CN110075820A - 一种Al2O3/ZrO2/SiO2复合可见光催化剂及其制备方法 - Google Patents
一种Al2O3/ZrO2/SiO2复合可见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Al2O3/ZrO2/SiO2三复合可见光催化剂及其制备方法，它涉及一种可见光催化剂及其制备方法。本发明可解决可见光催化剂对太阳能的利用率低，对染料污染物的吸附效率低、催化活性差，降解率低，以及现有的制备方法复杂、成本高的问题。本发明的制备方法包含以下步骤：(1)以柠檬酸、氧氯化锆、硝酸铝及去离子水为原料配制铝锆复合前驱体溶液；以乙醇为溶剂配制正硅酸乙酯乙醇溶液；将前驱体溶液与正硅酸乙酯乙醇溶液混合均匀调节pH得到铝锆硅前驱体溶液；(2)将铝锆硅前驱体溶液烘干，高温煅烧即可得。
Description
技术领域
本发明属于光催化剂的制备技术领域，特别涉及一种Al2O3/ZrO2/SiO2复合可见光催化剂及其制备方法。
背景技术
半导体光催化技术是一种新型的环境污染物处理技术，光催化氧化处理有机污染物具有方法简单、不产生二次污染，适用范围广等特点。光催化材料是指一类在光照作用下可以引发或诱发其他物质的氧化－还原反应的材料，以半导体光催化材料为主。目前，光催化材料的报道非常多，有TiO2、非TiO2氧化物、Ag@AgX、CdS、铋酸盐、钴酸盐、磷酸盐以及石墨相氮化碳(g-C3N4)等，其中最具代表性的是TiO2半导体材料，但是其本身具有仅对紫外光响应且量子效率不高，降解效率低的局限性，而其他各类的光催化材料仍然存在着光响应强度不够、制备工艺复杂、光稳定性不足以及经济成本高等问题。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种Al2O3/ZrO2/SiO2复合可见光催化剂及其制备方法，可解决可见光催化剂对染料污染物的吸附效率低、催化活性差，以及现有的制备方法复杂、成本高、可见光利用率低的问题。
为了实现上述目的，本发明采用的技术方案是：
一种Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，包括如下步骤：
(1)以柠檬酸、氧氯化锆、硝酸铝及去离子水为原料配制铝锆复合前驱体溶液；以无水乙醇为溶剂配制正硅酸乙酯乙醇溶液；将前驱体溶液与正硅酸乙酯乙醇溶液混合均匀调节pH＝7得到铝锆硅前驱体溶液；
(2)将所得铝硅锆前驱体溶液烘干，高温煅烧后即可得到Al2O3/ZrO2/SiO2复合可见光催化剂。
所述步骤(1)中，柠檬酸与氧氯化锆的质量比为0.5:1-10:1，硝酸铝与氧氯化锆的质量比为0.5:1-4:1，去离子水与柠檬酸的质量比为5:1-10:1
所述步骤(1)中，正硅酸乙酯与无水乙醇的体积比1:2-1:5。
所述步骤(1)中，氧氯化锆与正硅酸乙酯的摩尔比为0.1:3-1.5:3。
所述步骤(2)中，烘干温度为60-80℃，烘干时间为12-36h。
所述步骤(2)中，煅烧温度为500-900℃，煅烧时间为1.5-2.5h。
本发明还要求保护由所述制备方法制得的Al2O3/ZrO2/SiO2复合可见光催化。
与现有技术相比，本发明的有益效果是：
1.本发明制备的Al2O3/ZrO2/SiO2三复合可见光催化剂，与未改性的单一粉体相比，比表面积显著提高，表现出了很强的染料吸附能力和降解能力，同时复合粉体的光催化活性，明显优于市售的光催化剂。
2.本发明制备的Al2O3/ZrO2/SiO2三复合可见光催化剂具有很高的稳定性，同时具备较好的可重复使用性。在重复使用性验证试验中，本发明制备的Al2O3/ZrO2/SiO2三复合可见光催化剂，吸附降解完成后，进行晾干处理，再次进行吸附降解实验，吸附及降解性能未见明显降低。
3.本发明的原料易得，制备方法简单、易操作，可重复性高，整个过程制备成本低。
附图说明
图1为实施例1中所得到的Al2O3/ZrO2/SiO2复合光催化剂的扫描电镜照片。
图2为实施例1中所得到的Al2O3/ZrO2/SiO2复合光催化剂在可见光激发下降解染料的曲线图。
图3为可重复使用性实验中Al2O3/ZrO2/SiO2复合光催化剂在可见光激发下降解染料的曲线。
具体实施方式
下面结合附图和实施例详细说明本发明的实施方式。本发明技术方案不局限于以下所列的具体实施方式，还包括各具体实施方式间的任意组合。
实施例1
(1)铝锆复合前驱体溶液的配置：按照质量比为1-5:1:1分别称取一定质量的柠檬酸、硝酸铝和氧氯化锆备用，将柠檬酸、硝酸铝和氧氯化锆溶解于20mL去离子水中，得到铝锆前驱体溶液，磁力搅拌30min。
(2)正硅酸乙酯溶液的配置：按照氧氯化锆与正硅酸乙酯的摩尔比为0.5:3计算所需的正硅酸乙酯量，按照体积比1:2分别量取一定体积的正硅酸乙酯和无水乙醇，混合均匀，磁力搅拌10min。
(3)铝锆硅前驱体溶液的配置：在持续磁力搅拌下，将步骤2所制备的正硅酸乙酯溶液逐滴添加到铝锆复合前驱体溶液中，滴加0.1mL聚乙二醇，磁力搅拌30min，并调节pH＝7。
(4)Al2O3/ZrO2/SiO2三复合粉体的制备：将步骤3得到的铝锆硅前驱体溶液放置于鼓风干燥箱中，80℃下保温24h；将烘干后的铝锆硅前驱体放置于马弗炉中，800℃下热处理2h，得到Al2O3/ZrO2/SiO2三复合粉体，即Al2O3/ZrO2/SiO2三复合可见光催化剂。
从图1可以看出，通过本方法所制备的复合粉体呈均匀颗粒聚集结构，且粒径分布均匀。
利用该Al2O3/ZrO2/SiO2三复合可见光催化剂在可见光激发下降解染料，结果如图2所示，其中，随着光反应时间的延长，罗丹明B浓度不断降低，在光反应150min后，罗丹明B降解率达到90％左右。
可重复使用性实验中，Al2O3/ZrO2/SiO2三复合光催化剂在可见光激发下降解染料性能如图3所示，图中可见，随着光反应时间的延长，罗丹明B浓度不断降低，在光反应150min后，罗丹明B降解率基本都达到85％左右。由此可见，该发明所制备的复合光催化剂在重复使用性实验中，光降解性能优异。
实施例2：
(1)铝锆前驱体溶液的配置：按照质量比为1-5:0.5:1分别称取一定质量的柠檬酸、硝酸铝和氧氯化锆备用，将柠檬酸、硝酸铝和氧氯化锆溶解于25ml去离子水中，得到铝锆前驱体溶液，磁力搅拌30min。
(2)正硅酸乙酯溶液的配置：按照氧氯化锆与正硅酸乙酯的摩尔比为1:3计算所需的正硅酸乙酯量，按照体积比0.5:3分别量取一定体积的正硅酸乙酯和无水乙醇，混合均匀，磁力搅拌10min，并调节pH＝7.
(3)铝锆硅前驱体溶液的配置：在持续磁力搅拌下，将步骤2所制备的正硅酸乙酯溶液逐滴添加到铝锆前驱体溶液中，滴加0.1mL聚乙二醇，磁力搅拌30min。
(4)Al2O3/ZrO2/SiO2三复合粉体的制备：将步骤3得到的铝锆硅前驱体溶液放置于鼓风干燥箱中，60℃下保温36h；将烘干后的铝锆硅前驱体放置于马弗炉中，600℃下热处理4h，得到Al2O3/ZrO2/SiO2三复合粉体，即Al2O3/ZrO2/SiO2三复合可见光催化剂。
综上，本发明可解决可见光催化剂对太阳能的利用率低，对染料污染物的吸附效率低、催化活性差，降解率低，以及现有的制备方法复杂、成本高的问题。以上实施例为本发明较佳的实施方式，但本发明的实施方式不受上述实施例的限制，其他任何基于本发明的原理或精神实质下所作的改变、替代、组合、简化等均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (7)
1.一种Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，包括如下步骤：
(1)以柠檬酸、氧氯化锆、硝酸铝及去离子水为原料配制铝锆复合前驱体溶液；以无水乙醇为溶剂配制正硅酸乙酯乙醇溶液；将前驱体溶液与正硅酸乙酯乙醇溶液混合均匀调节pH＝7得到铝锆硅前驱体溶液；
(2)将所得铝硅锆前驱体溶液烘干，高温煅烧后即可得到Al2O3/ZrO2/SiO2复合可见光催化剂。
2.根据权利要求1所述Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，所述步骤(1)中，柠檬酸与氧氯化锆的质量比为0.5:1-10:1，硝酸铝与氧氯化锆的质量比为0.5:1-4:1，去离子水与柠檬酸的质量比为5:1-10:1。
3.根据权利要求1所述Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，所述步骤(1)中，正硅酸乙酯与无水乙醇的体积比1:2-1:5。
4.根据权利要求1或2或3所述Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，所述步骤(1)中，氧氯化锆与正硅酸乙酯的摩尔比为0.1:3-1.5:3。
5.根据权利要求1所述Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，所述步骤(2)中，烘干温度为60-80℃，烘干时间为12-36h。
6.根据权利要求1所述Al2O3/ZrO2/SiO2复合可见光催化剂的制备方法，其特征在于，所述步骤(2)中，煅烧温度为500-900℃，煅烧时间为1.5-2.5h。
7.由权利要求1-6任一项所述制备方法制得的一种Al2O3/ZrO2/SiO2复合可见光催化。
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