CN103933992B - 一种复合纳米磁性光催化剂和制备方法及其应用 - Google Patents
一种复合纳米磁性光催化剂和制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种复合纳米磁性光催化剂和制备方法,本发明的磁性光催化剂采用共沉淀法制备出镍锌铁氧体作为磁核,并通过均相沉淀法制备出ZnO为外包覆层的磁性纳米光催化剂,具有铁磁性和部分超顺磁性,在磁场下能够沿磁场均与分布且不易磁聚,同时具备高的光催化活性,而且可以通过磁性分离回收循环使用。本发明制备方法有生产工艺简单,成本低廉等优点。所制备的复合纳米磁性光催化剂适用于含金属粒子、含油废水、印染废水、生活污水等处理。经过对污水催化降解证明,与已有技术相比,具有处理效果好、降解速度快、用量低、易回收、可循环使用、且对环境无污染等优点。
Description
技术领域
本发明属于磁性光催化剂领域,特别涉及一种复合纳米磁性光催化剂和制备方法及在对高浓度难降解有机物的可见光降解中的应用。
背景技术
近年来随着科学技术的发展,通过光催化氧化技术降解水中的污染物(尤其是高浓度的污染物)已成为一项新型的水处理技术。然而投入何种光催化剂以实现污水处理的高效率,是目前水处理过程中的一个重要问题。另外,污水中的催化剂的回收也是一个重大难题,否则会提高污水处理成本,而且容易造成二次污染。因此,针对不同的废水,确定一种高效的可以利用可见光的磁性光催化剂是解决污水处理费用高昂、催化剂回收问题的一个基本途径。
随着对可以利用可见光的催化剂研究的深入,一些能够降解污水的新型光催化剂被开发出来。如一种可见光催化剂及其制备方法(CN102327770A)制备的可见光催化剂为铬参杂氧化锌,能够拓宽氧化锌的光催化响应波长范围,但是催化剂中含有污染元素铬,且不能回收,容易对环境造成污染。在磁性参杂纳米二氧化钛制备方法(CN102794164A)中制备的磁性光催化剂以Fe参杂二氧化钛的复合物,该光催化剂只能利用紫外光,对可见光利用率较低,而且在磁场中容易发生团聚现象。而在一种可磁控分离氧化锌基光催化剂的制备方法(CN102728369A)中氧化锌与磁性材料只是简单结合在一起,而非氧化锌包覆磁性材料,所以对氧化锌的比表面积有一定影响,从而降低它的光催化活性。另外,在一种磁可控氧化锌复合纳米晶光催化剂及其制备方法(CN103285881A)磁基是金和镍的化合物,具有铁磁性,不利于在污水中的均匀分散,降低了污水处理效果。
发明内容
本发明的目的之一是提供一种具有高光催化活性的磁性光催化剂。
目的之二是提供上述催化剂的制备方法。
目的之三是提供上述催化剂在对高浓度难降解有机物的可见光降解中的应用。
为了实现上述目的,本发明采用以下技术方案:一种复合纳米磁性光催化剂,所述催化剂为Ni0.5Zn0.5Fe2O4/ZnO,其中镍锌铁氧体为磁基,纳米颗粒ZnO包裹其表面。
所述催化剂的颗粒粒度为50~75nm。
一种复合纳米磁性光催化剂的制备方法,包括以下步骤:
(1)将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,搅拌均匀,以金属离子计,锌离子:镍离子:铁离子的摩尔比为0.5:0.5:2;向混合溶液中缓慢滴加NaOH溶液形成红棕色沉淀并不停搅拌,至pH=10停止,用去离子水抽滤洗涤,沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到镍锌铁氧体;
(2)将制备的镍锌铁氧体与尿素和硫酸锌混合并溶于去离子水中,镍锌铁氧体:尿素:硫酸锌的摩尔比为0.5:2:1,超声1h,将溶液装入反应釜中于100~120℃下进行溶剂热反应1h后,冷却,并用无水乙醇进行抽滤洗涤,将产物干燥4h,在500℃下煅烧3h,自然降温后得到复合纳米磁性光催化剂Ni0.5Zn0.5Fe2O4/ZnO。
一种复合纳米磁性光催化剂在对高浓度难降解有机物的可见光降解中的应用,包括以下步骤:在高浓度难降解有机物溶液中加入Ni0.5Zn0.5Fe2O4/ZnO,避光搅拌30min后,用日光镝灯照射,光源功率为400W,离液面10cm。
本发明提供的复合纳米磁性光催化剂Ni0.5Zn0.5Fe2O4/ZnO,其中镍锌铁氧体为磁基,ZnO包裹其表面。由于镍锌铁氧体具有部分超顺磁性,能够沿磁场均匀分布,不容易发生团聚现象,而且可以磁分离。ZnO作为半导体材料,能够利用可见光对高浓度难降解有机物进行降解。本发明提供的复合纳米磁性光催化剂具有磁分散、光催化等作用,可以通过磁回收循环使用,而且无二次污染。
具体实施方式
将下面结合具体的制备实施例和参照数据进一步详细地描述本发明。应理解,这些实施例只是为了举例说明本发明,而非以任何方式限制本发明的范围。
实施例1
复合纳米磁性光催化剂的制备:
(1)镍锌铁氧体的制备:按Ni0.5Zn0.5Fe2O4成分比列将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,混合均与后,缓慢滴加NaOH溶液,形成红棕色沉淀并不停搅拌,至pH=10停止。用去离子水抽滤洗涤数次。6g聚乙二醇6000加入300mL去离子水中配成聚乙二醇6000水溶液,将沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,并在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到棕红色粉末。
(2)Ni0.5Zn0.5Fe2O4/ZnO的制备:取1g上述复合物颗粒与14.378g硫酸锌和6.006g尿素混合于去380mL离子水中,在超声波中发散1h,将溶液装于反应釜中与120℃下进行溶剂热反应。反应1h后,冷却,并用无水乙醇进行抽滤洗涤数次。将所制备复合物干燥4h,干燥后在500℃下煅烧3h,自然降温后得到镍锌铁氧体为载体的ZnO光催化剂。该磁性光催化剂呈粉末状,粒径在50~75nm。
复合纳米磁性光催化剂在对高浓度难降解有机物的可见光降解中的应用:
称取0.1g上述磁性光催化剂,加入到100mL初始浓度为10mg/L的亚甲基蓝溶液中避光搅拌30min,再用日光镝灯照射,光源功率为400W,离液面10cm,用紫外可见光分光度计测量样品的吸光度,计算光催化反应后的溶液浓度,光催化反应90min后,亚甲基蓝的总去除率达到85%左右。
实施例2
复合纳米磁性光催化剂的制备:
(1)镍锌铁氧体的制备:按Ni0.5Zn0.5Fe2O4成分比列将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,混合均与后,缓慢滴加NaOH溶液,形成红棕色沉淀并不停搅拌,至pH=10停止。用去离子水抽滤洗涤数次。6g聚乙二醇6000加入300mL去离子水中配成聚乙二醇6000水溶液,将沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,并在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到棕红色粉末。
(2)Ni0.5Zn0.5Fe2O4/ZnO的制备:取1g上述复合物颗粒与14.378g硫酸锌和6.006g尿素混合于去380mL离子水中,在超声波中发散1h,将溶液装于反应釜中与110℃下进行溶剂热反应。反应1h后,冷却,并用无水乙醇进行抽滤洗涤数次。将所制备复合物干燥4h,干燥后在500℃下煅烧3h,自然降温后得到镍锌铁氧体为载体的ZnO光催化剂。
复合纳米磁性光催化剂在对高浓度难降解有机物的可见光降解中的应用:
称取0.1g上述磁性光催化剂,加入到100mL初始浓度为10mg/L的亚甲基蓝溶液中避光搅拌30min,光催化反应90min后,亚甲基蓝的总去率达到83%左右。
实施例3
复合纳米磁性光催化剂的制备:
(1)镍锌铁氧体的制备:按Ni0.5Zn0.5Fe2O4成分比列将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,混合均与后,缓慢滴加NaOH溶液,形成红棕色沉淀并不停搅拌,至pH=10停止。用去离子水抽滤洗涤数次。6g聚乙二醇6000加入300mL去离子水中配成聚乙二醇6000水溶液,将沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,并在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到棕红色粉末。
(2)Ni0.5Zn0.5Fe2O4/ZnO的制备:取1g上述复合物颗粒与14.378g硫酸锌和6.006g尿素混合于去380mL离子水中,在超声波中发散1h,将溶液装于反应釜中与100℃下进行溶剂热反应。反应1h后,冷却,并用无水乙醇进行抽滤洗涤数次。将所制备复合物干燥4h,干燥后在500℃下煅烧3h,自然降温后得到镍锌铁氧体为载体的ZnO光催化剂。
复合纳米磁性光催化剂在对高浓度难降解有机物的可见光降解中的应用:
称取0.1g上述磁性光催化剂,加入到100mL初始浓度为10mg/L的亚甲基蓝溶液中避光搅拌30min,光催化反应90min后,亚甲基蓝的总去率达到80%左右。
Claims (3)
1.一种复合纳米磁性光催化剂,其特征在于:所述催化剂为Ni0.5Zn0.5Fe2O4/ZnO,其中镍锌铁氧体为磁基,纳米颗粒ZnO包裹其表面;
所述催化剂的颗粒粒度为50~75nm;
所述催化剂采用以下方法制备而成:
(1)将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,搅拌均匀,以金属离子计,锌离子:镍离子:铁离子的摩尔比为0.5:0.5:2;向混合溶液中缓慢滴加NaOH溶液形成红棕色沉淀并不停搅拌,至pH=10停止,用去离子水抽滤洗涤,沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到镍锌铁氧体;
(2)将制备的镍锌铁氧体与尿素和硫酸锌混合,镍锌铁氧体:尿素:硫酸锌的摩尔比为0.5:2:1,并溶于去离子水中,超声1h,将溶液装入反应釜中于100~120℃下进行溶剂热反应1h后,冷却,并用无水乙醇进行抽滤洗涤,将产物干燥4h,在500℃下煅烧3h,自然降温后得到复合纳米磁性光催化剂Ni0.5Zn0.5Fe2O4/ZnO。
2.一种根据权利要求1所述复合纳米磁性光催化剂的制备方法,其特征在于包括以下步骤:
(1)将硝酸锌、硫酸镍、硝酸铁依次溶于去离子水中,搅拌均匀,以金属离子计,锌离子:镍离子:铁离子的摩尔比为0.5:0.5:2;向混合溶液中缓慢滴加NaOH溶液形成红棕色沉淀并不停搅拌,至pH=10停止,用去离子水抽滤洗涤,沉淀物加入聚乙二醇6000水溶液中搅拌至形成凝胶,在120℃干燥3h形成干凝胶,将干凝胶放入马弗炉中700℃下煅烧4h得到镍锌铁氧体;
(2)将制备的镍锌铁氧体与尿素和硫酸锌混合,镍锌铁氧体:尿素:硫酸锌的摩尔比为0.5:2:1,并溶于去离子水中,超声1h,将溶液装入反应釜中于100~120℃下进行溶剂热反应1h后,冷却,并用无水乙醇进行抽滤洗涤,将产物干燥4h,在500℃下煅烧3h,自然降温后得到复合纳米磁性光催化剂Ni0.5Zn0.5Fe2O4/ZnO。
3.一种根据权利要求1所述复合纳米磁性光催化剂在对亚甲基蓝溶液的可见光降解中的应用,其特征在于包括以下步骤:在亚甲基蓝溶液中加入Ni0.5Zn0.5Fe2O4/ZnO,避光搅拌30min后,用日光镝灯照射,光源功率为400W,离液面10cm。
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