CN109395761A - 一种氮掺杂BiOIO3光催化剂的制备方法及其应用 - Google Patents
一种氮掺杂BiOIO3光催化剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明属于纳米材料制备和应用技术领域,涉及光催化剂,具体涉及一种氮掺杂BiOIO3光催化剂的制备方法,包括:配制等摩尔的五水合硝酸铋和碘酸钾混合溶液,转入水热反应釜中120~160℃反应4~16h,自然冷却后过滤、水洗、烘干,研磨得BiOIO3纳米粒;将BiOIO3纳米粒与尿素混合研磨,置于马弗炉中180~260℃煅烧2~6h,自然冷却后,研磨得氮掺杂BiOIO3光催化剂。本发明还公开了将其应用于光催化降解废水中的有机污染物。本发明制备方法简单易行,安全环保,产物成本低,易于工业化生产,有很高的应用前景和实用价值。制得的氮掺杂BiOIO3光催化剂,有效提高了材料可见光吸收性能,提高材料的光电流强度,增强材料光生电子、空穴的反应活性,具有显著的光催化降解有机污染物效果。
Description
技术领域
本发明属于纳米材料制备和应用技术领域,涉及光催化剂,具体涉及一种氮掺杂BiOIO3光催化剂的制备方法及其应用。
背景技术
随着化学合成工业的迅速发展,大量有机化工物质,如染料、农药、日常护理品、抗生素等被大量使用和排放,造成严重的水污染,对人类的健康构成了巨大威胁。水体中有机污染物的治理技术通常包括生物净化法、化学氧化法、物理吸附法等,这些技术在当今水环境修复中起到了重要作用。不过生物净化法应用范围有限,对于一些低含量、难降解的有机污染物效果较差;化学氧化法容易产生二次污染;物理吸附法会形成大量固体废弃物,且成本高。环境光催化技术依据半导体材料在光激发下能活化分子氧和水分子产生强氧化能力的自由基,进而可把有机分子矿化的原理,被认为是一种低成本、环境友好的高级氧化技术和高效消除各种低含量有机污染物的绿色途径。其中BiOIO3是一种铋基层状化合物,具有内建电场,可以促进光生电子和空穴的分离,具有良好的化学稳定性和热稳定性而成为一种新型的光催化剂。不过BiOIO3的禁带宽度较大,对可见光响应性差,不能很好利用太阳光,其可见光催化活性较低。
通过掺杂改性是增强半导体材料可见光催化活性的有效途径,因为掺杂可在半导体带隙中产生新的能级,一方面可提高可见光响应性能,另一方面可提高光生电子和空穴的分离效率。如何通过简单易行的方法制备可见光响应性强、稳定性好的掺杂BiOIO3光催化材料,是将BiOIO3应用于环境光催化领域亟待解决的问题。
发明内容
针对上述现有技术中存在的不足,本发明的目的是在于提供一种氮掺杂BiOIO3光催化剂的制备方法。
为实现上述目的,本发明通过以下技术方案实现:
一种氮掺杂BiOIO3光催化剂的制备方法,包括如下步骤:
A、 将等摩尔的五水合硝酸铋和碘酸钾溶于蒸馏水中,得混合溶液;
B、 将混合溶液转入水热反应釜中120~160℃反应4~16h,优选130~140℃反应8~10h,自然冷却后过滤,水洗,60~90℃烘干,研磨得BiOIO3纳米粒;
C、将BiOIO3纳米粒与尿素混合研磨,置于马弗炉中180~260℃煅烧2~6h,优选200~240℃反应3~4h,自然冷却后,研磨得氮掺杂BiOIO3光催化剂。
本发明较优公开例中,步骤C所述尿素与BiOIO3的质量比为1:2~1:10,优选质量比为1:4~1:6。
根据本发明所述方法制得的氮掺杂BiOIO3光催化剂,由氮元素掺杂BiOIO3构成,形貌呈不规则颗粒状。
本发明还有一个目的,将所制得的氮掺杂BiOIO3光催化剂应用于光催化降解废水中的有机污染物。
进一步的,所述有机污染物为苯酚、罗丹明B或环丙沙星中的一种或多种。
氮掺杂BiOIO3光催化剂降解苯酚的性能评价:
配制浓度为10mg/L的苯酚溶液100mL,加入0.100g实施例1所制备的氮掺杂BiOIO3,避光磁力搅拌60min至体系吸附平衡,以30W的LED灯为光源,用紫外-可见分光光度计在270nm波长处测定苯酚溶液的吸光度,进行光降解实验,以C/C0~时间作图,表征材料的光催化活性,其中C0、C分别为光催化降解前后苯酚的浓度。同样条件下进行BiOIO3的光降解实验,结果如图4所示,可见氮掺杂BiOIO3具有比BiOIO3更好的光催化降解苯酚的活性。
氮掺杂BiOIO3光催化剂降解罗丹明B的性能评价:
配制浓度为10mg/L的罗丹明B溶液100mL,加入0.100g实施例2所制备的氮掺杂BiOIO3,避光磁力搅拌60min至体系吸附平衡,以30W的LED灯为光源,用紫外-可见分光光度计在553nm波长处测定罗丹明B溶液的吸光度,进行光降解实验,以C/C0~时间作图,表征材料的光催化活性,其中C0、C分别为光催化降解前后罗丹明B的浓度。同样条件下进行BiOIO3的光降解实验,结果如图5所示,可见氮掺杂BiOIO3具有比BiOIO3更好的光催化降解罗丹明B的活性。
氮掺杂BiOIO3光催化剂降解环丙沙星的性能评价:
配制浓度为10mg/L的环丙沙星溶液100mL,加入0.100g实施例3所制备的氮掺杂的BiOIO3,避光磁力搅拌60min至体系吸附平衡,以30W的LED灯为光源,用紫外-可见分光光度计在276nm波长处测定环丙沙星溶液的吸光度,进行光降解实验,以C/C0~时间作图,表征材料的光催化活性,其中C0、C分别为光催化降解前后环丙沙星的浓度。同样条件下进行BiOIO3的光降解实验,结果如图6所示,可见氮掺杂BiOIO3具有比BiOIO3更好的光催化降解环丙沙星的活性。
氮掺杂BiOIO3光催化剂的光电流响应性能评价:
采用CHI760D型电化学工作站测定样品光电流,采用三电极体系,以氧化铟锡(ITO)玻碳电极修饰样品后作为工作电极,甘汞电极为参比电极,铂丝为辅助电极,电解液Na2SO4溶液浓度为0.1mol/L。可见光光源为30W LED灯。同样条件下进行BiOIO3的光电流响应性能测试。实施例4中的BiOIO3和氮掺杂BiOIO3的光电流响应性能如图7所示,可见氮掺杂BiOIO3在光照时具有比BiOIO3更强的光电流。
氮掺杂BiOIO3光催化剂在50min降解罗丹明B达98%,120min降解环丙沙星达90%,100min可降解苯酚达91%,明显高于BiOIO3的光催化性能,可用于光催化降解有机污染物领域。
有益效果
本发明所公开的氮掺杂BiOIO3光催化剂的制备方法简单易行,安全环保,产物成本低,易于工业化生产,具有很高的应用前景和实用价值。所制得的氮掺杂BiOIO3光催化剂,有效提高了材料可见光吸收性能,提高材料的光电流强度,增强材料光生电子、空穴的反应活性。与现有的光催化材料相比,具有显著的光催化降解有机污染物效果。
附图说明
图1. 对照品BiOIO3和本发明的氮掺杂BiOIO3的X射线衍射图;
图2. 本发明的氮掺杂BiOIO3的扫描电镜图;
图3. 对照品BiOIO3和本发明的氮掺杂BiOIO3的紫外-可见吸收光谱图;
图4. 对照品BiOIO3和本发明的氮掺杂BiOIO3在可见光下催化降解苯酚的性能图;
图5. 对照品BiOIO3和本发明的氮掺杂BiOIO3在可见光下催化降解罗丹明B的性能图;
图6. 对照品BiOIO3和本发明的氮掺杂BiOIO3在可见光下催化降解环丙沙星的性能图;
图7. 对照品BiOIO3和本发明的氮掺杂BiOIO3在可见光下光电流响应性能图。
具体实施方式
下面结合实施例对本发明进行详细说明,以使本领域技术人员更好地理解本发明,但本发明并不局限于以下实施例。
除非另外限定,这里所使用的术语(包含科技术语)应当解释为具有如本发明所属技术领域的技术人员所共同理解到的相同意义。还将理解到,这里所使用的术语应当解释为具有与它们在本说明书和相关技术的内容中的意义相一致的意义,并且不应当以理想化或过度的形式解释,除非这里特意地如此限定。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1
一种氮掺杂BiOIO3光催化剂的制备方法,包括如下步骤:
BiOIO3的制备:称取0.485g五水合硝酸铋和0.214g碘酸钾溶于70 mL蒸馏水中,得溶液A;将溶液A转移至100 mL水热反应釜中,于120℃反应16h,自然冷却至室温后过滤,所得固体粉末用蒸馏水洗涤,60℃烘干,研磨得BiOIO3光催化剂粉末。
氮掺杂BiOIO3的制备:称取0.1g尿素和0.2g BiOIO3,置于研钵中研磨混合均匀,转移至坩埚中,然后置于马弗炉中于180℃煅烧6h,产物自然冷却至室温,研磨得氮掺杂BiOIO3。
所得BiOIO3和氮掺杂BiOIO3的X射线衍射图见图1所示。可见氮掺杂BiOIO3与BiOIO3的衍射峰一致,说明氮掺杂没有改变BiOIO3的晶相。
实施例 2
一种氮掺杂BiOIO3光催化剂的制备方法,包括如下步骤:
BiOIO3的制备:称取0.485g五水合硝酸铋和0.214g碘酸钾溶于70 mL蒸馏水中,得溶液A;将溶液A转移至100 mL水热反应釜中,于160℃反应4h,自然冷却至室温后过滤,所得固体粉末用蒸馏水洗涤,90℃烘干,研磨得BiOIO3光催化剂粉末。
氮掺杂BiOIO3的制备:称取0.02g尿素和0.2g BiOIO3,置于研钵中研磨混合均匀,转移至坩埚中,然后置于马弗炉中于260℃煅烧2h,产物自然冷却至室温,研磨得氮掺杂BiOIO3。
所得氮掺杂BiOIO3的扫描电镜图见图2所示,可见氮掺杂BiOIO3的形貌呈不规则颗粒状。
实施例 3
一种氮掺杂BiOIO3光催化剂的制备方法,包括如下步骤:
BiOIO3的制备:称取0.485g五水合硝酸铋和0.214g碘酸钾溶于70 mL蒸馏水中,得溶液A;将溶液A转移至100 mL水热反应釜中,于140℃反应10h,自然冷却至室温后过滤,所得固体粉末用蒸馏水洗涤,80℃烘干,研磨得BiOIO3光催化剂粉末。
氮掺杂BiOIO3的制备:称取0.05g尿素和0.2g BiOIO3,置于研钵中研磨混合均匀,转移至坩埚中,然后置于马弗炉中于230℃煅烧3h,产物自然冷却至室温,研磨得氮掺杂BiOIO3。
本实施例所得BiOIO3和氮掺杂BiOIO3的紫外-可见吸收光谱如图3所示。可见,BiOIO3的吸光波长<400nm,对可见光的利用率低,而氮掺杂BiOIO3的吸光波长拓宽到650nm左右,具有显著的可见光吸收性能。
实施例 4
一种氮掺杂BiOIO3光催化剂的制备方法,包括如下步骤:
BiOIO3的制备:称取0.485g五水合硝酸铋和0.214g碘酸钾溶于70 mL蒸馏水中,得溶液A;将溶液A转移至100 mL水热反应釜中,于150℃反应6h,自然冷却至室温后过滤,所得固体粉末用蒸馏水洗涤,70℃烘干,研磨得BiOIO3光催化剂粉末。
氮掺杂BiOIO3的制备:称取0.08g尿素和0.2g BiOIO3,置于研钵中研磨混合均匀,转移至坩埚中,然后置于马弗炉中于200℃煅烧4h,产物自然冷却至室温,研磨得氮掺杂BiOIO3。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (9)
1.一种氮掺杂BiOIO3光催化剂的制备方法,其特征在于,包括如下步骤:
A. 将等摩尔的五水合硝酸铋和碘酸钾溶于蒸馏水中,得混合溶液;
B. 将混合溶液转入水热反应釜中120~160℃反应4~16h,自然冷却后过滤,水洗,60~90℃烘干,研磨得BiOIO3纳米粒;
C. 将BiOIO3纳米粒与尿素混合研磨,置于马弗炉中180~260℃煅烧2~6h,自然冷却后,研磨得氮掺杂BiOIO3光催化剂。
2.根据权利要求1所述氮掺杂BiOIO3光催化剂的制备方法,其特征在于:步骤B所述将混合溶液转入水热反应釜中130~140℃反应8~10h。
3.根据权利要求1所述氮掺杂BiOIO3光催化剂的制备方法,其特征在于:步骤C所述将BiOIO3纳米粒与尿素混合研磨,置于马弗炉中200~240℃反应3~4h。
4.根据权利要求1所述氮掺杂BiOIO3光催化剂的制备方法,其特征在于:步骤C所述尿素与BiOIO3的质量比为1:2~1:10。
5.根据权利要求4所述氮掺杂BiOIO3光催化剂的制备方法,其特征在于:步骤C所述尿素与BiOIO3的质量比为1:4~1:6。
6.根据权利要求1-5任一所述方法制备的氮掺杂BiOIO3光催化剂。
7.根据权利要求6所述氮掺杂BiOIO3光催化剂,由氮元素掺杂BiOIO3构成,其特征在于:形貌呈不规则颗粒状。
8.一种如权利要求6或7所述氮掺杂BiOIO3光催化剂的应用,其特征在于:将氮掺杂BiOIO3光催化剂应用于光催化降解废水中的有机污染物。
9.根据权利要求8所述氮掺杂BiOIO3光催化剂的应用,其特征在于:所述有机污染物为苯酚、罗丹明B或环丙沙星中的一种或多种。
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