CN112642447A - 一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法 - Google Patents
一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法 Download PDFInfo
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Abstract
光催化技术已被广泛用作一种经济有效且环保的高级氧化过程，广泛用于环境污水处理环节中。具有Aurivilius‑Sillén结构的Bi4NbO8Cl材料作为一种新型的铋基氯氧化物光催化剂，其独特的层状分子结构有利于光生载流子的分离，拥有良好的光催化性能。然而由于Bi4NbO8Cl的禁带宽度仍达到约2.5eV，使其只能对波长约为500nm以下的蓝紫可见光区域响应。本发明采用熔盐法制备的Bi4NbO8Cl为基体，利用化学沉淀法制备了Ag2S负载的Bi4NbO8Cl复合光催化材料，拓展了Bi4NbO8Cl材料的光响应范围，同时Ag2S‑Bi4NbO8Cl异质结构的构建加强了光生电荷的分离，提高了光催化降解医疗废水的效率。
Description
技术领域：
本发明涉及一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，具体地说，采用熔盐法制备Bi4NbO8Cl片层结构为基体，利用银氨络合物构建Ag+-Bi4NbO8Cl之间的强相互作用，采用化学沉淀法制备Ag2S纳米颗粒，通过调控Ag2S不同的负载量，拓展了光催化剂的光响应范围和提高了光催化降解医疗废水的效率，本技术属于光催化材料制备领域。
背景技术：
随着世界人口老龄化进程和医疗产业的快速增长，医疗废水对环境污染已经成为一个严重的问题。医疗废水除了含有高致病性、高传染度的病毒病菌外，也含有较多的人体排出的抗生素物质。因此，严格处理医疗废水中残留抗生素对保护生态环境和人体健康具有重要意义。
光催化技术已被广泛用作一种经济有效且环保的高级氧化过程，以去除有害的环境污染物。传统的半导体催化剂如TiO2、ZnO等，只能对约占太阳光谱5％的紫外线响应，而对分别约占49％和46％的可见光和近红外光无响应能力。因此，拓展光催化剂的光谱响应范围成为一个具有挑战性的课题。
近年来的研究发现，具有Aurivilius-Sillén结构的Bi4NbO8Cl材料作为一种新型的铋基氯氧化物光催化剂，是由[Bi2O2]2+层、[NbO4]3-层和[Cl]-层组成，这种独特的层状分子结构有利于光生载流子的分离，从而提高催化剂的光催化性能。由于Bi4NbO8Cl的价带和导带都具有很强的Bi 6s轨道和O 2p轨道杂化，这种特性可以缩小带隙，提供可见光吸收和较高的光稳定性。然而，其约2.5eV的禁带宽度只能使得该光催化材料对约500nm以下的蓝紫可见光区域响应。因此，进一步通过对Bi4NbO8Cl材料改性以提高光响应范围势在必行。
硫化银(Ag2S)具有极小的光学带隙(0.9eV)，拥有良好的对近红外光响应性能。然而，正是由于该特有的能带间隙和结构，Ag2S具有较快的光生电荷复合率和较弱的氧化还原电位，难以单独作为光催化剂使用。因此，我们设计了一种Ag2S负载Bi4NbO8Cl复合光催化剂的制备方法，使得Ag2S拓展了光催化剂的光响应范围，同时Ag2S-Bi4NbO8Cl异质结构的构建加强了光生电荷的分离，提高了光催化降解医疗废水的效率。
发明内容：
本发明采用化学沉淀法，制备出一种性能优异的Ag2S-Bi4NbO8Cl复合可见光催化剂。
本发明是通过如下技术方案实现的：
一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，按以下步骤进行：
(1)Bi4NbO8Cl粉体的制备：室温下，分别称取物质的量为0.1mol的NaCl和KCl，放入玛瑙研钵中；再依次称取0.01mol的BiOCl、0.005mol的Nb2O5和0.015mol的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；进一步将上述混合物转移到玛瑙球磨罐中，同时加入10mm的玛瑙球，封闭球磨罐放置在行星球磨机中球磨2h，转速为300rpm；将球磨完毕的粉末转移到刚玉坩埚中，在马弗炉中煅烧一定时间，并保持一定的升温速率；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1mol/L的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体；
(2)配置银氨络合物溶液：取5mmol的AgNO3溶于50mL的去离子水中，将一定体积浓度的稀氨水溶液逐滴加入到上述AgNO3溶液中并震荡，直至最初产生的沉淀刚好溶解消失；将该银氨络合物溶液定容至100mL；
(3)称取物质的量为0.5mmol步骤(1)中制备的Bi4NbO8Cl粉体，分散到50mL去离子水中，超声处理10min使其均匀分散；将一定量配置好的银氨溶液滴加到上述悬浮液中，并持续搅拌30min；将一定量浓度为0.02mmol/L的Na2S的溶液逐滴加入到上述悬浮液中，避光搅拌3h；其中，银氨溶液的加入量为0.2mL-4.0mL，Na2S溶液的加入量按照n(S):n(Ag)＝1:2，为0.25mL-5.0mL；
(4)对(3)中的悬浮液10000rpm离心处理，收集沉淀，并依次用去离子水和乙醇对沉淀各洗涤3次；将收集的沉淀在60℃的鼓风干燥箱中干燥24h，收集粉末，即得到Ag2S-Bi4NbO8Cl。
优选的，步骤(1)中所述的煅烧温度为600-800℃，煅烧时间为0.5-5h，升温速率为2-5℃/min。
优选的，步骤(2)中所述的稀氨水的体积浓度为1％-5％。
优选的，步骤(3)中所述的银氨溶液的加入量(VAg)为0.2mL-4.0mL，硫化钠的加入量(VS)为0.25mL-5.0mL，且始终保持VAg：VS＝1：1.25。
与现有技术相比，本发明的有益效果：
本发明中使用熔盐法制备的Bi4NbO8Cl片状结构为基体，利用银氨络离子与Bi4NbO8Cl之间的强相互作用，采用化学沉淀法制备Ag2S纳米颗粒，制备Ag2S-Bi4NbO8Cl复合光催化材料，拓展了光催化材料的光响应范围和光催化活性。本发明以Bi4NbO8Cl可见光响应的光催化剂为基础，通过负载红外光窄带隙Ag2S半导体纳米颗粒并调控其在复合物中的比例，得到了红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂，用于光催化降解医疗废水的领域，取得了良好的效果，当VAg＝2.0mL和VS＝2.5mL时，Ag2S-Bi4NbO8Cl对目标污染物盐酸四环素的光催化降解效率最优。
附图说明：
图1为本发明制备的不同比例Ag2S负载的Bi4NbO8Cl复合光催化剂的XRD图。
图2为实施例1所制备样品的SEM图。
图3为本发明制备的不同比例Ag2S负载的Bi4NbO8Cl复合光催化剂的DRS图。
图4为实施例1制备的复合光催化剂与基体在近红外光照射下对盐酸四环素的降解曲线图。
具体实施方式：
实施例1：
室温下，分别称取物质的量为0.1mol的NaCl和KCl，放入玛瑙研钵中；再依次称取0.01mol的BiOCl、0.005mol的Nb2O5和0.015mol的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；进一步将上述混合物转移到玛瑙球磨罐中，同时加入10mm的玛瑙球，封闭球磨罐放置在行星球磨机中球磨2h，转速为300rpm；将球磨完毕的粉末转移到刚玉坩埚中，在马弗炉中750℃煅烧1h，并保持3°/min升温速率；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1M的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体。
称取物质的量为0.5mmol的Bi4NbO8Cl粉体，分散到50mL去离子水中，超声处理10min使其均匀分散；将2.0mL预先配置好的0.05mol/L银氨溶液滴加到上述悬浮液中，并持续搅拌30min；将2.5mL浓度为0.02mmol/L的Na2S的溶液逐滴加入到上述悬浮液中，避光搅拌3h；将悬浮液10000rpm离心处理，收集沉淀，并依次用去离子水和乙醇对沉淀各洗涤3次；将收集的沉淀在60℃的鼓风干燥箱中干燥24h，收集粉末，即得到Ag2S-Bi4NbO8Cl。按照理论计算生成的Ag2S和Bi4NbO8Cl的物质的量之比为0.10:1，将该样品标记为AB-10。
实施例2：
本实施例与实施例1不同之处在于：
加入的银氨溶液的体积为0.4mL，加入Na2S的溶液的体积为0.5mL。最终得到的Ag2S-Bi4NbO8Cl中Ag2S和Bi4NbO8Cl的物质的量之比为0.02:1，因此该实施例得到的样品标记为AB-2。
Claims (4)
1.一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，其特征在于，按以下步骤进行：
(1)Bi4NbO8Cl粉体的制备：室温下，分别称取物质的量为0.1mol的NaCl和KCl，放入玛瑙研钵中；再依次称取0.01mol的BiOCl、0.005mol的Nb2O5和0.015mol的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；进一步将上述混合物转移到玛瑙球磨罐中，同时加入10mm的玛瑙球，封闭球磨罐放置在行星球磨机中球磨2h，转速为300rpm；将球磨完毕的粉末转移到刚玉坩埚中，在600-800℃马弗炉中煅烧，保温时间为0.5-5h，并保持升温速率为2-5℃/min；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1mol/L的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体；
(2)配置银氨络合物溶液：取5mmol的AgNO3溶于50mL的去离子水中，将一定体积浓度的稀氨水溶液逐滴加入到上述AgNO3溶液中并震荡，直至最初产生的沉淀刚好溶解消失；将该银氨络合物溶液定容至100mL；
(3)称取物质的量为0.5mmol步骤(1)中制备的Bi4NbO8Cl粉体，分散到50mL去离子水中，超声处理10min使其均匀分散；将一定量配置好的银氨溶液滴加到上述悬浮液中，并持续搅拌30min；将一定量浓度为0.02mmol/L的Na2S的溶液逐滴加入到上述悬浮液中，避光搅拌3h；
(4)对(3)中的悬浮液10000rpm离心处理，收集沉淀，并依次用去离子水和乙醇对沉淀各洗涤3次；将收集的沉淀在60℃的鼓风干燥箱中干燥24h，收集粉末，即得到Ag2S-Bi4NbO8Cl。
2.如权利要求1所述的一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，其特征在于，步骤(2)中稀氨水的体积浓度为1％-5％。
3.如权利要求1所述的一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，其特征在于，步骤(3)中银氨溶液的加入量为0.2mL-4.0mL。
4.如权利要求1所述的一种近红外光响应的Ag2S-Bi4NbO8Cl复合光催化剂的制备方法，其特征在于，步骤(3)中Na2S溶液的加入量为0.25mL-5.0mL，且Na2S溶液与银氨溶液的体积之比始终保持为1.25比1。
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