CN113941353B - FeWO4/g-C3N4光催化剂及其制备方法和应用 - Google Patents
FeWO4/g-C3N4光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种FeWO4/g‑C3N4光催化剂制备方法,包括如下步骤:将FeWO4与g‑C3N4分散于溶剂中超声,利用两种物质在溶液中的表面电负性,通过静电自组装的方式进行复合,当蒸干溶剂后即可得到FeWO4/g‑C3N4光催化剂。FeWO4/g‑C3N4光催化剂,由所述制备方法所制得。FeWO4/g‑C3N4光催化剂在草酸活化下光催化降解RhB或Cr(Ⅵ)中的应用。制备方法具有操作简单、成本低廉等优点;所制备的FeWO4/g‑C3N4光催化剂纯度高,且可以通过改变草酸的含量控制FeWO4/g‑C3N4光催化剂光催化降解性能;所获得的FeWO4/g‑C3N4光催化剂的催化活性高。
Description
技术领域
本发明涉及光催化剂领域,具体涉及一种FeWO4/g-C3N4光催化剂及其制备方法和应用。
背景技术
目前,污水中含有的有机污染物和重金属离子如铬等严重威胁人类的生命安全和生态安全,对单一污染物的研究也已经无法满足处理复杂水体系的需求。高级氧化技术主要通过产生强氧化性的活性物种·OH,进而将有机污染物氧化成无机小分子,其中Fenton反应应用广泛,但是传统Fenton反应面临需要在反应过程中补充Fe2+和H2O2以提高效率的问题,因此,实现铁的循环转换以及连续产生活性自由基是提高降解效率的重中之重。草酸,作为一种具有配位能力的无机小分子酸,通过与金属铁形成配合物,在光的照射下,发生价态转换,同时可以生成活性自由基用于污染物降解。
[FeⅢ(C2O4)3]3-+hν→[FeⅡ(C2O4)2]2-+·C2O4 - (1)
·C2O4 -→·O2 -+CO2 (2)
FeⅡ+·O2 -+H+→FeⅢ+H2O2 (3)
FeWO4是一种具有可见光响应的材料,带隙为2.0eV,但是其载流子利用低,为了提高其活性,科学家们进行大量研究,如调控形貌、制备复合材料等,其中,通过与别的材料复合可以有效提高光生电子-空穴对的分离效率,进一步提高催化剂的光催化活性。g-C3N4同样是对可见光有较强吸收能力的层状材料,同时其具备生产成本低廉,制备简单和热稳定性良好等优点,层状纳米片结构不仅可以提高对光的吸收能力,而且可以作为催化剂的载体,提高分散性和缩短电荷传输的距离。
研究表明,FeWO4/g-C3N4催化剂在光催化降解罗丹明B、四环素、水杨酸和气体甲苯等方面具有很大的潜力,而目前,关于在草酸的活化作用下,提高FeWO4/g-C3N4光催化剂同步去除有机污染物和Cr(Ⅵ)的活性尚未见报道。
发明内容
本发明所要解决的技术问题是提供一种FeWO4/g-C3N4光催化剂及其制备方法和应用,以克服上述现有技术中的不足。
本发明解决上述技术问题的技术方案如下:一种FeWO4/g-C3N4光催化剂制备方法,包括如下步骤:
将FeWO4与g-C3N4分散于溶剂中超声,利用两种物质在溶液中的表面电负性,通过静电自组装的方式进行复合,当蒸干溶剂后即可得到FeWO4/g-C3N4光催化剂。
在上述技术方案的基础上,本发明还可以做如下改进。
进一步,FeWO4与g-C3N4的比例为0.5~1.5。
进一步,FeWO4与g-C3N4的比例为0.5、1.0或1.5。
进一步,溶剂为无水乙醇。
进一步,超声复合的反应温度为室温,反应时间为360±5min。
进一步,蒸干溶剂的为温度为80±2℃。
一种FeWO4/g-C3N4光催化剂,由所述制备方法所制得。
一种FeWO4/g-C3N4光催化剂在草酸活化下光催化降解RhB或Cr(Ⅵ)中的应用。
本发明的有益效果是:
1)制备方法具有操作简单、成本低廉等优点;
2)本发明所制备的FeWO4/g-C3N4光催化剂纯度高,且可以通过改变草酸的含量控制FeWO4/g-C3N4光催化剂光催化降解性能;
3)本发明所获得的FeWO4/g-C3N4光催化剂的催化活性高,在光催化领域具有良好的应用前景。
附图说明
图1为本发明制备的系列FWO/CN光催化剂的XRD谱图,且图中曲线(d)为实施例1制备得到的1%FWO/CN光催化剂的XRD谱图;
图2为本发明制备的FWO/CN光催化剂的TEM图;
图3为本发明制备的1%FWO/CN光催化剂的光催化去除RhB性能图,图中曲线(d)和(e)为应用例1和应用例2得到的1%FWO/CN光催化剂的光催化去除RhB性能图;
图4为本发明制备的1%FWO/CN光催化剂的光催化去除Cr(Ⅵ)性能图,图中曲线(d)和(e)为应用例1和应用例2得到的1%FWO/CN光催化剂的光催化去除Cr(Ⅵ)性能图。
图5为本发明制备的1%FWO/CN光催化剂在不同草酸量活化下光催化去除RhB性能图,图中曲线(b)、(c)和(d)为应用例3、应用例4和应用例5得到的1%FWO/CN光催化剂的光催化去除RhB性能图;
图6为本发明制备的1%FWO/CN光催化剂在草酸活化下光催化去除不同初始pH的RhB性能图,图中曲线(a)、(b)、(c)、(e)、(f)、(g)分别为应用例6、应用例7、应用例8、应用例9、应用例10和应用例11得到的1%FWO/CN光催化剂的光催化去除RhB性能图;
具体实施方式
以下结合附图对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
实施例1
一种FeWO4/g-C3N4光催化剂,通过如下方法制备得到:
1)将0.0020g的FeWO4和0.2000g的g-C3N4分散到30mL无水乙醇中;
2)将步骤1)中混合溶液在超声反应器中超声,利用两种物质在溶液中的表面电负性,通过静电自组装的方式进行复合,反应温度为室温,时间为360±5min,复合结束,在80±2℃的温度下蒸干溶剂,即可得到FeWO4/g-C3N4光催化剂,记作1%FWO/CN光催化剂。
本实施例制备得到的1%FWO/CN光催化剂的XRD谱图见图1中(d),图1中(d)表明,所获得产物的XRD峰均与标准CN的特征峰一致,由于FWO的含量低造成没有明显检测到其特征峰,图2中可以看出小片状FWO分布在薄层CN上,证明所合成的样品为FWO/CN。同理,调整FeWO4和g-C3N4的比例,可以分别获得不同的FeWO4/g-C3N4光催化剂,例如,FeWO4与g-C3N4的比例为0.5时,获得0.5%FWO/CN光催化剂,FeWO4与g-C3N4的比例为1.5时,获得1.5%FWO/CN光催化剂。
应用例1
实施例1所得1%FWO/CN光催化剂,在草酸活化下,光催化降解RhB或Cr(Ⅵ);
具体操作方法如下:
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L的RhB或100mL浓度为5mg/L的Cr(Ⅵ)溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入18.9mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
而Cr(Ⅵ)溶液的测定采用二苯碳酰二肼分光光度法测定:
取5mL溶液于50mL比色管,用水稀释至标线,加入0.5mL(1+1)硫酸溶液、0.5mL(1+1)磷酸溶液和2mL显色剂(二苯碳酰二肼溶液),摇匀,5min后,采用分光光度计在波长540nm处测得吸光度值;
本实施例降解RhB实验结果见图3(d),光催化反应30min后,与条件不加草酸(见图3中(b))和CN催化剂(见图3中(c))相比,1%FWO/CN降解90.3%RhB,同理,与条件不加草酸(见图4中(b))和CN催化剂(见图4中(c))相比较,本实施例降解47.9%Cr(Ⅵ)(见图4(d))。
应用例2
实施例1所得1%FWO/CN光催化剂,在草酸活化下,光催化降解RhB和Cr(Ⅵ);
具体操作方法如下:
将10.0mg 1%FWO/CN分散到50mL浓度为10mg/L的RhB和50mL浓度为10mg/L的Cr(Ⅵ)溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入18.9mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
而Cr(Ⅵ)溶液的测定采用二苯碳酰二肼分光光度法测定:
取5mL溶液于50mL比色管,用水稀释至标线,加入0.5mL(1+1)硫酸溶液、0.5mL(1+1)磷酸溶液和2mL显色剂(二苯碳酰二肼溶液),摇匀,5min后,采用分光光度计在波长540nm处测得吸光度值;
本实施例同步降解RhB实验结果见图3(e),光催化反应30min后,与降解单一RhB(见图3中(d))相比,1%FWO/CN同步降解84.6%RhB,同理,与降解单一Cr(Ⅵ)(见图4中(d))相比较,本实施例同步降解83.0%Cr(Ⅵ)(见图4(e))。
实施例2
实施例1所得1%FWO/CN光催化剂,在不同草酸量的活化下光催化降解RhB,具体步骤如下:
1)将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L的RhB溶液里;
2)在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入不同量草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
3)每间隔5min用针管取一次样,用滤头过滤催化剂;
4)RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值。
应用例3
实施例2条件下,加入0.5mM草酸;
具体操作方法如下:
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入6.3mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图5(b),光催化反应30min之后,与不加草酸(图5中(a))相比,1%FWO/CN光催化降解93%RhB。
应用例4
实施例2条件下,加入1.0mM草酸;
具体操作方法如下:
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图5(c),光催化反应30min之后,与不加草酸(图5中(a))相比,1%FWO/CN光催化降解94%RhB。
应用例5
实施例2条件下,加入1.5mM草酸;
具体操作方法如下:
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入18.9mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图5(d),光催化反应30min之后,与不加草酸(图5中(a))相比,1%FWO/CN光催化降解89%RhB。
实施例3
实施例1所得1%FWO/CN光催化剂,在草酸活化下光催化降解不同初始pH的RhB,具体步骤如下:
1)将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L不同初始pH的RhB溶液里;
2)在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
3)每间隔5min用针管取一次样,用滤头过滤催化剂;
4)RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值。
应用例6
实施例3条件下,初始RhB的pH调整为1;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为1,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为1的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(a),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为1的RhB降解率为95%。
应用例7
实施例3条件下,初始RhB的pH调整为3;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为3,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为3的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(b),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为3的RhB降解率为91%。
应用例8
实施例3条件下,初始RhB的pH调整为5;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为5,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为5的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(c),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为5的RhB降解率为92%。
应用例9
实施例3条件下,初始RhB的pH调整为7;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为7,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为7的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(e),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为7的RhB降解率为89%。
应用例10
实施例3条件下,初始RhB的pH调整为9;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为9,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为9的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(f),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为9的RhB降解率为93%。
应用例11
实施例3条件下,初始RhB的pH调整为11;
具体操作方法如下:
采用0.1M HCl和0.1M NaOH溶液,调整初始RhB的pH为11,
将10.0mg 1%FWO/CN分散到100mL浓度为5mg/L初始pH为11的RhB溶液里;
在黑暗条件下吸附30min达到吸脱附平衡后,打开光源的同时加入12.6mg草酸,采用300W氙灯作为光源,照射光的波长λ≥420nm;
每间隔5min用针管取一次样,用滤头过滤催化剂;
RhB溶液的测定直接采用分光光度计在波长554nm处测得吸光度值;
本实施例降解RhB实验结果如图6(g),光催化反应30min之后,与降解原RhB溶液(pH为5.2,图6中(d))相比,1%FWO/CN对初始pH为11的RhB降解率为78%。
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (3)
1.一种FeWO4/g-C3N4光催化剂的应用,其特征在于,FeWO4/g-C3N4光催化剂在草酸活化下光催化降解RhB或Cr(Ⅵ),其制备方法包括如下步骤:
将FeWO4与g-C3N4分散于溶剂中超声,溶剂为无水乙醇,超声复合的反应温度为室温,反应时间为360 ± 5 min,利用两种物质在溶液中的表面电负性,通过静电自组装的方式进行复合,在80±2℃的温度下蒸干溶剂,当蒸干溶剂后即可得到FeWO4/g-C3N4光催化剂。
2.根据权利要求1所述应用,其特征在于:FeWO4与g-C3N4的比例为0.5~1.5。
3.根据权利要求2所述应用,其特征在于:FeWO4与g-C3N4的比例为0.5、1.0或1.5。
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