CN111450898B - 光催化降解有机染料的无定形CoSx/MOF复合催化剂及制备方法 - Google Patents
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Abstract
本发明公开一种光催化降解有机染料的无定形CoSx/MOF复合催化剂及制备方法,属于光催化材料合成技术领域。该方法以六水合硝酸钴为钴源、硫代乙酰胺为硫源、NH2‑MIL‑125为MOF前体和以溶剂乙醇为还原剂,三种物质分散在乙醇中,经过水热反应釜加热反应,即可得到不同量无定形CoSx负载的MOF复合催化剂。本发明制备无定形CoSx/MOF复合催化剂的方法简单,反应条件温和,得到的复合催化剂的稳定性和催化性能好,能高效去除水中有机染料污染物。该复合催化剂结合可见光构建的光催化降解有机染料体系可以有效去除水中污染物,本发明方法经济高效,环保,催化剂能够循环回收使用。
Description
技术领域:
本发明属于复合光催化剂制备及应用技术领域,具体涉及光催化降解有机染料的无定形 CoSx/MOF复合催化剂及制备方法,本发明尤其适用于有机染料罗丹明B的去除。
背景技术:
工业染料废水是水污染的主要来源,其中三苯甲烷染料由于色泽鲜艳、固色率高、染色牢度好等特点而被广泛用作工业染料,而且用量很大。但该类染料废水的色度高、毒性强、难降解且易致癌,因而现阶段急需治理的废水之一。罗丹明B作为三苯甲烷衍生物,具有较好的水溶性,易于分析,代表性强,广泛用于制造油漆和腈纶等织物的染色以及生物制品的染色,直接排入水中对生物体产生的毒性非常大。现有多种方法用于有机染料的去除包括吸附、电化学法等,但是这传统的方法不经济、不环保、还会二次污染且不能彻底降解有机物。因此急需发展经济环保的方法,光催化降解的方法可以克服上述问题,但是仍需发展高催化活性的光催化体系。
近年来,以金属有机骨架材料(MOF)为载体制备光催化剂显示了巨大的应用潜力。MOF 具有尺寸可调、稳定性好以及结构和光吸收可调的特点,具有广泛的应用前景。通过在MOF 表面原位生长无定形CoSx,可拓展光吸收范围和增强光催化性质,利用光催化降解有机染料的原理与方法,建立快速去除罗丹明B的技术。
发明内容:
本发明的目的是提供无定形CoSx/MOF复合催化剂及制备方法,本发明在不引入强还原剂的条件下,乙醇即作为溶剂又作为还原剂,简化材料制备过程,在温和反应条件下合成无定形CoSx/MOF复合催化剂,通过CoSx调控催化剂的光吸收和催化性能,实现光催化高效去除有机染料罗丹明B。本发明无定形CoSx/MOF复合催化剂可用于水样中有机染料罗丹明B的降解去除。
本发明提供一种光催化降解有机染料的无定形CoSx/MOF复合催化剂,该复合催化剂包括钴源化合物、硫源化合物及金属有机骨架材料MOF;所述钴源化合物的浓度为0.001~0.014 mol/L,所述钴源化合物、硫源化合物中钴原子与硫原子的摩尔比为1:5;所述钴源化合物与所述金属有机骨架材料MOF(NH2-MIL-125)的质量比为1:(0.5~20);所述钴源化合物为六水合硝酸钴,所述硫源化合物为硫代乙酰胺。
本发明同时提供所述光催化降解有机染料的无定形CoSx/MOF复合催化剂的制备方法,该制备方法具体步骤如下:
(1)制备金属有机骨架材料MOF(NH2-MIL-125):将钛酸四异丙酯、2-氨基对苯二甲酸、甲醇、N,N-二甲基甲酰胺置于反应釜混合均匀,设置反应温度为150℃,反应时间为16h;反应结束后用N,N-二甲基甲酰胺和甲醇多次洗涤黄色样品,自然干燥制得金属有机骨架材MOF:NH2-MIL-125。本发明中的MOF是按文献(Dalton Trans.2011,40,4879-4881)制备得到的。
(2)向50-100mL的反应釜中依次加入20~100mg步骤(1)制得的MOF:NH2-MIL-125、5-100mg的硫代乙酰胺、5~40mg的六水合硝酸钴,最后向反应釜中加入10~80mL的无水乙醇,将混合物搅拌0.1~5h后,将反应釜加热到温度90~120℃,加热1~12h后反应得到粉末样品;所述金属有机骨架材料MOF与所述无水乙醇的质量比为1:78~3150。
(3)将反应得到的所述粉末样品用无水乙醇多次洗涤,然后将粉末样品自然干燥即可得到所述无定形CoSx/MOF复合催化剂。
本发明方法以乙醇为溶剂和还原剂在金属有机骨架材料MOF表面制备生成无定形CoSx。本发明无定形CoSx/MOF复合催化剂光催化降解罗丹明B的效率在60min能够去除其中的 96%;本发明无定形CoSx/MOF复合催化剂能够重复利用,三次循环使用之后降解性能保留为第一次的90.8%。
所述加热反应温度固定后,控制加不同的钴源化合物的量,能够得到不同催化性能的光催化剂。如当设定反应温度在120℃时,加52mg的硫代乙酰胺时;不加钴源化合物时,得到的催化剂,1h光降解去除48.4%的有机染料;加钴源化合物10mg时,得到的催化剂,1h光降解去除65.9%的有机染料;加钴源化合物20mg时,得到的催化剂,1h光降解去除96%有机染料;加钴源化合物30mg时,得到的催化剂,1h光降解去除95.2%的有机染料;加钴源化合物40mg时,得到的催化剂,1h光降解去除89.2%的有机染料。
本发明制备无定形CoSx/MOF方法温和简单;相比传统的吸附法,光催化降解有机染料的过程简单,成本低,可控易操作,适合批量降解。
附图说明:
图1为本发明中不同CoSx负载量的无定形CoSx/MOF复合催化剂的X射线衍射图;
图2为本发明实施例3中制备的无定形CoSx/MOF复合催化剂的透射电镜;
图3为本发明实施例3中制备的无定形CoSx/MOF复合催化剂降解速率图;
图4为本发明实施例3中制备的无定形CoSx/MOF复合催化剂降解循环性能示意图。
具体实施方式:
下述实施例是对于本发明内容的进一步说明,以作为对本发明技术内容的阐释,但本发明的实质内容并不限于下述实施例所述,本领域的普通技术人员可以且应当知晓任何基于本发明实质精神的简单变化或替换均应属于本发明的保护范围。
实施例1:取40mg六水合硝酸钴、52mg硫代乙酰胺以及100mg MOF(NH2-MIL-125)分散于10mL乙醇中,搅拌均匀得到前驱液。将前驱液置于烘箱反应器中,设定反应温度为100℃,反应进行12h,即得到无定形CoSx/MOF复合催化剂。
实施例2:取5mg六水合硝酸钴、100mg硫代乙酰胺以及50mg MOF(NH2-MIL-125) 分散于10mL乙醇中,搅拌均匀得到前驱液。将前驱液置于烘箱反应器中,设定反应温度为 120℃,反应进行12h,即得到无定形CoSx/MOF复合催化剂。
实施例3:取20mg六水合硝酸钴、52mg硫代乙酰胺以及100mg MOF(NH2-MIL-125)分散于10mL乙醇中,搅拌均匀得到前驱液。将前驱液置于烘箱反应器中,设定反应温度为120℃,反应进行12h,即得到无定形CoSx/MOF复合催化剂。
Claims (3)
1.一种光催化降解有机染料的无定形CoSx/MOF复合催化剂的制备方法,其特征在于该制备方法具体步骤如下:
(1)制备金属有机骨架材料MOF:将钛酸四异丙酯、2-氨基对苯二甲酸、甲醇、N, N-二甲基甲酰胺置于反应釜混合均匀,设置反应温度为150 ℃,反应时间为16 h;反应结束后用N,N-二甲基甲酰胺和甲醇多次洗涤黄色样品,自然干燥得到金属有机骨架材料MOF;
(2)向50-100 mL的反应釜中依次加入20~100 mg步骤(1)制备得到的所述MOF、5~100mg的硫代乙酰胺,5~40 mg的六水合硝酸钴,最后向反应釜中加入10~80 mL的无水乙醇,将混合物搅拌0.1~5 h后,将反应釜加热到温度90~120℃,加热1~12 h后反应得到粉末样品;所述金属有机骨架材料MOF与所述无水乙醇的质量比为1:78~3150;
(3)将所述粉末样品用无水乙醇多次洗涤,然后将粉末样品自然干燥即可得到所述复合催化剂。
2.根据权利要求1所述无定形CoSx/MOF复合催化剂的制备方法,其特征在于该方法是以乙醇为溶剂和还原剂在金属有机骨架材料MOF表面制备生成无定形CoSx。
3.如权利要求1或2所述制备方法制备得到的光催化降解有机染料的无定形CoSx/MOF复合催化剂。
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