CN109019693B - 一种单斜相wo3纳米长方体的制备方法及其光催化应用 - Google Patents
一种单斜相wo3纳米长方体的制备方法及其光催化应用 Download PDFInfo
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Abstract
本发明涉及一种单斜相WO3纳米长方体的制备方法及其光催化应用，具体的说是通过WO3粒子为前驱体，水热合成单斜相WO3纳米长方体，单斜相WO3纳米长方体室温下高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
本发明涉及单斜相WO3纳米长方体的制备方法及其光催化应用，属于光催化剂的制备与应用领域。
背景技术
单斜相WO3是稳定且常见的WO3相，以[WO6]为基本结构单元，通过共角组成，其晶体结构是三氧化铼(ReO3)型。单斜相WO3独特的晶体结构，使其具有光、电和催化性能，在光/电致变色器件、锂离子电池、气敏传感器、光催化剂等领域具有重要的应用前景。近期研究表明WO3材料的化学性质与其形貌密切相关，因此形貌可控合成WO3材料成为了人们研究的热点。
液相合成方法，特别是水热法或者溶剂热法，因其过程简单、条件温和、效率高、成本低廉成为单斜相WO3材料合成的主要方法。主要是利用酸化含W物质形成前驱体，进一步分解形成WO3。例如：Meng等使用HCl和柠檬酸酸化Na2WO4溶液，调节pH值至1，通过180℃水热12h合成了花状结构的WO3(D.Meng,et al.,Journal of Alloys and Compounds,2015,649, 731-738)。Sangpour等用HBF4酸化Na2WO4·2H2O，160℃水热10h得到WO3纳米盘(P.Sangpour,et al.,Journal of Energy Chemistry,2015,24,171-177)。另外，利用一些复杂的路径或价格高的前驱体制备WO3材料。例如：Li等将WCl6加入到苯甲醇体系中，再加入离子液体氯化(1-丁基-3-甲基咪唑)，180℃水热24h得到中间产物，然后再在马弗炉中400℃煅烧2h 得到WO3纳米粒子(Z.Li,et al.,Journal of Materials Chemistry A,2013,1,15377-15382)。因此，利用新路径合成单斜相WO3材料来避免使用环境污染的酸、价格高的W的前驱体以及有机溶剂是十分必要的，并使其能够高活性的实现催化反应。
亚甲基蓝，是一种阳离子型碱性染料，广泛用于棉、麻、蚕丝物品、造纸、染料等工业领域。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。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。因此，研究单斜相WO3材料可控合成及调控，使其能够高活性的去除亚甲基蓝，具有潜在的实用价值。
综上所述，作为过渡金属氧化物，单斜相WO3材料传统的合成方法是酸化钨酸盐水热分解和有机体系合成，以商品化单斜相WO3为前驱体水热合成单斜相WO3纳米材料尚未有报道。因此，通过新型路径合成单斜相WO3纳米长方体，使其能够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合成单斜相WO3纳米长方体的方法和在光催化去除亚甲基蓝的应用，实现近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)单斜相WO3纳米长方体的制备：将在50mL烧杯中加入0.3g商品化WO3粒子和11mL(30％)H2O2，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240℃水热处理12h，然后自然冷却至室温，产物经离心洗涤，50℃真空干燥得到单斜相 WO3纳米长方体，宽度为74-490nm、长度为76-770nm，厚度为24-58nm。
2)将单斜相WO3纳米长方体催化剂用于光催化降解去除亚甲基蓝反应。单斜相WO3纳米长方体在室温反应30min，亚甲基蓝去除率为58％，反应45min，去除率为68％，反应210min达100％。
本发明具有如下优点：
1)利用商品化WO3粒子前驱体。水热合成了单斜相WO3纳米长方体，有效的拓展了单斜相WO3纳米材料的制备方法，使其不再主要局限于酸化钨酸盐分解体系，并能形貌可控合成单斜相WO3。
2)室温下单斜相WO3纳米长方体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WO3纳米长方体的表征结果，(a)XRD和(b-f)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。
实施例1
单斜相WO3纳米长方体具体制备过程如下：在50mL烧杯中加入0.3g商品化的WO3粒子和11mL(30％)H2O2，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240℃水热处理12h，然后自然冷却至室温，产物经离心洗涤，50℃真空干燥得到单斜相WO3纳米长方体，宽度为74-490nm、长度为76-770nm，厚度为24-58nm(如图1所示)。
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(30-240min)，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单斜相WO3纳米长方体光降解亚甲基蓝废水溶液的反应结果
由表1可以看出：单斜相WO3纳米长方体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、150min、240min时，脱除率分别为58％、68％、75％、83％、89％、95％、100％。当浓度为1mg/L、2mg/L、5mg/L 时反应240min，脱除率为100％。
Claims (2)
1.一种单斜相WO3纳米长方体的制备方法，具体的说是通过WO3粒子为前驱体，水热合成单斜相WO3纳米长方体，该单斜相WO3纳米长方体室温下可高效光催化降解染料废水中的亚甲基蓝；单斜相WO3纳米长方体由如下步骤制得：将WO3粒子加入到H2O2水溶液，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240 oC水热处理10-14 h，得到单斜相WO3纳米长方体。
2.按照权利要求1所述的一种单斜相WO3纳米长方体的制备方法，其特征在于：
单斜相WO3纳米长方体在20-40 oC光催化4-8 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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