CN113818247A - 一种超双疏型材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种超双疏型材料及其制备方法,属于功能材料领域。本发明所述制备超双疏材料的方法,包括(1)将聚四氟乙烯、纳米二氧化硅、溶剂混合均匀,得到溶液A;(2)将全氟己基乙基甲基丙烯酸酯、二环己基碳二亚胺、十三氟辛基三乙氧基硅烷、溶剂混合均匀,得到溶液B;(3)溶液A和溶液B混合均匀,得到溶液C;(4)采用溶液C对基材进行处理,得到处理后的基材;(5)将3‑三聚环氧六氟丙烷酰胺基丙基甜菜碱、硅油、溶剂混合均匀,之后加入分散剂、偶联剂、固化剂,继续混合,得到溶液D;(6)采用溶液D对步骤(4)的基材进行处理,得到超双疏材料。本发明的超双疏材料的水和油接触角均达到150°以上。
Description
技术领域
本发明涉及一种超双疏型材料及其制备方法,属于功能材料领域。
背景技术
市场上的多数面料存在容易被水润湿、沾染油污、沾污后洗涤困难等问题,比如:宴会时红酒洒在浅色衬衫上、下大雨时衣服被雨水打湿、衣服的袖口和领口很容易弄脏等,这就导致面料打理费时费力、洗涤用水量大,而且洗涤剂过多使用会污染环境。随着生活水平的提高,消费者对纺织面料的防水、防油、易去污面料提出前所未有的高要求。
双疏(疏水疏油)表面由于具有非常低的表面能,所以在自清洁、油水分离、防污、防雾、防结冰、减阻、有机液体运输、防腐蚀等方面表现出了优异的性能,通过双疏表面整理的织物具有多种应用,例如医用制服、包装、时装、极限运动服和军用装备。
目前,研究者采用化学方法制备超疏水/超疏油的双疏表面,如模板法、光刻法、沉积法、静电纺丝、溶胶-凝胶法等,通过制造微纳米级的粗糙度和降低表面能来实现的;但是这些制备方法复杂、成本昂贵,依赖于特殊的基材等问题,使得超双疏表面的应用范围狭窄,投入市场的产品并不多。
因此,亟需一种能够在各种基材上适用、制备方法简单易行的超疏水/超疏油材料。
发明内容
[技术问题]
目前,超双疏(疏水疏油)材料的制备存在制备方法复杂、适用范围小、耐水洗效果差的问题。
[技术方案]
为了解决上述至少一个问题,本发明采用不同的溶液分批整理基材之后,在不改变材料原有性能的同时改善了疏水疏油性能,使基材的应用范围更加广泛。
本发明的第一个目的是提供一种制备超双疏材料的方法,包括如下步骤:
(1)将聚四氟乙烯14-17份、纳米二氧化硅8-11份、溶剂80-100份混合均匀,得到溶液A;
(2)将全氟己基乙基甲基丙烯酸酯(CAS:2144-53-8)9-10份、二环己基碳二亚胺6-9份、十三氟辛基三乙氧基硅烷6-7份、溶剂80-100份混合均匀,得到溶液B;
(3)将步骤(1)的溶液A和步骤(2)的溶液B按照体积比1:1-3混合均匀,得到溶液C;
(4)采用步骤(3)的溶液C对基材进行处理,使得溶液C均匀的涂覆在基材表面,干燥,得到第一步处理的基材;
(5)将3-三聚环氧六氟丙烷酰胺基丙基甜菜碱5-6份、硅油12-15份、溶剂80-100份混合均匀,之后加入分散剂2-3份、偶联剂2-3份、固化剂4-7份,继续混合,得到溶液D;
(6)采用步骤(5)的溶液D对步骤(4)所述的第一步处理的基材进行处理,使得溶液D均匀的涂覆在基材表面,干燥,得到所述的超双疏材料。
在本发明的一种实施方式中,所述方法中所有的份数为质量份数。
在本发明的一种实施方式中,步骤(1)所述的混合均匀是在20-30℃、300-600rpm下搅拌10-20分钟。
在本发明的一种实施方式中,步骤(2)所述的混合均匀是在20-30℃、400-800rpm下搅拌10-20分钟。
在本发明的一种实施方式中,步骤(3)所述的混合均匀是在20-30℃、1000-1500rpm下搅拌3-5分钟。
在本发明的一种实施方式中,步骤(4)所述处理是采用浸渍、刷涂、喷涂的方法使得溶液C均匀的涂覆在基材表面;其中浸渍是在20-30℃下浸渍10-20分钟;刷涂、喷涂的用量为100-200g/m2。
在本发明的一种实施方式中,步骤(4)所述基材包括织物、金属片、木材、玻璃;所述的织物包括棉织物、涤纶织物;所述的金属片包括铜片。
在本发明的一种实施方式中,步骤(5)所述的混合均匀是在20-30℃、400-800rpm下搅拌10-20分钟。
在本发明的一种实施方式中,步骤(5)所述的继续混合是在20-30℃、1000-1500rpm下搅拌3-5分钟。
在本发明的一种实施方式中,步骤(5)所述的固化剂为乙烯基三胺DETA、间苯二胺、氨乙基哌嗪中的一种或者两种。
在本发明的一种实施方式中,步骤(5)所述的偶联剂为3-三乙氧基甲硅烷基-1-丙胺、γ-缩水甘油醚氧丙基三甲氧基硅烷、全氟丁基磺酰氟中的一种或者几种。
在本发明的一种实施方式中,步骤(5)所述的分散剂为硬脂酸单甘油酯、三乙醇胺中的一种或者两种。
在本发明的一种实施方式中,步骤(1)、步骤(2)和步骤(5)所述的溶剂为水、乙醇中的一种或者两种。
在本发明的一种实施方式中,步骤(6)所述处理是采用浸渍、刷涂、喷涂的方法使得溶液D均匀的涂覆在基材表面;其中浸渍是在20-30℃下浸渍10-20分钟;刷涂、喷涂的用量为100-200g/m2。
本发明的第二个目的是本发明所述的方法制备得到的超双疏材料。
本发明的第三个目的是本发明所述的超双疏材料在特种用品中的应用。
[有益效果]
本发明采用的各个原料之间具有协同作用,使得制备得到的超双疏材料的水接触角和油接触角均达到150°以上,而且水洗50次和摩擦1000次后其水接触角和油接触角还能达到150°以上,具有很广泛的市场前景。
具体实施方式
以下对本发明的优选实施例进行说明,应当理解实施例是为了更好地解释本发明,不用于限制本发明。
实施例中采用的棉织物为纯棉机织布(C14.5 tex×C14.5 tex,133根/10cm×172根/10cm);
实施例中提及的份数均为质量份数。
测试方法:
静态接触角测试:将布样置于载玻片上,滴加10μL去离子水或丙三醇(油),利用接触角测量仪(德国Kruss公司,DSA25)测量水滴静态接触角。每个样品测试6个不同位点,并取其平均值。
耐水洗性能测试:根据AATCC Test Method 61-2003标准对织物的耐水洗性能进行测试,每次洗涤时间为15min,洗涤温度为40℃,采用的洗涤剂为ECE无磷标准洗涤剂,1个洗涤循环相当于5个日常家庭洗涤循环。
耐摩擦性能:根据GB/T 21196.2—2007《马丁代尔法织物耐磨性的测定第2部分:试样破损的测定》进行测试。
实施例1
一种制备超双疏材料的方法,包括如下步骤:
(1)将聚四氟乙烯16份、纳米二氧化硅10份、水80份在25℃、500rpm下搅拌20分钟,混合均匀,得到溶液A;
(2)将全氟己基乙基甲基丙烯酸酯10份、二环己基碳二亚胺8份、十三氟辛基三乙氧基硅烷7份、水95份在25℃、700rpm下搅拌15分钟,混合均匀,得到溶液B;
(3)将步骤(1)的溶液A和步骤(2)的溶液B按照体积比1:1,在25℃、1000rpm下搅拌5分钟,混合均匀,得到溶液C;
(4)将棉织物在步骤(3)的溶液C中25℃浸渍10min,使得溶液C均匀的涂覆在基材表面,干燥,得到第一步处理的棉织物;
(5)将3-三聚环氧六氟丙烷酰胺基丙基甜菜碱6份、硅油14份、水95份在25℃、800rpm下搅拌20分钟混合均匀,之后加入硬脂酸单甘油酯3份、3-三乙氧基甲硅烷基-1-丙胺3份、氨乙基哌嗪6份,在25℃、1500rpm下搅拌4分钟,得到溶液D;
(6)将步骤(4)所述的第一步处理的棉织物在步骤(5)的溶液D中25℃浸渍10min,使得溶液D均匀的涂覆在基材表面,干燥,得到所述的超双疏棉织物。
对照例1
省略实施例1中的步骤(5)和(6),其他和实施例1保持一致,得到第一步处理的棉织物。
对照例2
省略步骤(1),将棉织物直接浸渍在步骤(2)的溶液B中,其他和实施例1保持一致,得到棉织物。
对照例3
省略步骤(2),将棉织物直接浸渍在步骤(1)的溶液A中,其他和实施例1保持一致,得到棉织物。
对照例4
将棉织物直接浸渍在实施例1的步骤(5)的溶液D中,干燥,得到棉织物。
对照例5
将棉织物直接浸渍在实施例1的步骤(2)的溶液B中,干燥,得到棉织物。
对照例6
将棉织物直接浸渍在实施例1的步骤(1)的溶液A中,干燥,得到棉织物。
对照例7
将实施例1中所有的原料一起混合,在25℃、1000rpm下搅拌20分钟,得到棉织物。
对照例8
将实施例1步骤(1)和(2)中所有的原料一起混合,在25℃、1000rpm下搅拌20分钟;之后按照实施例1步骤(4)-(6)进行,得到棉织物。
将实施例1和对照例1-8得到的棉织物进行性能测试,测试结果如下:
表1施例1和对照例1-8的测试结果
注:表中的“水洗后”是50次水洗后;“摩擦后”是砂轮摩擦1000次之后;接触角是静态接触角。
对照例9
调整实施例1步骤(2)中的十三氟辛基三乙氧基硅烷为全氟己基乙基甲基丙烯酸酯;其他和实施例1保持一致,得到棉织物。
对照例10
调整实施例1步骤(5)中的聚四氟乙烯为纳米二氧化硅;其他和实施例1保持一致,得到棉织物。
对照例11
调整实施例1步骤(5)中的硅油为3-三聚环氧六氟丙烷酰胺基丙基甜菜碱;其他和实施例1保持一致,得到棉织物。
对照例12
调整实施例1步骤(5)中的纳米二氧化硅为聚四氟乙烯;其他和实施例1保持一致,得到棉织物。
对照例13
调整实施例1步骤(5)中的3-三聚环氧六氟丙烷酰胺基丙基甜菜碱为3-三聚环氧六氟丙烷酰胺基丙基(2-亚硫酸)乙基二甲基铵;其他和实施例1保持一致,得到超双疏棉织物。
对照例14
调整实施例1步骤(2)中的十三氟辛基三乙氧基硅烷为氟丙基三氯硅烷;其他和实施例1保持一致,得到超双疏棉织物。
将对照例9-14得到的棉织物进行性能测试,测试结果如下:
表2对照例9-14的测试结果
例 | 水接触角/° | 油接触角/° |
原布 | 0 | 0 |
实施例1 | 163.8 | 157.6 |
对照例9 | 136.7 | 132.4 |
对照例10 | 134.5 | 133.2 |
对照例11 | 140.1 | 139.5 |
对照例12 | 138.8 | 135.6 |
对照例13 | 137.6 | 136.8 |
对照例14 | 141.2 | 138.3 |
注:表中的“水洗后”是50次水洗后;“摩擦后”是砂轮摩擦1000次之后;接触角是静态接触角。
实施例2
调整实施例1的棉织物为铜片、玻璃,其他和实施例1保持一致,得到超双疏的材料。
将得到的超双疏的材料进行性能测试,测试结果如下:
表3实施例2的测试结果
基材 | 水接触角/° | 油接触角/° |
铜片 | 164.7 | 159.3 |
玻璃 | 162.6 | 158.1 |
实施例3
一种制备超双疏材料的方法,包括如下步骤:
(1)将聚四氟乙烯14份、纳米二氧化硅8份、水80份在25℃、500rpm下搅拌20分钟,混合均匀,得到溶液A;
(2)将全氟己基乙基甲基丙烯酸酯9份、二环己基碳二亚胺6份、十三氟辛基三乙氧基硅烷6份、水95份在25℃、700rpm下搅拌15分钟,混合均匀,得到溶液B;
(3)将步骤(1)的溶液A和步骤(2)的溶液B按照体积比1:1,在25℃、1000rpm下搅拌5分钟,混合均匀,得到溶液C;
(4)将棉织物在步骤(3)的溶液C中25℃浸渍10min,使得溶液C均匀的涂覆在基材表面,干燥,得到第一步处理的棉织物;
(5)将3-三聚环氧六氟丙烷酰胺基丙基甜菜碱5份、硅油12份、水95份在25℃、800rpm下搅拌20分钟混合均匀,之后加入硬脂酸单甘油酯2份、3-三乙氧基甲硅烷基-1-丙胺2份、氨乙基哌嗪4份,在25℃、1500rpm下搅拌4分钟,得到溶液D;
(6)将步骤(4)所述的第一步处理的棉织物在步骤(5)的溶液D中25℃浸渍10min,使得溶液D均匀的涂覆在基材表面,干燥,得到所述的超双疏棉织物。
实施例4
一种制备超双疏材料的方法,包括如下步骤:
(1)将聚四氟乙烯17份、纳米二氧化硅11份、水90份在25℃、500rpm下搅拌20分钟,混合均匀,得到溶液A;
(2)将全氟己基乙基甲基丙烯酸酯10份、二环己基碳二亚胺9份、十三氟辛基三乙氧基硅烷7份、水95份在25℃、700rpm下搅拌15分钟,混合均匀,得到溶液B;
(3)将步骤(1)的溶液A和步骤(2)的溶液B按照体积比1:1,在25℃、1000rpm下搅拌5分钟,混合均匀,得到溶液C;
(4)将棉织物在步骤(3)的溶液C中25℃浸渍10min,使得溶液C均匀的涂覆在基材表面,干燥,得到第一步处理的棉织物;
(5)将3-三聚环氧六氟丙烷酰胺基丙基甜菜碱6份、硅油15份、水95份在25℃、800rpm下搅拌20分钟混合均匀,之后加入硬脂酸单甘油酯3份、3-三乙氧基甲硅烷基-1-丙胺3份、氨乙基哌嗪7份,在25℃、1500rpm下搅拌4分钟,得到溶液D;
(6)将步骤(4)所述的第一步处理的棉织物在步骤(5)的溶液D中25℃浸渍10min,使得溶液D均匀的涂覆在基材表面,干燥,得到所述的超双疏棉织物。
将得到的超双疏的材料进行性能测试,测试结果如下:
表4实施例4的测试结果
例 | 水接触角/° | 油接触角/° |
实施例3 | 154.3 | 150.1 |
实施例4 | 159.9 | 155.3 |
本发明采用的聚四氟乙烯具有抗酸抗碱、抗各种有机溶剂的特点,同时具有耐高温的特点,它的摩擦系数极低,有较好的疏水性;纳米二氧化硅除了提供疏水疏油性能外,还可以改善涂料悬浮稳定性差、触变性差、耐候性差、耐洗刷性差等问题,使涂膜与金属结合强度大幅提高,涂膜硬度增加,表面自洁能力也获得改善;全氟己基乙基甲基丙烯酸酯和二环己基碳二亚胺都在一定程度上起到了疏水疏油的效果,在本发明中复配使用进一步提升了超疏水超疏油性能,十三氟辛基三乙氧基硅烷的分子能渗透至坚硬、多空隙的无机结构类基材内达几毫米,从而达到深层次的长期的憎水防污保护,并且其形成的防水防污保护层是完全看不见的,不会导致基材光学上的损害;3-三聚环氧六氟丙烷酰胺基丙基甜菜碱,其特点是化学性能稳定,在强酸强碱条件下都具有很高的表面活性,可以与其他材料起到协同增效的作用,硅油在本发明中作添加剂,并有优良的疏水疏油效果。
Claims (10)
1.一种制备超双疏材料的方法,其特征在于,包括如下步骤:
(1)将聚四氟乙烯14-17份、纳米二氧化硅8-11份、溶剂80-100份混合均匀,得到溶液A;
(2)将全氟己基乙基甲基丙烯酸酯9-10份、二环己基碳二亚胺6-9份、十三氟辛基三乙氧基硅烷6-7份、溶剂80-100份混合均匀,得到溶液B;
(3)将步骤(1)的溶液A和步骤(2)的溶液B按照体积比1:1-3混合均匀,得到溶液C;
(4)采用步骤(3)的溶液C对基材进行处理,使得溶液C均匀的涂覆在基材表面,干燥,得到第一步处理的基材;
(5)将3-三聚环氧六氟丙烷酰胺基丙基甜菜碱5-6份、硅油12-15份、溶剂80-100份混合均匀,之后加入分散剂2-3份、偶联剂2-3份、固化剂4-7份,继续混合,得到溶液D;
(6)采用步骤(5)的溶液D对步骤(4)所述的第一步处理的基材进行处理,使得溶液D均匀的涂覆在基材表面,干燥,得到所述的超双疏材料。
2.根据权利要求1所述的方法,其特征在于,所述方法中所有的份数为质量份数。
3.根据权利要求1所述的方法,其特征在于,步骤(4)所述基材包括织物、金属片、木材、玻璃;所述的织物包括棉织物、涤纶织物;所述的金属片包括铜片。
4.根据权利要求1所述的方法,其特征在于,步骤(5)所述的偶联剂为3-三乙氧基甲硅烷基-1-丙胺、γ-缩水甘油醚氧丙基三甲氧基硅烷、全氟丁基磺酰氟中的一种或者几种。
5.根据权利要求1所述的方法,其特征在于,步骤(1)、步骤(2)和步骤(5)所述的溶剂为水、乙醇中的一种或者两种。
6.根据权利要求1所述的方法,其特征在于,步骤(1)所述的混合均匀是在20-30℃、300-600rpm下搅拌10-20分钟。
7.根据权利要求1所述的方法,其特征在于,步骤(2)所述的混合均匀是在20-30℃、400-800rpm下搅拌10-20分钟。
8.根据权利要求1所述的方法,其特征在于,步骤(3)所述的混合均匀是在20-30℃、1000-1500rpm下搅拌3-5分钟。
9.权利要求1-8任一项所述的方法制备得到的超双疏材料。
10.权利要求9所述的超双疏材料在特种用品中的应用。
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CN106458649A (zh) * | 2014-03-21 | 2017-02-22 | 通用电气公司 | 用于水处理的抗污垢膜 |
CN109233482A (zh) * | 2018-09-14 | 2019-01-18 | 河北工业大学 | 一种水性体系超双疏耐久涂层的制备方法 |
CN110144593A (zh) * | 2019-06-28 | 2019-08-20 | 上海市第一人民医院 | 一种具有超疏水疏油性能的含氟纳米聚合物修饰镍钛合金材料及其制备方法 |
CN112831241A (zh) * | 2021-02-18 | 2021-05-25 | 华东理工大学 | 一种超疏水超疏油环氧树脂涂料及其制备方法 |
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