CN1123700A - 改性的杀菌活性碳 - Google Patents

改性的杀菌活性碳 Download PDF

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CN1123700A
CN1123700A CN95107587A CN95107587A CN1123700A CN 1123700 A CN1123700 A CN 1123700A CN 95107587 A CN95107587 A CN 95107587A CN 95107587 A CN95107587 A CN 95107587A CN 1123700 A CN1123700 A CN 1123700A
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activated carbon
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carbon fiber
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A·V·皮缅诺夫
A·I·利伯曼
J·L·施密特
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Electrophor Inc
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Abstract

对活性碳进行改性以使其具有杀菌性能。所述改性的活性碳特别适于饮用水的纯化，可针对不同地区的饮用水杂质进行改性。按照本发明，对活性碳进行处理以至少吸附一种有机杀菌化合物。

Description

改性的杀菌活性碳
城市处理的或未处理的饮用水至少有下面一些杂质：细菌、悬浮固体、有机物质、重金属、阴离子、氯以及溶解的气体。杂质的组成和浓度常因地区而异。而细菌、危险的有机物、重金属离子和氯尤其是有害的，最好从饮用水中除去。本发明涉及改性的活性碳纤维(activated carbon fiber)材料，它们可作为吸附剂用于从流体中除去这些不想要的成分。在本说明书中术语“ACF”代表活性碳纤维。所述改性的ACF不但具有与普通ACF相似的吸附容量，而且还含有物理附着于其表面上的杀菌剂。这对于饮用水的纯化是非常有效的。
活性碳纤维(称作ACF)或其它形式的碳例如碳粉是通过在活化气氛通常为水蒸汽和/或二氧化碳和/或氨中，在高温下通过将碳化材料活化生产的。碳化纤维是通过在惰性气氛中将聚丙烯腈、酚树脂、沥青或纤维素纤维碳化制成的。在常规的碳化中，将有机材料加热至200-800℃，通常超过400℃足够长的时间以除去低分子量有机物和焦油，剩下超过90％的碳，该碳通常是晶态-非晶态结构形式(石墨层)而不是多孔结构。避免使用水蒸汽或二氧化碳以保留碳纤维强度。碳化之前的预处理步骤是本领域已知的。碳化后，将碳化材料在800-1200℃之间的温度下，在包含水蒸汽和/或二氧化碳的活化气氛中活化。
活性碳，尤其是已知的活性碳纤维对于有机物具有良好的吸附容量，且具有极佳的从水中除去氯的能力。在先有技术中已知可通过附着银或碘而使吸附材料带有抑菌或杀菌性。然而，银和碘均具有有害的副作用。而碘由于其对于甲状腺的作用就更具危险性。
对活性碳的一些改性是本领域已知的。Shimazaki等的美国专利4576929叙述了通过将丙烯酸类纤维预氧化、活化和酸处理而得到的纤维状活性碳。将所述纤维状活性碳用硫酸银水溶液处理。从而吸附银而产生含银ACF。所述含银ACF已显示出具有杀菌性。但载有银的活性碳的缺点在于银价格昂贵，而且它几乎只具杀菌功效，而且根据EPA规章，饮用水中银浓度不能超过十亿分之五十。本发明比该参考文献的优越之处在于它使用了不含银的杀菌有机化合物。银价格昂贵，而且能浸出到水中。
因而，先有技术的方法和产物的缺点在于不能提供有效且廉价的的生产具有杀菌性能的改性ACF的方法，以针对于不仅需要除去有机物和/或重金属阳离子还需要除去细菌和/或病毒的不同的水纯化问题对ACF进行适当的改性。
本发明包含改进的活性碳纤维材料(来自将纤维素纤维碳化并活化的ACF)或类似来源的非纤维状材料，所述材料除了具有吸附有机材料的能力外，还通过改性，而具有杀菌性。本发明也涉及生产这种改性的吸附材料的方法，本发明吸附材料包括活性碳纤维基材和物理附着于其表面的有机化合物。所述有机化合物与活性碳基材形成强的物理结合，并在其结构中具有提供杀菌性能的功能活性基团。
虽然制备改性的活性碳纤维是优选的，但本发明的产物也可以是其它形式，例如粉末、压制粉末或颗粒，它们或是通过将碳纤维产物细分散或直接将已在水蒸汽和/或二氧化碳存在下在800-1200℃活化的碳化粉末或颗粒改性而获得。
该吸附材料尤其可用于从饮用水中除去有害物质。为适于饮用水的纯化，改性的吸附材料应同时具有多个不同性能，例如大的有机吸附容量，对于宽范围细菌和病毒具有杀菌吸附能力。
除了饮用水的纯化外，本发明的生产改性吸附材料的方法可用于制备生物化学和医药领域的特殊改性吸附材料。
本发明通过吸附而不是传统的化学反应将官能团联接到化学惰性基材的表面上。这使得可通过非常简单的方法得到具有所需特性的吸附材料。通过在所指出的数个适合的有机化合物之中选择合适的改性添加剂，可得到对于给定添加剂具有所需吸附性能的活性碳纤维材料。
在使用碳纤维作为活性碳时，用作前体材料的碳纤维的直径通常在1-30微米之间变化，优选2-10微米。最终产物可以是非织造布、丝、织物以及其它形式。
下列实施例用于说明本发明，除非另外指出，本申请中所有份数和百分数均为重量份。
在下面实施例中使用的碳化纤维购自Kuibishey Fiber Corpora-tion(白俄罗斯共和国)。其制法是：将人造纤维浸入到硅-碳水化合物表面活性剂在四氯化碳中的溶液中，除去过剩溶液，先在150-350℃，然后在400-800℃将处理的人造纤维碳化，碳化总共用时72小时。
用在下列实施例中的活性碳纤维是在950-1100℃通过将预处理的碳化纤维素纤维活化制得的。
在本改性方法中，通过在活性碳上吸附结构中含活性杀菌基团(即含仲、叔或季氮的基团)以及能吸附在活性碳纤维表面上的结构即芳香结构的有机杀菌剂例如煌绿或利凡诺(6，9-二氨基-2-乙氧基吖啶乳酸盐)以及有机卤(Cl或Br)化物而将杀菌能力赋予活性碳纤维。这些杀菌剂是阳离子的。其它合适的有机杀菌剂包括苄醇、氨琥胺、nitractin、苄烷铵、对氨基酚、五氯酚钠、N-烷基-2-甲基-5-乙基-piridinium、呋喃西林和青霉素V。
吸附步骤通常在0-90℃，优选10-40℃进行5秒至2小时。反应时间优选15秒至10分钟。处理溶液中的改性剂的浓度可从1微克/克纤维至其最大溶解度之间变化，这因吸附剂而异。实施例1-3
将10g活性碳纤维(ACF)放置在1升0.01％(重量)煌绿水溶液中(实施例1)(实施例2中0.02％，实施例3中0.03％)。将1g本发明的改性ACF吸附10毫克煌绿(实施例1中)、20毫克煌绿(实施例2中)和30毫克煌绿(实施例3中)。然后将活性碳纤维用水洗涤并放置在100立方厘米圆柱中。将含E.大肠菌(E.Colibacteria)(指数2000)的水用泵以150ml/min速度通过该柱。改性的活性碳纤维与E.大肠菌溶液的接触时间为40秒。测示滤过水的E.大肠菌指数。分析结果是：实施例1：E.大肠菌指数15；实施例2：E.大肠菌指数4；实施例3：E.大肠菌指数少于3(无法检测)。实施例4
将10g活性碳纤维(ACF)浸渍在100ml0.2％(重量)煌绿的乙醇溶液中。在乙醇溶液完全脱色后，将ACF在空气中干燥。1g该改性的ACF吸附20mg煌绿。然后将活性碳纤维放置在100立方厘米圆柱中。将含E.大肠菌(指数2000)的水用泵以150ml/min速度通过该柱。改性的活性碳纤维与E.大肠菌溶液的接触时间为40秒。滤过水的E.大肠菌指数少于3(无法检测)。实施例5-7
将13g活性碳纤维(ACF)浸渍在1升0.039％(重量)利凡诺水溶液中(实施例5)(实施例6中为0.039％(重量)呋喃西林水溶液，实施例7中为0.039％(重量)青霉素V)，浸15分钟。1g该改性的ACF吸附30mg利凡诺(实施例5)、30mg呋喃西林(实施例6)和30mg青霉素V。然后将活性碳纤维放置在108立方厘米的圆柱中。将含E.大肠菌的水(3000000个细菌/升)用泵以150ml/min速度通过该柱。改性的活性碳纤维与E.大肠菌溶液的接触时间为43秒。测示滤过水的E.大肠菌指数。分析结果是：实施例5：滤过水的E.大肠菌计数为30000个细菌/升，实施例6：滤过水的E.大肠菌计数为10000个细菌/升，实施例7：滤过水的E.大肠菌计数为40000个细菌/升。实施例8
将13g活性碳纤维(ACF)放置在1升0.039％(重量)利凡诺的水溶液中。1g该改性的ACF吸附30毫克利凡诺。然后将活性碳纤维用水洗涤，并放置在108立方厘米圆柱中。将1升含沙门氏菌(6000000个细菌/升)的水用泵以150ml/min的速度通过圆柱。测示滤过水的沙门氏菌浓度。在滤过水中未发现沙门氏菌。实施例9-12
将1g活性碳纤维(ACF)放置在100毫升0.03％(重量)利凡诺水溶液中(实施例9、10、11、12中也分别与上相同)。lg该改性的ACF吸附30毫克利凡诺。然后将活性碳用水洗涤，并放置在8.3立方厘米的圆柱中(实施例9)，(实施例10中为5立方厘米，实施例11中为5立方厘米，实施例12中为3立方厘米圆柱)。将含E.大肠菌的水(实施例9中15000个细菌/升，实施例10中16000个细菌/升，实施例11中1000个细菌/升，实施例12中16000个细菌/升)以20ml/min的速度用泵通过圆柱。改性的活性碳纤维和E.大肠菌溶液的接触时间为25秒(实施例9)、15秒(实施例10)、15秒(实施例11)和9秒(实施例12)。测示滤过水的E.大肠菌浓度。分析结果是：实施例9：未发现E.大肠菌，实施例10：E.大肠菌计数为56个细菌/升。实施例11：未发现E.大肠菌，实施例12：E.大肠菌数为40个细菌/升。
可将改性的活性碳纤维装填到合适的柱中，装填密度从0.5g/cm3-0.4g/cm3。较高的ACF装填密度是理想的，以用长纤束保留住微生物。优选装填密度为每立方厘米0.08-0.3g改性的碳纤维。
可在活性碳纤维上吸附每克碳0.5-200mg，优选每克碳5-50mg的不同浓度的有机杀菌剂。
本发明提供的改性的活性碳纤维材料可用于纯化饮用水，从中除去添加剂和/或不希望有的杂质以及从溶液中除去存活细菌和病毒。可存在的细菌的浓度范围很宽，包括非常小的浓度。它也可以用于医疗领域(用于从全血或部分血(blood fractions)中除去细菌)，本领域技术人员会发现改性的活性碳纤维的其它功用。

Claims (9)

1.用于纯化液体介质的具有碳基材的改性的活性碳纤维材料，包含活性碳基材以及物理吸附于其上的有机化合物；所述有机化合物包含功能活性基团，选自有机杀菌剂，所述改性的活性碳能将欲从待测溶液中除去的细菌结合和/或杀死。
2.权利要求1的碳材料，其中所述碳基材是通过将含纤维的纤维素碳化和活化得到的。
3.权利要求1的碳纤维材料，其中使用碳纤维，所述碳基材包含直径1.0-10.0微米的碳纤维。
4.权利要求1的碳材料，其中所述吸附在碳基材之上的有机化合物包含至少一种有机杀菌剂。
5.权利要求4的碳材料，其中所述有机芳族杀菌剂是利凡诺、煌绿、呋喃西林和/或青霉素V。
6.生产纯化液体介质用的改性活性碳材料的方法，包括使选自有机杀菌剂的具有功能活性基团的有机化合物在吸附条件下吸附到活性碳基材上，以使有机基团结合到所述碳基材上，这样，所述改性的碳材料能够从所述液体介质中除去不想要的物质。
7.权利要求6的方法，其中所述碳基材通过将纤维素纤维碳化并活化制得。
8.权利要求6的方法，其中所述吸附在0-90℃进行5秒-2小时。
9.权利要求6的方法，其中所述碳材料以碳纤维基材的形式存在，所述碳纤维基材上吸附有多种有机杀菌剂，以对其进行改性，增进其结合和/或杀死不同种类存活细菌的能力。
CN95107587A 1994-07-04 1995-07-04 改性的杀菌活性碳 Pending CN1123700A (zh)

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