CN109225266A - 一种钨酸锌/硫化镉复合可见光催化剂的制备方法 - Google Patents
一种钨酸锌/硫化镉复合可见光催化剂的制备方法 Download PDFInfo
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 43
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Abstract
本发明涉及一种钨酸锌/硫化镉复合可见光催化剂的制备方法，包括硫化镉光催化剂的制备和钨酸锌/硫化镉复合光催化剂的制备。本发明的有益效果是：该制备方法简单，易于操作，且制备条件容易控制，所制备的钨酸锌/硫化镉复合可见光催化剂为绿色无污染高性能催化剂，且光催产氢效率高，具有一定应用前景。
Description
技术领域
本发明属于光催化纳米材料技术领域，涉及一种钨酸锌/硫化镉复合可见光催化剂的制备方法。
背景技术
钨酸盐是一类重要的无机半导体材料，其价带具有较高的电荷流动性和氧化活性，由金属原子的最外层s和O2p轨道杂化而成，在光致发光、微波、闪烁材料等方面均具有广泛的应用前景。钨酸锌(ZnWO4)属于AWO4结构的二价过渡金属钨酸盐，根据阳离子A的大小，可分为四方白钨矿结构或单斜黑钨矿结构结晶。钨酸锌是一种新型半导体光催化剂，具有化学稳定性高、折射率高、光产率高、发光衰变时间短、无毒等优点，可以通过光催化作用降解各种有机染料,在空气净化及污水处理方面有显著的光催化效果，在光催化领域具有十分潜在的应用前景。
硫化镉因能隙较窄(2.4eV)，吸收太阳光的波长范围较宽，同时量子尺寸效应带来的能级改变及能隙变宽使得其氧化还原能力增强，因而纳米硫化镉半导体材料具有优异的光催化性能，然而，诸多研究显示，硫化镉存在容易发生光腐蚀、光生电荷-空穴容易复合、颗粒容易团聚等缺点，严重降低了硫化镉的光催化效率。将硫化镉与能带结构不同的半导体材料行复合，以形成异质结结构，改变其光生电子空穴对的转移机制，从而使其光催化材料的活性提高。
本专利主要采用原位沉淀法制备钨酸锌/硫化镉复合可见光催化剂，这种催化剂可应用于光催化水解制氢技术中。
发明内容
本发明要解决的技术问题是：基于上述问题，本发明提供一种制备高效钨酸锌/硫化镉复合可见光催化剂的制备方法。
本发明解决其技术问题所采用的一个技术方案是：一种钨酸锌/硫化镉复合可见光催化剂的制备方法，包括以下步骤：
(1)硫化镉的制备：将硝酸镉和硫脲同时加入乙二胺中，超声搅拌0.5h，混合溶液转至水热反应釜中，160℃反应24h，冷却，抽滤，洗涤，烘干；
(2)钨酸锌/硫化镉复合光催化剂的制备：蒸馏水中加入硫化镉，超声搅拌0.5h，加入硝酸锌，超声搅拌0.5h。蒸馏水中加入钨酸钠，超声搅拌0.5h，然后将其滴加入硫化镉和硝酸锌溶液中，超声搅拌0.5h，加入氟化铵，超声搅拌0.5h，混合溶液转至水热反应釜中，180℃反应6h，冷却，离心，用水洗涤，烘干即得产品。
进一步地，步骤(1)中硝酸镉和硫脲的质量比为1：3。
进一步地，步骤(2)中钨酸锌与硫化镉的质量比为1.2～1.6：1，钨酸锌与硝酸锌与钨酸钠与氟化铵的摩尔比为1：1：1：6。
本发明的有益效果是：该制备方法简单，易于操作，且制备条件容易控制，所制备的钨酸锌/硫化镉复合可见光催化剂为绿色无污染高性能催化剂，且催化效率高，具有一定应用前景。
附图说明
下面结合附图对本发明进一步说明。
图1是本发明实施例1-3制备得到的钨酸锌/硫化镉复合可见光催化剂的X射线衍射图；
图2是本发明实施例2制备得到的钨酸锌/硫化镉复合可见光催化剂的扫描电镜图；
图3是本发明实施例2制备得到的钨酸锌/硫化镉复合可见光催化剂的透射电镜图；
图4是本发明实施例1-3制备得到的钨酸锌/硫化镉复合可见光催化剂的水解制氢效果图。
图5本发明实施例2制备得到的钨酸锌/硫化镉复合可见光催化剂的水解制氢循环效果图。
具体实施方式
现在结合具体实施例对本发明作进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
(1)硫化镉的制备：量取70mL的乙二胺同时加入4.66g的四水合硝酸镉及3.45g硫脲，搅拌0.5h，将反应容器中的溶液转至水热反应釜中，160℃反应24h，冷却，抽滤，洗涤，烘干；
(2)钨酸锌/硫化镉复合光催化剂的制备：将0.1g硫化镉加入30mL蒸馏水，超声搅拌0.5h，加入1.1396g六水合硝酸锌，超声搅拌0.5h。将1.2635g二水合钨酸钠加入30mL蒸馏水，超声搅拌0.5h，然后将其滴加入硫化镉和硝酸锌溶液中，超声搅拌0.5h，加入0.1418g氟化铵，继续超声搅拌0.5h，混合溶液转至水热反应釜中，180℃反应6h，冷却，离心，用水洗涤，烘干即得产品。
实施例2
(1)硫化镉的制备：量取70mL的乙二胺同时加入4.66g的四水合硝酸镉及3.45g硫脲，搅拌0.5h，将反应容器中的溶液转至水热反应釜中，160℃反应24h，冷却，抽滤，洗涤，烘干；
(2)钨酸锌/硫化镉复合光催化剂的制备：将0.1g硫化镉加入30mL蒸馏水，超声搅拌0.5h，加入1.3295g六水合硝酸锌，超声搅拌0.5h。将1.4741g二水合钨酸钠加入30mL蒸馏水，超声搅拌0.5h，然后将其滴加入硫化镉和硝酸锌溶液中，超声搅拌0.5h，加入0.1654g氟化铵，超声搅拌0.5h，混合溶液转至水热反应釜中，180℃反应6h，冷却，离心，用水洗涤，烘干即得产品。
实施例3
(1)硫化镉的制备：量取70mL的乙二胺同时加入4.66g的四水合硝酸镉及3.45g硫脲，搅拌1h，将反应容器中的溶液转至水热反应釜中，160℃反应24h，冷却，抽滤，洗涤，烘干；
(2)钨酸锌/硫化镉复合光催化剂的制备：将0.1g硫化镉加入30mL蒸馏水，超声搅拌0.5h，加入1.5195g六水合硝酸锌，超声搅拌0.5h。将1.6847g二水合钨酸钠加入30mL蒸馏水，超声搅拌0.5h，然后将其滴加入硫化镉和硝酸锌溶液中，超声搅拌0.5h，加入0.1890g氟化铵，继续超声搅拌0.5h，混合溶液转至水热反应釜中，180℃反应6h，冷却，离心，用水洗涤，烘干即得产品。
应用例：钨酸锌/硫化镉复合可见光催化剂的水解产氢性能测定
实施例1-3所制备的钨酸锌/硫化镉复合可见光催化剂的晶相结构由日本理学D/max2500PC自转X-射线衍射仪分析，其中，X射线为Cu靶Kα电压40kV，电流100mA，步长为0.02°，扫描范围10°～80°。X射线衍射图谱如图1所示，在(100)、(011)、(111)等位置的峰形充分表明了钨酸锌的成功合成。复合材料良好匹配的强烈衍射峰证明该样品是不含其他杂质的两相结构且具有高结晶度。
采用日本JSM-6360A型扫描电子显微镜观察实施例2制备的钨酸锌/硫化镉复合可见光催化剂的形貌，扫描电镜图如图2所示，从图可以看出，本实施方式制备的复合可见光催化剂中硫化镉纳米棒的尺寸约为长1mm，宽35nm，其表面负载着尺寸均匀的颗粒状钨酸锌。
采用日本JEM-2100型透射电子显微镜观察实施例2制备的钨酸锌/硫化镉复合可见光催化剂，透射电镜图如图3所示，从图可以看出，硫化镉棒表面分布着大量尺寸均匀的颗粒状钨酸锌，这与扫描的分析结果符合。
钨酸锌/硫化镉复合可见光催化剂的光催化性能以及潜在应用性研究
将实施例1中制备的钨酸锌/硫化镉作为光催化剂分解水产氢。取钨酸锌/硫化镉光催化剂10mg加入100mL蒸馏水，牺牲剂为2.7314g硫化钠及3.151g亚硫酸钠。使用的氙灯光源为PLS-SXE300/300UV并配有420UVcut滤波片，光分解水产生的氢气由在线热导率检测器(TCD)气相色谱分析仪检测(NaX沸石柱，TCD探测器，N2载气)。
实施例1-3所制备的钨酸锌/硫化镉复合可见光催化剂分解水制氢效果如图4所示，其光解水制氢速率分别为62.66mmol/h/g，79.27mmol/h/g，73.93mmol/h/g，而纯硫化镉的光解水制氢速率最低，为1.21mmol/h/g。
实施例2所制备的钨酸锌/硫化镉复合可见光催化剂分解水产氢循环效果如图5所示，在连续催化反应5次循环共15小时后，钨酸锌/硫化镉复合可见光催化剂的制氢量仍可保持第一次循环制氢量的92.4％以上，而同等条件下，纯硫化镉的制氢量仅可保持第一次循环制氢量的38％。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (3)
1.一种钨酸锌/硫化镉复合可见光催化剂的制备方法，其特征是：包括以下步骤：
(1)硫化镉的制备：将硝酸镉和硫脲同时加入乙二胺中，超声搅拌0.5h，混合溶液转至水热反应釜中，160℃反应24h，冷却，抽滤，洗涤，烘干；
(2)钨酸锌/硫化镉复合光催化剂的制备：蒸馏水中加入硫化镉，超声搅拌0.5h，加入硝酸锌，超声搅拌0.5h。蒸馏水中加入钨酸钠，超声搅拌0.5h，然后将其滴加入硫化镉和硝酸锌溶液中，超声搅拌0.5h，加入氟化铵，继续超声搅拌0.5h，混合溶液转至水热反应釜中，180℃反应6h，冷却，离心，用水洗涤，烘干即得产品。
2.根据权利要求1所述的硫化镉光催化剂的制备方法，其特征是：所述的步骤(1)中硝酸镉和硫脲的摩尔比为1：3。
3.根据权利要求1所述的钨酸锌/硫化镉复合可见光催化剂的制备方法，其特征是：所述的步骤(2)中钨酸锌与硫化镉的质量比为1.2～1.6：1，钨酸锌与硝酸锌与钨酸钠与氟化铵的摩尔比为1：1：1：6。
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