CN116324065A - 用于制备包含纳米纤维的纤维材料的制剂和方法及包含该纤维材料的过滤器 - Google Patents
用于制备包含纳米纤维的纤维材料的制剂和方法及包含该纤维材料的过滤器 Download PDFInfo
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- CN116324065A CN116324065A CN202180051370.6A CN202180051370A CN116324065A CN 116324065 A CN116324065 A CN 116324065A CN 202180051370 A CN202180051370 A CN 202180051370A CN 116324065 A CN116324065 A CN 116324065A
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- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 26
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Abstract
一种用于制备包括纳米纤维的纤维材料的制剂和方法,以及由该制剂制备的纤维材料和纤维材料的应用。该制剂包含(a)至少一种聚合物,(b)至少一种溶剂,至少一种聚合物溶解于其中以提供聚合物溶液,和(c)至少一种赋予纤维材料功能性的功能性添加剂。至少一种功能性添加剂溶解或悬浮在聚合物溶液中。该制剂能够去除或降低细菌、病毒和重金属的浓度,同时保持高过滤效率。
Description
相关申请的交叉引用
本申请要求于2020年11月30日提交的序列号为63/119,120的美国临时申请的权益,其全部内容通过引用并入本文。
发明领域
本发明涉及制备纳米级和/或亚微米级纤维材料的制剂和方法,该纤维材料可以被功能化以表现出一种或多种有利特性,包括去除或降低细菌、病毒和重金属浓度的同时具有良好的过滤性、渗透性和吸附性的能力。本发明还涉及由制剂制备的纤维材料和该纤维材料的应用。
发明背景
由于高度多孔结构、纳米级孔隙和分布以及高比表面积的特性,由纳米级和/或亚微米级纤维制成的具有多孔结构的材料的重要性迅速增加,这导致了在面罩、空气过滤、水净化、液体过滤、海水淡化、蒸馏、组织工程、防护服、复合材料、电池隔膜、传感器、伤口敷料、高透气织物等方面的各种应用。特别是,纳米尺寸的膜可以过滤掉纳米级的有害颗粒,例如会损害人体肺部的PM2.5颗粒。
对于具有多孔结构的聚合物材料,会生成直径从几十纳米到几十微米的纤维。许多合成和制造方法已经被证明可以产生纤维形式的纳米结构。在这些方法中,静电纺丝是用于制造直径从几十纳米到几十微米的高质量超细纤维以供具有多孔结构的聚合物材料的最流行和最简单的制造方法之一。静电纺丝制备的纳米纤维具有多种特性,如高表面积、高孔结构、小孔径等。因此,它们可用于各种目的,包括过滤。纳米纤维可以极大地提高过滤介质去除气流中的微粒和水中存在的杂质的能力。纳米纤维可能是用于面罩和其他空气过滤应用,以及滤水器和其他水处理应用中的过滤材料的关键要素,因为它们每单位质量的表面积非常高,可以提高它们的捕获效率。
因此,宜用纳米纤维形成用于各种类型的过滤应用的纤维材料。在纳米纤维中包含一种或多种功能性添加剂以增强多孔纤维的抗微生物作用、清洁和/或消毒性能,并能够从水中全面去除各种不需要的颗粒和其他杂质也是有益的。
发明概要
本发明的主要目的是提供用于制备用于纳米纤维生产的聚合物溶液的制剂。该制剂包含一种或多种功能性添加剂,以使聚合物溶液功能化,从而使电纺纳米纤维功能化,从而提高性能。
本发明的第一方面满足了这个和其他目的,其提供了用于制备包含纳米纤维的纤维材料的制剂,其包含以下组分:
(a)至少一种聚合物,
(b)至少一种溶剂,其中溶解至少一种聚合物以提供聚合物溶液,和
(c)赋予纤维材料功能性的至少一种功能性添加剂,其中至少一种功能性添加剂包括选自下组(c1)至(c3)中的一种或多种:
(c1)抗微生物剂,
(c2)加工助剂,
(c3)物理和/或化学污染物的屏障剂,
其中至少一种功能性添加剂可溶解或悬浮在聚合物溶液中。
在本发明的一个优选实施方式中,组分(a)至(c)总计为制剂的100重量%,其中组分(c1)、(c2)和(c3)可以单独或以任何组合存在于制剂中。
在本发明的某些情况下,抗微生物剂可选自下组:聚维酮碘(PVP-I)、奥替尼啶(octenidine,OCT)、聚双胍、季铵化合物、氯二甲酚、银纳米颗粒(Ag-NP)、二氧化硅纳米颗粒(Si-NP)、聚乙烯亚胺(PEI)、N-卤胺、柠檬酸锌、三氯生、多酚、苯基羧酸、鞣花酸及它们的任意组合。在本发明的某些情况下,抗微生物剂可选自下组:聚己缩胍(polyexanide,PHMB)、聚氨基丙基双胍(PAPB)、氯化铵、苯扎氯铵、苯并十二烷基氯化铵、苄索氯铵、苄基三乙基氯化铵(BTEAC)、甲基苄索氯铵、氯己定盐、氯化十六烷吡啶(cetylpyridiniumchloride)、西他氯铵(cetalkonium chloride)、西曲溴铵(cetrimonium bromide)、十六烷基三甲基铵盐、溴棕三甲铵、多法氯铵(dofanium chloride)、四乙基溴化铵、二癸基二甲基氯化铵、多米芬溴化物、儿茶素多酚、柿子单宁多酚、葡萄籽多酚、大豆多酚、柠檬皮多酚、咖啡多酚及它们的任意组合。
在本发明的某些情况下,加工助剂可以是亲水性生物相容性聚合物,优选选自:聚乙二醇(PEG)、聚(N-异丙基丙烯酰胺)、聚丙烯酰胺、聚乙烯亚胺、聚(丙烯酸)、聚(乙烯醇)(PVA)、聚(乙烯基吡咯烷酮)及它们的任意组合。
在本发明的某些情况下,屏障剂可以选自由氢氧化铝氧化物(AlO(OH))、电气石、电气石、沸石、光催化剂、活性炭及它们的任意组合组成的组。
在本发明的一个优选实施方式中,用于制备用于空气过滤器的纳米纤维的制剂包括:
(a)5-20重量%的至少一种聚合物,
(b)55-95重量%,优选65-95重量%的至少一种溶剂,
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,以及
(c3)0.1-5重量%的屏障剂,
其中,组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,和
其中,如果制剂包含两种或更多种添加剂,功能性添加剂(c1)、(c2)和(c3)各自占至少0.1-5重量%。
在本发明的另一个优选实施方式中,用于制备用于滤水器的纳米纤维的制剂包括:
(a)5-20重量%的PVDF,
(b)55-95重量%,优选65-94.7重量%的DMF,PVDF溶解在其中以提供聚合物溶液,和
(c1)抗微生物剂,包含0.1-10重量%的PVP-I,0.1-5重量%的OCT,以及0.1-5重量%的BTEAC,
其中组分(a)、(b)和(c1)总计为制剂的100重量%。
在本发明的一个进一步优选的实施方式中,制剂包括:
(a)5-20重量%的至少一种聚合物,
(b)55-94重量%,优选65-94重量%的至少一种溶剂,和
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,和
(c3)0.1-5重量%的屏障剂,
其中组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,并且
其中如果制剂包含两种或更多种添加剂,功能性添加剂(c1)、(c2)和(c3)各自占至少0.1-5重量%。
在本发明的又一优选实施方式中,制剂包含:
(a)5-20重量%的PAN,
(b)65-93.9重量%的DMF,PAN溶解在其中以提供聚合物溶液,
(c1)抗微生物剂,包含0.1-5重量%的BTEAC,以及
(c3)用于去除重金属的屏障剂,包含1-10重量%的氢氧化铝氧化物,
其中组分(a)、(b)、(c1)和(c3)总计为制剂的100重量%。
本发明的纤维材料适合用作气体过滤器、气液过滤器或液固过滤器的过滤介质。因此,在第二方面,本发明提供了一种过滤器,其包含的纤维材料用作过滤器的过滤介质的材料,该纤维材料由本发明的制剂制备。
发现本发明的纤维材料具有均匀分布的纳米纤维,平均直径小,过滤效率高,流速高,可用于气体和液体的过滤,特别是空气和水的过滤。由此制成的过滤器不仅能够去除物理和化学污染物,而且尤其能够过滤和杀灭生物污染物。
在本发明的一个实施方式中,过滤器是面罩类型,包括:
暴露于外部环境的外保护层,
构造成适合覆盖佩戴者的口和鼻的内层,以及
至少一个中间层,其包括由纤维材料制成,夹在外层和内层之间的过滤介质。
面罩的外层、中间过滤层和/或内层宜沿从内层到中间层的方向改变亲水性或疏水性,使得佩戴面罩时,在内层之间形成水分浓度梯度,内层水分最少,中间层水分最多。
在本发明的另一个实施方式中,过滤器是适用于便携式和家用水过滤系统的滤水器类型。
根据本发明的第三方面,一种用于制备包含纳米纤维的纤维材料的方法,包括以下步骤:
a)提供由根据本发明的制剂配制的聚合物溶液,
b)提供一个或多个收集电极和一个或多个纺丝电极,基材在它们之间穿过,
c)在一个或多个收集电极和一个或多个纺丝电极之间施加电压以产生静电场,该静电场在收集电极和纺丝电极之间产生静电纺丝区,和
d)供应聚合物溶液到一个或多个纺丝电极,在静电纺丝区从每个纺丝电极被拉成纳米纤维,以便将纳米纤维沉积到基材上。
本发明的方法还可以包括在将聚合物溶液供应到纺丝电极之前将粘合剂施加到聚合物溶液中的步骤,或者将水性分散体形式的粘合剂施加到其上沉积纳米纤维的基材上的步骤。
在本发明的一个实施方式中,该方法可以包括加载被赋予相同或不同功能的相同类型或不同类型的聚合物溶液用于静电纺丝的步骤,从而将相同类型或不同类型的纳米纤维内容物沉积到基材上。
在另一个实施方式中,该方法可以包括将不同性质的纳米纤维交织以形成具有更大柔韧性的交织结构的纤维层的步骤。
优选实施方式的详细描述
所公开的发明主要涉及用于纳米纤维生产的制剂的开发。纳米纤维包括一种或多种功能性添加剂,以改善纳米纤维的性能,包括去除或减少各种类型的污染物,例如那些难以去除的重金属、细菌和病毒、挥发性有机化合物(VOC)。纳米纤维具有多种用途,特别适用于生产过滤材料,可用于各种过滤工具。
在本发明中,由制剂制备的纤维材料可以由基材层和沉积在基材上的纳米纤维层组成。
在某些情况下,用于制备包含纳米纤维的纤维材料的制剂包含以下组分:
(a)至少一种聚合物,
(b)至少一种溶剂,至少一种聚合物溶解在其中以提供聚合物溶液,和
(c)赋予纤维材料功能性的至少一种功能性添加剂,
其中至少一种功能性添加剂包括选自下组(c1)至(c3)中的一种或多种:
(c1)抗微生物剂,
(c2)加工助剂,
(c3)物理和/或化学污染物的屏障剂,
其中组分(a)至(c)总计为制剂的100重量%,和
其中至少一种功能性添加剂可溶解或悬浮在聚合物溶液中。
宜将制剂配制成用于通过制剂的静电纺丝生产纳米纤维的聚合物溶液。制剂的静电纺丝可以在针型或无针型工具中进行。
组分(c1)、(c2)和(c3)可以单独或以任何组合存在于制剂中。在一些情况下,制剂可包含组分(a)、(b)和(c1)。在一些情况下,制剂可包含组分(a)、(b)和(c2)。在一些情况下,制剂可包含组分(a)、(b)和(c3)。在一些情况下,制剂可包含组分(a)、(b)、(c1)和(c2)。在一些情况下,制剂可包含组分(a)、(b)、(c1)和(c3)。在一些情况下,制剂可包含组分(a)、(b)、(c2)和(c3)。在一些情况下,制剂可包含组分(a)、(b)、(c1)、(c2)和(c3)。
本文中的术语“抗微生物剂”是指在接触时可以捕获、杀死或至少削弱感染源(包括细菌、病毒和/或真菌)以提供抗微生物和抗病毒功能的物质。感染源的实例包括金黄色葡萄球菌(S.aureus)、大肠杆菌(E.coli)、铜绿假单胞菌(P.aeruginosa)、表皮葡萄球菌(Staphylococcus epidermidis)、溶血性葡萄球菌(Staphylococcus haemolyticus)、肺炎克雷伯菌(Klebsiella pneumoniae)、药物敏感和耐药细菌、白色念珠菌(Candidaalbicans)、流感病毒等。根据本发明,抗微生物剂包括抗细菌剂、抗真菌剂和抗病毒剂,它们具有对抗感染的作用。抗微生物剂的实例可以选自聚维酮碘(PVP-I)、奥替尼啶(OCT)、聚双胍(例如聚己缩胍(PHMB)、聚氨基丙基双胍(PAPB))、季铵化合物(例如氯化铵、苯扎氯铵、苯并十二烷基氯化铵、苄索氯铵、苄基三乙基氯化铵(BTEAC)、甲基苄索氯铵、氯己定(CHX)盐、十六烷基氯化吡啶、西他氯铵、西曲溴铵(十六烷基三甲基铵盐)、溴棕三甲铵、多法氯铵、四乙基溴化铵、二癸基二甲基氯化铵、多米芬溴化物)、氯二甲苯酚、银纳米颗粒(Ag-NP)、二氧化硅纳米颗粒(Si-NP)、聚乙烯亚胺(PEI)、N-卤胺、柠檬酸锌、三氯生、多酚(例如儿茶素多酚、柿子单宁多酚、葡萄籽多酚、大豆多酚、柠檬皮多酚、咖啡多酚、香豆素)、苯基羧酸、鞣花酸及它们的任意组合。一些天然化合物,例如桑树皮、藤黄果粗提物,也可用作抗微生物剂。“它们的任意组合”是指同时选择上述化合物中的任意两种或更多种作为制剂的抗微生物剂。
本文中的术语“加工助剂”是指充当促进抗微生物剂的抗微生物能力的试剂或充当增强功能性添加剂与聚合物和/或聚合物溶液的结合的粘合剂的物质。在本发明的一个优选实施方式中,加工助剂是亲水性生物相容性聚合物。亲水性生物相容性聚合物可选自聚乙二醇(PEG)、聚(N-异丙基丙烯酰胺)、聚丙烯酰胺、聚乙烯亚胺、聚(丙烯酸)、聚(乙烯醇)(PVA)、聚(乙烯基吡咯烷酮),和它们的任意组合。“它们的任意组合”是指同时选择上述化合物中的任意两种或两种以上作为该制剂的高分子加工助剂。
本文中术语“物理和/或化学污染物的屏障剂”是指能够去除或减少物理和/或化学污染物的物质,例如重金属、氯、VOC和/或气味。例如,屏障剂可以选自用于去除重金属的氢氧化铝氧化物(AlO(OH))和/或电气石;或去除氯的电气石;或用于去除VOC的沸石、光催化剂(例如TiO2)和/或活性炭;或用于去除异味的沸石和/或活性炭。根据实际需要,可以在制剂中加入一种或多种屏障剂。
应当理解,如果需要,可以将其他添加剂添加到聚合物溶液中以提供具有其他功能的聚合物溶液/纳米纤维。
可用于本发明制剂的聚合物包括由疏水单体和/或亲水单体形成的聚合物。疏水单体可选自下组:偏二氟乙烯、丙烯腈、甲基丙烯酸酯、丙烯酸乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、乙酸乙烯酯、乙烯基吡咯烷酮、偏二氯乙烯、氯乙烯及它们的任意组合。亲水性单体可选自下组:丙烯酸、烯丙醇、甲基烯丙醇(methallyl alcohol)、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、丁二醇单丙烯酸酯、丙烯酸二甲基氨基乙酯、丁烯三羧酸、乙二醇、N-异丙基丙烯酰胺、丙烯酰胺、乙烯亚胺、乙烯醇、乙烯基吡咯烷酮及它们的任意组合。
本发明的制剂中可以使用的溶剂包括有机溶剂和无机溶剂,包括但不限于甲醇、乙醇、异丙醇(IPA)、丙酮、四氢呋喃、二氯甲烷、氯仿、二甲基亚砜(DMSO)、乙二醇、二甲基甲酰胺(N,N-二甲基甲酰胺,DMF)、二甲基乙酰胺(N,N-二甲基乙酰胺,DMAc)、N-甲基-2-吡咯烷酮(N-甲基吡咯烷酮,NMP)、环己烷、水或它们的任意组合。
为了说明的目的,在下文中讨论示例性的制剂。
用于制备用于空气过滤的聚合物溶液的示例性制剂具有以下组成:
(a)5-20重量%的至少一种聚合物,
(b)55-95重量%,优选65-95重量%的至少一种溶剂,所述至少一种聚合物溶解在其中以提供聚合物溶液,和
(c)赋予纤维纳米材料功能性的至少一种功能性添加剂,
其中至少一种功能性添加剂包括选自下组(c1)至(c3)中的一种或多种:
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,和
(c3)0.1-5重量%的物理和/或化学污染物屏障剂,
其中组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,和
其中如果制剂包含两种或更多种添加剂,每种功能性添加剂占至少0.1-5重量%。
在本发明的一个具体实施方式中,用于制备用于空气过滤的聚合物溶液的制剂具有以下组成:
(a)5-20重量%的PVDF,
(b)55-95重量%,优选65-94.7重量%的DMF,PVDF溶解在其中以提供聚合物溶液,和
(c1)抗微生物剂,包含0.1-10重量%的PVP-I,0.1-5重量%的OCT及0.1-5重量%的BTEAC,
其中组分(a)、(b)和(c1)总计为制剂的100重量%。
PVP-I和OCT在抗菌和抗病毒领域具有优异的功能。此外,它们对人体皮肤的刺激非常轻微或没有,因此是空气过滤和纺织品或床垫套等应用的良好添加剂。
用于制备用于水过滤的聚合物溶液的示例性制剂具有以下组成:
(a)5-20重量%的至少一种聚合物,
(b)55-94重量%,优选65-94重量%的至少一种溶剂,其中溶解至少一种聚合物以提供聚合物溶液,和
(c)赋予纤维纳米材料功能性的至少一种功能性添加剂,其中至少一种功能性添加剂包括选自下组(c1)至(c3)中的一种或多种:
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,和
(c3)0.1-5重量%的物理和/或化学污染物屏障剂,
其中组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,和
其中如果制剂包含两种或更多种添加剂,每种功能性添加剂占至少0.1-5重量%。
在本发明的一个具体实施方式中,用于制备用于水过滤的聚合物溶液的制剂具有以下组成:
(a)5-20重量%的PAN,
(b)65-93.9重量%的DMF,其中溶解PVDF以提供聚合物溶液,
(c1)抗微生物剂,包含0.1-5重量%的BTEAC,以及
(c3)用于去除重金属的屏障剂,包含1-10重量%的氢氧化铝氧化物(AIO(OH)),
其中组分(a)、(b)、(c1)和(c3)总计为制剂的100重量%。
BTEAC是一种极好的杀灭细菌、真菌和病毒的消毒剂,而氢氧化铝氧化物不溶于水,可有效应用于水过滤以便杀灭微生物和去除重金属。
在进行静电纺丝之前,通常将本发明的制剂制备的聚合物溶液的粘度配制在150-1800mPa.s,优选200-1500mPa.s,更优选300-1000mPa.s的范围内。已经发现具有不在上述数值范围内的粘度的聚合物溶液不容易或不适合形成聚合物电纺纤维。
本发明的优选制剂列于下表1中。
表1
应当理解,本发明不限于上述具体制剂。
本发明的制剂特别适用于将纳米纤维静电纺丝到基材上以制造纤维材料。在本发明的一个方面,一种用于制备包含纳米纤维的纤维材料的方法,包括以下步骤:
a)提供由本发明的制剂配制的聚合物溶液,
b)提供一个或多个收集电极和一个或多个纺丝电极,基材从其间穿过,
c)在一个或多个收集电极和一个或多个纺丝电极之间施加电压以产生静电场,该静电场在收集电极和纺丝电极之间形成静电纺丝区,和
d)提供聚合物溶液到一个或多个纺丝电极,从每个纺丝电极拉成纳米纤维,用于将纳米纤维沉积到基材上以产生纤维材料。
本发明的方法可以进一步包括在将聚合物溶液供应到纺丝电极之前将粘合剂施加到聚合物溶液中的步骤,以便增强制剂中的功能性添加剂、聚合物和聚合物溶液之间的结合。或者,粘合剂可以以水性分散体的形式提供,该水性分散体被施加到其上沉积纳米纤维的基材,以帮助沉积在基材上的电纺聚合物纳米纤维与聚合物溶液中的功能性添加剂之间的结合。更有利地,在进入纺丝区之前将粘合剂施加到基材上以进一步增强基材和电纺聚合物纳米纤维之间的粘附力。粘合剂的一个例子是Akrylep 417E。
任选地,沉积有纳米纤维的所得基材可重复进入静电纺丝装置(例如,无针型装置)以允许进一步沉积相同/不同纤维以增加纤维层的厚度和/或附加功能,或不同直径和/或聚合物特性的纤维形成两个或多个纤维层。在某些情况下,根据待制备的纤维的实际需要,可以使用两种或更多种不同的制剂来分别制备两种或更多种不同的聚合物溶液,用于电纺两层或更多层纳米纤维。
基材可以是平坦的和平面的片材,例如呈离散片材或连续片材的形式。基材可包括可提供机械强度以支撑一层或多层纳米纤维的任何多孔针织、机织和无纺材料。它可以包含一种或多种基于聚合物的纤维,选自聚丙烯、聚酯、尼龙、聚乙烯、聚氨酯、纤维素、聚对苯二甲酸丁二醇酯、聚对苯二甲酸乙二醇酯(PET)、纺粘聚丙烯(PPSB)、聚碳酸酯、聚甲基戊烯和/或聚苯乙烯,以及本领域已知的可用聚合物。在本发明的一个优选实施方式中,基材是纺粘聚丙烯(PPSB)。通常,PPSB具有至少106Ω的电阻,例如在106至1011Ω的范围内,优选在107至1010Ω的范围内,以产生小而细的纤维直径并防止在基材上形成含珠粒的纤维。
在无针静电纺丝过程中,可以通过调整以下参数来改变纤维层的结构、厚度、沉积密度和纳米纤维的直径,包括基材通过活性纺丝区的速度、在纺丝电极和收集电极之间施加的电压、电极之间的距离,以及聚合物溶液的成分。电极间距优选调整在20cm-250cm之间,更优选在30cm-220cm之间;施加的电压优选保持在-80kV~100kV之间,更优选在-60kV-90kV之间;温度优选保持在5℃-50℃之间,更优选在10℃-40℃之间;湿度优选保持在5%~70%之间,更优选保持在10%~60%之间。
使用本发明的方法,可以电纺一层或多层具有所需直径的纳米纤维,从而可以更大的灵活性制备包含至少一种类型的纳米纤维的梯度材料,以及具有不同特性的纳米纤维和微米纤维交织结构的材料。这里的“梯度”是指材料的特性,例如密度、孔径、纤维直径等。
优选在基材上应用一层或多层纳米纤维以适应不同的应用场景。纤维材料的纳米纤维层可以在厚度、直径、平均孔径和最大孔径方面变化。取决于制剂中存在的功能性添加剂,由制剂制造的一层或多层纳米纤维被功能化以具有各种功能,例如杀菌能力、杀微生物性能、去除重金属和气味。
本发明的纤维材料表现出优异的过滤性、渗透性和吸附性,重量轻,因此适合用作过滤介质。由此制造的纤维材料可以找到广泛的应用,包括但不限于过滤材料和纺织品。值得注意的是,纤维材料是空气过滤材料聚丙烯熔喷(PPMB)的极佳替代品,PPMB在本领域中已广泛用于制造个人防护设备,包括呼吸器、面罩等。具有由本发明的纤维材料制成的过滤介质的面罩是本发明的主题。
具体地,面罩包括:
暴露于外部环境的外保护层,
构造成适合覆盖佩戴者的口和鼻的内层,和
至少一个中间层,包含过滤介质并夹在外层和中间层之间。
面罩保护佩戴者免受空气中的污染物、杂质、细菌和病毒的吸入。由于中间层的过滤材料中存在一层或多层纳米纤维,面罩能够全面去除各种不需要的空气颗粒物、化学物质、生物污染物和其他杂质,从而实现全面的深度过滤。污染物包括但不限于病毒、细菌、灰尘或过敏物质。
面罩的外层和内层可以选自本领域已知的那些,并且优选地由无纺材料制成,所述无纺材料包括选自下组的一种或多种聚合物:聚烯烃(聚丙烯、聚乙烯等)、聚酯、聚酰胺、聚碳酸酯、聚苯乙烯或其混合物。外层是流体排斥性的,能够阻挡较大的颗粒。内层是吸湿的,并且更优选地由对穿戴者而言柔软、舒适和/或低过敏性材料制成。
优选地,所述外层、中间过滤层和/或内层沿从内层到中间层的方向改变亲水性或疏水性,使得佩戴面罩时,内层和中间层之间随着形成水分浓度梯度,内层水分最少,中间层水分最多。
本发明的过滤材料还可用作适用于便携式和家用水过滤系统的滤水器的过滤介质,例如用于饮用瓶中。水过滤器可以是圆柱形过滤器或其他配置的形式。
因此,本发明提供了多种制剂,以便制备可根据实际需要和便利的要求作功能化的纤维材料。纤维材料宜用作过滤材料或过滤屏障剂。本发明使静电纺丝各种聚合物溶液成为可能,从而获得能够去除或减少各种污染物的过滤材料,包括难以去除的重金属、细菌和病毒、挥发性有机化合物。
虽然本文所述的实施方式旨在作为用于制造纤维材料的示例性制剂及其生产以及包含纤维材料的过滤器,但本领域技术人员将理解本发明不限于所示实施方式。在不脱离本发明范围的情况下,本领域技术人员凭借本领域技术人员的公知常识,会想到许多其他可能的变化和修改,但是,这些变化和修改也落入本发明的范围。
Claims (25)
1.一种用于制备包含纳米纤维的纤维材料的制剂,包括以下组分:
(a)至少一种聚合物,
(b)至少一种溶剂,所述至少一种聚合物溶解在其中以提供聚合物溶液,和
(c)赋予纤维材料功能性的至少一种功能性添加剂,其中至少一种功能性添加剂包括选自下组(c1)至(c3)中的一种或多种:
(c1)抗微生物剂,
(c2)加工助剂,
(c3)物理和/或化学污染物的屏障剂,
其中至少一种功能性添加剂可溶解或悬浮在聚合物溶液中。
2.根据权利要求1所述的制剂,其特征在于,组分(a)至(c)总计为制剂的100重量%。
3.根据权利要求1所述的制剂,其特征在于,组分(c1)、(c2)和(c3)单独或以任何组合存在于所述制剂中。
4.如权利要求1所述的制剂,其特征在于,所述抗微生物剂选自下组:聚维酮碘(PVP-I)、奥替尼啶(OCT)、聚双胍、季铵化合物、氯二甲苯酚、银纳米颗粒(Ag-NP)、二氧化硅纳米颗粒(Si-NP)、聚乙烯亚胺(PEI)、N-卤胺、柠檬酸锌、三氯生、多酚、苯基羧酸、鞣花酸及它们的任意组合。
5.如权利要求1所述的制剂,其特征在于,所述抗微生物剂选自下组:聚己缩胍(PHMB)、聚氨丙基双胍(PAPB)、氯化铵、苯扎氯铵、苯并十二烷基氯化铵、苄索氯铵、苄基三乙基氯化铵(BTEAC)、甲基苄索氯铵、氯己定盐、氯化十六烷吡啶、西他氯铵、西曲溴铵、十六烷基三甲基铵盐、溴棕三甲铵、多法氯铵、四乙基溴化铵、二癸基二甲基氯化铵、多米芬溴化物、儿茶素多酚、柿子单宁多酚、葡萄籽多酚、大豆多酚、柠檬皮多酚、咖啡多酚及它们的任意组合。
6.根据权利要求1至5中任一项所述的制剂,其特征在于,所述加工助剂是亲水性生物相容性聚合物,优选选自下组:聚乙二醇(PEG)、聚(N-异丙基丙烯酰胺)、聚丙烯酰胺、聚乙烯亚胺、聚(丙烯酸)、聚(乙烯醇)(PVA)、聚(乙烯基吡咯烷酮)及它们的任意组合。
7.根据权利要求1至5中任一项所述的制剂,其特征在于,所述屏障剂选自氢氧化铝氧化物(AlO(OH))、电气石、电气石、沸石、光催化剂、活性炭及它们的任意组合。
8.根据权利要求1至5中任一项所述的制剂,其特征在于,所述聚合物包括由疏水单体和/或亲水单体形成的聚合物。
9.如权利要求8所述的制剂,其特征在于,所述疏水单体选自下组:偏氟乙烯、丙烯腈、丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、乙酸乙烯酯、乙烯基吡咯烷酮、偏二氯乙烯、氯乙烯和它们的任意组合。
10.根据权利要求8所述的制剂,其特征在于,所述亲水性单体选自下组:丙烯酸、烯丙醇、甲基烯丙醇、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、丁二醇单丙烯酸酯、丙烯酸二甲基氨基乙酯、丁烯三羧酸、乙二醇、N-异丙基丙烯酰胺、丙烯酰胺、乙烯亚胺、乙烯醇、乙烯基吡咯烷酮及它们的任意组合。
11.如权利要求1至5中任一项所述的制剂,其特征在于,所述溶剂选自下组:甲醇、乙醇、异丙醇(IPA)、丙酮、四氢呋喃、二氯甲烷、氯仿、二甲基亚砜(DMSO)、乙二醇、二甲基甲酰胺(N,N-二甲基甲酰胺,DMF)、二甲基乙酰胺(N,N-二甲基乙酰胺,DMAc)、N-甲基-2-吡咯烷酮(N-甲基吡咯烷酮,NMP)、环己烷、水或它们的任意组合。
12.如权利要求1至5中任一项所述的制剂用于制备用于空气过滤器的纳米纤维,包含:
(a)5-20重量%的至少一种聚合物,
(b)55-95重量%,优选65-95重量%的至少一种溶剂,
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,和
(c3)0.1-5重量%的屏障剂,
其中组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,和
其中如果制剂包含两种或更多种添加剂,功能性添加剂(c1)、(c2)和(c3)各自占至少0.1-5重量%。
13.如权利要求12所述的制剂,其包含:
(a)5-20重量%PVDF,
(b)55-95重量%,优选65-94.7重量%的DMF,PVDF溶解在其中以提供聚合物溶液,和
(c1)抗微生物剂,包含0.1-10重量%的PVP-I,0.1-5重量%的OCT,以及0.1-5重量%的BTEAC,
其中组分(a)、(b)和(c1)总计为制剂的100重量%。
14.如权利要求1至5中任一项所述的制剂用于制备用于滤水器的纳米纤维,包含:
(a)5-20重量%的至少一种聚合物,
(b)55-94重量%,优选65-94重量%的至少一种溶剂,和
(c1)0.1-15重量%,优选0.1-10重量%,更优选0.1-5重量%的抗微生物剂,
(c2)0.1-5重量%的加工助剂,和
(c3)0.1-5重量%的屏障剂,
其中组分(a)、(b)、(c1)至(c3)总计为制剂的100重量%,和
其中如果制剂包含两种或更多种添加剂,功能性添加剂(c1)、(c2)和(c3)各自占至少0.1-5重量%。
15.如权利要求14所述的制剂,其包含:
(a)5-20重量%的PAN,
(b)65-93.9重量%的DMF,PAN溶解在其中以提供聚合物溶液,
(c1)抗微生物剂,包含0.1-5重量%的BTEAC,和
(c3)用于去除重金属的屏障剂,包含1-10重量%的氢氧化铝氧化物,
其中组分(a)、(b)、(c1)和(c3)总计为制剂的100重量%。
16.根据权利要求1至5中任一项所述的制剂,其特征在于,所述聚合物溶液的粘度范围为150-1800mPa.s,优选200-1500mPa.s,更优选300-1000mPa.s。
17.权利要求1至5任一项所述的制剂,选自表1。
18.一种过滤器,其包含用作过滤器的过滤介质的材料的纤维材料,其中所述纤维材料由权利要求1至16中任一项所述的制剂制备。
19.根据权利要求18所述的过滤器,其特征在于,所述过滤器是面罩类型,包括:
暴露于外部环境的外保护层;
被配置为适合覆盖佩戴者的口和鼻的内层;和
至少一个中间层,包含过滤介质并夹在外层和内层之间。
20.根据权利要求19所述的过滤器,其特征在于,所述外层、中间过滤层和/或内层沿从内层到中间层的方向改变亲水性或疏水性,使得佩戴面罩时,在内层和中间层之间形成水分浓度梯度,内层水分最少,中间层水分最多。
21.根据权利要求18所述的过滤器,其特征在于,所述过滤器是适用于便携式和家用水过滤系统的滤水器类型。
22.一种生产包含纳米纤维的纤维材料的方法,包括以下步骤:
a)提供由根据权利要求1至17中任一项所述的制剂配制的聚合物溶液,
b)提供一个或多个收集电极和一个或多个纺丝电极,基材在它们之间穿过,
c)在一个或多个收集电极和一个或多个纺丝电极之间施加电压以产生静电场,该静电场在收集电极和纺丝电极之间产生静电纺丝区,和
d)将聚合物溶液供应至一个或多个纺丝电极,从每个纺丝电极被拉成纳米纤维,以便将纳米纤维沉积到基材上。
23.根据权利要求22所述的方法,进一步包括在将聚合物溶液供应到纺丝电极之前将粘合剂施加到聚合物溶液中的步骤,或者将水性分散体形式的粘合剂施加到其上沉积纳米纤维的基材上的步骤。
24.如权利要求22或23所述的方法,包括将所述纳米纤维交织以形成具有交织结构的纤维层的步骤。
25.一种纤维材料,其包含:
基材;
施加在基材上的一层或多层纳米纤维,
其中,所述纳米纤维由权利要求1至17的制剂制成。
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CN115323522B (zh) * | 2022-09-20 | 2023-08-18 | 江苏集萃先进纤维材料研究所有限公司 | 一种抗菌聚酰胺纤维及其制备方法 |
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