CN107428973B - 用于材料的表面改性的方法 - Google Patents

用于材料的表面改性的方法 Download PDF

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CN107428973B
CN107428973B CN201680014609.1A CN201680014609A CN107428973B CN 107428973 B CN107428973 B CN 107428973B CN 201680014609 A CN201680014609 A CN 201680014609A CN 107428973 B CN107428973 B CN 107428973B
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range
hydrophobic particles
particles
surface modification
microns
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CN107428973A (zh
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S·达斯
G·穆拉利达拉恩
A·普拉马尼克
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Unilever IP Holdings BV
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Abstract

本发明涉及材料的表面改性。具体地说，本发明涉及用于对聚合材料进行表面改性的方法，所述表面改性使所述表面不粘，以便降低材料粘着在其上的能力，并由此提供易流动性。所述方法包括用包括具有不同形状(圆形、正方形、矩形、多边形棱形)的微柱的图案对物体的所述表面进行压纹，所述微柱具有在10‑200微米的范围内的等同圆直径、高度和间距；通过喷涂或浸涂施加一层粘合剂以获得在所述压纹表面上0.1‑5mg/cm2的覆盖率；沉积0.2‑1.2mg/cm2的疏水性颗粒，其中所述疏水性颗粒具有在0.1‑10微米的范围内的粒径。

Description

用于材料的表面改性的方法
技术领域
本发明涉及材料的表面改性。具体地说，本发明涉及用于对可变形材料如聚合材料进行表面改性的方法，所述表面改性使所述表面不粘，以便降低诸如粘稠性食品或个人护理和卫生组合物等材料粘着在其上的能力，并由此提供易流动性。
背景技术
不粘性表面涉及衬底改性和/或处理，以降低材料粘着在其上的能力。通常具有高粘度的各种组合物，像食品配制物如番茄酱至个人护理配制物如洗发剂、液体肥皂、保湿洗剂等被包装在容器中。由于容器内的材料或内容物粘着至其壁上而造成的材料损耗是巨大的。
用于制作不粘性表面的最常用且商业上实践的方法之一是使用聚四氟乙烯(PTFE或特氟隆Teflon)涂层。然而，该工艺是昂贵的，并且构成环境和健康问题。
US20110069361(Jun Hyun-Woo等)公开了通过蚀刻或注射成型或热压纹(embossing)产生图案或压痕以用于制造超疏水表面的不同方式。这具有有限的应用，因为所获得的接触角将不会很高，原因在于该方法将仅形成微柱(micropillar)，由此通过这种处理赋予的疏水性将较低。
使用一种或多种尺寸的疏水性颗粒和它们的组合已公开于WO 12138992(Trustees of Univ.of Pennsylvania)中，用以产生透明的疏水表面。使用具有不同粒径的颗粒的组合产生增强的粗糙度，这进而增强了疏水性质。然而，这些颗粒不会强烈地粘结至表面，因此它们不能耐受对表面的损害，随后就会丧失防水性质。
为了避免该问题，已提出使用粘结剂(US 2012107581，美国能源部)或偶联剂(WO14038701，Toppan Printing有限公司)。US 2012107581公开了用于生产光学透明、良好接合的超疏水涂层的组合物，其包含疏水性颗粒、粘结剂和溶剂。他们使用氰基丙烯酸乙酯、聚丙烯酸、聚四氟乙烯、聚氨酯作为粘结剂。在此类情况下，低浓度的粘结剂通常与颗粒混合，并且需要多个浸渍循环来实现超疏水性。或者，WO 14038701中已经公开了偶联剂的使用，但它们并不产生微柱，且所用方法不同。
US 2001/0051273 A1(Veerasamy)公开了涂覆有疏水层的衬底，其包括例如高度四面体的无定形碳(其是类金刚石碳(DLC)的形式)或任何其它适合的材料。所得经涂覆制品的外表面具有足够的表面粗糙度，使得所述制品具有至少约100度的初始接触角。在某些实施方案中，所述层具有不大于约20.2mN/m的表面能和/或至少约10GPa的平均硬度。
上述用于制备表面疏水的方法的问题在于，表面不能耐受甚至受到轻度磨损所造成的损坏，且随后丧失防水性质，或所导致的接触角相对较低。这主要归因于疏水性颗粒从表面脱落。本发明人已能够选择允许颗粒强烈粘合至表面以提供良好且稳定的疏水性质的粘合剂。获得稳定的超疏水表面是一种挑战，本发明人已能够通过特定的方法及通过产生微柱连同使用特定的粘合剂和疏水性颗粒的组合来实现该目的。
本发明的一个目的是提供对物体的表面进行改性以使所述表面不粘并由此提供粘稠性材料的易流动性的方法。
本发明的另一目的是提供通过产生微柱及使用粘合剂层沉积疏水性颗粒对物体的表面进行改性以提供超疏水表面的方法。
本发明的另一目的是提供对物体表面进行改性以使所述表面疏水并且即使当所述表面经受轻度磨损所造成的损坏时仍保持该性质的方法。
发明内容
根据本发明，提供了用于材料的表面改性的方法，其包括：
(i)用包括具有各自在10-200微米范围内的等同圆直径、高度和间距的微柱的压纹器对物体的表面进行压纹；
(ii)在从步骤(i)产生的压纹表面上施加0.1-5mg/cm2的粘合剂；
(iii)沉积从步骤(ii)产生的0.2-1.2mg/cm2的疏水性颗粒；
其中所述疏水性颗粒具有d50在0.1-10微米范围内的粒径。
具体实施方式
本发明涉及用于材料的表面改性的方法，其包括：
(i)用包括具有各自在10-200微米的范围内的等同圆直径、高度和间距的微柱的压纹器对物体的表面进行压纹；
(ii)在从步骤(i)产生的压纹表面上施加0.1-5mg/cm2的粘合剂；
(iii)在从步骤(ii)产生的表面上沉积0.2-1.2mg/cm2的疏水性颗粒；
其中所述疏水性颗粒具有d50在0.1-10微米范围内的粒径。
通过根据本发明的方法对材料的表面改性使材料的表面疏水，并且优选使得它们即使在所述表面经受轻度磨损所造成的损坏时也能够保持该性质，所述轻度磨损优选用在5kg的载荷下操作的塑料清洁拖把摩擦所述表面2分钟。
压纹：
选择用于对表面进行改性的物体优选任何可变形材料且更优选聚合材料，因为它们通常用于包装粘稠食品或个人护理和卫生组合物。聚合材料优选选自高密度聚乙烯(HDPE)、低密度聚乙烯(LDPE)、聚对苯二甲酸乙二酯(PET)、聚丙烯(PP)或聚苯乙烯(PS)或它们的衍生物。
通过优选使用压纹器来进行对物体表面的压纹以在它们的表面上产生图案，所述压纹器为金属网且更优选具有不同形状的不锈钢网，所述形状可优选圆形、正方形、矩形或多边形棱形，其具有各自在10-200微米且优选30-100微米范围内的等同圆直径、高度和间距。等同圆直径是指具有与其它形状的二维投影面积相等的面积的圆的直径。对物体表面的压纹适合地通过热压制或软光刻技术在可能在环境室温至高温范围内的温度下实现。优选使用热压制来对物体的表面进行压纹。在热压纹过程中，优选将所述网加热至70℃至约120℃且更优选80℃至约100℃的温度，并且优选将其在所述物体的表面上压制。该物体优选在去除金属网之后进行冷却。
粘合剂的施加：
所述粘合剂优选选自在约1Hz的频率下具有<0.3MPa的剪切弹性模量且更优选在约1Hz的频率下具有0.1-约0.2MPa的剪切弹性模量的那些。粘合剂的剪切弹性模量优选依照Dahlquist准则。通过优选喷涂或浸涂将粘合剂施加至物体的压纹表面上。粘合剂优选包括丙烯酸类、苯乙烯嵌段共聚物类、天然橡胶和硅酮配制物，其具有在约1Hz的频率下<0.3MPa的剪切弹性模量。
粘合剂的所述施加是在压纹表面上提供0.1-5mg/cm2且更优选0.3-2mg/cm2的粘合剂。
疏水性颗粒：
疏水性颗粒被沉积在粘合剂层上，且优选选自水不溶性无机材料，如金属氧化物或非金属氧化物，其选自二氧化硅、二氧化钛、氧化铝、氧化锌、氧化镁或氢氧化镁；金属碳酸盐，其选自碳酸钙、碳酸镁、碳酸锌；金属磷酸盐，其选自磷酸钙、磷酸镁；天然或合成的硅酸盐，其选自粘土、沸石、滑石、硅酸钙、硅酸镁；或交联聚合物，其选自聚苯乙烯、聚乙烯、聚丙烯酸乙烯基酯。疏水性颗粒优选选自具有d50在0.1-10微米、优选0.2-8微米且更优选0.2-1微米范围内的粒径的水不溶性无机材料。优选通过标准光散射实验来确定疏水性颗粒的d50。疏水性颗粒优选两种不同尺寸的颗粒的混合物，且更优选较小的颗粒在比较大的颗粒小2-8倍的范围内。优选较小的疏水性颗粒的d50在0.2-2微米且更优选0.2-0.5微米的范围内，且较大的疏水性颗粒的d50在0.8-8微米且更优选0.8-1微米的范围内。
优选沉积疏水性颗粒以提供在表面上有0.2-1.2mg/cm2的疏水性颗粒，且更优选在表面上0.25-0.5mg/cm2的疏水性颗粒。疏水性颗粒可通过各种途径如喷涂、浸涂、旋涂和在塑料成型期间在原材料进料中混合而被沉积在可变形材料的表面上，且更优选通过施加包含所述颗粒的在25℃下蒸气压大于50mmHg的溶剂而被沉积在可变形材料的表面上。所述溶剂优选地选自甲醇、乙醇、异丙醇、己烷、氯仿、苯、二甲苯或甲苯。所述疏水性颗粒不溶于水中，并且也不溶在于在25℃下蒸气压大于50mmHg的溶剂中。
疏水改性的物体：
根据本发明的方法制备的具有压纹表面的物体优选为可变形材料且更优选聚合材料。聚合材料优选选自高密度聚乙烯(HDPE)、低密度聚乙烯(LDPE)、聚对苯二甲酸乙二酯(PET)、聚丙烯(PP)或聚苯乙烯(PS)或它们的衍生物。
物体的压纹表面包含具有不同形状的微柱，所述微柱优选可以是圆形、正方形、矩形或多边形棱形，其等同圆直径、高度和间距各自在10-200微米且优选在30-100微米的范围内，其中疏水性颗粒通过粘合剂层粘合在微柱上。
根据本发明制备的物体的压纹表面可优选具有大于120°的水接触角，并且所述表面还可对于具有高于100cP粘度的液体显示出≤10°的倾斜角的液体滚动(roll off)，并且，还优选使得即使在所述表面经受轻度磨损所造成的损坏时它们也能够保持该性质，所述轻度磨损优选用在5kg的载荷下操作的塑料清洁拖把摩擦所述表面2分钟。
通过放置10μL水滴并水平固持测试样品并且捕获用于接触角测定的图像来测量接触角。借助于DropSnake插件，使用
Figure BDA0001402468590000051
软件来估计接触角。
通过将50μL粘稠性液滴放置在测试样品上，然后将其以10°斜度倾斜，以观察液体是否滚动来确定粘稠性液体的滚动。
实施例
(1)疏水表面改性材料的制备
(a)对表面进行压纹的方法：
使用80μm间距(pitch)的不锈钢网，在90℃通过将所述不锈钢网在尺寸为2cm×2cm的可变形材料高密度聚乙烯(HDPE)上压制1分钟，对所述可变形材料进行压纹。在去除不锈钢网之后将材料冷却，获得压纹的可变形材料。
(b)施加粘合剂的方法：
基于粘合剂的剪切弹性模量，使用两种类型的粘合剂。在约1Hz的频率下，粘合剂1具有大于0.3MPa的剪切弹性模量，而粘合剂2具有低于0.3MPa的剪切弹性模量。将所述粘合剂分别喷涂在两种压纹材料上以获得1.5mg/cm2的覆盖率。在当前的研究中，使用基于氰基丙烯酸酯的可商购的
Figure BDA0001402468590000061
[ex-Pidilite Industries有限公司，印度]作为粘合剂1，而使用可再贴的75
Figure BDA0001402468590000062
[ex-3M]作为粘合剂2。为了比较的目的，还研究了包含无任何粘合剂的压纹材料的组。
(c)沉积疏水性颗粒的方法：
(i)在喷雾上述粘合剂之后，将疏水性颗粒沉积在压纹的可变形材料的表面上。
(ii)如现有技术方法中所述的对照样品，其中将粘合剂和疏水性颗粒混合在一起，并施加在压纹的可变形材料的表面上。
(iii)另一组对照样品是其中将疏水性颗粒沉积在未被喷涂所述粘合剂的经压纹的可变形材料的表面上。
将分散在氯仿中的0.16ml 1％的疏水性二氧化硅颗粒[Sipernat d10ex-EvonikCorp]喷雾在经压纹的可变形材料的表面上，获得0.40mg二氧化硅/cm2的压纹可变形材料，在室温下干燥30分钟。在将疏水二氧化硅与粘合剂混合并喷雾的组中，将压纹表面上的疏水二氧化硅的量维持在0.40mg二氧化硅/cm2压纹可变形材料。
通过上述方法制备的各种材料被定义为表1中的实施例。
表1：可变形材料的表面改性
实施例 压纹 疏水性颗粒 粘合剂 粘合剂类型 颗粒和粘合剂的喷雾
1 是 否 否 - -
2 是 是 否 - -
3 是 是 是 1 依顺序
4 是 是 是 2 依顺序
5 是 是 是 1 同时
6 是 是 是 2 同时
2.超疏水性和粘稠性液体滚动以及疏水性颗粒结合的稳定性的定量化：
通过放置10μL水滴并水平固持如表1中所示的样品，并且捕获用于接触角测定的图像来测量所述样品的接触角。借助于DropSnake插件，使用
Figure BDA0001402468590000071
软件估计接触角。
通常，粘稠性液体是具有高于100cP的粘度的那些。在本研究中，使用含有0.5％黄原胶水溶液的模型液体测试粘稠性液体滚动，该量等同于通常用于诸如番茄酱的产品中的量。发现该0.5％黄原胶水溶液在3s-1的剪切速率下的粘度为600cP。将50μL粘稠性液滴水平放置在如表1中所述及的表面上，然后以10°斜度倾斜，以观察液体是否滚动。
测量按照实施例1-6制备的材料的接触角和粘稠性液体滚动。在使压纹且涂覆颗粒的表面经受用在5kg的载荷下操作的塑料清洁拖把摩擦2分钟之后再次重复测量，以便检查在等同于洗涤或清洁此类表面的处理之后，此类涂层的稳定性。
数据见表2中所示。
表2：粘合剂的性质对颗粒结合和超疏水性的影响
Figure BDA0001402468590000072
表2中呈现的数据显示，对于用疏水性颗粒喷雾的压纹可变形材料，接触角从90°增加至150°(实施例2)。然而，在不存在粘合剂的情况下，所述颗粒的结合不稳定，因此，当使材料的表面经受如上文所述的摩擦时，导致接触角降低至103°(实施例2)。
根据本发明制备的材料，即通过使用粘合剂2制备的材料具有具高接触角的良好疏水表面，并且即使在摩擦后它们也保持了从146°的接触角观察到的疏水性(实施例4)，而使用粘合剂1的类似研究并未产生良好的疏水性表面，并且在摩擦表面后，观察到接触角进一步降低至低于60°(实施例3)。
还观察到喷涂粘合剂2(剪切弹性模量<0.3MPa)后依顺序施加疏水性颗粒明显优于其中将疏水性颗粒与喷涂的粘合剂一起沉积在压纹表面上的现有技术的方法。在经受表面摩擦之前和之后观察到这种效果。
观察到只有当根据本发明制备疏水表面时，才看见良好的粘稠性滚动性质，并且即使在摩擦表面之后也维持了该效果。
3.疏水性颗粒的沉积程度对粘稠性液体滚动的影响
对尺寸为2cm×2cm的可变形材料高密度聚乙烯(HDPE)进行压纹并用粘合剂2喷涂，获得1.5mg/cm2的如上所述的覆盖率。在以按照本发明的顺序方式喷涂粘合剂之后，沉积如表3中所示的各种水平的疏水性二氧化硅。按照上述程序，在有疏水表面的摩擦和无疏水表面的摩擦的情况下测量接触角。
表3：颗粒沉积水平对水接触角的影响
实施例 颗粒(mg/cm<sup>2</sup>) 接触角(摩擦前) 接触角(摩擦后)
实施例1 0 90 90
实施例7 0.18 122 111
实施例8 0.25 136 121
实施例4 0.40 150 146
实施例9 0.57 136 129
实施例10 1.55 129 116
数据显示疏水二氧化硅在0.2-1.2mg/cm2的根据本发明的范围内的沉积在表面摩擦之前和之后具有良好的接触角，但当沉积水平超出该范围时，接触角显著下降，导致差的疏水性。

Claims (13)

1.一种用于材料的表面改性的方法，其包括：
(i)用包括具有各自在10-200微米的范围内的等同圆直径、高度和间距的微柱的压纹器对物体的表面进行压纹；
(ii)在从步骤(i)产生的压纹表面上施加0.1-5mg/cm2的粘合剂；
(iii)在从步骤(ii)产生的表面上沉积0.2-1.2mg/cm2的疏水性颗粒；
其中所述疏水性颗粒具有d50在0.1-10微米的范围内的粒径；并且其中所述粘合剂具有在1Hz的频率下<0.3MPa的剪切弹性模量。
2.根据权利要求1所述的用于材料的表面改性的方法，其中所述粘合剂的施加是通过喷涂或浸涂。
3.根据权利要求1或2所述的用于材料的表面改性的方法，其中所述疏水性颗粒是两种不同尺寸的颗粒的混合物，其中较小的颗粒在比较大的颗粒小2-8倍的范围内。
4.根据权利要求1或2所述的用于材料的表面改性的方法，其中所述较小的疏水性颗粒的d50在0.2-2微米的范围内，且所述较大的疏水性颗粒的d50在0.8-8微米的范围内。
5.根据权利要求1或2所述的用于材料的表面改性的方法，其中所述较小的疏水性颗粒的d50在0.2-0.5微米的范围内，并且所述较大的疏水性颗粒的d50在0.8-1微米的范围内。
6.根据权利要求1或2所述的用于材料的表面改性的方法，其中所述疏水性颗粒选自水不溶性无机材料或交联聚合物。
7.根据权利要求6所述的用于材料的表面改性的方法，其中所述水不溶性无机材料选自金属氧化物或非金属氧化物；金属碳酸盐；金属磷酸盐；天然或合成的硅酸盐；和/或所述交联聚合物选自交联的聚苯乙烯、聚乙烯、聚丙烯酸乙烯基酯。
8.根据权利要求1或2所述的用于材料的表面改性的方法，其中所述疏水性颗粒是通过施加包含所述颗粒的在25℃下蒸气压大于50mmHg的溶剂来沉积的。
9.根据权利要求8所述的用于材料的表面改性的方法，其中溶剂选自甲醇、乙醇、异丙醇、己烷、氯仿、苯、二甲苯或甲苯。
10.一种包含通过根据权利要求1至9中任一项所述的方法获得的压纹表面的物体，其中所述压纹表面包含具有各自在10-200微米范围内的等同圆直径、高度和间距的微柱，并且其中所述微柱的表面涂覆有0.1-5mg/cm2的粘合剂和0.2-1.2mg/cm2的疏水性颗粒，其中所述疏水性颗粒具有d50在0.1-10微米范围内的粒径，并且，其中所述粘合剂具有在1Hz的频率下<0.3MPa的剪切弹性模量。
11.根据权利要求10所述的物体，其包含疏水改性的压纹的表面。
12.根据权利要求10或11所述的物体，其中所述物体是选自以下的聚合材料：高密度聚乙烯(HDPE)、低密度聚乙烯(LDPE)、聚对苯二甲酸乙二酯(PET)、聚丙烯(PP)或聚苯乙烯(PS)或它们的衍生物。
13.根据权利要求10或11所述的物体，其中所述疏水改性表面具有大于120°的水接触角，和对于具有高于100cP的粘度的液体在≤10°的倾斜角下的液体滚动。
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