CN110038557A - 一种电催化GOx/MnCO3复合材料及其制备和应用 - Google Patents
一种电催化GOx/MnCO3复合材料及其制备和应用 Download PDFInfo
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- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 12
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- 239000011702 manganese sulphate Substances 0.000 claims description 10
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
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- 235000006748 manganese carbonate Nutrition 0.000 description 1
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- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
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- B01J23/32—Manganese, technetium or rhenium
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Abstract
本发明属于材料催化领域，具有设计一种电催化GOx/MnCO3复合材料及其制备和在防污中的应用。本发明GOx/MnCO3复合材料通过一步共沉淀法制备的，制备得到的材料呈现出氧化石墨烯气凝胶(GO,1wt％)均匀的包裹在MnCO3方块的表面，结构规整，具有良好的杀菌防污性能。该材料对于海水环境中的建筑设施具有很好的应用价值。
Description
技术领域
本发明属于材料催化领域，具有设计一种电催化GOx/MnCO3复合材料及其制备和在防污中的应用。
背景技术
电催化产活性氧的电极材料及其机理已经被广泛研究，特别是锰氧化物电极催化材料已经发展得比较成熟，其它的电催化材料包括硼掺杂的金刚石电极、纳米金属颗粒等在燃料电池氧还原研究、电化学高级氧化废水有机物和光电化学氧化消毒技术研究等方面有着很多的研究应用。电催化材料在电化学氧化技术中应用于水体消毒等方面已经有广泛研究，但在海水的生物污损防护技术方面的研究仍明显不足。因此，可以结合海洋电化学防污的特点和需求，开展新型导电防污材料在海洋防污领域的研究十分重要。
发明内容
针对上述电催化材料在海洋防污中应用问题，本发明目的在于提供一种电催化GOx/MnCO3复合材料及其制备和在防污中的应用。
为实现上述目的，本发明采取以下技术方案为：
一种电催化GOx/MnCO3复合材料，GOx/MnCO3为GO均匀包覆在MnCO3纳米材料表面，形成3-5nm厚度的氧化石墨烯包覆的MnCO3纳米材料，即GOx/MnCO3；其中，x＝0.05-1；优选为x＝0.05-0.5。
一种电催化GOx/MnCO3复合材料的制备，将GO与MnCO3方块纳米材料，按质量比例值为0.05-1混合，而后溶于过量的去离子水中，在超声清洗仪中，超声混合30-50min，即得到GOx/MnCO3复合材料。
所述MnCO3方块纳米为：通过一步共沉淀法将硫酸锰溶于含聚乙烯吡咯烷酮的溶液中，通过加入碳酸氢钠进行沉淀反应，反应持续搅拌下沉淀10-15h，将反应后的溶液洗涤干燥得到结构为规则的立方体的MnCO3材料。
所述溶液为水和无水乙醇，水和无水乙醇体积比为1:0-0:1；
所述含聚乙烯吡咯烷酮的溶液中聚乙烯吡咯烷酮的终浓度为15-25mg/mL。
所述硫酸锰溶于含聚乙烯吡咯烷酮的溶液中的终浓度为6-8mM；
所述碳酸氢钠与硫酸锰的质量比为10:1-50：1。
一种电催化GOx/MnCO3复合材料的应用，所述电催化GOx/MnCO3复合材料在生物污损防护中的应用。
本发明的有益效果在于：
本发明将具有良好导电性和催化活性的氧化石墨烯气凝胶和具有强的催化产生活性氧的碳酸锰纳米材料复合，进而增加其材料的电催化产生活性氧的性能，使其能在模拟海水中具有较强的抗菌防污性能。
本发明通过简单的共沉淀超声的方法合成GOx/MnCO3电催化复合材料，可用于模拟海水中设施的防护，绿色无二次污染，对于海洋设施的污损防污具有重要的意义，具体在于：
(1)将电催化材料引入到海洋污损生物防护上，扩宽了生物污损防护的技术方法。
(2)电催化防污损生物方法，可降低防护成本，应用的范围广。
附图说明
图1为本发明实施例提供的MnCO3(a)与GOx/MnCO3(b)复合材料的扫描电镜(SEM)照片。
图2为本发明实施例提供的电催化GOx/MnCO3复合材料在防污中应用的照片，其中，(a)碳钢没有修饰催化剂进行阴极极化后的荧光照片，(b)碳钢修饰催化剂进行阴极极化后的荧光照片。
具体实施方式
以下通过具体的实施例对本发明作进一步说明，有助于本领域的普通技术人员更全面的理解本发明，但不以任何方式限制本发明。
本发明GOx/MnCO3复合材料通过一步共沉淀法制备的，制备得到的材料呈现出氧化石墨烯气凝胶(GO,1wt％)均匀的包裹在MnCO3方块的表面，结构规整，具有良好的杀菌防污性能。该材料对于海水环境中的建筑设施具有很好的应用价值。
实施例1：
0.6g的聚乙烯吡咯烷酮溶于30mL无水乙醇和10mL去离子水的混合溶剂中，然后，向上述溶液中加入0.045g的硫酸锰，室温搅拌45分钟，得到溶液A。将0.35g的碳酸氢钠溶于10mL离子水中，得到溶液B。将B溶液在搅拌的条件下滴加到溶液B中，持续搅拌15h。反应完成后，将溶液进行抽滤，并分别用去离子水和无水乙醇洗涤数次。最后得到的样品于60℃真空干燥箱中过夜干燥。得到样品的形貌图和如图1a一样，MnCO3为规则的为方块状纳米结构。
实施例2：
0.6g的聚乙烯吡咯烷酮溶于30mL无水乙醇和10mL去离子水的混合溶剂中，然后，向上述溶液中加入0.045g的硫酸锰，室温搅拌45分钟，得到溶液A。将0.35g的碳酸氢钠溶于10mL离子水中，得到溶液B。将B溶液在搅拌的条件下滴加到溶液B中，持续搅拌12h。反应完成后，将溶液进行抽滤，并分别用去离子水和无水乙醇洗涤数次。最后得到的样品于60℃真空干燥箱中过夜干燥。得到样品如图1a所示，MnCO3为方块状的纳米结构。
将合成的MnCO3纳米方块与GO按质量比1:0.2，溶于去离子水中，在超声清洗仪中，超声混合30min。得到GO0.2/MnCO3复合材料的溶液，如图1b所示。图1b表明GO薄层均匀的包裹着方块状的MnCO3，这种结构不仅有利于增加MnCO3的导电性，又能防止MnCO3在溶液中降解，增加了其稳定性。
实施例3：
0.6g的聚乙烯吡咯烷酮溶于30mL无水乙醇和10mL去离子水的混合溶剂中，然后，向上述溶液中加入0.045g的硫酸锰，室温搅拌45分钟，得到溶液A。将0.35g的碳酸氢钠溶于10mL离子水中，得到溶液B。将B溶液在搅拌的条件下滴加到溶液B中，持续搅拌12h。反应完成后，将溶液进行抽滤，并分别用去离子水和无水乙醇洗涤数次。最后得到的样品于60℃真空干燥箱中过夜干燥。得到样品如图1a所示，MnCO3为方块状的纳米结构。
将合成的MnCO3纳米方块与GO按质量比1:0.1，溶于去离子水中，在超声清洗仪中，超声混合30min。得到GO0.1/MnCO3复合材料的溶液。随着GO量的减少，相对于图1b，GO包覆方块状的MnCO3的层数减少。对防止MnCO3在溶液中降解作用减弱，稳定性相应减弱。
实施例4：
0.6g的聚乙烯吡咯烷酮溶于30mL无水乙醇和10mL去离子水的混合溶剂中，然后，向上述溶液中加入0.045g的硫酸锰，室温搅拌45分钟，得到溶液A。将0.35g的碳酸氢钠溶于10mL离子水中，得到溶液B。将B溶液在搅拌的条件下滴加到溶液B中，持续搅拌12h。反应完成后，将溶液进行抽滤，并分别用去离子水和无水乙醇洗涤数次。最后得到的样品于60℃真空干燥箱中过夜干燥。得到样品如图1a所示，MnCO3为方块状的纳米结构。
将合成的MnCO3纳米方块与GO按质量比1:0.05，溶于去离子水中，在超声清洗仪中，超声混合30min。得到GO0.05/MnCO3复合材料的溶液。随着GO量进一步减少，相对于图1b，GO包覆方块状的MnCO3的层数变的稀薄。使得防止MnCO3降解能力变差，稳定性相应变差。
应用例：
首先准备细菌悬液，将大肠杆菌储存液接种到灭菌的LB培养基中，然后将其置于37℃、150rpm的恒温摇床中，过夜培养。培养得到的细菌悬液离心后分散于3.5％的NaCl中，溶液用3.5％的NaCl作为模拟海水，得到浓度为1.0×108cfu/mL的大肠杆菌悬液。
以上述实施例2合成的GOx/MnCO3复合材料为例，将其修饰在海洋设施常用材料碳钢表面，而以无GOx/MnCO3复合材料修饰的碳钢作为空白对照。取上述细菌浓度为1.0×108cfu/mL的悬液100mL作为电解质溶液，然后分别对两种不同处理的碳钢进行阴极极化4h，极化电压为-0.2V，通过荧光显微镜观察碳钢表面大肠杆菌的附着量。结果如图2所示。从图2a空白对照图中可以明显看出，即碳钢没有修饰催化剂进行阴极极化后的，碳钢表面生物的附着量较多。而进行电催化材料修饰并进行阴极极化后，碳钢材料表面生物的附着量很少，如图2b所示。
同时，上述的复合材料由其它实施例合成的GOx/MnCO3复合材料进行替换，复合材料均为包覆结构，而这种结构不仅有利于增加MnCO3的导电性，又能防止MnCO3在溶液中降解，进而增加了其催化性能，均能得到相应的杀菌效果，使得碳钢表面没有细菌的浮着，或附着量很少。
Claims (6)
1.一种电催化GOx/MnCO3复合材料，其特征在于：GOx/MnCO3为GO均匀包覆在MnCO3纳米材料表面，形成3-5nm厚度的氧化石墨烯包覆的MnCO3纳米材料，即GOx/MnCO3；其中，x＝0.05-1。
2.一种权利要求1所述的电催化GOx/MnCO3复合材料的制备，其特征在于：将GO与MnCO3方块纳米材料，按质量比例值为0.05-1混合，而后溶于过量的去离子水中，在超声清洗仪中，超声混合30-50min，即得到GOx/MnCO3复合材料。
3.按权利要求2所述的电催化GOx/MnCO3复合材料的制备，其特征在于：所述MnCO3方块纳米为：通过一步共沉淀法将硫酸锰溶于含聚乙烯吡咯烷酮的溶液中，通过加入碳酸氢钠进行沉淀反应，反应持续搅拌下沉淀10-15h，将反应后的溶液洗涤干燥得到结构为规则的立方体的MnCO3材料。
4.按权利要求3所述的电催化GOx/MnCO3复合材料的制备，其特征在于：所述溶液为水和无水乙醇，水和无水乙醇体积比为1:0-0:1；
所述含聚乙烯吡咯烷酮的溶液中聚乙烯吡咯烷酮的终浓度为15-25mg/mL。
5.按权利要求3所述的电催化GOx/MnCO3复合材料的制备，其特征在于：所述硫酸锰溶于含聚乙烯吡咯烷酮的溶液中的终浓度为6-8mM；
所述碳酸氢钠与硫酸锰的质量比为10:1-50：1。
6.一种权利要求1所述的电催化GOx/MnCO3复合材料的应用，其特征在于：所述电催化GOx/MnCO3复合材料在生物污损防护中的应用。
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