CN107803198B - 一种钨酸铋光催化薄膜的电化学制备方法及其应用 - Google Patents
一种钨酸铋光催化薄膜的电化学制备方法及其应用 Download PDFInfo
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Abstract
一种钨酸铋光催化薄膜的电化学制备方法，属于Bi基薄膜光催化材料研发、太阳能光催化剂固定化技术、有机污染物处理及光催化水解制氢领域，解决现有Bi2WO6薄膜固定化技术复杂或能耗较高的问题，以Na2WO6溶液、Bi板和石墨分别作为电解质、阳极和阴极，常温恒电压下在Bi板原位生长Bi2WO6薄膜，是一种简单经济可行的纳米片状Bi基催化剂薄膜固定化技术。本发明应用于罗丹明B的降解以及光催化分解水制氢，过程环保、工艺简单、易于操作、重复性强和周期短。
Description
技术领域
本发明属于Bi基薄膜光催化材料研发、太阳能光催化剂固定化技术、有机污染物处理及光催化水解制氢领域，具体涉及一种钨酸铋光催化薄膜的电化学制备方法及其应用。
背景技术
随着经济的发展和人口的膨胀，人类对于大自然中的石油、天然气、煤等不可再生能源的消耗已经达到了前所未有的高度，且由于我们的过分依赖以及在开采和使用过程中效率偏低的缘故，使得我们不仅无法有效、充分、快捷的利用这类能源，造成了极大的浪费，而且当这类能源中的有害物质排入空气或者水中时还会给我们带来严重的环境污染。故近几年来关于利用可再生能源以及污染物处理的研究已成为全球性的重点关注课题，各国也相应的提出了治理方案和措施。
光催化氧化技术作为一种催化技术，不仅可以将许多水中、空气中难生物降解的有机物质彻底矿化，而且具有操作简单、无污染、反应彻底、速率快等优点，更为重要的是此项技术是以清洁可再生能源—太阳能为基础，真正做到了绿色环保、取之不尽用之不竭。因此，自从上世纪70年代首次被提出以来，就迅速的获得了科学家的青睐，并吸引了大量研究者的深度研究和探索，被国际上公认为是一种最具应用前景的治理有机污染物的经济环保技术。
钨酸铋（Bi2WO6）作为一种可见光响应光催化材料，是结构通式为Bi2An−1BnO3n+3（A=Ca，Sr，Ba，Pb，Bi，Na，K和B=Ti，Nb，Ta，Mo，W，Fe）Aurivillius家族中最简单的氧化物，属于正交晶系，其Bi2O2层和WO4层交替组成层状结构能使空穴与电子对有效的分离，使Bi2WO6成为了Bi基氧化物中具有最高可见光活性的光催化材料（Chem. mater. 17 (2005) 1952-8），成为Bi基光催化材料的新星。同时为了进一步提高其光吸收能力和光催化性能，Zhang等人通过制备了Bi2S3/Bi2WO6粉体，通过表征得知，Bi2S3的修饰使得Bi2WO6的活性大大提高（Ceram. Int. 43 (2017) 11296-11304）。但是，粉体光催化剂普遍存在易团聚、分散性差、固液分离难且不易回收循环利用等缺陷，故越来越多的研究者开始关注于负载技术和薄膜固定化以解决上述问题，目前针对Bi2WO6薄膜固定化的制备技术报道并不多，且所用方法大多数较复杂或能耗较高，电化学方法未见报道。
发明内容
本发明为了解决现有Bi2WO6薄膜固定化技术复杂或能耗较高的问题，提供一种钨酸铋光催化薄膜的电化学制备方法及其应用。
本发明采用如下技术方案：
一种钨酸铋光催化薄膜的电化学制备方法，包括如下步骤：
第一步，配制电解质溶液，称取1～17g分析纯Na2WO4放置于烧杯中，加入50～200ml蒸馏水，充分搅拌使其溶解配置成溶液A；
第二步，打磨Bi板，采用磨砂纸打磨Bi板至光滑，并分别用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，制备Bi2WO6薄膜，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为2～8 cm，溶液A作为电解质，在80～130 V常温恒电压下沉积2～4 h后，将Bi板取出自然晾干，即得Bi2WO6薄膜。
所述Bi板的尺寸为4 cm×1.5 cm×0.5 cm。
所述磨砂纸为400目的磨砂纸。
一种钨酸铋光催化薄膜应用于罗丹明B的降解以及光催化分解水制氢。
本发明以Na2WO4溶液、Bi板和石墨分别作为电解质、阳极和阴极，常温恒电压下在Bi板原位生长Bi2WO6薄膜，是一种简单经济可行的纳米片状Bi基催化剂薄膜固定化技术。
常温常压下，所制备的Bi2WO6薄膜在不同光源照射下可有效矿化罗丹明B、双酚A、苯酚任一种有机污染物（初始浓度为10 mg/L）以及光催化分解水制氢。所述光源为紫外光、可见光、模拟太阳光的任一种光源。
本发明的有益效果如下：
1. 电化学方法过程环保、工艺简单、易于操作、重复性强和周期短；
2. Bi板原位生长制备Bi2WO6薄膜，从物质基础属性出发制备薄膜样品，其与基体为化学结合，所以其与基体结合了强、分散均匀、不易脱落，用拉伸法测得的本发明制得的Bi2WO6薄膜与基底结合力为25～35 MPa，比常规方法制得的薄膜与基体的结合力提高了50%～60%；
3. Bi板既为原料又作电极，避免了其他固定化催化剂多带来的繁琐工序；
4. 该电化学制备技术可推广至其他Bi基薄膜材料的应用。
附图说明
图1为本发明实施例1制备的Bi2WO6薄膜光催化材料的XRD图谱。
具体实施方式
实施例1，
第一步，配置200 mL蒸馏水，称取17 g分析纯Na2WO4放置于烧杯中充分搅拌使其溶解配置成溶液A；
第二步，采用400目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为5 cm，溶液A作为电解质，在120 V电压下沉积2 h后，将Bi板取出自然晾干，即得Bi2WO6薄膜，记为Bi2WO6-1。
实施例2，
第一步，配置50 mL蒸馏水，称取1 g分析纯Na2WO4放置于烧杯中充分搅拌使其溶解配置成溶液A；
第二步，采用400目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为2 cm，溶液A作为电解质，在80 V电压下沉积4 h后，将Bi板取出自然晾干，即得Bi2WO6薄膜，记为Bi2WO6-2。
实施例3，
第一步，配置100 mL蒸馏水，称取8 g分析纯Na2WO4放置于烧杯中充分搅拌使其溶解配置成溶液A；
第二步，采用400目大小的磨砂纸将4 cm×1.5 cm×0.5 cm的Bi板打磨光滑，用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为8 cm，溶液A作为电解质，在130 V电压下沉积3 h后，将Bi板取出自然晾干，即得Bi2WO6薄膜，记为Bi2WO6-3。
Bi2WO6薄膜光催化材料应用于罗丹明B的降解。
准确称取10 mg的罗丹明B，将其放入盛有900 mL蒸馏水的1000 mL定量瓶中使其充分溶解，加蒸馏水至1000 mL，制得10 mg/L的待降解液，放置24 h待用；用移液管准确移取100 mL10 mg/L的待降解液放入分别固定好Bi2WO6-1、Bi2WO6-2、Bi2WO6-3薄膜样品的光催化反应装置，室温下在避光条件下吸附1 h，以期达到吸附平衡，然后打开模拟太阳光灯，进行光催化降解实验，每隔1 h取样一次，利用紫外-可见分光光度法对溶液中的染料浓度进行分析并计算其降解率，见表1所示。
表1 罗丹明B的降解速率
从表1中看出，随着时间的延长，Bi2WO6薄膜对罗丹明B的降解率高达95.3%。
Bi2WO6薄膜应用于光催化分解水制氢。
配置80 mL 20%的甲醇溶液置于特制的石英光催化反应器中，加入所制的Bi2WO6-1、Bi2WO6-2、Bi2WO6-3薄膜样品，通N2 30 min后密封，在磁力搅拌和水浴控温下，使用500 W，光强为110 mW/cm3的氙灯连续光照3 h，每30 min从反应瓶中采集3 mL气体样品进行H2含量的定量分析，Bi2WO6-1、Bi2WO6-2、Bi2WO6-3薄膜样品最终的产氢速率分别为110.1、89.4、105.3 μmol·h-1·gcat-1。
Claims (4)
1.一种钨酸铋光催化薄膜的电化学制备方法，其特征在于：包括如下步骤：
第一步，配制电解质溶液，称取1～17g分析纯Na2WO4放置于烧杯中，加入50～200ml蒸馏水，充分搅拌使其溶解配置成溶液A；
第二步，打磨Bi板，采用磨砂纸打磨Bi板至光滑，并分别用无水乙醇和蒸馏水将打磨后的Bi板冲洗干净，待用；
第三步，制备Bi2WO6薄膜，将第二步的Bi板作阳极，石墨作阴极，阴阳电极距离为2～8cm，溶液A作为电解质，在常温恒电压下沉积2～4 h后，将Bi板取出自然晾干，即得Bi2WO6薄膜；其中，电压为80~130V。
2.根据权利要求1所述的一种钨酸铋光催化薄膜的电化学制备方法，其特征在于：所述Bi板的尺寸为4 cm×1.5 cm×0.5 cm。
3.根据权利要求1所述的一种钨酸铋光催化薄膜的电化学制备方法，其特征在于：所述磨砂纸为400目的磨砂纸。
4.一种利用如权利要求1所述的电化学制备方法制备的钨酸铋光催化薄膜应用于罗丹明B的降解以及光催化分解水制氢。
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