CN111774053A - 一种制备镝掺杂纳米片钨酸铋光催化剂的方法 - Google Patents
一种制备镝掺杂纳米片钨酸铋光催化剂的方法 Download PDFInfo
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Abstract
一种制备镝掺杂纳米片钨酸铋光催化剂的方法，其属于无机催化材料技术领域。本发明先将Bi(NO3)3·5H2O、Dy(NO3)3·5H2O固体溶解于稀硝酸溶液，再将Na2WO4·2H2O水溶液缓慢滴入稀硝酸溶液中，然后用NaOH溶液调节反应液pH值形成前驱体悬浊液并转入反应釜，再通过水热法制备出了镝掺杂纳米片钨酸铋光催化剂(Dy3+/Bi2WO6)。本发明方法制备工艺简单、使用设备少、能耗低。制备的Dy3+/Bi2WO6光催化活性高，在模拟太阳光氙灯照射下，用0.1g磁性复合光催化剂降解100mL浓度为10mg/L的罗丹明B溶液，105min对罗丹明B的降解率达到99.8％。本发明制备出的产品可广泛用于光催化降解有机污染物领域。
Description
技术领域
本发明涉及一种制备镝掺杂纳米片钨酸铋光催化剂(Dy3+/Bi2WO6)的方法，属于无机催化剂技术领域。
背景技术
Bi2WO6具有特殊的层状结构，是Aurivillius家族中最简单氧化物之一，具有光催化活性。Bi2WO6属于正交晶型，是由萤石状的(Bi2O2)n 2+层和钙钛矿状的(WO4)n 2-层沿(100)晶面方向交错叠合而构成的层状化合物。制备Bi2WO6常见的几种方法有：高温固相法、液相合成法、溶胶凝胶法、微乳液法、(微波辅助)水热法、非晶态络合物法等。Bi2WO6半导体催化剂存在一些缺点，如光生载流子的再结合率较高，主要响应紫外光，对可见光有响应微弱。基于此，科研工作者开始了对Bi2WO6光催化剂的改性工作，常见的改性方法有离子掺杂、形貌调控、贵金属负载、构筑异质结等。
目前，对Bi2WO6的研究主要集中在如何提高其光催化活性方面，用稀土元素镝(Dy)掺杂改性Bi2WO6光催化剂活性的研究鲜有报道。如“Applied Catalysis B:Environmental”2009年第92卷中的“Enhanced photocatalytic activity of Bi2WO6 loaded with Agnanoparticles under visible light irradiation”(对比文件1)，采用醇热法(乙二醇)制备得到银纳米颗粒负载的Bi2WO6光催化剂，该方法的不足之处在于：(1)合成过程在纯有机溶剂(乙二醇)系统中进行，存在安全隐患，未反应的乙二醇将随水洗过程进入废水中而增加了环境污染源；(2)使用贵金属银，并用纯乙二醇作为溶剂，成本高；(3)通过对E.coli和S.epidermidis灭活效果评价光催化剂的活性，未开展对废水中有机物的降解特性研究。
又如“稀土”2015年35卷第1期“Gd3+、Dy3+掺杂Bi2WO6的合成及光催化脱硫活性的研究”(对比文件2)，采用水热法制备了Gd3+、Dy3+掺杂的Bi2WO6光催化剂。该方法的不足之处在于：(1)制备Dy3+掺杂Bi2WO6时，以钨酸铵、硝酸镝、硫脲等为主要原料，酸性环境下可能产生有毒气体硫化氢，同时产生含氨氮的废水(氨氮属于国家水体污染总量控制指标)；(2)脱硫效率不高，掺杂后效率提高不明显(开展的是脱出模拟汽油中硫的实验)，当汽油中硫初始浓度为586μg/g(0.586mg/g)时，光照3h下，Bi2WO6和Dy3+掺杂Bi2WO6的脱硫率分别约为86％和89％(文中未给出数据，从其中的图5初略估算)。
发明内容
本发明的目的是针对Bi2WO6光催化活性不佳、可见光响应差的问题，提出一种镝对Bi2WO6光掺杂改性制备Dy3+/Bi2WO6光催化剂的方法，制备方法简单、成本低。制备的Dy3+/Bi2WO6光催化剂在模拟太阳光照射下具有较高的光催化效率。
本发明Dy3+/Bi2WO6光催化剂的制备方法如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比1％-10％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
本发明采用上述技术方案，主要有以下效果：
(1)本发明方法制备的Dy3+/Bi2WO6光催化剂具有较高的光催化活性，在模拟太阳光氙灯照射下，0.1g磁性Dy3+/Bi2WO6光催化剂分散于100mL浓度为10mg/L的罗丹明B溶液中，光照105min后对罗丹明B的降解率达到99.8％，远高于未掺杂的Bi2WO6(86.7％)。
(2)本发明方法制备的Dy3+/Bi2WO6光催化剂的带隙为3.28eV(低于未掺杂Bi2WO6的3.40eV)，增强了其可见光的响应性；Dy3+/Bi2WO6光催化剂的比表面积为25.2m2/g(大于未掺杂Bi2WO6的21.4m2/g)，其制备操作简单，所需设备少，能耗低。
附图说明
图1为Bi2WO6、Dy3+/Bi2WO6的X射线衍射图谱。
图2为Bi2WO6、Dy3+/Bi2WO6的扫描电子显微镜图。
图3为Bi2WO6、Dy3+/Bi2WO6的RhB降解曲线图。
图4为Bi2WO6、Dy3+/Bi2WO6的荧光光谱图。
具体实施方式
下面结合具体实施方式，进一步说明本发明。
实施例1
一种制备Dy3+/Bi2WO6光催化剂的方法，具体步骤如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比1％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
实施例2
一种制备Dy3+/Bi2WO6光催化剂的方法，具体步骤如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比3％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
实施例3
一种制备Dy3+/Bi2WO6光催化剂的方法，具体步骤如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比5％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
实施例4
一种制备Dy3+/Bi2WO6光催化剂的方法，具体步骤如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比7％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
实施例5
一种制备Dy3+/Bi2WO6光催化剂的方法，具体步骤如下：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比10％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到Dy3+/Bi2WO6光催化剂。
实验结果
实施例3制备的Dy3+/Bi2WO6光催化剂对罗丹明B的催化降解活性最佳。为了方便对比，制备了Bi2WO6样品。Bi2WO6制备方法为实施例3中不加入Dy(NO3)3·5H2O4。
Bi2WO6、Dy3+/Bi2WO6的X射线衍射图谱如图1所示。可见，Dy3+离子掺杂不改变Bi2WO6的晶体结构，即不同掺杂量的样品其特征衍射峰的位置均一致。样品在衍射角2θ＝28.3°、32.9°、47.2°、56.0°、58.9°、68.8°、76.5°、79.0°处的特征衍射峰分别与(131)、(200)、(202)、(133)、(262)、(193)、(402)、(462)晶面相对应，所有衍射峰均对应于正交相的Bi2WO6(JCPDSNo.39-0256)，晶胞参数为
Dy3+/Bi2WO6的晶粒尺寸为16.2nm，小于Bi2WO6的21nm。
Bi2WO6、Dy3+/Bi2WO6的扫描电子显微镜图如图2所示。纯Bi2WO6(图2a)是由分散性良好、不规则且表面光滑的纳米薄片积聚而成，纳米片直径介于250-300nm之间，厚度大约在25-30nm之间；Dy3+/Bi2WO6(图2b)样品也呈现不规则纳米片状，但纳米片尺寸介于150-200nm，厚度约为15nm，且表面不光滑，分散性较差；Dy3+离子掺杂不会改变Bi2WO6的微观形貌，但会抑制Bi2WO6晶体的生长，导致晶粒尺寸变小。
Bi2WO6、Dy3+/Bi2WO6的RhB降解曲线如图3所示。可见，Dy3+/Bi2WO6样品的曲线下降最快，在105min时，其降解率达到99.8％，远高于未掺杂Bi2WO6(86.9％)。
Bi2WO6、Dy3+/Bi2WO6的荧光光谱图如图4所示。可以看出，两者的PL光谱曲线相似，但Dy3+掺杂Bi2WO6的荧光发射峰强度明显低于纯相的Bi2WO6，导致Bi2WO6纳米片表面产生更多缺陷位点或氧空位，使得光生电子容易迁移至这些新位点，进而降低了光生载流子的复合几率；较低的光生载流子结合率意味着更高的光催化活性，这与光催化测试结果是一致的。
Claims (2)
1.一种制备镝掺杂纳米片钨酸铋光催化剂的方法，其特征在于包括以下步骤：
称取4mmol的Bi(NO3)3·5H2O固体于烧杯中，按摩尔比1％-10％称取Dy(NO3)3·5H2O放入扇贝柱，加入40mL浓度为1mol/L的稀硝酸溶液，超声溶解得到无色透明溶液A；称取2mmol的Na2WO4·2H2O于另一烧杯中，加入20mL去离子水充分溶解得到无色透明溶液B；在地磁力搅拌的作用下，将溶液B液缓慢逐滴加入溶液A中，得到白色前驱体悬浊液C；用2mol/L的NaOH溶液精确调节悬浊液C的pH为4.0，继续磁力搅拌1h后，将悬浊液C转移至100mL高压不锈钢反应釜内衬中，将反应釜放入恒温烘箱，160℃下反应时间24h；反应结束，取出反应釜自然冷却至室温，过滤，滤饼用蒸馏水和无水乙醇各洗涤三次后，放入烘箱中，60℃下烘干即得到镝掺杂纳米片钨酸铋光催化剂。
2.根据权利要求1所述的镝掺杂纳米片钨酸铋光催化剂的制备方法，其特征在于以水热法制备，提高了钨酸铋的光催化活性。
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