CN109603906A - 一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂及其制备方法和应用 - Google Patents
一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种蒽醌‑2‑磺酸钠/氧化石墨烯复合光催化杀菌剂及其制备方法和应用,该复合光催化杀菌剂是在片层氧化石墨烯的表面负载蒽醌‑2‑磺酸钠。本发明的复合光催化杀菌剂具有高效光催化杀菌性能,对水体中的有害微生物具有高效的杀灭效果,在水体净化等领域将具有很好的应用前景。
Description
技术领域
本发明属于光催化领域,具体涉及一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂及其制备方法。
背景技术
由工业发展带来的水体污染日益成为严重的环境威胁之一,水体中的污染物多种多样,包括微生物、金属离子、有机物、染料等。而微生物污染是一个严峻的环境问题,多种细菌可引发各种感染性疾病,威胁到人类健康和经济发展。非抗生素类抗菌物质的研究也因此成为近年来的科学热点,其中纳米抗菌材料的研发则被认为是最有希望克服细菌耐药问题并有实际应用前景的策略。这主要得益于纳米抗菌材料独特的物理化学特性及其固有或通过功能化修饰获得的高效杀菌活性,而这些纳米特性正是常态结构物质所不具备的,为此很多学者甚至提出了“纳米抗生素”的概念。
作为新兴纳米材料,氧化石墨烯(GO)由于超高的比表面体积、优异的平面性、丰富的可修饰功能基团以及良好的生物相容性,成为了抗菌活性物质的理想载体。然而单一氧化石墨烯的抗菌性能是有限的,因此如何提高氧化石墨烯的抗菌活性,使其得到广泛应用,引起了研究者的极大兴趣。蒽醌-2-磺酸钠(AQS)是良好的光敏剂,能够在光线照射下生成羟基自由基和其他活性氧。若能将蒽醌-2-磺酸钠与氧化石墨烯以合适的方法、适当的比例进行复合,或可提高材料的光催化杀菌性能。
发明内容
为避免上述现有技术所存在的不足,本发明公开了一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂及其制备方法和应用,以期可以有效提高氧化石墨烯的光催化杀菌性能。
为实现上述目的,本发明采用如下技术方案:
本发明公开了一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂,其特点在于:所述复合光催化杀菌剂是在片层氧化石墨烯的表面负载蒽醌-2-磺酸钠。
本发明所述蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂的制备方法为:
将片层氧化石墨烯加入去离子水中并超声分散均匀,得到氧化石墨烯分散液;将蒽醌-2-磺酸钠加入到所述氧化石墨分散液中,然后超声分散均匀,获得复合溶液;
对所述复合溶液用去离子水离心、洗涤、冷冻干燥后,即获得蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂。
进一步地,氧化石墨烯分散液的超声时间为10~60min。
进一步地,复合溶液的超声时间为5~20h。
进一步地,所述蒽醌-2-磺酸钠与氧化石墨烯的质量比为1:0.5~2。
本发明还公开了所述蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂的应用,是用于作为光催化杀菌剂,在光照条件下,净化去除水体中的微生物。
与已有技术相比,本发明的有益效果体现在:
1、本发明的复合光催化杀菌剂,是将无机光催化剂氧化石墨烯与光敏剂蒽醌-2-磺酸钠(AQS)进行了有效的复合,在该复合体系中,AQS可以有效降低氧化石墨烯的电子-空穴耦合速率,提高了光照条件下AQS-GO产生活性氧的水平,从而提高其光催化抗菌性能,使其在水体净化等领域具有很好的应用前景。
2、本发明的复合光催化杀菌剂采用简单的物理共混法一步合成,制备工艺简单、易于控制、成本低廉。
3、本发明的复合光催化杀菌剂具有较大的比表面积和良好的可见光吸收性能,有利于其光催化杀菌性能的进一步提高。
4、本发明的复合光催化杀菌剂对水体中的微生物有非常好的净化效果,尤其是对大肠杆菌,其杀灭率可达到99%。
附图说明
图1为本发明制备的GO(图1a)和AQS-GO(图1b)的透射电子显微镜(TEM)图;
图2为本发明制备的AQS-GO的X射线光电子能谱分析(XPS)图;
图3为本发明制备的GO和AQS-GO的拉曼光谱(Raman)图;
图4为本发明制备的GO和AQS-GO的电化学阻抗谱(EIS)图;
图5为本发明制备的GO和AQS-GO在暗处理(GO(D)、AQS-GO(D))和可见光处理(GO(L)、AQS-GO(L))条件下大肠杆菌的存活率图。
具体实施方式
下面对本发明的实施例作详细说明,下述实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
下述实施例所用片层氧化石墨烯按如下方法制得:将2g石墨粉与1g NaNO3粉末加入三口烧瓶中,再加入50mL质量浓度为98%的浓H2SO4,冰水浴下机械搅拌,将6g KMnO4固体颗粒在5℃条件下分批加入三口烧瓶中,加完后升温至35℃搅拌反应24h;反应结束后向反应液中加入100mL去离子水,搅拌混合均匀后再加入250mL去离子水,随后向反应液中滴加15mL 30wt%的双氧水,再加入200mL 1mol/L的HCl溶液,搅拌混合均匀,随后以11000r/min的转速离心,除去上层清液,用水洗涤并离心沉淀物直至pH接近中性;将离心后的沉淀物转移至500mL大烧杯中并加300mL去离子水,超声2h以上,再用4500r/min的转速离心溶液20min,收集离心管上部液体,即为棕色氧化石墨烯溶液,用截留分子量为12000~14000的透析袋透析一周后,再在-50℃下冷冻干燥24~48h,即获得片层氧化石墨烯。
实施例1
本实施例按如下步骤制备蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂:
将0.0030g片层氧化石墨烯(GO)分散于4mL去离子水中,超声30min分散均匀,得到氧化石墨烯分散液;将0.0030g蒽醌-2-磺酸钠(AQS)加入到氧化石墨分散液中,然后超声8h分散均匀,获得复合溶液;对复合溶液用去离子水离心、洗涤,再在-50℃下冷冻干燥24h,即获得蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂(AQS-GO)
图1为本实施例制备的GO(图1a)和AQS-GO(图1b)的透射电子显微镜(TEM)图。从图1a中可以看出,GO具有褶皱的表面,且具有片层结构;从图1b中可以看出,AQS-GO也具有褶皱的表面,且具有片层结构,这说明在AQS-GO的合成过程中,片层结构没有被破坏。
图2为本实施例制备的AQS-GO的X射线光电子能谱分析(XPS)图。从图中可知,AQS-GO的XPS图中有S2p的峰,其中,S2p的峰在168.66V,表明了GO表面负载了AQS。
图3为本实施例制备的GO和AQS-GO的拉曼光谱(Raman)图。从图中可知:GO中D(~1350cm-1)和G(~1591cm-1),ID:IG=0.88;AQS-GO中(D~1350cm-1)和G(~1594cm-1),ID:IG=0.91;比值变化很小,说明AQS的加入并没有对GO的结构造成破坏,并且GO与AQS之间通过π-π相互作用很好的负载在一起。
图4为本实施例制备的GO和AQS-GO的电化学阻抗谱(EIS)图。从图中可以看出纯的GO电化学阻抗曲线具有较宽的半圆弧度,但是在引入AQS后,这种弧度大大降低。表明GO与AQS结合大大的提高复合材料的电子传输性能,这可以有效地抑制光生电子与空穴的耦合,从而有效地提高光催化杀菌性能。
本实施例的蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂应用于水体中,可以对有害微生物进行可见光催化杀灭,以大肠杆菌为例,其光催化杀菌活性的具体测试方法为:
首先将大肠杆菌储存液接种到灭菌LB液体培养基中,然后将其置于37℃、220rpm的恒温摇床中,过夜培养,即得到大肠杆菌的细菌悬浮液。取30mL灭菌的LB液体培养基加入到反应器中,再加入200μL细菌悬浮液,使大肠杆菌浓度为106~8cfu/mL。然后加入光催化杀菌剂,加入量为25μg/mL。加入完成后,采用3W白灯作为光源(波长范围为390~780nm),开始光照,光照过程中间隔一定时间取样,通过平板计数法测定菌落数来计算灭菌率。平板计数法的具体步骤为:取40μL反应液,将其均匀涂抹在LB固体培养基上。然后将培养基倒置,放入生化恒温培养箱中37℃培养,通过计数培养基上长出的菌落个数,以确定细菌的存活率。实验中每组实验均需平行测定3次,取平均值作为最后结果。
为测试光照对其性能的影响,本实施例同时以暗处理的试验结果(以上述光照处理的方法步骤相同,区别仅在于不加光照,在黑暗条件下进行)作为对比。
图5为本实施例制备的GO和AQS-GO在暗处理(GO(D)、AQS-GO(D))和可见光处理(GO(L)、AQS-GO(L))条件下大肠杆菌的存活率图。从图中看出,在可见光照下,AQS-GO复合材料显示出比单体GO更好的光催化活性,在160min光照后,活的大肠杆菌数目已经很少,几乎被完全杀灭,光催化杀菌率达到99%。相比于暗处理条件下,AQS-GO基本无抗菌性,表明光照条件可以大大增强其光催化杀菌性能。
由上可知,本发明的复合光催化杀菌剂对水体中的微生物有非常好的净化效果,使其在水体净化等领域具有很好的应用前景。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂,其特征在于:所述复合光催化杀菌剂是在片层氧化石墨烯的表面负载蒽醌-2-磺酸钠。
2.一种权利要求1所述的蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂的制备方法,其特征在于:
将片层氧化石墨烯加入去离子水中并超声分散均匀,得到氧化石墨烯分散液;将蒽醌-2-磺酸钠加入到所述氧化石墨分散液中,然后超声分散均匀,获得复合溶液;
对所述复合溶液用去离子水离心、洗涤、冷冻干燥后,即获得蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂。
3.根据权利要求2所述的制备方法,其特征在于:氧化石墨烯分散液的超声时间为10~60min。
4.根据权利要求2所述的制备方法,其特征在于:复合溶液的超声时间为5~20h。
5.根据权利要求2所述的制备方法,其特征在于:所述蒽醌-2-磺酸钠与氧化石墨烯的质量比为1:0.5~2。
6.一种权利要求1所述的蒽醌-2-磺酸钠/氧化石墨烯复合光催化杀菌剂的应用,其特征在于:用于作为光催化杀菌剂,在光照条件下,净化去除水体中的微生物。
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