CN114855512A - 一种双氟硅型抗指纹乳液的制备方法及其在三聚氰胺浸渍纸中的应用 - Google Patents
一种双氟硅型抗指纹乳液的制备方法及其在三聚氰胺浸渍纸中的应用 Download PDFInfo
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Abstract
本发明公开了一种双氟硅型抗指纹乳液,乳液包含2‑4份聚全氟乙丙烯粉体、金属或非金属氧化物纳米粒子,4‑6份复配型全氟烷基硅氧烷与90‑94份无水乙醇。还公开了其在三聚氰胺浸渍纸中的应用方法。本发明的双氟硅型抗指纹乳液具备疏水疏油、原料成本低、制备工艺简便的特征,用其制备的三聚氰胺浸渍纸,可以提高纸面水、油接触角,提高装饰人造板疏水、疏油性能,提升耐污性。可广泛用于建材、家具、室内装饰装修以及车船等领域。
Description
技术领域
本发明属于涂料技术领域,具体涉及一种双氟硅型抗指纹乳液的制备方法及其在三聚氰胺浸渍纸中的应用。
背景技术
抗指纹材料由于其强大的自清洁性和防污染性能,被广泛应用于智能手机和平板电脑的屏幕、数码相机的镜头以及精密光学元件等高级光学制品的表面。指纹是由油脂、水分、粉尘、细菌等附在物品表面,所形成的固态外观。因此,要想达到抗指纹效果,必须要考虑疏水疏油性。20世纪90年代以来,不少学者通过对“荷叶效应”的研究,制备出了各类仿生材料,能同时达到疏水疏油的效果,即双疏材料。
研究表明,固体表面的双疏性主要是由低表面能物质和构筑合适的微纳表面决定的。降低表面能的方法包括氟硅型低表面能改性、长链型硅氧烷低表面能改性和无氟型聚合物低表面能改性。尽管现在已成功研究出许多方法来制备双疏、超双疏涂层,如化学蚀刻法、沉积法、溶胶-凝胶法和等离子技术等。但仍然存在原材料昂贵、使用溶剂有毒易污染环境、制作步骤复杂、稳定性差、制造工艺复杂等问题,这些都极大地阻碍了双疏材料的实际生产和应用范围。因此,选择原材料成本低、环境友好型溶剂、操作便捷、可重复性高、制备工艺简单的双疏、超双疏表面是亟待解决的问题。
目前,市面上研究最多的材料是具有疏水疏油性能的全氟聚醚硅氧烷体系。专利(申请号201710127998.5)公开了一种超疏水疏油氟碳涂料,组分包括环氧树脂、氟化石墨、碳酸铵、聚氧乙烯醚、有机溶剂a、固化剂和有机溶剂b。该发明还公开了所述超疏水疏油氟碳涂料的制备方法和使用方法。专利(申请号202121114054.2)公开了一种新型UV抗指纹涂料,基材设有防水涂层、高温涂层、抗指纹涂层、硅胶防护涂层等;专利(申请号202110778093.0)公开了一种全氟聚醚硅氧烷化合物的制备方法及抗指纹剂,本发明通过酰氟和含不同数目双键的醇或胺化合物反应,高效的制备一系列含1~4个硅氧烷基团的全氟聚醚硅氧烷化合物。专利(申请号202120378797.4)公开了一种抗指纹的触摸屏面板,包括面框和触摸屏,所述触摸屏上覆盖有防指纹涂层。然而,目前的抗指纹材料多应用于PVC、不锈钢、触摸屏、玻璃等基体上,而在三聚氰胺浸渍纸上尚无应用。且由于三聚氰胺浸渍纸是三聚氰胺树脂经浸渍与纸复合、加热预固化形成,工艺参数和过程复杂,添加助剂极易引起气泡、表面花纹、湿花等质量缺陷,因此目前的抗指纹材料不适用于三聚氰胺浸渍纸。由于行业不同,不锈钢、触摸屏、玻璃等行业人员也无法短时间掌握三聚氰胺浸渍纸生产工艺。
在家具表面装饰中,三聚氰胺浸渍纸(MIP)是人造板行业用量最大的饰面材料之一。用三聚氰胺浸渍纸装饰的人造板(三胺板)在使用、展示和运输过程中很容易被指纹印污染,将具有疏水疏油功能性的组分,添加到三聚氰胺浸渍纸中,不仅使三胺板表面具有抗指纹的效果,而且还具有良好的透光性及手感舒适度。因此,研究一种应用在三聚氰胺浸渍纸上的抗指纹乳液能够提升改善三胺板的美观性和耐用性,增加经济利益。经过抗指纹乳液处理的三聚氰胺浸渍纸可用于家具、地板、墙面、室内装饰、建材等多种场所,具有广阔的应用前景。
发明内容
本发明的目的是提供一种双氟硅型抗指纹乳液的制备方法及其在三聚氰胺浸渍纸中的应用方法。该抗指纹乳液制备工艺简单,具有良好的疏水疏油特性。
具体的,本发明是通过如下技术方案达到的:
本发明通过以下技术手段来实现:
一种双氟硅型抗指纹乳液,按涂料溶质质量与涂料溶剂质量的份数比例来计算,涂料乳液通常包含2-4份的聚全氟乙丙烯(PVDF-HEP)粉体、金属或非金属氧化物纳米粒子,4-6份的复配型全氟烷基硅氧烷与90-94份的无水乙醇,溶质与溶剂在烧杯中充分混合。
进一步明确,所述可广泛用于构筑微纳表面结构的金属/非金属氧化物纳米粒子,来自于高岭土、氧化锡、二氧化钛、氧化铜、氧化硅、碳纳米管等材料中较常见的其中一种或几种,所述纳米粒子的粒径范围为20-40nm。
本发明还提出了上述双氟硅型抗指纹乳液的制备方法,其步骤如下所示:
A、将2-4份的PVDF-HEP粉体、金属或非金属氧化物纳米粒子与90-94份无水乙醇共混,搅拌均匀。
B.使用超声波振荡器对上述乳液进行超声处理,形成分散稳定的纳米粒子乳液,超声时间为5-30min。
C.向超声后的乳液中滴加4-6份复配型全氟烷基硅氧烷,置于磁力搅拌器上搅拌2~5h,使PVDF-HEP粒子与金属、非金属氧化物纳米粒子形成三维结构,以便后期构筑稳定的微纳表面。
进一步明确,所述复配型全氟烷基硅氧烷制备过程为先加入全氟辛基三甲氧基硅,再滴加全氟癸基三乙氧基硅烷并进行磁力搅拌,二者复配比例为1:1-1:3;所述滴加条件为室温搅拌下缓慢滴加。
本发明还提出了上述氟硅型抗指纹乳液在三聚氰胺浸渍纸中的应用方法,其步骤如下所示:
A.用调配的三聚氰胺合成树脂对浸渍纸表面进行预增湿并进行一道浸渍。
B.用调配的三聚氰胺混合树脂进行二道辊涂或喷涂。
C.将双氟硅型抗指纹乳液通过涂刷或喷涂的方式均匀涂布在三聚氰胺浸渍纸表面,涂布量为5-30g/m2。
D.将上述处理过的浸渍纸置于干燥室中进行干燥。
E.冷却后进行检验堆垛并包装入库。
进一步明确,先进行预增湿,再从纸的一面浸入三聚氰胺合成树脂,浸渍量为纸总量的40-50%;在浸透过程中逐渐润湿另一面,排出内部空气,然后再将纸完全浸入三聚氰胺混合树脂中,浸渍量为纸总量的50-60%。
进一步明确,所述三聚氰胺合成树脂的固体含量为55%-56%,合成原料为三聚氰胺树脂、氯化铵、水等。
进一步明确,所述三聚氰胺混合树脂的固体含量为15%-25%,混合原料为三聚氰胺树脂、丙烯酸树脂、水等,三聚氰胺与丙烯酸树脂用量比例为1:1。
进一步明确,所述干燥参数为:温度120~160℃,干燥时间大于5min。
上述制备方法制备的双氟硅型抗指纹乳液。
上述双氟硅型抗指纹乳液制备的三聚氰胺浸渍纸。
与现用生产技术相比,具有如下的技术优势:
本发明提出的双氟硅型抗指纹乳液材料的制备过程步骤较简单,操作十分便捷,均为通过磁力搅拌均匀或采用超声振动分散,危险系数较低,其各步工艺反应操作条件均温和,在各步骤反应过程中的最高温度仅低为接近室温;不仅如此,制备的原材料成本低,生产过程环保。所用的溶剂为无水乙醇,不需要额外的催化剂或助剂,降低了成本,可适应大规模工业生产。该方法所合成的乳液具有良好的分散性,长期储存后轻轻震荡即可恢复为均一乳液形态。
本发明提出的双氟硅型抗指纹乳液的制备流程简单,成本易得,对操作者友好;
本发明提出的双氟硅型抗指纹乳液制备的三聚氰胺浸渍纸疏水疏油性良好,抗指纹能力强。
附图说明
图1为双氟硅型抗指纹乳液的制备方法及其在三聚氰胺浸渍纸中的应用方法流程图。
具体实施方式
下面结合具体的实施案例对本发明做进一步的详细说明,所述是对本发明的解释而非限定。
如图1所示,本发明的合成方法原理为,首先通过PVDF-HEP粉体,金属/非金属氧化物纳米粒子与无水乙醇溶解,混合成纳米粒子乳液,以便后期构建粗糙的三维结构,最后在表面修饰复配型全氟烷基硅氧烷。其中PVDF-HEP粉体、改性金属/非金属纳米粒子可以提供一定的表面粗糙度,复配型全氟烷基硅氧烷可以降低表面自由能,由此可以产生双疏界面,让浸渍纸表面具有抗指纹功能。
实施例1
首先将9ml无水乙醇、0.1gPVDF-HEP粉体、0.06g亲水性SiO2纳米粒子、0.03g疏水SiO2纳米粒子混合,超声分散10min后,得到乳白色稳定悬浮液。超声波功率为240W,超声波频率为40kHz,工作方式为间歇式,工作5min,停止2min。之后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加0.4ml复配型全氟辛基三甲氧基硅烷,再持续磁力搅拌2h。最后,将乳液均匀涂刷在三聚氰胺浸渍纸上,放入烘箱以160°固化10min。取出三聚氰胺浸渍纸,静置半小时,结束制备,得到具有超疏水性能的三聚氰胺浸渍纸。
实施例2
首先将9.4ml无水乙醇、0.2gPVDF-HEP粉体、0.05g疏水SiO2纳米粒子、0.15gSnO2纳米粒子混合,超声分散20min后磁力搅拌1h,得到乳白色稳定悬浮液。超声波功率为240W,超声波频率为40kHz,工作方式为间歇式,工作5min,停止2min。随后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加0.5ml复配型全氟癸基三乙氧基硅烷,再持续磁力搅拌4h,超声20分钟得到均一乳液。最后,用空气压缩喷漆喷涂在三聚氰胺浸渍纸上, 放入烘箱以150°固化10min。取出三聚氰胺浸渍纸,静置半小时,结束制备,得到具有抗指纹性能的三聚氰胺浸渍纸。
实施例3
首先将9ml无水乙醇、0.1gPVDF-HEP粉体、0.15g改性后的SiO2纳米粒子、0.05gSnO2纳米粒子混合,超声分散20分钟后磁力搅拌1小时,得到乳白色稳定悬浮液。超声波功率为240W,超声波频率为40kHz,工作方式为连续超声。随后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加0.6ml复配型全氟癸基三乙氧基硅烷,再超声10min,持续磁力搅拌2h,得到均一乳液。最后,将乳液均匀涂刷在三聚氰胺浸渍原纸上,放入烘箱以 140°固化20min。取出三聚氰胺浸渍纸,再重复涂刷一次,放入烘箱中干燥2h。取出三聚氰胺浸渍纸,静置半小时,结束制备,得到具有抗指纹性能的三聚氰胺浸渍纸。
实施例4
首先将9.4ml无水乙醇、0.2g改性后的SiO2纳米粒子、0.2gPVDF-HEP粉体混合,超声分散5min后得到乳白色稳定悬浮液。超声波功率为240W,超声波频率为40kHz,工作方式为连续超声。随后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加 0.5ml复配型全氟癸基三乙氧基硅烷,再持续磁力搅拌2h,得到均一乳液。最后,将乳液均匀涂刷在三聚氰胺浸渍原纸上,放入烘箱以160°固化5min。取出三聚氰胺浸渍纸,再重复涂刷一次,放入烘箱中干燥20min。取出三聚氰胺浸渍纸,静置10min,结束制备,得到具有抗指纹性能的三聚氰胺浸渍纸。
实施例5
实施例5的抗指纹乳液与实施例4的区别仅在于:加入了4ml三聚氰胺树脂,烘箱固化温度由160°调整为120°,其余组成、制备方法相同。
实施例6
首先将9.2ml无水乙醇、0.1gPVDF-HEP粉体、0.2g改性后的SiO2纳米粒子、0.05gZnO 纳米粒子混合,超声分散10min后得到乳白色稳定悬浮液。纳米粒子粒径均为20-40nm,超声波功率为240W,超声波频率为40kHz,工作方式为连续超声。随后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加0.5ml复配型全氟癸基三乙氧基硅烷,再持续磁力搅拌2h,得到均一乳液。最后,将乳液均匀涂刷在三聚氰胺浸渍原纸上,放入烘箱以140°固化5min。取出三聚氰胺浸渍纸,再重复涂刷一次,放入烘箱中干燥20min。取出三聚氰胺浸渍纸,静置10min,结束制备,得到具有抗指纹性能的三聚氰胺浸渍纸。
实施例7
首先将9.4ml无水乙醇、0.29g改性后的SiO2纳米粒子、0.05gPVDF-HEP粉体混合,超声分散10min后得到乳白色稳定悬浮液。纳米粒子粒径均为20-40nm,超声波功率为240W,超声波频率为40kHz,工作方式为连续超声。随后,将悬浮液置于磁力搅拌器上室温条件下搅拌,搅拌过程中滴加0.5ml复配型全氟癸基三乙氧基硅烷,再持续磁力搅拌2h,得到均一乳液。最后,用空气压缩喷漆喷涂在三聚氰胺浸渍原纸上,放入烘箱以130°固化10min。取出三聚氰胺浸渍纸,再重复喷涂一次,放入烘箱中干燥5min。取出三聚氰胺浸渍纸,结束制备,得到具有抗指纹性能的三聚氰胺浸渍纸。
Claims (3)
1.本发明的主要内容是:制备双氟硅型抗指纹乳液并用其对三聚氰胺浸渍纸进行涂刷或喷涂工艺后干燥,干燥温度为120~160℃。所述双氟硅型抗指纹乳液包含2-4份聚全氟乙丙烯(PVDF-HEP)粉体、金属或非金属氧化物纳米粒子,4-6份复配型全氟烷基硅氧烷与90-94份无水乙醇;所述金属或非金属氧化物纳米粒子为高岭土、氧化锡、二氧化钛、氧化铜、氧化硅、碳纳米管中的一种或几种,所述纳米粒子粒径为20-40nm;
所述双氟硅型抗指纹乳液的制备方法步骤包括:
A、将2-4份的PVDF-HEP粉体、金属或非金属氧化物纳米粒子与90-94份无水乙醇共混,搅拌均匀;
B.使用超声波振荡器对上述乳液进行超声处理,形成分散稳定的纳米粒子乳液,超声时间为5-30min;
C.向超声后的乳液中滴加4-6份复配型全氟烷基硅氧烷,置于磁力搅拌器上搅拌2~5h,使PVDF-HEP粒子与金属、非金属氧化物纳米粒子形成三维结构,以便后期构筑稳定的微纳表面。
2.根据权利要求1所述双氟硅型抗指纹乳液的制备方法步骤,其特征在于:所述复配型全氟烷基硅氧烷制备过程为先加入全氟辛基三甲氧基硅,再滴加全氟癸基三乙氧基硅烷并进行磁力搅拌,二者复配比例为1:1-1:3;所述滴加条件为室温搅拌下缓慢滴加。
3.所述双氟硅型抗指纹乳液在三聚氰胺浸渍纸中的应用方法,其主要步骤如下:
A.将双氟硅型抗指纹乳液通过涂刷或喷涂的方式均匀涂布在三聚氰胺浸渍纸表面,涂布量为5-30g/m2;
B.将上述处理的浸渍纸置于干燥室进行干燥;
C.冷却后检验堆垛并包装入库。
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