CN1509257A - 微孔过滤介质、包含它的过滤体系以及制造和使用方法 - Google Patents

微孔过滤介质、包含它的过滤体系以及制造和使用方法 Download PDF

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Publication number
CN1509257A
CN1509257A CNA03800271XA CN03800271A CN1509257A CN 1509257 A CN1509257 A CN 1509257A CN A03800271X A CNA03800271X A CN A03800271XA CN 03800271 A CN03800271 A CN 03800271A CN 1509257 A CN1509257 A CN 1509257A
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Prior art keywords
active particle
microvoid structure
filtration medium
cationic materials
microbiological interception
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CNA03800271XA
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CN1232333C (zh
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Ee
E·E·科斯洛
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KX Technologies LLC
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Koslow Technologies Corp
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Abstract

本发明涉及一种微生物截取增强过滤介质，其包括平均流动通道低于约2微米和由活性颗粒的排列组成的微孔结构。微孔结构的至少一部分表面在其上形成有包含阳离子材料以及生物活性金属的微生物截取增强剂。本发明的微生物截取增强过滤介质提供大于约4的病毒截取对数值，和大于约6的细菌截取对数值。

Description

微孔过滤介质、包含它的过滤体系 以及制造和使用方法
本发明涉及具有微生物截取能力的过滤介质，包含该过滤介质的过滤体系，以及制造和使用它的方法。
现代消费者水过滤器通常提供″健康要求″，包括减少颗粒、重金属、毒性有机化学品和所选微生物危害物。这些过滤体系可使用大致1.0微米结构截取微生物如似隐孢菌属(Cryptosporidium)和贾第虫属。但为了提供对甚至更小微生物危害物如病毒的微生物截取，需要一种具有亚微米微孔结构的过滤介质。现有技术过滤体系通常尝试使用具有不够小的孔尺寸和具有不好的物理整体性的过滤介质来实现宽微生物截取。尚未实现成功的微生物截取所要求的必需孔结构和令人满意的过滤性能之间的平衡。
发明概述
本发明在第一方面涉及一种过滤介质，包括：包含活性颗粒排列的微孔结构，所述微孔结构的平均流动通道低于约2微米；和微生物截取增强剂，其包含吸附在微孔结构的至少一部分上的具有中至高电荷密度和分子量大于约5000道尔顿的阳离子材料和直接接近阳离子材料而且也在微孔结构的至少一部分上的生物活性金属。
另一方面，本发明涉及一种过滤体系，包括：具有入口和出口的外壳；位于外壳内的与入口和出口流体连通的过滤介质，所述过滤介质包含：具有平均流动通道低于约2微米的微孔结构，其包含活性炭、活化矾土、沸石、硅藻土、硅酸盐、硅铝酸盐、钛酸盐、骨炭、钙羟基磷灰石、氧化锰、氧化铁、氧化镁、珍珠岩、滑石、聚合物颗粒、粘土、碘化树脂、离子交换树脂、陶瓷或其组合的活性颗粒；和微生物截取增强剂，其包含具有高电荷密度、大于约5000道尔顿分子量和具有与其缔合的抗衡离子的阳离子材料，所述阳离子材料吸附在微孔结构的至少一部分上，和其中使用至少一部分与阳离子材料缔合的抗衡离子使生物活性金属沉淀，其中流过外壳和接触过滤介质的微生物污染的流入物在流出外壳的排放物中具有至少约4的微生物污染物的对数下降。
另一方面，本发明涉及一种制造具有增强的微生物截取能力的过滤介质的方法，包括步骤：提供具有平均颗粒尺寸约0.1微米-约5,000微米的活性颗粒；将活性颗粒用包含具有高电荷密度和分子量大于约5000道尔顿的阳离子材料的微生物截取增强剂并结合生物活性金属进行处理；和将处理的活性颗粒成型为平均流动通道低于约2微米的微孔结构。
又一方面，本发明涉及一种制造具有增强的微生物截取能力的过滤介质的方法，包括步骤：提供具有平均颗粒尺寸约0.1微米-约5,000微米的活性颗粒；将活性颗粒凝聚成平均流动通道低于约2微米的微孔结构；和将微孔结构用包含具有高电荷密度和分子量大于约5000道尔顿的阳离子材料的微生物截取增强剂并结合生物活性金属进行处理。
在进一步的方面，本发明涉及一种从流体中去除微生物污染物的方法，包括：提供包含微孔结构的过滤介质，所述微孔结构包含活性颗粒和具有低于约2微米的平均流动通道；和吸附在微孔结构的至少一部分上的微生物截取增强剂，其包含具有中至高电荷密度和分子量大于约5000道尔顿的阳离子材料以及生物活性金属；使微生物污染的流体接触过滤介质至低于或等于约12秒的时间；和得到具有大于约4的微生物污染物的对数下降的排放物。
附图的简要描述
据信新颖的本发明特点和本发明的子特性在所附权利要求书中特别给出。附图仅用于说明且没有按比例画出。但本发明本身(在组成和操作方法上)可参考对以下优选的实施方案的描述并结合附图而得到最佳理解，其中：
图1是描绘本发明微生物截取增强活性炭过滤介质的空床接触时间对MS2噬菌体的对数下降值的图。
优选实施方案的详细描述
在描述本发明优选的实施方案时，在此参考附图中的图1。
定义
本文所用的″吸收剂″应该是指能够将物质吸收到其内结构中的任何材料。
本文所用的″吸附剂″应该是指能够通过物理方式而没有任何共价键合地将物质吸引到其表面的任何材料。
本文所用的″粘结剂″应该是指主要用于将其它材料粘结在一起的材料。
本文所用的″污染物下降″应该是指化学、机械或生物方式地减少被截取、去除、和/或惰性化的流体中的杂质，以使得该流体更安全地，例如用于人类使用，或在工业场合更有用。
本文所用的″空床接触时间″或″EBCT″应该是指对颗粒例如活性炭和流体之间在该流体流过颗粒床时发生多少接触的一种度量。
本文所用的″纤维″应该是指一种特征在于高纵横比(长度/直径)例如几百比一的固体。有关纤维的任何讨论还应该理解为包括晶须。
本文所用的″过滤介质″应该是指进行流体过滤的材料。
本文所用的″流体″应该是指液体、气体、或其组合。
本文所用的″截取″是指干预或停止通过以实现影响、去除或灭活。
本文所用的″对数下降值″或″LRV″应该是指生物体在流入物中的数目除以生物体在经过过滤器的排放物中的数目的常用对数值。
本文所用的″金属″应该意味着包括给定金属元素的盐、胶体、沉淀物、基底金属和所有的其它形式。
本文所用的″微生物截取增强过滤介质″应该是指具有微孔结构的过滤介质，其中微孔结构的至少一部分用微生物截取增强剂处理。
本文所用的″微生物截取增强剂″应该是指具有与其缔合的抗衡离子的阳离子材料并结合有生物活性金属。
本文所用的″微生物″应该是指可悬浮在流体中的任何活的生物体，包括但不限于细菌，病毒，真菌，原生动物，及其生殖形式包括孢囊和孢子。
本文所用的″微孔结构″应该是指平均流动通道低于约2.0微米，和通常低于约1.0微米的结构。
本文所用的″天然有机物质″或″NOM″应该是指通常存在于可饮或非可饮水中的有机物质，其一部分能够降低或抑制带正电荷的过滤介质的流动，或ξ电势。示例性NOM是聚阴离子酸如但不限于腐殖酸和灰黄霉酸。
本文所用的″无纺布″是指网或织物或具有相互叠放(但不以针织或织制织物中的高度组织化方式)的各个纤维的结构的其它介质。无纺网一般可通过本领域熟知的方法而制成。这些方法的例子包括但不限于熔体吹制，纺粘，梳理和气流成网。
本文所用的″颗粒″应该是指尺寸范围从胶体至肉眼可见，且对形状没有特别限制但一般具有有限长/宽比的固体。
本文所用的″预过滤器″应该是指一般位于其它过滤层、结构或设备的上游和能够在流入物接触随后过滤层、结构或设备之前降低颗粒污染物的过滤介质。
本文所用的″晶须″应该是指具有有限的纵横比且介于颗粒和纤维的纵横比之间的一种长丝。有关纤维的任何讨论还应该理解为包括晶须。
微生物截取增强过滤介质
本发明过滤介质具有微孔结构，通过使用合适的孔结构和化学处理的组合而提供微生物截取能力。微孔结构包含具有特定孔结构以及吸附剂和/或吸收剂性能的活性颗粒排列。该排列可以是使用粘结剂或承载纤维成型到粘附介质中的粘结或固定颗粒的实心复合块、整块、陶瓷棒、平板复合体和类似物。这些颗粒排列可通过本领域已知的工艺例如挤塑、模塑或滑移浇铸而制成。用于处理微孔结构的表面的化学处理工艺利用阳离子材料和生物活性金属之间的协同相互作用，这样在组合时对所接触的微生物污染物提供广谱降低作用。阳离子材料向过滤介质所提供的电荷有助于微生物污染物的电-动力学截取，而紧密的孔结构提供短扩散通道和因此流动流体中的微生物污染物至微孔结构表面的快速扩散动力学。微孔结构还提供对微生物污染物的补充直接机械截取。对于极小颗粒的截取，由于扩散起主要作用，病毒颗粒的对数下降值和流入物在过滤介质内的接触时间之间有直接关系，而不是取决于过滤介质的厚度。
微生物截取增强过滤介质的特性
为了提供充分的微生物截取能力，本发明微生物截取增强过滤介质的平均流动通道低于约2微米，和更优选低于或等于约1微米。如果平均流动通道大于约2微米，那么病毒颗粒的扩散效率快速下降且不能有效地生物截取。本发明微生物截取增强过滤介质的量与流过过滤介质的流体的流速相比必须足以提供适合污染物扩散至过滤介质表面的接触时间。为了提供对大多数带负电荷的微生物的增加的电-动力学截取，微孔结构的至少一部分涂有阳离子材料以在至少一部分这些微孔结构上产生正电荷。阳离子材料具有足够的分子尺寸以防对活性颗粒的微孔和中孔的污染。
通过使用基本上去除NOM的吸附剂预过滤器而优选阻止可减少或去除微生物截取增强过滤介质上的电荷的天然有机物质(NOM)，如聚阴离子酸(即腐殖酸或灰黄霉酸)接触电荷微孔结构。可以将NOM去除材料直接引入微生物截取增强过滤介质，从而消除对单独的吸附剂预过滤器的需求。另外，根据所用活性颗粒的种类，微生物截取增强过滤介质自身的上游部分也可自然地减少或去除NOM并防止微生物截取增强过滤介质的下游部分的性能损失。
如果用于重力流动水过滤体系，优选的是微生物截取增强过滤介质由亲水材料制成或用润湿剂处理以提供良好的自发可润湿性。另外，在其它场合中，微生物截取增强过滤介质可根据需要被处理以提供亲水或憎水特性。微生物截取增强过滤介质有可能具有带正荷和负电荷的和未带电荷的区域，和/或亲水和憎水区域。例如，带负电荷的区域可用于增加不太常见的带正电荷的污染物的截取和未带电荷的憎水区域可用于提供吸引到憎水表面的污染物的增强截取。
活性颗粒
本发明具有增强的微生物截取能力的微生物截取增强过滤介质包含具有颗粒尺寸分布为80×325目和约20％-约24％盘(pan)的吸附剂和/或吸收剂活性颗粒(小于-325目的颗粒)的排列。活性颗粒可包括但不限于此活性炭，活化矾土，沸石，硅藻土，硅酸盐，硅铝酸盐，钛酸盐，骨炭，钙羟基磷灰石，氧化锰，氧化铁，氧化镁，珍珠岩，滑石，聚合物颗粒，粘土，碘化树脂，离子交换树脂，陶瓷，超吸收聚合物(SAPs)和其组合。具有必需性能的微生物截取增强过滤介质可通过合并一种或多种这些活性颗粒而得到。
一种优选的微孔结构包含活性炭的活性颗粒，它天然地耐受NOM的污染并有效地吸附微孔结构的外周区域中的可能影响的NOM，同时保护内区域。优选，活性炭是酸洗涤烟煤基活性炭。适用于本发明的市售活性炭可以商品名TOG-NDS得自Calgon CarbonCorporation(Pittsburgh，Pa.)，或以商品名1240ALC得自Calif.Carbon Company(Wilmington，California)。最优选，活性颗粒由具有如下颗粒尺寸分布的来自Calgon Carbon Corporation的酸洗涤烟煤基活性炭组成：约3％-约7％，优选约5％的80目尺寸颗粒；约12％-约18％，优选约15％100目；约44％-约50％，优选47％200目；约8％-约14％，优选约11％325目；和约20％-约24％盘，优选约22％盘(pan)。
微生物截取增强剂
微孔结构的活性颗粒用能够在活性颗粒的表面上产生正电荷的微生物截取增强剂化学处理。化学处理在处理表面上产生例如使用流动电势分析测定的强正电荷且该正电荷在低于10的pH值下保持。通过将活性颗粒用阳离子材料处理，阳离子金属配合物在活性颗粒的至少一部分表面上形成。阳离子材料可以是带电的小分子或沿着聚合物链长度具有带正电荷的原子的线型或支化聚合物。
如果阳离子材料是聚合物，电荷密度优选大于约1带电原子/约每20埃，优选大于约1带电原子/约每10埃，和更优选大于约1带电原子/约每5埃分子长度。阳离子材料上的电荷密度越高，与其缔合的抗衡离子的浓度越高。高浓度的合适的抗衡离子可用于驱使金属配合物沉淀。阳离子聚合物的高电荷密度提供吸附和明显逆转活性颗粒如碳的正常负电荷的能力。无论在高或低pH环境中，阳离子材料应该始终向微孔结构提供高度正电性的表面，例如通过流动或ξ电势分析器测定。
具有足够高分子量的聚合物的使用能够处理活性颗粒的表面而不会严重地影响活性颗粒的中孔和微孔的吸附能力。阳离子材料可具有大于或等于约5000道尔顿，优选大于或等于100,000道尔顿，更优选大于或等于约400,000道尔顿的分子量，和可大于或等于约5,000,000道尔顿。
阳离子材料包括但不限于此季铵化胺，季铵化酰胺，季铵盐，季铵化酰亚胺，苄烷铵化合物，双胍，阳离子氨基硅化合物，阳离子纤维素衍生物，阳离子淀粉，季铵化聚二醇胺缩合物，季铵化胶原多肽，阳离子甲壳质衍生物，阳离子瓜尔胶，胶体如阳离子蜜胺-甲醛酸胶体，无机处理过的硅石胶体，聚酰胺-表氯醇树脂，阳离子丙烯酰胺，聚合物和其共聚物，其组合，和类似物。可用于该应用的电荷分子可以是具有单个电荷单元和能够连接到微孔结构的至少一部分上的小分子。阳离子材料优选具有一个或多个与其缔合的抗衡离子，在暴露于生物活性金属盐溶液时使得靠近阳离子表面的金属优先沉淀以形成阳离子金属沉淀物配合物。
示例性胺可以是吡咯，表氯醇衍生的胺，其聚合物，和类似物。示例性酰胺可以是公开于国际专利申请No.WO 01/07090的那些聚酰胺，和类似物。示例性季铵盐可以是二烯丙基二甲基卤铵化的均聚物，表氯醇衍生的聚季胺聚合物，衍生自二胺和二卤化物的季铵盐，例如公开于美国专利2,261,002,2,271,378,2,388,614，和2,454,547(在此将其作为参考引入本发明)，和公开于国际专利申请No.WO 97/23594(也在此将其作为参考引入本发明)的那些，聚六亚甲基二甲基溴化铵，和类似物。阳离子材料可化学键接、吸附、或交联至自身和/或至活性颗粒。
另外，适用作阳离子材料的其它材料包括得自BioShieldTechnologies，Inc.，Norcross，Georgia的BIOSHIELD。BIOSHIELD是一种有机硅烷产品，包括约5％重量的十八烷基氨基二甲基三甲氧基甲硅烷基丙基氯化铵和低于3％的氯丙基三甲氧基硅烷。可以使用的另一材料是SURFACINE，其得自Surfacine Development CompanyLLC，Tyngsboro，Massachusetts。SURFACINE包含一种通过使聚(六亚甲基双胍)(PHMB)与4，4’-亚甲基-二-N，N-二缩水甘油苯胺(MBGDA)(交联剂)反应以将PHMB共价键接到聚合物表面上而得到的三维聚合物网状结构。碘化银形式的银被引入该网状结构，和作为亚微米尺寸的颗粒被截留。该组合是一种可用于本发明的有效的杀虫剂。根据活性颗粒，MBGDA可以或不可以将PHMB交联至微孔结构。
阳离子材料暴露于生物活性金属盐溶液使得金属配合物沉淀到至少一些活性颗粒的至少一部分表面上。为此，生物活性的金属是优选的。这些生物活性金属包括但不限于此银，铜，锌，镉，汞，锑，金，铝，铂，钯，和其组合。最优选的生物活性金属是银和铜。优选选择生物活性金属盐溶液使得阳离子材料的金属和抗衡离子基本上不溶于含水环境以驱使金属配合物沉淀。优选，金属的存在量是总组合物的约0.01％-约2.0％重量。
尤其有用的微生物截取增强剂是银-胺-卤化物配合物。阳离子胺优选为具有分子量约400,000道尔顿的二烯丙基二甲基卤铵化的均聚物或具有类似电荷密度和分子量的其它季铵盐。可用于本发明的二烯丙基二甲基氯化铵的均聚物可以商品名MERQUAT100购自NalcoChemical Company(Naperville，Illnois)。氯抗衡离子可被替代为溴或碘抗衡离子。如果与硝酸银溶液接触，银-胺-卤化物配合物沉淀在微生物截取增强过滤介质的微孔结构的至少一部分活性颗粒上。
如果活性颗粒包含活性炭，则阳离子材料优选具有高电荷密度和足够的高的分子量以产生与活性炭的带负电荷的表面基团的强吸引和高配位能量。另外，在存在生物活性金属的胶体的情况下使用活性炭的带电荷表面增强的截取通过活性炭的憎水吸附机理而补充。该憎水机理一般耐受NOM的污染影响，和在高离子强度的条件下实际上更有效。碳表面的未处理部分利用其富氧化学往往具有可连续吸附带正电荷的颗粒的负电荷。正、负和憎水表面的组合为小颗粒的通过提供几乎不可逾越的障阻。在用微生物截取增强剂处理碳之后，生物活性金属和其缔合的抗衡离子在活性颗粒上的存在可使用X-射线荧光检测。
制造微生物截取增强过滤介质的方法
本发明微生物截取增强过滤介质可按照本领域熟练技术人员已知的工艺制备。这些工艺包括挤塑，模塑，滑移浇铸，固定活性颗粒在基材上和类似工艺。示例性工艺公开于美国专利5,019,311，和5,792,513.
使用本领域熟练技术人员已知的方式(例如喷涂)用阳离子材料处理活性颗粒。优选，活性颗粒涂有总重的约0.5％-约3％重量，和更优选约1％重量的微生物截取增强过滤介质。一旦阳离子材料涂覆到至少一部分活性颗粒上，则将颗粒暴露于生物活性金属盐。金属盐的溶液渗入颗粒以使生物活性金属沉淀在活性颗粒的至少一部分表面上。沉淀工艺精确地将阳离子涂层附近的大部分金属胶体直接沉积，因为与该涂层缔合的抗衡离子与所施用的金属盐反应以形成胶体颗粒。金属盐可喷涂到处理过的颗粒上或使用本领域熟练技术人员已知的其它方法施用。阳离子材料和金属盐的溶液优选用几乎无离子的水制备，这样与阳离子材料缔合的抗衡离子被牢固地吸引到处理过的活性颗粒的阳离子表面上并消除可造成生物活性金属不受控制地沉淀在远离阳离子表面的位置上的非所需离子。
随后一般在加热或在真空下从颗粒中去除过量水分至所需水分含量。优选，水分含量应该低于约10％，和更优选低于约5％，如果颗粒随后使用热塑性粘结剂挤出或模塑。
一旦微生物截取增强剂涂覆到至少一部分活性颗粒上，则将活性颗粒研磨至所需尺寸和可能地与粘结剂材料混合以形成匀质混合物，然后将活性颗粒固定成具有所需微孔结构的所需最终形式。选择粘结剂使得粘结剂材料的熔点足够低于活性颗粒的熔点，这样微生物截取增强过滤介质可被加热以活化粘结剂材料，同时微孔结构不会熔化和因此损失孔隙率。粘结剂颗粒优选充分均匀地分布在整个活性颗粒中，使得随后在转化成微孔结构时粘结剂颗粒截留或键接至基本上所有的活性颗粒上。
在本发明中可用于将活性颗粒凝固成微孔结构的粘结剂材料可潜在地包括纤维、粉末或颗粒形式的本领域已知的任何热塑性或热固性材料。有用的粘结剂材料可包括材料如但不限于聚烯烃，聚乙烯基卤化物，聚乙烯基酯，聚乙烯基醚，聚乙烯基硫酸酯，聚乙烯基磷酸酯，聚乙烯基胺，聚酰胺，聚酰亚胺，聚噁二唑，聚三唑，聚碳酰二亚胺，聚砜，聚碳酸酯，聚醚，聚亚芳基氧化物，聚酯，聚芳基化物，酚醛树脂，蜜胺-甲醛树脂，甲醛-脲，乙基-乙烯基乙酸酯共聚物，其共聚物和嵌段互聚物，和其组合。以上材料和其它有用的聚合物的变型包括基团如羟基，卤素，低级烷基，低级烷氧基，单环状芳基和类似物的取代。
可用于本发明的粘结剂的更详细列举可包括封端聚缩醛，如聚甲醛，聚三氯乙醛，聚正戊醛，聚乙醛，和聚丙醛；丙烯酸聚合物，如聚丙烯酰胺，聚丙烯酸，聚甲基丙烯酸，聚丙烯酸乙酯，和聚甲基丙烯酸甲酯；氟碳聚合物，如聚四氟乙烯，全氟化乙烯-丙烯共聚物，乙烯-四氟乙烯共聚物，聚氯三氟乙烯，乙烯-氯三氟乙烯共聚物，聚偏二氟乙烯，和聚氟乙烯；聚酰胺，如聚6-氨基己酸或聚e-己内酰胺，聚亚己基己二酰胺，聚亚己基癸二酰胺，和聚11-氨基十一酸；聚芳酰胺，如聚亚氨基-1，3-亚苯基亚氨基异邻苯二甲酰或聚间-亚苯基异邻苯二甲酰胺；聚对亚苯基二甲基，如聚-2-亚二甲苯基，和聚氯-1-亚二甲苯基；聚芳基醚，如聚氧基-2，6-二甲基-1，4-亚苯基或聚对苯氧；聚芳基砜，如聚氧基-1，4-亚苯基磺酰基-1，4-亚苯基氧基-1，4-亚苯基亚异丙基-1，4-亚苯基，和聚磺酰基-1，4-亚苯基-氧基-1，4-亚苯基磺酰基-4，4’-二亚苯基；聚碳酸酯，如聚双酚A或聚羰基二氧基-1，4-亚苯基亚异丙基-1，4-亚苯基；聚酯，如聚对苯二甲酸乙二醇酯，聚对苯二甲酸丁二醇酯，和聚亚环己基-1，4-二亚甲基对苯二甲酸酯或聚氧基亚甲基-1，4-环亚己基亚甲基氧基对苯二甲酰；聚芳基硫化物，如聚对亚苯基硫或聚硫代-1，4-亚苯基；聚酰亚胺，如聚均苯四亚氨基-1，4-亚苯基；聚烯烃，如聚乙烯，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，和聚4-甲基-1-戊烯；乙烯基聚合物，如聚乙酸乙烯酯，聚偏二氯乙烯，和聚氯乙烯；二烯聚合物，如1，2-聚-1，3-丁二烯，1，4-聚-1，3-丁二烯，聚异戊二烯，和聚氯丁二烯；聚苯乙烯；以及前述的共聚物，如丙烯腈丁二烯-苯乙烯(ABS)共聚物。可以使用的聚烯烃包括聚乙烯，线型低密度聚乙烯，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，和类似物。
其它潜在可使用的材料包括聚合物如聚苯乙烯和丙烯腈-苯乙烯共聚物，苯乙烯-丁二烯共聚物，和其它非结晶或无定形聚合物和结构。
优选的粘结剂材料包括聚乙烯，聚乙烯乙酸乙烯酯和尼龙。尤其优选的粘结剂是以商品名MICROTHENEF得自EquistarChemicals，L.P.，Tuscola，Illinos的FN 510级微细聚乙烯。
粘结剂可具有的平均颗粒尺寸为约0.1微米-约250微米，优选约1微米-约100微米，和更优选约5微米-约20微米。优选的是，粘结剂材料的软化点明显低于活性颗粒的软化点，这样微生物截取增强过滤介质可被加热以活化粘结剂材料，同时微孔结构不会熔化和因此损失孔隙率。
粘结剂材料的用量取决于微孔结构是通过挤塑、模塑或其它工艺如何形成。例如，如果活性颗粒挤出或模塑成实心复合块，则粘结剂材料的存在量优选为微生物截取增强过滤介质的约15％-约22％重量，和更优选约17％-约19％重量。如果活性颗粒被固定到基材(例如无纺材料)上，则粘结剂材料的存在量优选为总组合物的约5％-约20％，和优选约9％-约15％重量。
颗粒、纤维、晶须或粉末形式的一种或多种添加剂也可与活性颗粒混合以有助于对其它污染物的吸附或吸收或参与形成微孔结构和截取微生物污染物。有用的添加剂可包括但不限于金属颗粒，活化矾土，活性炭，硅石，聚合物粉末和纤维，玻璃珠粒或纤维，纤维素纤维，离子交换树脂，工程树脂，陶瓷，沸石，硅藻土，活化铝土矿，漂白土，硫酸钙，其它吸附剂或吸收剂材料，或其组合。添加剂也可根据特定应用被化学处理以产生微生物截取能力。这些添加剂优选以足以使得在用于过滤用途时所得微生物截取增强过滤介质中的流体流动基本上不受阻碍的量存在。添加剂的量取决于过滤体系的特定用途。
另外，最终微孔结构可通过颗粒或纤维或其混合物的滑移浇铸或湿成型和随后使粘结剂或颗粒将这些成分烧结在一起而形成。在一些情况下，颗粒可例如在双组分纤维或低熔点树脂中形成其自身的粘结剂。在一些情况下，粘结剂可以是水溶性的或可交联的树脂或盐，其在干燥或加热或反应时形成所需键。也可使用化学粘结剂以及沉淀粘结剂如某些磷酸盐。
采用微生物截取增强过滤介质的过滤体系
本发明微生物截取增强过滤介质可容易被引入采用被固定作为实心复合块、平板、螺旋或折叠片材、整块或棒的颗粒过滤介质的现有技术过滤体系中。优选，颗粒预过滤器与微生物截取增强过滤介质结合使用，其位于微生物截取增强过滤介质的上游，在流入物接触微生物截取增强过滤介质之前尽可能多地去除流入物中的颗粒污染物。
实施例
以下实施例用于说明本发明而不应理解为限定本发明的范围。
孔隙学研究使用得自Porous Materials Inc.，Ithaca，N.Y.的自动毛细管流动孔隙计进行。使用由设备制造商公开的标准步骤测定的参数包括平均流动孔尺寸和透气(空气)性。在可变压力下在干和湿微生物截取增强过滤介质上分析空气流动。
微生物截取增强过滤介质的细菌挑战使用美国模式培养物保藏所(ATCC)No.11775的大肠杆菌的悬浮液进行以评估对细菌挑战的响应。对病毒挑战的响应使用MS2噬菌体ATTC No.15597-Bi评估。所测试的其它微生物包括Brevundimonas diminuta ATCC No.4335，枯草杆菌(还称作BG，ATCC No.9375)。使用ATCC的标准操作步骤繁殖细菌和噬菌体，并使用本领域熟知的标准微生物步骤制备和量化受到微生物悬浮液挑战的过滤器的流入物和排放物中的微生物。
各个过滤器使用每种微生物在NSF国际标准53孢囊减少试验程序的改进形式下重复试验。设计该程序用于评定过滤器在加速暴露于细颗粒以模拟污垢聚集时的性能。过滤器用反渗透/去离子(RO/DI)水冲洗并校正至起始流速0.5-1.0加仑/分钟(gpm)。过滤介质的平均流动通道是约0.9微米-1.1微米。
在试验过程中，起始样品在起动体系流动过程中取自流入物和排放物取样孔以确保没有来自不当消毒试验装置的背景干扰。过滤器随后用微生物的悬浮液挑战，其中样品在最低2L挑战溶液之后取样，确保挑战水在取样之前通过整个试验台。
所有的流入物和排放物样品根据需要连续稀释并一式三份制板。在某些情况下，将给定设计的碳块在几种流速下进行测试以确定它们对改变流速的响应。
如下制备出具有增强的微生物截取能力的活性炭块过滤器。将20磅12×40目酸洗烟煤基活性炭(得自Calgon Carbon Company)与3％MERQUAT100在去离子水中的溶液温和地混合以充分涂覆碳颗粒并确保MERQUAT100已吸附到至少一部分碳颗粒上。然后，将70g结晶硝酸银在1.0L去离子水中的溶液加入MERQUAT处理过的碳以使银以氯化银胶体形式沉淀在碳颗粒的至少一部分表面上。将处理过的碳颗粒在135℃下干燥直至低于5％的水分存在于碳颗粒中。干燥时间在约3-约5小时之间改变。将干燥碳在双辊研磨机中磨碎至80×325目尺寸，具有约14％重量-325目盘，然后与FN510(低密度聚乙烯粘结剂材料)在约17％重量下混合。混合物在例如描述于美国专利5,019,311的合适的热、压力和温度条件下挤出。将具有各种尺寸的所得碳块过滤器通过使用热熔树脂施用合适的顶盖而用于构建水过滤体系，这是本领域熟知的。
过滤器在起始清洁条件下并随后在污垢聚集之后间隔地分析微生物截取性能，其中与原始的清洁过滤器所测定的流速相比流量减少25％，50％和75％。
为了实现流量的所需下降，采用"标称"试验粉剂挑战水。标称试验粉剂是一种颗粒直径约0-5.0微米且96％重量颗粒在该范围内和20％-40％颗粒大于2.5微米的硅酸盐粉末。如果已实现所需流动下降，则省略标称试验粉剂挑战并将过滤器用4.0L反渗透/去离子(RO/DI)水冲洗以去除流入物和排放物线中的任何残余试验粉剂。随后如上所述用微生物的悬浮液挑战过滤器。
本发明微生物截取增强过滤介质的效力在下表I和II中给出。
表I
微生物截取增强活性炭块过滤介质的LRVs
    实施例  过滤器尺寸O.D.×I.D.×长度(英寸)     流速(gpm)   B.diminuta(LRV)     大肠杆菌(LRV)     B.subtilis(LRV)     MS2(LRV)
    1  1.85×0.375×2.94     0.50     3.82
    2  1.375×0.375×4.735     0.25   8.20     4.83
    3  1.85×0.50×2.94     0.75     2.15
    4  2.00×0.75×2.55     0.75     4.92
    5  2.25×1.00×4.00     0.50   8.49     8.88     8.97     8.35
    6  2.40×1.19×9.628     1.0     5.79
    7  1.50×0.375×6.055     0.50   8.80     5.31
    8  1.50×0.375×6.055     0.60     3.51
    9  1.50×0.375×6.055     0.75     8.79     3.16
    10  2.00×0.50×5.82     0.50   9.45     9.45     9.46     9.27
表II
微生物截取增强活性炭块过滤介质在起始和下降的流速下的LRVs
  实施例   起始流速(gpm)     过滤器尺寸0.D.×I.D.×长度(英寸)   流速下降   大肠杆菌(LRV)   MS2(LRV)
  11   0.50     2.50×1.25×7.236   0％   8.39   5.14
  25％   8.46   5.73
  50％   8.48   5.26
  75％   8.61   6.99
  12   0.50     1.50×0.375×6.055   0％   5.31
  25％
  50％   7.03
  75％   8.17
  13   0.60     1.50×0.375×6.055   0％   3.52
  25％   4.88
  50％   4.89
  75％   5.71
  14   0.75     1.50×0.375×6.055   0％   8.79   3.16
  25％   8.79   4.27
  50％   8.76   4.08
  75％   8.74   4.86
  15   0.50     2.25×1.00×4.00   0％   8.88   8.35
  25％   8.88   9.50
  50％   8.87   8.34
  75％   8.91   8.22
  16   0.50     2.00×0.50×5.82   0％   9.45   9.27
  25％   9.41   9.25
  50％   9.48   9.25
  75％   9.44   9.25
本发明微生物截取增强活性炭块过滤介质对于较大微生物如B.diminuta，大肠杆菌和B.subtilis提供大于8的对数下降值。实际上，对这些微生物的截取在所有情况下超出的试验程序的敏感度。MS2渗透的结果表明壁厚度和截取水平之间没有明显关联。这表明传统机械截取机理不适用于MS2截取。但过滤器的log截取和空床接触时间(EBCT)之间存在直接关系。图1给出了起始清洁过滤器的MS2的对数下降和过滤器的EBCT之间的明显线性关系，表明一种扩散截取机理，同时要求约6秒的EBCT以实现该噬菌体在具有平均流动通道约0.9-约1.1微米的微生物截取增强过滤介质中的有效下降。为此，在较低流速下操作的较大过滤器比在升高的流速下操作的小过滤器更有效。
尽管本发明已结合特定优选的实施方案被具体描述，但本领域熟练技术人员根据上文描述显然看出许多替换，修改和变化。因此认为，所附权利要求书包括落入本发明真实范围和主旨内的任何这些替换，修改和变化。

Claims (20)

1.一种过滤介质，包括：
包含活性颗粒排列的微孔结构，所述微孔结构的平均流动通道低于约2微米；和
微生物截取增强剂，包括吸附在所述微孔结构的至少一部分上的、具有中至高电荷密度和分子量大于约5000道尔顿的阳离子材料，和直接接近阳离子材料而且也在所述微孔结构的至少一部分上的生物活性金属。
2.根据权利要求1的过滤介质，其中活性颗粒由活性炭、活化矾土、沸石、硅藻土、硅酸盐、硅铝酸盐、钛酸盐、骨炭、钙羟基磷灰石、氧化锰、氧化铁、氧化镁、珍珠岩、滑石、聚合物颗粒、粘土、碘化树脂、离子交换树脂、陶瓷或其组合组成，和进一步包括粘结剂。
3.根据权利要求1的过滤介质，其中所述微孔结构具有低于或等于约1微米的平均流动通道。
4.根据权利要求1的过滤介质，其中微生物截取增强剂通过将至少一部分所述微孔结构用具有与其缔合的抗衡离子的阳离子材料处理，随后将生物活性金属用至少一部分与阳离子材料缔合的抗衡离子沉淀而形成。
5.根据权利要求4的过滤介质，其中阳离子材料包含分子量大于或等于约400,000道尔顿的二烯丙基二甲基氯化铵的均聚物。
6.根据权利要求1的过滤介质，其中所述微孔结构包括活性颗粒的实心复合块，或固定的活性颗粒的平板结构。
7.根据权利要求1的过滤介质，其中所述微孔结构通过挤塑、模塑、滑移浇铸、粉末涂覆、湿成型或干成型活性颗粒而形成。
8.根据权利要求1的过滤介质，其中当流入物与所述过滤介质的空床接触时间低于约12秒时，所述过滤介质提供大于约6的流入物中微生物污染物的对数下降。
9.一种过滤体系，包括：
具有入口和出口的外壳；
位于外壳内的与入口和出口流体连通的过滤介质，所述过滤介质包含：
平均流动通道低于约2微米的微孔结构，其包含活性炭、活化矾土、沸石、硅藻土、硅酸盐、硅铝酸盐、钛酸盐、骨炭、钙羟基磷灰石、氧化锰、氧化铁、氧化镁、珍珠岩、滑石、聚合物颗粒、粘土、碘化树脂、离子交换树脂、陶瓷或其组合的活性颗粒；和
微生物截取增强剂，其包含具有高电荷密度、分子量大于约5000道尔顿和具有与其缔合的抗衡离子的阳离子材料，所述阳离子材料吸附在微孔结构的至少一部分上，和其中使用至少一部分与阳离子材料缔合的抗衡离子使生物活性金属沉淀；
其中流过外壳和接触过滤介质的微生物污染的流入物在流出外壳的排放物中具有至少约4的微生物污染物的对数下降。
10.根据权利要求9的过滤体系，其中微孔结构的活性颗粒是实心复合块，或固定的活性颗粒的平板结构。
11.根据权利要求9的过滤体系，其中微孔结构的活性颗粒被滑移浇铸、湿成型或干成型。
12.一种制造具有增强的微生物截取能力的过滤介质的方法，包括步骤：
提供平均颗粒尺寸约0.1微米-约5,000微米的活性颗粒；
将活性颗粒用包含具有高电荷密度和分子量大于约5000道尔顿的阳离子材料的微生物截取增强剂并结合生物活性金属进行处理；和
将处理的活性颗粒成型为平均流动通道低于约2微米的微孔结构。
13.一种制造具有增强的微生物截取能力的过滤介质的方法，包括步骤：
提供平均颗粒尺寸约0.1微米-约5,000微米的活性颗粒；
将活性颗粒凝聚成平均流动通道低于约2微米的微孔结构；和
将微孔结构用包含具有高电荷密度和分子量大于约5000道尔顿的阳离子材料的微生物截取增强剂并结合生物活性金属进行处理。
14.根据权利要求12或13的方法，其中提供活性颗粒的步骤包括提供活性炭、活化矾土、沸石、硅藻土、硅酸盐、硅铝酸盐、骨炭、钙羟基磷灰石、氧化锰、氧化镁、珍珠岩、滑石、聚合物颗粒、粘土或其组合的活性颗粒，和进一步包括加入粘结剂的步骤。
15.根据权利要求12或13的方法，其中处理步骤包括以下步骤：
将至少一部分微孔结构或活性颗粒用具有与其缔合的抗衡离子阳离子材料涂覆；和
使生物活性金属与至少一部分与阳离子材料缔合的抗衡离子在至少一部分微孔结构或活性颗粒上沉淀。
16.根据权利要求12或13的方法，其中在处理步骤中，阳离子材料选自胺、季铵盐、苄烷铵化合物、双胍、氨基硅化合物、其聚合物和其组合。
17.根据权利要求12或13的方法，其中在处理步骤中，生物活性金属选自银、铜、锌、镉、汞、锑、金、铝、铂、钯和其组合。
18.根据权利要求12或13的方法，其中使活性颗粒成型或凝聚成微孔结构的步骤包括将活性颗粒挤塑、滑移浇铸、或固定成平板结构。
19.一种从流体中去除微生物污染物的方法，包括：
提供一种的过滤介质，其包括：包含活性颗粒和具有低于约2微米的平均流动通道的微孔结构；和吸附在所述多孔结构的至少一部分上的微生物截取增强剂，其包含具有中至高电荷密度和分子量大于约5000道尔顿的阳离子材料以及生物活性金属；
使微生物污染的流体接触过滤介质至低于或等于约12秒的时间；和
得到具有大于约4的微生物污染物对数下降值的排放物。
20.权利要求19的方法，其中在提供过滤介质的步骤中，微孔结构包含包括活性炭的活性颗粒。
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EP1470083B1 (en) 2008-03-26
MXPA03010212A (es) 2004-03-10
DE60319952D1 (de) 2008-05-08
KR100917075B1 (ko) 2009-09-15
CA2444808C (en) 2009-12-22
TWI284055B (en) 2007-07-21
US6630016B2 (en) 2003-10-07
JP5244867B2 (ja) 2013-07-24
US20030140785A1 (en) 2003-07-31
ATE390389T1 (de) 2008-04-15
IL158362A (en) 2007-09-20
WO2003064330A1 (en) 2003-08-07
BR0302962A (pt) 2004-07-06
BR0302962B1 (pt) 2012-11-27
HK1065303A1 (en) 2005-02-18
CN1232333C (zh) 2005-12-21
IL158362A0 (en) 2004-05-12
JP2005515892A (ja) 2005-06-02
AU2003202859B2 (en) 2008-01-31
JP2010279945A (ja) 2010-12-16
EP1470083A4 (en) 2005-11-02
EP1470083A1 (en) 2004-10-27
TW200400077A (en) 2004-01-01
CA2444808A1 (en) 2003-08-07

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