CN111468134A - 一种3D花状Bi2WO6@CoO异质结光催化剂及其制备方法和应用 - Google Patents
一种3D花状Bi2WO6@CoO异质结光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种3D花状Bi2WO6@CoO异质结光催化剂及其制备方法和应用。是将半导体CoO纳米粒子负载到Bi2WO6上制成,其中,按重量百分比,CoO纳米粒子为1~7%。本发明构建了一种新颖的3D花状分级的Bi2WO6@CoO(BWC)异质结光催化,该复合材料具有大的比表面积,超高的可见光吸收能力,增强的电子‑空穴对分离效率,相比于单独Bi2WO6和CoO,本发明异质结材料展示了增强的催化活性。
Description
技术领域
本发明属于光催化剂领域,特别涉及一种具有3D花状结构的Bi2WO6@CoO异质结光催化剂及其制备方法和在光催化氧化四环素及还原Cr(VI)中的应用。
背景技术
近年来,抗生素被广泛应用在医疗及畜牧业等领域,由于人或动物往往不能完全将其代谢吸收,导致了大量抗生素以其原态进入环境水体,造成水体的污染,它不仅会对水生生物造成危害,也会因食物链而威胁着人类的生存健康。
四环素类抗生素是一类广谱抗生素,应用最为广泛。然而,抗生素的滥用也造成了生物体的耐药性,且含抗生素的水体对水生生物及人体有一定的毒害作用,因此,探寻一种净化水中四环素类抗生素的高效方法是十分必要的。
重金属污染对人体健康和环境也造成了严重的威胁。铬,作为一种典型的重金属,是常见的重金属污染物。其中,Cr(VI)是一种致癌物、诱变物和致畸物,然而,Cr(III)毒性较低,是人体必需的微量元素。因此,将废水中的高毒性的Cr(VI)还原为低毒的Cr(III)是一种高效的含铬废水处理技术。
可见光驱动的半导体催化技术,是十分有前景的水处理技术,它利用占太阳光46%的可见光作为光源,具有高效、环保及可持续等优点,且因成本低、操作简单、氧化性强等特点,引起了人们的关注。但是,由于宽带隙半导体材料很难利用太阳光中的可见光部分,且单一半导体材料的光生载流子极容易复合等缺陷,限制了光催化技术的应用。因此,构建具有可见光响应且高电荷分离效率的半导体异质结催化剂是该技术的关键。
发明内容
为了解决上述技术问题,本发明设计并构建了3D花状Bi2WO6@CoO异质结光催化剂,并用于光催化氧化四环素及还原Cr(VI)。
本发明采用的技术方案是:一种3D花状Bi2WO6@CoO异质结光催化剂,是将半导体CoO纳米粒子负载到Bi2WO6上制成,其中,按重量百分比,CoO纳米粒子为1~7%。
一种3D花状Bi2WO6@CoO异质结光催化剂的制备方法,包括如下步骤:将Bi2WO6加入到含有Co(CH3COO)2·4H2O的甲醇溶液中,10~30℃下搅拌60~120min,所得混合物在30~80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400~450℃下煅烧1-2h,得3D花状Bi2WO6@CoO异质结光催化剂。
进一步的,上述的制备方法,所述Bi2WO6的制备方法,包括如下步骤:将Bi(NO3)3·5H2O溶解于醋酸水溶液中,于室温下搅拌30min,得溶液A;将Na2WO4·2H2O溶解于水中,得溶液B;将溶液A滴加到溶液B中,混合均匀后,转移至反应釜中,180℃下水热反应16h,所得产物经洗涤、干燥,得Bi2WO6。
进一步的,上述的制备方法,按摩尔比,Bi(NO3)3·5H2O:Na2WO4·2H2O=2:1。
本发明提供的3D花状Bi2WO6@CoO异质结光催化剂在光催化降解四环素中的应用。
进一步的,方法如下:在可见光照射下,于含有四环素的废水中加入3D花状Bi2WO6@CoO异质结光催化剂,进行光催化降解。
本发明提供的3D花状Bi2WO6@CoO异质结光催化剂在光催化还原Cr(VI)中的应用。
进一步的,方法如下:在可见光照射下,于含有Cr(VI)的废水中加入3D花状Bi2WO6@CoO异质结光催化剂,进行光催化还原。
本发明的有益效果是:
Bi2WO6是一种n型半导体,具有合适的带隙值、能带位置和良好的稳定性,本发明成功将p型半导体CoO纳米粒子负载到三维花状Bi2WO6上,形成稳定的p-n异质结,可以有效抑制光生电子-空穴对的复合,提高光催化效率。
本发明设计并构建的三维分级花状Bi2WO6@CoO异质结。由二维纳米片自组装的三维花状结构,不仅有利于目标物在其开放孔道内的快速传导,而且利于入射光在材料表面和内部的多次反射和散射,从而提高了对可见光的利用率。
在可见光辐射下,相比于单独Bi2WO6和CoO,构建的Bi2WO6@CoO异质结展示了增强的催化活性。并且,异质结不但可以高效地催化氧化四环素(TC),也能够催化还原Cr(VI),是一个高效的双功能催化剂。
附图说明
图1是实施例2制备的Bi2WO6、CoO和3%BWC的XRD图谱。
图2是实施例2制备的Bi2WO6(a)和3%BWC(b)的SEM图。
图3是不同催化剂对TC的催化氧化效果。
图4是不同催化剂对TC的催化动力学。
图5是3%BWC复合材料催化还原Cr(VI)的效果。
具体实施方式
实施例1
Bi2WO6@CoO异质结(1%BWC)的制备,包括如下步骤:
1、Bi2WO6的制备
将4mmol Bi(NO3)3·5H2O溶解在20mL醋酸水溶液(按体积比,醋酸:水=3:5)中,25℃下搅拌30min,得溶液A。
将2mmol Na2WO4·2H2O溶解在10mL水中,得溶液B。
将溶液A滴加入溶液B中,混合均匀后,将混合液转移至反应釜中,于180℃下水热反应16h,所得产物经洗涤、干燥,得Bi2WO6。
2、Bi2WO6@CoO异质结(1%BWC)的制备
将0.5g的Bi2WO6加入到40mL含有0.02g Co(CH3COO)2·4H2O的甲醇溶液中,25℃下搅拌120min,所得混合物在80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400℃煅烧1h,得按重量百分比,CoO负载量为1%的3D花状Bi2WO6@CoO异质结光催化剂,记为1%BWC。
实施例2
(一)Bi2WO6@CoO异质结(3%BWC)的制备,包括如下步骤:
1、Bi2WO6纳米片的制备:同实施例1。
2、Bi2WO6@CoO异质结(3%BWC)的制备
将0.5g的Bi2WO6加入到40mL含有0.05g Co(CH3COO)2·4H2O的甲醇溶液中,25℃下搅拌120min,所得混合物在80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400℃煅烧1h,得按重量百分比,CoO负载量为3%的3D花状Bi2WO6@CoO异质结光催化剂,记为3%BWC。
3、对比例——CoO的制备
将Co(CH3COO)2·4H2O在N2气氛下,直接于400℃煅烧1h,得CoO。
(二)检测
1、图1是Bi2WO6、CoO和3%BWC的XRD图谱。由图1可见,制得的纯Bi2WO6在28.31°,32.68°,47.15°,55.82°,58.54°,69.04°,76.07°和78.01°分别对应了Bi2WO6(JCPDS No:65-2902)的(131),(060),(202),(133),(262),(400),(333)和(451)晶面,证明了Bi2WO6的成功合成。纯的CoO在36.52°,42.42°,61.56°和73.61°峰分别对应了CoO(JCPDS No:65-2902)的(111),(200),(220)和(222)晶面。3%BWC仅观测到Bi2WO6的衍射峰,由于峰强度较低及复合中较低的含量,CoO没有被观测到。
2、图2是Bi2WO6(a)和3%BWC(b)的SEM图。由图2中a可见,Bi2WO6展现了3D分级的花状结构。由图2中b可见,负载了CoO之后的复合材料3%BWC,分级的花状结构没有改变,其表面能够看到CoO纳米粒子。
实施例3
(一)Bi2WO6@CoO异质结(5%BWC)的制备,包括如下步骤:
1、Bi2WO6纳米片的制备:同实施例1。
2、Bi2WO6@CoO异质结(5%BWC)的制备
将0.5g的Bi2WO6加入到40mL含有0.07g Co(CH3COO)2·4H2O的甲醇溶液中,25℃下搅拌120min,所得混合物在80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400℃煅烧1h,得按重量百分比,CoO负载量为5%的3D花状Bi2WO6@CoO异质结光催化剂,记为5%BWC。
实施例4
(一)Bi2WO6@CoO异质结(7%BWC)的制备,包括如下步骤:
1、Bi2WO6纳米片的制备:同实施例1。
2、Bi2WO6@CoO异质结(7%BWC)的制备
将0.5g的Bi2WO6加入到40mL含有0.1g Co(CH3COO)2·4H2O的甲醇溶液中,25℃下搅拌120min,所得混合物在80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400℃煅烧1h,得按重量百分比,CoO负载量为7%的3D花状Bi2WO6@CoO异质结光催化剂,记为7%BWC。
实施例5
以四环素为污染物代表评价催化剂的催化活性。
方法:于50mL初始浓度为10mg·L-1的四环素水溶液中,分别加入20mg催化剂Bi2WO6、CoO、1%BWC、3%BWC、5%BWC、7%BWC,先在闭光下吸附-解析平衡30min。光源采用300W氙灯(λ>420nm)。在可见光辐射过程中,采用紫外可见吸收光谱监测污染物的浓度。
图3是不同催化剂催化氧化四环素的效果,由图3可见,相比于单独的Bi2WO6和CoO,Bi2WO6@CoO展现了增强的催化活性。并且,随着CoO负载量从1%增加到3%,降解效果增加,进一步增加其负载量,催化效果反而降低。因此,本发明优选3%CoO负载量作为最佳的催化剂。
图4是不同催化剂催化氧化四环素的动力学常数。该催化过程符合一级动力学,由图4可见,各种催化剂中,CoO负载量为3%的3D花状Bi2WO6@CoO异质结光催化剂(3%BWC)展现了最大的速率常数,再一次证明了其超高的催化活性。
实施例6
以Cr(VI)为污染物代表评价催化剂的催化活性。
方法:于50mL Cr(VI)初始浓度为10mg·L-1的水溶液中,加入20mg催化剂3%BWC,先在闭光下吸附-解析平衡30min。光源采用300W氙灯(λ>420nm)。在可见光辐射过程中,采用紫外可见吸收光谱监测污染物的浓度。
图5是3%BWC复合材料催化还原Cr(VI)的效果,由图5可见,CoO负载量为3%的3D花状Bi2WO6@CoO异质结光催化剂(3%BWC)在可见光照下,具有催化还原性能,能够高效地还原有毒的Cr(VI)为无毒的Cr(III)。
Claims (9)
1.一种3D花状Bi2WO6@CoO异质结光催化剂,其特征在于,所述Bi2WO6@CoO异质结光催化剂是将半导体CoO纳米粒子负载到Bi2WO6上制成,其中,按重量百分比,CoO纳米粒子为1~7%。
2.一种3D花状Bi2WO6@CoO异质结光催化剂的制备方法,其特征在于,包括如下步骤:将Bi2WO6加入到含有Co(CH3COO)2·4H2O的甲醇溶液中,10~30℃下搅拌60~120min,所得混合物在30~80℃下蒸发甲醇后,将所得产物烘干,然后在N2气氛下,于400~450℃下煅烧1-2h,得3D花状Bi2WO6@CoO异质结光催化剂。
3.根据权利要求2所述的制备方法,其特征在于,所述Bi2WO6的制备方法,包括如下步骤:将Bi(NO3)3·5H2O溶解于醋酸水溶液中,于室温下搅拌30min,得溶液A;将Na2WO4·2H2O溶解于水中,得溶液B;将溶液A滴加到溶液B中,混合均匀后,转移至反应釜中,180℃下水热反应16h,所得产物经洗涤、干燥,得Bi2WO6。
4.根据权利要求3所述的制备方法,其特征在于,按摩尔比,Bi(NO3)3·5H2O:Na2WO4·2H2O=2:1。
5.权利要求1所述的3D花状Bi2WO6@CoO异质结光催化剂在光催化降解四环素类抗生素中的应用。
6.根据权利要求5所述的应用,其特征在于,方法如下:在可见光照射下,于含有四环素类抗生素的废水中加入权利要求1所述的3D花状Bi2WO6@CoO异质结光催化剂,进行光催化降解。
7.根据权利要求5或6所述的应用,其特征在于,所述四环素类抗生素为四环素。
8.权利要求1所述的3D花状Bi2WO6@CoO异质结光催化剂在光催化还原Cr(VI)中的应用。
9.根据权利要求8所述的应用,其特征在于,方法如下:在可见光照射下,于含有Cr(VI)的废水中加入权利要求1所述的3D花状Bi2WO6@CoO异质结光催化剂,进行光催化还原。
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