CN104619411A - 乙烯去除剂 - Google Patents
乙烯去除剂 Download PDFInfo
- Publication number
- CN104619411A CN104619411A CN201280063018.5A CN201280063018A CN104619411A CN 104619411 A CN104619411 A CN 104619411A CN 201280063018 A CN201280063018 A CN 201280063018A CN 104619411 A CN104619411 A CN 104619411A
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- CN
- China
- Prior art keywords
- particle
- compound particle
- fluoridizing
- compound
- golden nanometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 83
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 9
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- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
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- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/144—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor
- A23B7/152—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor in a controlled atmosphere comprising other gases in addition to CO2, N2, O2 or H2O ; Elimination of such other gases
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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Abstract
本发明涉及一种复合粒子、包含此类粒子的制品以及使用所述粒子和所述制品去除乙烯的方法,所述复合粒子包含氟化的表面和设置在所述氟化的表面上的金纳米粒子的不连续层。
Description
背景技术
乙烯去除是用于水果和花卉收获后运输与储藏期间保鲜的主要方法之一。乙烯的去除通常通过诸如活性炭或沸石材料的吸附剂,或通过化学计量的氧化剂(例如,高锰酸钾),或通过高温下的催化氧化剂,或甚至通过化学计量的环加成反应(例如,乙烯与四嗪化合物的狄尔斯–阿尔德反应(Diels-Alder reaction))实现。
发明内容
在一个方面,本公开描述一种复合粒子,其包含:氟化的表面;和设置在所述氟化的表面上的金纳米粒子的不连续层。
在另一方面,本公开描述一种制品,其包含:基底;设置在所述基底的表面上、设置在基底内或两者的多个复合粒子;其中所述多个复合粒子中的各个复合粒子包含:氟化的表面;和设置在所述氟化的表面上的金纳米粒子的不连续层。
在另一方面,本公开描述一种制品,其包含:容器;设置在容器内的多个复合粒子;其中所述多个复合粒子中的各个复合粒子包含:氟化的表面;和设置在氟化的表面上的金纳米粒子的不连续层。
在另一方面,本公开描述一种去除乙烯的方法,该方法包括:将乙烯去除剂置于乙烯生成源的附近,其中所述乙烯去除剂包含:多个复合粒子,其中所述多个复合粒子中的各个复合粒子包含:氟化的表面;和设置在所述氟化的表面上的金纳米粒子的不连续层。
在考虑具体实施方式以及所附权利要求书之后,将进一步理解本公开的特征和优点。
附图说明
图1是用于执行将金沉积到粒子上的物理气相沉积(PVD)工艺的设备的示意性侧视图。
图2是图1的设备的示意性透视图。
具体实施方式
在本说明书的实施例中,复合粒子包含设置在氟化的表面上的金纳米粒子的不连续层。我们已观察到,本说明书的复合粒子可用于去除由乙烯生成源生成的乙烯(即,作为乙烯去除剂)。去除由乙烯生成源生成的乙烯的复合粒子可用于例如收获的水果、收获的蔬菜和收获的花卉的保鲜。
在一些实施例中,本公开的复合粒子具有在0.1微米至10000微米的范围内(在一些实施例中,0.1微米至1000微米,0.1微米至100微米,0.1微米至10微米,或甚至0.1微米至1微米;在一些实施例中,100微米至10000微米,500微米至5000微米,或甚至500微米至2000微米;在一些实施例中,3微米至1000微米,或甚至5微米至约500微米)的粒度。粒度通常为多个复合粒子的平均粒度;对于非球形粒子,粒度为粒子的最大尺寸。
在一些实施例中,本公开的复合粒子具有至多1:10000(在一些实施例中,至多1:1000,至多1:100,至多1:10,至多1:5,至多1:2,以及甚至至多1:1)的纵横比。纵横比是指平均粒子宽度与平均粒子长度的比率(即,最短粒子尺寸与最长粒子尺寸的比率)。
本说明书的氟化的表面可包含高度氟化的材料。“高度氟化的”意指氟的含量为40重量%或更高(在一些实施例中,50重量%或更高、60重量%或更高、70重量%或更高、80重量%或更高、90重量%或更高,或甚至95重量%或更高)。在一些实施例中,氟化的表面包含全氟化材料。合适的全氟化的材料的例子为聚四氟乙烯(“PTFE”)。其他合适的高度氟化的和全氟化的材料包括但不限于部分或完全氟化的聚硅氧烷、聚(丙烯酸酯)、聚甲基丙烯酸酯和聚苯乙烯。
众所周知,金是一种淡黄色、相对惰性的贵金属。然而,金的特性在纳米级(即,小于100纳米)尺度上可以发生显著变化(特别是在纳米级尺度的下端;例如,在特征在于至少一个尺度小于约10纳米(“nm”)的尺寸范围上),此时金可以成为催化活性物质。
在本说明书的实施例中,将金纳米粒子的不连续层设置在氟化的表面上。“不连续”是指将金纳米粒子布置在氟化的表面上的“岛状区域”中。通常,将金纳米粒子以不连续层布置在复合粒子的氟化的表面上产生不导电的复合粒子。如本文所用的“不导电”是指复合粒子具有一定的粉末体积电阻率值(如实例章节中所述而测定),其中该粉末体积电阻率值为至少1×106Ω·cm。
构成不连续层的金纳米粒子的“岛状区域”的所有尺度(例如,纳米粒子直径或原子簇直径)的平均尺寸可在至多(即,小于或等于)5nm的范围内(在一些实施例在,平均尺寸至多4nm,平均尺寸至多3nm,或甚至平均尺寸至多2nm)。在一些实施例中,金纳米粒子的岛状区域在至少一个尺度上为至少0.1nm(在一些实施例中,在至少一个尺度上为至少0.5nm),并且不大于上述上限。该细纳米级金进一步例如在美国已公布的专利申请No.2009/0054230(Badri等人)中有所描述。
在本说明书的实施例中,使用物理气相沉积将金纳米粒子的不连续层沉积在氟化的表面上。物理气相沉积(“PVD”)是指将金从含金源或目标物理转移到基底的表面。PVD可视为涉及一个原子接一个原子地沉积,但在实际的实施过程中,金也可以作为极其细小的团粒进行转移,每个团粒由不止一个原子构成。一旦到达氟化的表面,金就可以与表面发生物理形式的、化学形式的或离子形式的相互作用。进行PVD以在基底表面上沉积金纳米粒子的方法进一步在例如美国专利No.8,058,202(Brady等人)和美国已公布的专利申请No.2009/0054230(Veeraraghavan等人)中有所描述。
在氟化的表面上提供的金的量可在大范围内变化。然而,由于金是昂贵的,为了获得所需程度的乙烯去除活性,使用不超过合理需要的金是理想的。另外,由于纳米级金在使用PVD进行沉积时是高度流动的,因此如果使用过多的金则乙烯去除活性可能受损,原因是至少一些金聚结成较大的团粒,继而例如可降低金的催化活性。
在本公开的复合粒子的一些实施例中,金纳米粒子的不连续层相对于复合粒子在0.05重量%至5重量%的范围内(在一些实施例中,在0.05重量%至4重量%、0.05重量%至3重量%、0.05重量%至2重量%、0.05重量%至1重量%、0.1重量%至5重量%或甚至0.1至1重量%的范围内)。
在本公开的PVD处理的典型实施例中,PVD处理在多个复合粒子的粉末体积电阻率变得低于1×106Ω·cm时中止,然后分离所述多个复合粒子。不受理论的约束,据认为,金纳米粒子的非导电层因为在非导电层中的金纳米粒子之中的低接触程度而为非导电的。使用PVD处理形成本说明书的复合粒子的方法的示例性实施例包括在实例章节中,其中观察到粉末体积电阻率不大于2×106Ω·cm。
在一些实施例中,氟化的表面为芯粒子上的氟化的涂层。芯粒子可以为宽泛的合适材料范围中的任一种。在一些实施例中,芯粒子可包含含碳材料、沸石或金属氧化物中的任一种。
适于本公开的芯粒子的含碳材料的例子包括源于椰子的热解碳、煤基碳和炭黑中的任一者。可用于本公开的芯粒子的含碳材料的典型例子包括石墨和活性炭或其组合中的任一者,包括可以商品名“KURARAY GG12×20”购自日本大阪的可乐丽化工株式会社(KurarayChemical Company,Osaka,Japan)的粒状活性炭(12×20目,即粒度在约0.8mm至约1.7mm的范围内)。
已证实,金可通过PVD技术(例如,通过溅射)沉积以在纳米粒子芯粒子表面上形成催化活性、细纳米级粒子或原子簇(参见例如Brady等人的美国专利No.8,058,202)。不受理论的约束,通常认为,存在3种可能的薄膜成核和生长机理模式(有关不同的膜生长机理模式的描述,参见例如“Nucleation and Growth of Thin Films”,Reports onProgress in Physics,1984,Vol.47,issue4,pp.399-459(“薄膜的成核和生长”,《物理学进展报告》,1984年,第47卷,第4期,第399-459页))。通过按一层接一层生长而沉积膜从而均匀覆盖基底称为层状生长模式(Frank-Van der Merwe growth mode)。通过岛的成核和凝聚促进的沉积称为岛状生长模式(Volmer-Weber growth mode)。第三种模式即混合生长模式(Stranski-Krastinov mode)描述前两种模式的组合。在低表面能材料(例如,本公开的高度氟化的或全氟化的材料)上的PVD沉积可促进在复合粒子的氟化的表面上的Volmer-Weber型岛状生长模式。
对于一些含碳材料,可能需要将包含一种或多种组分的活化剂结合到所需的载体中。这种结合可以按任意所需的方式发生。始润浸渍是一种合适的技术。始润浸渍可涉及在混合下将包含所需活化剂的溶液缓慢添加到干燥的载体介质。如果要添加不止一种活化剂物质,则它们可以一起或单独地添加,或者按交错的方式添加。浸渍之后,可以干燥载体介质并任选进行煅烧(热处理)。可用的浸渍剂的例子包括一种或多种金属、金属合金、金属间组合物和/或包含Cu、Zn、Mo、Ag、Ni、V、W、Y、Co等中的一种或多种的化合物,以及它们的组合。金属通常可以作为盐浸渍,并且在一些模式的浸渍过程中可以将其转化成其他形式(如氧化物)。
选择将哪一种或哪几种过渡金属化合物结合到芯粒子中可取决于所需的特性范围。例如,当与Cu浸渍剂联合使用时,Mo、V和Y或W可独立地协助去除空气流中诸如氯化氰和氰化氢的气体。
浸渍剂可根据常规实践结合到含碳材料中。通常可以按盐、氧化物、碳酸盐等形式提供这些浸渍剂,并且可以通过溶液处理、升华处理、流化床处理等实施浸渍。优选的是,这种浸渍发生在金沉积之前。根据浸渍剂的性质、载体的性质以及所需的特性,浸渍剂的用量可以有很大的不同(例如,基于含碳材料的总重量计为约0.01重量%至约20重量%)。
用于本公开的芯粒子的沸石材料的合适例子包括沸石3A、沸石4A、沸石5A、沸石13X或沸石13Y中的任一种。
用于本公开的芯粒子的金属氧化物材料的合适例子包括二氧化钛、氧化铝、二氧化硅或其组合中的任一种。
在包含芯粒子的复合粒子的实施例中,通常通过在芯粒子的外表面的至少一部分上形成氟化的涂层而提供氟化的表面。用于提供氟化的涂层的典型方法包括以下任一种:芯粒子表面的等离子体氟化、将氟化聚合物等离子体聚合到芯粒子表面上、芯粒子表面的气相氟化、芯粒子与氟化的介质的干混、用氟化的介质喷涂芯粒子,或将芯粒子浸入/浸涂到含有氟化剂或氟化的介质的溶液中。芯粒子还可以在整个材料主体中包含氟组分,如以无机氟化物的形式,包括但不限于碱金属氟化物、碱土金属氟化物和过渡金属氟化物。芯粒子的其他例子包括使用至少一种氟化单体制备的含氟聚合物。
芯粒子可具有微孔、中孔、大孔范围内或任何这些范围的组合的孔隙度。氟化的涂层可存在于芯粒子的外表面上,但也可以至少部分地存在于芯粒子的一些内部孔表面内。金纳米粒子还可以存在于氟化的涂层和/或芯粒子的内外两个表面上。
在一些实施例中,芯粒子适用于从周围环境中去除水分。水分可以为周围空气中的湿度的形式。芯粒子可具有从周围空气中吸收水分的能力。
在一些实施例中,芯粒子是挥发性有机化合物的吸附剂。挥发性有机化合物的例子可包括挥发性胺和挥发性有机硫化物,其中许多可带有强烈气味(odiferous)。
在制备复合粒子的方法的一个实施例中,提供具有氟化的表面的芯粒子,并且使用PVD在氟化的表面上沉积金纳米粒子,以在氟化的表面上提供金纳米粒子的不连续层;在粉末体积电阻率值变为低于1×106Ω·cm前中止PVD处理,然后分离在氟化的表面上具有金纳米粒子的不连续层的复合粒子。
物理气相沉积优选发生在金具有相当的移动性并倾向于在载体介质的表面上迁移直到以某种方式(例如通过粘附于载体表面上的或非常接近载体表面的位点)被固定的温度和真空条件下。粘附位点可以包含缺陷(如表面空位)、结构间断(如台阶和位错)以及相或晶体或其他金物质(如小金簇)之间的界面边界。
可以按多种不同方式进行物理气相沉积。代表性的方法包括溅射沉积(优选的)、蒸发和阴极电弧沉积。虽然PVD技术的性质可影响所得的纳米金的活性,但是本发明的处理中可以采用这些或其他PVD方法中的任一种。
例如,物理气相沉积技术的能量能影响到沉积的金的移动性,并因此影响到其聚结的倾向。较高的能量倾向于对应较高的金聚结倾向。增加的聚结继而倾向于在将材料用作纳米金催化剂时降低催化活性。一般来说,由蒸发沉积物质的能量最低,更高的是溅射沉积(其可以包含一些离子含量,其中碰撞金属物质中的一小部分被离子化),而最高的是阴极电弧沉积(其可以包含数十个百分比的离子含量)。因此,如果某种PVD技术产生的沉积金的移动性超出所需,则适用的可以是采用能量较少的PVD技术代替之。
为了确保载体表面受到足够的处理,优选在充分混合(例如,翻滚、流化或研磨)待处理的载体介质的同时进行物理气相沉积。粒子在PVD期间在真空室中翻滚例如在美国专利No.4,618,525(Chamberlain等人)中有所描述。
在本公开的方法的一些实施例中,将乙烯去除剂置于乙烯生成源的附近。乙烯去除剂包含本公开的多个复合粒子(即,多个在复合粒子的氟化的表面上设有金纳米粒子的不连续层的任何复合粒子)。
“附近”是指与乙烯生成源足够近,以允许乙烯生成源中的乙烯到达乙烯去除剂。在一些典型的实施例中,将乙烯去除剂置于乙烯生成源的10米内(在一些实施例中,5米内、2米内、1米内、10cm内、5cm内、2cm内或甚至1cm内)。在一些实施例中,将乙烯去除剂直接靠着乙烯生成源放置。
在一些实施例中,将乙烯去除剂与乙烯生成源一起置于封闭系统中。“封闭系统”是指正常封闭的容器或多个互连的容器中的任一种,其中乙烯气体可从乙烯生成源移动到乙烯去除剂。在一些实施例中,封闭系统包括用于增强气体从乙烯生成源流动到乙烯去除剂的装置。
在一些实施例中,用于增强气体从乙烯生成源流动到乙烯去除剂的装置通常包括风扇、泵或任何其他增强气体除扩散以外的流动的装置中的任一种。在一些实施例中,气体流动可通过温差增强。
在一些实施例中,乙烯生成源为收获的水果、收获的蔬菜或收获的花卉中的任一种。
本公开的乙烯去除剂可结合到可用于去除由乙烯生成源生成的乙烯气体的宽泛的制品范围中。在一些实施例中,本公开的制品包括基底,该基底具有多个设置在基底表面上、设置在基底内或两者的本说明书的任何复合粒子。可以使用宽泛的基底范围。许多类型的材料均适合用作基底,包括聚合物材料、陶瓷材料、金属材料以及任何这些材料或所有这些材料的复合物。在一些实施例中,基底为片材、膜、非织造幅材或多个粒子中任一种的形式。在一些实施例中,基底包含过滤介质。
在一些实施例中,本公开的制品包括容器,该容器具有设置在容器内的本说明书的乙烯去除剂。在一些实施例中,容器可以为渗透性袋、限定入口和出口的管或非织造纤维幅材中的任一种。对容器进行选择以允许气体流向乙烯去除剂或从乙烯去除剂流走。
渗透性袋的合适例子包括织造或非织造织物(例如,棉、尼龙或其组合)袋、闪纺高密度聚乙烯纤维(例如,得自特拉华州威尔明顿的杜邦公司(DuPont,Wilmington,DE)的“TYVEK”材料)聚合物渗透性袋以及由嵌入有粒子的聚乙烯或其他聚合物膜制成的渗透性袋。
在容器为限定入口和出口的管的制品中,可以使用任何合适的管尺寸或形状。通常,管包括过滤器或玻璃料以将乙烯去除剂保持在管内,同时允许气体从乙烯生成源流过管。
本公开的乙烯去除剂可用于例如制冷系统,特别是用于收获的水果、收获的蔬菜或收获的花卉的保鲜的制冷系统。
实施例
项1.一种复合粒子,包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
项2.根据项1所述的复合粒子,其中所述氟化的表面为芯粒子上的氟化的涂层。
项3.根据项2所述的复合粒子,其中所述芯粒子包含含碳材料、沸石或金属氧化物中的任一种。
项4.根据项2所述的复合粒子,其中所述芯粒子包含活性炭。
项5.根据前述项中任一项所述的复合粒子,其中所述复合粒子具有至多1:10000的纵横比。
项6.根据前述项中任一项所述的复合粒子,其中所述复合粒子具有在0.1微米至10000微米的范围内的粒度。
项7.根据前述项中任一项所述的复合粒子,其中所述氟化的表面包含聚四氟乙烯。
项8.根据前述项中任一项所述的复合粒子,其中所述芯粒子适用于去除水分。
项9.根据前述项中任一项所述的复合粒子,其中所述芯粒子为挥发性有机化合物的吸附剂。
项10.根据前述项中任一项所述的复合粒子,其中所述金纳米粒子的不连续层相对于所述复合粒子在0.05重量%至5重量%的范围内。
项11.根据前述项中任一项所述的复合粒子,其具有至少106Ω·cm的粉末体积电阻率值。
项12.一种制品,包含:
基底;
设置在所述基底的表面上、设置在所述基底内或两者的多个复合粒子;
其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
项13.根据项12所述的制品,其中所述基底为片材、膜、非织造幅材或多个粒子中的任何形式。
项14.一种制品,包含:
容器;
设置在所述容器内的多个复合粒子;
其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
项15.根据项14所述的制品,其中所述容器包括渗透性袋、限定入口和出口的管或非织造纤维幅材中的任一种。
项16.一种去除乙烯的方法,所述方法包括:
将乙烯去除剂置于乙烯生成源的附近,其中所述乙烯去除剂包含:
多个复合粒子,其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
项17.根据项16所述的方法,其中所述乙烯去除剂和所述乙烯生成源在封闭系统内。
项18.根据项17所述的方法,其中所述封闭系统包括用于增强气体从所述乙烯生成源流动到乙烯去除剂的装置。
项19.根据项16至18中任一项所述的方法,其中所述乙烯生成源为收获的水果、收获的蔬菜或收获的花卉中的任一种。
项20.一种制冷系统,包含项1至11中任一者所述的复合粒子。
项21.一种制备复合粒子的方法,所述方法包括:
提供具有氟化的表面的芯粒子;
将金纳米粒子沉积在所述氟化的表面上,以在所述氟化的表面上提供金纳米粒子的不连续层;以及
分离在所述氟化的表面上设有所述金纳米粒子的不连续层的芯粒子。
项22.根据项21所述的方法,其中沉积金纳米粒子包括粒子气相沉积。
项23.根据项21至22中任一项所述的方法,其中沉积金纳米粒子在所述多个复合粒子的粉末体积电阻率值为至少106Ω·cm时中止。
项24.一种复合粒子,包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的非导电层。
项25.根据项24所述的复合粒子,其中所述氟化的表面为芯粒子上的氟化的涂层。
项26.根据项25所述的复合粒子,其中所述芯粒子包含含碳材料、沸石或金属氧化物中的任一种。
项27.根据项25所述的复合粒子,其中所述芯粒子包含活性炭。
项28.根据项24至27中任一项所述的复合粒子,其中所述复合粒子具有至多1:10000的纵横比。
项29.根据项24至28中任一项所述的复合粒子,其中所述复合粒子具有在0.1微米至10000微米的范围内的粒度。
项30.根据项24至29中任一项所述的复合粒子,其中所述氟化的表面包含聚四氟乙烯。
项31.根据项24至30中任一项所述的复合粒子,其中所述芯粒子适用于去除水分。
项32.根据项24至31中任一项所述的复合粒子,其中芯粒子为挥发性有机化合物的吸附剂。
项33.根据项24至32中任一项所述的复合粒子,其中所述金纳米粒子的非导电层相对于所述复合粒子在0.05重量%至5重量%的范围内。
项34.根据项24至33中任一项所述的复合粒子,其具有至少106Ω·cm的粉末体积电阻率值。
项35.一种去除乙烯的方法,所述方法包括:
将乙烯去除剂置于乙烯生成源的附近,其中所述乙烯去除剂包含:
多个复合粒子,其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的非导电层。
项36.根据项35所述的方法,其中所述乙烯去除剂和所述乙烯生成源在封闭系统内。
项37.根据项36所述的方法,其中所述封闭系统包括用于增强气体从所述乙烯生成源流动到乙烯去除剂的装置。
通过以下非限制性实例进一步说明本公开的目的和优点,但这些实例中所引用的具体材料及其用量,以及其他条件和细节不应视为对本公开进行不当限定。
实例
除非另外指明,否则在实例及本说明书的其余部分中的所有份数、百分数、比率等均为以重量计。
粒子气相沉积(PVD)设备
用于执行PVD处理的示例性实施例的设备10在图1和图2中示出。设备10包括限定真空室14的外壳12,真空室14包括粒子搅拌器16。外壳12是垂直取向的中空圆柱体(高为45cm,直径为50cm)。基座18限定用于高真空闸门阀22(其后接六英寸(15cm)扩散泵24)的端口20以及用于粒子搅拌器16的支承体26。真空室14能够被抽空到在10-6托(1.3×10-4Pa)的范围内的背景压力。
外壳12的顶部包括可拆卸的、L形橡胶垫片密封的板28,该板配有外部安装三英寸(7.6厘米)直径的直流磁控管溅射沉积源30(以商品名“US GUN II”购自加利福利亚州圣荷西的美世公司(US,Inc.,SanJose,CA))。溅射沉积源30内固定有金溅射靶32(直径7.6cm(3.0英寸)×厚0.48cm(3/16英寸))。溅射沉积源30由配有消弧器(以商品名“SPARC-LE20”得自科罗拉多州科林斯堡的领先能源工业公司(Advanced Energy Industries,Inc,Fort Collins,CO))的磁控管驱动电源(magnetron drive)(以商品名“MDX-10MAGNETRON DRIVE”购自科罗拉多州科林斯堡的领先能源工业公司(Advanced Energy Industries,Inc,Fort Collins,CO))提供电力。
粒子搅拌器16为在顶部36中具有矩形开口34(4.5cm×3.5cm)的中空圆柱体(长6cm×横向直径5.5cm)。开口34位于金溅射靶32的表面36的正下方7cm处,使得溅射的金属原子可进入搅拌器空间38。搅拌器16配有与其轴线对准的轴40。轴40具有矩形横截面(1cm×1cm),其上螺栓连接四个矩形叶片42,所述矩形叶片形成用于使载体粒子翻滚的搅拌机构或桨轮。叶片42各具有两个通孔44,以促进包含在由叶片42和粒子搅拌器圆柱体16形成的四个象限的每一个中的粒子体积之间的连通。
实例1
将聚四氟乙烯(PTFE)粉末(1微米粒度,购自马萨诸塞州沃德山的阿法埃莎公司(Alfa Aesar,Ward Hill,MA))与粒状活性炭(12×20目,以商品名“KURARAY GG12×20”购自德克萨斯州休斯顿的可乐丽化工公司(Kuraray Chemical Company,Houston,TX))干混以形成PTFE粉末涂布的碳颗粒,其在碳上包含12重量%的PTFE。
将上面制得的涂布了12重量%的PTFE的碳颗粒的40cc(17.68g)的部分在150℃下在对流烘箱中干燥5小时。将干燥的粒子置于上述设备10的真空室14中的粒子搅拌器16中。将真空室14抽真空到8×10-6托(1.07×10-3Pa),并将足量的氩溅射气体(购自明尼苏达州圣保罗的氧气服务公司(Oxygen Service Company,St.Paul,MN))引入,以达到约10毫托(1.33Pa)的压力。然后通过施加60瓦特的阴极功率来启动纳米金沉积过程。在纳米金沉积过程中,粒子搅拌器轴40以约4rpm的速度旋转。阴极功率在1小时后中止。将真空室反充空气,并去除纳米金涂布的粒子。金溅射靶32在涂布前重273.38g,在涂布后重271.60g。基于搅拌器的捕获效率,涂布在PTFE粉末涂布的碳颗粒上的金的量为约0.7重量%。
使用由热塑性塑料块(由可以商品名“DELRIN”从特拉华州威尔明顿的杜邦公司(E.I.DuPont de Nemours and Company,Wilmington,DE)商购获得的缩醛树脂制成)组成的测试单元测量了所得的金涂布的粒子的粉末体积电阻率,所述热塑性塑料块包含圆形横截面为1.0cm2的圆柱形腔体。腔体的底部被黄铜电极覆盖。第二电极为1.0cm2横截面的配合到腔体中的黄铜圆柱体。将待测试的上文所制得的金涂布的粉末置于腔体中,然后将黄铜圆柱体插入。将砝码置于黄铜圆柱体的顶部,以在粉末上施加18psi(120kPa)的总压力。将电极连接到数字万用表以测量电阻。当粉末床为1.0cm高时,观测到的电阻(Ω)等同于粉末体积电阻率(Ω·cm)。实例1的金涂布的粒子的粉末体积电阻率大于2×106Ω·cm。
比较例A
比较例A样品为无任何进一步处理的上文用于实例1的粒状活性炭。
比较例B
比较例B样品为无进一步处理的上文在实例1中制得的PTFE粉末涂布的粒状碳。
比较例C
除了以下方面外,以与实例1相同的方式制备了比较例C样品:将活性炭颗粒用8重量%的磁性Fe2O3纳米粉末(以商品“NANOARCMAGNETIC Fe2O3”购自马萨诸塞州沃德山的阿法埃莎公司(Alfa-Aesar,Ward Hill,MA))而不是PTFE粉末涂布。
比较例D
除了以下方面外,以与实例1相同的方式制备了比较例D样品:通过在PVD设备中插入银靶以替代金靶,将在粒状碳上含有12重量%的PTFE的PTFE粉末涂布的碳颗粒用银而不是金涂布。
乙烯去除测试
对得自实例1和比较例A-D的样品测试了其乙烯去除能力。使用流通式、固定床反应器进行了乙烯去除测试。反应器为4.5cm(外径)×4.1cm(内径)硼硅酸盐玻璃管,使用配有电子控制器(分别以商品名“SYNTRON MAGNETIC FEEDER FT0-C”和“POWERPULSE”购自德克萨斯州休斯顿FMC科技公司(FMC Technologies,Houston TX))的振动给料器将样品填充到管中以得到25mL的总样品床体积。样品支承在玻璃反应器管内部的不锈钢网状圆盘上,将玻璃绒插入管的任一端,以最大程度降低挑战性气体流动期间介质的移动。将压缩的乙烯气体混合物(在N2中含有1000ppm的C2H4,购自明尼苏达州圣保罗的氧气服务公司(Oxygen Service Company,St.Paul,MN))和经过滤的压缩空气(室内空气,通过3M FILTER CARTRIDGE-2811过滤,可以商品名“3M FILTER CARTRIDGE-2811”从明尼苏达州圣保罗的3M公司(3M Company,St.Paul,MN)商购获得)在引入反应器空间前预混,其中将质量流控制器(以商品名“MODEL GFC17”购自纽约州奥兰治堡的奥尔堡仪器与控件公司(Aalborg Instruments and Controls,Inc.,Orangeburg,NY))用于控制相应进料气体的流量。将压缩空气流在与乙烯气体混合前通过使空气流经热水浴而预湿。将湿度控制器(以商品“SD SERIES PID CONTROLLER”购自密苏里州圣路易斯的瓦特隆电子科技公司(Watlow Electric Manufacturing Co.,St.Louis,MO))以反馈方式连接到浸入水浴中的浸入式加热器线圈(购自密苏里州圣路易斯的瓦特隆电子科技公司(Watlow Electric Manufacturing Co.,St.Louis,MO))和位于水浴下游气体空间中的湿度探头(以商品名“MODELHMT100”购自芬兰赫尔辛基的维萨拉公司(Vaisala,Helsinki,Finland)),以将气相相对湿度在22℃下维持在99%附近。所有测试均在室温(约22℃)下进行。调节C2H4和空气的体积流量以产生总流量为1L/min的在空气中5ppm的C2H4的挑战性预混物。在这些测试条件下,获得了1.5秒的停留时间和2,400h-1的气体每小时空速。使来自反应器的出口气体直接进入FTIR光谱仪的可变光程长光程吸收池(以商品名“MIDAC M4100”购自马萨诸塞州韦斯特菲尔德的MIDAC公司(MIDAC Corporation,Westfield,MA),包括“MODEL16-V”长光程吸收池)。将气体吸收池的光程长设为10米,以每分钟64次扫描的平均值采集数据。将位于949cm-1附近的红外波段的峰高度用于对气体吸收池中的乙烯浓度(ppm)定量。通过监测随着时间的推移来自反应器的出口气体中的乙烯浓度而获得穿透曲线。将出口气体流中观察到的浓度为输入乙烯浓度的50%时的时间取为介质的乙烯去除能力的度量。因此,值越高表示在这些条件下的乙烯去除能力越高。实例1和比较例A-D的所测量的值汇总在表1中。
表1
实例 | t1/2(min) |
1 | 11.10 |
比较例A | 4.81 |
比较例B | 4.45 |
比较例C | 6.38 |
比较例D | 4.95 |
除非另外指明,否则本文给出的所有实例均认为是非限制性的。在不脱离本公开的范围和精神的条件下,本领域的技术人员可对本公开进行各种变型和更改,并且应当理解,本公开不应不当地受限于本文所述的示例性实施例。
Claims (21)
1.一种复合粒子,包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
2.根据权利要求1所述的复合粒子,其中所述金纳米粒子的不连续层包含所述金纳米粒子的多个岛状区域。
3.根据权利要求1或权利要求2所述的复合粒子,其中所述氟化的表面为芯粒子上的氟化的涂层。
4.根据权利要求3所述的复合粒子,其中所述芯粒子包含含碳材料、沸石或金属氧化物中的任一种。
5.根据权利要求3所述的复合粒子,其中所述芯粒子包含活性炭。
6.根据前述权利要求中任一项所述的复合粒子,其中所述复合粒子具有至多1:10000的纵横比。
7.根据前述权利要求中任一项所述的复合粒子,其中所述复合粒子具有在0.1微米至10000微米的范围内的粒度。
8.根据前述权利要求中任一项所述的复合粒子,其中所述氟化的表面包含聚四氟乙烯。
9.根据前述权利要求中任一项所述的复合粒子,其中所述芯粒子适用于去除水分。
10.根据前述权利要求中任一项所述的复合粒子,其中所述芯粒子为挥发性有机化合物的吸附剂。
11.根据前述权利要求中任一项所述的复合粒子,其中所述金纳米粒子的不连续层相对于所述复合粒子在0.05重量%至5重量%的范围内。
12.根据前述权利要求中任一项所述的复合粒子,其具有至少106Ω·cm的粉末体积电阻率值。
13.一种制品,包含:
基底;
设置在所述基底的表面上、设置在所述基底内或两者的多个复合粒子;
其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
14.根据权利要求13所述的制品,其中所述基底为片材、膜、非织造幅材或多个粒子中的任何形式。
15.一种制品,包含:
容器;
设置在所述容器内的多个复合粒子;
其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
16.根据权利要求15所述的制品,其中所述容器包括渗透性袋、限定入口和出口的管或非织造幅材中的任一种。
17.一种去除乙烯的方法,所述方法包括:
将乙烯去除剂置于乙烯生成源的附近,其中所述乙烯去除剂包含:
多个复合粒子,其中所述多个复合粒子中的各个复合粒子包含:
氟化的表面;和
设置在所述氟化的表面上的金纳米粒子的不连续层。
18.根据权利要求17所述的方法,其中所述乙烯去除剂和所述乙烯生成源在封闭系统内。
19.根据权利要求18所述的方法,其中所述封闭系统包括用于增强气体从所述乙烯生成源流动到乙烯去除剂的装置。
20.根据权利要求17至19中任一项所述的方法,其中所述乙烯生成源为收获的水果、收获的蔬菜或收获的花卉中的任一种。
21.一种制冷系统,包含权利要求1至12中任一项所述的复合粒子。
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US20040231511A1 (en) * | 2003-05-22 | 2004-11-25 | Karwacki Christopher J. | Process for the removal of ethylene oxide from air |
JP2006111922A (ja) * | 2004-10-14 | 2006-04-27 | Nippon Valqua Ind Ltd | フッ素系高分子材料表面への金皮膜の形成方法及び該方法により得られた金皮膜付きフッ素系高分子材料 |
US20060148971A1 (en) * | 2004-12-30 | 2006-07-06 | 3M Innovative Properties Company | Fluoropolymer nanoparticle coating composition |
CN101111538B (zh) * | 2004-12-30 | 2011-03-30 | 3M创新有限公司 | 氟聚合物纳米颗粒涂料组合物 |
WO2008035347A2 (en) * | 2006-09-21 | 2008-03-27 | Ariel-University Research And Development Company Ltd. | Superhydrophobic nanotextured polymer and metal surfaces |
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CN111229159A (zh) * | 2020-01-15 | 2020-06-05 | 武汉世林福幸科技发展有限公司 | 一种乙烯吸附剂及其制备方法 |
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US20140363554A1 (en) | 2014-12-11 |
EP2794089A4 (en) | 2015-09-09 |
WO2013096039A1 (en) | 2013-06-27 |
US20160330986A1 (en) | 2016-11-17 |
JP2015509915A (ja) | 2015-04-02 |
EP2794089A1 (en) | 2014-10-29 |
US10004243B2 (en) | 2018-06-26 |
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