术—平板热压技术应用到超疏水表面的制备过程中,不需要隔绝空气或特殊环境,不需要低表面能化学物质的修饰,方法简单易行,无需共混其它材料,仅需对塑料粒料进行压片、层压、剥离三步便可完成,无需化学试剂,适合大规模、大批量、大面积制备,不仅能制作平面状超疏水片材,还可制作超疏水曲面容器。
本发明与现有技术相比,具有以下优点:一是仅使用单一的聚合物本体材料—高密度聚乙烯,不使用和添加其他任何的材料和化学试剂,绿色环保;二是采用传统的叠压(或层压、热压)工艺制样,辅以手动、铁钳或万能试验机等方式剥离制备聚合物超疏水表面,工艺简单,加工时间短,成本低,所得聚合物表面近乎100%具备超疏水效果,可大规模、低成本生产各种片材或三维立体形状的聚合物超疏水产品;三是能够实现超疏水低黏附与超疏水高黏附聚合物表面的制备,制得的超疏水材料与水的接触角均大于150°,滚动角小于5°,大于0°,最大可达90~180°;其方法简单易行,原理科学,操作简便,制备成本低,环境友好,制备的超疏水片材/容器具有很高的水接触角,并且滚动角可控。
附图说明:
图1为本发明实施例1水滴在高密度聚乙烯表面的照片和接触角159°测试照片(a)、水滴在倾斜的高密度聚乙烯表面滚动的视频截图(b,滚动角<5°)、低黏附高密度聚乙烯表面低倍扫描电镜照片(c)和高倍扫描电镜照片(d);
图2为本发明实施例2中高黏附高密度聚乙烯表面低倍扫描电镜照片(a)、高倍扫描电镜照片(b)、接触角152°测试照片(c)、水滴在90°垂直的高密度聚乙烯表面的照片(d)以及水滴在倒置的高密度聚乙烯表面的照片(e)。
图3为本发明实施例3所述高密度聚乙烯超疏水曲面凹形容器的照片(a,容器口直径为4.2cm,高度为0.8cm)、曲面凹形容器的侧视图(b)以及曲面凹形容器装有5毫升蓝色硫酸铜水溶液的照片(c)。
具体实施方式:
下面通过实施例并结合附图对本发明作进一步说明。
实施例1:
本实施例在85*115*1.5mm的模具中放入高密度聚乙烯粒料15g,用平板硫化机在138℃下将模具预热10min,在保压压力5MPa条件下保压5min,冷却至室温制得高密度聚乙烯片,然后在85*115*3mm模具中将制得的两片高密度聚乙烯片叠压在一起放入平板硫化机中,在127℃预热5min,在3MPa压力下保压3min,冷却至室温后用铁钳将叠压在一起的高密度聚乙烯片进行剥离,制得低黏附高密度聚乙烯超疏水片材,图1为水滴在高密度聚乙烯超疏水表面的照片、接触角(159°)测试照片、滚动角(<5°)测量视频截图及高密度聚乙烯表面扫描电镜照片。
实施例2:
本实施例在85*115*0.5mm的模具中放入高密度聚乙烯粒料5g,用平板硫化机在150℃下将模具预热6min,在保压压力3MPa条件下保压时间5min,冷却至室温制得高密度聚乙烯薄片,然后在85*115*1mm模具中将制得的两片高密度聚乙烯薄片叠压在一起放入平板硫化机中,在125℃预热10min,在2MPa压力下保压2min,冷却至室温后用手将叠压在一起的高密度聚乙烯薄片进行剥离,制得高黏附高密度聚乙烯超疏水片材,图2为高密度聚乙烯表面扫描电镜照片、接触角(152°)测试照片、水滴在90°垂直和倒置的高密度聚乙烯表面的照片。
实施例3:
本实施例在85*115*1mm的模具中放入高密度粒料10g,用平板硫化机在140℃下将模具预热5min,在保压压力5MPa条件下保压3min,冷却至室温制得高密度聚乙烯片材,然后在85*115*2mm模具中将制得的两片高密度聚乙烯片材叠压在一起放入平板硫化机中,在127℃预热3min,在2MPa压力下保压2min,迅速将叠压在一起的片材转移到曲面凹形模具上并使其与曲面型模具贴合,待降到室温后用铁钳将叠压在一起的聚乙烯片材进行剥离,制得低黏附高密度聚乙烯超疏水曲面凹形容器,图3是高密度聚乙烯曲面容器照片及其装有蓝色硫酸铜水溶液的照片。
Claims (1)
1.一种滚动角可控的高密度聚乙烯超疏水片材的制备方法,其特征在于具体步骤如下:在85*115*1.5mm的模具中放入高密度聚乙烯粒料15g,用平板硫化机在138℃下将模具预热10min,在保压压力5MPa条件下保压5min,冷却至室温制得高密度聚乙烯片,然后在85*115*3mm模具中将制得的两片高密度聚乙烯片叠压在一起放入平板硫化机中,在127℃预热5min,在3MPa压力下保压3min,冷却至室温后用铁钳将叠压在一起的高密度聚乙烯片进行剥离,制得低黏附高密度聚乙烯超疏水片材,其接触角为159°,滚动角<5°。
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