CN1897981A - 细菌粘附产品 - Google Patents
细菌粘附产品 Download PDFInfo
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- CN1897981A CN1897981A CNA200480038555XA CN200480038555A CN1897981A CN 1897981 A CN1897981 A CN 1897981A CN A200480038555X A CNA200480038555X A CN A200480038555XA CN 200480038555 A CN200480038555 A CN 200480038555A CN 1897981 A CN1897981 A CN 1897981A
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Abstract
提供用于从表面除去带负电荷的粒子如细菌的产品。该产品具有可通过使用阳离子处理物形成的正电荷。可将该产品或制备它的基底浸在具有正电荷的非抗菌处理物的水溶液中并挤出过量的溶液。在一定温度和足够时间下用热处理得到的带涂层基底以粘着涂层到基底上。或者,非抗菌的带阳电荷的化学物品可被嵌入到基底网中,从而当网暴露于水时,它浮现在表面上。合适的基底网可为通过共成形或水力缠结制造的纸浆和合成纤维布,并可为包括其它层的叠层。处理的基底和该产品从表面除去大量细菌但不会相当多地杀死细菌。在该产品的制备中不使用苛刻的氧化性化学物品,从而该产品在其对使用者皮肤的影响方面是温和的。与杀死细菌相比,细菌的除去不会促进细菌形成对处理物的免疫性。
Description
本申请为2003年12月23日提交的共同转让美国专利申请10/745266的部分继续,并要求其文件的权益。
发明背景
本发明涉及在不使用苛刻的化学物品时用于粘附和除去带负电荷的粒子如细菌的方法和产品。
由于对化学物品过敏反应和细菌对常见药物治疗耐性提高的关注增加,因而关注和需要能避免苛刻化学物品但又达到它们的目的的产品。在目前可用的湿抹布的情况下,例如,用化学物品的溶液浸渍抹布。典型的化学物品可为抗菌化学物品,抹布的使用有助于输送化学物品到污染表面。但是,更理想地,抹布将在从表面除去微生物的同时保留化学物品。能除去细菌但不在表面上留下化学物品的抹布提供了所需的去污作用而不会令人不快地暴露人到化学物品。
大量不同的消费产品可从这种细菌除去中受益。本发明的一个目的是提供能除去带负电荷的粒子而不留下化学物品残留物的产品。
发明简述
与本领域那些技术人员遇到的前述困难相对应,我们开发了从表面上粘附和除去带负电荷的粒子如细菌的产品。该产品具有可通过使用阳离子处理物形成的正电荷。处理物化学物品可为官能化聚合物、有机或无机低聚物、或涂有官能化聚合物、有机或无机低聚物的粒子。在施加处理物后,可在足以使涂层交联并附着涂层到基底的温度和时间下用热来处理得到的产品。
适用于本文的处理物不会氧化施加它们的产品的表面。这避免了在产品制造过程中对非常苛刻条件的需要。但是,处理物与产品表面交联。
附图简述
图1为尿布的图。
图2为训练裤的图。
图3为女性卫生垫的图。
图4为吸收性内衣裤的图。
发明详述
本发明涉及从表面粘附和除去带负电荷的粒子如细菌、细胞、过敏原、病原体和分子。由于耐常规处理的细菌的数目增加,这对消费者来说变得日益重要。其对不应暴露于苛刻化学物品的消费者来说也日益重要。
引入本文化学物质的产品能从表面除去带负电荷的粒子。带负电荷的粒子被除去而不需要使用苛刻的化学物品,即有腐蚀性或对一般人皮肤产生刺激的化学物品,因而消费者不需要接触带化学物品的产品。在为细菌时,例如,由于细菌不被暴露于能大量即超过20%杀死它们的化学物品,因此细菌不会被促进形成对产品基底上化学处理物的免疫性。通过应用物理手段和库仑吸引就可简单地除去细菌。一种成功的处理化合物不会以足以充分杀死细菌的量从基底中浸出,因此具有至少80%的对照菌落存活率,即处理物将杀死20%或更少的细菌菌落。
多种产品被考虑除去如本文揭示的带负电荷的粒子。这些产品包括个人护理产品,如尿布、训练裤、抹布、女性卫生产品(棉塞、女用垫)、吸收性内衣裤和失禁外衣。该产品还包括口腔护理产品和存储物品、个人修饰产品如头发和头皮用物品、指甲处理物和皮肤清洁产品。该产品包括面巾纸和卫生纸、面膜、外科长外衣、被单和医疗器械、和手套。该产品可包括家用清洁物品如抽水马桶清洗器、硬表面清洁器、海绵和其它厨房清洁材料。该产品可包括农业、动物和宠物护理物品,如刷子、抹布、猫粪土、种子制备物和土壤处理物。该产品可包括空气和水过滤器、用于除灰尘、过敏原和其它污染物的离子去除过滤器。该产品还可包括用于家禽和其它肉类的食品贮藏垫。
图1-4分别为典型的个人护理产品如尿布、训练裤、女用垫和吸收性内衣裤的图。各自具有衬里12和外罩或背层14。个人护理或吸收性产品一般具有贴着穿戴者的衬里、最外层的背层,并还可包含其它层如吸收芯。衬里有时被称为身体侧衬里或顶层。在制品的厚度方向上,衬里材料为靠着穿戴者皮肤的层,因而第一层接触穿戴者的液体或其它分泌液。衬里还用于将穿戴者的皮肤与吸收结构中保留的液体隔开,并应有舒服柔软感觉和没有刺激性。
在形成身体侧衬里时可使用各种材料,包括有孔的塑料膜、纺织布、无纺网、多孔泡沫、网状泡沫等。发现无纺材料尤其适用于形成身体侧衬里,包括聚烯烃、聚酯、聚酰胺(或其它类型成纤维聚合物)细丝的纺粘或熔喷网,或天然聚合物(例如人造丝或棉纤维)和/或合成聚合物(例如聚丙烯或聚酯)纤维的粘合梳理网。例如,身体侧衬里可为合成聚丙烯细丝的无纺纺粘网。无纺网可具有例如从约1克/平方米(gsm)到约70gsm的基重。
除了上述网外,共成形(coform)网、粘合梳理网和气流成网材料也可用于个人护理产品中,可能为任意的常规已知无纺布的叠层。也可使用纤维素材料如纸巾和薄纸。也可通过引入织构和提高蓬松性的方法如通过起绉、通过零应变拉伸粘合、点未粘合(pointunbonding)、Z-向取向和其它方式来制造网。
无纺布通常以生产它们时的一定方式被粘合,以便给予它们足够的结构完整性来承受进一步加工成成品时的僵硬。可用大量方法实现粘合,如水力缠结、针刺、超声粘合、粘合剂粘合、缝编、气流粘合和热粘合,它们全部适合于实施本发明。
处理物应具有正电荷以便吸引和持有带负电荷的粒子。可用多种方法产生正电荷;例如,可向产品中加入带阳电荷的化学处理物,和/或可将驻极体处理物施加到产品上,产生正电荷。合适的化学物品包括官能化的带阳电荷的聚合物、和无机或有机低聚物。纳米颗粒涂有官能化的带阳电荷的聚合物或无机或有机低聚物。合适的无机低聚物的例子为二氢氯酸铝(aluminum chlorohydrol)和氢氯酸铝。
用于在产品表面上产生正电荷的化学物品包括美国特拉华Wilmington的Hercules Inc以商标名KYMENE、RETEN、美国新泽西Bridgewater的National Starch and Chemical Company以COBOND出售的阳离子聚合物,和美国宾夕法尼亚州匹兹堡的Calgon Inc.的Calgon聚合物,和其它一些,如聚乙烯亚胺,高电荷密度聚合电解质如聚(甲基丙烯氧乙基)溴化三甲氨、聚(丙烯酸)和表氯醇官能化的聚胺。也可使用纳米颗粒,如美国德克萨斯州休斯顿NissanChemicals Inc.的SNOWTEXAK和美国新泽西Berkeley Heights的Reheis Inc.的氢氯酸铝。除了具有正电荷外,适于实施本发明的化学物品在对皮肤的作用上是温和的,在性质上不会明显地抗菌,并且一旦被粘合到基底表面就基本上不浸出。
应加入的化学物品的量将随起作用的所选具体化学物品的电荷量变化。但是,通常,化学物品的有效量将在约0.01和10wt%之间,更理想地在0.05和7wt%之间,还更理想地在0.1和5wt%之间。
化学处理物可通过方法如传统的浸涂和挤压技术来施加,其中物品被浸涂到化学处理物中,过量的化学物品被挤压,或通过刷涂、喷涂、喷墨印刷等。如下面所述,还可以将化学处理物作为内部处理物加入到例如聚合物纤维中。
可在足以使涂层交联并使其粘着到网上的温度和时间下热处理化学处理的产品表面。官能化的带阳电荷的聚合物的交联过程包括涂层的可交联官能团(例如环氧基)与涂层的另一官能团(例如羟基)或与基底官能团之间的反应。例如,基底可为纤维素,其中纤维的羟基将与涂层的环氧基进行分子间交联。在为氧化铝低聚物的情况下,交联过程包括低聚物的Al-OH基与低聚物OH(分子内交联)或与基底OH基(分子间交联)。认为涂有氧化铝低聚物的纳米颗粒将通过OH基与低聚物的Al-OH基交联粘着到含OH的表面上。足以使聚合物交联的时间和温度的组合将取决于选择的聚合物和基底。但是,一般而言,时间将在1和60分钟之间,更理想地在5和45分钟之间,还更理想地在15和35分钟之间,温度在约50和300℃之间,更理想地在约80和200℃之间,还更理想地在约90和125℃之间。本发明人发现,例如,100℃的温度持续约20-30分钟能固化所关注的大多数聚合物。
取决于纤维的特性,官能化聚合物(如具有环氧基的KYMENEs)能包括分子内(即只在涂层内)和分子间(即只与基底)两种交联过程。认为可能是如果基底被官能化的话,交联过程将结合分子内和分子间过程。或者,如果基底不能参与化学交联过程,则只发生分子内交联。在任何一种情况下,当在涂敷前通过预处理使非官能化基底可润湿时,经常能得到耐久涂层。因此术语“粘着到基底上”包括在纤维基底周围形成“套”的分子内交联、以及化学物品或化学物品载体(如涂有氧化铝低聚物的纳米颗粒)在基底上形成共价键的分子间交联和它们的组合的情况。如果带阳电荷的化学物品在使用过程中从基底不浸出,则它“粘着到基底上”,其中从基底“不浸出”是指在接触基底的表面上留下的液体中化学物品的浓度小于化学物品具有抗菌性质的临界浓度。
或者,通过熔融挤压在网纤维中包含所需量的带阳电荷化合物作为添加剂的成纤维聚合物在由纤维制成的产品中嵌入带阳电荷的化合物。当网暴露于亲水溶剂如水时,这种化合物可“浮现”在表面上。这些熔融可挤压纤维可包含聚烯烃和带阳电荷的化合物。带阳电荷的化合物还可包含在聚烯烃中可溶的化学段(即相容剂),从而盐与聚合物相容。带阳电荷的化合物品可为例如与疏水网相容的两性季铵盐,其例子公开在Nohr和Macdonald的美国专利5853883中,本文引入其作为参考。如果与疏水聚合物相容的盐的疏水段较大(相对于盐的离子段),则浸出网的盐量不足以杀死细菌,于是网将不具有抗菌活性。当网暴露于水时,带阳电荷的基团通常到达主要为聚合物纤维的表面。这种浮现给予网类似于涂有带阳电荷化合物的基底的性质。
本发明人试验了大量基底和化学处理物的除去效率和化学浸出。下面显示了这些材料、处理物、试验过程和结果。
PBS对照:这指无菌磷酸盐缓冲盐水(PBS)并说明该样品中不存在织物、处理物或带负电荷的粒子。用蒸馏水稀释磷酸盐缓冲盐水(可从Gibco和Invitrogen以10X浓度得到)至1X,并在使用前无菌过滤。
水刺布:水刺方法也称为水力缠结。水刺方法使纤维网在高压下经受细的水射流。当射流撞击到网时,它重新定位纤维并使其缠结成连结的“水刺”网。然后在热炉中干燥网。一般而言,水刺网不包含化学粘合剂,并且它们具有优异的类似织物的悬垂性和蓬松性、良好的机械和美学性质、和良好的吸收性和润湿性。可使用各种天然和合成纤维制造水刺网,包括聚丙烯、人造丝、PET和尼龙。人造短纤维也用于水刺无纺产品中。本文试验的水刺布由65wt%的人造丝和35wt%的PET制成。在未起皱状态下和在起皱状态下试验布,其中按照美国专利6197404和6150002进行起皱,本文全文引入它们作为参考用于各种目的。这些起皱材料具有永久弯出面的丝间粘合区域,交替具有未丝间粘合的区域。未粘合区域包括大量在起皱的丝间粘合区域中在粘合端处终止的细丝环。有绒毛的薄膜,聚氨酯:这种有绒毛的薄膜通过粘纺方法由聚氨酯(PU)泡沫和聚乙烯(PE)薄膜制成。在粘纺中,PU和PE被层压到一起,PE在热辊上被部分熔化,通过从辊上拉离材料并在其上面或穿过它吹空气来冷却以使表面纤维化。
粘合梳理网:“粘合梳理网”是指由被送往精梳或梳理单元的人造短纤维制成的网,精梳或梳理单元将人造短纤维分裂开并在加工方向上排列形成通常加工方向定向的纤维无纺网。通常大捆购买这种纤维,并在梳理单元前放到分离纤维的拣选机中。一旦形成网,就通过几种已知的粘合方法中的一种或多种将它粘合。一种这样的粘合方法为粉末粘合剂粘合,其中粉末粘合剂被分布在整个网内,然后被活化,通常通过用热空气加热网和粘合剂。另一种合适的粘合方法为花纹粘合,其中使用加热的砑光辊或超声粘合设备粘合纤维到一起,通常以局部粘合花纹的方式,但可在它的整个表面上粘合网,如果需要这样的话。另一种合适的众所周知的粘合方法为气流成网粘合,尤其当使用双组分人造短纤维时。
织构化共成形叠层(TCL):这种材料为在芯的任何一侧上具有外层的弹性叠层。外层各自具有35克/平方米(gsm)的基重,并按照共成形方法由60wt%的Weyerhaeuser Corp.的CF405纤维化软青莴纸浆和40wt%的荷兰Hoofddorp的Basell Polyolefins Company N.V.的PF-105聚丙烯熔喷纤维的混合物制成。芯基重为30gsm,由细丝和无纺布制成。细丝构成芯的70wt%,并由美国MI中部的Dow ChemicalCompany的AFFINITY茂金属基聚乙烯制成。无纺布按照熔喷方法由80wt%的AFFINITY聚乙烯、15wt%的美国田纳西州金斯波特Eastman Chemical Company的REGALREZ1126烃树脂和5wt%的Dow Chemical Company的DNDB 1077线性低密度聚乙烯制成。
在熔喷方法中,通过大量细(通常是圆形)模毛细管挤压熔融热塑性材料成熔融细线或细丝进入到会聚的高速(通常是热的)气体(例如空气)流中来形成纤维,气流能缩小熔融热塑性材料的细丝以减小它们的直径,可至微纤维直径。熔喷纤维然后被高速气流携带并沉积到收集表面上形成随机分散的熔喷纤维的网。这种方法公开在例如Butin等人的美国专利3849241中。熔喷纤维为微纤维,在堆积到收集表面上时,其可能是连续的或不连续的,通常平均直径小于10微米,并通常粘着。
在共成形方法中,在斜槽附近布置至少一个熔喷模头,其它材料在熔喷网成形时通过斜槽被加入到熔喷网中。这种其它材料可为天然纤维、超吸收性颗粒、天然聚合物(例如人造纤维)和/或合成聚合物(例如聚丙烯或聚酯)纤维,例如,其中纤维可具有定长。Lau的普通转让的美国专利4818464和Anderson等人的美国专利4100324中说明了共成形方法。共成形方法产生的网通常被称为共成形材料。天然纤维包括羊毛、棉、亚麻、大麻和木纸浆。木纸浆包括标准软木抖松级如CR-1654(US Alliance Pulp Mills,Coosa,Alabama)。可对纸浆改性以便增强纤维的固有特性和它们的加工性。可通过包括化学处理或机械扭曲的方法使纤维卷曲。一般在交联或硬挺整理前提供卷曲。通过使用交联剂如甲醛或它的衍生物、戊二醛、表氯醇、羟甲基化化合物如脲或脲衍生物、二醛如马来酐、非羟甲基化脲衍生物、柠檬酸或其它多羧酸使纸浆变硬。由于环境和健康关注,这些试剂中的一些与其它相比不太优选。还可通过使用热或碱处理如丝光处理使纸浆变硬。这类纸浆纤维的例子包括NHB416,其为增加了湿模量的化学交联软青莴纸浆纤维,可从Weyerhaeuser Corporation of Tacoma,WA得到。其它有用的纸浆有松解纸浆(NF405)和非松解纸浆(NB416),也得自Weyerhaeuser。田纳西州孟菲斯的Buckeye Technologies公司的HPZ3除了为纤维提供额外的干和湿硬度以及弹性外,还具有在卷曲和扭曲中定形的化学处理物。另一种合适的纸浆为Buckeye HP2纸浆,还一种为International Paper Corporation的IP Supersoft。合适的人造丝纤维为亚拉巴马州Axis的Acordis Cellulose Fibers Incorporated的1.5丹尼尔Merge18453纤维。
HYDROKNIT材料:HYDROKNIT材料可从美国德克萨斯州达拉斯的Kimberly Clark公司得到,为软吸收性纤维素纤维和纺粘合成纤维的水力缠结网。合成纤维通常为聚丙烯。本文中试验的材料具有64gsm的基重,并只由75wt%的纸浆和25wt%聚丙烯纺粘纤维一个层组成。本文使用的术语“具有PP纤维的HYDROKNIT”是指在其表面上沉积有纺粘聚丙烯纤维附加层的上述HYDROKNIT布。这在HYDROKNIT基底上产生粗质地PP纤维层以提高磨损性。
术语“纺粘纤维”是指通过由喷丝头的多个细(通常为圆形)的毛细管将熔融热塑性材料挤压成细丝并且挤压细丝的直径然后被快速减小来形成的小直径纤维,例如在Appel等人的美国专利4340563和Dorschner等人的美国专利3692618、Matsuki等人的美国专利3802817、Kinney的美国专利3338992和3341394、Hartman的美国专利3502763和Dobo等人的美国专利3542615中所述。纺粘纤维在堆积到收集表面上时通常不粘着。纺粘纤维通常是连续的,并具有大于7微米,更尤其在约10和20微米之间的平均直径(来自至少10个样品)。
VIVA擦洗布:这种材料为纤维素纸巾,并可从Kimberly-Clark公司得到。它在基片的两侧上具有印刷的聚乙烯醋酸酯粘合剂,基片由72wt%的软木漂白牛皮纸、13wt%的聚乙烯醋酸乙烯酯粘合剂、11wt%合成(聚酯)纤维、3wt%的硬木牛皮纸、1wt%的总氮构成。
WYPALLX80材料:WYPALL材料也可从Kimberly-Clark公司得到。WYPALLX80材料为具有高的湿强度和容量的强吸收性松散HYDPOKNIT材料。本文试验的材料具有125gsm的基重,并由75wt%的纸浆和25wt%的聚丙烯纺粘纤维制成。
气流成网布:“气流成网”为众所周知的形成纤维无纺层的气动成形方法。在气流成网方法中,典型长度为约3-约52毫米(mm)的小纤维的束被分离并夹带在给气中,然后堆积到成形筛上,通常借助真空。然后使用例如热空气或喷雾粘合剂将随机堆积的纤维彼此粘合。气流成网无纺复合材料的生产明确记载在本领域的文献和文档中。例子包括Laursen等人的并转让给Scan Web of North America Inc.的美国专利4640810中描述的DanWeb方法、Kroyer等人的美国专利4494278和Soerensen的转让给Niro Separation a/s的美国专利5527171中描述的Kroyer方法、Appel等人的转让给Kimberly-ClarkCorporation的美国专利4375448的方法或其它类似方法。本文试验的材料由83wt%的Weyerhaeuser CF504纸浆和17wt%的乳胶粘合剂(National Starch Dur-O-Set Elite PE)制成,并具有68gsm的基重。
可在本发明的实施中使用大量其它方法和材料,但没有在本文中全部试验。下面描述这些其它材料和方法的一部分。
点未粘合或“PUB”是指连续粘合区域限定大量不连续未粘合区域的布图案,如Stokes等人的美国专利5858515中所述。不连续未粘合区域内的纤维或细丝在尺寸上被围绕或环绕每个未粘合区域的连续粘合区域稳定,从而不需要薄膜或粘合剂的支撑或衬背层。未粘合区域被专门设计来提供未粘合区域内纤维或细丝之间的空间。形成点未粘合无纺材料的合适方法包括提供无纺布或网,提供相对布置的第一和第二砑光辊和在其中间限定辊隙,至少一个辊被加热并在它的最外表面具有粘合图案,包括限定大量不连续开口、隙缝或孔的凸区连续图案,和在辊形成的辊隙内通过无纺布或网。由连续凸区限定的辊中的每个孔在无纺布或网的至少一个表面上形成不连续未粘合区域,其中网的纤维或细丝基本或完全未粘合。另外说明,辊中凸区的连续图案在无纺布或网的至少一个表面上形成限定大量不连续未粘合区域的粘合区域连续图案。上述方法的另一实施方案包括在由砑光辊形成的辊隙内通过布或网前预粘合无纺布或网,或提供多个无纺网形成图案未粘合叠层。
零应变拉伸方法通常是指在松弛(因此为零应变)条件下将至少两个层彼此粘合的方法,其中一个层可拉伸并有弹性且第二个可拉伸但不必有弹性。通过使用能降低网经受的应变率的一对或多对啮合沟纹辊渐增地拉伸这种叠层。这导致叠层的z-方向膨化变形,随后在初始拉伸方向上弹性伸长至少达到初始拉伸点。可在美国专利5143679、5151092、5167897和5196000中找到这种叠层及其生产方法的例子。
在本发明的实施中还可使用Z-方向定向纤维网。可在NonwovensIndustry杂志1997年10月号第74页Krema、Jirsak、Hanus和Saunders的题为“What’s new in Highloft Production?”的论文中以及在1995年5月15日公布的题目为“Fibre Layer,Method of its Production andEquipment for Application of Fibre Layer Production Method”的捷克专利235494和1989年4月14日公布的题目为“Method for VoluminousBonded Textiles Production”的捷克专利263075中找到这种方法的论述。
其它合适的材料包括根据美国专利4741941制备的那些,该专利教导了具有突起的无纺网。将制造产品的网成形到具有有或没有缝隙的突起且具有真空辅助的表面上。布具有伸出布外且被平坦凸区分开的中空突起阵列的纤维。可根据任意一种无纺生产技术如熔喷、纺粘、气流成网等制造这种类型的布。
合适的产品还包括美国专利4775582、4853281和4833003中教导的那些。’582和’281专利教导了由聚烯烃熔喷纤维制成的均匀湿抹布。’003专利教导了具有粘合到熔喷支撑层的磨损面的均匀湿抹布。
在下面描述的试验中使用大量不同的处理。按以下进行网的处理:
KYMENE2064:通过用去离子水(995mL)稀释储备KYMENE2064(来自Hercules Inc.,Wilmington,DE,USA)溶液(20wt%水溶液,5mL)制备0.1wt%的KYMENE2064溶液。通过用NaOH(0.4M)调整溶液pH“活化”KYMENE2064,测得pH为8.8。基底的处理需要“浸渍和挤压”规程。每个基底都被浸没在0.1wt%的KYMENE2064溶液中并搅拌大约1分钟以确保饱和。然后使用装备有5磅重物作为挤压压力的Atlas Laboratory Wringer Type LW-1(Atlas Electrical Device Co.,Chicago,IL,USA)挤压处理的材料以除去多余的处理溶液。在100℃下固化材料20分钟,使之冷却到室温,用去离子水洗涤两次。使用相同的上述“浸渍和挤压”规程除去多余的水。使洗涤的材料在100℃下干燥30分钟。
KYMENE450:通过用去离子水(995mL)稀释储备KYMENE450(来自Hercules Inc.)溶液(20wt%水溶液,5mL)制备0.1wt%的KYMENE450溶液。通过用NaOH(0.4M)调整溶液pH“活化”KYMENE450,测得pH为9.2。按与上述KYMENE2064相同的方式进行基底处理。
KYMENE557LX:通过用去离子水(992mL)稀释储备KYMENE557LX(来自Hercules Inc.)溶液(12.5wt%水溶液,8mL)制备0.1wt%的KYMENE557LX溶液。用NaOH(0.4M)调整溶液pH,测得pH为8.0。按与上述KYMENE2064相同的方式进行基底处理。
KYMENE736:通过用去离子水(997.4mL)稀释储备KYMENE736(来自Hercules Inc.,Wilmington,DE)溶液(38wt%水溶液,2.6mL)制备0.1wt%的KYMENE736溶液。用NaOH(0.4M)调整溶液pH,测得pH为8.0。按与上述KYMENE2064相同的方式进行基底处理。
氧化铝低聚物(二氢氯酸铝和氢氯酸铝):通过用去离子水(980mL)稀释储备氧化铝低聚物(来自GEO Specialty Chemicals,Little Rock,AR,USA)溶液(50wt%水溶液,20mL)制备1wt%的氧化铝低聚物溶液。测得的pH为4.6。基底的处理需要“浸渍和挤压”规程。每个基底都被浸没在1wt%的氧化铝低聚物溶液中并搅拌大约1分钟以确保饱和。然后使用装备有5磅重物作为挤压压力的AtlasLaboratory Wringer Type LW-1(Atlas Electrical Device Co.)挤压处理的材料以除去多余的处理溶液。在100℃下加热材料20分钟,使之冷却到室温,用去离子水洗涤两次。使用相同的上述“浸渍和挤压”规程除去多余的水。使材料在100℃下干燥30分钟。
SNOWTEXAK纳米颗粒(氧化铝涂敷的二氧化硅纳米颗粒):通过用去离子水(1425mL)稀释储备SNOWTEXAK纳米颗粒(来自Nissan Chemicals Ltd,Houston,TX,USA)溶液(20wt%水溶液,75mL)制备1wt%的SNOWTEXAK纳米颗粒溶液。测得的pH为4.0。基底的处理需要“浸渍和挤压”规程。每个基底都被浸没在1wt%的SNOWTEXAK纳米颗粒溶液中并搅拌大约1分钟以确保饱和。每个基底的处理溶液不循环用于随后的处理。然后使用装备有5磅重物作为挤压压力的Atlas Laboratory Wringer Type LW-1(Atlas ElectricalDevice Co.)挤压处理的材料以除去多余的处理溶液。在100℃下加热材料20分钟,使之冷却到室温,用去离子水洗涤两次。使用相同的上述“浸渍和挤压”规程除去多余的水。使材料在100℃下干燥30分钟。
试验1-细菌生长抑制试验
KYMENE类化学物品通常是温和的,并且不腐蚀皮肤。但是,已知某些KYMENE化学物品在一定水平下能杀死细菌。为了确定KYMENE处理物化学物品是否会从基底逸出和可能杀死保留在表面上的细菌,设计分析方法测量从被处理材料浸出的化学物品对细菌细胞生长的抑制。该分析过程如下。
将2×2英寸(5×5cm)平方的处理和未处理材料放在包含5mL无菌磷酸盐缓冲盐水(PBS)溶液的15mL管中。将管放在37℃下的振荡培育箱中2-3小时。然后转移1毫升每种溶液到干净培养管中。向每个管中加入抗氨苄青霉素的大肠杆菌(10微升,~1000个细胞)。向干净培养管中加入无菌PBS作为对照。将管送回到振荡培育箱中保持30分钟以上。从每个管中取出100微升并培养到包含氨苄青霉素的LB琼脂培养皿上。在37℃下培育培养物,第二天对细菌菌落计数以确定是否在溶液中存在抑制菌落形成的KYMENE。
LB琼脂是指量为25克的Luria-Bertani液体培养基(可从Difcoand Becton Dickinson得到)和量为15克的琼脂(也从Difco and BectonDickinson得到)混合,并溶解到1升蒸馏水中和高压灭菌。在加入氨苄青霉素(100微克/mL)到LB琼脂中后倒出圆形培养物(100mm×15mm)。
列出了与PBS对照相比的培养皿上存在的菌落百分数的数据。
材料 | KYMENE类型 | 对照百分比 |
PBS对照 | - | 100 |
水刺 | - | 100 |
水刺 | 2064 | 75 |
水刺,被软化 | - | 87 |
水刺,被软化 | 2064 | 82 |
Fuzzy薄膜,聚氨酯 | - | 84 |
Fuzzy薄膜,聚氨酯 | 2064 | 75 |
粘合梳理网Web | - | 81 |
粘合梳理网 | 2064 | 100 |
TCL | - | 80 |
TCL | 2064 | 81 |
TCL | 736 | 3 |
HYDROKNIT | - | 93 |
HYDROKNIT | 2064 | 81 |
具有PP纤维的HYDROKNIT | - | 69 |
具有PP纤维的HYDROKNIT | 2064 | 38 |
VIVA抹布 | - | 100 |
VIVA抹布 | 2064 | 95 |
WYPALLX80 | - | 100 |
WYPALLX80 | Aegis季铵盐 | 100 |
WYPALLX80 | 2064 | 87 |
WYPALLX80 | 736 | 14 |
由结果可看出,除了具有聚丙烯(PP)纤维的HYDROKNIT外,未处理材料似乎对菌落生长没有严重影响。除了具有PP纤维的HYDROKNIT外,KYMENE2064材料没有表现出对生长的明显抑制。用KYMENE736处理的材料浸出KYMENE到溶液中,其杀死溶液中的大多数大肠杆菌。这个结果不令人惊奇,因为已知KYMENE2064材料将交联到上面列出的材料上,而KYMENE736通常不会。被交联到基底的处理物比未交联的处理物更稳定和不易于浸出,因此是所需要的。成功的处理物将具有至少80%的对照样品细胞菌落生长,即它将抑制20%或更少的细菌菌落。
试验2-细菌生长抑制试验
直接在大肠杆菌上试验SNOWTEX纳米颗粒和铝低聚物。在无菌PBS中制备用于涂敷纳米颗粒的SNOWTEX纳米颗粒和铝低聚物两者的系列稀释液。将1毫升每种溶液加入到干净培养管中,一式二份。将无菌PBS加入到培养管中作为对照。向每种溶液中加入抗氨苄青霉素的大肠杆菌(10微升,~1000个细胞)。将培养管放到37℃的振荡培育箱中保持30分钟。培育后,从每个管中取出100微升并培养到包含氨苄青霉素的LB琼脂培养皿上。在37℃下培育培养物,第二天对细菌菌落计数以确定SNOWTEX纳米颗粒或铝低聚物是否抑制菌落形成。列出了与PBS对照相比的培养皿上存在的菌落百分数的数据。
SNOWTEXAK纳米颗粒 | 对照百分比 | AI低聚物 | 对照百分比 |
PBS对照 | 100 | PBS对照 | 100 |
10mg/mL | 96 | 1% | 10 |
1mg/mL | 99 | 0.5% | 57 |
0.5mg/mL | 94 | 0.1% | 100 |
0.1mg/mL | 100 | 0.05% | 100 |
0.05mg/mL | 93 | 0.01% | 100 |
0.01mg/mL | 89 | - | - |
结果表明,SNOWTEX纳米颗粒对大肠杆菌菌落形成没有影响,甚至在高浓度(10mg/mL)下。当在0.5%和更高的浓度下时,铝低聚物降低了大肠杆菌菌落的量。用于处理纳米颗粒的铝低聚物的浓度为1%。这些结果表明,只有用于处理材料的全部低聚物都浸出到溶液中才观察到细菌细胞死亡。如上所述,成功的处理物将具有至少80%的对照样品菌落存活率,即它将杀死20%或更少的细菌菌落。
试验3-粘附细菌效力的试验方法
成功的处理物不仅必须不能杀死大量细菌,而且还必须粘附大部分细菌。为了测定基底和处理物在保留从表面清除的细菌时如何有效,进行以下试验过程。
切割并称量2×2英寸(5×5cm)平方的材料,一式二份。使抗氨苄青霉素的大肠杆菌溶液的系列稀释液达到~105个细胞/ml的最终浓度。向每种材料中加入100微升无菌PBS。5分钟后,向每种材料上加100微升细菌溶液。取出材料并放在50mL管中的10mL无菌PBS内。在水浴中对管进行超声处理(30秒开、30秒关的五次循环)以去除没有紧密粘附到材料上的任何细菌。将包含材料的管中的100微升PBS溶液一式二份在含氨苄青霉素的LB琼脂培养皿上培养。在37℃下培育培养物,第二天对细菌菌落计数。数据显示为与PBS对照相比溶液中细菌减少的百分比。
材料 | 处理物 | 溶液中细菌减少(%)N=4 |
PBS对照 | - | 0 |
WYPALLX80 | - | 62 |
WYPALLX80 | KYMENE2064 | 72 |
WYPALLX80 | KYMENE450 | 63 |
WYPALLX80 | KYMENE557 | 40 |
WYPALLX80 | Al低聚物 | 84 |
WYPALLX80 | SNOWTEXAK纳米颗粒 | 84 |
TCL | - | 47 |
TCL | KYMENE2064 | 77 |
TCL | KYMENE450 | 70 |
TCL | KYMENE557 | 41 |
TCL* | Al低聚物 | 94,97 |
TCL | SNOWTEXAK纳米颗粒 | 95 |
VIVA抹布* | - | 58,48 |
VIVA抹布* | KYMENE2064 | 83,73,78 |
VIVA抹布 | KYMENE450 | 59 |
VIVA抹布 | KYMENE557 | 80 |
VIVA抹布 | Al低聚物 | 82 |
VIVA抹布 | SNOWTEXAK纳米颗粒 | 68 |
Airlaid | - | 10 |
Airlaid | KYMENE2064 | 64 |
Airlaid | KYMENE450 | 67 |
Airlaid | KYMENE557 | 36 |
Airlaid | Al低聚物 | 75 |
Airlaid | SNOWTEXAK纳米颗粒 | 57 |
*多次试验的材料
所有材料,处理的和未处理的,在超声处理后都表现出PBS溶液中细菌的减少。最引人注目的结果存在于用KYMENE2064、KYMENE450、铝低聚物,某些情况下用SNOWTEXAK纳米颗粒处理的材料中。在除WYPALL材料外的所有情况下,处理的材料都表现出比未处理材料大的溶液中的细菌减少。希望处理材料按照这种细菌粘附过程减少细菌生长至少50%;更希望至少75%,还更希望至少90%。
试验4-汽蒸ζ电势分析-用于测量被处理基底的表面电荷:
当迫使电解质溶液通过多孔材料塞时,由于离子在扩散层的运动而形成汽蒸电势,其可用Electro Kinetic Analyzer(来自BrookhavenInstruments Corporation,Holtsville,NY,USA)测量。然后使用该值按照D.Fairhurst和Ribitsch(Particle Size Distribution II,Assessmentand Characterization,第22章,ACS Symposium Series 472,Provder编辑,Theodore,ISBN 0841221170)公布的公式计算ζ电势。
在样品制备期间,将处理和未处理的基底切成两个相同的片(120mm×50mm),然后放入样品电池中,在它们之间具有TEFLON隔片。在将样品电池装到仪器上后,通过吹扫除去全部空气气泡。然后迫使KCl溶液(1mM,pH=5.9,温度=22℃)通过介质的两个层,并使用Ag/AgCl电极测量汽蒸电势。在类似的pH、溶液导电性下使用相同的隔片数目测试所有样品。
每次测试重复4次,结果汇总在下面的表中。
材料 | 处理物 | 汽蒸ζ电势(mV) |
WYPALLX80 | - | -1 |
WYPALLX80 | KYMENE2064 | +11 |
WYPALLX80 | KYMENE450 | +12 |
WYPALLX80 | KYMENE557 | +5 |
WYPALLX80 | Al低聚物 | +8 |
WYPALLX80 | SNOWTEXAK | +25 |
TCL | - | -2 |
TCL | KYMENE2064 | +29 |
TCL | KYMENE450 | +33 |
TCL | KYMENE557 | +15 |
TCL* | Al低聚物 | +25 |
TCL | SNOWTEXAK | +27 |
VIVA抹布* | - | -11 |
VIVA抹布* | KYMENE2064 | +23 |
VIVA抹布 | KYMENE450 | +22 |
VIVA抹布 | KYMENE557 | +11 |
VIVA抹布 | Al低聚物 | +7.3 |
VIVA抹布 | SNOWTEXAK | +13 |
Airlaid | - | -6 |
Airlaid | KYMENE2064 | +40 |
Airlaid | KYMENE450 | +38 |
Airlaid | KYMENE557 | +31 |
Airlaid | Al低聚物 | +17 |
Airlaid | SNOWTEXAK | +25 |
由数据可看出,未处理基底的ζ电势是负的,在pH~5.9下为-11mV到-1mV。未处理基底的负值表明在多数细菌和未处理基底之间应存在斥力。处理后,全部基底的ζ电势变成正的。发现大多数带阳电荷的基底为用KYMENE2064、KYMENE450、铝低聚物和SNOWTEXAK纳米颗粒处理的材料。
试验5-通过擦拭除去细菌:
将氢氯酸铝处理(1wt%)和未处理的TCL材料切成5cm×15cm样品。在进行擦拭试验前,在无菌过滤PBS(3mL每个样品)中浸泡材料2小时。使抗氨苄青霉素的大肠杆菌溶液的系列稀释液达到~106个细胞/ml的最终浓度。将500微升106个细胞/ml的大肠杆菌溶液点到一片瓷砖上。在大肠杆菌点上面放置材料样品,进行多次擦拭(1~5)。擦拭后,擦洗细菌完全离开砖表面。将擦洗液放到1mL无菌PBS中。将100微升PBS溶液一式二份在含氨苄青霉素的LB琼脂培养皿上培养。数据描述为擦拭后砖上存在的残留细菌的百分比,并提供在下面的表中。
材料 | 输入细菌 | 擦拭次数 | 残留菌落(×0.1) | 细菌除去率% |
TCL | 7.5×105 | 1 | 211 | 99.7 |
2 | 75 | 99.9 | ||
3 | 167 | 99.8 | ||
4 | 28 | 99.96 | ||
5 | 46 | 99.94 | ||
9.35×105 | 1 | 328 | 99.6 | |
2 | 173 | 99.8 | ||
3 | 336 | 99.6 | ||
4 | 295 | 99.7 | ||
5 | 53 | 99.9 | ||
8.45×105 | 1 | 123 | 99.9 | |
2 | 45 | 99.95 | ||
3 | 19 | 99.98 | ||
4 | 18 | 99.98 | ||
5 | 290 | 99.7 | ||
氢氯酸铝TCL | 7.5×105 | 1 | 98 | 99.9 |
2 | 46 | 99.94 | ||
3 | 1 | 99.999 | ||
4 | 2 | 99.997 | ||
5 | 1 | 99.999 | ||
9.35×105 | 1 | 88 | 99.9 | |
2 | 77 | 99.9 | ||
3 | 39 | 99.96 | ||
4 | 6 | 99.99 | ||
5 | 10 | 99.99 | ||
8.45×105 | 1 | 26 | 99.97 | |
2 | 25 | 99.97 | ||
3 | 24 | 99.97 | ||
4 | 8 | 99.99 | ||
5 | 8 | 99.99 |
试验6-通过擦拭转移细菌:
按上面试验5所述使用处理和未处理的TCL材料进行擦拭。四次擦拭后,用包含细菌的材料擦拭无菌砖表面4次。按如上所述擦洗砖表面以捕获被转移到表面上的任何细菌。将擦洗物放在1mL无菌PBS中。将100微升PBS溶液一式二份在含氨苄青霉素的LB琼脂培养皿上培养。数据提供在下面的表中(数据为LB/氨苄青霉素培养皿上存在的菌落数)。
材料 | 残留细菌 | 转移的细菌 |
TCL | 52 | 4 |
15 | 59 | |
165 | 6 | |
Al-TCL | 1 | 0 |
4 | 1 | |
5 | 1 |
输入细菌=7.1×105个细胞
材料 | 转移的细菌 |
TCL | 68 |
104 | |
80 | |
Al-TCL | 3 |
1 | |
0 |
输入细菌=7.0×105个细胞
试验7-通过直接接触转移细菌:
进行另一组试验,其中将细菌直接加到搁置在瓷砖上的试验材料上。将氢氯酸铝(1wt%)处理的TCL、Scott纸巾和海绵(3M的ScotchBrite)放在瓷砖上。将500微升含细菌的溶液(~5×105个细胞)直接加入到每种材料上。使材料离开砖,用放在1mL PBS中的药签除去通过材料渗漏的任何细菌。然后将材料沿细菌侧向下放到干净的无菌砖上。然后在材料顶部放置1.2kg重物几分钟。除去重物和材料,用放在1mL PBS中的药签除去转移到干净砖表面上的任何细菌。培养100微升PBS/药签溶液。一式二份。数据提供在下面的表中(数据为LB/氨苄青霉素培养皿上存在的菌落数)。
材料 | 细菌穿透 | 转移的细菌 |
Al-TCL | 0 | 0 |
0 | 1 | |
0 | 0 | |
Scott纸巾 | >500 | 44 |
>500 | 223 | |
>500 | 151 | |
ScotchBrite海绵 | 0 | 24 |
(15次洗涤) | 0 | 19 |
0 | 1 |
输入细菌=5.8×105个细胞
材料 | 转移的细菌 |
Al-TCL | 2 |
2 | |
4 | |
海绵 | 19 |
(20次洗涤) | 13 |
27 | |
Scott纸巾 | 199 |
试验8-捕获的可见指示:
进行另一组试验,其中使用大小类似于细菌(约1μm)的蓝色负电荷微珠提供捕获的可见证据。在PBS中按1∶3稀释微珠。向尿布未处理的TCL和按上述用氢氯酸铝处理的TCL中加入100微升微珠溶液。然后在去离子水中用力洗涤基底。洗涤后,未处理的基底基本没有蓝色,表明微珠已被洗去。处理的TCL清楚地保留了蓝色,表明了微珠的保持性。
本领域那些技术人员能认识到,对本发明的改变和变化被认为在本领域那些技术人员的能力内。这种改变的例子包含在上面所述的专利中,本文在与本说明书一致的程度上全文引入它们中的每一个作为参考。这种改变和变化被本发明人预计在本发明的范围内。还应认识到,本发明的范围不应被解释为限制于本文公开的具体实施方案,而是在按照上述公开阅读时与附加的权利要求一致。
Claims (19)
1.一种用于除去带负电荷的粒子的产品,包括其上具有带正电荷的化合物的基底,其中所述化合物允许至少80%的细菌菌落存活率。
2.权利要求1的产品,其中所述带正电荷的化合物被嵌入在熔融挤出的聚合物纤维中。
3.权利要求1的产品,其中所述带正电荷的化合物被施加在所述基底的表面上。
4.权利要求1的产品,其中所述化合物为阳离子聚合物。
5.权利要求1的产品,其中所述化合物为表氯醇-官能化的聚胺。
6.权利要求1的产品,其中所述化合物为带正电荷的纳米颗粒。
7.权利要求1的产品,其中所述化合物为氧化铝低聚物。
8.权利要求3的产品,其中在足以粘着所述化合物到所述基底的温度和时间下热处理所述基底。
9.权利要求1的产品,其中所述基底由按照选自熔喷、共成形、纺粘、气流成网、粘合梳理、零应变拉伸和Z-方向定向中的方法制造的无纺布制成。
10.权利要求3的产品,其中所述化合物按水基计以0.01和10wt%之间的量被施加到所述基底上。
11.权利要求3的产品,其中所述化合物按水基计以0.05和7wt%之间的量被施加到所述基底上。
12.权利要求3的产品,其中所述化合物按水基计以0.1和5wt%之间的量被施加到所述基底上。
13.权利要求1的产品,其中所述基底按照细菌粘附过程减少细菌生长至少50%。
14.权利要求1的产品,其中所述基底按照细菌粘附过程减少细菌生长至少75%。
15.权利要求1的产品,其中所述基底按照细菌粘附过程减少细菌生长至少90%。
16.权利要求1的产品,其中所述基底选自个人护理产品、口腔护理产品和存储物品、个人修饰产品、面巾纸、卫生纸、面膜、外科长外衣、被单、医疗器械、手套、抽水马桶清洗器、硬表面清洁器、海绵、厨房清洁材料、农业、动物和宠物护理物品、猫粪土、种子制备物、土壤处理物、空气过滤器、水过滤器、离子去除过滤器和食品贮藏垫。
17.一种用于从表面除去细菌的产品,包括阳离子化合物,该化合物在足以粘着所述化合物到所述基底上的温度和时间下被涂覆在所述基底上,其中所述化合物允许至少80%的细菌菌落存活率。
18.权利要求17的产品,包括水力缠结纸浆和合成纤维。
19.一种用于从表面除去细菌的产品,包括其上具有阳离子纳米颗粒处理物的纸浆和合成纤维的网。
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- 2004-12-22 WO PCT/US2004/043301 patent/WO2005063307A1/en not_active Application Discontinuation
- 2004-12-22 CN CNB200480038555XA patent/CN100457193C/zh not_active Expired - Fee Related
- 2004-12-22 KR KR1020067012426A patent/KR20060117971A/ko not_active Application Discontinuation
- 2004-12-22 EP EP04815384.5A patent/EP1696967B1/en not_active Expired - Fee Related
- 2004-12-22 US US10/583,423 patent/US20070134337A1/en not_active Abandoned
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101896209A (zh) * | 2007-12-13 | 2010-11-24 | 金伯利-克拉克环球有限公司 | 从表面去除细菌的自指示擦拭品 |
CN101896209B (zh) * | 2007-12-13 | 2014-05-07 | 金伯利-克拉克环球有限公司 | 从表面去除细菌的自指示擦拭品 |
Also Published As
Publication number | Publication date |
---|---|
EP1696967A1 (en) | 2006-09-06 |
WO2005065727A1 (en) | 2005-07-21 |
US20070134337A1 (en) | 2007-06-14 |
EP1696967B1 (en) | 2013-05-22 |
US20050137540A1 (en) | 2005-06-23 |
WO2005063307A1 (en) | 2005-07-14 |
KR20060117971A (ko) | 2006-11-17 |
CN100457193C (zh) | 2009-02-04 |
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