CN113751030A - 一种CoWO4/BiOBr复合声催化剂及其制备方法和应用 - Google Patents
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Abstract
本发明属于化学催化剂技术领域，具体公开了一种CoWO4/BiOBr复合声催化剂及其制备方法和应用。分别称取KBr和Bi(NO3)3·5H2O，前者加入乙二醇溶解，后者加入去离子水溶解，将溶解后的液体混合，在剧烈搅拌下将CoWO4加入到上述溶液中，搅拌，抽滤，用蒸馏水清洗数次，干燥，研磨成粉末，即得CoWO4/BiOBr复合物。通过与BiOBr复合实现CoWO4的改性。BiOBr将卤素原子Br夹在Bi2O2层间形成内部电场，使电荷迅速迁移从而使电子和空穴分离。本发明条件温和，化学性能稳定，是一种新型声催化剂。
Description
技术领域
本发明属于化学催化剂技术领域，特指一种CoWO4/BiOBr复合声催化剂及其制备方法和应用。
背景技术
钨酸钴(CoWO4)是一种p型半导体，在室温下表现为顺磁行为。CoWO4的禁带能约为2.24eV，因此常被用作声催化剂。为了提高CoWO4的活性，利用多种金属盐纳米粒子与CoWO4偶联形成异质结构，如CoWO4/Bi2WO6，CoWO4/Ag2O，CoWO4/Cu2O等。
受这些研究的启发，我们采用沉淀法制备了CoWO4/BiOBr异质结构纳米复合声催化剂，并研究了其对溶液中四环素的声催化活性。通过将CoWO4纳米颗粒的窄带隙与BiOBr的宽带隙相结合，构建CoWO4/BiOBr异质结构是一种利用超声波和诱导电子空穴对分离的有前途的方法，可以提高声催化活性。预期制备的CoWO4/BiOBr异质结构声催化剂与母体化合物相比，对声的响应性更好，比表面积更大，电荷分离效率和声催化活性更高。
发明内容
本发明的第一目的是提供一种CoWO4/BiOBr复合声催化剂；
本发明的第二目的是提供该声催化材料的制备方法。
本发明采用的技术方案为：一种CoWO4/BiOBr复合声催化剂，制备方法包括如下步骤：
分别取KBr和Bi(NO3)3·5H2O，前者加入乙二醇溶解，后者加入去离子水溶解，将溶解后的液体混合，在剧烈搅拌下将CoWO4加入到上述溶液中，搅拌，抽滤，用蒸馏水清洗数次，干燥，研磨成粉末，即得CoWO4/BiOBr复合物。
优选地，上述的一种CoWO4/BiOBr复合声催化剂，按摩尔比，Bi(NO3)3·5H2O：KBr：CoWO4为1-12:4:4。
优选地，上述的一种CoWO4/BiOBr复合声催化剂，搅拌时间为30min。
优选地，上述的一种CoWO4/BiOBr复合声催化剂，干燥温度为60-80℃，干燥时间为2h。
优选地，上述的CoWO4/BiOBr复合声催化剂在降解有机污染物中的应用。
优选地，上述的应用，方法如下：向含有有机污染物的溶液中加入CoWO4/BiOBr复合声催化剂，超声催化。
优选地，上述的应用，CoWO4/BiOBr复合声催化剂的加入量为1g/L。
优选地，上述的应用，所述有机污染物的浓度为20mg/L。
优选地，上述的应用，所述有机污染物是四环素。
本发明的有益效果是：
本发明通过与BiOBr复合实现CoWO4的改性。BiOBr将卤素原子Br夹在Bi2O2层间形成内部电场，使电荷迅速迁移从而使电子和空穴分离。本发明条件温和，化学性能稳定，是一种新型声催化剂。制备的声催化材料具有高效电荷分离和优异的氧化还原能力。能够促进载流子的迁移，从而提高声催化能力。本工作为开发其他基于CoWO4的声催化系统提供了一种有效的途径，可用于环境净化和能量转换。BiOBr将卤素原子Br夹在Bi2O2层间形成内部电场，使电荷迅速迁移从而使电子和空穴分离。本发明条件温和，化学性能稳定，是一种新型声催化剂。
附图说明
图1为CoWO4和本发明CoWO4/BiOBr-50％复合声催化剂的XRD图。
图2为CoWO4和本发明CoWO4/BiOBr-50％复合声催化剂的XPS图谱。
图3为不同复合比对CoWO4/BiOBr复合声催化剂降解四环素溶液效果对比图。
具体实施方式
实施例1 CoWO4的制备
将1.4551g Co(NO3)2·6H2O和1.6493g Na2WO4·2H2O于30mL去离子水中溶解，混合物磁力搅拌30min；再超声反应30min后倒入高压反应釜中，将高压反应釜置于鼓风干燥箱中180℃加热24h；反应结束后将反应釜降至室温，抽滤，在80℃条件下干燥2h得到目标产物，记为CoWO4。
实施例2 CoWO4/BiOBr复合声催化剂
分别称取0.16245g KBr和0.1576g Bi(NO3)3·5H2O，置于两个100ml烧杯中，前者加入20ml乙二醇溶解，后者加入100ml去离子水溶解。将溶解后的液体混合，在剧烈搅拌下将0.4g CoWO4加入到上述溶液中，并将其置于磁力搅拌器上反应30min。抽滤，用蒸馏水清洗3次，最后得到的固体于预热至80℃的烘箱中干燥2h。置于玛瑙研钵中研磨成粉末，即得CoWO4/BiOBr复合物，记为CoWO4/BiOBr-25％。(BiOBr：CoWO4为1:4)
实施例3 CoWO4/BiOBr复合声催化剂
分别称取0.3249g KBr和0.3152g Bi(NO3)3·5H2O，置于两个100ml烧杯中，前者加入20ml乙二醇溶解，后者加入100ml去离子水溶解。将溶解后的液体混合，在剧烈搅拌下将0.4g CoWO4加入到上述溶液中，并将其置于磁力搅拌器上反应30min。抽滤，用蒸馏水清洗3次，最后得到的固体于预热至80℃的烘箱中干燥2h。置于玛瑙研钵中研磨成粉末，即得CoWO4/BiOBr复合物，记为CoWO4/BiOBr-50％。(BiOBr：CoWO4为1:2)
实施例4 CoWO4/BiOBr复合声催化剂
分别称取0.6498g KBr和0.6304g Bi(NO3)3·5H2O，置于两个100ml烧杯中，前者加入20ml乙二醇溶解，后者加入100ml去离子水溶解。将溶解后的液体混合，在剧烈搅拌下将0.4g CoWO4加入到上述溶液中，并将其置于磁力搅拌器上反应30min。抽滤，用蒸馏水清洗3次，最后得到的固体于预热至80℃的烘箱中干燥2h。置于玛瑙研钵中研磨成粉末，即得CoWO4/BiOBr复合物，记为CoWO4/BiOBr-100％。(BiOBr：CoWO4为1:1)
实施例5 CoWO4/BiOBr复合声催化剂
分别称取1.9494g KBr和1.8912g Bi(NO3)3·5H2O，置于两个100ml烧杯中，前者加入20ml乙二醇溶解，后者加入100ml去离子水溶解。将溶解后的液体混合，在剧烈搅拌下将0.4g CoWO4加入到上述溶液中，并将其置于磁力搅拌器上反应30min。抽滤，用蒸馏水清洗3次，最后得到的固体于预热至80℃的烘箱中干燥2h。置于玛瑙研钵中研磨成粉末，即得CoWO4/BiOBr复合物，记为CoWO4/BiOBr-300％。(BiOBr：CoWO4为3:1)
实施例6 BiOBr声催化剂
分别称取1.9494g KBr和1.8912g Bi(NO3)3·5H2O，置于两个100ml烧杯中，前者加入20ml乙二醇溶解，后者加入100ml去离子水溶解。将溶解后的液体混合，并将其置于磁力搅拌器上反应30min。抽滤，用蒸馏水清洗3次，最后得到的固体于预热至80℃的烘箱中干燥2h。置于玛瑙研钵中研磨成粉末，记为BiOBr。
实施例6 CoWO4/BiOBr复合声催化剂的表征分析
图1为合成的CoWO4纳米颗粒和CoWO4/BiOBr纳米复合材料的XRD谱图。CoWO4纳米颗粒在15.60°，19.17°，23.82°，24.71°，30.77°，36.48°，38.63°，41.30°，44.36°，45.96°，48.87°，50.62°，52.10°，61.84°和65.19°处分别有衍射峰，对应于(010)，(001)，(-110)，(011)，(-111)，(120)，(002)，(-201)，(-211)，(-112)，(-220)，(022)，(031)，(-311)和(-231)面的反射(JCPDS No.72-0479)。CoWO4/BiOBr复合材料的XRD谱图显示了BiOBr和CoWO4相的衍射峰。在2θ＝19.17°，23.82°，30.77°，36.48°和41.32°处的峰对应于四方BiOBr中的单斜CoWO4纳米颗粒(JCPDS No.09-0393)，表明CoWO4/BiOBr纳米复合材料的形成。
图2为合成的CoWO4和CoWO4/BiOBr样品的XPS谱图。XPS光谱表明CoWO4/BiOBr中存在Bi、Br、O、Co和W元素。以上XPS研究结果证实了该复合材料由BiOBr和CoWO4纳米颗粒组成。
实施例7 CoWO4/BiOBr复合声催化剂对催化超声降解四环素溶液效果影响
通过使用超声降解四环素溶液，并测定其最大吸收波长，通过计算吸光度评价CoWO4/BiOBr复合材料的声催化活性。在声催化过程中，120min后取反应悬浮液样品10mL,18000rpm离心20min，去除悬浮颗粒。上清液在360nm处的四环素特征吸收峰上进行分析.
降解率计算如下:
降解率(％)＝[(A0-At)/A0]×100％
其中A0为四环素的初始吸光度，At为四环素在t时刻的吸光度。
此外，CoWO4、CoWO4/BiOBr-25％、CoWO4/BiOBr-50％、CoWO4/BiOBr-100％、CoWO4/BiOBr-300％和BiOBr催化剂对水溶液中四环素的降解率分别为27.89％、50.50％、62.64％、54.81％和39.32％。均具有良好的声催化活性。虽然不同复合比的声催化剂催化活性不同，说明BiOBr的诱导电荷转移性能对其声催化活性也有很大影响。当BiOBr含量为50％时，复合材料的声催化活性最高。
Claims (9)
1.一种CoWO4/BiOBr复合声催化剂，其特征在于，制备方法包括如下步骤：
分别取KBr和Bi(NO3)3·5H2O，前者加入乙二醇溶解，后者加入去离子水溶解，将溶解后的液体混合，在剧烈搅拌下将CoWO4加入到上述溶液中，搅拌，抽滤，用蒸馏水清洗数次，干燥，研磨成粉末，即得CoWO4/BiOBr复合物。
2.根据权利要求1所述的一种CoWO4/BiOBr复合声催化剂，其特征在于，按摩尔比，Bi(NO3)3·5H2O：KBr：CoWO4为1-12:4:4。
3.根据权利要求2所述的一种CoWO4/BiOBr复合声催化剂，其特征在于，搅拌时间为30min。
4.根据权利要求3所述的一种CoWO4/BiOBr复合声催化剂，其特征在于，干燥温度为60-80℃，干燥时间为2h。
5.权利要求1-4任意一项所述的CoWO4/BiOBr复合声催化剂在降解有机污染物中的应用。
6.根据权利要求5所述的应用，其特征在于，方法如下：向含有有机污染物的溶液中加入CoWO4/BiOBr复合声催化剂，超声催化。
7.根据权利要求6所述的应用，其特征在于，CoWO4/BiOBr复合声催化剂的加入量为1g/L。
8.根据权利要求7所述的应用，其特征在于，所述有机污染物的浓度为20mg/L。
9.根据权利要求8所述的应用，其特征在于，所述有机污染物是四环素。
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