CN114950563B - 一种可降解有机染料和/或重金属离子的光催化剂及其制备 - Google Patents
一种可降解有机染料和/或重金属离子的光催化剂及其制备 Download PDFInfo
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Abstract
本发明涉及光催化领域,具体说是一种具有在可见光的激发下可以降解有机染料和/或重金属离子的光催化剂及其制备和应用。先将含Zr的金属化合物与有机适配体混合再与含Mo的金属化合物的水溶液混合,在水存在下经水热法制备获得含Mo/Zr的材料。本发明制备的光催化剂具有方法简单、成本低、性能显著等优点。
Description
技术领域
本发明涉及光催化领域,具体说是一种具有在可见光的激发下可以降解有机染料和/或重金属离子的光催化剂及其制备和应用。
背景技术
有机染料和重金属离子的降解是污水处理中的两大方面。传统的降解有机染料和还原重金属离子的方法有很多,包括微生物降解法、电化学法、物理吸附法,离子交换法、光催化法等,其中光催化还原因其具有能耗低、效率高、环境友好。
发明内容
本发明的目的在于提供一种具有在可见光激发下可降解有机染料和/或重金属离子的光催化剂及其制备和应用。
为实现上述目的,本发明采用的技术方案为:
一种可降解有机染料和重金属离子的光催化剂的制备方法,先将含Zr的金属化合物与有机适配体混合再与含Mo的金属化合物的水溶液混合,在水存在下经水热法制备获得含Mo/Zr的材料。
所述的将含Zr的金属化合物与有机适配体混合形成水溶液,而后再与含Mo的金属化合物的水溶液混合,在100-140℃下进行水热反应8-12h,即得到含Mo/Zr的材料。
所述的含Mo的金属化合物的水溶液与含Zr的金属化合物的水溶液按体积比1:1混合;
所述的含Zr的金属化合物的水溶液中Zr与有机适配体摩尔比为1:1。
所述的含Mo的金属化合物的水溶液与含Zr的金属化合物的水溶液按体积比1:1混合;
所述的含Zr的金属化合物的水溶液中Zr与有机适配体摩尔比为1:1。
所述的有机适配体为4,4-联吡啶;
所述含Mo的金属化合物的水溶液中Mo的金属化合物的摩尔量为5-10mmol;其中,Mo的金属化合物为Na2MoO4或(NH4)2MoO4;
所述含Zr的金属化合物与有机适配体混合形成水溶液中Zr的金属化合物的摩尔量为1-5mmol;其中,Zr的金属化合物为ZrCl4或ZrOCl2;
反应釜的规格与水热反应过程中添加的蒸馏水的体积比为5:3。
所述水溶液时还可添加分散剂使其形成均匀分散的水溶液;其中,分散剂为聚乙烯吡咯烷酮(PVP),每100mL水需加入0.5g的PVP。
可降解有机染料和重金属离子的光催化剂,所述方法制备片层状Mo/Zr材料可降解有机染料和重金属离子的光催化剂。
一种光催化剂的应用,所述光催化剂在降解有机染料和重金属离子方面的应用。
所述有机染料为亚甲基蓝(MB);重金属离子为Cr6+。
本发明所得催化剂的降解原理:光催化激发催化剂产生·O2 -和·OH直接将有机染料降解为CO2。H2O和无毒小分子,将有毒对身体有害的Cr6+还原为无毒的Cr3+。
本发明与现有技术相比,具有以下优点及突出性效果:
本发明通过一步水热法制备光催化剂,具有利用可见光降解有机染料效果。通过XRD分析,确认为Mo/Zr-MOF。根据TEM图能看出材料表现为片层状结构。其具有利用可见光降解有机染料效果。
本发明研制方法具有原料廉价易得、成本低、制备方法简单。材料性能优异的优点。这些优点对于光催化剂的实际应用。本发明所得的光催化剂,在医疗卫生、能源开发和环境治理等领域具有潜在的实际应用价值,在新型光催化分析中具有广阔的应用前景。
附图说明:
图1为本发明实施例1提供的光催化剂的XRD图;
图2为本发明实施例1提供的光催化剂的TEM图;
图3为本发明实施例2提供的光催化剂的XRD图;
图4为本发明实施例1提供的光催化剂在可见光激发下的,针对有机染料降解的性能图;
图5为本发明实施例1提供的光催化剂在可见光激发下的,针对重金属离子降解的性能图;
具体实施方式
一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。
实施例1:
5mmol ZrCl4和5mmol 4,4联吡啶,0.5g聚乙烯吡咯烷酮(分散剂)溶解在35mL水中搅拌10分钟。7.5mmol Na2MoO4分散在30mL水强烈搅拌10分钟。将上述获得两种溶液混合,混合后转移至100mL聚四氟乙烯内衬,再装入不锈钢反应釜内,加热在120℃,12h,然后自然冷却到室温。经蒸馏水和无水乙醇反复洗五次,离心条件为4500转/min,离心5-10分钟,放入60℃烘箱干燥至少10h,即获得Mo/Zr-MOF(参见图1和2)。
由图1可以看出,通过对比可能存在中间体的PDF标准卡片,通过排除得出该物质为Mo/Zr-MOF。由图2可以看出,材料的形貌为片层状。
实施例2
5mmol ZrCl4和5mmol 4,4联吡啶,0.5g聚乙烯吡咯烷酮(分散剂)溶解在35mL水中搅拌10分钟。10mmol Na2MoO4分散在30mL水强烈搅拌10分钟。将上述获得两种溶液混合,混合后转移至100mL聚四氟乙烯内衬,再装入不锈钢反应釜内,加热在120℃,12h,然后自然冷却到室温。经蒸馏水和无水乙醇反复洗五次,离心条件为4500转/min,离心5-10分钟,放入60℃烘箱干燥至少10h,即获得Mo/Zr-MOF(参见图3)。
由上述实施例制备所得Mo/Zr-MOF经XRD分析可见,均具有相同的衍射峰。
应用例1
空白组加入20mg/mL的亚甲基蓝(MB),在实验组加入20mg/mL的亚甲基蓝(MB)和1mg/mL的上述实施例1的光催化剂。对上述对照组和实验组进行光照处理,光辐照度为400-450mW/cm2,而后在不同时间点取出1mL溶液离心获得上清液,在655nm处测试其吸光度值。
如图4所示,在光照下,空白组的染料几乎未被降解,证明单纯的光照对染料降解并无影响。实验组中,在同样强度的光照下,添加了光催化剂后,MB逐渐被降解,进而可见本发明所得催化剂针对亚甲基蓝(MB),在可见光的激发下,可以实现对该染料的良好降解。
应用例2
空白组加入10mg/L的Cr6+,在实验组加入10mg/L的Cr6+和1mg/mL的上述实施例1的光催化剂。光辐照度为400-450mW/cm2,而后在不同时间点取出1mL溶液离心获得上清液,利用二苯碳酰二肼显色法测试其吸光度值。
如图5所示,在光照下,空白组的重金属离子几乎未被还原降解,证明单纯的光照对重金属离子的降解并无影响。在实验组中,在同样强度的光照下,添加了光催化剂后,Cr6+逐渐被降解,进而可见本发明所得催化剂针对重金属离子(Cr6+),在可见光的激发下,可以实现对该重金属离子的高效还原降解。
Claims (8)
1.一种可降解有机染料和重金属离子的光催化剂的制备方法,其特征在于:先将含Zr的金属化合物与有机适配体混合再与含Mo的金属化合物的水溶液混合,在水存在下经水热法制备获得含Mo/Zr-MOF的材料;Mo的金属化合物为Na2MoO4或(NH4)2MoO4;
所述的有机适配体为4,4-联吡啶。
2.按权利要求1所述的可降解有机染料和重金属离子的光催化剂的制备方法,其特征在于:所述将含Zr的金属化合物与有机适配体混合形成含Zr的金属化合物的水溶液,而后再与含Mo的金属化合物的水溶液混合,在100-140 ℃下进行水热反应8-12 h,即得到含Mo/Zr-MOF的材料。
3.按权利要求2所述的可降解有机染料和重金属离子的光催化剂的制备方法,其特征在于:所述的含Mo的金属化合物的水溶液与含Zr的金属化合物的水溶液按体积比1:1混合;
所述的含Zr的金属化合物的水溶液中Zr与有机适配体摩尔比为1:1。
4.按权利要求3所述的可降解有机染料和重金属离子的光催化剂的制备方法,其特征在于:所述含Mo的金属化合物的水溶液中Mo的金属化合物的摩尔量为5-10 mmol;所述的含Zr的金属化合物与有机适配体混合形成水溶液中Zr的金属化合物的摩尔量为1-5 mmol;其中,Zr的金属化合物为 ZrCl4或ZrOCl2;
反应釜的规格与水热反应过程中添加的蒸馏水的体积比为5:3。
5.按权利要求1或2所述的可降解有机染料和重金属离子的光催化剂的制备方法,其特征在于:所述水溶液时还添加分散剂使其形成均匀分散的水溶液;其中,分散剂为聚乙烯吡咯烷酮,每50-100 mL水加入0.5 g的PVP。
6.按权利要求1所述方法制备的光催化剂,其特征在于,所述Mo/Zr-MOF材料为片层状结构。
7.一种权利要求6所述光催化剂的应用,其特征在于:所述光催化剂在降解有机染料和重金属离子方面的应用。
8.按权利要求7所述的所述光催化剂的应用,其特征在于:所述有机染料为亚甲基蓝;重金属离子为Cr6+。
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