CN108940281B - 一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法 - Google Patents
一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法 Download PDFInfo
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Abstract
本发明属于纳米材料领域，具体涉及一种新型纳米光催化材料Ag2MoO4‑WO3异质结的制备方法，将WO3加入到超纯水中并进行超声分散得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤若干次，所得沉淀在真空干燥箱中干燥，即得Ag2MoO4‑WO3异质结。此异质结生产成本低，光催化降解有机污染物效率高且无二次污染，极大提高对太阳光的利用率，节约能源，可循环使用。
Description
技术领域
本发明属于纳米材料领域，具体涉及一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法。
背景技术
为了更大限度的利用太阳光，人们开发了更高效的可见光响应型光催化剂。WO3是一种 n型可见光响应的半导体催化剂，具有较高的光活性，稳定的物理化学性质，抗光腐蚀效应强的可见光响应的光催化剂，在解决环境污染和能源短缺问题上拥有巨大潜力。然而，WO3作为可见光响应的半导体光催化剂还有很多缺陷，比如相对较窄的禁带宽度(2.4-2.8eV)， WO3光催化剂的导带位置偏低，光生电子难以还原溶液中吸附的O2，导致光生空穴与电子的复合率较高，从而限制其在光降解反应中的催化活性。为了弥补单独WO3作为可见光响应的光催化剂的缺陷，已经提出形貌修饰，离子参杂，构建异质结等方法。Ag2MoO4是一种p型的半导体催化剂，在光致发光，生物消毒，电催化氧还原等方面应用广泛。由于其形貌和微观结构容易被控制，所以Ag2MoO4作为光催化剂的催化性能受到很多因素的影响。但是，Ag2MoO4单独作为半导体催化剂的对可见光利用效率较低，因而催化效果很低。
发明内容
根据以上现有技术的不足，本发明提供一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，此异质结生产成本低，光催化降解有机污染物效率高且无二次污染，极大提高对太阳光的利用率，节约能源，可循环使用。
本发明所述的一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：将WO3加入到超纯水中并进行超声分散得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤若干次，所得沉淀在真空干燥箱中干燥，即得 Ag2MoO4-WO3异质结，为方便描述，下文统一称为Ag-Wp-n异质结。
其中，优选方案如下：
所述Ag2MoO4-WO3异质结中，Ag2MoO4与WO3的质量百分比为Ag2MoO4： WO3＝0.05～0.2:1，可以为Ag2MoO4：WO3＝0.05:1、Ag2MoO4：WO3＝0.1:1、Ag2MoO4： WO3＝0.15:1、Ag2MoO4：WO3＝0.2:1，其中，最优选为Ag2MoO4：WO3＝0.1:1
所述AgNO3与Na2MoO4的摩尔比为2:1。
将WO3加入到超纯水中并进行超声分散20～40min得到WO3的悬浮液。
逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌10～60min。
逐滴加入Na2MoO4·2H2O溶液并遮光搅拌2～5h。
用去离子水和乙醇洗涤的次数为2～5次。
所得沉淀在真空干燥箱中50～70℃条件下干燥5～7h。
本发明的优点在于：(1)本发明所制备的Ag-Wp-n异质结与单独Ag2MoO4和WO3的相比，降解罗丹明B(RhB)的效率能达到单独Ag2MoO4或WO3的2倍；(2)本发明所制备的Ag-Wp-n异质结在210min内降解抗生素盐酸四环素(TC)的效率高达100％且没有二次产物生成；(3)本发明所制备的Ag-Wp-n异质结在320min内降解无色染料4-氯苯酚(4-CP) 的效率高达70％；(4)本发明所制备的Ag-Wp-n异质结作为光催化剂经过4次循环实验，其催化降解有机污染物的性能基本没有降低，可以有效的回收循环使用。
附图说明
图1为实施例5中不同含量的Ag-Wp-n异质结与单独Ag2MoO4，WO3以及标准催化剂二氧化钛(P25)降解罗丹明B(RhB)的性能对比图；
图2为实施例6中Ag-Wp-n异质结光催化降解盐酸四环素(TC)的高效液相色谱图；
图3为实施例7中Ag-Wp-n异质结光催化降解4-氯苯酚(4-CP)的高效液相色谱图；
图4为实施例8中Ag-Wp-n异质结光催化降解RhB四次循环性能图；
图5为实施例8中Ag-Wp-n异质结光催化降解RhB四次循环前后的XRD对比图；
图6为实施例2中Ag-Wp-n异质结的SEM图以及EDS图，图6(a)和图6(c)均为 200nm倍数下SEM图，图6(b)为400nm倍数下SEM图，图6(d)为EDS图；
图7为实施例2中Ag-Wp-n异质结的TEM图，图7(a)为100nm倍数下TEM图，图 7(b)为50nm倍数下TEM图，图7(c)为20nm倍数下TEM图，图7(d)为50nm倍数下TEM图；
图8为实施例2中Ag-Wp-n异质结与单独Ag2MoO4和WO3的XRD对比图；
图9为实施例2中Ag-Wp-n异质结与单独Ag2MoO4和WO3的固体紫外对比图。
具体实施方式
以下结合实施例和附图对本发明作进一步描述。
实施例1：
一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，按照Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.05:1进行各原材料称量选取，将WO3加入到超纯水中并进行超声分散30min得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌30min，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌4h，所述AgNO3与Na2MoO4的摩尔比为2:1；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤3次，所得沉淀在真空干燥箱中中60℃条件下干燥6h，即得Ag2MoO4-WO3异质结。
实施例2：
一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，按照Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.1:1进行各原材料称量选取，将WO3加入到超纯水中并进行超声分散40min得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌 40min，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌4h，所述AgNO3与Na2MoO4的摩尔比为 2:1；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤4次，所得沉淀在真空干燥箱中中 60℃条件下干燥6h，即得Ag2MoO4-WO3异质结。
如图6和图7所示，反映了通过上述方法制备的Ag-Wp-n异质结的形貌，Ag2MoO4颗粒沉积在片状结构的WO3上，改变了WO3的初始形貌。TEM中的Ag2MoO4和WO3的晶格间距与XRD的标准卡对应。
如图8所示，Ag-Wp-n异质结的结晶度很好，与Ag2MoO4和WO3的标准卡相对应；纯度很高，没有杂质参杂。
如图9所示，Ag-Wp-n异质结对可见光的响应更大，可以更加有效的利用太阳光，异质结的光催化性能更高。
实施例3：
一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，按照Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.15:1进行各原材料称量选取，将WO3加入到超纯水中并进行超声分散40min得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌40min，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌4h，所述AgNO3与Na2MoO4的摩尔比为2:1；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤4次，所得沉淀在真空干燥箱中中60℃条件下干燥6h，即得Ag2MoO4-WO3异质结。
实施例4：
一种新型纳米光催化材料Ag2MoO4-WO3异质结的制备方法，按照Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.2:1进行各原材料称量选取，将WO3加入到超纯水中并进行超声分散30min得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液并中持续搅拌 30min，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌2～5h，所述AgNO3与Na2MoO4的摩尔比为2:1；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤5次，所得沉淀在真空干燥箱中中60℃条件下干燥6h，即得Ag2MoO4-WO3异质结。
实施例5：
如图1所示，将实施例1～4制备的Ag-Wp-n异质结与单独Ag2MoO4，WO3以及标准催化剂二氧化钛(P25)降解罗丹明B(RhB)，采用带有420nm紫外光滤波片的氙灯做模拟可见光光源，功率为300W。100mg的催化剂分别加入到盛有100mL10mg/LRhB的反应器中并在黑暗中搅拌60min后达到催化剂和污染物分子之间的吸附-脱附平衡。可见光照射下，在一定时间间隔内去2.0mL样品离心后的上清液通过紫外可见分光光度计测RhB溶液在特征波长处的吸光度,通过标准曲线对应相应RhB的浓度。
对比可以发现，Ag-Wp-n异质结降解罗丹明B(RhB)的效率能达到单独Ag2MoO4或WO3的2倍。
实施例6：
如图2所示，采用实施例2制备的Ag-Wp-n异质结光催化降解盐酸四环素(TC)，采用带有420nm紫外光滤波片的氙灯做模拟可见光光源，功率为300W。100mg的催化剂分别加入到盛有100mL 20mg/L TC溶液的反应器中并在黑暗中搅拌60min后达到催化剂和污染物分子之间的吸附-脱附平衡。一定时间间隔内取TC样品2.0mL，用0.22μm注射器式过滤器过滤后，液相色谱仪(HPLC安捷伦1100系列)分析TC浓度变化。HPLC紫外检测器280nm,流动相为80％甲醇，20％超纯水，流速为0.5mLmin-1。
可以发现，210min内降解抗生素盐酸四环素(TC)的效率高达99％且没有二次污染物生成。
实施例7：
如图3所示，采用实施例2制备的Ag-Wp-n异质结光催化降解4-氯苯酚(4-CP)，采用带有420nm紫外光滤波片的氙灯做模拟可见光光源，功率为300W。100mg的催化剂分别加入到盛有100mL5mg/LTC溶液的反应器中并在黑暗中搅拌60min后达到催化剂和污染物分子之间的吸附-脱附平衡。一定时间间隔内取4-CP样品2.0mL，用0.22μm注射器式过滤器过滤后，液相色谱仪(HPLC安捷伦1100系列)分析4-CP浓度变化。HPLC紫外检测器280nm, 流动相为8％甲醇，72％草酸，乙腈20％，流速为0.5mLmin-1。
可以发现，在320min内降解无色染料4-氯苯酚(4-CP)的效率高达70％。
实施例8：
如图4和图5所示，采用实施例2制备的Ag-Wp-n异质结进行循环实验，循环实验通过降解4次RhB来评估，其降解方法与降解RhB一致。一次降解完成后，将催化剂离心回收，干燥后，进行下一次循环实验。Ag-Wp-n异质结作为光催化剂经过4次循环实验，其催化降解有机污染物的性能基本没有降低，XRD图显示Ag-Wp-n异质结的稳定性很高，只有少量钼酸银还原成银，但并不影响Ag-Wp-n异质结的催化性能，可以有效的回收循环使用。
Claims (9)
1.一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：将WO3加入到超纯水中并进行超声分散得到WO3的悬浮液；逐滴加入AgNO3溶液到上述WO3的悬浮液中并持续搅拌，再逐滴加入Na2MoO4·2H2O溶液并遮光搅拌；上述搅拌后的溶液经离心后，用去离子水和乙醇洗涤若干次，所得沉淀在真空干燥箱中干燥，即得Ag2MoO4-WO3异质结。
2.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：所述Ag2MoO4-WO3异质结中，Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.05～0.2:1。
3.根据权利要求2所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：所述Ag2MoO4-WO3异质结中，Ag2MoO4与WO3的质量百分比为Ag2MoO4：WO3＝0.1:1。
4.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：AgNO3与Na2MoO4的摩尔比为2:1。
5.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：将WO3加入到超纯水中并进行超声分散20～40min得到WO3的悬浮液。
6.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：逐滴加入AgNO3溶液到上述WO3的悬浮液中并持续搅拌10～60min。
7.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：逐滴加入Na2MoO4·2H2O溶液并遮光搅拌2～5h。
8.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：用去离子水和乙醇洗涤的次数为2～5次。
9.根据权利要求1所述的一种纳米光催化材料Ag2MoO4-WO3异质结的制备方法，其特征在于：所得沉淀在真空干燥箱中50～70℃条件下干燥5～7h。
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