CN107243348B - 一种抑菌性光催化剂的生物辅助合成方法 - Google Patents
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Abstract
本发明公开了一种具有抑菌性能光催化剂的生物辅助合成方法，具体步骤为：将氧化石墨烯和六水合三氯化铁固体按一定质量比配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中200℃加热，反应结束后冷却至室温，所得产物离心，经水和无水乙醇清洗后于60℃真空干燥7h得到RGO/Fe3O4。利用硅烷偶联剂APTES对所得RGO/Fe3O4进行改性。纳米银的负载方法如下，将改性后的RGO/Fe3O4和AgNO3按一定质量比配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中，置于烘箱中120℃下加热，磁性分离所得产品，洗涤并干燥。所得RGO/Fe3O4/Ag表现出良好的抑菌性能，和优异的催化性能。
Description
技术领域
本发明属于光催化剂技术领域，具体涉及一种抑菌性光催化剂的生物辅助合成方法。
背景技术
随着人类社会的进步，工业发展的同时也带来了不可忽视的环境问题，在众多环境问题中，不得不提就是有机染料废水的排放，这些染料大都具有高毒性和致癌性，会对水生生物、动物、植物和人类形成潜在危害，如果得不到有效的治理，将对人类社会造成很大的威胁。已被用于染料废水降解的技术有很多，包括化学方法、物理化学方法、生物方法或者多种联合的方法，例如，活性炭吸附和微生物降解等。以均相Fenton反应为代表的传统水处理办法普遍存在着催化剂难分离等缺点。在此基础上发展起来的Fe3O4作催化剂的非均相Fenton氧化虽利用Fe3O4优异的磁性能很好的解决了分离难、二次污染等问题，但因材料的单一性，依然存在催化效率低、适用pH范围窄等弊端。同时，污水中存在的大量细菌病毒等微生物可成为各类疾病的传播媒介，这一问题在传统的水处理方法中并未得到妥善解决。研究发现，近紫外光和可见光的引入可大大提高Fenton反应的速率，因此Photo-Fenton法得到了广泛的研究，尤其是以碳基磁性纳米抑菌材料为催化剂的非均相Photo-Fenton反应不但能高效剔除废液中的有机染料不造成二次污染，而且低能耗适用pH范围广，同时也能抑制水中各类细菌的生长，有着良好的应用前景和极高的应用价值。虽然，催化剂使用中所产生的环境问题虽已得到有效解决，但催化剂合成过程中因有毒试剂，例如水合肼的使用而带来的环境污染仍不容忽视，而且现有技术中的光催化剂催化效率不高。
发明内容
本发明解决的技术问题是在生物分子海藻酸钠的辅助下，得到了形貌均一的碳基磁性纳米抑菌材料(RGO/Fe3O4/Ag)，并将所得材料进行了抑菌和催化的应用，替换了有毒试剂的使用，提高了催化效率。
本发明为解决上述技术问题采用如下技术方案：
一种抑菌性光催化剂的生物辅助合成方法，包括以下步骤：
(1)将氧化石墨烯和六水合三氯化铁配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中200℃加热20h，反应结束后冷却至室温，所得产物离心、清洗、干燥后得到RGO/Fe3O4纳米复合材料；
(2)取RGO/Fe3O4纳米复合材料置于水和无水乙醇的混合溶液中超声分散，并加入硅烷偶联剂APTES进行改性，室温下搅拌，真空干燥；
(3)纳米银的负载：取改性后的RGO/Fe3O4和AgNO3配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中200℃加热8h，反应结束后冷却至室温，所得产物离心、清洗、干燥后得到所述抑菌性光催化剂RGO/Fe3O4/Ag；
所述氧化石墨烯和六水合三氯化铁质量比为1∶15-20，尿素和海藻酸钠的质量比为2-4∶1。
所述的制备RGO/Fe3O4纳米复合材料时，所述的水的用量为20-40mL，反应釜为20-80mL的聚四氟乙烯不锈钢反应釜。
所述的制备RGO/Fe3O4纳米复合材料时，所述的清洗为将离心的产物经水和无水乙醇交替清洗6次，所述的干燥为于60℃真空干燥7h。
所述的进行RGO/Fe3O4纳米复合材料改性时，所述的水和无水乙醇体积比为1∶1，室温下搅拌7h，所述的干燥为于60℃真空干燥7h。
所述的进行纳米银的负载时，RGO/Fe3O4和AgNO3的比例为8∶8-13，尿素和海藻酸钠的质量比为2-4∶1，所述的水的用量为20-40mL，反应釜为20-80mL的聚四氟乙烯不锈钢反应釜。
所述的进行纳米银的负载时，所述的清洗为将离心的产物经水和无水乙醇交替清洗6次，所述的干燥为于60℃真空干燥7h。
本发明合成条件易控，操作方便，环境友好，具有合成设备简单，原料常见易得，反应快速高效和产品的催化效率较高等优点，对抑菌性催化剂的开发有着重要的指导意义。
附图说明
图1是本发明实施例1制得的氧化石墨烯(GO)，Fe3O4，RGO/Fe3O4和RGO/Fe3O4/Ag的XRD图谱。
图2是本发明实施例1制得RGO/Fe3O4/Ag的透射电镜图谱。
图3是本发明在抑菌应用中的效果图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
图1是本实施例制得纳米复合材料的XRD图谱，上到下依次是氧化石墨烯(GO)，Fe3O4，RGO/Fe3O4和RGO/Fe3O4/Ag的XRD图谱，最下方为Fe3O4标准图谱(JCPDS card No.65-3107)和Ag的标准图谱(JCPDS card No.65-2871)。其中GO在2θ＝10.8°处出现的衍射峰对应(001)晶面，而从GO到RGO/Fe3O4和RGO/Fe3O4/Ag，(001)晶面特征峰的消失意味着GO在一定程度上已被生物分子海藻酸钠还原。RGO/Fe3O4和Fe3O4拥有相同位置的衍射峰，并且能准确对应图中最下方的Fe3O4标准图谱(JCPDS card No.65-3107)，RGO/Fe3O4/Ag图谱中在角度为38°和44°左右出现的衍射峰对应Ag的标准图谱(JCPDS card No.65-2871)中的(111)晶面和(200)晶面，其余的衍射峰均能与Fe3O4标准图谱(JCPDS card No.65-3107)准确照应，说明无论是Fe3O4还是Ag都是独立存在的并未生成合金，且Ag的负载并未改变Fe3O4的晶相。
图2是本实施例制得RGO/Fe3O4/Ag的透射电镜图，其中由(a)、(b)可以看出，石墨烯片层结构清晰可见，Fe3O4和Ag纳米颗粒的形状较为规则，分散性良好，颗粒的尺寸分布在10nm～20nm之间。(c)和(d)图分别是样品RGO/Fe3O4/Ag的选区衍射与晶格条纹。根据此样品XRD图谱，在衍射图中找到了Fe3O4的(311)、(200)、(111)晶面和Ag的(200)、(111)晶面，在晶格条纹图中找出了两种晶格条纹，晶格间距分别为0.210nm和0.200nm，对应Fe3O4的(400)晶面和Ag的(200)晶面。
在抑菌实验中的方法为：应用在样品中放入50μL细菌后，在37℃环境中存放24h。取100μL培养后的细菌放入到900μL无菌生理盐水(试管1)中，混合均匀，取管1中100μL菌液再次放入到另一支900μL无菌生理盐水(试管2)中，重复操作一直到试管6，也就意味着稀释106倍，取稀释后菌悬液20μL置于固体培养基上，均匀涂抹一直到其表面干燥，把它在37℃环境中存放24h后，查看菌落生长情况。
图3是本发明所得纳米复合材料的抑菌效果图，以苏云金芽孢杆菌为例，(a)为空白，有223个菌落；(b)是0.7mg/mL实验所得纳米Ag溶液涂抹后的效果，有56个菌落，抑菌率74.8％；(c)为0.6mg/mL所得RGO/Fe3O4/Ag溶液涂抹后的效果，菌落数11，抑菌率95.1％；(d)为0.7mg/mL所得RGO/Fe3O4/Ag溶液涂抹后的效果，没有菌落生长，抑菌率100％，由此推测RGO/Fe3O4/Ag对苏云金芽孢杆菌的最小抑菌浓度为0.7mg/mL。由于石墨烯能让纳米颗粒有效分散且复合材料中存在协同作用，因此所得复合材料有着比纳米银更突出的抑菌性能。
应用在室温25℃，控制时间为60min，双氧水起始浓度为10.0mmol·L-1，亚甲基蓝的起始浓度为20mg·L-1，RGO/Fe3O4/Ag投加量为0.25g·L-1的条件下，调节溶液起始pH为6的实验条件下探究所得材料在Photo-Fenton体系催化降解亚甲基蓝实验中的催化性能。实验结果表明，60min后最高能达到95％的降解率，且多次循环使用降解率并无明显下降，在实际水样中使用时也同样能保持良好的催化性能，有着很高的应用价值和优秀的应用前景。
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (7)
1.一种抑菌性光催化剂的生物辅助合成方法，其特征在于，包括以下步骤：
(1)将氧化石墨烯和六水合三氯化铁配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中200℃加热20h，反应结束后冷却至室温，所得产物离心、清洗、干燥后得到RGO/Fe3O4纳米复合材料；
(2)取RGO/Fe3O4纳米复合材料置于水和无水乙醇的混合溶液中超声分散，并加入硅烷偶联剂APTES进行改性，室温下搅拌，真空干燥；
(3)纳米银的负载：取改性后的RGO/Fe3O4和AgNO3配成水溶液，加入尿素和海藻酸钠，随后转移至反应釜中200℃加热8h，反应结束后冷却至室温，所得产物离心、清洗、干燥后得到所述抑菌性光催化剂RGO/Fe3O4/Ag。
2.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法，其特征在于：所述步骤(1)中合成RGO/Fe3O4纳米复合材料时氧化石墨烯和六水合三氯化铁质量比为1:15-20，尿素和海藻酸钠的质量比为2-4:1。
3.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法，其特征在于：制备RGO/Fe3O4纳米复合材料时，所述步骤(1)中将氧化石墨烯和六水合三氯化铁配成水溶液时水的用量为20-40mL，反应釜为20-80mL的聚四氟乙烯不锈钢反应釜。
4.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法其特征在于：制备RGO/Fe3O4纳米复合材料时，所述的清洗为将离心的产物经水和无水乙醇交替清洗6次，所述的干燥为于60℃真空干燥7h。
5.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法，其特征在于：步骤(2 )中进行RGO/Fe3O4纳米复合材料改性时，所述配置水和无水乙醇混合溶液时水和无水乙醇体积比为1:1，加入硅烷偶联剂APTES后混合溶液室温下搅拌7h，所述的干燥为于60℃真空干燥7h。
6.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法，其特征在于：进行纳米银的负载时，RGO/Fe3O4和AgNO3的比例为8:8-13，尿素和海藻酸钠的质量比为2-4:1，步骤(3)中改性后的RGO/Fe3O4和AgNO3配成水溶液时水的用量为20-40mL，反应釜为20-80mL的聚四氟乙烯不锈钢反应釜。
7.根据权利要求1所述的一种抑菌性光催化剂的生物辅助合成方法，其特征在于：进行纳米银的负载时，所述的清洗为将离心的产物经水和无水乙醇交替清洗6次，所述的干燥为于60℃真空干燥7h。
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