CN112517081B - 金属锡卟啉轴向功能化二氧化钛的复合光催化剂及其制备方法 - Google Patents
金属锡卟啉轴向功能化二氧化钛的复合光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种金属锡卟啉轴向功能化二氧化钛的复合光催化剂及其制备方法，属于降解燃料废水污染物的光催化材料技术领域。合成步骤包括：将锐钛型二氧化钛在有机溶剂中与金属锡卟啉按比例混合，进行加热，然后经过滤、洗涤及干燥后得金属锡卟啉敏化的二氧化钛光催化剂。本发明合成方法简单，所制备复合材料性质稳定、光催化活性高，可作为光催化处理有机污染物的环境净化材料。
Description
技术领域
本发明属于降解染料废水污染物(罗丹明B)的光催化材料技术领域，具体涉及一种新型“有机-无机”金属锡卟啉轴向功能化二氧化钛的复合光催化剂及其制备方法。
背景技术
随着社会经济的快速发展及工业化进程的加快，环境污染问题日益严峻，大量化工原料的消耗和排放，使人们周围的生活环境日益恶化。其中，有机染料污水的色度深、浓度高、毒性大，难于在自然条件下降解，已成为水处理领域的一大难题。因此，开发一种简便有效的方法来降解有机污染物是人类社会急需解决的问题。近年来，光催化降解水中有机污染物为废水的治理提供了新的思路。光催化法反应条件温和、设备简单、二次污染小、易于操作控制、运行成本低，是一种非常有前途的水污染治理技术，越来越受到人们广泛的关注。
目前光催化研究中，研究最多的、同时也被视为最佳材料的是二氧化钛，由于其具有光催化活性高、耐光腐蚀性强、稳定性好、环境友好、价格相对低廉、对人体无毒等优点，在信息、能源、环境等新兴领域表现出广泛的应用前景。但是，二氧化钛自身也缺点，其带隙宽、光谱响应范围窄，只能吸收波长小于387.5nm的紫外光，对太阳光能的利用率仅为4％。如何拓展二氧化钛在可见光区的光谱响应范围，使之具有可见光活性，并提高其对太阳光的总利用效率是制约二氧化钛光催化技术的关键问题。
利用金属锡卟啉作为敏化剂敏化二氧化钛是提高其可见光催化效果的有效途径之一。将金属锡卟啉与二氧化钛形成复合物，在光照的条件下就能够使金属卟啉产生的电子由敏化剂输送至二氧化钛半导体的导带，从而使复合物体系的激发波长拓宽至可见光范围，使得对可见光和近红外区的利用成为可能。但是人们对许多问题尚不清楚，如卟啉结构对二氧化钛催化剂的影响以及光降解过程中的反应机理等。不同结构的卟啉配合物负载于二氧化钛表面，对于废水中的有机物的去除效果并非均为理想状态，并且卟啉修饰二氧化钛往往需要分步骤进行，控制复杂的实验条件，本发明人经过多年实践经验，提出一种金属锡卟啉轴向功能化二氧化钛的复合光催化剂及其制备方法，制备方法简单，光催化剂的处理效果优异。
发明内容
本发明的目的在于研制一类新型的用于降解染料废水污染物的可见光光催化复合光催化剂，以提高光催化材料对可见光及近红外区域的光谱利用率。
本发明提供了一种金属锡卟啉轴向功能化二氧化钛复合光催化剂的制备方法，步骤简单，容易实现，制备的复合光催化剂光催化性能好。
一种金属锡卟啉轴向功能化二氧化钛复合光催化剂，包括金属锡卟啉和锐钛矿型二氧化钛，所述金属锡卟啉轴向复合在所述二氧化钛表面。卟啉的结构式为
本发明所述一种金属锡卟啉轴向功能化二氧化钛复合光催化剂的制备方法包括如下步骤：
将二氧化钛超声分散在极性有机溶剂中，分散均匀后，再加入吡啶和金属锡卟啉，进行亲核取代反应，反应结束后，将反应物经冷却、过滤、洗涤，干燥，得到白色粉末状产物，即为金属锡卟啉轴向功能化二氧化钛的复合光催化剂SnTpp/TiO2。
上述步骤中，所述二氧化钛和金属锡卟啉的质量比为2:8；所述的反应溶剂为吡啶，所述制备方法中超声时间均为1小时；所述反应的温度为60-90℃，优选90℃，反应时间为5-7天，优选为6天；
所述制备方法中所述分离为将反应液用0.45μm的尼龙膜进行过滤；所述洗涤为分别用去离子水和吡啶洗涤；所述干燥为真空室温下干燥24小时。
本发明的优点是：
(1)本发明的制备方法简单，反应条件简单，无须合成中间产品的多步骤反应，过程易于控制，适合扩大化生产的要求；
(2)本发明所制备的复合光催化剂光热稳定性好，活性高，无须引入助催化剂，可多次重复使用；
(3)本发明所制备的催化剂对可见光有很好的吸收，在可见光条件下对有机污染物罗丹明B在极短时间内即可获得良好的降解效果；
(4)本发明所制备复合光催化剂在可见光区对有机污染物罗丹明B表现出比金属锡卟啉和二氧化钛更好的光催化性能，为今后开发制备方法简单，光催化性能高的的复合催化剂提供了新的途径。
附图说明
图1是本发明方法制备的SnTpp/TiO2复合光催化剂与未敏化的TiO2光催化剂的XRD对比图；
图2是本发明方法制备的SnTpp/TiO2复合光催化剂降解罗丹明B水溶液随时间变化的紫外-可见光谱图；
图3是本发明方法制备的SnTpp/TiO2复合光催化剂、与对比例复合光催化剂、金属锡卟啉SnTpp、未敏化的TiO2光催化剂降解罗丹明B水溶液降解率随时间变化的曲线图。
具体实施方式
以下通过具体实施例对本发明进行描述或作进一步的说明，并且给出了详细的实施方式和具体的操作过程，其目的在于更好地理解本发明的技术内涵，但本发明的保护范围不限于下述的实施例。
实施例金属锡卟啉轴向功能化二氧化钛复合光催化剂SnTpp/TiO2的制备：
将二氧化钛(0.20g)超声1小时分散在极性有机溶剂吡啶(30mL)中，分散均匀后，再加入金属锡卟啉(0.80g)，进行亲核取代反应，搅拌，反应温度为90℃，反应时间为6天。反应结束后，待反应液冷却至室温，将反应液用0.45μm的尼龙膜进行过滤，再分别用去离子水和吡啶洗涤，然后室温真空干燥24小时得到白色粉末状产物，即为金属锡卟啉共价功能化的二氧化钛SnTpp/TiO2。
对比例称取一定量的反-二羟基-5，10，15，10-四苯基卟啉锡(SnTPP)为敏化剂，并溶解于二氯甲烷中。将0.20g超声1小时分散在极性有机溶剂吡啶(30mL)中的TiO2加入溶液中，搅拌，升温至50℃并保持，反应结束后，待反应液冷却至室温，用0.45μm的尼龙膜进行过滤，再分别用去离子水和吡啶洗涤，然后室温真空干燥24小时得到白色粉末状产物，即为对比例锡卟啉敏化二氧化钛。
下面通过应用实验对本发明中制备的金属锡卟啉轴向功能化二氧化钛纳米复合光催化剂在可见光下对罗丹明B水溶液的降解百分率说明复合光催化材料的效果。
为了验证本发明所制备金属锡卟啉轴向功能化二氧化钛纳米复合光催化剂SnTpp/TiO2的潜在应用性，发明人将其与对比例复合光催化剂、锐钛矿型TiO2、金属锡卟啉SnTpp在同一光源辐射下，做一系列对比。以罗丹明B水溶液为目标溶液，光催化实验采用的光源为400W卤钨灯。目标溶液置于200mL烧杯内，烧杯与灯垂直放置，二者之间的距离为10厘米。根据光照前后罗丹明B水溶液吸光度的变化计算得到降解百分率，对比结果如图3所示。
图3是用30mg金属锡卟啉轴向功能化二氧化钛纳米复合光催化剂SnTpp/TiO2、对比例复合光催化剂、锐钛矿型TiO2、金属锡卟啉SnTpp降解30mL 8mg/L罗丹明B溶液在光源下溶液吸光率随时间变化的曲线。从图3中可以看出，在400W卤钨灯照射条件下，本发明所制备的金属锡卟啉敏化二氧化钛复合光催化剂SnTpp/TiO2有比对比例复合光催化剂、金属锡卟啉SnTpp和无卟啉敏化催化剂二氧化钛TiO2更高的催化效果。可以看出，在金属锡卟啉为敏化剂和锐钛型二氧化钛为载体的协同作用下，本发明所制备的纳米复合光催化剂与现有催化剂相比，光催化效果显著提高。
本发明并不局限于前述的具体实施方式。本发明扩展到任何在本说明书中披露的新特征或任何新的组合，以及披露的任一新的方法或过程的步骤或任何新的组合。不能以此限定本发明实施的范围，故其等同组件的置换，或依本发明专利保护范围所作的等同变化与修改，皆应仍属本发明权利要求书涵盖之范畴。
Claims (7)
1.一种金属锡卟啉轴向功能化二氧化钛的复合光催化剂的制备方法，其特征在于由二氧化钛和金属锡卟啉反应制得，二氧化钛和金属锡卟啉的质量比为2:8，所述金属锡卟啉轴向共价修饰在二氧化钛表面；其中，金属锡卟啉的结构为：
其制备步骤为：
将二氧化钛超声分散在极性有机溶剂中，分散均匀后，再加入吡啶和所述金属锡卟啉，进行亲核取代反应，反应结束后，将反应物经冷却、过滤、洗涤，干燥，得到白色粉末状产物，即为金属锡卟啉轴向功能化二氧化钛的复合光催化剂SnTpp/TiO2；反应温度为60-90℃，反应时间为5-7天。
2.根据权利要求1所述的方法，所述二氧化钛的晶型为锐钛型。
3.根据权利要求2所述的方法，超声时间为1小时。
4.根据权利要求3所述的方法，反应温度为90℃，反应时间为6天。
5.根据权利要求4所述的方法，所述过滤为将反应液用0.45μm的尼龙膜进行过滤；所述洗涤为分别用去离子水和吡啶洗涤；所述干燥为真空室温下干燥24小时。
6.根据权利要求1-5任一方法所制备的金属锡卟啉轴向功能化二氧化钛复合光催化剂。
7.根据权利要求1-5任一方法所制备的金属锡卟啉轴向功能化二氧化钛复合光催化剂作为光催化处理有机污染物的绿色环保材料的应用。
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