CN112058316A - 一种BiOBr/UMOFNs Z型光催化剂及其制备方法和应用 - Google Patents
一种BiOBr/UMOFNs Z型光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于光催化降解技术领域,公开了一种BiOBr/UMOFNs Z型光催化剂的制备方法,其主要通过调节BiOBr和UMOFNs的质量比调控复合材料对太阳光的光吸收能力和光稳定性,得到目标的BiOBr/UMOFNs Z型光催化材料,通过简单沉积沉淀法制备得到的BiOBr/UMOFNs Z型光催化材料的光吸收能力和光稳定性得到了有效增强,且该Z性光催化材料有效的提高了光生载流子的迁移率,对苯酚有良好的降解效果,可以用于光催化降解废水中的有毒有害污染物。
Description
技术领域
本发明涉及光催化剂领域,更具体的,涉及一种BiOBr/UMOFNs Z型光催化剂及其制备方法和应用。
背景技术
能源短缺和环境污染是当今社会面临的两大可持续发展过程中的两大难题。光催化技术是一种基于太阳能为驱动的,成本较低、安全环保的技术,能够有效的去除环境中的有毒有害污染物,还能将其直接转化为有工业价值的产物。
在近年来,因具有带隙可调节性、光化学稳定性和层状结构等特点,BiOX(X=Cl,Br,I)在光降解废水污染物上受到了极大的关注。在BiOX中,溴氧化铋BiOBr具有可见光响应,合适的价带位置和导带位置,因此受到了科学家们的广泛研究。然而,单纯的溴氧化铋光生电子-空穴对的转移和分离效率低,容易产生光生电子-空穴对的快速复合,严重地影响了其光催化活性及在实际工业生产中的应用。最近,通过构建Z型光催化剂以达到材料内部光生电荷的快速转移证明是一种有效提高BiOBr的光催化活性的方法。
金属有机框架化合物(MOF)是由金属离子和有机配体组成的,由于其具有比表面积大、孔隙率高、官能团可调等结构特征,近年来受到了科学家的广泛研究。作为具有纳米级厚度的二维材料的超薄金属有机框架纳米片[Ultrathin Metal-organic Frameworksnanosheets(UMOFNs)]可以加速电荷转移和电子空穴对分离,暴露出更多的不饱和金属活性位点,符合光催化剂的要求。而且UMOFNs具有较大的比表面积,很容易与其他半导体形成异质结以提高光催化活性。
发明内容
针对上述现有技术中存在的缺陷,本发明首先提供了一种BiOBr/UMOFNs Z型光催化剂的制备方法。
本发明的第二个目的是提供上述方法得到的BiOBr/UMOFNs Z型光催化剂。
本发明的第三个目的是提供上述BiOBr/UMOFNs Z型光催化剂的应用。
本发明的目的通过以下技术方案实现:
一种BiOBr/UMOFNs Z型光催化剂的制备方法,包括以下步骤:
S1、对苯二甲酸加入到DMF、无水乙醇和去离子水混合溶液中,得到溶液A;
S2、硝酸钴和硝酸镍加入到溶液A后,加入三乙胺,得到溶液B;
S3、溶液B超声后,离心洗涤,得到钴镍超薄有机金属框架化合物UMOFNs;
S4、硝酸铋、溴化钾和UMOFNs混合于水中搅拌,即得到BiOBr/UMOFNs Z型光催化剂。
本发明采用简单的沉积沉淀法制备得到光催化材料,通过构建Z型异质结结构,提高了材料对太阳光的光吸收能力和光稳定性。同时在Z型光催化材料的内部,通过Co3+/2+氧化还原对分别对光生电子和光生空穴的消耗,促进了光生电子空穴对的分离和转移。
本发明主要是通过调节BiOBr和UMOFNs的质量比来调节复合材料的光吸收能力和光稳定性,得到目标的BiOBr/UMOFNs Z型光催化材料。
因此,优选的,上述制备方法中,S4中硝酸铋和溴化钾的摩尔比为1:1,溴氧化铋和UMOFNs的质量比为1:(0.2~0.5)。
优选的,S4中溴氧化铋和UMOFNs的质量比为1:0.4。
优选的,所述苯二甲酸、硝酸钴、硝酸镍的摩尔比为5:2:2。
优选的,所述DMF、无水乙醇、无离子水和三乙胺的体积比为16:1:1:0.4;所述对苯二甲酸和溶液A的用量比为1M:48mL。
优选的,S4中搅拌时间为3~8h。
本发明还提供上述方法得到的BiOBr/UMOFNs Z型光催化剂。
本发明还提供上述BiOBr/UMOFNs Z型光催化剂在光催化降解污染物中的应用。具体的,制备得到的BiOBr/UMOFNs Z型光催化材料的光吸收能力和光稳定性得到了有效的增强,对光生电子空穴对的分离和迁移率有效的提高,对苯酚具有良好的降解效果。
与现有技术相比,本发明具有以下有益效果:
本发明公开了一种BiOBr/UMOFNs Z型光催化剂的制备方法,其主要通过调节BiOBr和UMOFNs的质量比调控复合材料对太阳光的光吸收能力和光稳定性,得到目标的BiOBr/UMOFNs Z型光催化材料,通过简单沉积沉淀法制备得到的BiOBr/UMOFNs Z型光催化材料的光吸收能力和光稳定性得到了有效增强,且该Z性光催化材料有效的提高了光生载流子的迁移率,对苯酚有良好的降解效果,可以用于光催化降解废水中的有毒有害污染物。
附图说明
图1为各光催化剂对苯酚降解性能图;
图2为BiOBr/UMOFNs Z型光催化材料的降解循环测试;
图3为BiOBr/UMOFNs Z型光催化材料的扫描电镜图。
具体实施方式
为了对本发明的技术特征、目的和效果有更加清楚的理解,现对照附图详细说明本发明的具体实施方式。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
取0.75mmol的对苯二甲酸于混合均匀的32ml DMF,2ml无水乙醇和2ml去离子水的溶液中,超声10分钟,使其分散均匀,得到溶液A;称取0.3mmol的硝酸钴和0.3mmol的硝酸镍溶于溶液A后,将0.8ml三乙胺迅速加入到上述溶液,并搅拌5分钟,得到溶液B;将溶液B置于超声仪中,超声8小时,离心洗涤,在60℃的条件下干燥12小时,得到UMOFNs。
称取1.64mmol硝酸铋,1.64mmol溴化钾和0.20g上述UMOFNs分散于30ml去离子水中,剧烈搅拌5小时,后将溶液离心洗涤,在60℃的条件下干燥12小时,得到BiOBr/UMOFNs-20%。
实施例2
取0.75mmol的对苯二甲酸于混合均匀的32ml DMF,2ml无水乙醇和2ml去离子水的溶液中,超声10分钟,使其分散均匀,得到溶液A;称取0.3mmol的硝酸钴和0.3mmol的硝酸镍溶于溶液A后,将0.8ml三乙胺迅速加入到上述溶液,并搅拌5分钟,得到溶液B;将溶液B置于超声仪中,超声8小时,离心洗涤,在60℃的条件下干燥12小时,得到UMOFNs。
称取1.64mmol硝酸铋,1.64mmol溴化钾和0.30g上述UMOFNs分散于30ml去离子水中,剧烈搅拌3小时,后将溶液离心洗涤,在60℃的条件下干燥12小时,得到BiOBr/UMOFNs-30%。
实施例3
取0.75mmol的对苯二甲酸于混合均匀的32ml DMF,2ml无水乙醇和2ml去离子水的溶液中,超声10分钟,使其分散均匀,得到溶液A;称取0.3mmol的硝酸钴和0.3mmol的硝酸镍溶于溶液A后,将0.8ml三乙胺迅速加入到上述溶液,并搅拌5分钟,得到溶液B;将溶液B置于超声仪中,超声8小时,离心洗涤,在60℃的条件下干燥12小时,得到UMOFNs。
称取1.64mmol硝酸铋,1.64mmol溴化钾和0.40g上述UMOFNs分散于30ml去离子水中,剧烈搅拌8小时,后将溶液离心洗涤,在60℃的条件下干燥12小时,得到BiOBr/UMOFNs-40%。
实施例4
取0.75mmol的对苯二甲酸于混合均匀的32ml DMF,2ml无水乙醇和2ml去离子水的溶液中,超声10分钟,使其分散均匀,得到溶液A;称取0.3mmol的硝酸钴和0.3mmol的硝酸镍溶于溶液A后,将0.8ml三乙胺迅速加入到上述溶液,并搅拌5分钟,得到溶液B;将溶液B置于超声仪中,超声8小时,离心洗涤,在60℃的条件下干燥12小时,得到UMOFNs。
称取1.64mmol硝酸铋,1.64mmol溴化钾和0.50g上述UMOFNs分散于30ml去离子水中,剧烈搅拌5小时,后将溶液离心洗涤,在60℃的条件下干燥12小时,得到BiOBr/UMOFNs-50%。
对比例1
称取1.64mmol硝酸铋和1.64mmol溴化钾分散于30ml去离子水中,剧烈搅拌5小时,后将溶液离心洗涤,在60℃的条件下干燥12小时,得到BiOBr。
实验例
取上述实施例和对比例已制备的光催化剂分别进行光催化效果实验,具体实验过程为:称取100mg光催化剂加入到150mL浓度为10mg/L的苯酚溶液中,在黑暗处搅拌30min使其达到吸附平衡,随后使用300W氙灯提供可见光照射进行光催化反应,每半小时取5ml溶液,离心过滤催化剂,利用紫外可见分光光度计测量滤液中苯酚的吸光度。结果如图一所示,由实施例所制备的BiOBr/UMOFNs Z型光催化剂的光催化降解性能是要优于对比例,其中BiOBr/UMOFNs-40%的光催化性能最优,在反应270min能达到99%的苯酚去除率,而BiOBr只有31%的降解率,UMOFNs几乎没有光催化降解性能。
如图2所示,BiOBr/UMOFNs-40%在5次连续的光催化降解实验中,仍保持良好的光催化降解活性(97%),说明BiOBr/UMOFNs Z型光催化剂具有良好的光稳定性。
上面结合附图对本发明的实施例进行了描述,但是本发明并不局限于上述的具体实施方式,上述的具体实施方式仅仅是示意性的,而不是限制性的,本领域的普通技术人员在本发明的启示下,在不脱离本发明宗旨和权利要求所保护的范围情况下,还可做出很多形式,这些均属于本发明的保护范围之内。
Claims (8)
1.一种BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,包括以下步骤:
S1、对苯二甲酸加入到DMF、无水乙醇和去离子水混合溶液中,得到溶液A;
S2、硝酸钴和硝酸镍加入到溶液A后,加入三乙胺,得到溶液B;
S3、溶液B超声后,离心洗涤,得到钴镍超薄有机金属框架化合物UMOFNs;
S4、硝酸铋、溴化钾和UMOFNs混合于水中搅拌,即得到BiOBr/UMOFNs Z型光催化剂。
2.根据权利要求1所述的BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,S4中硝酸铋和溴化钾的摩尔比为1:1,溴氧化铋和UMOFNs的质量比为1:(0.2~0.5)。
3.根据权利要求2所述的BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,S4中溴氧化铋和UMOFNs的质量比为1:0.4。
4.根据权利要求1所述的BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,所述对苯二甲酸、硝酸钴、硝酸镍的摩尔比为5:2:2。
5.根据权利要求1所述的BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,所述DMF、无水乙醇、无离子水和三乙胺的体积比为16:1:1:0.4;所述对苯二甲酸和溶液A的用量比为1M:48mL。
6.根据权利要求1所述的BiOBr/UMOFNs Z型光催化剂的制备方法,其特征在于,S4中搅拌时间为3~8h。
7.权利要求1至6任意一项所述方法制备得到的BiOBr/UMOFNs Z型光催化剂。
8.权利要求7所述BiOBr/UMOFNs Z型光催化剂在光催化降解污染物中的应用。
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