CN113134349B - 一种蓝色层状Nb2O5光催化剂的制备方法及应用 - Google Patents
一种蓝色层状Nb2O5光催化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明提供了一种蓝色层状Nb2O5光催化剂的制备方法及应用,属于环境功能材料领域。所述蓝色层状Nb2O5光催化剂按下述方法制得:(1)将Nb2C MXene置于管式炉中,空气气氛下热处理,冷却至室温得到白色层状Nb2O5;(2)在还原性气氛中,将白色层状Nb2O5继续热处理1~5h,冷却至室温,得到蓝色Nb2O5光催化剂。本发明所述方法制备的蓝色层状Nb2O5光催化剂具有明显的层状结构,可增大催化剂与气体污染物的接触面积;表面有丰富的氧空位,可拓展其光吸收区域,促进电荷分离和使电子局域化,具有较高的光催化去除NO效率。
Description
技术领域
本发明属于环境功能材料领域,尤其是涉及一种蓝色层状Nb2O5光催化剂的制备方法及其在光催化去除NO中的应用。
背景技术
随着工业化和城市化进程的加快,空气污染已成为人类社会可持续发展面临的重要挑战。氮氧化物(NOx)是大气中的主要污染物之一,会引起缺氧、肺水肿和神经衰弱等身体疾病,并与光化学烟雾、酸雨、雾霾、臭氧层破坏等密切相关。NO为NOx的主要形态,在目前诸多NO去除方法中,光催化法具有设备简单、反应条件温和、能耗低、二次污染少等优点,成为研究的热点。
光催化剂是光催化处理NO技术的核心,主要为半导体或具有半导体性质的材料。传统的金属氧化物半导体如Nb2O5为白色颗粒,禁带宽度较大,可见光响应弱,且光生电子和空穴复合率高,导致对太阳光能利用率低。此外,用作光催化剂时,颗粒易堆积,影响催化活性位与反应气体接触。发明专利CN201911354599.8通过湿法化学处理手段,制备了蓝色的Nb2O5光催化剂,其能带结构发生改变,增强了对可见光和近红外光的吸收,提高了对太阳能的利用率。发明专利CN201310692528.5制备了氮掺杂棒状五氧化二铌光催化剂,具有大比表面积和较优长径比,有效抑制了光生电子和空穴复合,提高了催化剂的光能转换效率。因此,通过对Nb2O5光催化剂进行合理设计,改变其宏观构型和能带结构,可增强催化活性位与反应物接触,促进光生电子和空穴分离,提升光催化去除NO性能。
发明内容
有鉴于此,本发明旨在提出一种蓝色层状Nb2O5光催化剂的制备方法及应用,本发明的Nb2O5光催化剂通过氧化Nb2C MXene制备,方法工艺简单,操作方便,易于规模化生产;Nb2O5光催化剂保持了MXene的层状结构,比表面积远高于传统粉体Nb2O5,有利于反应气体与活性位的充分接触;本发明的Nb2O5光催化剂为蓝色,在可见光区内有明显的吸光度,光生电子和空穴的复合被明显抑制;本发明的光催化剂具有较高的光催化去除NO转化率,在气体污染物治理领域具有良好的应用前景。
为达到上述目的,本发明的技术方案是这样实现的:
一种蓝色层状Nb2O5光催化剂的制备方法,包括如下步骤:将Nb2C MXene置于管式炉中,升温至400~700℃,空气中热处理1~10h,冷却至室温得到白色层状Nb2O5;在还原性气氛中将白色层状Nb2O5升温至400~700 ℃,继续热处理1~5h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
高温下空气中热处理比较关键。温度过低,氧化效果不好;温度过高, Nb2O5晶型发生转变,催化活性下降。
进一步的,升温至400~700℃的升温速率为1~20℃/min,冷却至室温为自然冷却。
进一步的,还原性气氛为氢气与惰性气体的混合气,惰性气体为氮气、氩气、氦气中的一种,还原性气氛中氢气的体积分数为2~20%。
本发明的第二目的在于提出一种上述方法制得的蓝色层状Nb2O5光催化剂。
进一步的,所述Nb2O5光催化剂为蓝色,具有明显层状结构,表面有丰富的氧空位,在可见光区内有明显的吸光度。
商业化的粉末状Nb2O5比表面积3m2/g,本申请专利方法制备的层状 Nb2O5可达60m2/g。
本发明的第三目的在于提出一种上述蓝色层状Nb2O5光催化剂在光催化去除NO中的应用。
相对于现有技术,本发明所述的蓝色层状Nb2O5光催化剂的制备方法具有以下有益效果:
本发明从Nb2C MXene出发,在空气中热处理得到白色层状Nb2O5,再以还原性气氛热处理,在白色层状Nb2O5表面引入氧空位,制备蓝色层状 Nb2O5光催化剂;本发明制备方法工艺简单,操作方便,易于规模化生产;本发明制备的蓝色层状Nb2O5光催化剂表面有丰富的氧空位,可在禁带中提供中间能级拓展光吸收区域,并促进电荷分离和使电子局域化,有效增强光催化活性。同时,层状结构有利于提高比表面积,增加反应气体与催化活性位的接触,进一步提高光催化去除NO效率。
所制备的Nb2O5光催化剂具有明显的层状结构,可增强催化活性位与气体污染物的接触;所制备的Nb2O5光催化剂为蓝色,表面有丰富的氧空位,可拓展其光吸收区域,促进电荷分离和使电子局域化,具有较高的光催化去除NO效率;本发明制备方法工艺简单,操作方便,易于规模化生产。
所述光催化剂的应用与上述制备方法相对于现有技术所具有的优势相同,在此不再赘述。
附图说明
构成本发明的一部分的附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。在附图中:
图1是本发明实施例1制备蓝色层状Nb2O5光催化剂的扫描电镜照片;
图2是本发明实施例1制备蓝色层状Nb2O5光催化剂的X射线衍射图谱;
图3是本发明实施例1制备蓝色层状Nb2O5光催化剂的光催化去除NO 性能。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
下述实施例中所述试验方法,如无特殊说明,均为常规方法;所述试剂和材料,如无特殊说明,均可从商业途径获得。
一种蓝色层状Nb2O5光催化剂的制备方法,包括下述工艺步骤:
(1)制备白色层状Nb2O5:将Nb2C MXene置于管式炉中,以1~20℃/min 速率升温至400~700℃,空气中热处理1~10h,冷却至室温得到白色层状 Nb2O5。
(2)制备蓝色层状Nb2O5光催化剂:在含2~20%氢气的氮气、氩气、氦气等气氛中,将白色层状Nb2O5以1~20℃/min速率升温至400~700℃,继续热处理1~5h,冷却至室温,得到蓝色Nb2O5光催化剂。
下述实施例中,所述Nb2C MXene按下述方法制得:
取75mL浓盐酸,加入25mL去离子水中,配置100mL 9M盐酸;向配制的盐酸中加入8gLiF,600rpm下搅拌至完全溶解,形成混合溶液;向混合溶液中加入5g Nb2AlC,600rpm搅拌下于40℃反应96h;将反应后悬浊液200rpm离心1min,取上层液体在4000rpm离心10min,用去离子水将沉淀洗涤至中性,得到Nb2C MXene。
实施例1
(1)将Nb2C MXene置于管式炉中,以10℃/min速率升温至500℃,空气中热处理2h,冷却至室温得到白色层状Nb2O5。
(2)在含10%氢气的氩气气氛中将白色层状Nb2O5以5℃/min速率升温至700℃,继续热处理1h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对 500ppb NO进行处理,NO去除率高达62.2%。
实施例2
(1)将Nb2C MXene置于管式炉中,以5℃/min速率升温至600℃,空气中热处理8h,冷却至室温得到白色层状Nb2O5。
(2)在含8%氢气的氩气气氛中将白色层状Nb2O5以10℃/min速率升温至600℃,继续热处理2h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对 500ppb NO进行处理,NO去除率高达58.9%。
实施例3
(1)将Nb2C MXene置于管式炉中,以10℃/min速率升温至400℃,空气中热处理9h,冷却至室温得到白色层状Nb2O5。
(2)在含5%氢气的氩气气氛中将白色层状Nb2O5以10℃/min速率升温至600℃,继续热处理3h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对500ppb NO进行处理,NO去除率高达57.4%。
实施例4
(1)将Nb2C MXene置于管式炉中,以3℃/min速率升温至700℃,空气中热处理4h,冷却至室温得到白色层状Nb2O5。
(2)在含10%氢气的氩气气氛中将白色层状Nb2O5以5℃/min速率升温至700℃,继续热处理2h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对 500ppb NO进行处理,NO去除率高达59.3%。
实施例5
(1)将Nb2C MXene置于管式炉中,以5℃/min速率升温至600℃,空气中热处理5h,冷却至室温得到白色层状Nb2O5。
(2)在含10%氢气的氩气气氛中将白色层状Nb2O5以10℃/min速率升温至600℃,继续热处理2h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对 500ppb NO进行处理,NO去除率高达60.7%。
实施例6
(1)将Nb2C MXene置于管式炉中,以10℃/min速率升温至500℃,空气中热处理6h,冷却至室温得到白色层状Nb2O5。
(2)在含15%氢气的氩气气氛中将白色层状Nb2O5以5℃/min速率升温至600℃,继续热处理4h,冷却至室温,得到蓝色层状Nb2O5光催化剂。
(3)取0.1g蓝色Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对 500ppb NO进行处理,NO去除率高达61.5%。
对比例1
(1)在含15%氢气的氩气气氛中将商业化Nb2O5粉末以5℃/min速率升温至600℃,继续热处理2h,冷却至室温,得到粉末状Nb2O5光催化剂。
(3)取0.1g粉末状Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对500ppb NO进行处理,NO去除率为32.6%。
对比例2
(1)将Nb2C MXene置于管式炉中,以5℃/min速率升温至500℃,空气中热处理4h,冷却至室温得到白色层状Nb2O5。
(2)取0.1g白色层状Nb2O5光催化剂分散于5mL水中形成悬浊液,将悬浊液均匀滴涂在5cm×10cm的测试片上。室温干燥后,将测试片放入连续流动式光催化反应器中,以300W氙灯为模拟太阳光光源,在50%相对湿度下对500ppb NO进行处理,NO去除率为39.3%。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种蓝色层状Nb2O5光催化剂在光催化去除NO中的应用,其特征在于:所述蓝色层状Nb2O5光催化剂的制备方法包括如下步骤:将Nb2C MXene置于管式炉中,升温至400~700℃,空气中热处理1~10 h,冷却至室温得到白色层状Nb2O5;在还原性气氛中将白色层状Nb2O5升温至400~700℃,继续热处理1~5 h,冷却至室温,得到蓝色层状Nb2O5光催化剂;
所述还原性气氛为氢气与惰性气体的混合气,惰性气体为氮气、氩气和氦气中的一种,还原性气氛中氢气的体积分数为2~20%。
2.根据权利要求1所述的应用,其特征在于:两处所述升温至400~700 ℃的升温速率均为1~20 ℃/min,两处所述冷却至室温均为自然冷却。
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