CN110003248B - 一种多羧酸铀酰配合物光催化剂及其制备方法 - Google Patents
一种多羧酸铀酰配合物光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种多羧酸铀酰配合物光催化剂及其制备方法。该光催化剂分子式为C18H14N2O27U3,其化学结构式为[(UO2)3(L)2(H2O)3]·2H2O(5‑硝基‑1,2,3‑苯三甲酸缩写为H3L);该方法包括以下步骤:将5‑硝基‑1,2,3‑苯三甲酸、硝酸酰铀以及碱液加入反应釜中,再加水,于120~150℃密闭反应40~60h,最后冷却至室温即可。本发明制备方法简便,制备得到的光催化剂稳定性好,降解率高,且能通过离心分离进行回收。
Description
技术领域
本发明属于光催化剂制备技术领域,具体涉及一种多羧酸铀酰配合物光催化剂及其制备方法。
背景技术
水是生命的源泉,是人类赖以生存和发展的宝贵自然资源。但是随着工业进步和社会发展,人们享受着现代生活便利的同时,也遭受着水污染所带来的危害。如何低耗能,低耗费,高效能的去除废水中的染料等有毒物质已成为人们关注的焦点。光催化技术是一种在能源和环境领域有着重要应用前景的绿色技术,在清除有机污染物方面有着广阔的应用前景。因此,光催化剂的制备也引起了人们的广泛关注。
半导体光催化剂在室温下可将废水中有机污染物氧化成H2O、CO2或无机离子等,且无二次污染。其中,TiO2以其催化活性高、廉价易得、性质稳定、无毒、抗化学和光腐蚀等优点而成为众多科研工作者研究的首选。但是,由于TiO2是一种宽带隙半导体,只能在紫外光下才能发挥作用,且光生电子与空穴易复合、比表面积不够大,因此,从实际应用的方面来看有必要寻找新型的光催化剂。铀酰离子具有独特的可见光波段的强吸收和响应,具有更高的光催化效率,有望解决TiO2光催化剂中存在的光响应范围窄、量子效率低等缺点,成为颇具应用潜力的光催化剂。
发明内容
针对现有技术中的上述不足,本发明提供一种多羧酸铀酰配合物光催化剂及其制备方法,可制备得到一种催化效率高,且能再回收的光催化剂。
为实现上述目的,本发明解决其技术问题所采用的技术方案是:
一种多羧酸铀酰配合物光催化剂,该光催化剂分子式为C18H14N2O27U3,其化学结构式为[(UO2)3(L)2(H2O)3]·2H2O;分子结构图见图1,其空间结构见图2。
进一步地,该光催化剂晶系为Monoclinic,空间群P21/c,晶胞参数为:a=10.5009,b=15.3256,c=17.7150,α=90,β=98.0570,γ=90。
上述光催化剂的方法,包括以下步骤:
将5-硝基-1,2,3-苯三甲酸(缩写为H3L)、硝酸酰铀以及碱液加入反应釜中,再加水,于120~150℃密闭反应40~60h,最后冷却至室温即可;其中,5-硝基-1,2,3-苯三甲酸和硝酸酰铀的摩尔比为0.5~0.9:1~2;5-硝基-1,2,3-苯三甲酸与碱液的料液比为0.5~0.8:100~200。
进一步地,5-硝基-1,2,3-苯三甲酸和硝酸酰铀的摩尔比为0.7:1。
进一步地,5-硝基-1,2,3-苯三甲酸与碱液的料液比为0.7:100。
进一步地,碱液为氨水。
进一步地,反应温度为150℃,反应时间为48h。
进一步地,反应釜材质为聚四氟乙烯。
本发明的有益效果为:
1、本发明采用5-硝基-1,2,3-苯三甲酸、硝酸酰铀、碱液以及水反应制备光催化剂,制备方法简便,纯度高;制备得到的光催化剂稳定好,光催化降解效率高,且可通过离心分离的方法对光催化剂进行回收,避免催化剂可能引起的二次污染。
2、本发明制备得到的光催化剂,在氙灯照射下模拟可见光,55分钟内可将浓度为20mg/L的RhB溶液降解78%左右,降解效率高,稳定好。
附图说明
图1为本发明制备得到的光催化剂的分子结构图;
图2为本发明制备得到的光催化剂的空间结构图;
图3为本发明制备得到的光催化剂的紫外光谱;
图4为本发明制备得到的光催化剂的红外光谱;
图5为本发明制备得到的光催化剂的粉末衍射图谱;
图6为本发明制备得到的光催化剂的热分析检测图;
图7为本发明制备得到的光催化剂的降解效率检测图谱。
具体实施方式
下面对本发明的具体实施方式进行描述,以便于本技术领域的技术人员理解本发明,但应该清楚,本发明不限于具体实施方式的范围,对本技术领域的普通技术人员来讲,只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内,这些变化是显而易见的,一切利用本发明构思的发明创造均在保护之列。
实施例1
一种利用5-硝基-1,2,3-苯三甲酸制备光催化剂的方法,包括以下步骤:
在万分之一天平上分别准确称取0.07mmol的配体5-硝基-1,2,3-苯三甲酸、0.1mmol的硝酸酰铀、10μL以及1.0mL的水,然后将上述原料装入体积为23mL的聚四氟乙烯反应釜中,盖上盖子密封于烘箱中,在150℃的条件下反应两天,最后自然冷却至室温,得到纯度不低于99%的黄色透明晶体,即为多羧酸铀酰配合物光催化剂。
实施例2
一种利用5-硝基-1,2,3-苯三甲酸制备光催化剂的方法,包括以下步骤:
在万分之一天平上分别准确称取0.05mmol的配体5-硝基-1,2,3-苯三甲酸、0.15mmol的硝酸酰铀、15μL以及1.0mL的水,然后将上述原料装入体积为23mL的聚四氟乙烯反应釜中,盖上盖子密封于烘箱中,在120℃的条件下反应40h,最后自然冷却至室温,得到纯度不低于99%的黄色透明晶体,即为多羧酸铀酰配合物光催化剂。
实施例3
一种利用5-硝基-1,2,3-苯三甲酸制备光催化剂的方法,包括以下步骤:
在万分之一天平上分别准确称取0.09mmol的配体5-硝基-1,2,3-苯三甲酸、0.2mmol的硝酸酰铀、20μL以及1.0mL的水,然后将上述原料装入体积为23mL的聚四氟乙烯反应釜中,盖上盖子密封于烘箱中,在140℃的条件下反应两天,最后自然冷却至室温,得到纯度不低于99%的黄色透明晶体,即为多羧酸铀酰配合物光催化剂。
实施例4
对实施例1制备得到的多羧酸铀酰配合物光催化剂进行X-射线单晶衍射、紫外-可见光谱、红外光谱、X-射线粉末衍射以及热分析检测,其检测结果见图1~6。
对该光催化剂进行X-射线单晶衍射结构解析,检测得到其分子式为C18H14N2O27U3,化学结构式为[(UO2)3(L)2(H2O)3]·2H2O;晶系为Monoclinic,空间群P21/c,晶胞参数为:a=10.5009,b=15.3256,c=17.7150,α=90,β=98.0570,γ=9;具体分子结构图见图1,空间结构图见图2。
同时,实施例1制备得到的多羧酸铀酰配合物光催化剂的样品粉末的衍射图谱与单晶模拟的PXRD进行对比,两者可以完美吻合,见图5,表明本发明方法制备得到的产品的纯度不低于99%。
热分析检测见图6,通过图6的检测结果可知,本发明制备得到的光催化剂具有良好的热稳定性。
实施例5
1、实验组
将实施例1制备得到的光催化剂样品研磨成粉末,分散到浓度为20mg/L的RhB水溶液中,通过超声搅拌将其充分混合均匀后继续搅拌30min以建立吸附-脱附平衡,整个过程要求避光。待吸附-脱附平衡后开启300W的氙灯光源照射,每隔10min取出2mL溶液经0.22μm的滤头过滤后于紫外分光光度计(Uvmini-1280)上进行测定。
2、空白组:与实验组相比,区别在于缺少5-硝基1,2,3-苯三甲酸铀酰配合物光催化剂,其余过程与实验组相同。
3、实验组和空白组的检测结果见图7,如图7所示,在氙灯照射下模拟可见光,实施例1制备得到的光催化剂的作用下,在氙灯照射下模拟可见光,55分钟内可将浓度为20mg/L的RhB溶液降解78%左右;而空白组中RhB溶液几乎无降解;由此说明,本发明制备得到的光催化剂降解效率高,稳定好。
Claims (7)
1.一种多羧酸铀酰配合物光催化剂,其特征在于,所述光催化剂分子式为C18H14N2O27U3,其化学结构式为[(UO2)3(L)2(H2O)3]·2H2O,其制备方法为:将5-硝基-1,2,3-苯三甲酸、硝酸酰铀以及碱液加入反应釜中,再加水,于120~150℃密闭反应40~60h,最后冷却至室温即可;其中,所述5-硝基-1,2,3-苯三甲酸和硝酸酰铀的摩尔比为0.5~0.9:1~2;所述5-硝基-1,2,3-苯三甲酸与碱液的料液比为0.5~0.8:100~200,所述光催化剂晶系为Monoclinic,空间群P21/c,晶胞参数为:a=10.5009,b=15.3256,c=17.7150,α=90,β=98.0570,γ=90。
2.根据权利要求1所述的多羧酸铀酰配合物光催化剂的制备方法,其特征在于,将5-硝基-1,2,3-苯三甲酸、硝酸酰铀以及碱液加入反应釜中,再加水,于120~150℃密闭反应40~60h,最后冷却至室温即可;其中,所述5-硝基-1,2,3-苯三甲酸和硝酸酰铀的摩尔比为0.5~0.9:1~2;所述5-硝基-1,2,3-苯三甲酸与碱液的料液比为0.5~0.8:100~200。
3.根据权利要求2所述的制备方法,其特征在于,所述5-硝基-1,2,3-苯三甲酸和硝酸酰铀的摩尔比为0.7:1。
4.根据权利要求2所述的制备方法,其特征在于,所述5-硝基-1,2,3-苯三甲酸与碱液的料液比为0.7:100。
5.根据权利要求2所述的制备方法,其特征在于,所述碱液为氨水。
6.根据权利要求2所述的制备方法,其特征在于,所述反应温度为150℃,反应时间为48h。
7.根据权利要求2所述的制备方法,其特征在于,所述反应釜材质为聚四氟乙烯。
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