CN109234910B - 拒水亲油复合针刺无纺布及其制备方法 - Google Patents

拒水亲油复合针刺无纺布及其制备方法 Download PDF

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CN109234910B
CN109234910B CN201810897693.7A CN201810897693A CN109234910B CN 109234910 B CN109234910 B CN 109234910B CN 201810897693 A CN201810897693 A CN 201810897693A CN 109234910 B CN109234910 B CN 109234910B
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water repellent
water
nonwoven fabric
preparation
fiber
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CN109234910A (zh
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赵荟菁
张迎梅
董伊航
章梦雪
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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Priority to US16/606,755 priority patent/US11473238B2/en
Priority to PCT/CN2018/100820 priority patent/WO2020029315A1/zh
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Abstract

本发明涉及一种拒水亲油复合针刺无纺布及其制备方法，包括以下步骤：将PET纤维与聚烯烃类纤维按照质量比为3:1‑1:3进行共混，经针刺得到复合针刺无纺布；将复合针刺无纺布在110‑160℃下进行热烘处理，处理时间为40‑90min；采用浓度为50‑70mL/L的改性树脂类无氟防水剂水溶液对热烘处理过的织物进行浸轧拒水整理，浸轧拒水整理的气压为1.8kPa，带液率为160％‑230％，烘干后得到拒水亲油复合针刺无纺布。本发明的制备方法简单，相对于处理前的织物，所制备的复合针刺无纺布的拒水性、亲油性、拉伸强度得到明显提升。

Description

拒水亲油复合针刺无纺布及其制备方法
技术领域
本发明涉及纺织品整理技术领域，尤其涉及一种拒水亲油复合针刺无纺布及其制备方法。
背景技术
随着科技的发展，原油泄漏和工厂含油废水排放对海洋、河流环境造成了很大的影响，对人类环境造成威胁。拒水亲油材料具有特殊的润湿性能，能够吸收水分中的油性液体，但不吸收多余的水分，造成水油分离，从而能够起到净化水源的作用。
利用拒水亲油材料来处理油污问题是一种低成本高效率的方法，以纺织品为基底构建拒水亲油表面，增加了纺织品的应用价值。近年来非织造技术发展势头突飞猛进，相比传统织造方法而言，其制备工艺流程简单，生产速度快且产量高。合成纤维大分子主链上主要是亲油性的有机基团，缺乏一定数量的亲水基团，与各类油性分子有较好的相似相溶性，具有一定的疏水性和亲油性。
中国专利CN102953268A公开了一种超亲油超疏水油水分离涤纶纺织品的制备方法，虽然使用了无氟防水剂对织物进行处理，但其制备方法操作复杂，且纺织品的拉伸强度在处理后并没有得到提高。中国文献“改性MBPP/拒水PET复合吸油材料的制备及性能研究，王丹等，产业用纺织品，2016，(1)：6-11，44”公开了基于PET的复合吸油材料的制备方法，虽然也使用了无氟防水剂对织物进行处理，但是该方法所制备的复合材料在重复使用时，吸油率仍不理想，且织物的强力没有得到明显提高。
目前，利用拒水亲油材料来处理油污问题仍处于研发阶段，因此现有的拒水亲油产品依然具有一定的问题，比如生产工艺流程复杂、产品综合性能不佳、油水分离效率低、产品成本高、吸收能力差等缺点，尤其是在亲油的过程中进行拒水处理往往容易发生水分吸收过多或过少的情况。
发明内容
为解决上述技术问题，本发明的目的是提供一种拒水亲油复合针刺无纺布及其制备方法，制备方法简单，相对于处理前的织物，所制备的复合针刺无纺布的拒水性、亲油性、拉伸强度得到明显提升。
在一方面，本发明提供了一种拒水亲油复合针刺无纺布的制备方法，包括以下步骤：
(1)将PET纤维与聚烯烃类纤维按照质量比为3:1-1:3进行共混，经针刺得到复合针刺无纺布；
(2)将复合针刺无纺布在110-160℃下进行热烘处理，处理时间为40-90min；
(3)采用浓度为50-70mL/L的改性树脂类无氟防水剂水溶液对热烘处理过的织物进行浸轧拒水整理，浸轧拒水整理的气压为1.8kPa，带液率为160％-230％，烘干后得到拒水亲油复合针刺无纺布。
进一步地，在步骤(1)中，聚烯烃类纤维为聚乙烯(PE)纤维、聚丙烯(PP)纤维和ES纤维(聚乙烯-聚丙烯复合纤维)中的一种或几种。优选地，聚烯烃类纤维为ES纤维。
本发明中，所使用的PET(聚酯)纤维由对苯二甲酸乙二醇酯聚合后得来，对苯二甲酸乙二醇酯的结构式为ES纤维由聚乙烯和聚丙烯(聚乙烯和聚丙烯分别由单体聚合得来)接枝后得来。PET和ES双组份纤维都属于合成纤维，吸湿性差，聚酯单体、聚丙烯、聚乙烯，都是大分子的非极性结构，结晶度高，不含亲水基团，故有一定的拒水效果。且ES双组份纤维有独特的热粘合特性，在热处理条件下可与其他材料发生粘合，形成纤维增强材料。
优选地，在步骤(1)中，PET纤维与聚烯烃类纤维的质量比为3:1、1:1或1:3。
进一步地，在步骤(1)中，采用针刺工艺对共混的纤维进行加工，得到复合针刺无纺布。复合针刺无纺布表面本身呈现一定的粗糙度。针刺工艺包括以下步骤：
将PET纤维与聚烯烃类纤维开松混合，然后梳理成网，铺网后进行预针刺，然后将预针刺后的面料对叠进行主针刺。
优选地，在步骤(2)中，热烘处理温度为120-130℃，热烘处理时间为60-70min。
通过步骤(2)的热烘处理，ES热熔性纤维、PE纤维或PP纤维的表面发生变化，不仅能够增大无纺布的力学性能，而且也可以使无氟防水剂更加均匀的分散，改善其拒水性能。
进一步地，在步骤(3)中，改性树脂类无氟防水剂为阳离子改性树脂类无氟防水剂，所述改性树脂类无氟防水剂的pH值为3.5-4.5。
进一步地，在步骤(3)中，改性树脂类无氟防水剂为ECO-0C无氟防水剂。拒水整理时选用的ECO-0C无氟防水剂是不含有氟系的绿色环保型单防整理剂，无氟防水剂能降低织物的表面张力，使其表面张力低于水而高于油，因此无氟防水剂只能赋予织物防水功能，而对其亲油功能并无影响。
进一步地，在步骤(3)中，改性树脂类无氟防水剂与织物的浴比为10:1-20:1。
进一步地，在步骤(3)中，采用二浸二轧法进行浸轧拒水整理。
优选地，在步骤(3)中，带液率为200％-230％。
进一步地，在步骤(3)中，烘干温度为60-90℃。
从改变接触角角度出发，构建拒水亲油材料需具备两个条件，即材料表面的微纳米级的粗糙结构和低表面能。根据Wenzel理论，对于具有疏水性且水滴的本征接触角大于90°的表面，粗糙度增大，则接触角越大，拒水性能越好；若在同一表面，油的本征接触角小于90°，则粗糙度增大后，油滴的接触角接近为0°，说明该表面的亲油性越好。
本文用无氟防水剂对复合针刺无纺布进行拒水整理，通过在纤维表面涂覆低表面能的无氟防水剂和对纤维之间的空隙进行填充从而降低无纺布的表面张力获得一定的拒水效果。PET和ES/PE/PP纤维本身吸湿性差，PET除了两端的醇羟基之外无其它极性基团，ES双组份纤维中，无论是聚丙烯还是聚乙烯，都是大分子的非极性结构，结晶度高，不含亲水基团，具有一定的拒水效果。经无氟防水剂整理后，复合针刺无纺布的纤维与纤维交叉处、纤维表面涂覆有无氟防水剂，增强了其拒水效果。
在另一方面，本发明还提供了一种采用上述制备方法所制备的拒水亲油复合针刺无纺布，拒水亲油复合针刺无纺布的水接触角为120-150°，每克复合针刺无纺布可吸油3.2-4.4g。
借由上述方案，本发明至少具有以下优点：
(1)本发明在制备复合针刺无纺布时，PET纤维和ES/PE/PP纤维都属于疏水性纤维，所制得的复合针刺无纺布有完整的外观形貌，PET纤维和聚烯烃类纤维有效地缠结在一起，无氟防水剂附着在纤维上，起到防止纤维吸水的作用。
(2)在拒水处理后，由于密度增大，材料的拉伸强度会有所提升。热烘处理后，强度变化明显，混有ES纤维原料的无纺布的拉伸强度增加。
(3)在对无纺布进行拒水处理后，材料的接触角明显增大。且当PET纤维和ES纤维共混比为1:1，无氟防水剂浓度为70mL/L时，拒水性能最好。在拒水性能较好的情况下，热烘处理对无纺布吸油率和接触角均有一定的增强效果。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是未经过热烘处理但经过拒水整理后所制备的产物在不同放大倍数下的电镜图；
图2是经过热烘处理且经过拒水整理后所制备的产物在不同放大倍数下的电镜图；
图3是采用70mL/L无氟防水剂，对未经热烘处理后的织物整理前后材料接触角照片；
图4为无氟防水剂整理浓度对接触角的影响结果测试图；
图5为经热烘处理后，再对无纺布用无氟防水剂拒水整理后织物的接触角测试结果；
图6为经过热烘处理所制备的针刺无纺布的吸油率测试结果；
图7为经热烘处理和未经热烘处理的拒水无纺布的吸油率测试结果。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
本发明以下实施例中，所使用的PET纤维、ES纤维均为市购；无氟防水剂(ECO-0C)，浙江福尔普生新型材料有限公司生产，其pH值为3.5-4.5；所用的含油废水的具体制备方法为：先将1000mL去离子水倒入烧杯中，然后缓缓倒入250mL煤油，用磁力搅拌器在60r/min下搅拌10分钟后静置30分钟，使水油混合，得到含油废水。
所使用的仪器型号如下：
针刺生产线(万龙机械有限公司，常熟，中国)，万能材料试验机(Instron5967试验机，美国，英斯特朗公司)，全自动视频接触角测试仪(OCA50，Dataphysics，德国)，台式电镜(TM3030，Hitachi，日本)，磁力搅拌器(84-1，上海梅颖浦仪器仪表制造有限公司，中国)，电子天平(Adventurer，奥豪斯仪器有限公司，德国)，烘箱(型号WGLL-125BE，天津市泰斯特仪器有限公司)
实施例1
(1)PET/ES针刺无纺布的制备：按质量比为3:1充分混合PET纤维和ES纤维，然后采用针刺工艺对共混的纤维进行加工，针刺工艺流程：PET/ES开松混合→梳理成网→铺网机→预针刺→主针刺，即得到PET/ES针刺无纺布。为了增加无纺布的强力，将预针刺过后的材料对叠进行主针刺，电源频率设置为13Hz。
(2)取部分步骤(1)制备的PET/ES针刺无纺布进行热烘处理，将样品放入烘箱中，在温度为120℃条件下热烘处理60分钟。
(3)然后用浓度为50mL/L的无氟防水剂水溶液对经过热烘处理的样品进行拒水处理，无氟防水剂水溶液与样品的浴比为10:1-20:1，拒水整理工艺流程：PET/ES针刺无纺布→二浸二轧(将样品在无氟防水剂水溶液中浸泡30秒使样品充分浸湿，台式轧车上气压值设置为1.8kPa，带液率为230％)→于烘箱中60℃烘干，即得到拒水亲油复合针刺无纺布。
实施例2
按照实施例1的方法制备拒水亲油复合针刺无纺布，不同之处在于，在步骤(1)中，PET纤维和ES纤维的质量比为1:1。
实施例3
按照实施例1的方法制备拒水亲油复合针刺无纺布，不同之处在于，在步骤(1)中，PET纤维和ES纤维的质量比为1:3。
实施例4
按照实施例1-3的方法制备出3种拒水亲油复合针刺无纺布，不同之处在于，在步骤(3)中，无氟防水剂水溶液的浓度为60mL/L。
实施例5
按照实施例1-3的方法制备出3种拒水亲油复合针刺无纺布，不同之处在于，在步骤(3)中，无氟防水剂水溶液的浓度为70mL/L。
对比例1
为了作为对照，按照实施例1-5的方法制备5组对照样，不同之处在于，将步骤(1)中所使用的ES纤维换为等质量的PET，即ES:PET＝0:4。
对比例2
为了作为对照，按照实施例1-5的方法制备5组对照样，不同之处在于，将步骤(1)中所使用的PET纤维换为等质量的ES，即PET:ES＝0:4。
对比例3
为了作为对照，按照实施例1-5的方法制备对照样，不同之处在于，省略步骤(2)的热烘处理步骤。
以上实施例所制得的拒水亲油PET/ES针刺无纺布的克重为390～750g/m2，厚度均在6mm左右，采用台式电镜对所制备的样品中的纤维形貌进行观察，选择PET:ES＝1:1所制备的样品对观察对象，图1a、b分别为未经过热烘处理但经过拒水整理后所制备的产物在不同放大倍数下的电镜图；图2a、b分别为经过热烘处理且经过拒水整理后所制备的产物在不同放大倍数下的电镜图。如图1-2所示，PET和ES纤维有效地缠结在一起，且纤维形貌清晰完整，有些许断裂现象，经过120℃热烘处理的无纺布表面无明显差别。无氟防水剂附着在纤维上并且纤维之间仍然存在大的孔隙，良好分散的无氟聚合物表现为覆盖物并防止纤维吸水。由于产品厚度、密度、热风温度等影响，图1-2中可看出部分ES热熔纤维产生粘合现象。
在现实生活中，工业废水废油、印刷废水、石油溢油等是环境污染的主要污染源，油水分离材料的主要任务就是解决这类污染物，然而需进一步提高油水分离材料的机械稳定性、耐久性等使其适用于各种恶劣环境中的使用。因此，样品的拉伸性能十分关键。
对以上实施例和对比例制备的产品进行拉伸测试，结果如表1所示，表中断裂强力的单位为N，表中灰色阴影部分为热烘后再经拒水整理的PET/ES针刺无纺布的断裂强力(N)的数值)。
从表1可看出，当PET/ES针刺无纺布进行热烘处理后，将热烘处理后的材料的强度与未处理的材料强度比较时发现，无纺布在先热烘处理后再拒水整理后的拉伸强度与只经过拒水处理的拉伸强度有明显不同，且PET:ES＝3:1、1:1和1:3时，拉伸强度均得到提高。当PET纤维与ES纤维比例相同时，先经过热烘处理后再拒水整理的无纺布的断裂强力和断裂伸长率普遍大于只经过拒水整理的无纺布。PET纤维与ES纤维比例不同对无纺布的强度没有明显影响，热烘干燥使具有ES纤维的无纺布的力学性能得到改性，增强了纤维强度，且当PET/ES比例为1:1时，热烘对强度影响明显。ES纤维本身具有的独特的受热后强度增大的特点，使得具有ES纤维的无纺布拉伸性能更加显著。
表1PET/ES不同比例及不同防水剂浓度对PET/ES针刺无纺布断裂强力的影响
一般来说，当水的接触角大于150°且接触角滞后小的表面被称为超疏水表面，接触角是判断无纺布润湿性能的指标，接触角越大，无纺布润湿性能越差，即无纺布的吸水性越差，拒水性增强。当水的接触角到达135°时，无纺布便具有一个良好的拒水性能。
图3a、b分别为采用70mL/L无氟防水剂，对未经热烘处理后的织物整理前、整理后材料接触角照片(PET:ES＝1:1)。由图片可以看出，当水滴落在拒水处理后的无纺布上时，接触角都较大，织物没有将水滴吸收(图3b)。而在无处理的无纺布上滴下水滴时，接触角明显小于经过拒水处理后的无纺布的接触角(图3a)。图4为无氟防水剂整理浓度对接触角的影响结果测试图(经热烘处理后)。可以发现，同一浓度的无氟防水剂拒水整理时，PET纤维和ES纤维比例不同时，无纺布的接触角也不同，无纺布的原料全部为PET纤维时，材料的接触角最小，即材料的拒水性能最差。在PET纤维和ES纤维比例相同时，纤维的接触角达到较大，即无纺布的拒水性能越强。PET/ES针刺无纺布的接触角随着无氟防水剂浓度变化而变化，且随着无氟防水剂浓度的增加呈现增大的趋势，即当无氟防水剂浓度设置为70mL/L时，PET/ES针刺无纺布的接触角最大，拒水性能最好。
图5为经热烘处理后，再对无纺布用无氟防水剂(浓度为70mL/L)拒水整理后织物的接触角测试结果，经热烘处理后，再进行拒水整理，织物的接触角为148°，有明显的增大。一定程度下，热烘处理对无纺布的水接触角有一定影响，增加了无纺布的拒水性能。
进一步对所制备的织物的吸油率进行测试，研究无氟防水剂的含量，PET纤维和ES纤维原料的配比，以及热风烘燥对无纺布带来的影响。在研究了各组试样的水接触角后，由于无处理的无纺布和只经过热烘干燥的无纺布接触角较小，具有一定的吸水性，在吸油实验中，吸收的部分可能包含水和油两种成分，对吸油后的无纺布的重量测定不具有准确性，所以，在研究吸油率时，着重研究只经过拒水处理和先经过热烘处理后经过拒水处理的两组具有拒水性的无纺布。
图6为经过热烘处理所制备的针刺无纺布的吸油率测试结果。从图中可以看出，当原材料组成仅为PET或者ES纤维时，所制得的针刺无纺布经拒水整理后，其吸油率数值明显低于PET/ES共混针刺无纺布，即在PET纤维比ES纤维为4:0和0:4时，无纺布的吸油率最小，在PET和ES纤维比例相同时，材料的吸油率达到一个较大的数值，可以看出，PET纤维和ES纤维的混合原料制作出的无纺布的吸油性能大于单种纤维原料的吸油性能。
图7为PET/ES比例为1:1，经热烘处理和未经热烘处理的拒水无纺布的吸油率测试结果，由图7可知，经过热烘后再拒水处理的无纺布的吸油率的曲线高于只经过拒水处理后的无纺布吸油率的曲线，即在相同条件相同浓度的无氟防水剂含量下，事先经过热烘处理的无纺布的吸油率要较高于只经过拒水处理的无纺布。
本发明中，在制备复合针刺无纺布时选用了PET和ES纤维，其中的ES纤维也可以替换为PP纤维和/或PE纤维，同样得到具有类似性质的拒水亲油复合针刺无纺布。热烘处理温度也可以在110-160℃范围内调节，优选为120-130℃，热烘处理时间优选为60-70min。
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。

Claims (8)

1.一种拒水亲油复合针刺无纺布的制备方法，其特征在于，包括以下步骤：
(1)将PET纤维与ES纤维按照质量比为3:1-1:3进行共混，经针刺得到复合针刺无纺布；
(2)将所述复合针刺无纺布在110-160℃下进行热烘处理，处理时间为40-90min；
(3)采用浓度为50-70mL/L的改性树脂类无氟防水剂水溶液对热烘处理过的织物进行浸轧拒水整理，浸轧拒水整理的气压为1.8kPa，带液率为160％-230％，烘干后得到所述拒水亲油复合针刺无纺布。
2.根据权利要求1所述的制备方法，其特征在于：在步骤(1)中，采用针刺工艺对共混的纤维进行加工，所述针刺工艺包括以下步骤：
将PET纤维与ES纤维开松混合，然后梳理成网，铺网后进行预针刺，然后将预针刺后的面料对叠进行主针刺。
3.根据权利要求1所述的制备方法，其特征在于：在步骤(3)中，所述改性树脂类无氟防水剂为阳离子改性树脂类无氟防水剂，所述改性树脂类无氟防水剂的pH值为3.5-4.5。
4.根据权利要求1所述的制备方法，其特征在于：在步骤(3)中，所述改性树脂类无氟防水剂为ECO-0C无氟防水剂。
5.根据权利要求1所述的制备方法，其特征在于：在步骤(3)中，所述改性树脂类无氟防水剂与织物的浴比为10:1-20:1。
6.根据权利要求1所述的制备方法，其特征在于：在步骤(3)中，采用二浸二轧法进行浸轧拒水整理。
7.根据权利要求1所述的制备方法，其特征在于：在步骤(3)中，烘干温度为60-90℃。
8.一种权利要求1-7中任一项所述的制备方法所制备的拒水亲油复合针刺无纺布，其特征在于：所述拒水亲油复合针刺无纺布的水接触角为120-150°，吸油率为3.2-4.4g/g。
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