CN113955823B - 1T/2H MoSe2/Bi2WO6压电-光复合催化剂的应用 - Google Patents
1T/2H MoSe2/Bi2WO6压电-光复合催化剂的应用 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 229910016001 MoSe Inorganic materials 0.000 title claims abstract description 20
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims description 23
- 230000000593 degrading effect Effects 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 13
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- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001782 photodegradation Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明属于压电光催化剂领域，特别涉及一种混合相1T/2H MoSe2/Bi2WO6(1T/2H MS/BWO)复合催化剂的应用。采用简单的浸渍法合成1T/2H MS/BWO复合催化剂，通过太阳光照射和超声波振动协同作用下，进行压电光催化降解罗丹明B。本发明合成简单，绿色无污染，操作性强，制备的催化剂具有丰富的活性位点和优异的稳定性，不产生二次污染等特点。
Description
技术领域
本发明属于压电光催化剂及应用领域，具体涉及一种压电光降解罗丹明B的混合相1T/2H MoSe2/Bi2WO6(1T/2H MS/BWO)复合催化剂及其制备方法。
背景技术
近年来，生态环境污染和能源资源短缺问题变得越来越严重，尤其是工业废水和有机染料的造成的污染。通过压电光催化解决有机污染物问题的应用受到了广泛的关注。压电催化是指压电材料利用机械振动能诱导催化剂颗粒表面产生正负电荷，形成还原和氧化能力很强的活性物质，进而发生一系列氧化还原反应，达到降解有机污染物的目的。但是，压电催化效率受很多因素的影响，例如比表面积，载流子分离效率等。将压电催化与光催化结合起来，能够大大的提升压电催化应用的性能。然而，构建高效的压电光催化剂到目前为止仍然是一大难题。
最近，钙钛矿型铁电体如NaNbO3，BiFeO3，ZnSnO3和铋层铁电体BWO和Bi4Ti3O12等，这些材料同时具有压电和光催化活性，能有效的降解有机污染物。其中，Bi2WO6是一种典型的压电-光催化材料，由类钙钛矿(WO4)2-和类萤石(Bi2O2)2+交替层构成，有较窄的带隙(2.7eV)，并且花球状结构的BWO能为催化反应能够提供较多的活性位点，被广泛应用到降解污染物中。但是，纯BWO的光生电子和空穴有较高重组率，阻碍了催化活性，限制了在催化性能上的大规模应用。
通过构建具有丰富电子捕获的助催化复合材料作为氧化还原反应的活性位点，可以有效提高催化性能。因此，制备出具有压电光催化活性的复合材料对于光生载流子的分离和压电光催化的活性具有重要意义。MoSe2作为一种优异的压电光催化材料，其带隙约为1.4eV，混合相1T/2HMoSe2纳米片显示出强大的压电响应，压电电位建立在1T和2H两相的界面区域，而且在MoSe2纳米片的顶面和底面的极化表面上观察到了压电和弯曲电位耦合效应，从而建立的内部电场以分离电子-空穴，达到降解的效果。然而，目前尚未报道过混合相1T/2HMS/BWO复合催化剂的制备及其在压电-光催化上的应用。
因此，本专利采用简单的浸渍法制备了一种具有优异的压电-光催化的1T/2HMS/BWO复合材料。BWO的花球状结构可以为片状的MoSe2提供了较大的接触界面，能使它们更好的耦合，更有利于光电子跟空穴的分离。进一步探究了混合相态1T/2HMS/BWO复合材料在光催化，压电催化和压电-光催化中对有机污染物的降解。结果表明，1T/2HMS/BWO复合材料在降解有机污染物方面表现出显著的压电光催化效率和很强的稳定性，证实了其在处理污染物上具有良好的应用前景。
发明内容
本发明的目的在于提供一种混合相1T/2H MS/BWO复合催化剂及其制备方法，并将其应用在压电光降解罗丹明B，具有高催化活性和较好的稳定性。
本发明的技术方案：本发明提供的混合相1T/2H MS/BWO复合催化剂的制备方法为：
(1)Bi2WO6制备：铋源和钨源加入去离子水中，室温搅拌溶解。将混合液转移到内衬聚四氟乙烯的反应釜中，在烘箱中进行水热反应；待冷却至室温后过滤、洗涤、干燥、研磨，最终得到白色粉末，即为Bi2WO6催化剂(BWO)；Bi(NO)3 ·5H2O作为铋源；Na2WO4.2H2O作为钨源；其中Bi(NO)3 .5H2O和Na2WO4 .2H2O的质量比为2.9：1，水热反应温度为190℃，反应时间为2h。
(2)1T/2H MoSe2制备：将Se粉作为硒源，Na2MoO4作为钼源，加入还原剂NaBH4混于去离子水中，搅拌至红棕色溶液。将所得红棕色溶液转移到内衬聚四氟乙烯的反应釜中，在烘箱中进行水热反应；待冷却至室温后过滤、洗涤、干燥、研磨，最终得到黑色粉末，即为1T/2H MoSe2催化剂；硒粉、Na2MoO4、NaBH4的质量比为1：1.53：0.92；水热反应温度为120℃-240℃，优选220℃，反应时间为20h。
(3)1T/2H MS/BWO复合催化剂制备：将1T/2H MoSe2催化剂和BWO催化剂溶于无水乙醇中，进行超声、搅拌，混合均匀，室温下过滤、洗涤、干燥、研磨，最终得到灰色粉末，即为1T/2H MS/BWO复合催化剂。加入的Bi2WO6质量是1T/2H MoSe2质量的0.5％～5％。
上述方法制备的1T/2H MS/BWO复合催化剂具有纳米片集成的花球状结构。
使用本发明具有的优点：
(1)本发明提供的催化剂为混合相1T/2H MS/BWO复合催化剂，其合成条件简单且易于操作、快速高效、节能环保，稳定性好等特点；
(2)MoSe2催化剂的引入没有改变BWO的晶体结构，没有出现其他衍射峰，表明1T/2H MS/BWO复合材料具有优异的结晶度和纯度。通过对于稳定性前后的XRD图谱进行比较，发现循环后样品的晶体结构没有明显变化。同时具有良好的稳定性。
(3)1.5％1T/2H MS/BWO复合催化剂在纯光催化、纯压电催化和压电-光协同作用下仅在20min内即可降解大部分的有机物，降解能力很强，且降解RhB的效率比纯BWO分别高16％、12％、27.4％，表明混合相1T/2HMoSe2负载在BWO上能够提升降解效率，同时说明催化剂在压电-光协同作用下降解RhB效果明显。
附图说明：
图1是实施例4、7、10、1合成的不同比例和相态的1T/2H MS/BWO催化剂和BWO的XRD图。
图2是实施例1合成的BWO催化剂的扫描电镜图。
图3为实施例7合成的1.5％1T/2H MS/BWO催化剂的扫描电镜图。
图4是在太阳光照射下不同比例1T/2H MS/BWO催化剂和BWO的降解罗丹明B的性能图。
图5是在超声波振动下不同比例1T/2H MS/BWO催化剂和BWO的降解罗丹明B的性能图。
图6是同时在太阳光照射和超声波振动作用下不同比例1T/2HMS/BWO催化剂和BWO的降解罗丹明B的性能图。
图7为1.5％1T/2H MS/BWO和BWO氮气吸附脱曲线
图8为1.5％1T/2H MS/BWO和BWO孔径分布图。
具体实施方式
下面结合具体的实施例对本发明进行详细说明。
降解效率是按如下公式计算：
R＝(C-C0)/C0*100％
R:降解效率
C0:初始浓度
C:降解反应后的浓度
实施例1
称取1.94g Bi(NO)3 .5H2O溶于50ml去离子水中搅拌溶解，再将0.66gNa2WoO4 .2H2O加入上述混合液中，室温剧烈搅拌1h。将混合液转移到100ml内衬聚四氟乙烯的反应釜中，在190℃的烘箱中加热2h，待冷却至室温后过滤、洗涤、干燥、研磨，最终得到白色粉末，即为BWO粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在太阳光照射下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为34.4％。
实施例2
其他同实施例1，得到白色粉末，即为BWO粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在超声波振动(超声波振动条件没有限定,只要能起到超声作用就行)。下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为21.2％。
实施例3
其他同实施例1，得到白色粉末，即为BWO粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，同时在太阳光照射和超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为72.4％。
实施例4
其他同实施例1，得到白色粉末，即为BWO粉末。称取0.316g的硒粉加入75ml的去离子水中，搅拌10min。再将0.304gNaBH4加入上述溶液中，当混合液颜色变成无色时，再向其中加入0.484gNa2MoO4,溶液立马变成红棕色溶液，然后再搅拌20min。将混合液转移到100ml内衬聚四氟乙烯的反应釜中，在220℃的烘箱中加热20h，待冷却至室温后过滤、洗涤、干燥、研磨，最终得到黑色粉末，即为1T/2H MoSe2催化剂。再称取0.5gBWO和0.0025g 1T/2HMoSe2溶于一定量的无水乙醇中，超声2h，将上述混合液在室温下剧烈搅拌4h，室温下过滤、洗涤、干燥、研磨，最终得到0.5％1T/2HMS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在太阳光照射下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为45.4％。
实施例5
其他同实施例4，得到0.5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为21.6％。
实施例6
其他同实施例4，得到0.5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，同时在太阳光照射和超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为83％。
实施例7
称取0.5g BWO和0.0075g 1T/2H MoSe2其他同实施例4，得到1.5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在太阳光照射下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为50.4％。
实施例8
其他同实施例7，得到1.5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为33.2％。
实施例9
其他同实施例7，得到1.5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，同时在太阳光照射和超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为99.8％，基本实现完全降解。
稳定性实验：重复四次稳定性实验之后，在压电光催化中20min降解效果任然达到99％，稳定性极好。
实施例10
称取0.5g Bi2WO6和0.025g 1T/2H MoSe2其他同实施例4，得到5％1T/2H MS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在太阳光照射下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为40.8％。
实施例11
其他同实施例10，得到5％1T/2HMS/BWO灰色粉末。
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，在超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为24.4％。
实施例12
其他同实施例10，得到5％1T/2H MS/BWO灰色粉末
称取10mg催化剂和30ml的10mol/L的罗丹明B，在暗态条件下搅拌30min达到吸附-脱附平衡，同时在太阳光照射和超声波振动下降解20min，每5min取一次样，通过测量吸光度，计算降解效率，经分析计算得降解效率为83.1％。
由降解效率可得最好得比例为1.5％1T/2H MS/BWO。
BWO，1.5％1T/2H MS/BWO的BET数据见表1。
表1
Claims (3)
1.一种1T/2H MS/BWO复合催化剂在压电光降解罗丹明B中的应用，其特征在于：所述1T/2H MS/BWO复合催化剂制备方法为：先制备Bi2WO6，再制备1T/2H MoSe2，将1T/2H MoSe2和Bi2WO6溶于无水乙醇中，进行超声、搅拌，混合均匀，室温下过滤、洗涤、干燥、研磨，得1T/2H MoSe2/Bi2WO6复合催化剂；加入的Bi2WO6质量是1T/2H MoSe2质量的0.5%~5%；
取催化剂加入罗丹明B中，在暗态条件下搅拌达到吸附-脱附平衡，同时在太阳光照射和超声波振动下降解。
2.根据权利要求1所述1T/2HMS/BWO复合催化剂在压电光降解罗丹明B中的应用，其特征在于，所述Bi2WO6的制备方法为：Bi(NO)3 5H2O作为铋源；Na2WO4 2H2O作为钨源，将铋源和钨源加入去离子水中，室温搅拌溶解得混合液，将混合液转移到内衬聚四氟乙烯的反应釜中，在烘箱中进行水热反应；待冷却至室温后过滤、洗涤、干燥、研磨，最终得到白色粉末；其中Bi(NO)3 5H2O和Na2WO4 . 2H2O的质量比为2 .9：1，水热反应温度为190℃，反应时间为2h，并且所得的Bi2WO6为纳米花球状催化剂。
3.根据权利要求1所述1T/2HMS/BWO复合催化剂在压电光降解罗丹明B中的应用，其特征在于，加入的Bi2WO6质量是1T/2H MoSe2质量的1.5%。
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