CN113333002B - 一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法及其制得的产品 - Google Patents
一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法及其制得的产品 Download PDFInfo
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 26
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- AUIZLSZEDUYGDE-UHFFFAOYSA-L cadmium(2+);diacetate;dihydrate Chemical compound O.O.[Cd+2].CC([O-])=O.CC([O-])=O AUIZLSZEDUYGDE-UHFFFAOYSA-L 0.000 claims abstract description 9
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Abstract
本发明公开了一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,首先以Bi‑MOF为前驱体合成Bi2O3,然后以Bi2O3和二水合醋酸镉为原料采用原位油浴法负载硫化镉量子点于氧化铋表面,合成得到负载CdS量子点的氧化铋复合可见光催化材料。此外还公开了上述制备方法制得的产品。本发明制得的氧化铋复合可见光催化材料呈棒状结构,CdS量子点均匀分散于棒状氧化铋结构表面,有效增加了材料的比表面积,暴露出更多活性位点,从而有效提高了其可见光催化性能。
Description
技术领域
本发明涉及光催化材料技术领域,尤其涉及一种负载型氧化铋复合可见光催化材料的制备方法及其制得的产品。
背景技术
目前,随着现代工业技术的不断发展,越来越多的污染物被排放到水生生态系统中。其中,有机染料的污染占据主导地位,然而,传统的水处理工艺对其处理效果不佳。因此,亟需研发去除水中有机染料污染物的高效降解技术。在众多高级水处理技术中,光催化技术由于其高效、绿色环保等特点而受到研究者的广泛青睐。
光催化材料大致可以分为七大类,即金属氧化物、金属硫化物、Bi基光催化剂、Ag基光催化剂、g-C3N4、元素半导体催化剂与其他光催化材料。其中,Bi基光催化剂因其对人体无毒无害、成本低廉、较窄的带隙等性质引起了广泛关注。然而,单相的铋氧化物,其光生电荷的复合率较高,可见光响应差,从而限制了其光催化治污的能力。如何通过改性方法有效提升铋基材料的光催化性能,一直是本领域所要研究和解决的问题。
发明内容
本发明的目的在于克服现有技术的不足,提供一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,通过将硫化镉量子点均匀分散于棒状氧化铋结构表面,以有效增加材料的比表面积、暴露出更多活性位点,从而提高其可见光催化性能。本发明的另一目的在于提供上述负载CdS量子点的氧化铋复合可见光催化材料的制备方法制得的产品。
本发明的目的通过以下技术方案予以实现:
本发明提供的一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,包括以下步骤:
(1)以Bi-MOF为前驱体合成Bi2O3
(1-1)按照Bi2O3化学计量比称取Bi(NO3)3·5H2O和均苯三甲酸,并溶解于甲醇的DMF溶液中,搅拌均匀得到混合溶液;
(1-2)将所述混合溶液转入反应釜中,在120~140℃温度下反应12~24h,待反应产物冷却后,经洗涤、干燥,得到白色Bi-MOF前驱体;
(1-3)将所述Bi-MOF前驱体在空气氛围中进行煅烧处理,得到淡黄色Bi2O3产物;
(2)CdS@Bi2O3复合可见光催化材料的制备
按照摩尔比二水合醋酸镉∶硫代乙酰胺∶Bi2O3=0.025~0.15∶0.025~0.15∶1,将二水合醋酸镉与所述Bi2O3产物混合后分散于乙醇中形成混合液,在60~100℃温度下油浴加热10~20min后,加入硫代乙酰胺溶液,继续加热1~2h;反应产物自然冷却后,经洗涤、干燥,即制得负载CdS量子点的氧化铋复合可见光催化材料。
进一步地,本发明制备方法所述步骤(1-3)的煅烧温度为500~550℃。
本发明提供的上述负载CdS量子点的氧化铋复合可见光催化材料的制备方法制得的产品,所述CdS均匀分散于棒状氧化铋结构表面,所述CdS的尺寸为4~7nm。
本发明具有以下有益效果:
(1)CdS是一种n型半导体,且具有非常合理的能带结构,其禁带宽度是2.4eV,不但能够响应可见光,而且能够同时满足光吸收和光利用的要求;同时,CdS的光生载流子迁移速率和分离效率都较高,因此具有非常高的光催化活性。本发明制备方法将硫化镉量子点负载在氧化铋棒状结构上,可快速高效去除水中的亚甲基蓝。通过实验模拟去除含MB的废水,结果表明,在150min内对MB的去除率达到90~98.8%,为实际应用提供了可靠的理论和实际支撑。
(2)本发明制得的负载CdS量子点的氧化铋复合可见光催化材料呈棒状结构,硫化镉量子点均匀分散于棒状氧化铋结构表面,颗粒均一、分散性好,有效增加了材料的比表面积,暴露出更多活性位点,从而有效提高了其可见光催化性能。
附图说明
下面将结合实施例和附图对本发明作进一步的详细描述:
图1是本发明实施例制得的CdS@Bi2O3复合可见光催化材料的SEM图;
图2是本发明实施例制得的CdS@Bi2O3复合可见光催化材料的TEM图;
图3是本发明实施例制得的CdS@Bi2O3复合可见光催化材料对MB的降解曲线图。
具体实施方式
实施例一:
本实施例一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,其步骤如下:
(1)以Bi-MOF为前驱体合成Bi2O3
(1-1)将0.45gBi(NO3)3·5H2O和2.25g均苯三甲酸(H3BTC)溶解于180mL甲醇的DMF溶液(按照体积比DMF∶甲醇=4∶1)中,磁力搅拌30min后得到混合溶液;
(1-2)将上述混合溶液转入反应釜中,在120℃温度下反应24h,待反应产物冷却后,用DMF及甲醇试剂离心洗涤3次,之后于真空干燥箱中在60℃温度下干燥10h,得到白色Bi-MOF前驱体;
(1-3)将上述Bi-MOF前驱体置于马弗炉中,于空气氛围中在500℃温度下煅烧2h,得到淡黄色Bi2O3产物;
(2)CdS@Bi2O3复合可见光催化材料的制备
将0.025mol二水合醋酸镉(Cd(COOH)2·2H2O)与1.0mol上述Bi2O3产物混合后分散于50mL的乙醇中形成混合液,在80℃温度下油浴加热10min后,缓慢滴加硫代乙酰胺(TAA)溶液(含0.025mol硫代乙酰胺,溶液浓度与混合液相同),继续加热2h;反应产物自然冷却后,用乙醇离心洗涤3次,置于真空干燥箱中在60℃温度下干燥后,即制得负载CdS量子点的氧化铋复合可见光催化材料。
实施例二:
本实施例一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,其步骤如下:
(1)以Bi-MOF为前驱体合成Bi2O3
(1-1)将0.45gBi(NO3)3·5H2O和2.25g均苯三甲酸(H3BTC)溶解于180mL甲醇的DMF溶液(按照体积比DMF∶甲醇=4∶1)中,磁力搅拌30min后得到混合溶液;
(1-2)将上述混合溶液转入反应釜中,在130℃温度下反应20h,待反应产物冷却后,用DMF及甲醇试剂离心洗涤3次,之后于真空干燥箱中在60℃温度下干燥10h,得到白色Bi-MOF前驱体;
(1-3)将上述Bi-MOF前驱体置于马弗炉中,于空气氛围中在520℃温度下煅烧2h,得到淡黄色Bi2O3产物;
(2)CdS@Bi2O3复合可见光催化材料的制备
将0.050mol二水合醋酸镉(Cd(COOH)2·2H2O)与1.0mol上述Bi2O3产物混合后分散于50mL的乙醇中形成混合液,在60℃温度下油浴加热20min后,缓慢滴加硫代乙酰胺(TAA)溶液(含0.050mol硫代乙酰胺,溶液浓度与混合液相同),继续加热2h;反应产物自然冷却后,用乙醇离心洗涤3次,置于真空干燥箱中在60℃温度下干燥后,即制得负载CdS量子点的氧化铋复合可见光催化材料。
实施例三:
本实施例一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,其步骤如下:
(1)以Bi-MOF为前驱体合成Bi2O3
(1-1)将0.45gBi(NO3)3·5H2O和2.25g均苯三甲酸(H3BTC)溶解于180mL甲醇的DMF溶液(按照体积比DMF∶甲醇=4∶1)中,磁力搅拌30min后得到混合溶液;
(1-2)将上述混合溶液转入反应釜中,在140℃温度下反应12h,待反应产物冷却后,用DMF及甲醇试剂离心洗涤3次,之后于真空干燥箱中在60℃温度下干燥10h,得到白色Bi-MOF前驱体;
(1-3)将上述Bi-MOF前驱体置于马弗炉中,于空气氛围中在550℃温度下煅烧2h,得到淡黄色Bi2O3产物;
(2)CdS@Bi2O3复合可见光催化材料的制备
将0.010mol二水合醋酸镉(Cd(COOH)2·2H2O)与1.0mol上述Bi2O3产物混合后分散于50mL的乙醇中形成混合液,在90℃温度下油浴加热10min后,缓慢滴加硫代乙酰胺(TAA)溶液(含0.010mol硫代乙酰胺,溶液浓度与混合液相同),继续加热1h;反应产物自然冷却后,用乙醇离心洗涤3次,置于真空干燥箱中在60℃温度下干燥后,即制得负载CdS量子点的氧化铋复合可见光催化材料。
实施例四:
本实施例一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,其步骤如下:
(1)以Bi-MOF为前驱体合成Bi2O3
(1-1)将0.45gBi(NO3)3·5H2O和2.25g均苯三甲酸(H3BTC)溶解于180mL甲醇的DMF溶液(按照体积比DMF∶甲醇=4∶1)中,磁力搅拌30min后得到混合溶液;
(1-2)将上述混合溶液转入反应釜中,在120℃温度下反应24h,待反应产物冷却后,用DMF及甲醇试剂离心洗涤3次,之后于真空干燥箱中在60℃温度下干燥10h,得到白色Bi-MOF前驱体;
(1-3)将上述Bi-MOF前驱体置于马弗炉中,于空气氛围中在500℃温度下煅烧2h,得到淡黄色Bi2O3产物;
(2)CdS@Bi2O3复合可见光催化材料的制备
将0.15mol二水合醋酸镉(Cd(COOH)2·2H2O)与1.0mol上述Bi2O3产物混合后分散于50mL的乙醇中形成混合液,在80℃温度下油浴加热10min后,缓慢滴加硫代乙酰胺(TAA)溶液(含0.015mol硫代乙酰胺,溶液浓度与混合液相同),继续加热2h;反应产物自然冷却后,用乙醇离心洗涤3次,置于真空干燥箱中在60℃温度下干燥后,即制得负载CdS量子点的氧化铋复合可见光催化材料。
如图1所示,本发明实施例制备的CdS@Bi2O3复合可见光催化材料为棒状结构,硫化镉量子点均匀地分散于棒状氧化铋结构表面。如图2所示,CdS@Bi2O3复合可见光催化材料中CdS的尺寸为4nm。
本发明实施例制备的CdS@Bi2O3复合可见光催化材料,以单相的Bi2O3为对比例,其检测如下:
以亚甲基蓝(MB)水溶液模拟印染废水,配制含MB的模拟废水(20mg/L),在250mL烧杯中加入100mL含MB的印染废水以及10mg所制备的光催化材料,首先,在黑暗中磁力搅拌悬浮液30min,达到吸附-解吸平衡,吸附达到饱和,然后打开光源(氙灯,λ>420nm)。在一定时间间隔内,用注射器吸取2mL样品,通过0.45μm滤膜后,用紫外-可见分光光度计在MB的特征吸收波长664nm处测定样品吸光度,并进而分析MB的浓度变化。
MB的降解率按如下公式计算:
μ=(C0-C)/C0×100%
其结果如图3所示,本发明实施例制备的CdS@Bi2O3复合可见光催化材料,不仅对MB的去除率高,且具有可见光响应,在150min内对MB的降解率,实施例一、实施例二、实施例三、实施例四分别为93.0%、92.1%、98.8%、97.8%。
Claims (2)
1.一种负载CdS量子点的氧化铋复合可见光催化材料的制备方法,其特征在于包括以下步骤:
(1) 以Bi-MOF为前驱体合成Bi2O3
(1-1) 按照Bi2O3化学计量比称取Bi(NO3)3·5H2O和均苯三甲酸,并溶解于甲醇的DMF溶液中,搅拌均匀得到混合溶液;其中,所述甲醇的DMF溶液中按照体积比DMF∶甲醇=4∶1;
(1-2) 将所述混合溶液转入反应釜中,在120~140℃温度下反应12~24h,待反应产物冷却后,经洗涤、干燥,得到白色Bi-MOF前驱体;
(1-3) 将所述Bi-MOF前驱体在空气氛围中在500~550℃温度下进行煅烧处理,得到淡黄色Bi2O3产物;
(2) CdS@Bi2O3复合可见光催化材料的制备
按照摩尔比二水合醋酸镉∶硫代乙酰胺∶Bi2O3=0.025~0.15∶0.025~0.15∶1,将二水合醋酸镉与所述Bi2O3产物混合后分散于乙醇中形成混合液,在60~100℃温度下油浴加热10~20min后,加入硫代乙酰胺溶液,继续加热1~2h;反应产物自然冷却后,经洗涤、干燥,即制得负载CdS量子点的氧化铋复合可见光催化材料,其中CdS均匀分散于棒状氧化铋结构表面,所述CdS的尺寸为4~7nm;所述催化材料对于含MB的废水,在150min内对MB的去除率达到90~98.8%。
2.权利要求1所述负载CdS量子点的氧化铋复合可见光催化材料的制备方法制得的产品。
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