CN116212921A - 一种g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂及其制备方法和应用 - Google Patents
一种g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于抗菌材料技术领域,具体涉及一种g‑C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂及其制备方法和应用。制备过程中采用简单的La3+刻蚀ZIF‑67一步衍生LaCoO3/Co3O4纳米复合材料,并采用湿法浸渍法合成LaCoO3/Co3O4/g‑C3N4三元纳米复合光响应抗菌剂,以g‑C3N4纳米薄片为载体,将La3+刻蚀ZIF‑67衍生LaCoO3/Co3O4纳米复合材料与之相结合,进而形成三元异质结。本发明所制备的三元纳米复合材料具有优异的紫外光和可见光响应性、载流子传输和抗菌性能。在环境污染和生物医疗方面也具有潜在的应用。
Description
技术领域
本发明属于抗菌材料技术领域,具体涉及一种g-C3N4/LaCoO3/Co3O4三元纳米抗菌剂及其制备方法和应用。
背景技术
在当今生活中,细菌感染已成为威胁人类生命健康的主要问题。大肠杆菌(E.coli)和金黄色葡萄球菌(S.aureus)是引起伤口感染和疾病的主要致病菌。抗生素的研发和使用是一种处理细菌感染问题的有效方法,但是抗生素的长期使用致使细菌产生强的耐药性,并导致多重耐药病原体的出现和传播。因此,迫切需要开发一种新型、安全、高效的抗菌剂。近年来,随着纳米技术的发展,许多基于纳米材料的抗菌剂被开发并广泛应用于环保、医疗保健、抗菌材料等领域。
目前为止,大量的研究都集中在金属-有机框架(MOF)衍生物方面,如金属合金,过渡金属氧化物和层状双氢氧化物等。特别是,沸石咪唑酯骨架-67(ZIF-67)由于其具有一定的稳定性、结构设计简单、合成方便而受到广泛关注。在各种ZIF-67的衍生物中,过渡金属氧化物是最受欢迎的候选者。例如,ZIF-67衍生制备的Co/CoO复合材料;ZIF-67通过简单的一步煅烧法衍生尖晶石金属氧化物(AB2O4)。然而,对于MOF衍生的钙钛矿氧化物在抗菌领域的研究还鲜见报道。
通常钙钛矿氧化物具有典型的ABO3式,包括A位的稀土或碱金属离子和B位的过渡金属离子。受益于特定的混合离子电子电导率和结构缺陷,钙钛矿氧化物在多个领域受到了极大的关注,如电磁、电源和环境保护等。LaCoO3钙钛矿氧化物因具有相对适中的禁带宽度,可与其它金属或非金属半导体、金属粒子相结合形成异质结结构来提高光响应强度,抑制电子空穴易复合等问题,成为近年来研究比较热的光催化材料。然而,基于ZIF-67衍生钴酸镧(LaCoO3)钙钛矿且应用于抗菌方面的研究少之又少。
石墨相氮化碳(g-C3N4)是一种具有类似于石墨烯结构的聚合物半导体,其中C和N原子均通过sp2杂化形成芳香族C-N六元杂环,且在二维网络结构中具有高度离域的π电子共轭体系。由于不完全缩聚,还可能有少量的H杂质以片层边缘上的伯胺或仲胺基团(如CNH2、C2NH)的形式存在。另外,因其刚性C-N杂环网络结构、高度共轭的体系和较高的缩合度,g-C3N4的稳定性极佳,耐热温度高达600℃,是所有有机材料中最高的。此外,g-C3N4还具有良好的化学稳定性,它不溶于水、大多数酸、碱和各种有机溶剂。因此,将其与其它半导体复合可进一步增强载流子的传输效率。
发明内容
本发明的目的在于提供一种g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂及其制备方法和应用,采用简单的La3+刻蚀法刻蚀ZIF-67一步衍生出LaCoO3/Co3O4纳米复合材料,改善单一材料的载流子易复合的问题,并将其与g-C3N4复合而达到进一步增强载流子传输能力,从而提高纳米复合材料的抗菌活性,形成一种具有良好生物相容性和优异的光响应性三元纳米复合材料。
为了实现上述目的,本发明采用以下技术方案予以实现:
一种g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂的制备方法,包括以下步骤:
步骤一:称取六水合硝酸钴Co(NO)2·6H2O和2-甲基咪唑C4H6N2分别加入到20~50mL的甲醇中搅拌30min后,所述六水合硝酸钴Co(NO)2·6H2O和2-甲基咪唑C4H6N2的摩尔比为1:4,将两种溶液混合搅拌,并在室温条件静置;将静置后的溶液用无水乙醇离心、洗涤3次;然后将收集的紫色沉淀物在50℃下干燥12h获得ZIF-67十二面体纳米材料;
步骤二:首先,将ZIF-67分散在无水乙醇和去离子水混合溶液中超声15min,并搅拌30min,无水乙醇与去离子水的摩尔比为1:0~1;随后,在上述混合溶液中加入六水合硝酸镧La(NO3)3·6H2O,所述ZIF-67与La(NO3)3·6H2O的质量比为1:0.5~2,并在磁力搅拌器下持续搅拌,待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末,煅烧处理后,可得LaCoO3/Co3O4纳米材料;
步骤三:称取上述制备好的LaCoO3/Co3O4纳米材料和双氰胺经马弗炉两次500℃下煅烧所得的g-C3N4纳米片,所述LaCoO3/Co3O4与g-C3N4的质量比为1:0.1~2,分别分散在一定量的甲醇溶液中并超声处理1h;接着,将制备好的LaCoO3/Co3O4溶液和g-C3N4溶液进行混合,并在通风橱中使用磁力搅拌器持续搅拌直到甲醇完全挥发;将所得到的黑色固体收集后在80℃烘箱中干燥12h,得到LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂。
进一步地,所述步骤二中采用马弗炉在为500℃~900℃的煅烧温度下保温2~5h。
如上述任一种制备方法制得的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂。
进一步地,LaCoO3/Co3O4纳米颗粒均匀负载在g-C3N4纳米薄片上。
进一步地,LaCoO3/Co3O4纳米颗粒的粒径为10~30nm。
如上述任一种的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂在环境污染和生物医疗方面的应用。
与现有技术相比,本发明具有如下有益效果:
1.有效抑制了单一材料光生电子-空穴对易复合的问题;同时利用优异可见光响应的g-C3N4纳米薄片进一步扩宽了纳米复合材料的光响应性,提高了纳米复合材料的氧化还原能力,实现了优异的抗菌性能。
2.本发明所制备的纳米复合抗菌剂安全环保、耐药性强。
3.采用本发明所制备的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂,其对大肠杆菌和金黄色葡萄球菌的最小抑菌浓度(MIC)分别为0.8mg/mL和0.9mg/mL;此外,1mg/mL该纳米复合材料在紫外灯下照射20min,对大肠杆菌和金黄色葡萄球菌的抑菌率可分别达到99.7%、96.28%;1mg/mL该材料在可见光灯下照射20min,对大肠杆菌和金黄色葡萄球菌的抑菌率可分别达到99.6%、95.66%。
附图说明
图1从上至下依次为实施例1制备的g-C3N4负载ZIF-67衍生的LaCoO3/Co3O4三元纳米复合抗菌剂(LaCoO3/Co3O4/g-C3N4)、对比例1制备的ZIF-67衍生的Co3O4、对比例1制备的La3+/ZIF-67衍生的LaCoO3/Co3O4二元纳米复合抗菌剂XRD图谱;
图2为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的TEM照片;
图3为ZIF-67衍生的Co3O4、La3+刻蚀ZIF-67衍生的LaCoO3/Co3O4纳米颗粒、LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的瞬态光电流测试结果;
图4为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对大肠杆菌的抑菌浓度测试结果;
图5为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对金黄色葡萄球菌的抑菌浓度测试结果;
图6为未处理大肠杆菌的菌落生长照片及紫外光下LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂处理后大肠杆菌的菌落生长照片;
图7为未处理金黄色葡萄球的菌落生长照片及紫外光下LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂处理后金黄色葡萄球菌的菌落生长照片;
图8为未处理大肠杆菌的菌落生长照片及可见光下LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂处理后大肠杆菌的菌落生长照片;
图9为未处理金黄色葡萄球的菌落生长照片及可见光下LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂处理后金黄色葡萄球菌的菌落生长照片;
具体实施方式
以下结合实施例对本发明的具体内容做进一步详细解释说明。
本发明采用简单的La3+刻蚀ZIF-67一步衍生LaCoO3/Co3O4纳米复合材料并采用湿法浸渍法合成LaCoO3/Co3O4/g-C3N4三元纳米复抗菌剂,制备的过程中以g-C3N4纳米薄片为载体,将La3+刻蚀ZIF-67衍生LaCoO3/Co3O4纳米复合材料与之相结合,进而形成三元异质结,有效抑制了单一材料光生电子和空穴对易复合的问题;同时具有优异可见光响应的g-C3N4纳米薄片能够进一步扩宽纳米复合材料的光响应性,提高纳米复合材料的氧化还原能力,实现优异的抗菌性能。进一步的,LaCoO3/Co3O4/g-C3N4三元纳米复合光响应抗菌剂能够有效增强纳米复合材料对于载流子的迁移能力。在可见光和紫外光下,LaCoO3/Co3O4/g-C3N4三元纳米复合光响应抗菌剂能够产生大量的超氧阴离子(·O2 -)和羟基自由基(·OH),这些活性物质能够诱导细菌细胞膜脂质过氧化、增加细菌细胞膜的通透性,致使细菌内部的酶蛋白失活变性。最终,造成细菌不可逆的损伤,从而达到杀死细菌的目的。因此,采用简单的La3+刻蚀法一步衍生出LaCoO3/Co3O4纳米复合材料,改善单一材料的载流子易复合的问题,并将其与g-C3N4复合而达到进一步增强载流子传输能力,从而提高纳米复合材料的抗菌活性,形成一种具有良好生物相容性和优异的光响应性三元纳米复合材料;
实施例1
步骤一:称取2.42g六水合硝酸钴Co(NO)2·6H2O和2.732g 2-甲基咪唑C4H6N2分别加入到20mL的甲醇中搅拌30min后,将两种溶液混合搅拌,并在室温条件静置12h;将静置后的溶液用无水乙醇离心、洗涤3次;收集的紫色沉淀物在50℃下干燥12h,获得ZIF-67十二面体纳米材料。
步骤二:首先,将ZIF-67分散在摩尔比为1:1的无水乙醇和去离子水混合溶液中超声15min,并搅拌30min;随后,在上述混合溶液中加入0.1g六水合硝酸镧La(NO3)3·6H2O并在磁力搅拌器下持续搅拌。待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末在700℃煅烧处理3h,可得到LaCoO3/Co3O4纳米材料。
步骤三:称取适量上述制备好的0.1g LaCoO3/Co3O4纳米材料和0.1gg-C3N4纳米片,双氰胺经马弗炉两次煅烧,分别分散在一定量的甲醇溶液中并超声处理1h;接着,将制备好的LaCoO3/Co3O4溶液和g-C3N4溶液进行混合,并在通风橱中使用磁力搅拌器持续搅拌直到甲醇完全挥发;将所得到的黑色固体收集后在80℃烘箱中干燥12h,得到LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂。
实施例2
步骤一:称取0.58g六水合硝酸钴Co(NO)2·6H2O和0.64g 2-甲基咪唑C4H6N2分别加入到50mL的甲醇中搅拌30min后,将两种溶液混合搅拌,并在室温条件静置12h;将静置后的溶液用无水乙醇离心、洗涤3次;收集的紫色沉淀物在50℃下干燥12h获得ZIF-67十二面体纳米材料。
步骤二:首先,将ZIF-67分散在摩尔比为1:2的无水乙醇和去离子水混合溶液中超声15min,并搅拌30min;随后,在上述混合溶液中加入0.2g六水合硝酸镧La(NO3)3·6H2O并在磁力搅拌器下持续搅拌。待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末在800℃煅烧处理2h,可得到LaCoO3/Co3O4纳米材料。
步骤三:称取适量上述制备好的0.1g LaCoO3/Co3O4纳米材料和0.05gg-C3N4纳米片,双氰胺经马弗炉两次煅烧,分别分散在一定量的甲醇溶液中并超声处理1h;接着,将制备好的LaCoO3/Co3O4溶液和g-C3N4溶液进行混合,并在通风橱中使用磁力搅拌器持续搅拌直到甲醇完全挥发;将所得到的黑色固体收集后在80℃烘箱中干燥12h,得到LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂。
实施例3
步骤一:称取2.42g六水合硝酸钴Co(NO)2·6H2O和2.732g 2-甲基咪唑C4H6N2分别加入到50mL的甲醇中搅拌30min后,将两种溶液混合搅拌,并在室温条件静置12h;将静置后的溶液用无水乙醇离心、洗涤3次;收集的紫色沉淀物在50℃下干燥12h,获得ZIF-67十二面体纳米材料。
步骤二:首先,将ZIF-67分散在摩尔比为1:0.5的无水乙醇和去离子水混合溶液中超声15min,并搅拌30min;随后,在上述混合溶液中加入0.3g六水合硝酸镧La(NO3)3·6H2O并在磁力搅拌器下持续搅拌。待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末在600℃煅烧处理5h,可得到LaCoO3/Co3O4纳米材料。
步骤三:称取适量上述制备好的0.1g LaCoO3/Co3O4纳米材料和0.2gg-C3N4纳米片,双氰胺经马弗炉两次煅烧,分别分散在一定量的甲醇溶液中并超声处理1h;接着,制备好的LaCoO3/Co3O4溶液和g-C3N4溶液进行混合,并在通风橱中使用磁力搅拌器持续搅拌直到甲醇完全挥发;将所得到的黑色固体收集后在80℃烘箱中干燥12h,得到LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂。
对比例1
步骤一:称取2.42g六水合硝酸钴(Co(NO)2·6H2O)和2.732g 2-甲基咪唑(C4H6N2)分别加入到50mL的甲醇中搅拌30min后,将两种溶液混合搅拌,并在室温条件静置12h;将静置后的溶液用无水乙醇离心、洗涤3次;收集的紫色沉淀物在50℃下干燥12h,获得ZIF-67十二面体纳米材料并将其放置在700℃下煅烧处理2h可得到Co3O4纳米材料。
对比例2
步骤一:称取2.42g六水合硝酸钴Co(NO)2·6H2O和2.732g 2-甲基咪唑C4H6N2分别加入到50mL的甲醇中搅拌30min后,将两种溶液混合搅拌,并在室温条件静置12h;将静置后的溶液用无水乙醇离心、洗涤3次;收集的紫色沉淀物在50℃下干燥12h,获得ZIF-67十二面体纳米材料。
步骤二:首先,将ZIF-67分散在摩尔比为1:1的无水乙醇和去离子水混合溶液中超声15min,并搅拌30min;随后,在上述混合溶液中加入0.2g六水合硝酸镧La(NO3)3·6H2O并在磁力搅拌器下持续搅拌。待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末在700℃煅烧处理2h,可得到LaCoO3/Co3O4纳米材料。
图1至图9为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的表征结果。图1从下至上依次为对比例1制备的Co3O4纳米抗菌剂、对比例2制备的LaCoO3/Co3O4纳米复合抗菌剂、实施例1制备的LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂的XRD图谱;图1中ZIF-67衍生物(Co3O4)及其La3+刻蚀ZIF-67衍生物(LaCoO3/Co3O4)图谱都清晰的显示出了Co3O4衍射峰与标准的尖晶石四氧化三钴(JCPDS 43-1003)相匹配,同时经La3+刻蚀ZIF-67衍生物也表现出了标准的菱方相钴酸镧衍射峰(JCPDS 48-0123)。另外,衍生的LaCoO3/Co3O4纳米复合材料与g-C3N4纳米薄片复合后,出现了一个小峰,其属于g-C3N4纳米薄片的(002)晶面,表明LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的成功制备。
图2为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的TEM照片;从图2中可以看出,其衍生的LaCoO3/Co3O4纳米复合材料呈现颗粒状且均匀地分散在g-C3N4纳米薄片上,其颗粒尺寸分布范围为10~30nm。g-C3N4呈现纳米薄片而非块状结构等,薄的纳米片有利于LaCoO3/Co3O4纳米复合材料的负载,解决了颗粒易团聚的问题。测试结果进一步表明了LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的成功制备。
图3为ZIF-67衍生的Co3O4、La3+刻蚀ZIF-67衍生的LaCoO3/Co3O4纳米颗粒、LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的瞬态光电流测试结果;在图3中,衍生物Co3O4纳米颗粒表现出一般的光生载流子迁移效率,而经La3+刻蚀ZIF-67衍生的LaCoO3/Co3O4纳米颗粒表现出更加稳定的载流子传输效率。而LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂表现出更加稳定的载流子传输效率和优异的光电流强度。结合半导体能带理论可知,半导体异质结结构可有效抑制光生电子-空穴的复合、加速光生电子-空穴的转移,因而三元纳米复合抗菌剂表现出优异的载流子迁移效率,可改善材料表面的氧化还原反应,进而提高其抗菌性能。
图4为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对大肠杆菌的抑菌浓度测试结果;在图4中,LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂的浓度为0.8mg/mL时,对大肠杆菌表现出明显的抑制作用,即其对大肠杆菌的MIC为0.8mg/mL。图5为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对金黄色葡萄球菌的抑菌浓度测试结果;从图5可以发现LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对金黄色葡萄球菌的MIC为0.9mg/mL。LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂对金黄色葡萄球菌的最小抑菌浓度略高于大肠杆菌的最小抑菌浓度,这是因为金黄色葡萄球菌的细胞壁较厚导致的。
图6和图7分别为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂经紫外光照射后对大肠杆菌和金黄色葡萄球菌的抗菌效果;图8和图9分别为LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂经可见光照射后对大肠杆菌和金黄色葡萄球菌的抗菌效果;从图中可以看到,未处理大肠杆菌和金黄色葡萄球菌的菌落生长良好,而在紫外光和可见光下LaCoO3/Co3O4/g-C3N4三元纳米复合抗菌剂处理后大肠杆菌和金黄色葡萄球菌的菌落数都明显的减少,其抗菌率均可达到95%以上;值得注意的是,处理后,金黄色葡萄球菌的菌落数相比与大肠杆菌菌的菌落数多一些,这与MIC的测试结果一致。
综上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂的制备方法,其特征在于,包括以下步骤:
步骤一:称取六水合硝酸钴Co(NO)2·6H2O和2-甲基咪唑C4H6N2分别加入到20~50 mL的甲醇中搅拌30 min后,所述六水合硝酸钴Co(NO)2·6H2O和2-甲基咪唑C4H6N2的摩尔比为1:4,将两种溶液混合搅拌,并在室温条件静置;将静置后的溶液用无水乙醇离心、洗涤3次;然后将收集的紫色沉淀物在50 ℃下干燥12 h获得ZIF-67十二面体纳米材料;
步骤二:首先,将ZIF-67分散在无水乙醇和去离子水混合溶液中超声15 min,并搅拌30min,无水乙醇与去离子水的摩尔比为1:0~1;随后,在上述混合溶液中加入六水合硝酸镧La(NO3)3·6H2O,所述ZIF-67与La(NO3)3·6H2O的质量比为1:0.5~2,并在磁力搅拌器下持续搅拌,待搅拌结束后,将混合溶液用无水乙醇离心、洗涤3次,干燥后收集紫色粉末,煅烧处理后,可得LaCoO3/Co3O4纳米材料;
步骤三:称取上述制备好的LaCoO3/Co3O4纳米材料和双氰胺经马弗炉两次500 ℃下煅烧所得的g-C3N4纳米片,所述LaCoO3/Co3O4与g-C3N4的质量比为1:0.1~2, 分别分散在一定量的甲醇溶液中并超声处理1 h;接着,将制备好的LaCoO3/Co3O4溶液和g-C3N4溶液进行混合,并在通风橱中使用磁力搅拌器持续搅拌直到甲醇完全挥发;将所得到的黑色固体收集后在80 ℃烘箱中干燥12 h,得到LaCoO3/Co3O4/g-C3N4纳米复合抗菌剂。
2.如权利要求1所述g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂的制备方法,其特征在于,所述步骤二中采用马弗炉在为500 ℃~900 ℃的煅烧温度下保温2~5 h。
3.如权利要求1或2所述制备方法制得的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂。
4.如权利要求3所述的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂,其特征在于,LaCoO3/Co3O4纳米颗粒均匀负载在g-C3N4纳米薄片上。
5.如权利要求4所述的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂,其特征在于,LaCoO3/Co3O4纳米颗粒的粒径为10~30 nm。
6.如权利要求3-5任一项所述的g-C3N4/LaCoO3/Co3O4三元纳米复合抗菌剂在环境污染和生物医疗方面的应用。
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