CN106976909B - 一种六方相h-MoO3微米棒的制备方法和光催化应用 - Google Patents
一种六方相h-MoO3微米棒的制备方法和光催化应用 Download PDFInfo
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Abstract
本发明涉及一种六方相h‑MoO3微米棒的制备方法和光催化应用，具体的说是通过六方相h‑MoO3微米棒室温下高效光催化降解染料废水中的亚甲基蓝。本发明所述的六方相h‑MoO3微米棒是以正交相α‑MoO3为前驱体，通过水热方法合成的，能够有效光催化降解浓度为1‑10mg/L的亚甲基蓝溶液，脱除率为100％，无副产物产生。
Description
技术领域
本发明涉及六方相h-MoO3微米棒及其在光催化中的应用，属于光催化剂的制备与应用领域。
背景技术
六方相h-MoO3具有ReO3结构，是MoO3的一种亚稳相态，基本结构单元是[MoO6]八面体。 h-MoO3是由MoO6八面体共角构成链，链与链之间通过顺位连接成片，片与片之间沿着z轴方向堆积，构成三维阵列。h-MoO3中存在四面体和八面体空位，适合Li+、Na+、K+、NH4 +等离子插入且自由流动。由于h-MoO3独特的晶体结构，使其具有优异的光学、电致变色、催化和电性能。与热力学稳定的正交相α-MoO3比较，亚稳结构的化合物常常表现出新的和增强的物理化学性质，但制备比较困难，制约了其应用研究。
目前使用液相合成方法，特别是水热法或者溶剂热法，是形貌可控合成h-MoO3材料最简便、最有效的方法。常用的合成方法主要有钼酸水热分解和过氧钼酸分解。例如：Bose等HNO3酸化(NH4)6Mo7O24·4H2O，通过120℃加热3h合成了h-MoO3微米棒(A.C.Bose,etal.,Catal.Sci. Technol.,2013,3,1405-1414)。Song等将H2MoO4溶于氨水，用HCl调节pH，通过100℃水热8 h合成了长度为14-25μm、直径为6-7μm的h-MoO3微米棒(J.Song et al.,Mater.Res.Bull., 2005,40,1751-1756)。Chen等在冰水浴条件下将Mo粉溶解于30％H2O2水溶液中，再加入 NH4Cl，160℃水热24h得到长度为12-25μm，直径为1.0-3.5μm的h-MoO3纳米带(W.Chen et al.,Appl.Surf.Sci.,2015,359,114-119)。Xie等将金属钼粉加入30％H2O2中溶解，再加入 NaNO3,150℃水热12h，得到直径为150nm的的h-MoO3纳米材料(Y.Xie etal.,Chem.Mater., 2009,21,5681-5690)。这些制备方法中由于加入酸或使用剧烈反应的钼粉，使制备方法需要进一步提升来调控制备六方相h-MoO3。
亚甲基蓝，是一种阳离子型碱性染料。亚甲基蓝是工业上常使用的阳离子型有机染料，广泛用于棉、麻、蚕丝物品、造纸、染料等工业领域。目前，制浆造纸、化工染料、纺织等行业产生大量包含亚甲基的燃料废水。由于亚甲基蓝含有相对稳定的芳香分子结构，很难被水中的微生物降解，对生态环境和人类存在严重危害。因此，含有机染料亚甲基蓝的废水处理对缓解资源危机及改善人类生活环境具有重要的现实意义。光催化氧化法是采用光敏化半导体在紫外线照射下，将价带电子激发跃迁到导带并产生空穴，从而发生氧化反应破坏染料的发色基团，将染料分子降解，最终生成CO2、H2O及无机盐等物质。光催化氧化法具有降解脱色彻底、不造成二次污染等优点，在染料废水处理中的应用前景广阔。目前常用的光催化剂是TiO2、WO3、Fe2O3等，但关于六方相h-MoO3材料对亚甲基蓝的去除，则还研究的较少。因此，研究六方相h-MoO3材料可控合成及调控，使其能够高活性的吸附亚甲基蓝，具有潜在的实用价值。
综上所述，作为半导体氧化物，六方相h-MoO3在光降解亚甲基蓝领域研究的比较少。传统的合成氧化钼的方法中使用酸容易造成环境污染或使用剧烈反应的钼粉存在安全隐患，而以正交相α-MoO3为前驱体水热合成六方相h-MoO3材料尚未有报道。因此，通过绿色、新型路径合成了六方相h-MoO3微米棒，并实现了高活性的催化去除染料废水中的亚甲基蓝。
发明内容：
本发明旨在提供一种新型合成六方相h-MoO3微米棒的方法和在光催化去除亚甲基蓝的应用，实现100％的去除率。
基于上述目的，本发明所涉及的技术方案如下：
1)六方相h-MoO3微米棒具体制备过程如下：在50mL烧杯中加入1.44g正交相α-MoO3粒子和11mL(30％)H2O2，30℃搅拌至溶解，将7g NaNO3加入到上述溶液的烧杯中，搅拌均匀后，将所得液体转入50ml以聚四氟乙烯为内衬的不锈钢反应釜中于170℃水热处理 12h，然后自然冷却至室温，产物经离心洗涤，50℃真空干燥得到六方相h-MoO3微米棒，直径为0.5-1.6μm、长度为2.2-6.1μm。
2)正交相α-MoO3粒子的制备：将商品化的钼酸铵((NH4)6Mo7O24·4H2O)放入蒸发皿，将其放在马弗炉里，在空气气氛下以5℃/min从室温升到500℃，并在此温度保持4h，最后，空气气氛下自然降至室温，得到正交相α-MoO3粒子，粒径大约为0.6-3.1μm。
3)将六方相h-MoO3微米棒催化剂用于光催化降解去除亚甲基蓝反应。六方相h-MoO3微米棒在室温反应30min，亚甲基蓝去除率为37％，反应45min，去除率为52％，反应360min达100％。
本发明具有如下优点：
1)利用正交相α-MoO3为前驱体。水热合成了六方相h-MoO3微米棒，有效的拓展了h-MoO3微米棒的制备方法。
2)室温下六方相h-MoO3微米棒光催化降解亚甲基蓝，实现了亚甲基蓝废水溶液的有效脱除，脱除率为100％。
3)本发明具有环境友好、过程效率高且其光催化降解十分稳定的特点。
附图说明：
图1是六方相h-MoO3微米棒的表征结果，(a)XRD、(b)FT-IR和(c-d)电镜图片。
具体实施方式
下列实施例用来进一步说明本发明，但不因此而限制本发明。
正交相α-MoO3粒子的制备：将8g商品化的钼酸铵((NH4)6Mo7O24·4H2O)放入蒸发皿，将其放在马弗炉里，在空气气氛下以5℃/min从室温升到500℃，并在此温度保持4h，最后，空气气氛下自然降至室温，得到正交相α-MoO3粒子，粒径大约为0.6-3.1μm。
实施例1
六方相h-MoO3微米棒具体制备过程如下：在50mL烧杯中加入1.44g正交相α-MoO3粒子和11mL(30％)H2O2，30℃搅拌至溶解，将7g NaNO3加入到上述溶液的烧杯中，搅拌均匀后，将所得液体转入50ml以聚四氟乙烯为内衬的不锈钢反应釜中于170℃水热处理 12h，然后自然冷却至室温，产物经离心洗涤，50℃真空干燥得到六方相h-MoO3微米棒。
实施例2-11
实施例1所制备的材料用于光催化降解亚甲基蓝废水溶液。
将50mg实施例1中的材料加入到含有100mL浓度为1-10mg/L亚甲基蓝溶液的250mL锥形瓶中，在暗处处理30min以达到吸附/脱附平衡。将反应体系在搅拌条件下室温用300WXe灯照射一定时间(30-480min)，反应产物离心分离后取上层清夜，分光光度仪PerkinElmer Lambda 750在最大吸收波长为664nm处分析其组成。反应结果如下。
表1六方相h-MoO3微米棒光降解亚甲基蓝废水溶液的反应结果
由表1可以看出：六方相h-MoO3微米棒光催化降解废水染料中亚甲基蓝有机物，在浓度为10mg/L时反应30min、45min、60min、90min、120min、180min、480min时，脱除率分别为37％、52％、59％、78％、90％、97％、100％。当浓度为1mg/L、2mg/L、5mg/L 时反应180min，脱除率为100％。
Claims (3)
1.一种六方相h-MoO3微米棒的制备方法，具体的说是通过正交相α-MoO3粒子为前驱体，水热合成六方相h-MoO3微米棒，该六方相h-MoO3微米棒室温下可高效光催化降解染料废水中的亚甲基蓝；六方相h-MoO3微米棒由如下步骤制得：将正交相α-MoO3粒子在30 oC下溶解于H2O2，将NaNO3加入到上述溶液中，将所得液体转入以聚四氟乙烯为内衬的不锈钢反应釜中于150-250 oC水热处理2-24 h，得到六方相h-MoO3微米棒。
2.按照权利要求1所述的方法，其特征在于：
将商品化的钼酸铵放在马弗炉里，在空气气氛下从室温升到500 oC，并在此温度保持4h，得到正交相α-MoO3粒子。
3.按照权利要求1或2所述的方法，其特征在于：
六方相h-MoO3微米棒在20-60 oC光催化3-8 h，可光催化降解浓度为1-10 mg/L的亚甲基蓝溶液，脱除率为100%，无副产物产生。
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