CN109225313A - 一种Pt@CeO2/SBA-15复合光催化剂的制备方法与用途 - Google Patents
一种Pt@CeO2/SBA-15复合光催化剂的制备方法与用途 Download PDFInfo
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Abstract
本发明属于环境保护材料制备技术领域，提供一种Pt@CeO2/SBA‑15复合光催化剂的制备方法与用途。本发明包括(1)CeO2/SBA‑15催化剂的制备；(2)Pt@CeO2/SBA‑15复合催化剂的制备；本发明制备的Pt@CeO2/SBA‑15复合光催化剂用于降解废水中的2,4‑二氯苯酚；本发明所述的制备方法简单、不会造成资源浪费与二次污染的形成，是一种绿色环保高效污染处理技术。
Description
技术领域
本发明属于环境保护材料制备技术领域，涉及一种Pt@CeO2-SBA-15复合光催化剂的制备方法及其用途。
背景技术
氯酚作为有机化合物，被广泛应用于杀菌剂、木材预处理、染料、药物、除草剂等方面。工业中大量使用氯酚，是导致水污染的主要来源。大多数氯酚类化合物具有高毒性、致突变、致癌性、高持久性和环境中生物积累的特点，对人类健康具有巨大的潜在风险。因此，在许多国家，氯酚已被列为重要的优先污染物，2，4-二氯苯酚(DCP)是一种重要的有机化工中间产品，主要应用于生产农药，医药产品，助剂产品和增塑剂等，是一种有毒，生物难解降的有机污染物，又由于其化学性质稳定，不易被分解，容易在水中和土壤中富集，越来越多的这些化合物进入水体不仅会造成严重的水污染，而且会降低水质，并会给饮用水安全带来严重的问题。因此，寻求合理的处理方法来去除它们至关重要的。
酚类废水处理方法有氧化法(如臭氧氧化法)，物化法，生物法和光催化法。其中，半导体光催化还原法作为一种环境友好型，绿色无污染的处理技术被广泛应用。此外，半导体光催化剂在化工生产、能源转化、超级电容器和环境处理等方面引起了广泛的关注。一些新型半导体材料，如铋系半导体催化剂、碳基化合物、稀土氧化物、石墨烯基化合物、负载分子筛型光催化剂等，已发展为具有优良的光催化活性。CeO2作为稀土氧化物，具有独特的4f电子结构，较高的热稳定性和化学稳定性，近几年来收到人们的关注。由于CeO2具有氧空位(Ov)，在氧化还原条件下，氧空位(Ov)开始在表面上形成，这伴随着相邻Ce4+离子还原成Ce3 +。这种还原被认为有利于氧空位形成。此外，Ce3+和氧空位(Ov)可以作为许多催化反应的活性位点，提高光催化活性。但是，CeO2特别易于团聚，不利于与目标物充分接触，因此可以通过引入载体来提高其分散性。
SBA-15介孔材料具有高度有序的孔道结构、大的比表面积和孔径分布。利用其孔径来增加扩散速度，能够取得更好的催化效果。因此，可以用来作为新的催化剂或者催化剂载体。通过引入SBA-15模板，使CeO2分布在模板孔道内外表面，参与光降解2,4-二氯苯酚的作用。通过制备含铂纳米粒子的复合光催化剂来降解去除水体中的有机污染物也成为目前研究的热点。而目前还没有此类催化剂用于降解2,4-二氯苯酚。
发明内容
针对目前现有技术的空白，本发明通过引入贵金属，一方面增加电子的转移速率，降低光激电子-空穴对的重组率；另一方面，利用贵金属的局域表面等离子体共振效应提高光源利用率。本发明以煅烧法为技术手段，制备出Pt@CeO2-SBA-15复合光催化剂并用于光降解2,4-二氯苯酚。
本发明是通过以下技术手段实现上述技术目的。
一种Pt@CeO2/SBA-15复合光催化剂的制备方法，包括以下步骤
(1)CeO2/SBA-15催化剂的制备：
将六水硝酸铈Ce(NO3)3·6H2O和SBA-15加入去离子水中，搅拌混合均匀，然后放入真空干燥箱中干燥，将干燥好的粉末放入马弗炉中煅烧，即得到CeO2/SBA-15催化剂；
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将六水氯铂酸于纯净水中，得到氯铂酸水溶液；
称取步骤(1)制备的CeO2/SBA-15催化剂放入纯净水中，磁力搅拌一段时间；然后滴加氯铂酸水溶液，继续磁力搅拌一段时间后，放入真空干燥箱中干燥，然后将干燥的样品放入管式炉中，在氢气的氛围中煅烧，得到Pt@CeO2/SBA-15复合光催化剂。
步骤(1)中，所述六水硝酸铈和SBA-15的质量比为(0.0631～1)：1
步骤(1)中，所述煅烧温度为300-600℃，煅烧时间为2-4h。
步骤(1)中，所述搅拌混合的时间为12-36h。
步骤(2)中，所述氯铂酸水溶液的浓度为10g/L，所述氯铂酸和CeO2/SBA-15的质量比为(0.005～0.05)：1。
步骤(2)中，两次磁力搅拌的时间均为6h。
步骤(2)中，所述煅烧温度为400-650℃，煅烧时间为2-4h。
步骤(1)和(2)中，干燥温度均为60-80℃。
本发明所述Pt@CeO2/SBA-15的形貌为Pt纳米粒子分散在CeO2包裹的SBA-15上。
将本发明制备的Pt@CeO2/SBA-15复合光催化剂用于降解抗生素废水中的2,4-二氯苯酚的用途。
上述技术方案中去离子水用量为能使可溶性固体完全溶解。
2,4-二氯苯酚为标品，购买于阿拉丁股份有限公司。
本发明的有益效果：
(1)本发明利用贵金属Pt的局域表面等离子体共振效应提高催化剂对可见光的响应能力，提高复合催化剂对光的利用率。
(2)通过采用SBA-15为模板，使CeO2均匀的分散SBA-15的内外表面，一方面可以降低CeO2的团聚性，另一方面使氧化铈暴露更多的活性位点。
(3)本发明实现了以Pt@CeO2/SBA-15纳米复合材料作为光催化剂用于降解废水中2,4-二氯苯酚的目的。半导体作为光催化剂，在可见光下激发，利用电子和空穴的氧化还原过程将目标污染物降解为小分子物质，该方法不会造成资源浪费与二次污染的形成，且操作简便，是一种绿色环保处理技术。
附图说明
图1为CeO2、CeO2/SBA-15、Pt@CeO2/SBA-15复合光催化剂的XRD图。
图2为CeO2、CeO2/SBA-15、Pt@CeO2/SBA-15复合光催化剂的UV-vis图。
图3为Pt@CeO2/SBA-15复合光催化剂的TEM图。
具体实施方式
下面结合说明书附图以及具体实施实例对本发明做进一步说明。
本发明中所制备的光催化剂的光催化活性评价：在DW-01型光化学反应仪(购自扬州大学城科技有限公司)中进行，紫外-可见光灯照射下，将100mL的2,4-二氯苯酚模拟废水加入反应器中并测定其初始值，然后加入所制得的光催化剂，磁力搅拌并开启曝气装置通入空气保持催化剂处于悬浮或飘浮状态，光照过程中间隔30min取样分析，离心分离后取上层清液，在λmax＝284nm处用分光光度计测量吸光度，并通过公式：Dr＝[1-Ci/C0]×100％计算出降解率。其中C0为达到吸附平衡时2,4-二氯苯酚溶液的吸光度，Ci为定时取样测定的2,4-二氯苯酚溶液的吸光度。
实施例1：
(1)CeO2/SBA-15催化剂的制备：
将0.0631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌12h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.5mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉中，在氢气的氛围中煅烧2h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到23.53％。
实施例2：
(1)CeO2/SBA-15催化剂的制备：
将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌18h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.5mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉中，在氢气的氛围中煅烧2h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到44.94％。
实施例3：
(1)CeO2/SBA-15催化剂的制备：
将1.008g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.5mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉中，在氢气的氛围中煅烧2h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到60.87％。
实施例4
(1)CeO2/SBA-15催化剂的制备：
将1.262g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌36h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.5mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉，在氢气的氛围中煅烧2h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到55.24％。
实施例5：
(1)CeO2/SBA-15催化剂的制备：
将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中300℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.25mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入400℃的管式炉中，在氢气的氛围中煅烧4h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到37.23％。
实施例6：
(1)CeO2/SBA-15催化剂的制备：
将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中400℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.75mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉中，在氢气的氛围中煅烧4h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到46.89％。
实施例7：
(1)CeO2/SBA-15催化剂的制备：
将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中600℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加1.0mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入650℃的管式炉中，在氢气的氛围中煅烧4h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到55.23％。
实施例8：
(1)CeO2/SBA-15催化剂的制备：
将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将1g的六水氯铂酸溶于100mL的娃哈哈纯净水中，得到氯铂酸溶液；称取0.2g步骤(1)制备的CeO2/SBA-15催化剂放入100mL的烧杯中，加水磁力搅拌；然后滴加0.75mL氯铂酸水溶液，搅拌6h后，放入80℃真空干燥箱中干燥，然后将干燥的样品放入500℃的管式炉中，在氢气的氛围中煅烧2h，得到Pt@CeO2/SBA-15复合光催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到60.13％。
实施例9：
按实施例6中步骤，不同的是(1)中将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃中，在氢气的氛围中煅烧4h，即得到CeO2/SBA-15催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到63.69％。
实施例10：
按实施例2中步骤，不同的是(1)中将0.631g的六水硝酸铈(Ce(NO3)3·6H2O)和0.5g的SBA-15放入烧杯中，加入30mL去离子水搅拌24h混合均匀，然后放入60℃真空干燥箱中干燥，将干燥好的粉末放入马弗炉中500℃煅烧2h，即得到CeO2/SBA-15催化剂。
(3)取(2)中制备的样品0.1g在光化学反应仪中进行光催化降解实验，测得该催化剂对2,4-二氯苯酚的降解率在3h内达到78.12％。
图1为Pt@CeO2/SBA-15复合光催化剂的XRD图，图中展示了图中很清楚的展现了Pt的(111)特征峰。
图2为Pt@CeO2/SBA-15复合光催化剂的UV-vis图，可以看出Pt纳米粒子的存在提高了CeO2对可见光的响应能力。
图3为Pt@CeO2/SBA-15复合光催化剂的TEM图，本发明所述Pt@CeO2/SBA-15的形貌为Pt纳米粒子分散在CeO2包裹的SBA-15上。
上所述实施例为本发明的优选的实施方式，但本发明并不限于上述实施方式，在不背离本发明的实质内容的情况下，本领域技术人员能够做出的任何显而易见的改进、替换或变型均属于本发明的保护范围。
Claims (10)
1.一种Pt@CeO2-SBA-15复合光催化剂的制备方法，其特征在于，包括如下步骤：
(1)CeO2/SBA-15催化剂的制备：
将六水硝酸铈Ce(NO3)3·6H2O和SBA-15加入去离子水中，搅拌混合均匀，然后放入真空干燥箱中干燥，将干燥好的粉末放入马弗炉中煅烧，即得到CeO2/SBA-15催化剂；
(2)Pt@CeO2/SBA-15复合光催化剂的制备
将六水氯铂酸于纯净水中，得到氯铂酸水溶液；
称取步骤(1)制备的CeO2/SBA-15催化剂放入纯净水中，磁力搅拌一段时间；然后滴加氯铂酸水溶液，继续磁力搅拌一段时间后，放入真空干燥箱中干燥，然后将干燥的样品放入管式炉中，在氢气的氛围中煅烧，得到Pt@CeO2/SBA-15复合光催化剂。
2.根据权利要求2所述的一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(1)中，所述六水硝酸铈和SBA-15的质量比为(0.0631～1)：1。
3.根据权利要求2所述的一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(1)中，煅烧温度为300-600℃，煅烧时间为2-4h。
4.根据权利要求1所述得一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(1)中，所述六水硝酸铈和SBA-15搅拌混合的时间为12-36h。
5.根据权利要求1所述得一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(2)中，氯铂酸水溶液的浓度为10g/L，所述氯铂酸和CeO2/SBA-15的质量比为(0.005～0.05):1。
6.根据权利要求1所述得一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(2)中，两次磁力搅拌的时间均为6h。
7.根据权利要求1所述得一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(2)中，所述煅烧温度为400-650℃，煅烧时间为2-4h。
8.根据权利要求1所述得一种Pt@CeO2/SBA-15复合光催化剂的制备方法，其特征在于，步骤(1)和(2)中，干燥温度均为60-80℃。
9.根据权利要求1-8中任意一项所述制备方法得到的Pt@CeO2/SBA-15复合光催化剂，其特征在于，所述Pt@CeO2/SBA-15的形貌为Pt纳米粒子分散在CeO2包裹的SBA-15上。
10.将权利要求9所述的Pt@CeO2/SBA-15复合光催化剂用于降解废水中的2,4-二氯苯酚。
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| CN110252371A (zh) * | 2019-05-31 | 2019-09-20 | 江苏大学 | 一种用于光催化还原CO2的Pt@CeO2/3DCN复合光催化剂的制备方法 |
| CN111450827A (zh) * | 2020-04-20 | 2020-07-28 | 兰州大学 | 光催化剂及其制备方法 |
| CN111450827B (zh) * | 2020-04-20 | 2021-09-24 | 兰州大学 | 光催化剂及其制备方法 |
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