CN1278757C - 预涂层过滤介质及制备和使用方法 - Google Patents

预涂层过滤介质及制备和使用方法 Download PDF

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Publication number
CN1278757C
CN1278757C CNB038030195A CN03803019A CN1278757C CN 1278757 C CN1278757 C CN 1278757C CN B038030195 A CNB038030195 A CN B038030195A CN 03803019 A CN03803019 A CN 03803019A CN 1278757 C CN1278757 C CN 1278757C
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Prior art keywords
filtration adjuvant
cationic materials
composition
fiber
microbiological interception
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Expired - Fee Related
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CNB038030195A
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CN1625428A (zh
Inventor
E·E·科斯洛
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KX Technologies LLC
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Koslow Technologies Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
    • C02F1/505—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment by oligodynamic treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/0005—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts
    • A61L2/0011—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts using physical methods
    • A61L2/0017—Filtration
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/0005—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts
    • A61L2/0082—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts using chemical substances
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
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    • A61L9/00—Disinfection, sterilisation or deodorisation of air
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    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249982—With component specified as adhesive or bonding agent

Abstract

本发明涉及包括微生物拦截增强过滤助剂的预涂层或主体原料组合物。优选微生物拦截增强过滤助剂包括在其至少一部分表面上涂布微生物拦截增强剂的原纤化Lyocell纳米纤维。微生物拦截增强剂包括与生物活性金属结合的阳离子材料。单独或与主体未处理的过滤助剂结合采用微生物拦截增强过滤助剂实现细菌拦截至少约4的对数下降。包括微生物拦截增强过滤助剂的预涂层可用于饮料的一步冷冻灭菌。

Description

预涂层过滤介质及制备和使用方法
本发明涉及用于从液体、尤其是饮料中分离固体的预涂层过滤体系中有用的过滤助剂。
过滤的机械方法典型地通过物理排阻操作。污染的流入液流经多孔介质，所述多孔介质保留尺寸比多孔介质孔径大的颗粒并允许含有尺寸小于多孔介质孔径的颗粒的流出液流过。在截留被污染的流入液中的最小可能颗粒与流入液流经多孔介质的流速之间存在平衡，其中必须实现该平衡，以提供高的产量。
已知现有技术使用多孔床或粉末过滤体系过滤饮料、尤其是发酵饮料。例如，啤酒或白酒在发酵后被过滤以除去酵母和其它引起混浊的材料，以实现胶体和微生物的稳定性。在粉末过滤过程中，在隔膜上形成过滤助剂的预涂层，一种通常具有特定孔径的多孔材料如硅藻土或纤维素纤维。当过滤助剂的分散液流过隔膜时，太大的过滤助剂纤维或颗粒不能流过隔膜的孔，结果在隔膜上累积，从而形成滤饼。比隔膜孔小的过滤助剂纤维或颗粒将最终在较大过滤助剂纤维或颗粒后面存留，从而在滤饼内提供用于最佳过滤的孔径分布。
为了提供流体的深度精制，单次过滤流过是不足的，因此，需要多次过滤步骤。为了除去微生物污染物，如在制备发酵饮料中使用的酵母，过滤器的孔径必须小于10微米。此外，冷冻灭菌技术要求小于约2微米的孔径。使用预涂层的现有技术的过滤体系，在没有使用多步过滤步骤提供流体的深度精制或提供单步冷冻灭菌流体方面，尚未获得成功。
发明概述
第一方面，本发明涉及包括过滤助剂的组合物，其中在该过滤助剂的至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料，其中在与阳离子材料直接相邻处用抗衡离子沉淀生物活性金属。
另一方面，本发明涉及包括下述的组合物：吸附剂、与吸附剂混合的过滤助剂，该过滤助剂在其至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料和在与该阳离子材料直接相邻处用抗衡离子沉淀的生物活性金属。
再一方面，本发明涉及过滤流入液的方法：提供支撑介质；用过滤助剂涂布该支撑介质，以形成预涂层，其中该过滤助剂在其至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料和在与阳离子材料直接相邻处用抗衡离子沉淀的生物活性金属；使流入液流过预涂层；在预涂层上保留来自流入液的污染物；和获得澄清的流出液。
优选实施方案的详述
定义
在整个说明书中，单数或复数形式的下述术语具有下述含义。
″吸收剂″是指能够主要通过将杂质吸引到其内部结构内而吸附杂质的任何材料。
″吸附剂″是指能够主要通过物理吸附到其表面上而吸附杂质的任何材料。本文中吸附剂包括纤维素纤维。
“主体(bulk)过滤助剂”是指没有电荷改性的常规用作预涂层的材料和/或主体原料成分的那些材料。这些材料包括但不限于活性炭、珍珠岩、硅藻土、纤维素、二氧化硅和类似物。
″污染物下降″是指以化学、机械或生物方式减少被拦截、除去、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。
“纤维”是指特征在于高长径比例如几百比一的固体。有关纤维的任何讨论包括晶须。
“过滤助剂”或“过滤助剂材料”是指用于从流体中除去污染物的预涂层过滤体系中可使用的材料。
“过滤介质”是指进行流体过滤的材料。
“流体”是指液体、气体或其结合。
″拦截(intercept)″或″拦截(interception)″认为是指干预或阻止流过，以实现改变、除去、灭活或影响。
″对数下降值″或″LRV″是指在流入液中的生物体数目除以在过滤器的流出液中的生物体数目的常用对数值。
″微生物拦截增强过滤助剂″是指包括带正电的过滤助剂的过滤助剂或它的一部分，其中在该过滤助剂的至少一部分上涂布与生物活性金属组合的阳离子材料。可添加额外的添加剂，以制备在其目的应用中更有用的微生物拦截增强过滤助剂。
″微生物拦截增强剂″是指具有与其缔合的抗衡离子的阳离子材料与生物活性金属的组合。
“微生物”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，及其繁殖形式，包括孢囊和孢子。
″颗粒″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。
″晶须″是指具有有限的长径比且介于颗粒和纤维的长径比之间的一种长丝。有关纤维的任何讨论包括晶须。
通用的预涂层组合物的特征
本发明的预涂层组合物包括微生物拦截增强过滤助剂，其中使用合适的孔结构和化学处理的组合，该过滤助剂提供增强的过滤，包括微生物拦截能力。微生物拦截增强过滤助剂当用作预涂层组合物的唯一成分时，提供小于约2微米的孔径，和可以小于约1微米。当与主体过滤助剂结合使用时，微生物拦截增强过滤助剂增强过滤器性能，延长过滤器寿命，并提供更坚实的滤饼。当微生物拦截增强过滤助剂与主体过滤助剂混合时，在至少一部分该材料上的孔径和电荷使得可拦截较小的污染物。通过以变化的用量组合微生物拦截增强过滤助剂与主体过滤助剂，可满足特定的过滤需求。微生物拦截增强过滤助剂也可用作主体原料成分。
微生物拦截增强过滤助剂包括能具有小于约2.0微米的平均流动通道的任何材料。优选地，微生物拦截增强过滤助剂包括用微生物拦截增强剂处理的单独的或结合的纳米纤维和/或晶须，或活性颗粒。由本发明的预涂层组合物提供的所得滤饼的致密孔结构提供从流体到滤饼表面的短扩散距离。处理微生物拦截增强过滤助剂所使用的化学处理方法利用阳离子材料与生物活性金属之间的协同相互作用，即当它们结合时，提供接触时的微生物污染物的广谱下降。阳离子材料提供给微生物拦截增强过滤助剂的电荷将提供微生物污染物的增强的电动拦截，而致密的孔结构提供短的扩散路径，并进而提供在流向预涂层组合物表面的流动流体内污染物的快速扩散动力学。微生物拦截增强过滤助剂还提供微生物污染物的补充直接机械拦截。
微生物拦截增强过滤助剂可由能在其表面的至少一部分上保留电荷的任何材料组成，其中电荷保留通过流动或ξ电势来确定。当预涂层组合物用于过滤饮料时，在水中不溶的食品安全的亲水材料是优选的。微生物拦截增强过滤助剂可以是有机或无机纤维、晶须、粉末和/或颗粒。优选微生物拦截增强过滤助剂可由活性炭、珍珠岩、硅藻土、纤维素、二氧化硅和类似物组成。处理微生物拦截增强过滤助剂所使用的化学处理方法利用阳离子材料与生物活性金属之间的协同相互作用，即当它们组合时，提供细菌污染物至少约3的对数下降。由阳离子材料提供给微生物拦截增强过滤助剂的电荷支持细菌污染物和在流出液中非所需的其它带负电的颗粒的电动拦截。
过滤助剂材料
本发明的预涂层组合物包括微生物拦截增强过滤助剂，该过滤助剂在其至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料和在与该阳离子材料直接相邻处用抗衡离子沉淀的生物活性金属。优选微生物拦截增强过滤助剂由多根纳米纤维和/或有机与无机材料的颗粒成分组成，其中所述材料包括但不限于聚合物树脂、离子交换树脂、工程树脂、硅酸盐、陶瓷、纤维素、云母、玻璃、金属、活化矾土、碳或活性炭、二氧化硅、沸石、硅藻土、珍珠岩、活性铝土矿、漂白土、钙羟基磷灰石、其它吸附材料或其结合。可以考虑有机和无机纤维和/或晶须或颗粒的结合且在本发明的范围内，例如可与能配制到预涂层组合物内的非常小的粒状吸附剂或颗粒一起使用玻璃、陶瓷、金属纤维和聚合物纤维。
预涂层组合物可以完全由微生物拦截增强过滤助剂组成或可仅仅含有一部分所述助剂。预涂层组合物的一个优选实施方案包括根据本发明处理的基本上为纳米纤维的过滤助剂材料。优选纳米纤维是加拿大标准游离度小于或等于约100和最优选小于或等于约45的纤维素或聚合物纤维。优选大部分纤维的直径应当小于或等于约1000纳米，更优选小于或等于约400纳米，和最优选直径小于或等于约250纳米的纤维。优选切断纤维到约1mm至约8mm的长度，优选约2mm至约6mm，和更优选约3mm至约4mm。最优选原纤化纤维，这是因为它们特别小的尺寸和潜在的低成本。
优选地，根据本发明加工的原纤化合成纤维素纤维可产生在本发明的预涂层组合物中使用的超细亲水微生物拦截过滤助剂。可通过在有机溶剂如氧化胺中直接溶解和纺丝木浆来制备这种原纤化纤维素纤维，和它被称为Lyocell纤维。Lyocell纤维的优点是以一致、均匀的方式生产，从而得到可重复的结果，这与例如天然纤维素纤维的情况不同。此外，Lyocell的原纤常常卷曲。卷曲提供大量的纤维缠结，从而导致显著残留的湿强度。另外，可使用中等投资成本的设备大量地生产原纤化Lyocell纤维。应当理解，除纤维素以外的纤维可被原纤化，以生产极细原纤，如合成纤维，尤其是丙烯酸或尼龙纤维，或其它天然纤维素材料。可在微生物拦截增强过滤助剂中使用原纤化和非原纤化纤维的组合。
微生物拦截增强剂
用能在过滤助剂材料的表面上产生正电荷的微生物拦截增强剂来化学处理过滤助剂材料。化学处理在处理表面上产生强的正电荷，这使用流动或ξ电势分析来确定，和这一正电荷在低于10的pH值下得到保留。阳离子材料可以是小的带电分子或在沿着聚合物链的长度方向上具有带正电荷的原子的直链或支链聚合物，其中所述聚合物链具有与其缔合的抗衡离子。阳离子材料吸附在过滤助剂材料的至少一部分上，和在与阳离子材料直接相邻处以及在至少一部分过滤助剂材料上用抗衡离子沉淀生物活性金属。
若阳离子材料是聚合物，则电荷密度优选大于约1个带电原子/约每30埃的分子长度，优选大于约1个带电原子/约每20埃分子长度，和更优选大于约1个带电原子/约每10埃分子长度。在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。可使用高浓度的合适抗衡离子以驱使生物活性金属的沉淀。阳离子材料的高电荷密度提供吸附和显著反转在制备微生物拦截增强过滤助剂中有用的原料的正常负电荷，阳离子材料不管在高或者在低pH环境下，应当始终给微生物拦截增强过滤助剂提供高度带正电的表面，这通过流动或ξ电势分析仪来确定。
使用足够高分子量的阳离子聚合物使得在没有严重地附带影响过滤助剂材料如活性炭的中孔(mezo-pore)和微孔的任何吸附能力的情况下，可处理微生物拦截增强过滤助剂的表面。阳离子材料的分子量可大于或等于约5000道尔顿，优选大于或等于100000道尔顿，更优选大于或等于约400000道尔顿，和可大于或等于约5000000道尔顿。
阳离子材料包括但不限于季铵化胺，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，阳离子瓜耳胶，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。可用于该应用的带电分子可以是具有单个带电单元和能够连接到过滤助剂材料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胶态金属沉淀络合物。
例举的胺可以是吡咯，表氯醇衍生的胺，其聚合物和类似物。例举的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。例举的季铵盐可以是二烯丙基二甲基卤化铵的均聚物，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/或至过滤助剂材料上。
此外，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杀生物剂。取决于过滤助剂材料，MBGDA可以或不将PHMB交联至微生物拦截增强过滤助剂上。
将阳离子材料暴露于生物活性金属盐溶液下，以便金属胶体络合物沉淀到至少一些过滤助剂材料的至少一部分表面上。为此，生物活性金属是优选的。这些生物活性金属包括但不限于银，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，使得阳离子材料中的金属和抗衡离子基本上不溶于含水环境以驱使金属络合物沉淀。优选地，金属的存在量是微生物拦截增强过滤助剂重量的约0.01％至约2.0％。
尤其有用的微生物拦截增强剂是银-胺-卤化物络合物。阳离子胺优选分子量为约400,000道尔顿的二烯丙基二甲基卤化铵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Nalco ChemicalCompany(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，则银-胺-卤化物络合物沉淀在至少一部分微生物拦截增强过滤助剂上。
活性炭常用作过滤助剂材料用于制备无色的麦芽饮料。当微生物拦截增强过滤助剂包括活性炭时，阳离子材料优选具有高的电荷密度和足够高的分子量，以便产生对活性炭的带负电的表面基团的强烈吸引和高的配位能。同样，通过活性炭的疏水吸附机理，使用活性炭的带电表面补强了在生物活性金属胶体存在下的增强拦截。具有富氧化学的碳表面的未处理部分，倾向于具有负电荷，该负电荷可继续吸附带正电的颗粒。正、负、和疏水表面的组合对于污染物的流过来说呈现出几乎不可逾越的阻挡。
在用微生物拦截增强剂处理过滤助剂材料之后，可使用X-射线荧光检测在活性颗粒上生物活性金属和其抗衡离子的存在。
制备微生物拦截增强过滤助剂的方法
可用本领域熟练技术人员已知的工艺，包括喷涂、浸涂和类似方法，用微生物拦截增强剂处理可用于制备本发明微生物拦截增强过滤助剂的过滤助剂材料。以下概述了制备微生物拦截增强过滤助剂的例举方法，所述过滤助剂包括用微生物拦截增强剂处理的纳米纤维。粒状过滤助剂材料的类似处理工艺是本领域熟练技术人员已知的。
在制备包括纳米纤维的微生物拦截增强过滤助剂中，将纤维丝束切断成特定的长度，通常在约1mm至约8mm范围内，和尤其在约3mm至约4mm范围内。在具有类似于掺合器特征的设备内，或在较大规模上在常称为“hi-low”、“打浆机”或“匀浆机”的机器内，原纤化短切纤维。使纤维经历反复的应力，同时进一步切断，并使纤维长度的下降最小。当纤维经历这些应力时，由于无定形和结晶区域之间的作用力弱导致纤维劈裂，和加拿大标准游离度(CSF)开始下降，其中所述加拿大标准游离度通过本领域公知的方法来测定。可间隔地取出所得纸浆样品，和CSF可用作原纤化程度的间接量度。尽管CSF值略微敏感于纤维长度，但它更强烈敏感于纤维的原纤化程度。因此，CSF是从纸浆中除水的容易程度的量度，它是监控纤维原纤化程度的合适方式。若表面积非常高，则在给定量的时间下非常少的水从纸浆中排出，和随着纤维更深入地原纤化，CSF值将逐渐变低。一般地，对于本发明的应用来说，使用CSF低于100的纸浆，和优选CSF应当小于或等于约45。
用阳离子材料处理纸浆，其方式使得阳离子材料涂布至少一些纤维的至少一部分表面，从而在纤维上赋予电荷。施加阳离子材料到纤维上的方法是本领域已知的，和包括但不限于喷涂、浸涂，或浸没涂布，以引起阳离子材料吸附、化学反应或交联到纤维表面上。然后在反渗透/去离子水(RO/DI)水中漂洗已处理纸浆，通常在真空下部分脱水，产生预涂层，然后可将其暴露于生物活性金属盐溶液中。使用几乎无离子的漂洗水引起与阳离子材料缔合的抗衡离子朝已处理的纤维表面紧密地吸引并排除了不想要的离子，所述不想要的离子可能引起生物活性金属不可控地沉淀到远离阳离子表面的位置上。
使金属盐溶液渗透到纤维内，以使阳离子金属胶体络合物在至少一部分纤维表面上沉淀。该沉淀精确地沉积与阳离子涂层相邻的金属胶体，这是因为与该涂层缔合的抗衡离子同施加的金属盐反应形成胶体颗粒所致。在充分暴露于生物活性金属盐溶液之后，可漂洗纤维并除去过量的水。当将硝酸银用作金属盐溶液时，可使用获自KratosAnalytical(日本的Shimadzu Group Company)的Kratos EDX-700/800X-射线荧光分光计，证明沉淀银的存在。
也可将颗粒、纤维、晶须或粉末形式的一种或多种添加剂与微生物拦截增强过滤助剂混合，以吸附其它污染物或参与微生物或其它污染物的拦截。有用的添加剂可包括但不限于金属颗粒，活化矾土，活性炭，二氧化硅，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，其它吸附剂材料如超吸收性聚合物(SAP)，或其组合。也可根据特定应用化学处理添加剂，以赋予微生物拦截能力。这些添加剂优选以使得在用于过滤用途时所得预涂层组合物和/或滤饼中的流体流动基本上不受阻碍的充分量存在。添加剂的量取决于过滤体系的特定用途。
微生物拦截增强过滤助剂可以基于组合物重量为约0.5％至约50％的少量与主体过滤助剂混合，以增强本体过滤助剂的性能。
在本发明的预涂层组合物中使用微生物拦截增强过滤助剂的方法
使包括微生物拦截增强过滤助剂的流体形式的分散液经过支撑介质，如隔膜或滤网，和在支撑介质上形成厚度通常为约0.5至约3mm的预涂层。支撑介质具有的尺寸和平方英尺数使得待过滤的流体的流速没有慢到使大规模的制备工艺受到限制。待过滤的流体经过滤饼和粒状微生物污染物截留在滤饼上。在流体过滤经过滤饼之前，可包括微生物拦截增强过滤助剂的主体原料组合物可与流体混合。添加主体原料组合物促进了(open up)滤饼的渗透性和防止在滤饼上形成截留污染物的不可渗透网。当终止过滤时，反冲刷滤饼和滤饼脱离支撑介质。已用过的滤饼作为饼或浆料被弃置。
包括微生物拦截增强过滤助剂的预涂层组合物可提供微生物污染物(包括病毒)至少约3的对数下降，从而提供单步冷冻灭菌技术。若不需要这种全面拦截，则可将微生物拦截增强过滤助剂以基于预涂层组合物重量为约0.5％至约50％的量与不带电的主体过滤助剂混合，以提供所需程度的拦截。
实施例
提供以下实施例说明本发明，而不应理解为限定本发明的范围。
使用American Type Culture Collection(ATCC)No.11775的大肠杆菌(Escherichia coli)的悬浮液，进行过滤助剂的细菌挑战，以评估对细菌挑战的响应。使用ATCC的标准操作步骤繁殖细菌，并使用本领域熟知的标准微生物步骤制备和量化受到细菌悬浮液挑战的过滤助剂的流入液和流出液中的细菌。
在下述实施例中使用的预涂布表面的直径为47mm和在获自Fischer Scientific，Pittsburgh，Pennsylvania的Osmonics/MSIGRAVI-SEALTM分析漏斗上形成该预涂布表面。用以商品名REEMAYTM2004商购于BBA Nonwovens Reemay，Inc.(Old Hickory，Tennessee)的纺粘聚酯做分析漏斗的衬里。
实施例1(比较)：未处理纤维素对E.coli的拦截
在分析漏斗内，将获自International Fiber Corporation、干重为约0.63g的Alpha-Cel BH-40纤维素纸浆形成为预涂层。使用蠕动泵，使RO/DI水流过预涂层，以实现31ml/min的流量。用含有1.06×105E.coli的细菌悬浮液挑战预涂层。含未处理纤维素纸浆的预涂层的对数下降值小于约1。
实施例2(比较)：在与5％未处理Lyocell纳米纤维混合的未处理纤维素上E.coli的拦截
在350ml RO/DI水中，使用与干重为0.03g的未处理原纤化Lyocell纤维混合的干重为0.60g的BH-40纤维素纸浆，制备预涂层。使用蠕动泵，使RO/DI水以约80ml/min的流量流过预涂层。用含有1.06×105E.coli的细菌悬浮液挑战预涂层。预涂层的对数下降值小于约1。
实施例3(比较)：与5％过滤助剂混合的未处理纤维素的E.col拦截，其中所述过滤助剂用经阳离子材料处理的Lyocell纤维制备
将用量为干重约11.4g(120.0g湿重)、加拿大标准游离度为45的原纤化Lyocell纳米纤维分散在含有3.0ml MERQUAT100(30％的水溶液)和0.27g溴化钠的1.0L RO/DI水中过夜。将所得带电纤维倾倒入配有100目成形丝网的标准8英寸Brit过滤器中，并在真空下除去过量水，从而形成纸片。用500ml RO/DI水漂洗纸片。
使用与干重为0.03g带电原纤化Lyocell纤维混合的干重为0.60gBH-40纤维素纸浆制备预涂层。使用蠕动泵，使RO/DI水以约28ml/min的流量流过预涂层。用含有1.06×105E.coli的细菌悬浮液挑战预涂层。预涂层的对数下降值为约2.10。
实施例4：用与微生物拦截增强过滤助剂混合的未处理纤维素对E.coli的拦截
将用量为干重约11.4g(120.0g湿重)、加拿大标准游离度为45的原纤化Lyocell纳米纤维分散在含有3.0ml MERQUAT100(30％的水溶液)和0.27g溴化钠的1.0L RO/DI水中过夜。将所得带电纤维倾倒入配有100目成形丝网的标准8英寸Brit广口瓶中，并在真空下除去过量水，从而形成纸片。用500ml RO/DI水漂洗纸片。通过添加60ml RO/DI水稀释稀硝酸银溶液，一种3.0ml的储液(在60ml RO/DI水内的1.8g AgNO3)，并均匀倾倒在纸片上，以提供充分的暴露和饱和度。使硝酸银溶液在纸片上静置至少约15分钟和在真空压力下除去过量水，得到本发明的微生物拦截增强过滤助剂。
使用与干重为0.03g的微生物拦截增强过滤助剂混合的干重为0.60g的未处理BH-40纤维素纸浆，制备预涂层。使用蠕动泵，使RO/DI水以约31ml/min的流量流过预涂层。用含有1.06×105E.coli的细菌悬浮液挑战预涂层。该预涂层的对数下降值为约5.02，这表明E.coli完全除去。
实施例5：微生物拦截增强过滤助剂对E.coli的拦截
使用蠕动泵，使RO/DI水以约28ml/min的流量流过实施例4所述的干重为0.63g的微生物拦截增强过滤助剂的预涂层。用含有1.0×104E.coli的细菌悬浮液挑战预涂层。微生物拦截增强过滤助剂的对数下降值为4.00，这表明E.coli完全除去。
下表I示出了实施例1-5的结果。
表I实施例1-5中E.coli的对数下降值
  实施例号  Wt％MIEFA   E.coli挑战   #CFU   LRV
  1  0   1.06×105   2.00×104   ＜1
  2  0   1.06×105   3.20×104   ＜1
  3  0   1.06×105   8.33×102   2.10
  4  5％   1.06×105   0   5.02
  5  100％   1.0×104   0   4.00
MIEFA＝本发明的微生物拦截增强过滤助剂
CFU＝每块板上的菌落形成单位。
如实施例4所示，添加甚至少量的本发明微生物拦截增强过滤助剂看上去提供预涂层组合物显著的微生物拦截能力用于降低E.coli。仅仅包括所述微生物拦截增强过滤助剂的实施例5的预涂层组合物提供优良的细菌拦截。
尽管已结合特定优选的实施方案具体描述了本发明，但显然根据上文描述，许多替换、修改和变化对本领域熟练技术人员来说是显而易见的。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 (16)

1.一种组合物，它包括微生物拦截增强过滤助剂，其中在该过滤助剂的至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料，其中在与所述阳离子材料直接相邻处用抗衡离子沉淀生物活性金属。
2.权利要求1的组合物，其中所述过滤助剂包括加拿大标准游离度小于或等于45的纤维。
3.权利要求1的组合物，其中所述过滤助剂包括纳米纤维、纤维素、硅藻土、活性炭、活化矾土、硅酸盐、聚合物树脂或纤维、或其组合。
4.一种组合物，它包括：
吸附剂；
与所述吸附剂混合的微生物拦截增强过滤助剂，在所述过滤助剂的至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料和在与该阳离子材料直接相邻处用抗衡离子沉淀的生物活性金属。
5.权利要求1或4的组合物，其中阳离子材料具有高的电荷密度、分子量大于或等于5000道尔顿，和包括季铵化胺、季铵化酰胺、季铵盐、季铵化酰亚胺、苄烷铵化合物、阳离子氨基硅化合物、其聚合物、或其组合。
6.权利要求1或4的组合物，其中阳离子材料是二烯丙基二甲基卤化铵的均聚物。
7.权利要求1或4的组合物，其中生物活性金属是银、铜、锌、镉、汞、锑、金、铝、铂、钯或其组合。
8.权利要求4的组合物，其中所述吸附剂包括纤维素纤维，和其中所述过滤助剂包括加拿大标准游离度小于或等于100的原纤化Lyocell纤维。
9.一种过滤流入液的方法：
提供支撑介质；
用微生物拦截增强过滤助剂涂布该支撑介质以形成预涂层，其中在该过滤助剂的至少一部分上涂布具有与其缔合的抗衡离子的阳离子材料和在与阳离子材料直接相邻处用抗衡离子沉淀的生物活性金属；
使流入液经过所述预涂层；
在预涂层上保留来自流入液的污染物；和
获得澄清的流出液。
10.权利要求9的方法，进一步包括在使流入液经过预涂层之前，添加过滤助剂到流入液中的步骤。
11.权利要求9的方法，其中在用过滤助剂涂布支撑介质的步骤中，所述过滤助剂包括纳米纤维、纤维素、硅藻土、活性炭、活化矾土、硅酸盐、聚合物树脂或纤维、或其组合。
12.权利要求9的方法，其中在用过滤助剂涂布支撑介质的步骤中，使所述过滤助剂与未被涂布的过滤助剂材料混合。
13.权利要求9的方法，其中在用过滤助剂涂布支撑介质的步骤中，用阳离子材料涂布所述过滤助剂，其中所述阳离子材料选自季铵化胺、季铵化酰胺、季铵盐、季铵化酰亚胺、苄烷铵化合物、阳离子氨基硅化合物、其聚合物和其组合。
14.权利要求9的方法，其中在用过滤助剂涂布支撑介质的步骤中，用二烯丙基二甲基卤化铵的均聚物涂布所述过滤助剂。
15.权利要求9的方法，其中在用过滤助剂涂布支撑介质的步骤中，所述生物活性金属是银、铜、锌、镉、汞、锑、金、铝、铂、钯或其组合。
16.权利要求9的方法，进一步包括提供流入液中微生物污染物至少4的对数下降的步骤。
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US6835311B2 (en) 2004-12-28
US6959820B2 (en) 2005-11-01
AU2003209149B2 (en) 2008-02-14
EP1483039A1 (en) 2004-12-08
CA2474980A1 (en) 2003-08-07
CA2474858A1 (en) 2003-08-07
DE60320542D1 (de) 2008-06-05
US6913154B2 (en) 2005-07-05
US6953604B2 (en) 2005-10-11
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JP4726415B2 (ja) 2011-07-20
TW200302812A (en) 2003-08-16
CN1625434A (zh) 2005-06-08
US20030205531A1 (en) 2003-11-06
WO2003064013A1 (en) 2003-08-07
EP1483039B1 (en) 2008-04-23
ATE393125T1 (de) 2008-05-15
HK1074019A1 (en) 2005-10-28
US20030168401A1 (en) 2003-09-11
KR20040088046A (ko) 2004-10-15
CN1625428A (zh) 2005-06-08
US7008537B2 (en) 2006-03-07
US7144533B2 (en) 2006-12-05
US20030196964A1 (en) 2003-10-23
DE60319810D1 (de) 2008-04-30
ATE389618T1 (de) 2008-04-15
EP1483028B1 (en) 2008-03-19
EP1483039A4 (en) 2005-11-02
US20030201231A1 (en) 2003-10-30
US20030196963A1 (en) 2003-10-23
BR0307316A (pt) 2005-01-11
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AP2004003098A0 (en) 2004-09-30
US6998058B2 (en) 2006-02-14
CA2474858C (en) 2009-12-15
US20030205530A1 (en) 2003-11-06
US7011753B2 (en) 2006-03-14
EP1483028A4 (en) 2005-11-02
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KR100982596B1 (ko) 2010-09-15
US20030205529A1 (en) 2003-11-06
JP2005515879A (ja) 2005-06-02
MXPA04007355A (es) 2004-11-26
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BR0307316B1 (pt) 2013-02-05
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CN1280001C (zh) 2006-10-18

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