CN106890655A - 一种具有高效可见光催化活性的Ag/AgCl/CdWO4催化剂 - Google Patents
一种具有高效可见光催化活性的Ag/AgCl/CdWO4催化剂 Download PDFInfo
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Abstract
本发明提供了一种具有高效可见光催化活性的Ag/AgCl/CdWO4催化剂的制备方法及在可见光下催化降解多种染料的应用。本发明采用钨酸钠和硝酸铬为主要原料,以水和乙二醇作混合溶剂,通过水热法制得CdWO4材料,然后采用浸渍和光还原法制备了具有等离子共振效应的Ag/AgCl/CdWO4光催化剂。此法制备的催化剂在可见光照射下对金橙II、甲基橙、甲基蓝、孔雀绿、结晶紫和罗丹明B等多种染料具有优异的光催化降解性能,10分钟降解率达95%以上,矿化率高,可重复使用。本发明涉及的生产工艺条件简单、原料易得,所得的材料具有高效的光响应程度,具有广阔工业应用前景。
Description
技术领域
本发明属于光催化技术领域,涉及一种在可见光下具有高效降解多种有机染料活性的光催化剂的制备方法。更具体地说,是一种具有等离子共振效应的Ag/AgCl/CdWO4光催化剂的制备和降解多种有机染料的应用。
背景技术
随着现代社会经济的发展,能源和环境问题日益突出,人们迫切希望能通过绿色、环保的方法来获得清洁能源和去除污染物。近年来,半导体光催化技术,因其环境友好性、反应条件温和、能矿化有机污染物等优点,成为处理难降解废水的有效方法。TiO2凭借其高效的光催化活性、化学稳定性、廉价、无毒等特性,被作为光催化剂来广泛研究。但TiO2只能在紫外光下激发,对太阳能的利用率较差,而限制了它的实际应用。尽管科学家尝试通过各种方法,如:形貌调控、掺杂、异质结、表面改性、等离子共振等方法对其改性,但都无法从根本上解决其可见光响应差的问题。因此,研制和开发具有优良可见光响应性能的光催化材料,成为光催化走向实用化的发展趋势之一。
近年来,人们发现CdWO4具有较好的紫外光降解有机污染物性能,光学性能优于TiO2,是一类具有开发前景的光催化材料。但由于其禁带宽度较宽(约为3.8eV),只能对紫外光进行响应,同样,限制了它的实际应用。人们发现异质结能有效改善其可见光催化性能。2016年申请专利CN105642316A公开了一种制备BiOI/CdWO4异质结光催化剂的方法,通过BiOI/CdWO4异质结得到了一种具有良好可见光催化活性的纳米复合光催化剂,90分钟降解罗丹明B可达90%,其活性较纯BiOI和CdWO4高。研究表明异质结能有效促进光生电子和空穴的分离,提高光催化性能。从文献报道看,目前还没有人通过等离子共振效应来改进CdWO4的光催化性能。
发明内容
本发明的目的在于提供一种在可见光下具有高效降解多种有机染料活性的光催化剂的制备。首先,以水和乙二醇作混合溶剂,通过水热法制得CdWO4材料,然后采用浸渍和光还原法制备了具有等离子共振效应的Ag/AgCl/CdWO4光催化剂。所得催化剂中的Ag/AgCl等离子共振效应将有利于材料对可见光的吸收;同时,材料特有的Ag/AgCl/CdWO4异质结结构将利于光生电子和空穴的有效分离,使光生电子和空穴得到充分利用。也就是说,通过异质结构造和等离子共振效应的协同作用,有效地提高了CdWO4的光催化性能。实现了在可见光下高效催化降解多种有机染料的特性。
本发明的效果和优点:
此法制备的催化剂在可见光照射下对金橙II、甲基橙、甲基蓝、孔雀绿、结晶紫和罗丹明B等有机染料具有优异的光催化降解性能;10分钟有机染料降解率为95%以上,矿化率高达93%,可重复使用。
本发明涉及的生产工艺条件简单、原料易得,所得的材料具有高效的光响应程度,工业应用前景广阔。
附图说明
图1为具有等离子共振效应的Ag/AgCl/CdWO4光催化剂和CdWO4的XRD图;
图2为可见光下Ag/AgCl/CdWO4光催化剂降解多种有机染料的降解效率图。
具体实施方式
1、具有等离子共振效应的Ag/AgCl/CdWO4光催化剂的制备
实施例1:
(1)CdWO4的合成
分别称取2mmol的Na2WO4·2H2O和2mmol的Cd(NO3)2·4H2O,溶于水和乙二醇组成的混合溶液中,不断搅拌至溶解;转入水热反应釜,100℃,水热晶化2天;抽滤,洗涤,干燥;即得CdWO4,与单斜相(卡片JCPDS14-0676)吻合,产物XRD见附图1,测定其比表面积为78.4m2/g。
(2)具有等离子共振效应的Ag/AgCl/CdWO4光催化剂的制备
(a)称取0.4mmol AgNO3,将其加到30mL的乙醇水溶液中,加入水热法制得的CdWO4,不断搅拌至分散均匀;称取0.4mmol KCl将其加到20mL的乙醇水溶液中,溶解,然后将其滴加到含CdWO4、AgNO3的乙醇水溶液中;滴加完成后,继续搅拌30~120分钟,至生成的AgCl充分浸渍到CdWO4上;
(b)将上述溶液在卤灯下光照30分钟,将AgCl部分还原成Ag;然后静置,抽滤,洗涤,并将其干燥,即得具有等离子共振效应的Ag/AgCl/CdWO4光催化剂;产物的XRD见附图1。
2、具有等离子共振效应的Ag/AgCl/CdWO4光催化剂降解有机染料实验
通过在可见光下降解金橙II、甲基橙、甲基蓝、孔雀绿、结晶紫和罗丹明B溶液来评价所制备催化剂的光催化性能。具体实施如下:
称取0.1g催化剂,将其分散于100ml的10mg/L所选染料溶液的烧杯(250ml)中,在黑暗条件下磁力搅拌30min,使其能够达到吸-脱附平衡,待其平衡后。以300W氙灯做为光源,并通过截波玻璃滤去波长小于420nm紫外光,每隔一定的反应时间,取5mL反应溶液,并通过高速离心机分离,取上层离心液。离心液经由紫外-可见分光光度计检测,并观测最大吸收峰值强度的变化来推测染料降解的浓度变化。结果表明,本发明的Ag/AgCl/CdWO4光催化剂,在10分钟内降解率为95%,见附图2。进一步测其TOC值,发现从起始的900ppm降为60ppm,矿化率达93%;重复使用4次,其降解率保持不变。
Claims (4)
1.一种具有高效可见光催化活性的Ag/AgCl/CdWO4催化剂的制备方法,其特征在于,采用钨酸钠和硝酸铬为主要原料,以水和乙二醇作混合溶剂,通过水热法制得CdWO4材料,然后采用浸渍和光还原法,制得在可见光照射下可高效降解多种染料的具有等离子共振效应的Ag/AgCl/CdWO4光催化剂。
2.根据权利要求1所述的制备方法,其特征在于,CdWO4的制备方法包括以下步骤:
按照Cd、W摩尔比为1∶1的比例分别称取Na2WO4·2H2O和Cd(NO3)2·4H2O,将其溶于水和乙二醇组成的混合溶液中;不断搅拌至溶解;转入水热反应釜,100~180℃,水热晶化1~3天,抽滤,洗涤,干燥,即得CdWO4。
3.根据权利要求1所述的制备方法,其特征在于,具有等离子共振效应的Ag/AgCl/CdWO4光催化剂的制备方法包括以下步骤:
(a)按照Ag、Cl摩尔比为1∶1的比例,分别配置AgNO3乙醇水溶液和KCl的乙醇水溶液;首先,将水热法制得的CdWO4加入AgNO3乙醇水溶液中,不断搅拌至分散均匀;然后滴加KCl的乙醇水溶液,滴加完成后,继续搅拌30~120分钟,至生成的AgCl充分浸渍到CdWO4上;Ag、W摩尔比为1∶5~2∶1;
(b)卤灯下光照5~30分钟,将AgCl部分还原成Ag;然后静置,抽滤,洗涤,并将其干燥,即得具有等离子共振效应的Ag/AgCl/CdWO4光催化剂。
4.根据权利要求1所述的制备方法,其特征在于,Ag/AgCl/CdWO4催化剂的用途为用于可见光下催化降解有机染料,有机染料有金橙II、甲基橙、甲基蓝、孔雀绿、结晶紫和罗丹明B或与前述染料分子具有相同生色团的有机染料。
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Cited By (5)
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CN107983377A (zh) * | 2017-11-13 | 2018-05-04 | 湖南大学 | 钨酸镉修饰的银/碘化银复合材料及其制备方法和应用 |
CN109092330A (zh) * | 2018-08-09 | 2018-12-28 | 齐齐哈尔大学 | CdSQDs@CdIn2S4/CdWO4材料的制备 |
CN109225282A (zh) * | 2018-10-24 | 2019-01-18 | 福建师范大学 | 一种p-n型CdWO4/BiOCl异质结光催化剂、制备方法及其用途 |
CN110152662A (zh) * | 2019-06-18 | 2019-08-23 | 陕西科技大学 | 一种Ag-Bi2SiO5/Bi12SiO20双异质可见光光催化剂的制备方法 |
CN115487836A (zh) * | 2022-09-26 | 2022-12-20 | 西南交通大学 | 一种复合材料及其制备方法和应用 |
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CN107983377A (zh) * | 2017-11-13 | 2018-05-04 | 湖南大学 | 钨酸镉修饰的银/碘化银复合材料及其制备方法和应用 |
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CN109092330B (zh) * | 2018-08-09 | 2021-03-02 | 齐齐哈尔大学 | CdSQDs@CdIn2S4/CdWO4材料的制备 |
CN109225282A (zh) * | 2018-10-24 | 2019-01-18 | 福建师范大学 | 一种p-n型CdWO4/BiOCl异质结光催化剂、制备方法及其用途 |
CN110152662A (zh) * | 2019-06-18 | 2019-08-23 | 陕西科技大学 | 一种Ag-Bi2SiO5/Bi12SiO20双异质可见光光催化剂的制备方法 |
CN115487836A (zh) * | 2022-09-26 | 2022-12-20 | 西南交通大学 | 一种复合材料及其制备方法和应用 |
CN115487836B (zh) * | 2022-09-26 | 2023-11-10 | 西南交通大学 | 一种复合材料及其制备方法和应用 |
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