CN108654601A - 光致热驱动Pt-CNTs催化净化VOCs - Google Patents
光致热驱动Pt-CNTs催化净化VOCs Download PDFInfo
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Abstract
本发明公开了一种具有光致热催化净化VOCs（如甲苯）的碳纳米管负载铂的催化剂及其应用。该催化剂的制备方法包括：（1）将贵金属前驱体的水溶液与碳材料混合；（2）超声分散5~30 min；（3）50~80℃温度下搅拌加热5~8小时；（4）80~120℃烘箱中干燥6~8小时；（5）在10~100 mL/min的氢气氛围下，以2~10℃/min的速率升至200~400℃,保持2~4小时。所述贵金属铂和碳纳米管的质量比为0~3%。本发明的有益效果在于：（1）本发明制备的催化剂，在紫外、可见及红外光谱区域都有很强的吸收，能够将全波段光谱吸收并转化为热能，高效催化净化VOCs；（2）制备工艺简单，反应条件温和。
Description
技术领域
本发明属于一种催化剂材料及其制备方法和应用，具体涉及一种光催化降解气相挥发性有机物的碳纳米管负载贵金属铂的催化剂及其制备方法和应用。
背景技术
挥发性有机污染物（Volatile Organic Compounds, VOCs）（如甲苯等）不仅对环境造成严重的污染，还危害人体的健康。因此，挥发性有机污染物的控制和消除已经成为环保领域的研究热点。常见VOCs 消除的主要技术方法包括：吸附、冷凝、催化氧化、等离子体氧化、光催化氧化法和生物降解等。其中，光催化法利用光源照射催化剂，产生具有强氧化性的光生空穴、羟基自由基和超氧自由基，把VOCs降解为无害的CO2和H2O。直接利用太阳光驱动催化剂矿化净化VOCs，成为一种理想的环境污染治理技术。TiO2光催化剂因其便宜、无毒、稳定性等，被广泛应用。它的半导体带隙为3.2 eV，但其仅具有紫外光催化响应，无法利用可见光和红外光。
在太阳入射到地球的能量中，紫外光区域只占了5%（<400 nm），而剩下的区域是50%的可见光（400~780 nm）和45%的红外光（>780 nm）。近几十年来，人们一直致力于拓宽催化剂光谱的响应范围，包括: （1）改性TiO2等带隙较宽的紫外光催化剂如离子掺杂、金属沉积、半导体材料复合、表面光敏化等。Choi等（Journal of Physical Chemistry C. 2010,114, (2), 783-792.）制备贵金属Pt/TiO2；Yang等（J. Mater. Chem. 2010, 20, (25),5301-5309.）合成氮掺杂TiO2；Xiao等（ACS Appl. Mater. Interfaces. 2012, 4, (12),7054-7062.）制备ZnO/TiO2异质结。（2）探索新型窄带隙半导体光催化剂材料，如g-C3N4（Nat. Mater. 2009, 8, (1), 76-80），BiVO4（Nat. Commun. 2013, 4, 7.）。这些研究工作将光催化响应范围拓展到可见光区域，但占据太阳光能量44%的近红外光部分的研究较少。Li等（ACS Catal. 2015, 5, (6), 3278-3286.）通过制备TiO2/CeO2复合材料，在全光谱照射下，光热协同，对气相苯的降解表现出很好的催化活性。中国发明专利（CN201310285858.2）中发明了一种全光谱太阳光驱动隐锰钾矿纳米棒催化剂，在紫外、可见及红外光谱有很强的吸收，具有高效的紫外、可见、红外光及全光谱光致热催化降解VOCs的催化活性和良好的稳定性。
发明内容
本发明的目的在于提供一种具有有效利用全光谱，吸收光能并转化为热能，高效催化净化VOCs（如甲苯等）的催化剂。
本发明的高效的VOCs催化降解材料的制备方法为：
（1）称取定量的铂金属前驱物的水溶液，加入定量的碳纳米管，混合均匀，得到碳纳米管和铂金属前驱物水溶液的混合液；
（2）将碳纳米管和铂金属前驱物水溶液的混合液放置于超声器中，得到分散较好的碳纳米管和铂金属前驱物水溶液的混合液；
（3）将超声好的碳纳米管和铂金属前驱物水溶液的混合液放置于加热式搅拌器上，加热搅拌蒸干；
（4）取出干燥箱中的负载铂的碳纳米管，装至石英管内，在氢气气氛下还原，得到负载纳米铂的碳纳米管。
本发明的创新内容是，在全波段光源照射下，负载铂的碳纳米管对全光谱有很强的吸收，吸收的光能转化为热能，高效热催化氧化VOCs（如甲苯等）为CO2和H2O，且具有良好的催化稳定性。
本发明的有益效果是：
（1）该制备方法原料易得、工艺简单、易于工业化；
（2）无需外来加热装置就可以实现光热条件。负载纳米铂的碳纳米管能够充分吸收全光谱，将吸收的光能转化为热能，无需使用外来加热装置就可以实现高效催化净化VOCs。在该铂-碳纳米管催化剂的光反应中，不是半导体催化剂的光反应，而是新的光热作用，这种光热作用极大地提高了催化净化挥发性有机污染物的催化活性，即：碳纳米管吸收光能，转化为热能，氧气分子在纳米铂催化剂表面发生解离吸附形成具有高氧活性的吸附态氧原子，这些吸附态氧原子可以催化氧化有机污染物分子，从而实现催化氧化功能；
（3）催化剂在经过多次循环后，仍保持高效的催化活性和稳定性；
例如，以200 ppm的气相甲苯为降解底物评价催化剂活性，本发明合成的催化剂能够在短时间内降解甲苯，其降解率高达97%，矿化率高达84%，稳定性好，能够有效利用全光谱，制备简单，具有工业应用价值。
附图说明
下面结合附图及实施例对本发明作进一步描述：
图1是本发明实施例1,2,3,4所制备催化剂和纯CNTs的紫外可见漫反射谱对比图；
图2是本发明实施例1,2,3,4所制备催化剂和纯CNTs在光强为320 mW/cm2的全光谱氙灯光源照射下，催化剂降解甲苯的降解率变化对比图；
图3是本发明实施例1,2,3,4所制备催化剂和纯CNTs在光强为320 mW/cm2的全光谱氙灯光源照射下，催化剂降解甲苯的矿化率变化对比图；
图4是本发明实施例3所制备催化剂在氙灯全光谱照射下的温度变化图；
图5是本发明实施例3所制备催化剂在不同滤光片的氙灯和红外灯照射下，催化剂降解甲苯的降解率变化对比图；
图6是本发明实施例3所制备催化剂在不同滤光片的氙灯和红外灯照射下，催化剂降解甲苯的矿化率变化对比图；
图7是本发明实施例3所制备催化剂外部供热时的甲苯的降解率和矿化率变化图，其供热温度与全光谱照射时催化剂表面的温度相同；
图8是本发明实施例3所制备催化剂在氙灯全光谱照射下，催化剂降解甲苯的降解率与催化剂循环使用次数的关系图。
具体实施方式
实施例1
量取0.1317 mL H2PtCl6水溶液（3.8 g/L），用20 mL超纯水稀释，称取0.5 g CNTs，混合，超声10分钟，80 ℃条件下搅拌蒸干6小时，放置在100℃烘箱中，干燥8小时后，在50 mL/min的氢气气氛下，以5 ℃/min，升至250℃保持2小时，所得碳纳米管负载Pt以总质量计，其中Pt占0.1%，即0.1wt% Pt-CNTs。
实施例2
量取0.6612 mL H2PtCl6水溶液（3.8 g/L），用20 mL超纯水稀释，称取0.5 g CNTs，混合，超声10分钟，80 ℃条件下搅拌蒸干6小时，放置在100 ℃烘箱中，干燥8小时后，在50mL/min的氢气气氛下，以5 ℃/min，升至250 ℃，保持2小时，所得碳纳米管负载Pt以总质量计，其中Pt占0.5%，即0.5wt% Pt-CNTs。
实施例3
量取1.3291 mL H2PtCl6水溶液（3.8 g/L），用20 mL超纯水稀释，称取0.5 g CNTs，混合，超声10分钟，80 ℃条件下搅拌蒸干6小时，放置在100 ℃烘箱中，干燥8小时后，在50mL/min的氢气气氛下，以5 ℃/min，升至250 ℃，保持2小时，所得碳纳米管负载Pt以总质量计，其中Pt占1%，即1wt% Pt-CNTs。
实施例4
量取4.0690 mL H2PtCl6水溶液（3.8 g/L），用20 mL超纯水稀释，称取0.5 g CNTs，混合，超声10分钟，80 ℃条件下搅拌蒸干6小时，放置在100 ℃烘箱中，干燥8小时后，在50mL/min的氢气气氛下，以5 ℃/min，升至250 ℃，保持2小时，所得碳纳米管负载Pt以总质量计，其中Pt占3%，即3wt% Pt-CNTs。
实施例5
由佛山德力梅塞尔气体有限公司提高的纯化空气分为两条支路，分别流经甲苯发生器（冰水浴20 ℃）与空白路，汇合于内体积为9 L的不锈钢混合罐内。用质量流量计控制气体流速，用Online GC检测，通过调节，即可得所需的甲苯浓度。
实施例6
通过测试样品对气相甲苯的降解率和矿化率来评价其活性，所用的反应器是一个定制的容积为40 mL的石英反应器。实验前，称取50 mg样品与3 mL无水乙醇混合，超声分散均匀，采用砂芯过滤的方法使其均匀涂布于玻璃纤维膜上（φ50 mm），40 ℃烘干。将干燥的玻璃纤维膜放置反应器内，气相甲苯通过反应器进行反应，反应时所用光源为北京泊菲莱科技有限公司生产的PLS-SXE300型氙灯和PHILIPS公司生产的IR375CH IR2型红外灯，反应过程中甲苯的浓度变化和最终产物CO2的生成由Online GC进行在线检。甲苯降解率（%）=100*（[甲苯]入口-[甲苯]出口）/[甲苯]入口；甲苯矿化率（%）=100*（[甲苯]入口-[甲苯]出口）/（7*[甲苯]入口）。
Claims (8)
1.碳材料负载贵金属铂的催化剂的制备方法，其特征在于其步骤如下：
（1）称取定量的铂金属前驱物的水溶液，加入定量的碳纳米管，混合均匀，得到碳纳米管和铂金属前驱物水溶液的混合液；
（2）将碳纳米管和铂金属前驱物水溶液的混合液放置于超声器中，得到分散较好的碳纳米管和铂金属前驱物水溶液的混合液；
（3）将超声好的碳纳米管和铂金属前驱物水溶液的混合液放置于加热式搅拌器上，加热搅拌蒸干；
（4）将装有负载铂粒子的碳纳米管的烧杯放置于烘箱中，干燥；
（5）取出干燥箱中的负载铂的碳纳米管，装至石英管内，在氢气气氛下还原，得到负载纳米铂的碳纳米管。
2.根据权利要求1所属的方法，其特征在于：所述步骤（1）中贵金属铂和碳纳米管的质量比为0~3%。
3.根据权利要求1所属的方法，其特征在于：所述步骤（2）中的超声时间为5~30分钟。
4.根据权利要求1所属的方法，其特征在于：所述步骤（3）中的搅拌蒸干温度为50~80℃，搅拌时间为5~8小时。
5.根据权利要求1所属的方法，其特征在于：所述步骤（4）中烘箱干燥温度为80~120℃，干燥时间为6~8小时。
6.根据权利要求1所属的方法，其特征在于：所述步骤（5）中氢气流量为10~100 mL/min。
7.根据权利要求1所属的方法，其特征在于：所述步骤（5）中氢气还原程序升温速率为2~10 ℃/min，升至200~400 ℃，保持2~4小时。
8.根据权利要求1所述方法制备的催化剂的应用，其特征在于：
（1）在全波段光谱照射下，催化剂吸收光能并转化为热能；
（2）对VOCs（如甲苯）具有高效的降解率和矿化率。
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| CN114566663A (zh) * | 2022-01-18 | 2022-05-31 | 陈九廷 | 一种燃料电池阴极用多层碳纳米管催化剂及其制备方法 |
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