CN100537020C - 气味脱除和控制用金属离子改性高表面积材料 - Google Patents

气味脱除和控制用金属离子改性高表面积材料 Download PDF

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CN100537020C
CN100537020C CNB038093421A CN03809342A CN100537020C CN 100537020 C CN100537020 C CN 100537020C CN B038093421 A CNB038093421 A CN B038093421A CN 03809342 A CN03809342 A CN 03809342A CN 100537020 C CN100537020 C CN 100537020C
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ion
nano particle
compound
metal ion
potential
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CN1649666A (zh
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J·G·麦克唐纳
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Kimberly Clark Worldwide Inc
Kimberly Clark Corp
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Kimberly Clark Worldwide Inc
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Abstract

本发明涉及高表面积材料，例如，纳米颗粒，其涂以金属离子。此种改性纳米颗粒具有能结合各种气体和/或有气味化合物的活性部位，借此从介质如空气或水中除掉这些化合物。金属离子被吸附到纳米颗粒的表面并牢固地结合在该表面上。通过金属离子的选择，可靶向特定气态化合物和/或有气味化合物并将它们有效地除掉，并且既可从水相中也可从空气中有效除掉。该改性纳米颗粒可用于许多工业和消费用制品中。

Description

气味脱除和控制用金属离子改性高表面积材料
技术领域
本发明涉及用于中和或脱除气体和/或有气味化合物的改性高表面积材料。高表面积材料，如纳米颗粒，被涂以可结合气体分子和/或有气味化合物的金属离子。该改性的高表面积材料可加入到各种不同工业和消费产品中，包括吸收制品、空气和水的过滤器、家用清洁剂、织物和纸巾。
背景技术
为配制有效脱除气味体系曾进行过许多尝试且目前已有各种消费产品供应，用于对付有气味化合物。某些产品设计成通过放出较强、占据主导地位的气味来掩盖臭味，例子包括香味空气清新喷雾剂和蜡烛。另一种对付有气味化合物，包括氨、甲硫醇、三甲胺以及其他各种硫化物和胺，的办法，是通过能吸收这些化合物的脱臭剂将这些化合物从介质中除掉。
活性炭和碳酸氢钠是两种能吸收气味的常用化合物。然而，活性炭的脱除气味能力通常比较低，尤其是对氨味以及当存在湿气时，而且活性炭的黑颜色缺乏用于吸收制品如尿布，所要求的美学上令人愉快的特性。碳酸氢钠，以及其他白色气味吸收剂如硅胶和沸石，通常吸收能力低于活性炭，因此效力差。
二氧化钛颗粒，例如美国专利5,480,636，授予Maruo等人，所公开的，也可用于脱除少数气味，例如，氨。美国专利5,480,636建议加入锌氧和硅氧化合物到二氧化钛中以拓宽二氧化钛的脱除气味能力。然而，这一做法仍然受到二氧化钛需要光才能将有气味化合物转变为无气味化合物这一二氧化钛的光催化剂本性的限制。再者，如美国专利5,480,636所公开的二氧化钛化合物不能用于水溶液中。
除了气味难闻的化合物之外，还需要能脱除那些虽然不一定有气味但却会引起负面效应的气体的产品。此种气态化合物的一个例子是乙烯。乙烯，一种天然荷尔蒙，由水果作为一种催熟剂放出。通过除掉乙烯气，可延缓和控制水果的成熟从而允许长期贮存和运输。
目前需要一种干态和在溶液中都有效的气体和/或气味-脱除/中和化合物。目前需要一种各种工业和消费产品都可使用的有效脱除气味/中和化合物。目前需要一种能轻易地施加到各种表面和材料上的气体和/或气味脱除/中和化合物。
发明概述
本发明涉及涂以金属离子的高表面积材料。此种改性高表面积材料具有能结合至少一种气态化合物和/或有气味化合物的活性部位，借此从介质如空气或水中除掉这些化合物。纳米颗粒是一类能在本发明中用来除掉至少一种气态化合物和有气味化合物的高表面积材料。至少一种类型金属离子被吸附到纳米颗粒的表面并牢固地结合在表面上。通过金属离子的选择，可靶向某些气态化合物和/或有气味化合物并将它们有效地除掉，并且既可从水相中也可从空气中有效除掉。本发明采用高表面积纳米颗粒作为模板来吸附以至少一种气态化合物和有气味化合物为目标的特定官能团(金属离子)，并与所述化合物形成络合物和从介质中除掉所述化合物。例如，二氧化硅纳米颗粒用铜离子改性(或替代地，银离子)以后，已证明能有效脱除基于胺和硫的有气味化合物类。
本发明的目的是创造一种有效的气态化合物脱除体系。本发明可用于各种工业和消费产品。本发明另一个目的是创造一种用于抑制植物体成熟的气态化合物脱除体系。
本发明另一个目的是创造一种既可用于水相也可用于空气中的有效脱除气味化合物。本发明另一个目的是创造一种能有效地用于各种工业和消费产品中的有效脱除气味化合物。本发明可与各种脱除气味产品组合使用。本发明改性高表面积材料可在诸如尿布和女性用品之类吸收制品中用于脱除气味。本发明的改性高表面积材料可用于过滤装置和涂布到墙壁、壁纸和玻璃上用以脱除气味。本发明改性高表面积材料可用于口腔护理产品如漱口剂和口香糖，以便去除口腔中引起不愉快气味的化合物。
上述以及其他特征和优点在结合附图研读了下文目前优选的实施方案的详述之后将进一步变得更加清楚。
附图简述
图1是本发明一种实施方案的改性纳米颗粒的图示。
图2A是高效液相色谱法色谱图。
图2B是高效液相色谱法色谱图。
图3A是高效液相色谱法色谱图。
图2B是高效液相色谱法色谱图。
目前优选实施方案详述
本发明涉及高表面积材料，例如纳米颗粒，其用至少一种金属离子改性。本发明的改性高表面积材料可用于去除气态化合物和/或有气味化合物。“气态化合物”或“气体”包括任何能以气体或蒸汽形式存在的分子或化合物。“有气味化合物”或“气味”是指任何可被嗅觉系统察觉的分子或化合物。有气味化合物可作为气态化合物存在，也可存在于其他介质如液体中。
本发明高表面积材料具有至少一种存在于高表面积材料表面的金属离子，该金属离子造成一种能结合至少一种气态化合物和/或有气味化合物的活性部位，借此从周围环境除掉该化合物。高表面积材料也可通过直接将某些气态化合物和/或有气味化合物吸附到高表面积材料的表面区域上，将它们从周围环境吸收。
本发明气体和/或气味脱除颗粒是改性高表面积材料。可用于本发明的高表面积材料，由于单个高表面积材料的颗粒尺寸小，而具有大表面积。可用于本发明的高表面积材料具有至少约200m2/g的适宜表面积，更适宜500m2/g，更适宜800m2/g。
纳米颗粒是可用于本发明的高表面积材料的例子。“纳米颗粒”指的是颗粒直径小于约500nm的高表面积材料。虽然下面将具体地以纳米颗粒为例来描述本发明，但要知道，本发明就各种不同的高表面积材料来说均是有效的。图1显示本发明的一种实施方案的改性纳米颗粒10，可用作气体和/或气味脱除颗粒。改性纳米颗粒10包括纳米颗粒15和金属离子20。然而图1显示，大量金属离子20改性的纳米颗粒10可具有各种不同数量的金属离子20，并将具有至少一个金属离子20。改性纳米颗粒10可用于去除各种气态化合物和/或有气味化合物。能除掉的具体化合物一般取决于所用具体金属离子20和纳米颗粒15的类型。
可用于本发明的纳米颗粒包括但不限于，二氧化硅、氧化铝、氧化镁、二氧化钛、氧化铁、金、氧化锌、氧化铜，有机纳米颗粒如聚苯乙烯，以及它们的组合。纳米颗粒一般不是离子的但却具有某一总ζ-电位。“ζ-电位”指的是存在于所有固体与液体界面两侧的电位或电动势。具有正或负ζ-电位的纳米颗粒都是已知的。在纳米颗粒表面自然发生的化学反应导致该纳米颗粒的ζ-电位的形成。例如，二氧化硅纳米颗粒是二氧化硅分子的四面体络合物。在二氧化硅颗粒的表面，二氧化硅分子可发生化学反应生成硅烷醇基(SiOH)，该硅烷醇基团与其他硅烷醇基团起反应生成硅氧烷键(Si-O-Si键)。硅烷醇基团的脱水反应生成硅烷醇键，而该逆反应产生负ζ-电位，并让带正电的金属离子吸附到二氧化硅上。
本发明使用的纳米颗粒通常将具有第一ζ-电位和，由于加入带相反电荷的金属离子导致金属离子吸附到纳米颗粒上以后的第二ζ-电位。纳米颗粒ζ-电位的变化与吸附到纳米颗粒上的金属离子数量有关。此种关系提供一种确定被吸附金属离子数量的测定法和控制吸附量的方法。例如，向二氧化硅纳米颗粒溶液中滴加氯化铜稀溶液，直至二氧化硅悬浮体的ζ-电位从-25mV改变到较高ζ-电位，例如，介于约-5mV～-15mV，据发现，将提供足以脱除特定有气味化合物的吸附到纳米颗粒上的金属离子的浓度。在本发明的一种实施方案中，纳米颗粒的第一与第二ζ-电位之差至少为约1.0mV，适宜地至少约5.0mV。
本发明纳米颗粒用能以离子键与诸如气体和有气味化合物等化合物结合的金属离子进行改性。“金属离子”是指在周期表上称作IB～VIIIB的过渡金属元素的盐离子和/或离子络合物。其他离子也可用于本发明中。金属离子由于电位不同而被吸附到高表面积材料上。带正电的金属离子被吸附到带负电的纳米颗粒表面，反之亦然。可用于本发明的金属离子的例子包括但不限于，铜离子(Cu+2)、银离子(Ag+1)、金离子(Au+1和Au+3)、铁(II)离子(Fe+2)、铁(III)离子(Fe+3)、高锰酸根离子(MnO4 -1)，以及它们的组合。
在本发明的一种实施方案中，可用于本发明的纳米颗粒具有负ζ-电位，因此吸附带正电的金属离子。一种合适的纳米颗粒具有约-1～-50mV，适宜地约-1～-20mV的负ζ-电位。在本发明的一种实施方案中，具有负ζ-电位的纳米颗粒是二氧化硅纳米颗粒。可用于本发明的二氧化硅纳米颗粒可从日产化学工业公司(休斯敦，德克萨斯)以商品名
Figure C03809342D00081
获得，具有1～100nm的颗粒尺寸。该二氧化硅纳米颗粒可用带正电的金属离子如铜离子、银离子、金离子、铁离子及其组合加以改性。
在本发明的另一种实施方案中，可用于本发明的纳米颗粒具有正ζ-电位，因此吸附带负电的金属离子络合物。一种合适的纳米颗粒具有约1～70mV，适宜地约10～40mV的正第一ζ-电位。在本发明的一种实施方案中，具有正ζ-电位的纳米颗粒是氧化铝纳米颗粒。氧化铝纳米颗粒也可从日产化学工业公司(休斯敦，德克萨斯)以商品名获得，具有约1～300nm的尺寸。氧化铝纳米颗粒能吸附带负电的金属离子和金属离子络合物，例如高锰酸根离子。
目前的气味控制材料，如活性炭或碳酸氢钠，依靠表面积来吸收某些气味。采用这些材料在脱除气味上不如本发明的改性高表面积材料有效。吸附到纳米颗粒表面上的金属离子的加入，正如本发明这样，提供一种俘获和中和气体和有气味化合物的活性部位。另外，本发明改性纳米颗粒还具有在吸收其他有气味化合物方面有用的大表面积。改性纳米颗粒的金属离子活性部位对于脱除诸如硫醇、氨、胺和单-和二-硫化物之类的有气味化合物特别有用。其他有气味化合物如脂族酮、羧酸、脂族醛和脂族萜类化合物，则可通过吸附到该改性纳米颗粒的大表面积上来脱除。改性纳米颗粒可用于脱除由硫化物、二硫化物、三硫化物、硫醇、硫醇、氨、胺、异戊酸、乙酸、丙酸、己醛、庚醛、2-丁酮、2-戊酮、4-庚酮及其组合所造成的气味。改性纳米颗粒还可除掉诸如乙烯气、香芹酮、二烯醛(dienals)和萜类化合物之类的气体。
可在纳米颗粒上涂布一种类型以上的金属离子。这样做的优点在于，某些金属离子可能在脱除特定气体和/或有气味化合物方面比其他金属离子好。在本发明的一种实施方案中，一种类型以上的金属离子被吸附到纳米颗粒上，以便从介质中更有效除掉一种类型以上气态化合物或有气味化合物。在本发明的一种实施方案中，一种类型以上的金属离子被吸附到纳米颗粒上，以便从介质中除掉至少一种气态化合物和至少一种有气味化合物。
本发明改性纳米颗粒可与其他改性纳米颗粒组合使用，以便有效地去除各种气体和气味。在本发明一种实施方案中，铜离子改性二氧化硅纳米颗粒与高锰酸根离子改性氧化镁纳米颗粒组合使用。通过两种不同改性纳米颗粒的组合使用，可除掉多种有气味化合物。例如，改性二氧化硅纳米颗粒可用于除掉硫和胺臭味，而改性氧化镁纳米颗粒则对于羧酸气味的去除有用。本发明改性纳米颗粒的组合使用能够除掉范围更宽的气味。
改性纳米颗粒是通过纳米颗粒与含金属离子的溶液彼此混合制造的。此种溶液的制备方法通常是，将金属化合物溶解在溶剂中从而在溶液中生成游离金属离子。金属离子，由于电位差，被吸引和吸附到纳米颗粒上。纳米颗粒ζ-电位按照本发明在吸附金属离子以后将发生改变。于是，可用ζ-电位来监测纳米颗粒吸附金属离子的进程。
本发明改性高表面积材料可多变，可单独使用也可与其他制品组合使用以便有效地去除和控制气味。不像活性炭除臭剂，本发明改性纳米颗粒在溶液中能保持其气味中和作用。本发明改性纳米颗粒当处于干态或气溶胶形式时仍维持其气味中和性能。此种灵活性使其能用于各种市售产品中。该改性纳米颗粒的其他优点是，它们在溶液中无色，处于粉末形式时呈白色(活性炭通常是黑色)。本发明改性高表面积材料还可与其他现有市售供应的脱除气味材料组合使用。
本发明改性纳米颗粒可施加到各种材料上。在本发明的一种实施方案中，改性纳米颗粒借助改性纳米颗粒(ζ-电位)与材料表面(泳动电势)之间的电位差而保持在材料的表面上。
本发明改性纳米颗粒可以溶液形式施涂到表面上，并在干燥后形成吸收气体和/或气味的表面。在本发明一种实施方案中，改性纳米颗粒被用于空气过滤器，例如，家用过滤器、放空过滤器、一次性面罩和面罩过滤器。在另一种实施方案中，改性纳米颗粒可施加到墙壁、壁纸、玻璃、马桶和/或柜台上。例如，改性纳米颗粒可用于休息室设备。其他用途包括但不限于，冰箱垫和织物柔软剂片材。
在本发明的一种实施方案中，改性纳米颗粒被施加到纤维布料上。各种类型纤维布料都可用于本发明中，包括但不限于，由天然纤维如木浆纤维、棉纤维或其他植物纤维制成的布料，以及非织造纤网，包括纺粘纤网、熔喷纤维、梳理纤维纤网、气流铺网纤网等，由热塑性材料如聚烯烃(例如，聚乙烯和聚丙烯均聚物和共聚物)、聚酯、聚胺等制成。改性纳米颗粒可涂布在各种类型织物、薄膜或纤维上。改性纳米颗粒的涂布量，根据需要可多可少。合适的是，改性纳米颗粒在织物、薄膜或纤维上的涂布量介于约0.001～10.0g/m2，更合适约0.1g/m2。
在本发明另一种实施方案中，改性纳米颗粒用来吸收植物所产生、使水果成熟的气体。乙烯气由植物产生，作为一种荷尔蒙以促使水果成熟。通过随着乙烯气的产生而不断除掉它，水果成熟过程可得到延缓和控制。高锰酸根离子改性的氧化铝纳米颗粒可用于脱除乙烯气。在一种实施方案中，高锰酸根离子改性的氧化铝纳米颗粒被吸附到纺粘聚丙烯布上。该布料具有负值泳动电势，因此带正电的纳米颗粒被牢固地保持在纤维表面。随后，该布料可用于包装和贮存水果如香蕉，通过除掉乙烯气来抑制其成熟。该布料可用来包裹水果，制成袋子装水果，或者可将小块布料装在目前的包装中。改性纳米颗粒还可喷涂到运输和贮存水果用的箱子或其他包装材料上。在一种实施方案中，布料因高锰酸根离子的缘故具有红紫色，而当布料被乙烯饱和时布料将变成褐色。此种颜色的变化可起到提示需要更换布料的指示剂作用。
本发明的改性纳米颗粒可用于从诸如水和尿等溶液中除掉有气味化合物。改性纳米颗粒可施加到用于从井水中除掉硫化合物用的水处理系统中，或施加在马桶槽中以减少尿产生的臭味。本发明改性纳米颗粒能够如此有效地除掉尿中令人厌恶的成分，以致经常存在于尿中的黄颜色也被中和，剩下澄清的液体。本发明的改性纳米颗粒还可用于液体洗涤剂和家用清洁剂中以脱除气味。
在本发明的一种实施方案中，该改性纳米颗粒被施涂到吸收制品上。术语“吸收制品”包括但不限于，尿布、训练裤、泳装、吸收性内裤、婴儿抹布、成人失禁用品、女性卫生用品、吸收性薄纸、医用服装、衬垫、绷带、吸收性幕帘和医用抹布，以及工业工作服。在一种实施方案中，改性纳米颗粒可加入到此种产品的吸收材料中。在另一种实施方案中，改性纳米颗粒可作为涂层涂布到任何布料或薄膜层上，例如，尿布的内衬或外包覆层上。在一种实施方案中，改性纳米颗粒可作为涂层涂布到吸收制品如尿布或失禁用品的外包覆层的透气性薄膜上以吸收臭味。改性纳米颗粒还可施涂到纸巾和湿抹布上，用于清除有气味的液体。吸收制品吸收有气味的液体，而改性纳米颗粒则从液体中结合有气味化合物，从而中和气味。
在本发明另一种实施方案中，纳米颗粒可用做气溶胶气味中和剂/脱除气味剂。改性纳米颗粒与喷射剂包装在一起，喷射剂能够将改性纳米颗粒喷雾到空气中以除掉气体和有气味化合物。改性纳米颗粒可用于家用空气清新剂或与从蒸发器或加湿器喷出的细雾组合使用。
改性纳米颗粒可用于口腔护理。硫和胺化合物经常是口臭的原因。改性纳米颗粒可加入到口腔护理产品如漱口剂、口腔护理口香糖、牙膏和/或牙刷丝中。采用铜离子改性的二氧化硅纳米颗粒是一种用于口腔护理的如此改性的纳米颗粒。二氧化硅广泛用于牙膏中作为磨料，而改性纳米颗粒通常含有少量铜离子，其含量远低于多种维生素片剂中的含量。不必担心此种改性纳米颗粒的应用会带来健康问题。
改性纳米颗粒还可用作呼吸指示剂。改性纳米颗粒可用作在有气味化合物存在下的颜色指示剂。在本发明的一种实施方案中，涂布铜离子改性的二氧化硅纳米颗粒的纤维素抹布放入到麦管之类的塑料管中。当使用者呼气进入到吸管中时，纤维素抹布从绿色变成蓝色，指出诸如氨蒸汽或硫化合物之类的气味。变色甚至可在少量有气味化合物存在的情况下发生。
实例1
一种改性二氧化硅纳米颗粒的稀悬浮体，通过把1mL SNOWTEXC
Figure C03809342D0011113109QIETU
，日产化学工业公司(休斯敦，德克萨斯)出品，加入到9mL去离子水中而制成。将该悬浮体按等份数用吸移管加入到4个比色杯中。制备各自为0.01wt％氯化铜(CuCl2)、硝酸银(AgNO3)和氯化锌(ZnCl2)，全部由Aldrich化学公司(Milwaukee，威斯康星)供应，的溶液，并将所得每种溶液各一滴分别加到单独的比色杯中。然后，用Zetapals装置，Brookhaven仪器公司(Holtsville，纽约)制造，测定所有4种悬浮体的ζ-电位。SNOWTEX C对照悬浮体的ζ-电位经测定为-25mV。SNOWTEX C/氯化铜悬浮体和SNOWTEX C/硝酸银悬浮体的ζ-电位据测定都是-11mV。SNOWTEX C/氯化锌悬浮体的ζ-电位据测定为-8mV。各种溶液之间在ζ-电位上的差别是金属离子已被吸收到二氧化硅纳米颗粒上的证据。
为试验改性二氧化硅纳米颗粒的脱除气味性能，制备了糠基硫醇溶液。在蒸馏水中配制一种0.001wt％糠基硫醇溶液(Aldrich化学公司(Milwaukee，威斯康星)供应)储备溶液。该溶液具有强烈气味。采用高效液相色谱法(HPLC)测定浓度变化。采用一种Zorbax EclipseXDB-C18，4.6 x 150mm，5μm柱和100％乙腈洗脱液。1μL糠基硫醇溶液注入到HPLC柱中，流率0.25mL/min。图2A，所产生的HPLC色谱图，显示糠基硫醇峰值具有16918毫吸收单位·秒(milliabsorptionunits·seconds(maus))的面积。
随后将一滴SNOWTEX C/铜离子悬浮体加入到10mL糠基硫醇溶液中。糠基硫醇的气味迅速消失，然后以0.25mL/min的流率将1μL此种糠基硫醇溶液注入到HPLC柱中。图2B，产生的HPLC色谱图，显示糠基硫醇峰值具有188毫吸收单位·秒(maus)的面积。随着改性纳米颗粒的加入，糠基硫醇的浓度以及可检测到的气味都有了大幅度下降。
实例2
将SNOWTEX C/铜离子悬浮体试用在人尿上，以确定气味减少的有效性。如实例1所述，HPLC被用来测定尿(从本发明人取得)的成分。一滴来自实例1的SNOWTEX C/铜离子悬浮体与0.1g Purite MicronetMN-150胶乳颗粒，Purolite公司(费城，宾夕法尼亚)供应，和0.1g活性炭，Aldrich化学公司(Milwaukee，威斯康星)供应，对比着进行试验。上述的每一种分别加入单独的3g尿中。加入SNOWTEX C/铜离子悬浮体的样品的尿气味在3～5s后几乎完全消失，相比之下活性炭却需要约10min。胶乳颗粒则根本不能脱除气味。图3A显示尿样的HPLC色谱图，图3B显示加入改性二氧化硅纳米颗粒以后尿样的色谱图。表1总括4种样品的HPLC峰值比较。改性二氧化硅纳米颗粒在去除尿成分上的表现大大好于目前的市售材料。
表1-尿成分HPLC峰(峰值保留时间(min))。
 
样品 峰面积，3.87min。 峰面积，4.04min。 峰面积，4.77min。 峰面积，5.64min。 峰面积，5.88min。 峰面积，6.23min。
尿 924maus 345maus 50maus 17maus 829maus 228maus
尿+改性二氧化硅纳米颗粒        0 0 12maus 0 701maus 2maus
尿+Purite胶乳颗粒  773maus 300maus 0maus 17maus 820maus 156maus
尿+活性炭 900maus 0 50maus 17maus 820maus 10maus
实例3
当干态和涂布在表面时，改性纳米颗粒的脱除气味性能，通过在10.16cm2单层HI-
Figure C03809342D00131
纸巾，Kimberly-Clark公司(Neenah，威斯康星)供应，上涂以实例1的进一步稀释50％的SNOWTEX C/铜离子悬浮体进行试验。纸巾是通过将纸巾样品浸渍在悬浮体中进行涂布的。湿纸巾放在玻璃板上风干。干燥纸巾放在100mL烧杯口上并用橡皮筋箍紧。烧杯装有20mL0.001wt％糠基硫醇溶液。第二种、未处理的对照HI-
Figure C03809342D00132
纸巾放在相同的烧杯上作为对照。来自糠基硫醇的气味透过了未处理的纸巾。然而，在约3h内，没有任何气味透过以改性纳米颗粒处理的纸巾。3h后，改性纳米颗粒达到饱和，于是可察觉出气味。处理过的纸巾，由于结合了糠基硫醇，致使在烧杯上显现深色区域。
实例4
通过用实例1铜改性的二氧化硅纳米颗粒处理Home Depot生产的标准浴室砖(15cm x 15cm)，对改性纳米颗粒作为浴室砖上的不可见涂层的脱除气味性能进行试验。将铜改性二氧化硅纳米颗粒的悬浮体施涂到KIM-
Figure C03809342D00133
(抹布)上。采用该打湿的KIM-擦拭浴室砖表面，然后用第二块干KIM-
Figure C03809342D00135
揩去任何多余的液体。将3.6μL氨、28％氨水，Aldrich化学公司(Milwaukee，威斯康星)供应，通过针筒引入到实验室干燥器中，10min后，采集等分数量空气/气味样品并进行分析以确定干燥器内的氨浓度。该实验重复3次；一次是没有砖在干燥器中，一次用未处理的对照砖放在干燥器中，一次是将改性纳米颗粒处理的砖放在干燥器中。氨气是采用Drager管，SKC公司(宾夕法尼亚)出品，测定的，它能测定在空气中2～30ppm的氨浓度。将60mL空气/气味利用针筒抽出干燥器。Drager管由Tygon软管连接在干燥器和针筒之间。干燥器内的氨浓度，在没有砖和放入未处理的砖时测得20ppm。当放入用改性纳米颗粒处理的砖时，干燥器内的氨浓度测得为2ppm以下。改性纳米颗粒在标准浴室砖上能有效地大大减少氨气和气味。
实例5
下面的实验旨在展示本发明改性纳米颗粒在延长水果贮存时间方面的应用。高锰酸盐改性的氧化铝纳米颗粒按照0.01％改性纳米颗粒重量/布料重量的比例被吸附到一块5.0cm x 5.0cm 2盎司纺粘聚丙烯布上。高锰酸根离子的数量大约为0.0001％离子重量/纳米颗粒重量，通过测定纳米颗粒ζ-电位的变化加以监测。将3根来自同一束不带褐斑的黄色香蕉分别放入到气密袋中。在第一个气密袋中，放入改性纳米颗粒处理的布料。在第二个袋中装有未处理的5.0cm2纺粘聚丙烯布作为对照样。第三个袋子不装任何布料，也作为对照样。3个气密袋放在环境温度下贮存4周。4周结束时，2个对照袋中的香蕉完全变黑，摸上去软软的并且像烂泥样渗液体。装有改性纳米颗粒处理的布料的袋子中，香蕉摸上去坚挺，仅有少数几个褐斑。这证明，成熟过程被改性纳米颗粒延缓。
实例6
为展示本发明改性有机纳米颗粒的脱除气味性能，将铜离子吸附到聚苯乙烯纳米颗粒上。一种改性聚苯乙烯纳米颗粒的稀悬浮体，通过将1.0mL聚苯乙烯纳米颗粒悬浮体，其中纳米颗粒的颗粒直径是64nm，由Polysciences公司(Warrington，宾夕法尼亚)供应，加入到9.0mL去离子水中而制成。该聚苯乙烯纳米颗粒悬浮体的ζ-电位采用实例1的Zetapals装置测定，是-49mV。将2滴0.01wt％氯化铜(CuCl2)溶液加入到聚苯乙烯纳米颗粒悬浮体中。在加入2滴氯化铜溶液以后，聚苯乙烯溶液的ζ-电位经测定为-16mV，据此确认铜离子已吸附到了聚苯乙烯纳米颗粒上。将一滴改性纳米颗粒溶液加入到2.0mL0.001wt％糠基硫醇溶液中。采用实例1所述高效液相色谱法测定在加入改性纳米颗粒前、后糠基硫醇的存在。加入改性纳米颗粒前，糠基硫醇峰面积是193毫吸收单位(milliabsorption units)，加入改性纳米颗粒以后是14毫吸收单位。铜改性聚苯乙烯钠米颗粒在脱除含硫化合物方面是有效的。
实例7
一种改性二氧化硅纳米颗粒的稀悬浮体，通过将1mL SNOWTEX
Figure C03809342D00151
日产化学工业公司(休斯敦，德克萨斯)出品，加入到9mL去离子水中制成。将该悬浮体按等份数用吸移管加入到3个不同比色杯中。制备各自为0.01wt％氯化铜(CuCl2)、氯化亚铁(II)(PeCl2)和氯化铁(III)(FeCl3)，全部由Aldrich化学公司(Milwaukee，威斯康星)，的溶液，将所得每种溶液各一滴分别加到单独的比色杯中。然后，用Zetapals装置测定所有3种悬浮体的ζ-电位。SNOWTEX 
Figure C03809342D00152
对照悬浮体的ζ-电位经测定为-22mV。SNOWTEX C/氯化铜悬浮体的ζ-电位测得为-10mV，和SNOWTEX C/氯化亚铁(II)悬浮体的ζ-电位据测定为-13mV。SNOWTEX C/氯化铁(III)悬浮体的ζ-电位据测定为+13mV。将每种改性纳米颗粒溶液各一滴加入到单独的2.0mL 0.001wt％糠基硫醇溶液中。采用实例1所述高效液相色谱法测定在加入不同改性纳米颗粒前、后糠基硫醇的存在。结果载于表2。每种改性纳米颗粒都成功地从溶液中除掉了糠基硫醇。另外，铁(III)离子改性的二氧化硅纳米颗粒具有正ζ-电位，因此能够施涂到由诸如聚丙烯、聚乙烯、尼龙和棉之类的材料制成的具有负值泳动电势的布料上。
表2
 
样品 ζ-电位 糠基硫醇峰面积 脱除气味百分率
SNOWTEX C/Cu<sup>+2</sup> -10 3.2maus 97％
SNOWTEX C/Fe<sup>+2</sup> -13 38maus 67％
SNOWTEX C/Fe<sup>+3</sup> +13 3.4maus 97％
虽然这里所描述的本发明实施方案是目前优选的，但在不偏离本发明精神和范围条件下仍可制定出各种修改和改进方案。本发明范围由所附权利要求规定，所有改变，只要符合等价物含义和范围都应包括在本发明范围内。

Claims (21)

1、一种组合物，包含：
纳米颗粒；以及
至少一种吸附在纳米颗粒上的金属离子或金属离子络合物，所述最少一种金属离子或金属离子络合物选自铜离子、银离子、金离子、高锰酸根离子、铁离子及其组合，其中纳米颗粒和金属离子或金属离子络合物中的至少之一能结合至少一种选自气态化合物、有气味化合物及其组合的化合物，所述有气味化合物是选自含硫化合物、含氮化合物、羧酸、醇、脂族醛、脂族酮及其组合的化合物，所述气态化合物是选自乙烯气体、香芹酮、二烯醛、萜类化合物及其组合的化合物。
2、权利要求1的组合物，其中纳米颗粒具有正或负值ζ-电位。
3、权利要求2的组合物，其中在将至少一种金属离子吸附到纳米颗粒上之后，纳米颗粒具有第二更高或更低的ζ-电位。
4、权利要求2的组合物，其中纳米颗粒具有-1～-50mV的负值ζ-电位。
5、权利要求2的组合物，其中纳米颗粒具有负值ζ-电位并且选自二氧化硅、二氧化钛、金、氧化锌、聚苯乙烯及其组合。
6、权利要求5的组合物，其中金属离子选自铜离子、金离子及其组合。
7、权利要求2的组合物，其中纳米颗粒具有1～70mV的正值ζ-电位。
8、权利要求2的组合物，其中纳米颗粒具有正值ζ-电位并且选自氧化铝、氧化镁及其组合。
9、权利要求8的组合物，其中金属离子络合物选自高锰酸根离子。
10、一种用于去除气态化合物和有气味化合物的组合物，包含：
第一改性纳米颗粒，包含具有正值ζ-电位的纳米颗粒和至少一种吸附在第一改性纳米颗粒上的带负电金属离子络合物，所述金属离子络合物选自高锰酸根离子；以及
第二改性纳米颗粒，包含具有负值ζ-电位的纳米颗粒和至少一种吸附在第二改性纳米颗粒上的带正电金属离子，所述金属离子选自铜离子、银离子、金离子、铁离子及其组合；
其中第一改性纳米颗粒能结合第一气态化合物，第二纳米颗粒能结合第二气态化合物，其中第一气态化合物和第二气态化合物中的至少之一包含有气味化合物；
所述有气味化合物是选自含硫化合物、含氮化合物、羧酸、醇、脂族醛、脂族酮及其组合的化合物，所述气态化合物是选自乙烯气体、香芹酮、二烯醛、萜类化合物及其组合的化合物。
11、一种组合物，包含：
纳米颗粒；和
至少一种吸附在纳米颗粒上的金属离子或金属离子络合物，所述至少一种金属离子或金属离子络合物选自铜离子、银离子、金离子、高锰酸根离子、铁离子及其组合；
其中纳米颗粒在吸附金属离子或金属离子络合物之前具有第一ζ-电位，而在吸附后具有第二ζ-电位，第一ζ-电位与第二ζ-电位之差为1.0mV。
12、权利要求11的组合物，其中第二ζ-电位取决于被吸附的金属离子的加入量。
13、权利要求1、10或11的组合物，其中纳米颗粒具有至少200m2/g的表面积。
14、权利要求1、10或11的组合物，其中纳米颗粒选自二氧化硅、氧化铝、氧化镁、二氧化钛、氧化铁、金、氧化锌、氧化铜、聚苯乙烯及其组合。
15、权利要求1或11的组合物，其中至少一种金属离子或金属离子络合物选自铜离子、金离子、高锰酸根离子铁离子及其组合。
16、包括权利要求1、10或11的组合物的制品。
17、权利要求16的制品，其中该制品是吸收制品。
18、权利要求17的制品，其中该制品选自纸巾、气溶胶喷雾剂、家用清洁剂、口腔卫生产品、过滤制品、和透气性薄膜。
19、一种生产改性纳米颗粒的方法，包括：
让至少一种金属离子吸附到具有第一ζ-电位的纳米颗粒上；以及
通过纳米颗粒ζ-电位的改变来测定金属离子吸附。
20、权利要求19的方法，其中让金属离子吸附的步骤包括将金属离子溶液滴加到纳米颗粒水悬浮体中。
21、权利要求19的方法，还包括将纳米颗粒的ζ-电位改变至少1.0mV。
CNB038093421A 2002-04-30 2003-03-04 气味脱除和控制用金属离子改性高表面积材料 Expired - Fee Related CN100537020C (zh)

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US20120202684A1 (en) 2012-08-09
US7578997B2 (en) 2009-08-25
MXPA04010105A (es) 2004-12-13
US8182800B2 (en) 2012-05-22
US8771661B2 (en) 2014-07-08
KR20040104567A (ko) 2004-12-10
MX263926B (zh) 2009-01-20
EP1503853B1 (en) 2007-04-18
KR100972890B1 (ko) 2010-07-28
US20030203009A1 (en) 2003-10-30
WO2003092885A1 (en) 2003-11-13
ATE359865T1 (de) 2007-05-15
BR0309282A (pt) 2005-02-09
EP1775018A1 (en) 2007-04-18
US20090318287A1 (en) 2009-12-24
DE60313315T2 (de) 2007-08-30
CN1649666A (zh) 2005-08-03
BRPI0309282B1 (pt) 2016-06-21
DE60313315D1 (de) 2007-05-31
AU2003220010B2 (en) 2008-06-26
CA2482788A1 (en) 2003-11-13

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