CN105597738B - 一种可见光光催化剂钨酸铋纳米晶片及其制备方法 - Google Patents
一种可见光光催化剂钨酸铋纳米晶片及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种可见光光催化剂钨酸铋纳米晶片，其制备方法包括以下步骤：1)将硝酸铋和甘油在异丙醇溶剂，进行溶剂热反应，经过滤、洗涤、烘干得甘油铋；2)将所得甘油铋均匀分散于钨酸钠水溶液中，调节所得溶液体系的PH值为0‑2，然后进行水热反应，经过滤、洗涤、烘干制得纳米钨酸铋。本发明以硝酸铋、甘油、钨酸钠为主要原料，采用两步法制备钨酸铋纳米晶片粉体，涉及的制备工艺设备简单、反应条件温和、能耗小，工艺独特新颖，所得产品钼酸铋钠的晶粒尺寸在20‑40nm，可直接用作光催化剂，能在可见光下光催化降解有机污染物。
Description
技术领域
本发明属于环保新材料领域，具体涉及一种可见光光催化剂纳米钨酸铋及其制备方法。
背景技术
光催化反应几乎能降解所有的有机污染物，如烷烃、卤代烷烃、醇、羧酸、烯、芳香烃、卤代芳香化合物、聚合物、杀虫剂、除草剂、染料以及溴代阻燃剂、消毒副产物等污染物。因此光催化技术被认为是理想的环境治理的新技术，是控制环境污染最具前景的一种手段，特别是可见光光催化降解污染物的处理技术，它利用自然界的太阳光，不需要额外的能量消耗。传统的TiO2光催化剂主要吸收紫外光，对太阳光的利用率低。
纳米钨酸铋(Bi2WO6)是近几年兴起的、受到广泛关注度的一种可见光半导体催化剂，它在可见光下具有良好的光催化活性。Bi2WO6在可见光下能有效降解有机污染物(RhB、苯酚、乙醛、抗生素类等)将其矿化，同时还能有效地利用CO2和水在催化作用下生成燃料。纳米钨酸铋是被认为是很有潜力的可见光响应型半导体光催化材料之一。目前为纳米钨酸铋材料，主要利用氧化铋和氧化钨进行固相反应，或以硝酸铋和钨酸钠为原料采用共沉淀法、溶胶凝胶法或水热法制备而成；普遍存在产物纯度不高，反应温度高或晶粒尺寸难以控制等缺点。因此开发一种制备方法简单、能耗低、纯度高，纳米晶片细小、光催化活性高的钨酸铋纳米材料具有重要意义。
发明内容
本发明的目的是提供一种可见光光催化剂纳米钨酸铋及其制备方法，涉及的制备工艺设备简单、反应条件温和、能耗小，制备的纳米钨酸铋可直接用作光催化剂，能在可见光下光催化降解有机污染物。
为实现上述目的，本发明采用的技术方案为：
一种可见光光催化剂钨酸铋纳米晶片的制备方法，包括以下步骤：1)将硝酸铋和甘油在异丙醇溶剂，进行溶剂热反应，经过滤、洗涤、烘干得甘油铋；2)将所得甘油铋均匀分散于钨酸钠水溶液中，调节所得溶液体系的PH值为0-2，然后进行水热反应，经过滤、洗涤、烘干制得纳米钨酸铋。
上述方案中，所述硝酸铋与甘油的摩尔比为1:(1.5-3)。
上述方案中，所述硝酸铋与异丙醇的摩尔比为1:(100-400)。
上述方案中，所述钨酸钠和甘油铋的摩尔比为1:(0.9-1.1)。
上述方案中，所述钨酸钠水溶液的浓度为0.1-1mol/L。
上述方案中，所述溶剂热反应条件为：加热至150-200℃保温反应1-24小时。
上述方案中，所述水热反应条件为：加热至150-200℃保温反应1-24小时。
上述方案中，步骤1)中所述烘干温度为80-100℃；步骤2)中所述烘干温度为80-150℃。
上述方案中，采用硝酸或盐酸溶液调节步骤2)中所得溶液体系的PH值。
根据上述方案制得的可见光光催化剂钨酸铋纳米晶片，其纯度大于99％，平均晶粒尺寸为20-100nm。
本发明的反应原理如下：
1)溶剂热合成甘油铋配合物
2)水热合成钨酸铋纳米晶片材料
本发明采用两步法，首先利用溶剂热反应合成非离子型的甘油铋配合物，再结合第二步水热反应步骤，利用柯肯达尔效应逐步完成纳米钨酸铋的制备过程，避免了常规无机盐沉淀反应速度过快、颗粒生长不均匀和所得晶粒尺寸不均一的缺点；同时引入的无机杂质少，使制备的产物钨酸铋具有较高的纯度。
本发明的有益效果为：
本发明以硝酸铋、甘油、钨酸钠为主要原料，采用两步法制备钨酸铋纳米晶片粉体，涉及的制备工艺设备简单、反应条件温和、能耗小，工艺独特新颖，所得产品钼酸铋的晶粒尺寸在20-40nm，可直接用作光催化剂，能在可见光下光催化降解有机污染物。
附图说明
图1为本发明实施例1所得钨酸铋纳米晶片的XRD图谱。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明不仅仅局限于下面的实施例。
以下实施例如无具体说明，采用的试剂为市售化学试剂或工业产品。
实施例1
一种可见光光催化剂钨酸铋纳米晶片的制备方法，包括以下步骤：
1)将10mmol硝酸铋和30mmol甘油溶于200ml的异丙醇中，搅拌均匀得到澄清液，将此溶液转移到容积为250ml的高压釜中，升温至160℃并保温6小时；待反应釜冷却至室温，过滤并用异丙醇洗涤滤饼3次，然后将滤饼在80℃下干燥12小时，得甘油铋粉体；
2)取10mmol钨酸钠溶于100ml去离子水中，配制均匀的钨酸钠水溶液，然后向其中加入9mmol甘油铋，强力搅拌使甘油铋分散均匀，并用硝酸调节所得溶液体系的pH值至0-1之间，再将所得混合液转移至容积为200ml的高压釜中，升温至180℃保温反应12小时。停止加热后待反应釜冷却至室温，过滤并用去离子水和乙醇各洗涤滤饼3次，滤饼在120℃干燥12小时，得目标产物钨酸铋纳米晶片粉体。
将本实施例所得产物进行X射线衍射分析，结果见图1。由图1可以看出，所得产物与JCPDS卡39–0256保持一致，为钨酸铋晶体。且本实施例所得钨酸铋纳米晶片粉体的纯度大于99％，平均粒径为30nm。本实施例所得钨酸铋晶体在浓度为1.0g/L时，在可见光照射下能在60min内完全降解浓度为0.01g/L的罗丹明。
实施例2
一种可见光光催化剂钨酸铋纳米晶片的制备方法，包括以下步骤：
1)将10mol硝酸铋和15mol甘油溶于100L的异丙醇中，搅拌均匀得到澄清液，将此溶液转移到容积为200L的高压釜中，升温至160℃并保温12小时；待反应釜冷却至室温，过滤并用异丙醇洗涤滤饼3次，然后将滤饼在80℃下干燥12小时，得甘油铋粉体；
2)取10mol钨酸钠溶于20L去离子水中，配制均匀的钨酸钠水溶液，然后向其中加入10mol甘油铋，强力搅拌使甘油铋分散均匀，并用硝酸调节所得溶液体系的pH值至0-1之间，再将所得混合液转移至容积为20L的高压釜中，升温至180℃保温反应24小时。停止加热后待反应釜冷却至室温，过滤并用去离子水和乙醇各洗涤滤饼3次，滤饼在120℃干燥12小时，得目标产物钨酸铋纳米晶片粉体。
本实施例所得钨酸铋纳米晶片粉体的纯度大于99％，平均粒径为25nm。本实施例所得钨酸铋晶体在浓度为1.0g/L时，在可见光照射下能在60min内完全降解浓度为0.01g/L的罗丹明。
实施例3
一种可见光光催化剂钨酸铋纳米晶片的制备方法，包括以下步骤：
1)将100mmol硝酸铋和200mmol甘油溶于2.5L的异丙醇中，搅拌均匀得到澄清液，将此溶液转移到容积为4L的高压釜中，升温至160℃并保温3小时；待反应釜冷却至室温，过滤并用异丙醇洗涤滤饼3次，然后将滤饼在80℃下干燥12小时，得甘油铋粉体；
2)取100mmol钨酸钠溶于100ml去离子水中，配制均匀的钨酸钠水溶液，然后向其中加入110mmol甘油铋，强力搅拌使甘油铋分散均匀，并用硝酸调节所得溶液体系的pH值至1-2之间，再将所得混合液转移至容积为200ml的高压釜中，升温至180℃保温反应4小时。停止加热后待反应釜冷却至室温，过滤并用去离子水和乙醇各洗涤滤饼3次，滤饼在120℃干燥12小时，得目标产物钨酸铋纳米晶片粉体。
本实施例所得钨酸铋纳米晶片粉体的纯度大于99％，平均粒径为35nm。本实施例所得钨酸铋晶体在浓度为1.0g/L时，在可见光照射下能在60min内完全降解浓度为0.01g/L的罗丹明。
以上所述仅为本发明的优选实施方式，应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，做出若干改进和变换，这些都属于本发明的保护范围。
Claims (5)
1.一种可见光光催化剂钨酸铋纳米晶片的制备方法，其特征在于，包括以下步骤：1）将硝酸铋和甘油在异丙醇溶剂，进行溶剂热反应，经过滤、洗涤、烘干得甘油铋；2）将所得甘油铋均匀分散于钨酸钠水溶液中，调节所得溶液体系的pH值为0-2，然后进行水热反应，经过滤、洗涤、烘干制得纳米钨酸铋；
所述硝酸铋与甘油的摩尔比为1:(1.5-3)；钨酸钠和甘油铋的摩尔比为1:(0.9-1.1)；
所述溶剂热反应条件为：加热至150-200℃保温反应1-24小时；
所述水热反应条件为：加热至150-200℃保温反应1-24小时。
2.根据权利要求1所述的制备方法，其特征在于，所述硝酸铋与异丙醇的摩尔比为1:(100-400)。
3.根据权利要求1所述的制备方法，其特征在于，所述钨酸钠水溶液的浓度为0.1-1mol/L。
4.根据权利要求1所述的制备方法，其特征在于，步骤1）中所述烘干温度为80-100℃；步骤2）中所述烘干温度为80-150℃。
5.根据权利要求1所述的制备方法，其特征在于，采用硝酸或盐酸溶液调节pH值。
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| CN103599771A (zh) * | 2013-11-12 | 2014-02-26 | 福州大学 | 一种Bi2WO6光催化剂及其制备方法和应用 |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN103041801A (zh) * | 2013-01-11 | 2013-04-17 | 南开大学 | 一种柿饼状形貌的钨酸铋光催化剂的制备方法 |
| CN103599771A (zh) * | 2013-11-12 | 2014-02-26 | 福州大学 | 一种Bi2WO6光催化剂及其制备方法和应用 |
Non-Patent Citations (2)
| Title |
|---|
| Surfactant-free hydrothermal synthesis and gas-sensing properties of NaBi(MoO4)2 nanocrystals;Zhidong Lin,et al;《Materials Letters》;20160111;第168卷;文章第72页2.1节，第73页右栏第2段 * |
| 水热合成纳米Bi2WO6粉末及其可见光催化活性;姚三丽等;《中国环境科学》;20080331;第28卷(第3期);文章第243页2.2节 * |
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