CN112142111A - 一种离子液体辅助制备钨酸铋的方法及其产物与用途 - Google Patents
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Abstract
本发明提供了一种离子液体辅助制备钨酸铋的方法及其产物与用途，离子液体和硝酸铋溶于乙二醇中形成溶液；将钨酸钠溶于乙二醇中形成溶液；在磁力搅拌的作用下，将钨酸钠溶液缓慢滴加到离子液体和硝酸铋溶液中，搅拌均匀形成混合溶液；将混合溶液转移至聚四氟乙烯内衬高压反应釜，进行水热反应，控制温度160℃～180℃，反应结束后离心洗涤，干燥处理。所得钨酸铋的131晶面衍射峰半峰宽增加，可增强在可见光条件下催化降解挥发性有机物的效率。
Description
技术领域
本发明属于化工催化技术领域，具体涉及一种离子液体辅助制备钨酸铋的方法及其产物与用途。
背景技术
近年来，半导体光催化材料在环境净化、污染物处理方面引起了广泛关注。半导体材料在被能量大于等于其禁带宽度的光子激发下，产生激发态的光生电子与光生空穴并迁移到半导体表面，与吸附在半导体表面的挥发性有机物(VOCs)发生氧化还原反应，将其氧化降解成CO2、H2O等无机小分子。钨酸铋(Bi2WO6)是层状Aurivillius相氧化物半导体，由[WO6]2-和[Bi2O2]2+层交替组成，其禁带宽度较窄(约2.7eV)，易于被激发，层状结构可以加速光生电子-空穴的分离，而且光稳定性良好、无毒性。钨酸铋自身特殊的电子结构和良好的光电特性使其成为极具前景的半导体光催化材料。
离子液体与其他溶剂相比，具有以下优点：(1)液相温度范围宽，热稳定性好；(2)溶解范围较宽，溶解能力强。可溶解许多有机物、无机物等，并且具有催化性能；(3)几乎无蒸汽压，即使应用于较高温度下，也不易挥发；(4)粘度大，常温下离子液体的粘度要比水的大几十倍甚至几百倍；(5)导电性能好。因此，在无机材料的制备过程中加入离子液体可调控产物的尺寸，形貌和分散性，从而制备出不同性能的无机材料。
发明内容
本发明的目的在于提供一种离子液体辅助制备Bi2WO6的方法及其产物与用途，将离子溶液引入Bi2WO6的制备过程，作为分散剂和结构导向剂调节其结构性能，以得到具有优异光催化性能的Bi2WO6，应用于光催化降解VOCs。
本发明的目的通过以下技术方案实现：一种离子液体辅助制备Bi2WO6的方法，包括以下步骤：
(1)将离子液体和硝酸铋溶于乙二醇中形成溶液；将钨酸钠溶于乙二醇中形成溶液；
(2)在磁力搅拌的作用下，将钨酸钠溶液缓慢滴加到离子液体和硝酸铋溶液中，搅拌均匀形成混合溶液；
(3)将混合溶液转移至聚四氟乙烯内衬高压反应釜，进行水热反应，控制温度160℃～180℃，反应结束后离心洗涤，干燥处理。
优选的，所述步骤(1)中离子液体为四氟硼酸盐，加入量为0～30μL。
优选的，所述步骤(2)中钨酸钠溶液的滴加速率为20～30滴/min；混合溶液中钨酸钠与硝酸铋的摩尔比为1：2。
一种离子液体辅助制备Bi2WO6的方法的产物，所述产物Bi2WO6的131晶面衍射峰半峰宽增加。
一种离子液体辅助制备Bi2WO6的方法的产物的用途，所述产物Bi2WO6在可见光条件下催化降解VOCs。
与现有技术相比，本发明的有益效果为：
1)将离子溶液引入Bi2WO6的制备过程，作为分散剂和结构导向剂调节其结构性能，随着离子液体加入量的增加，所制得的Bi2WO6(131)衍射峰半峰宽相比于未加离子溶液所制得的样品有所增加，表明离子液体对Bi2WO6纳米晶体的生长有修饰作用。
2)将加入不同离子液体所得的Bi2WO6用于光催化降解VOCs。离子液体加入量为20μL时，制得的Bi2WO6 120min的甲苯降解率为未加入1-乙基-3-甲基咪唑四氟硼酸盐制得的Bi2WO6的191％，光催化降解效率显著提高。
附图说明
图1为实施例1和2所得产物的XRD图；
图2为实施例1和2所得产物的甲苯降解率。
具体实施方式
实施例1
将0.97g硝酸铋溶于30ml乙二醇溶液中磁力搅拌，0.3298g钨酸钠溶于20ml乙二醇中。在磁力搅拌的作用下将钨酸钠溶液缓慢滴加到硝酸铋混合溶液中，继续搅拌2h。将混合溶液移至聚四氟乙烯内衬高压反应釜，水热温度160℃，水热时间24h，反应结束， 10000rpm/min离心，用乙醇和蒸馏水交替洗涤三次，置于干燥箱中，设置干燥温度60℃，干燥处理12h。
实施例2
将20μl的1-乙基-3-甲基咪唑四氟硼酸盐和0.97g硝酸铋溶于30ml乙二醇溶液中磁力搅拌，0.3298g钨酸钠溶于20ml乙二醇中。在磁力搅拌的作用下将钨酸钠溶液缓慢滴加到硝酸铋混合溶液中，继续搅拌2h。将混合溶液移至聚四氟乙烯内衬高压反应釜，水热温度160℃，水热时间24h，反应结束，10000rpm/min离心，用乙醇和蒸馏水交替洗涤三次，置于干燥箱中，设置干燥温度60℃，干燥处理12h。
如图1所示，实施例2所得Bi2WO6样品均在2θo＝28.3°，32.8°，47.1°，55.8°，58.5°处出峰，分别对应斜方晶面Bi2WO6的(131)，(200)，(202)，(133)和 (262)晶面的特征峰。加入20μl1-乙基-3-甲基咪唑四氟硼酸盐所制得的Bi2WO6(131)衍射峰半峰宽相比于未加1-乙基-3-甲基咪唑四氟硼酸盐所制得的样品有所增加。表明1-乙基- 3-甲基咪唑四氟硼酸盐的加入对Bi2WO6的晶相基本没有影响，但对Bi2WO6纳米晶体的生长有修饰作用。
实施例3
将实施例1、2所得Bi2WO6平铺于光催化反应仪器底部，装填量为0.1g。充入甲苯气体(浓度100ppm/L)，以氮气为载气，并混合14％体积浓度的氧气。甲苯混合气体与Bi2WO6共同静置，并开启冷却装置，共同静置60min达到吸附脱附平衡。可见光光源1000W氙灯催化降解甲苯混合气体，并开启循环装置，反应每隔一段时间取样，反应前后甲苯浓采用气相色谱仪(GC6890)检测。
如图2所示，1-乙基-3-甲基咪唑四氟硼酸盐加入量为20μL时，制得的Bi2WO6120min的甲苯降解率为未加入1-乙基-3-甲基咪唑四氟硼酸盐制得的Bi2WO6的191％，光催化降解效率显著提高。
Claims (5)
1.一种离子液体辅助制备钨酸铋的方法，其特征在于，包括以下步骤：
（1）将离子液体和硝酸铋溶于乙二醇中形成溶液；将钨酸钠溶于乙二醇中形成溶液；
（2）在磁力搅拌的作用下，将钨酸钠溶液缓慢滴加到离子液体和硝酸铋溶液中，搅拌均匀形成混合溶液；
（3）将混合溶液转移至聚四氟乙烯内衬高压反应釜，进行水热反应，控制温度160℃～180℃，反应结束后离心洗涤，干燥处理。
2.如权利要求1所述的离子液体辅助制备钨酸铋的方法，其特征在于，所述步骤（1）中离子液体为四氟硼酸盐，加入量为0~30μL。
3.如权利要求1所述的离子液体辅助制备钨酸铋的方法，其特征在于，所述步骤（2）中钨酸钠溶液的滴加速率为20~30滴/min；混合溶液中钨酸钠与硝酸铋的摩尔比为1：2。
4.权利要求1至3任一项所述的离子液体辅助制备钨酸铋的方法的产物，其特征在于，所述产物钨酸铋的131晶面衍射峰半峰宽增加。
5.权利要求4所述的离子液体辅助制备钨酸铋的方法的产物的用途，其特征在于，所述产物钨酸铋在可见光条件下催化降解挥发性有机物。
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| CN101785995A (zh) * | 2010-02-05 | 2010-07-28 | 华中科技大学 | 一种可见光光催化剂Bi2WO6纳米结构的溶剂热制备方法 |
| CN102373507A (zh) * | 2010-08-27 | 2012-03-14 | 中国科学院过程工程研究所 | 一种咪唑类离子液体辅助水热合成Bi2WO6材料的方法 |
| CN105727932A (zh) * | 2016-03-10 | 2016-07-06 | 浙江大学 | 一种钨酸铋纳米光催化剂及其制备方法 |
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