CN1348521A - 使用聚乙烯醇助剂施涂在疏水聚合物纤维上的阳离子带电涂层 - Google Patents

使用聚乙烯醇助剂施涂在疏水聚合物纤维上的阳离子带电涂层 Download PDF

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CN1348521A
CN1348521A CN99816258A CN99816258A CN1348521A CN 1348521 A CN1348521 A CN 1348521A CN 99816258 A CN99816258 A CN 99816258A CN 99816258 A CN99816258 A CN 99816258A CN 1348521 A CN1348521 A CN 1348521A
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卫宁
R·J·林
M·G·瓦里尔勒
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Abstract

一种其上带有阳离子带电涂层的疏水聚合物纤维,其中涂层包括已经过热而被交联的官能化阳离子聚合物,例如表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。本发明还提供一种纤维滤材,它包括上述表面带有阳离子带电涂层的疏水聚合物纤维。本发明还提供一种制备纤维滤材的方法。该方法涉及:提供由疏水聚合物纤维构成的纤维滤材;用可热交联官能化阳离子聚合物水溶液处理该纤维滤材,处理条件应足以使纤维基本上用该官能化阳离子聚合物涂布,其中该溶液包含官能化阳离子聚合物、聚乙烯醇、聚乙烯醇的极性溶剂以及水;以及对所获得的已涂布的纤维滤材进行热处理,处理温度和时间应足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。

Description

使用聚乙烯醇助剂施涂在疏水聚合物纤维上的阳离子带电涂层
发明背景
本发明涉及过滤材料。更具体地说，本发明涉及电荷改性的滤材。
电荷改性滤材在技术上是已知的。它们通常由微孔膜组成或者涉及玻璃纤维与纤维素纤维的共混物或者纤维素纤维与硅质颗粒的共混物之类材料的使用。电荷改性通常是在该膜或者至少部分纤维上涂布电荷改性剂以及一种保证涂层耐久性的单独交联剂实现的。
虽然微孔膜通常能有效地过滤，但通过膜的流率通常要低于通过纤维滤材的流率。加之，微孔膜在过滤期间的反压通常也比纤维滤材高。因此，目前存在着对能有效过滤带电颗粒的纤维滤材的需要。另外，还需要由玻璃纤维构成但不需要纤维素纤维或硅质颗粒的纤维滤材。
带孔薄膜、机织物以及非织造布材料已被当作过滤片材应用于从液体中清除或分离颗粒。此种过滤片材通常依靠某种形式的机械过滤或物理截留来工作。此种过滤片材在要移出的颗粒尺寸比该过滤片材平均孔径小时存在一定限制。就非织造布材料而言，要去除尺寸小于1μm的颗粒时情况尤其如此。
已开发出表面电荷特性改性的改良滤材，它利用滤材表面与含水液体中所含颗粒之间的电动相互作用来俘获和吸附颗粒。此种电荷改性的滤材一般由微孔膜组成，或者涉及玻璃纤维与纤维素纤维的共混物或者纤维素纤维与硅质颗粒的共混物之类材料的使用。电荷改性通常是在膜或者至少部分纤维上涂布电荷改性剂以及一种保证涂层耐久性的单独交联剂实现的。
虽然微孔膜通常能有效地过滤，但通过膜的流率通常要低于通过纤维滤材的。加之，微孔膜在过滤期间的反压通常也比纤维滤材高。
采用由合成聚合物制备的纤维是希望的，因为此种纤维成本低并且它们可成形为具有适合从流体物流中过滤颗粒的孔隙率的非织造纤网。然而，许多此种合成聚合物却是疏水的，此种特性使得很难在由此种聚合物制备的纤维上牢固地涂布上电荷改性材料。因此，存在着改良以疏水聚合物纤维为基础的电荷改性滤材的可能。
换句话说，倘若可用某种廉价材料生产具有适合从含水液体中过滤非常细的颗粒的表面电荷特性改性的滤材，那将是希望的。例如，聚烯烃被广泛用于制造带孔薄膜、机织物和非织造布材料等片材。许多类型聚烯烃片材具有疏水倾向并且相对惰性。就是说，聚烯烃(例如，聚丙烯)的低表面自由能及其相对而言的化学惰性使得许多未经改性的聚烯烃不能很好地适用于要求有能从含水液体中移出颗粒的具有改性的表面电荷特性的过滤片材应用领域。例如，许多化学电荷改性剂(例如，阳离子树脂、带电颗粒等)对传统未改性疏水聚烯烃片材即便有粘附力的话，其粘附也很差。
过去，一直在廉价材料制造的过滤片材上施加化学涂层和/或内添加剂，来赋予所要求的性能。这类涂层和/或添加剂中的许多，在有关成本、效力、耐久性和/或环境方面存在这样那样的问题。
曾建议，可以溶液形式在不同基材(即，材料片材)上沉积生物功能材料(例如，蛋白质)以改良该基材的表面性质和/或作为具有化学活性的功能化表面。然而，许多经济上希望的基材(例如，由诸如聚烯烃之类聚合物构成的基材)，其表面不适合快速和低成本地沉积生物功能材料，尤其是当要求涂层具有满意粘附力、耐久和粘合紧密时。
即便在经济上希望的基材上能够粘附廉价、耐久、坚韧的涂层，但仅仅由生物功能材料(例如蛋白质)构成的涂层也可能具有局限性，尤其是当涂层缺乏要求的诸如改性表面电荷特性之类化学特性时。
因此，目前仍然需要一种实用和廉价的化学带电改性滤材，用以从含水液体中移出微米～亚微米尺寸带电颗粒。目前，需要由未改性、相对惰性的疏水基材，例如未改性、相对惰性的聚烯烃基材来成形这样一种滤材。还需要一种从含水液体去除带电、微米～亚微米尺寸颗粒的方法，其中利用一种实用和廉价的、化学电荷改性滤材，例如由未改性、相对惰性的聚烯烃基材成形的化学电荷改性滤材。
除了上述需要之外，还需要一种简单、实用而低廉的化学电荷改性的滤材，用来从含水液体中移出水中病原体。该需要还延伸至一种从含水液体中移出水中病原体的简单方法，其中利用一种实用而低廉、化学电荷改性滤材。
从某些具有改性表面电荷特性的滤材观察到的一种现象是，该滤材对于不同类型水中病原体，如不同类型细菌，具有不同过滤效率。就是说，某些具有改性表面电荷的滤材对于某些类型水中病原体(例如，某些类型细菌)可提供可接受去除效果，而对于其他类型则不能。此种亲合性的本质似乎难以预测。鉴于在水中病原体去除效率方面哪怕比较小的差异也可能是重要的，因此，某种滤材或过滤系统对某种水中病原体具有不可预测强的亲合性这一发现，既是出乎意料又是非常希望的，尤其是当该滤材可用来生产饮用水时。满足这一要求之所以重要是因为，以一种实用和低廉方式从含水液体中去除水中病原体，在世界的许多地方至今仍是个挑战。
发明概述
本发明通过提供一种其上带有阳离子带电涂层的疏水聚合物纤维，其中涂层包括已通过热被交联的官能化阳离子聚合物，来着手解决上面所讨论的某些困难和问题。例如，官能化阳离子聚合物可以是表氯醇官能化的聚胺。另一个例子，官能化阳离子聚合物可以是表氯醇官能化的聚酰胺型胺。
本发明还提供一种纤维滤材，它包括其上带有阳离子带电涂层的疏水聚合物纤维。该涂层包括已通过热被交联的官能化阳离子聚合物。如上所述，该官能化阳离子聚合物是表氯醇官能化的聚胺或者是表氯醇官能化的聚酰胺型胺。
本发明还提供一种制备纤维滤材的方法。该方法包括：提供由疏水聚合物纤维构成的纤维滤材；用可热交联的官能化阳离子聚合物水溶液处理该纤维滤材，处理条件应足以使纤维基本上用该官能化阳离子聚合物涂布，其中该溶液包含官能化阳离子聚合物、聚乙烯醇、聚乙烯醇的极性溶剂以及水；以及对所获得的已涂布的纤维滤材进行热处理，处理温度和时间应足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。例如，官能化阳离子聚合物可以是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。不拟囿于理论，但据信，聚乙烯醇改变了通常为疏水的纤维表面，其改变程度足以促使官能化阳离子聚合物涂布在纤维上。另外，又据信，聚乙烯醇中存在的某些羟基基团可与存在于官能化阳离子聚合物中的活性基团(例如，环氧基团)交联，从而在纤维上形成耐久、带阳电涂层。
本发明另外还提供制备纤维滤材的方法。该方法包括：提供一种由疏水聚合物纤维构成的纤维滤材；让可热交联的官能化阳离子聚合物的溶液通过纤维滤材，通过的条件足以使纤维基本上用该官能化阳离子聚合物涂布，其中溶液包括官能化阳离子聚合物、聚乙烯醇以及水；以及对所获得的已涂布的纤维滤材进行热处理，处理温度和时间足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。同样，该官能化阳离子聚合物可以是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。
发明详述
本文中使用的术语“疏水聚合物”是指任何聚合物，只要它耐润湿，或者不容易被水打湿，即，缺乏对水的亲合性。就典型而言，疏水聚合物的表面自由能为约40 dyn/cm(10-5N/cm)或更低。疏水聚合物的例子，仅举例说明，包括聚烯烃，例如聚乙烯、聚异丁烯、聚异戊二烯、聚(4-甲基-1-戊烯)、聚丙烯、乙烯-丙烯共聚物以及乙烯-丙烯-己二烯共聚物；乙烯-醋酸乙烯共聚物；苯乙烯聚合物，例如聚苯乙烯、聚(2-甲基苯乙烯)、含低于约20mol％丙烯腈的苯乙烯-丙烯腈共聚物以及苯乙烯-2，2，3，3-四氟丙基甲基丙烯酸酯共聚物；卤化烃聚合物，例如聚(氯-三氟乙烯)、氯三氟乙烯-四氟乙烯共聚物、聚六氟丙烯、聚四氟乙烯、四氟乙烯-乙烯共聚物、聚三氟乙烯、聚氟乙烯以及聚偏二氟乙烯；乙烯基聚合物，例如聚丁酸乙烯酯、聚癸酸乙烯酯、聚十二烷酸乙烯酯、聚十六烷酸乙烯酯、聚己酸乙烯酯、聚丙酸乙烯酯、聚辛酸乙烯酯、聚(七氟异丙氧基乙烯)、1-七氟异丙氧基-甲基亚乙基-马来酸共聚物、聚(七氟异丙氧基丙烯)、聚甲基丙烯腈、聚乙烯醇、聚乙烯醇缩丁醛、聚乙氧基乙烯、聚甲氧基乙烯以及聚乙烯醇缩甲醛；丙烯酸类聚合物，例如聚乙酸正丁酯、聚丙烯酸乙酯、聚[丙烯酸(1-氯二氟甲基)-四氟乙基酯]、聚[丙烯酸二(氯氟甲基)氟甲基酯]、聚丙烯酸1，1-二氢七氟丁基酯、聚丙烯酸1，1-二氢五氟异丙基酯、聚丙烯酸1，1-二氢十五氟辛基酯、聚丙烯酸七氟异丙基酯、聚丙烯酸5-(七氟异丙氧基)-戊基酯、聚丙烯酸11-(七氟异丙氧基)十一烷基酯、聚丙烯酸2-(七氟丙氧基)-乙基酯以及聚丙烯酸九氟异丁基酯；甲基丙烯酸聚合物，例如聚甲基丙烯酸苄基酯、聚甲基丙烯酸正丁酯、聚甲基丙烯酸异丁酯、聚甲基丙烯酸叔丁酯、聚甲基丙烯酸叔丁氨基乙基酯、聚甲基丙烯酸十二烷基酯、聚甲基丙烯酸乙酯、聚甲基丙烯酸2-乙基己基酯、聚甲基丙烯酸正己酯、聚甲基丙烯酸二甲氨基乙基酯、聚甲基丙烯酸羟乙基酯、聚甲基丙烯酸苯酯、聚甲基丙烯酸正丙酯、聚甲基丙烯酸十八烷基酯、聚甲基丙烯酸1，1-二氢十五氟辛基酯、聚甲基丙烯酸七氟异丙基酯、聚甲基丙烯酸十七氟辛基酯、聚甲基丙烯酸1-氢四氟乙基酯、聚甲基丙烯酸1，1-二氢四氟丙基酯、聚甲基丙烯酸1-氢六氟异丙基酯以及聚甲基丙烯酸九氟叔丁酯；聚醚，例如聚氯醛(聚吡啶和三氯乙醛产物)、聚氧化丁烯二醇、聚氧化异丁烯二醇、聚氧基十亚甲基、分子量低于约1,500的聚氧化乙烯-二甲基醚聚合物、聚氧基六亚甲基二醇、聚氧化丙烯二醇、聚氧化丙烯二甲基醚以及聚氧基四亚甲基；聚醚共聚物，例如聚氧化乙烯-聚氧化丙烯-聚氧化乙烯嵌段共聚物、氧化丙烯含量大于约20mol％的氧化乙烯-氧化丙烯共聚物、氧四亚甲基-氧化丙烯共聚物，以及包含被聚(氧二甲基亚甲硅烷基)嵌段隔开的氧化乙烯-氧化丙烯共聚物嵌段的嵌段共聚物；聚酰胺，例如聚[亚氨基(1-氧代-十亚甲基)]、聚[亚氨基(1-氧代-十二亚甲基)]或尼龙12、聚[亚氨基(1-氧代-六亚甲基)]或尼龙6、聚[亚氨基(1-氧代-四亚甲基)]或尼龙4、聚(亚氨基壬二酰亚氨基九亚甲基)、聚(亚氨基癸二酰亚氨基十二亚甲基)、聚(亚氨基辛二酰亚氨基八亚甲基)；聚亚胺，例如聚[(苯甲酰亚氨基)亚乙基]、聚[(丁酰亚氨基)亚乙基]、聚[(十二烷酰亚氨基)亚乙基]、(十二烷酰亚氨基)亚乙基(乙酰亚氨基)三亚甲基共聚物、聚[(庚酰亚氨基)亚乙基]、聚[(己酰亚氨基)亚乙基]、聚{[(3-甲基)丁酰亚氨基]亚乙基}、聚[(十五氟十八烷酰亚氨基)亚乙基]以及聚[(戊酰亚氨基)亚乙基]；聚氨酯，例如由二苯甲烷二异氰酸酯与丁二醇、聚氧基四亚甲基二醇制备的那些，六亚甲基二异氰酸酯与三甘醇制备的那些，以及由4-甲基-1，3-亚苯基二异氰酸酯与三丙二醇制备的那些；聚硅氧烷，例如聚氧基二甲基亚甲硅烷基和聚氧甲基苯基亚甲硅烷基；以及纤维素类，例如直链淀粉、支链淀粉、乙酸丁酯纤维素、乙基纤维素、半纤维素和硝基纤维素。
本文在指疏水聚合物纤维上的涂层时所使用的术语“阳离子带电”以及提到官能化聚合物时使用的“阳离子(的)”，是分别指在涂层和聚合物中存在许多带阳电基团，因此“阳离子带电”和“带阳电”是同义词。此种带阳电基团在典型情况下包括大量季铵基团，然而不一定局限于这些。
本文使用的术语“官能化”是指在阳离子聚合物中存在除阳离子基团以外的大量官能团，它们在受到加热时能够交联。因此，这些官能团是可热交联基团。这些官能团的例子包括环氧、氮丙啶基以及环硫基。这些官能团很容易与阳离子聚合物中典型存在的其他基团起反应。该其他基团在典型情况下具有至少1个活性氢原子，例子是氨基、羟基和硫醇基。还应当指出的是，一个官能团与另一基团起反应常常产生另外一种能与官能团起反应的其他基团。例如，环氧基团与氨基基团起反应生成β-羟氨基基团。
因此，术语“官能化阳离子聚合物”应理解为包括任何聚合物，只要它包含大量带正电基团以及能借助加热而交联的大量其他官能团。此种聚合物的尤其有用例子是表氯醇官能化的聚胺，该聚合物包括表氯醇官能化的聚酰胺型胺。这两种类型聚合物的例子是Kymene树脂，由Hercules公司(Wilmington，特拉华)供应。其他合适的材料包括阳离子改性淀粉，例如RediBond，由National Starch公司供应。较好的是，官能化阳离子聚合物是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。
本文使用的术语“热交联的”是指该官能化阳离子聚合物涂层已经在足以使上面提到的官能团交联的温度下加热了足够时间。加热温度一般可介于约50℃～约150℃。加热时间通常随温度以及阳离子聚合物中存在的官能团类型而变化。例如，加热时间可从不足1分钟至约60分钟或更长。
前面已经提到，本发明提供一种疏水聚合物纤维，其上具有阳离子带电涂层，其中该涂层包括已经过热交联的官能化阳离子聚合物。作为例子，官能化阳离子聚合物可以是表氯醇官能化的聚胺。作为另一个例子，官能化阳离子聚合物可以是表氯醇官能化的聚酰胺型胺。
本发明还提供一种纤维滤材，它包括其上带有阳离子带电涂层的疏水聚合物纤维。该涂层包括已通过热而被交联的官能化阳离子聚合物。前面已经提到，官能化阳离子聚合物是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。
一般而言，该纤维滤材将包含，以滤材中存在的全部纤维重量为基准，至少约50wt％疏水聚合物纤维。在某些实施方案中，纤维基本上100％是疏水聚合物纤维。然而，当存在其他纤维时，它们通常将是纤维素纤维、玻璃纤维或其混合物。
纤维素纤维源，比如说，包括木材，例如软木和硬木；麦稻秸和草，例如稻子、西班牙草、小麦、黑麦以及sabai；甘蔗以及芦苇，例如甘蔗渣；竹子；木质茎，例如黄麻、亚麻、南非槿麻以及大麻；韧皮纤维，例如亚麻和苎麻；叶子，例如马尼拉麻和西沙尔麻；以及种子，例如棉籽和棉短绒。软木和硬木是比较常用的纤维素纤维源；该纤维可采用任何常用制浆方法制取，例如机械、化学-机械、半化学以及化学方法。软木的例子包括，仅作为举例说明，长叶松、短叶松、火炬松、湿地松、南方松、黑云杉、白云杉、斑克松、香脂冷杉、花旗松(黄衫属)、异叶铁杉、水杉、铅笔柏。硬木的例子包括，仍然仅作为举例说明，山杨、桦木、山毛榉、橡树、槭树和桉树。
疏水聚合物纤维较好是由热塑性聚烯烃制备的纤维或其混合物。热塑性聚烯烃的例子包括聚乙烯、聚丙烯、聚1-丁烯、聚2-丁烯、聚1-戊烯、聚2-戊烯、聚3-甲基-1-戊烯、聚4-甲基-1-戊烯等。另外，术语“聚烯烃”意在涵盖两种或更多种聚烯烃的共混物以及由两种或更多种不同不饱和单体制备的无规和嵌段共聚物。由于在商业上的重要性，最希望的聚烯烃是聚乙烯和聚丙烯。
纤维滤材(加工前或后)的织物单位重量(basis weight)可介于约6gsm(g/m2)～约400gsm。例如，纤维滤材的织物单位重量可介于约12gsm～约250gsm。较好的是，纤维滤材的织物单位重量介于约17gsm～约102gsm。然而，任意数目的本发明纤维滤材均可合在一起或者与其他材料合在一起形成结实的材料，其织物单位重量介于6gsm～400gsm或更大(例如大于400gsm)。
本发明还提供一种制备纤维滤材的方法。该方法包括：提供由疏水聚合物纤维构成的纤维滤材；用可热交联的官能化阳离子聚合物的水溶液处理该纤维滤材，处理条件应足以使纤维基本上用该官能化阳离子聚合物涂布，其中该溶液包含官能化阳离子聚合物、聚乙烯醇、聚乙烯醇的极性溶剂以及水；以及对所获得的已涂布的纤维滤材进行热处理，处理温度和时间应足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。例如，官能化阳离子聚合物可以是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。
实践中，官能化阳离子聚合物的水溶液在典型情况下将包含约0.1～约2wt％官能化阳离子聚合物、约0.1～约4wt％聚乙烯醇以及约10～约50wt％极性溶剂，溶液的其余部分是水。作为例子，官能化阳离子聚合物水溶液可包含约0.2～约1wt％官能化阳离子聚合物、约0.1～约2wt％聚乙烯醇以及约15～约45wt％异丙醇，溶液的其余部分是水。
聚乙烯醇在工业上通过聚醋酸乙烯酯的水解来制备。聚乙烯醇的物理性能在很大程度上取决于水解度和分子量。用于本发明的聚乙烯醇是通常被称之为热水可溶的聚乙烯醇。此种材料是被高度水解的，其水解度至少为约98％。较好的是，聚乙烯醇具有99％或更高的水解度。聚乙烯醇的分子量一般至少约10,000，大约相当于至少约200的聚合度。较好的是，聚乙烯醇的分子量介于约15,000～约20,000，大致相当于约325～约435的聚合度。
一般地，极性溶剂可以是任何能部分或完全溶解聚乙烯醇的有机溶剂。极性溶剂的例子包括，仅作为举例说明，低级醇，例如甲醇、乙醇、1-丙醇、异丙醇、1-丁醇、异丁醇和叔丁醇；酮，例如丙酮、丁酮以及二乙基甲酮；二氧杂环己烷；以及N，N-二甲基甲酰胺。较好的是，极性溶剂是异丙醇。
最后，本发明另外还提供一种制备纤维滤材的方法，其中该方法包括：提供由疏水聚合物纤维构成的纤维滤材；让一种可热交联的官能化阳离子聚合物的溶液通过纤维滤材，通过的条件足以使纤维上基本涂满该官能化阳离子聚合物，其中溶液包括官能化阳离子聚合物、聚乙烯醇以及水；以及对所获得的已涂布的纤维滤材进行热处理，处理温度和时间足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。同样，官能化阳离子聚合物可以是表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺。
依官能化阳离子聚合物之不同，希望或者必须调节含聚合物水溶液的pH。例如，希望表氯醇官能化的聚胺或表氯醇官能化的聚酰胺型胺水溶液的pH值是碱性或者微带酸性的。例如，此种溶液的pH可介于约6～约10。该pH很容易借助本领域技术人员熟知的手段加以调节。例如，pH可通过向聚合物溶液中加入，典型情况下，无机酸常规稀溶液，例如盐酸、硫酸，或者碱溶液，例如氢氧化钠、氢氧化钾或氢氧化铵溶液而进行调节。
官能化阳离子聚合物溶液通过纤维滤材可借助本领域技术人员已知的任何手段实现。例如，可通过降低与滤材施涂过溶液的那一侧相对一侧的压力将溶液抽过滤材。替代地，也可通过加压，迫使溶液透过滤材。
滤材的纤维一旦涂布上官能化阳离子聚合物，可通过在足以使聚合物中存在的官能团交联的温度下加热足够时间使聚合物交联。温度一般可介于约50℃～约150℃。加热时间一般随温度以及阳离子聚合物中存在的官能团类型而变化。例如，加热时间可介于约1～约60min或更长。
本发明将通过下面实施例进一步说明。然而，这些实施例从任何意义上均不构成对本发明精神或范围的限制。在实施例中，所有份数和百分数均指重量而言。
实例1
聚乙烯醇溶液的制备：0.5份聚乙烯醇(目录号18，934-0，Aldrich化学公司，Milwaukee，威斯康星，88％水解度，重均分子量96,000)在99.5份水中，在85℃加热直至聚合物溶解。所获得的溶液冷却至室温(约20℃～25℃)以后，向其中加入表氯醇官能化聚酰胺型胺水溶液(Kymene450，20％固体，Hercules公司，Wilmington，特拉华)和异丙醇(99.5％，HPLC(高压液相色谱)级，Aldrich化学公司)，各自的数量足以提供包含0.35％聚乙烯醇、0.35％Kymene450和29％异丙醇的最终水溶液。将一块7英寸×30英寸(约18cm×约76cm)、织物单位重量为1盎司/平方码或osy(约34g/m2或gsm)的熔喷纤网，浸泡在该最终聚乙烯醇溶液中直至完全湿透(1～2min)。该饱和浸渍的纤网从溶液中取出并风干。然后，纤网被放在85℃的烘箱内达1h，以便使存在于构成纤网的纤维表面上的表氯醇官能化聚酰胺型胺交联。
6层处理过的被裁切为1英寸(约2.5cm)直径圆盘的纤网，置于不锈钢注射器贮蓄器(25mm直径，目录号1980-002，Whatman公司，Clifton，新泽西)中，然后用来过滤不带表面活性剂而以108个颗粒/mL的浓度悬浮在水中的0.5μm直径聚苯乙烯胶乳微粒(带有给出7.0μeq/g表面滴定值的羧酸官能团)(Bangs实验室公司，Fishers，印第安纳)。该颗粒悬浮体利用固定在注射器贮蓄器上的注射器透过该多层滤材。99.9％以上的颗粒被这6层处理后的纤网去除。通过过滤该溶液透过合起来织物单位重量等于6osy(约203gsm)的纤网层去除了99.9％以上的颗粒。
实例2
聚乙烯醇溶液的制备：1份聚乙烯醇(Elvanol7006，杜邦化学公司，Wilmington，特拉华)在99份水中，在85℃加热直至聚合物溶解。所获得的溶液冷却至室温(20℃～25℃)以后，将50mL该溶液与2mL表氯醇官能化聚胺溶液(Kymene2064，20％固体，Hercules公司，Wilmington，特拉华)、30mL异丙醇(99.5％，HPLC(高压液相色谱)级，Aldrich化学公司)以及18mL去离子水充分混合。将一块7英寸×52英寸(约18cm×132cm)普通聚丙烯熔喷纤网，浸泡在100mL该聚乙烯醇/官能化阳离子聚合物溶液中直至它彻底被溶液润湿。将该纤网从溶液中取出并使之穿过实验室绞干机以除掉残留溶液。让纤网风干并置于85℃的烘箱内加热1h以便使存在于构成纤网的纤维表面上的表氯醇官能化聚胺交联。
从获得的处理过的纤网上切取直径1.875英寸(约4.8cm)的圆形样品。由6层圆形样品组成的滤材被放在2英寸(约5.1cm)直径的Nalgene可重复使用滤材贮蓄器(250mL，Nalgene#300-4000，NalgeNunc International，Naperville，伊利诺)中。滤材处于滤材贮蓄器中，以5L去离子水洗涤。然后，用100mL实例1使用的0.5μm直径聚苯乙烯胶乳微粒来试验滤材俘获效率。该颗粒悬浮体依靠重力透过滤材。90％以上的颗粒，通过过滤悬浮体透过合计织物单位重量6osy(约204gsm)的多层滤材而被去除。
实例3
聚乙烯醇溶液的制备：0.2份聚乙烯醇(Elvanol7006，杜邦化学公司，Wilmington，特拉华)在99.8份水中，在85℃加热直至聚合物溶解。所获得的溶液冷却至室温(20℃～25℃)后，将68mL该溶液与2mL表氯醇官能化聚胺溶液(Kymene2064，20％固体，Hercules公司，Wilmington，特拉华)充分混合。所获溶液的pH利用氢氧化钠水溶液调节到10，然后加入30mL异丙醇(99.5％，HPLC级，Aldrich化学公司)。将一块7英寸×52英寸(约18cm×132cm)普通聚丙烯熔喷纤网，浸泡在100mL该聚乙烯醇/官能化阳离子聚合物溶液中直至它彻底被溶液润湿。将该纤网从溶液中取出并使之穿过实验室绞干机以除掉残留溶液。让纤网风干并置于85℃的烘箱内加热1h以便使构成纤网的纤维表面上存在的表氯醇官能化聚胺交联。
从获得的处理过的纤网上切取直径1.875英寸(约4.8cm)的圆形样品。由6层圆形样品组成的滤材被放在2英寸(约5.1cm)直径的Nalgene可重复使用滤材贮蓄器(250mL，Nalgene#300-4000，NalgeNunc International，Naperville，伊利诺)中。滤材处于滤材贮蓄器中，以4L去离子水洗涤。然后，用100mL实例1使用的0.5μm直径聚苯乙烯胶乳微粒来试验滤材俘获效率。该颗粒悬浮体依靠重力透过滤材。99.9％以上的颗粒，通过悬浮体透过合计织物单位重量6osy(约204gsm)的多层滤材的过滤而被去除。
实例4
聚乙烯醇溶液的制备：0.2份聚乙烯醇(Elvanol7006，杜邦化学公司，Wilmington，特拉华)在97份水中，在85℃加热直至聚合物溶解。所获得的溶液冷却至室温(20℃～25℃)后，将其与3mL实例3中使用的表氯醇官能化聚胺溶液(Kymene2064，20％固体，Hercules公司，Wilmington，特拉华)充分混合。准备一块由6层直径1.875英寸(约4.8cm)圆盘形普通熔喷纤网组成的滤材。将滤材放在2英寸(约5.1cm)直径的Nalgene可重复使用滤材贮蓄器(250mL，Nalgene#300-4000，Nalge Nunc International，Naperville)中。通过降低滤材贮蓄器下游一侧的压力，在约10s内将上面制备的表氯醇官能化聚胺溶液抽过滤材。观察到，通过这样的处理，纤网变得可润湿了。随后，滤材放在85℃的烘箱内加热1h，以便使构成纤网的纤维表面上存在的表氯醇官能化聚胺交联。
加热以后，滤材先以4L去离子水洗涤，然后以100mL 0.1wt％氯化钠水溶液洗涤。按照实例3中所描述的那样试验滤材的俘获效率。99.9％以上的颗粒，通过过滤悬浮体透过合计织物单位重量6osy(约204gsm)已处理滤材而被去除。
在下面的实例中，试验了按本发明处理的熔喷材料的涂层耐久性、不同流速下的颗粒俘获效率以及病原体俘获效率。
实例5
织物单位重量1osy(约34 gsm)的聚丙烯熔喷纤网，基本按照前面实例所述那样被处理。处理溶液由400g聚乙烯醇(Elvanol7006，杜邦化学公司，Wilmington，特拉华)、600mL表氯醇官能化聚胺溶液(Kymene2064，20％固体，Hercules公司，Wilmington，特拉华)以及为凑足22L总体积的水组成。溶液的pH介于7.5～8。纤网放在85℃的烘箱内加热1h，以便使存在于构成纤网的纤维表面上的表氯醇官能化聚胺交联。
不同流速下的颗粒俘获效率
从处理过的纤网上切取直径1.875英寸(约4.8cm)圆形样品。由6层圆形样品组成的滤材被放在2英寸(约5.1cm)直径的Nalgene可重复使用滤材贮蓄器(250mL，Nalgene#300-4000，Nalge NuncInternational，Naperville，伊利诺)中。滤材处于滤材贮蓄器中，以100mL 0.1wt％氯化钠水溶液洗涤。用100mL实例1使用的0.5μm直径聚苯乙烯胶乳微粒来试验滤材的俘获效率。该颗粒悬浮体在施加受控制的减压下被抽过滤材。99％以上的颗粒，通过过滤悬浮体透过合计织物单位重量6osy(约204gsm)的多层滤材而被去除，其中悬浮体流速从3.8改变到470mLmin-1in-2。
大量自来水流过后涂层的耐久性
滤材是通过将6层处理过的熔喷纤网围绕着多孔金属芯缠绕而制成的。每层的织物单位重量是1osy(约34gsm)，面积为18.2平方英寸。制成的构件被固定在不锈钢贮蓄器中，它被设计成使流体流入外表面，穿过所有6层，然后进入到金属芯中。将龙头自来水，大约200加仑(约757L)，透过滤材流过。将该构件从贮蓄器中取出，将每层小心地从金属芯上退绕下来。每一层熔喷包缠物裁切成3块直径1.875英寸(约4.8cm)的圆形，并按照前面的实例所述在重力流动下试验颗粒俘获效率；但在本实例中，微粒悬浮体包含2.94×108个微粒每毫升。颗粒俘获效率数据总括在表1中。在表中，片材1代表最外层，而片材6代表最内层，或者最先缠绕在金属芯上的层。
        表1
  颗粒俘获效率归纳
    片材     俘获百分率
    1     74.1±2.3
    2     77.0±1.8
    3     78.6±3.2
    4     72.8±5.0
    5     74.1±2.3
    6     75.0±0.9
  对照样     76.6±1.4
从表1可以看出，平均颗粒俘获效率在约73％～约79％范围内变化。倘若将标准偏差值也考虑进去，该范围还要略微宽一些，即，约68％～约82％。对照纤网，即，用官能化阳离子聚合物处理过但未经自来水洗涤步骤处理的纤网，其平均颗粒俘获效率为约77％。表中数据显示，电荷改性涂层是耐久的，因为这些数据是以200加仑自来水洗涤滤材以后取得的。
病原体俘获结果
病原体过滤效率在本文中被规定为滤液中留下的细胞数目与原来存在于病原体悬浮体中的细胞数目的比值。其测定方法是，将原来的悬浮体和滤液的样品都滴在胰蛋白酶大豆琼脂(TSA)生长培养基平皿(BBLTSA平皿，Becton-Dickinson，Cockeyville，马里兰)上，并在37℃下培养过夜以后计算看到的菌落数目。一个菌落形成单位(CFU)算作1个单独的存活细胞(cell)。虽然，看上去简单容易，但是该试验并非总是没有复杂因素的。可溶性聚阳离子，例如本实例中使用的官能化阳离子聚合物是强抗微生物的。涂层的沥滤和洗涤将杀死滤液中可能存在的任何细胞。倘若出现这种情况，相应滤材将显示高得不真实的细菌减少效果，很重要的原因就是细胞在溶液中死亡。因此，滤材的效力是通过一种两部分试验程序确定的，即，涂层耐久性试验和滤材效力检验。
将几层处理过的聚丙烯熔喷纤网放在滤材容器设备中(Nalgene滤材贮蓄器；Nalgene公司，Rochester，纽约)；各层平均厚度等于3mm。为进行涂层耐久性试验，100mL体积0.1％消毒盐水在重力或减压作用下透过滤材。然后，用细菌将流出盐水污染到含大约105～106细胞/毫升，并培养30min。如同上面所述在37℃培养过夜以后那样测定细胞浓度。任何经由处理过的纤网中的官能化阳离子聚合物的沥滤导致的细胞死亡，通过与受污染对照溶液，即，没有透过滤材的受污染溶液之间的比较，将变得清楚。
沥滤检验或涂层耐久性试验只能确定与给定微生物对该官能化阳离子聚合物的敏感性有关的可检测的沥滤量。细菌的敏感性已通过最小抑制浓度研究(MIC)或观察不到生长时的浓度，而查明。表2总括了各种不同微生物的MIC。
                       表2
         对选择的聚阳离子的最小抑制浓度a
微生物  Reten201b  Kymene450c  Kymene2064d
V.cholerae(霍乱菌)    ＜250ppm     ＜33ppm     ＜16ppm
E.coli(大肠杆菌)       -     ＜33ppm     ＜16ppm
S.cholerasuis(猪霍乱沙门氏菌) - ＜16ppm -
K.terrigena(土生克雷伯氏菌) - - ＜16ppm
S.aureus(金黄色葡萄球菌) - ＜16ppm ＜8ppm
a见《微稀释(试管)肉汤法》，NCCLS，卷13，25期，1993-12
b含季铵基团的阳离子聚合物(Hercules公司，Wilmington，特拉华)
c表氯醇官能化聚酰胺型胺(Hercules公司，Wilmington，特拉华)
d表氯醇官能化聚胺(Hercules公司，Wilmington，特拉华)
过滤效率是通过让滤材过滤100mL污染的0.1％盐水来测定的。控制细菌污染，并将其浓度设定在105～106细胞/毫升。通过滤材的流动是依靠重力或者是在减压作用下推动的。如同涂层耐久性试验一样，流出的盐水培养30min。按上面所述滴在平皿上并在37℃培养过夜以后那样测定细胞浓度。该结果与原来悬浮体的平皿计数进行比较并以对数降低值作记录。研究的变量包括微生物类型、通过滤材的流率以及悬浮体pH。结果总括在表3～5中。
                              表3
                      不同微生物的过滤效率
            微生物     对数降低    沥滤
    K.terrigena(ATCC 33257)a    3.51±0.3b     无
       E.coli(ATCC 13706     3.36±0.3     无
aEPA试验微生物
b这代表微生物被滤材从悬浮体中彻底减少(或去除)
                       表4
       不同流速下对E.coli(大肠杆菌)的过滤效力
         流速     对数降低    沥滤
     5ml min-1in-2      ≥3.5     无
    10ml min-1in-2      ≥3.5     无
    15ml min-1in-2      ≥3.5     无
    20ml min-1in-2      ≥3.5     无
    50ml min-1in-2      ≥3.5     无
                    表5在不同pH值下对K.terragena(土生克雷伯氏菌)的过滤效力
  pH     对数降低    沥滤
  6.557.558.53     4.53±0.123.51±0.33.18±0.12    无无无
表3～5的数据表明：
-给定滤材的情况下，不同微生物的过滤效力之间可能存在小的差异(然而必须承认，此种差异很可能可以通过针对给定微生物来优化过滤材料而予以消除)；
-在研究的范围内，过滤效力不依赖于通过滤材的流速；以及
-就所研究的微生物而言，过滤效力依赖于待过滤液体的pH；该效应属预料之中，因为微生物的净电荷依赖于pH。
虽然已就本说明的具体细节做了详细描述，要知道，本领域技术人员在理解了上述内容以后，很容易设想出对这些实施方案的替代、改变和相应作法。因此，本发明范围应视为所附权利要求规定的范围及其等价物。

Claims (18)

1.一种其上带有阳离子带电涂层的疏水聚合物纤维，该涂层包含：
已通过热被交联的官能化阳离子聚合物。
2.权利要求1的疏水聚合物纤维，其中官能化阳离子聚合物是表氯醇官能化聚胺。
3.权利要求2的疏水聚合物纤维，其中官能化阳离子聚合物是表氯醇官能化聚酰胺型胺。
4.一种纤维滤材，它包含其上带有阳离子带电涂层的疏水聚合物纤维，该涂层包含：
已通过热被交联的官能化阳离子聚合物。
5.权利要求4的纤维滤材，其中官能化阳离子聚合物是表氯醇官能化聚胺。
6.权利要求5的纤维滤材，其中官能化阳离子聚合物是表氯醇官能化聚酰胺型胺。
7.一种制备纤维滤材的方法，该方法包括：
提供由疏水聚合物纤维构成的纤维滤材；
用可热交联的官能化阳离子聚合物的水溶液处理该纤维滤材，处理条件足以使纤维基本上用该官能化阳离子聚合物涂布，其中该溶液包含官能化阳离子聚合物、聚乙烯醇、聚乙烯醇的极性溶剂以及水；以及
对所获得的已涂布的纤维滤材进行热处理，处理温度和时间足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。
8.权利要求7的方法，其中官能化阳离子聚合物是表氯醇官能化聚胺。
9.权利要求8的方法，其中官能化阳离子聚合物是表氯醇官能化聚酰胺型胺。
10.权利要求7的方法，其中官能化阳离子聚合物的水溶液包含：
约0.1～约2wt％官能化阳离子聚合物；
约0.1～约4wt％聚乙烯醇；以及
约10～约50wt％极性溶剂；
而溶液的其余部分则是水。
11.权利要求10的方法，其中极性溶剂是异丙醇。
12.权利要求11的方法，其中官能化阳离子聚合物的水溶液包含：
约0.2～约1wt％官能化阳离子聚合物；
约0.1～约2wt％聚乙烯醇；以及
约15～约45wt％异丙醇；
而溶液的其余部分则是水。
13.一种制备纤维滤材的方法。该方法包括：
提供由疏水聚合物纤维构成的纤维滤材；让一种可热交联的官能化阳离子聚合物的溶液通过该纤维滤材，通过的条件足以使纤维基本上用该官能化阳离子聚合物涂布，其中溶液包含官能化阳离子聚合物、聚乙烯醇以及水；以及
对所获得的已涂布的纤维滤材进行热处理，处理温度和时间足以使存在于疏水聚合物纤维上的官能化阳离子聚合物交联。
14.权利要求13的方法，其中官能化阳离子聚合物是表氯醇官能化聚胺。
15.权利要求14的方法，其中官能化阳离子聚合物是表氯醇官能化聚酰胺型胺。
16.权利要求13的方法，其中官能化阳离子聚合物的水溶液包含：
约0.1～约4wt％官能化阳离子聚合物；以及
约0.1～约2wt％聚乙烯醇；
而溶液的其余部分则是水。
17.权利要求16的方法，其中极性溶剂是异丙醇。
18.权利要求17的方法，其中官能化阳离子聚合物的水溶液包含：
约0.2～约2wt％官能化阳离子聚合物；以及
约0.1～约1wt％聚乙烯醇；
而溶液的其余部分则是水。
CNB998162582A 1998-12-18 1999-12-16 使用聚乙烯醇助剂施涂在疏水聚合物纤维上的阳离子带电涂层 Expired - Fee Related CN1211527C (zh)

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CN107666947B (zh) * 2015-05-01 2020-09-25 特励达科学与成像有限责任公司 经涂布颗粒状过滤介质
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CN113301977B (zh) * 2019-01-16 2022-12-16 恩铂锘有限公司 水处理过滤器及其制造方法
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CN1211527C (zh) 2005-07-20
WO2000036207A1 (en) 2000-06-22
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ATE323794T1 (de) 2006-05-15
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US20020122939A1 (en) 2002-09-05
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