CN112569955A - 一种降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂及制备方法 - Google Patents
一种降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂及制备方法 Download PDFInfo
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Abstract
本发明公开了一种降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂及制备方法,属于光催化技术和环境污染治理技术领域。本发明方法为:称取一定量铋源和铁源溶解在DMF和乙酸的混合溶剂中,并向其中加入CeO2占BiFeO3理论质量1%~10%的Ce(NO3)3·6H2O,搅拌直至获得透明溶液,然后在透明溶液中加入PVP并搅拌均匀形成前驱体纺丝液;将前驱体纺丝液进行静电纺丝,收集的前驱体纳米纤维并干燥,之后在500~550℃空气中煅烧2~3h即可得到CeO2/BiFeO3纳米纤维光催化剂。本发明的光催化剂具有高效的可见光催化活性,可用于有机染料废水降解中,具有非常好的应用前景。
Description
技术领域
本发明涉及一种降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂及制备方法,属于光催化技术和环境污染治理技术领域。本发明通过调控硝酸铈的加入量来优化CeO2/BiFeO3纳米纤维光催化剂的光催化性能,该光催化剂具有高效的降解有机染料废水的能力。
背景技术
目前,环境污染日趋严重,特别是水污染已成为一个直接威胁人类生存,亟需解决的焦点问题。其中,纺织业产生的有机染料废水对水体污染非常严重。光催化技术是从二十世纪70年代逐步发展起来的在环境领域有着重要应用前景的绿色技术。该技术能使环境中的有机污染物发生氧化分解反应,最终降解为CO2、水和无机离子等小分子物质,由于不存在二次污染、降解程度高等优点被认为是目前最具开发潜力的环境污染处理方法。该技术的关键在于光催化剂的设计与选择。
目前,在众多的半导体光催化剂中,铋系光催化材料因其无毒、活性高和稳定等优势,具有潜在的应用价值,越来越受人们的关注。而BiFeO3是铋系光催化材料中的一种,其具有可见光催化活性。然而,BiFeO3具有难合成、快速的电子-空穴复合和低的量子产率限制了其广泛的应用。如何解决这些问题是提高BiFeO3光催化性能的关键。异质结构的构筑可有效结合不同组分的优势,建立有效界面促进光生载流子的分离和转移,是提高光催化性能的有效手段。CeO2因其价带位置较正,是一种具有较强氧化能力的光催化剂,因此,可以考虑构筑CeO2/BiFeO3异质结构能以有效分离光生电子-空穴对,从而实现光催化性能的提高。
发明内容
为了实现上述目的,本发明采用静电纺丝法一步构筑CeO2/BiFeO3纳米纤维光催化剂,通过该方法制得的CeO2/BiFeO3纳米纤维光催化剂尺寸均匀,光催化性能高,形成的异质结构可加快光生载流子的迁移速率,从而提高BiFeO3的光催化性能。该制备方法简单可靠,易操作,所制备的光催化剂能有效降解有机染料废水。
首先,本发明提供了一种用于降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂的制备方法,所述方法包括如下步骤:
称取一定量铋源和铁源溶解在DMF和乙酸的混合溶剂中,并向其中加入CeO2占BiFeO3理论质量1%~10%的Ce(NO3)3·6H2O,搅拌直至获得透明溶液,然后在透明溶液中加入PVP并搅拌均匀形成前驱体纺丝液;将前驱体纺丝液进行静电纺丝,收集的前驱体纳米纤维并干燥,之后在500~550℃空气中煅烧2~3h即可得到CeO2/BiFeO3纳米纤维光催化剂。
在本发明的一种实施方式中,所述铋源和铁源的Bi与Fe的摩尔比为6:(6~3)。
在本发明的一种实施方式中,所述铋源选自Bi(NO3)3·5H2O或氯化铋中的一种或两种。
在本发明的一种实施方式中,所述铁源选自Fe(NO3)3·9H2O或FeCl3·6H2O中的一种或两种。
在本发明的一种实施方式中,所述DMF和乙酸的体积比为(10~12):(2~3)。
在本发明的一种实施方式中,所述PVP的Mw=1.3×106。
在本发明的一种实施方式中,所述PVP的加入质量与铋源中Bi的摩尔数之比为1~1.2g:3mmol。
在本发明的一种实施方式中,所述静电纺丝的操作参数为:在端部和集电极上施加的电压分别为10~15kV和-1kV,针尖与收集器之间的距离保持在15~16cm,将进料速率设定为0.3~0.5mL·h-1,并且控制湿度水平50%RH。
在本发明的一种实施方式中,所述干燥是在60~70℃干燥6~12h。
本发明的第二个目的是提供上述制备方法制备得到的CeO2/BiFeO3纳米纤维光催化剂。
本发明的第三个目的是提供上述CeO2/BiFeO3纳米纤维光催化剂在处理废水中的应用。
在本发明的一种实施方式中,所述废水优选包含有机物染料的废水。
本发明的第四个目的是提供一种废水的处理方法,所述方法是利用上述的CeO2/BiFeO3纳米纤维光催化剂作为有机污染物降解剂。
本发明与现有技术相比,具有显著优点:
(1)本发明采用静电纺丝法同步合成CeO2/BiFeO3纳米纤维光催化剂,不需分步操作,方法简单可靠,易操作。所制备的光催化剂呈现纤维结构,易于回收。
(2)本发明所制备的CeO2/BiFeO3纳米纤维光催化剂,与纯BiFeO3相比,光生电子-空穴分离效率显著提高,在可见光照射下降解有机染料能力显著提升。
附图说明
图1BiFeO3、CeO2和实施例1~3制备得到的CeO2/BiFeO3纳米纤维光催化剂的X-射线衍射花样。
图2BiFeO3和实施例2制备得到的CeO2/BiFeO3纳米纤维光催化剂的扫描电镜照片;其中,(a,b)纯BiFeO3纳米纤维样品,(c,d)3%CeO2/BiFeO3纳米纤维样品。
图3实施例3制备得到的CeO2/BiFeO3纳米纤维光催化剂的透射电镜照片;其中,(a)3%CeO2/BiFeO3,(b)3%CeO2/BiFeO3的高分辨透射电镜照片。
图4BiFeO3、CeO2和实施例1~3制备得到的CeO2/BiFeO3纳米纤维光催化剂的光催化性能对比。
图5对比例1和2制备得到的CeO2/BiFeO3纳米纤维光催化剂的扫描电镜照片;其中,(a)对比例1;(b)对比例2。
具体实施方式
下面结合实施例对本发明作进一步的描述,但本发明的实施方式不限于此。
本发明CeO2/BiFeO3纳米纤维光催化剂,利用静电纺丝法一步实现CeO2/BiFeO3异质结构的构筑,显著增强对可见光的吸收,具有高效降解有机染料废水的光催化性能。
实施例1
一种可用于有机染料废水降解的CeO2/BiFeO3纳米纤维光催化剂的制备方法,包括以下步骤:
分别称取6mmolBi(NO3)3·5H2O和6mmolFe(NO3)3·9H2O溶解在10mL DMF和2mL乙酸的混合物中,并向其中加入占BiFeO3理论质量1%的Ce(NO3)3·6H2O,充分搅拌直至获得透明溶液。然后将2.16g PVP(Mw=1.3×106)缓慢加入到上述透明溶液中并搅拌形成前驱体纺丝液。转移到10mL注射器中,在端部和集电极上施加的电压分别为15kV和-1kV。针尖与收集器之间的距离保持在15cm。将进料速率设定为0.3mL·h-1,并且控制湿度水平约50%RH。收集的前驱体纳米纤维在60℃的烘箱中干燥12h。然后在550℃空气中煅烧2.5h得到1%CeO2/BiFeO3纳米纤维光催化剂。
实施例2
一种可用于有机染料废水降解的CeO2/BiFeO3纳米纤维光催化剂的制备方法,包括以下步骤:
分别称取6mmolBi(NO3)3·5H2O和6mmolFe(NO3)3·9H2O溶解在10mL DMF和2mL乙酸的混合物中,并向其中加入占BiFeO3理论质量3%的Ce(NO3)3·6H2O,充分搅拌直至获得透明溶液。然后将2.16g PVP(Mw=1.3×106)缓慢加入到上述透明溶液中并搅拌形成前驱体纺丝液。转移到10mL注射器中,在端部和集电极上施加的电压分别为15kV和-1kV。针尖与收集器之间的距离保持在15cm。将进料速率设定为0.3mL·h-1,并且控制湿度水平约50%RH。收集的前驱体纳米纤维在60℃的烘箱中干燥12h。然后在550℃空气中煅烧2.5h得到3%CeO2/BiFeO3纳米纤维光催化剂。
实施例3
一种可用于有机染料废水降解的CeO2/BiFeO3纳米纤维光催化剂的制备方法,包括以下步骤:
分别称取6mmolBi(NO3)3·5H2O和6mmolFe(NO3)3·9H2O溶解在10mL DMF和2mL乙酸的混合物中,并向其中加入占BiFeO3理论质量5%的Ce(NO3)3·6H2O,充分搅拌直至获得透明溶液。然后将2.16g PVP(Mw=1.3×106)缓慢加入到上述透明溶液中并搅拌形成前驱体纺丝液。转移到10mL注射器中,在端部和集电极上施加的电压分别为15kV和-1kV。针尖与收集器之间的距离保持在15cm。将进料速率设定为0.3mL·h-1,并且控制湿度水平约50%RH。收集的前驱体纳米纤维在60℃的烘箱中干燥12h。然后在550℃空气中煅烧2.5h得到5%CeO2/BiFeO3纳米纤维光催化剂。
实施例4
一种可用于有机染料废水降解的CeO2/BiFeO3纳米纤维光催化剂的制备方法,包括以下步骤:
分别称取6mmolBi(NO3)3·5H2O和6mmolFe(NO3)3·9H2O溶解在10mL DMF和2mL乙酸的混合物中,并向其中加入占BiFeO3理论质量10%的Ce(NO3)3·6H2O,充分搅拌直至获得透明溶液。然后将2.16g PVP(Mw=1.3×106)缓慢加入到上述透明溶液中并搅拌形成前驱体纺丝液。转移到10mL注射器中,在端部和集电极上施加的电压分别为15kV和-1kV。针尖与收集器之间的距离保持在15cm。将进料速率设定为0.3mL·h-1,并且控制湿度水平约50%RH。收集的前驱体纳米纤维在60℃的烘箱中干燥12h。然后在550℃空气中煅烧2.5h得到10%CeO2/BiFeO3纳米纤维光催化剂。
在对比实施例1基础上,不加入Ce(NO3)3·6H2O,保持其他条件不变,得到BiFeO3纳米纤维;同样在实施例1基础上,不加铋源和铁源,而加入6mmol的Ce(NO3)3·6H2O,以及PVP的用量减半,保持其他条件不变,得到CeO2纳米纤维。
对制备得到的BiFeO3,CeO2和不同比例CeO2/BiFeO3纳米纤维光催化剂进行了X-射线衍射表征。从图1可以看出,BiFeO3的衍射峰对应于标准卡片86-1518,CeO2的衍射峰对应于标准卡片75-0076,说明两者均为纯相物质。1%CeO2/BiFeO3纳米纤维光催化剂中的衍射峰主要对应BiFeO3的衍射峰,由于CeO2的含量较低,很难被检测出来。随着硝酸铈添加量的增加,CeO2的衍射峰可被检测到,说明CeO2/BiFeO3纳米纤维光催化剂的成功制备。
利用扫描电子显微镜对所制备样品的形貌进行了分析,如图2a和2b所示,纯BiFeO3为纳米纤维结构;从图2c和2d可以看出,掺杂3%硝酸铈所得到的CeO2/BiFeO3光催化剂保持了原来的纤维结构;从图3中同样可以看出掺杂3%硝酸铈所得到的CeO2/BiFeO3光催化剂保持了纤维结构,并且从高分辨透射电镜中可以看到清晰的晶格条纹,对应于CeO2和BiFeO3组分,说明CeO2/BiFeO3异质结构的形成。
通过300W氙灯加滤光片截取波长λ>420nm的可见光部分,以降解有机染料金橙II溶液来评价所制备光催化剂的可见光催化性能,具体的实验过程如下:称取15mg光催化剂加入到100mL 10mg/L的有机染料金橙II溶液,将配好的溶液置于暗处搅拌分散30min使其达到吸附平衡,然后打开氙灯光源使溶液进行光催化反应,每隔15min取约4mL的溶液,利用离心机离心分离出光催化剂,取上层清夜用紫外分光光度计来测量溶液中残留的有机染料金橙II溶液的吸光度。结果见图4,从图4中可以看出,120分钟内,3%CeO2/BiFeO3纳米纤维光催化剂可降解有机染料金橙II接近45%,而纯BiFeO3只能降解接近15%,CeO2只能降解接近30%,说明CeO2/BiFeO3纳米纤维光催化剂性能明显优于纯BiFeO3和CeO2。
实施例5
分别称取6mmol氯化铋和5mmolFeCl3·6H2O溶解在12mL DMF和3mL乙酸的混合物中,并向其中加入占BiFeO3理论质量7%的Ce(NO3)3·6H2O,充分搅拌直至获得透明溶液。然后将2.2g PVP(Mw=1.3×106)缓慢加入到上述透明溶液中并搅拌形成前驱体纺丝液。转移到10mL注射器中,在端部和集电极上施加的电压分别为15kV和-1kV。针尖与收集器之间的距离保持在16cm。将进料速率设定为0.5mL·h-1,并且控制湿度水平约50%RH。收集的前驱体纳米纤维在70℃的烘箱中干燥6h。然后在550℃空气中煅烧3h得到CeO2/BiFeO3纳米纤维光催化剂。
对比例1
在实施例1的基础上,改变纺丝参数设定,在端部和集电极上施加的电压分别为20kV和-1.5kV,将进料速率设定为1.0mL·h-1,保持其他条件不变,如图5a所示,发现所制备的1%CeO2/BiFeO3样品纤维形貌遭到破坏,样品大多为颗粒状,不利于光催化性能的提升。
对比例2
在实施例1的基础上,分别使用乙酰丙酮铋和乙酰丙酮铁作为铋源和铁源,保持其他条件不变,如图5b所示,发现所制备的1%CeO2/BiFeO3样品纤维形貌保持不是很好,并且组成纤维的颗粒尺寸变大,不利于光催化性能的提升。
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (10)
1.一种用于降解有机染料废水的CeO2/BiFeO3纳米纤维光催化剂的制备方法,其特征在于,所述方法包括如下步骤:
称取一定量铋源和铁源溶解在DMF和乙酸的混合溶剂中,并向其中加入CeO2占BiFeO3理论质量1%~10%的Ce(NO3)3·6H2O,搅拌直至获得透明溶液,然后在透明溶液中加入PVP并搅拌均匀形成前驱体纺丝液;将前驱体纺丝液进行静电纺丝,收集的前驱体纳米纤维并干燥,之后在500~550℃空气中煅烧2~3h即可得到CeO2/BiFeO3纳米纤维光催化剂
2.根据权利要求1所述的制备方法,其特征在于,所述铋源和铁源的Bi与Fe的摩尔比为6:(6~3)。
3.根据权利要求1或2所述的制备方法,其特征在于,所述铋源选自Bi(NO3)3·5H2O或氯化铋中的一种或两种。
4.根据权利要求1~3任一所述的制备方法,其特征在于,所述铁源选自Fe(NO3)3·9H2O或FeCl3·6H2O中的一种或两种。
5.根据权利要求1~4任一所述的制备方法,其特征在于,所述DMF和乙酸的体积比为(10~12):(2~3)。
6.根据权利要求1~5任一所述的制备方法,其特征在于,所述PVP的加入质量与铋源中Bi的摩尔数之比为1~1.2g:3mmol。
7.根据权利要求1~6任一所述的制备方法,其特征在于,在端部和集电极上施加的电压分别为10~15kV和-1kV,针尖与收集器之间的距离保持在15~16cm,将进料速率设定为0.3~0.5mL·h-1,并且控制湿度水平50%RH。
8.根据权利要求1~7任一所述的制备方法制备得到的CeO2/BiFeO3纳米纤维光催化剂。
9.权利要求8所述的CeO2/BiFeO3纳米纤维光催化剂在处理废水中的应用。
10.一种废水的处理方法,其特征在于,所述方法是利用权利要求8所述的CeO2/BiFeO3纳米纤维光催化剂作为有机污染物降解剂。
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