CN100356985C - 用于除臭的多层碳纳米球 - Google Patents

用于除臭的多层碳纳米球 Download PDF

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CN100356985C
CN100356985C CNB038258161A CN03825816A CN100356985C CN 100356985 C CN100356985 C CN 100356985C CN B038258161 A CNB038258161 A CN B038258161A CN 03825816 A CN03825816 A CN 03825816A CN 100356985 C CN100356985 C CN 100356985C
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shell
nano carbon
carbon balls
transition metal
deodorant
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金钟润
宋俊烨
朴承圭
姜润锡
尹锡本
俞宗成
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LG H&H Co Ltd
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Abstract

本发明公开了一种用于除臭的碳纳米球，其由圆形空心及多孔碳壳层组成，并且选自由过渡金属、过渡金属氧化物和碱金属盐组成的组中的至少一种除臭材料被附着到该多孔碳壳层中。这种用于除臭的碳纳米球的多孔碳壳层包括具有不同孔尺寸的两层以上的多个层，而且形成在外层的孔比形成在内层的孔具有更大的平均直径。用于除臭的多层碳纳米球可以吸附多种产生恶臭的物质，同时具有良好的除臭性能。因此，当将多层碳纳米球用作除臭剂，应用于各种散发臭味的日用品或住宅、办公室、工业设备及其它多种散发臭味的环境时，可以通过捕获和溶解恶臭物质而达到良好的除臭效果。

Description

用于除臭的多层碳纳米球
技术领域
本发明涉及一种用于除臭的碳纳米球，更具体而言，本发明涉及一种用于除臭的多层碳纳米球，该多层碳纳米球是由具有球形空心的多孔碳壳层组成的。
背景技术
通常，各种不良气味是产生自日用品如冰箱、空调、尿布、卫生带、香烟、鞋柜和衣柜以及日常生活场所如卧室、浴室和车库的。另外，不良气味也可以产生自机动车的废气以及工业装置如垃圾处理场、废水处理厂和工厂的废气。产生不良气味的代表性材料如下：甲硫醇、甲硫醚(二甲硫)、二甲基二硫醚、硫化氢、氨、三甲胺、乙醛、一氧化氮、一氧化二氮、苯乙烯等等。
此外，为了消除这些不良气味，人们已经开发了各种除臭剂。
最近，提出了一种用于制备碳纳米球的方法，该碳纳米球是由具有球形空心的多孔碳壳层组成的(Adv.Mater.2002，14，No.1，January4)。这种碳纳米球与传统的活性炭除臭剂相比，其优点在于可以吸附更多种的恶臭物质。然而，这种碳纳米球具有某些局限性，即在它吸附一定量的恶臭物质之后，就不能吸附更多的恶臭物质了。另外，上述碳纳米球的除臭能力也有限。
发明内容
本发明是设计用来解决现有技术的上述缺陷的，因而，本发明的目的在于提供一种碳纳米球，该碳纳米球具有极好的除臭性能，并且能够吸附多种恶臭物质。
为了实现上述目的，本发明提供了一种用于除臭的碳纳米球，该碳纳米球包括具有球形空心的多孔碳壳层，其中至少一种选自由过渡金属、过渡金属氧化物和碱金属盐组成的组中的除臭材料被浸渍到该壳层中，其中该多孔碳壳层具有多层结构，在该多层结构中包括具有不同孔尺寸的至少两层，并且其中形成在外层中的孔的平均直径大于形成在内层中的孔的平均直径，或者相反。
优选地，过渡金属是选自由铜(Cu)、铁(Fe)、锰(Mn)、镍(Ni)、钴(Co)、银(Ag)、金(Au)、钒(V)、钌(Ru)、钛(Ti)、铬(Cr)、锌(Zn)和钯(Pd)组成的组中的一种，而碱金属盐是选自由溴化钠(NaBr)、碘化钠(NaI)、溴化钾(KBr)、碘化钾(KI)和碘酸钾(KIO3)组成的组中的一种。
附图说明
在以下参照附图的详细描述中，对本发明优选实施例的这些和其它特征、方面和优点进行了更为全面的描述。在附图中：
图1是示出了根据本发明的用于制备除臭用碳纳米球的方法的示意图；
图2是通过电子显微镜拍摄的根据本发明的多层碳纳米球的照片；以及
图3是根据本发明的用于除臭的多层碳纳米球的动力学吸收性能的曲线图。
具体实施方式
在下文中，将对本发明的实施例进行描述，然而，本发明并不局限于以下实施例，在本发明的范围内能够以不同的方式进行修改。
本发明的用于除臭的碳纳米球具有由空心和多孔壳层组成的球状碳结构。过渡金属、过渡金属氧化物、碱金属盐或其混合物被浸渍到该壳层中。此外，多孔碳壳层具有不同尺寸的至少两层。形成在外层中的孔可以比形成在内层中的孔具有更大的平均直径，并且反之亦然，因此，各种恶臭物质可以依据其尺寸、形状或化学性质按顺序被吸收。孔的尺寸控制在0.01至50纳米的范围内。
由于该壳层具有不同孔尺寸的至少两层，因此可以吸收各种恶臭物质，并且浸渍在孔中以及该壳层的内外表面上的除臭材料可以化学吸附并破坏这些恶臭物质。本发明的这种用于除臭的碳纳米球与韩国的专利公开出版物第1999-80808号所披露的浸渍的活性炭相比，显示出更优异的除臭性能。换言之，由于活性炭具有微孔，当浸渍除臭材料时，这些孔可能被阻塞，从而消弱了其除臭性能。然而，由于本发明的用于除臭的碳纳米球在壳层中具有介孔(中孔)，因此，这类问题不会出现。另外，由于本发明的用于除臭的碳纳米球在其空心中捕获恶臭物质，其明显不同于浸渍的活性炭，因此，恶臭物质与浸渍在壳层内表面上的除臭材料之间可以有足够的接触时间。另外，当由除臭材料所产生的分解产物被散发到外部时，本发明的碳纳米球可以防止造成二次污染。
参照图1，将对根据本发明的用于制备用于除臭的碳纳米球的方法进行详细描述。
首先，制备球形的二氧化硅核心1。作为一个实例，二氧化硅核心1可以根据公知的Stober法(Stober，W.；Fink，A,；Bohn，E.J.Colloid Inter.Sci.1968，26，62)，由二氧化硅前体如正硅酸四甲酯和正硅酸四乙酯制得。该二氧化硅核心的直径优选为5至1,000纳米(nm)。
随后，在溶剂中，通过使二氧化硅前体与表面活性剂反应，由二氧化硅和表面活性剂形成的第一壳层2在二氧化硅核心1的表面上生长，例如，该表面活性剂是由以下化学式1表示的烷基三甲氧基硅烷、由以下化学式2表示的烷基三乙氧基硅烷、由以下化学式3表示的烷基三甲基卤化铵、由以下化学式4表示的烷基聚乙二醇、以及由以下化学式5表示的1，2，3-丙三基乙氧基化合物(glycerolethoxylate)。
化学式1
R1R2R3R4Si(OCH3)3
在化学式1中，R1、R2和R3独立地是甲基或乙基，而R4是碳数为12至22的烷基。
化学式2
R1R2R3R4Si(OC2H5)3
在化学式2中，R1、R2和R3独立地是甲基或乙基，而R4是碳数为12至22的烷基。
化学式3
R1R2R3R4NX
在化学式3中，R1、R2和R3独立地是甲基或乙基，R4是碳数为4至22的烷基，而X是卤素。
化学式4
R(OCH2CH2)nOH
在化学式4中，R是碳数为4至22的烷基，而n是3至20之间的整数。
化学式5
CH2(CH2O)n1HCH(CH2O)n2HCH2(CH2O)n3H
在化学式5中，n1、n2和n3独立地是4至20之间的整数。
然后，加入具有不同种类和摩尔比的二氧化硅前体和表面活性剂，并且使之进行反应以便在第一壳层2的表面上形成第二壳层3。形成在该壳层上的孔的尺寸是根据表面活性剂的种类以及二氧化硅前体的种类和摩尔比而变化的。因而，控制二氧化硅前体和表面活性剂的种类，以使形成在第二壳层3中的孔的尺寸大于形成在第一壳层2中的孔的尺寸。若需要的话，随后可以将具有较大孔的第三壳层形成在第二壳层3的表面上。
其后，在对形成有壳层的产物进行选择性过滤之后，在例如500～600℃下进行焙烧，用以去除表面活性剂组分。然后，得到具有多层二氧化硅壳层4的颗粒10，其中介孔形成在除去表面活性剂的位置上，并具有特定的尺寸。多层二氧化硅壳层4优选的厚度为10至500纳米。
随后，将能够形成作为碳前体的聚合物的单体11如丙烯腈、苯酚甲醛及二乙烯基苯、糖、糠基等注入形成于颗粒10的壳层中的孔内，在该壳层中形成有多层二氧化硅。其后，将该单体进行聚合以便形成聚合物。作为聚合反应的实例，当利用自由基聚合反应用以形成作为碳前体的聚合物时，将该单体与自由基引发剂充分混合，并注入二氧化硅颗粒的介孔中，然后根据单体的特性来进行聚合。此时，就自由基引发剂而言，可以使用偶氮二异丁腈(AIBN)、过氧乙酸叔丁酯、过氧化苯甲酰、过氧化乙酰、以及月桂基过氧化物。这种聚合反应在本技术领域是公知的，优选地，在60～130℃下进行聚合反应12小时，用以制备二氧化硅/聚合物复合物。
然后，将二氧化硅/聚合物复合物，在氮气氛中、大约1,000℃下进行处理，以便制备含有碳化聚合物13的二氧化硅。其后，将二氧化硅/聚合物复合物放入到氢氟酸溶液或氢氧化钠/乙醇的混合溶液中，用以除去该二氧化硅结构，这样，就得到了具有球形空心15和多孔碳壳层的碳纳米球20。
其后，根据本发明，将碳纳米球20浸入到由过渡金属、过渡金属氧化物、碱金属盐或其混合物组成的溶液中，并在室温下熟化(老化)2至3天，然后过滤，并在70至110℃下干燥，用以制备浸渍有除臭材料17的多层碳纳米球。对于可以被用来浸渍壳层的过渡金属或过渡金属氧化物而言，可以使用铜(Cu)、铁(Fe)、锰(Mn)、镍(Ni)、钴(Co)、银(Ag)、金(Au)、钒(V)、钌(Ru)、钛(Ti)、铬(Cr)、锌(Zn)、钯(Pd)或它们的氧化物。对于碱金属盐而言，可以使用溴化钠(NaBr)、碘化钠(NaI)、溴化钾(KBr)、碘化钾(KI)和碘酸钾(KIO3)。除臭材料17的浸渍量可以通过改变除臭材料的溶液浓度或渗入时间来进行控制，优选的是，以用于除臭的碳纳米球的总重量为基准，除臭材料浸渍量的范围为0.01～30wt％(重量)。
根据本发明的由除臭材料浸渍的碳纳米球可以提供有上述金属中的一种或多种的除臭材料。因此，根据本发明的含有由除臭材料浸渍的碳纳米球除臭剂，可以根据不良气味或其用法的不同而以不同的方式进行制备或组成。例如，除臭剂可以含有碳纳米球，该碳纳米球中只浸渍了一种除臭材料，或其中浸渍了两种不同种类的除臭材料，或者其中浸渍了两种以上的除臭材料。
根据本发明的由除臭材料浸渍的碳纳米球可以被用来除臭和消除多种有气味的物质，如甲硫醇、甲硫醚、二甲基二硫醚、硫化氢、氨、三甲胺、苯乙烯、乙醛、一氧化氮、一氧化二氮、产生自住宅内的浴室、厨房或鞋柜中的室内不良气味、以及烟草气味。这样，其在消除冰箱、空调、空气净化器、车库、汽车废气以及人体的不良气味方面也具有极好的效果。
另外，可以将根据本发明的由除臭材料浸渍的碳纳米球进行均匀地分散，并将其附着到一个具有薄片形状的包或垫上，这样可以将它应用于诸如婴儿或患有失禁的病人的尿布或妇女用卫生带这些使用这类物质的商品中。
实施例1～8
球形二氧化硅核心是根据公知的Stober法通过使用作为二氧化硅前体的四乙氧基硅烷而制得的。此时，将60mL的四乙氧基硅烷放入到包含有1000mL的乙醇、80mL的水和40mL浓度为28％的氨水的均相混合溶剂中，以便形成200至300纳米的球形二氧化硅核心。
然后，将59mL以摩尔比为11.8混合的十八烷基三甲氧基硅烷(C18-TMS)和四乙氧基硅烷的混合物作为表面活性剂放入到1180mL的二氧化硅核心中，然后进行反应，以便在二氧化硅核心的表面上生长第一壳层。接着，将另外59mL以摩尔比为47.2混合的十八烷基三甲氧基硅烷和四乙氧基硅烷的混合物放入到其中，并且进行反应，用于生长第二壳层。随后，将制成的二氧化硅颗粒进行过滤，然后在550℃下热处理5小时，以便在除去表面活性剂的位置形成一定尺寸的介孔。
然后，将二乙烯基苯与自由基引发剂偶氮二异丁腈(AIBN)进行充分混合，然后注入到二氧化硅颗粒的介孔中，接着在80℃下进行聚合约12小时，用以制得包含聚合物的二氧化硅结构。紧接着，将含有聚合物的二氧化硅结构在氮气氛中、于1,000℃下碳化，用以形成碳纳米球。随后，将这种碳纳米球放入到氢氟酸中，用以除去碳纳米球中的无机结构。这样得到了一种碳纳米球，该碳纳米球具有球形碳结构，其包括空心和多孔的多层壳层。
其后，为了浸渍如下表1中的除臭材料，将用上述方法制得的碳纳米球在1N的除臭材料溶液中浸渍约50小时，然后进行过滤，并在70℃下干燥，这样就得到了浸渍了除臭材料的碳纳米球。
表1
    浸渍金属的种类(金属的浸渍量，％)
    实施例1     铜(1.3)+锰(0.3)
    实施例2     镍(3.1)+铁(0.8)
    实施例3     金(0.8)+铬(0.9)+钯(0.8)
    实施例4     铜(3.1)+铁(0.8)+锌(0.8)
    实施例5     碘化钾(3.4)
    实施例6     银(4.2)
    实施例7     钴(2.1)+碘酸钾(1.3)
    实施例8     钒(2.1)+钌(0.3)+钛(0.6)
在表1中，金属的浸渍量(％)＝金属的重量/碳纳米球的重量×100。
比较例1和比较例2
选择由S公司和L公司制造的主要包括作为除臭材料的浸渍活性炭的碳纳米球作为比较例1和比较例2。
将根据实施例5和比较例1及比较例2的碳纳米球对于甲硫醇的除臭能力进行比较，并且将比较结果示于图3中。将50ppm的甲硫醇以100ml/min的速率通过含有除臭材料的反应器，并且利用质谱来分析其随时间的动力学吸附性能。参照图3，可以理解的是，具有根据本发明的多层壳层结构的浸渍了除臭材料的碳纳米球表现出优于比较例的极好的连续除臭效果。
工业实用性
如上所述，根据本发明的浸渍了除臭材料的多层碳纳米球吸附多种恶臭物质，并且表现出良好的除臭性能。因此，本发明的碳纳米球，当被用作除臭剂，应用于多种日用品、生活空间、工业场所以及其它多种产生臭味的环境时，在捕获和溶解恶臭物质方面可以表现出极好的除臭效果。
已经对本发明进行了详细描述。然而，应该理解的是，以上的详细描述和特定实施例仅以举例说明的方式给出了本发明的优选实施例而已，其并不用于限制本发明，本领域技术人员应该明了，本发明可以由这些详细描述出发在本发明的精神和保护范围之内作出各种更改和变化。

Claims (4)

1.一种用于除臭的碳纳米球，所述纳米球包括具有球形空心的多孔碳壳层，
其中，至少一种选自由过渡金属、过渡金属氧化物和碱金属盐组成的组中的除臭材料被浸渍到所述壳层中，
其中，所述多孔碳壳层具有多层结构，在所述多层结构中包括具有不同孔尺寸的至少两层，以及
其中，形成在外层中的孔的平均直径大于形成在内层中的孔的平均直径，或者相反。
2.根据权利要求1所述的用于除臭的碳纳米球，
其中，所述过渡金属是选自由铜、铁、锰、镍、钴、银、金、钒、钌、钛、铬、锌和钯组成的组中的一种，以及其中，所述碱金属盐是选自由溴化钠、碘化钠、溴化钾、碘化钾和碘酸钾组成的组中的一种。
3.根据权利要求1或2所述的用于除臭的碳纳米球，
其中，以所述用于除臭的碳纳米球的总重量为基准，所述除臭材料的浸渍量为0.01～30wt％。
4.根据权利要求1或2所述的用于除臭的碳纳米球，
其中，所述球形空心的直径为5～1,000纳米，而所述多孔碳壳层的厚度为10～500纳米。
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