CN107200351A - 钒酸铋纳米棒的制备方法 - Google Patents
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Abstract
本发明公开了一种钒酸铋纳米棒的制备方法，包括以下步骤：1)将Bi(NO3)3·5H2O溶于硝酸溶液中，得到A溶液；2)将NH4VO3溶于氨水溶液中，得到B溶液；3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至6.5～8，继续搅拌30～120min，得到混合液；4)向混合液中加入乙二胺四乙酸钠，搅拌，调节PH至8～9，搅拌15～60min后，超声分散，得到前驱液；5)将前驱液加入到高压反应釜中，在160～200℃的条件下进行水热反应，反应时间为3～10h，冷却，过滤，将沉淀物洗涤，离心，干燥，得到钒酸铋纳米棒。本发明制得的钒酸铋纳米棒尺寸小，比表面积大，光催化活性高。
Description
技术领域
本发明涉光催化降解有机污染物技术领域，具体涉及一种钒酸铋纳米棒的制备方法。
背景技术
环境污染问题已成为全球问题，不但阻碍社会的快速发展而且威胁着人类健康。在各种环境污染中，化学污染影响最大。光催化技术在室温下可实现，而且利用太阳能，成本低廉，安全环保。半导体材料均具有光催化活性，光催化反应的机理也逐渐被人们认知。在众多半导体光催化剂材料中，二氧化钛最典型，它具有氧化性强，光诱导性好，亲水性好，稳定无毒等优点，在治理环境问题方面有很好的应用。然而，二氧化钛也有其局限性。光生电子-空穴对的复合几率较高，禁带宽度较大，这些不利特性严重阻碍了二氧化钛在光催化氧化领域的推广和应用。
单斜晶相钒酸铋的禁带宽度为2.3-2.4eV，它足够高的价带完全可以实现空穴对有机污染物的降解，并且导带位置也有利于光生电子的还原，具有较高的氧化能力，且其价带氧化电位位于2.4eV附近，从理论上将，能够实现在可见光下分解水和降解有机污染物的目标。钒酸铋的光催化性能与其自身晶体结构、晶粒尺寸以及颗粒形貌有很大的关系。由于常规的钒酸铋晶体粒径大，导致光生电子和空穴迁移到催化剂表面的传输距离长，容易在长距离迁移过程中发生复合，降低光催化效率。其次，常规钒酸铋晶体比表面积小，不能有效吸附污染物，也大大降低了光催化效率。
发明内容
本发明所要解决的技术问题是提供一种钒酸铋纳米棒的制备方法，该方法制得的钒酸铋纳米棒尺寸小，比表面积大，催化活性强。
本发明提供的技术方案是一种钒酸铋纳米棒的制备方法，包括以下步骤：
1)将Bi(NO3)3·5H2O溶于1～4mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于1～4mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至6.5～8，继续搅拌30～120min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，搅拌，调节PH至8～9，搅拌15～60min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在160～200℃的条件下进行水热反应，反应时间为3～10h，冷却，过滤，将沉淀物洗涤，离心，干燥，得到钒酸铋纳米棒。
步骤4)中，所述乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的3～5倍。
步骤1)中，硝酸溶液的浓度为3～4mol/L。
步骤2)中，氨水溶液浓度为2～2.5mol/L。
步骤5)中，所述洗涤是将沉淀物用去离子水和/或乙醇洗涤。
步骤5)中，所述干燥是在40～100℃下干燥4～24h。
与现有技术相比，本发明具有以下有益效果：
1)在碱性条件下,OH-中的O原子的孤对电子会与钒酸铋晶核{010}晶面作用，使得{010}晶面带负电荷，这些带负电荷的晶面通过静电吸附作用，吸附乙二胺四乙酸钠，而乙二胺四乙酸容易与Bi3+形成配合物，从而引导Bi3+与VO3 3-组装在{010}晶面，使得钒酸铋晶体具有{010}取向。最终制得的催化剂的形貌为棒状，该纳米棒直径为20～30nm，长径比为20～40，对可见光有很好的吸收。
2)钒酸铋催化剂具有{010}取向，光生电子会聚集在纳米棒的两端，不仅提高了空穴的分离效率，空穴更稳定的分部在纳米棒侧面，非常有利于有机物的降解。
3)钒酸铋具有{010}取向，而{010}晶面活性高，产生的光生电子氧化能力最强，因而具有{010}取向的钒酸铋纳米棒光催化活性最强。
4)本发明制得的钒酸铋催化剂晶体尺寸小，能够缩短光生电子和空穴迁移到催化剂表面的传输距离，提高光生电子空穴存活率。
附图说明
图1是实施例1所制备的钒酸铋纳米棒在透射电镜下的形貌图；
图2是实施例1所制备的钒酸铋纳米棒的高分辨率图；
图3是实施例1所制备的钒酸铋纳米棒的XRD谱图；
图4是实施例1所制备的钒酸铋纳米棒在可见光条件下降解罗丹明B的速率常数对比，参考为商业性的Degussa P25为光催化剂时的速率常数。
具体实施方式
以下具体实施例对本发明作进一步阐述，但不作为对本发明的限定。
实施例1
1)将Bi(NO3)3·5H2O溶于1mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于1mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至6.5，继续搅拌30～120min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的3倍，搅拌，调节PH至8，搅拌15min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在160℃的条件下进行水热反应，反应时间为3h，冷却，过滤，将沉淀物用去离子水和/或乙醇洗涤洗涤3次，离心，在40℃下干燥4h，得到钒酸铋纳米棒。
由图1可知，钒酸铋纳米棒分散性良好，直径约为20nm,长径比为20～40。由图2可知，垂直于纳米棒生长方向的晶面的晶面间距与钒酸铋{040}晶面间距相吻合，证明该钒酸铋纳米棒是沿着{010}方向延伸的。由图3可知，钒酸铋纳米棒XRD图谱与单斜白钨矿相钒酸铋的标准谱图相比完全吻合，说明实施例1的纳米棒为单斜白钨矿结构。由图4可知，本实施例的纳米棒对罗丹明B的降解速率是P25的89倍，具有非常优越的光催化性能。
实施例2
1)将Bi(NO3)3·5H2O溶于4mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于4mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至8，继续搅拌120min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的5倍，搅拌，调节PH至9，搅拌60min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在200℃的条件下进行水热反应，反应时间为10h，冷却，过滤，将沉淀物用去离子水和/或乙醇洗涤洗涤5次，离心，在100℃下干燥24h，得到钒酸铋纳米棒。
透射电镜结果表明钒酸铋纳米棒为纳米棒状，分散性良好，直径为30nm，长径比为20～40，并沿着{010}方向延伸。X射线衍射结果表明为单斜白钨矿相。
实施例3
1)将Bi(NO3)3·5H2O溶于3mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于2mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至7.5，继续搅拌90min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的4倍，搅拌，调节PH至8.5，搅拌45min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在180℃的条件下进行水热反应，反应时间为6h，冷却，过滤，将沉淀物用去离子水和/或乙醇洗涤洗涤4次，离心，在80℃下干燥12h，得到钒酸铋纳米棒。
透射电镜结果表明钒酸铋纳米棒为纳米棒状，分散性良好，直径为25nm，长径比为20～40，并沿着{010}方向延伸。X射线衍射结果表明为单斜白钨矿相。
实施例4
1)将Bi(NO3)3·5H2O溶于4mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于2.5mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至6.5，继续搅拌120min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的3倍，搅拌，调节PH至9，搅拌15min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在200℃的条件下进行水热反应，反应时间为3h，冷却，过滤，将沉淀物用去离子水和/或乙醇洗涤洗涤5次，离心，在40℃下干燥24h，得到钒酸铋纳米棒。
透射电镜结果表明钒酸铋纳米棒为纳米棒状，分散性良好，直径为25nm，长径比为20～40，并沿着{010}方向延伸。X射线衍射结果表明为单斜白钨矿相。
Claims (6)
1.钒酸铋纳米棒的制备方法，其特征在于：包括以下步骤：
1)将Bi(NO3)3·5H2O溶于1～4mol/L的硝酸溶液中，得到A溶液；
2)将与Bi(NO3)3·5H2O等摩尔量的NH4VO3溶于1～4mol/L的氨水溶液中，得到B溶液；
3)将A溶液缓慢加入到B溶液中，搅匀，调节pH至6.5～8，继续搅拌30～120min，得到混合液；
4)向混合液中加入乙二胺四乙酸钠，搅拌，调节PH至8～9，搅拌15～60min后，超声分散，得到前驱液；
5)将前驱液加入到高压反应釜中，在160～200℃的条件下进行水热反应，反应时间为3～10h，冷却，过滤，将沉淀物洗涤，离心，干燥，得到钒酸铋纳米棒。
2.根据权利要求1所述的钒酸铋纳米棒的制备方法，其特征在于：步骤4)中，所述乙二胺四乙酸钠的加入量为Bi(NO3)3·5H2O重量的3～5倍。
3.根据权利要求1所述的钒酸铋纳米棒的制备方法，其特征在于：步骤1)中，硝酸溶液的浓度为3～4mol/L。
4.根据权利要求1所述的钒酸铋纳米棒的制备方法，其特征在于：步骤2)中，氨水溶液浓度为2～2.5mol/L。
5.根据权利要求1所述的钒酸铋纳米棒的制备方法，其特征在于：步骤5)中，所述洗涤是将沉淀物用去离子水和/或乙醇洗涤。
6.根据权利要求1所述的钒酸铋纳米棒的制备方法，其特征在于：步骤5)中，所述干燥是在40～100℃下干燥4～24h。
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