MWCNTs/TiO_2复合光催化剂优化制备及在光降解中的应用
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摘要
本论文从制备工艺、碳纳米管修饰改性和纳米TiO2掺杂改性三方面进行了MWCNTs/TiO2复合光催化剂的优化制备研究,通过其对模拟污染物甲基橙的光催化降解效果来研究考察不同制备工艺参数和改性条件对催化活性的影响,并选出催化活性最高的制备工艺和改性方法,最终应用于1,2,4-三氯苯的光催化降解。
以甲基橙为模拟污染物,通过考察不同制备工艺条件下复合光催化剂催化活性的差异,对比筛选出溶胶—凝胶法最佳制备工艺参数为：煅烧温度500℃、煅烧时间3h、溶胶体系pH值为3、固着剂聚苯乙烯磺酸钠投加量5g／L、碳纳米管投加量为TiO2质量的1.5%。采用微波辐照法、空气煅烧氧化法、硝酸氧化法及硝酸氧化与空气煅烧联用法对多壁碳纳米管进行了修饰改性,并研究考察多壁碳纳米管不同管长、管径结构和不同改性方法对复合光催化剂催化活性的影响,结果表明,复合光催化剂催化活性随碳纳米管管径的变大和管长的变长而逐渐增强；微波辐照和硝酸氧化与空气煅烧联用两种改性方法对提高复合光催化剂催化活性作用较大,其中N2载气环境下700W微波辐照功率改性碳纳米管制备的复合光催化剂催化活性最高。过渡金属离子掺杂纳米TiO2实验研究表明,Fe3+、Cr3+和Zr4+三种离子掺杂对复合光催化剂光催化活性的提高均有一定的促进作用；其中以Fe3+效果最好,Cr3+次之,而Zr4+对催化活性提高作用甚微。应用制备的高催化活性复合光催化剂光催化降解1,2,4-三氯苯的实验表明,与普通纳米TiO2光催化剂相比,复合光催化剂具有更高的光催化降解效果。
总之,经过优化制备的高催化活性复合光催化剂将弥补传统光催化氧化技术中半导体催化剂存在的缺陷,对于治理氯苯类有机污染物及其他持久性有机污染物造成的环境污染具有潜在的应用价值。
In this paper, the optimizing preparations such as preparation technology,modification of mutil-walled carbon nanotubes, doping modification of TiO2 of the composite photocatalysts (TiO2/MWCNTs) were investigated. The effects of photocatalytic activity with different preparation and modification had been studied, according to the photodegradation of the goal pollutant methyl orange.The composite photocatalysts with the highest photocatalytic activity were selected, and also had been used in the photodegradation of 1,2,4-trichlorobenzene.
Using methyl orange as the target pollutant and acoording to the difference of photocatalytic activities among the composite photocatalysts under different preparation technologies the best preparation technology of sol-gel method was selected, which was calcinated at temperature of 500℃for 3h, when pH=3,pss dosage 5g/L and multi-walled carbon nanotubes dosage 1.5%.
Adopting four different methods:microwave radiation, air-calcined oxidation, nitric acid oxidation and nitric oxide associated with the use of air-calcined to modified the multi-walled carbon nanotubes, and the effects of photocatalytic activity with multi-walled carbon nanotube of different length and diameter and different preparation and modification also had been studied. The results showed that photocatalytic activity of the composite photocatalysts would be better with the larger tube diameter and the longer tube length. Microwave radiation and nitric oxide associated with the use of air-calcined were the best methods, which had greater roles to improve photocatalytic activity of the composite photocatalysts. Photocatalytic activity of the composite photocatalysts with multi-walled carbon nanotube was highest which was modified with microwave radiation under the power of 700W.
The effects of photocatalytic activity with various transitional metal ions with doping modification of TiO2 had been also studied, and the results showed that the doping of three transitional metal ions(Fe3+,Cr3+,Zr4+) could improve photocatalytic activity of the composite photocatalysts. Among the three transitional metal ions, photocatalytic activity of the composite photocatalysts with Fe3+doping was the highest, and the Cr3+doping was lower. Photocatalytic activity of the composite photocatalysts with Zr4+ doping was lowest.
The composite photocatalysts with highest photocatalytic activity was used in the photodegradation of 1,2,4-trichlorobenzene, and the results showed that the composite photocatalysts had higher photocatalytic activity than TiO2.
The composite photocatalysts with highest photocatalytic activity under the optimizing preparation will make up the defects of the traditional semiconductor photocatalytic oxidation catalyst, and will also have potential applications in the treatment of environmental pollution with chlorobenzene organic pollutants and other persistent organic pollutants.
以甲基橙为模拟污染物,通过考察不同制备工艺条件下复合光催化剂催化活性的差异,对比筛选出溶胶—凝胶法最佳制备工艺参数为：煅烧温度500℃、煅烧时间3h、溶胶体系pH值为3、固着剂聚苯乙烯磺酸钠投加量5g／L、碳纳米管投加量为TiO2质量的1.5%。采用微波辐照法、空气煅烧氧化法、硝酸氧化法及硝酸氧化与空气煅烧联用法对多壁碳纳米管进行了修饰改性,并研究考察多壁碳纳米管不同管长、管径结构和不同改性方法对复合光催化剂催化活性的影响,结果表明,复合光催化剂催化活性随碳纳米管管径的变大和管长的变长而逐渐增强；微波辐照和硝酸氧化与空气煅烧联用两种改性方法对提高复合光催化剂催化活性作用较大,其中N2载气环境下700W微波辐照功率改性碳纳米管制备的复合光催化剂催化活性最高。过渡金属离子掺杂纳米TiO2实验研究表明,Fe3+、Cr3+和Zr4+三种离子掺杂对复合光催化剂光催化活性的提高均有一定的促进作用；其中以Fe3+效果最好,Cr3+次之,而Zr4+对催化活性提高作用甚微。应用制备的高催化活性复合光催化剂光催化降解1,2,4-三氯苯的实验表明,与普通纳米TiO2光催化剂相比,复合光催化剂具有更高的光催化降解效果。
总之,经过优化制备的高催化活性复合光催化剂将弥补传统光催化氧化技术中半导体催化剂存在的缺陷,对于治理氯苯类有机污染物及其他持久性有机污染物造成的环境污染具有潜在的应用价值。
In this paper, the optimizing preparations such as preparation technology,modification of mutil-walled carbon nanotubes, doping modification of TiO2 of the composite photocatalysts (TiO2/MWCNTs) were investigated. The effects of photocatalytic activity with different preparation and modification had been studied, according to the photodegradation of the goal pollutant methyl orange.The composite photocatalysts with the highest photocatalytic activity were selected, and also had been used in the photodegradation of 1,2,4-trichlorobenzene.
Using methyl orange as the target pollutant and acoording to the difference of photocatalytic activities among the composite photocatalysts under different preparation technologies the best preparation technology of sol-gel method was selected, which was calcinated at temperature of 500℃for 3h, when pH=3,pss dosage 5g/L and multi-walled carbon nanotubes dosage 1.5%.
Adopting four different methods:microwave radiation, air-calcined oxidation, nitric acid oxidation and nitric oxide associated with the use of air-calcined to modified the multi-walled carbon nanotubes, and the effects of photocatalytic activity with multi-walled carbon nanotube of different length and diameter and different preparation and modification also had been studied. The results showed that photocatalytic activity of the composite photocatalysts would be better with the larger tube diameter and the longer tube length. Microwave radiation and nitric oxide associated with the use of air-calcined were the best methods, which had greater roles to improve photocatalytic activity of the composite photocatalysts. Photocatalytic activity of the composite photocatalysts with multi-walled carbon nanotube was highest which was modified with microwave radiation under the power of 700W.
The effects of photocatalytic activity with various transitional metal ions with doping modification of TiO2 had been also studied, and the results showed that the doping of three transitional metal ions(Fe3+,Cr3+,Zr4+) could improve photocatalytic activity of the composite photocatalysts. Among the three transitional metal ions, photocatalytic activity of the composite photocatalysts with Fe3+doping was the highest, and the Cr3+doping was lower. Photocatalytic activity of the composite photocatalysts with Zr4+ doping was lowest.
The composite photocatalysts with highest photocatalytic activity was used in the photodegradation of 1,2,4-trichlorobenzene, and the results showed that the composite photocatalysts had higher photocatalytic activity than TiO2.
The composite photocatalysts with highest photocatalytic activity under the optimizing preparation will make up the defects of the traditional semiconductor photocatalytic oxidation catalyst, and will also have potential applications in the treatment of environmental pollution with chlorobenzene organic pollutants and other persistent organic pollutants.
引文
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