多壁碳纳米管负载TiO_2对氯苯的吸附与光降解作用研究
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摘要
本研究以甲基橙为模拟污染物,采用溶胶-凝胶法进行了复合光催化剂(MWNTs/TiO2)的优化制备,结果表明：在煅烧温度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及L20-40型多壁碳纳米管(MWNTs)用量为纳米二氧化钛(TiO2)质量1.5%的工艺条件下制备的复合光催化剂光催化活性最高。由扫描电镜观察发现,MWNTs负载纳米TiO2后,MWNTs管壁表面包裹着一层厚厚的、分布均匀的纳米TiO2,外壁直径也由20-40nm增粗至60-80nm左右。借助EDX可以看出MWNTs/TiO2中含有Ti、C、O、Na和S几种元素,其中主要以Ti、O和C元素为主。通过表面分析仪确定纯化后MWNTs与优化后MWNTs/TiO2的比表面积分别为80.103m2/g和39：610m2/g：MWNTs表面孔径主要属于细孔范围,而MWNTs/TiO2的表面孔径主要属于中孔范围。通过FTIR定性分析表面官能团可知,在纯化后MWNTs与优化后MWNTs/TiO2的表面均主要存在羟基(-OH)、羰基(-C=O)、羧基(-COOH)等含氧官能团。MWNTs具有较强吸收峰,而MWNTs/TiO2的吸收峰相对来说明显减少、减弱。
用优化后制备的MWNTs/TiO2与纳米Ti02对1,2,4-三氯苯进行光催化降解对比实验,结果发现此两种光催化降解均可用一级反应来描述。MWNTs/TiO2对1,2,4-三氯苯的光催化反应速率常数为0.0196h-1,比纳米TiO2提高了63.3%左右。用优化后制备的MWNTs/TiO2对甲基橙和1,2,4-三氯苯进行光催化降解对比实验,结果发现MWNTs/TiO2对甲基橙和1,2,4-三氯苯的光催化降解反应速率常数分别为0.0367h-1和0.0196h-1,比纳米TiO2分别提高了146%和63.3%左右。在实验室优化条件下制备的复合光催化剂对氯苯类化合物同样具有较好的光催化降解效果。
用MWNTs及MWNTs/TiO2对三氯苯进行吸附研究对比实验,结果表明：在相同条件下,MWNTs及MWNTs/TiO2对1,2,3-三氯苯的最大吸附量分别为71.8mg/g和3.0mg/g。MWNTs及MWNTs/TiO2对1,2,3-三氯苯的吸附动力学曲线基本一致,两种吸附反应均可用假二级动力学方程来描述,其速率常数分别为0.0836g·mg-1·min-1和0.4159g·mg-1·min-1,说明MWNTs/TiO2具有更强的吸附驱动力。两种吸附热力学均遵循Freundlich方程,且都为自发吸热反应。MWNTs及MWNTs/TiO2与三氯苯之间的强吸附作用力是由疏水作用、氢键作用和MWNTs及MWNTs/TiO2表面与三氯苯苯环之间的π电子共轭作用等共同作用的结果,但可能主要是通过π电子共轭作用而实现的。
以典型氯苯类化合物为目标去除物,研究MWNTs/TiO2对其光催化降解及协同作用,结果表明：MWNTs/TiO2对六氯苯和五氯苯的光催化降解速率常数分别为0.0664h-1和0.0670h-1,明显高于其它氯苯类化合物。而1,4-二氯苯的光催化降解反应速率常数仅为0.0430h-1,在典型氯苯类化合物中最小。典型氯苯类化合物1,2,4-三氯苯、1,2,4,5-四氯苯、五氯苯及六氯苯的主要光催化降解路径分别为：1,2,4-TCB→1,4-DCB;1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB; PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;HCB→PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB。将MWNTs和纳米TiO2复合之后,MWNTs/TiO2对1,2,3-TCB的去除效果得到明显提高,充分体现出其对氯苯类化合物的吸附与光降解协同作用。溶液中温度或pH值降低,将有利于MWNTs/TiO2对1,2,3-TCB去除；MWNTs/TiO2投加量增多或紫外光光强增大将提高MWNTs/TiO2对1,2,3-TCB去除率。
因此,利用MWNTs/TiO2对水中氯苯类化合物的吸附与光降解协同作用,快速、彻底去除该类有机化合物将具有广阔的市场应用前景。
In this research, using methyl orange as a model pollutant, the composite photocatalysts (MWNTs/TiO2) were optimized prepared by the Sol-Gel method. The results show that, photocatalytic activity of the composite photocatalysts was highest, which was calcinated at temperature of500℃for3h, when pH=3, pss dosage=5g/L and the amount of multi-walled carbon nanotubes was1.5%of nano-TiO2mass. The SEM images shows that nano-TiO2was evenly coated on the surface of the multi-walled carbon nanotubes after it was attached on mutil-walled carbon nanotubes. Its outer diameter was thickened from20-40nm to about60-80nm. It could be seen that MWNTS/TiO2contained Ti, C, O, Na and S elements, mainly to Ti, O and C elements based, via EDX. Determined by the surface analyzer, specific surface area of the purified MWNTs and the optimized MWNTs/TiO2were80.103m2/g and39.610m2/g respectively; MWNTs surface is mainly micro pore diameter range, and MWNTs/TiO2is mainly medium pore diameter range. Qualitative analysis by FTIR, it shows that the oxygen-containing functional groups of the purified MWNTs and optimized MWNTs/TiO2mainly existed on the surface are hydroxyl (-OH), carbonyl (-C=O), carboxyl (-COOH), etc. MWNTs has a strong absorption peak, while the absorption peak of MWNTS/TiO2has been reduced and weakened relatively.
Using the optimized prepared MWNTs/TiO2and nano-TiO2, the results of the comparative experiment revealed that both the photocatalytic degradation of1,2,4-trichlorobenzene can be used to describe by the first order reaction. The photocatalytic reaction rate constant of MWNTs/TiO2on1,2,4-trichlorobenzene was0.0196h-1, which was increased by about63.3%compared to that with nano-TiO2-The comparative experiments of photocatalytic degradation were studied, by the optimized MWNTs/TiO2on methyl orange and1,2,4-trichlorobenzene. The results were found that photocatalytic degradation reaction rate constants of MWNTs/TiO2on methyl orange and1,2,4-trichlorobenzene were0.0367h-1and0.0196h-1, which was increased by14.6%and63.3%compared to that with nano-TiO2respectively. Under optimal conditions the prepation of the composite photocatalyst had good photocatalytic degradation effects on chlorobenzenes.
The comparative experiments of the adsorption of trichlorobenzene by MWNTs and MWNTs/TiO2were studied, and the results showed that, under the same conditions, the maximum adsorption capacities of1,2,3-trichlorobenzene were71.8mg/g by MWNTs and3.0mg/g by MWNTs/TiO2. the adsorption kinetics curve of the adsorption of1,2,3-trichlorobenzene by MWNTs and MWNTs/TiO2was agreement, the two adsorption reaction can be used to describe by the pseudo second order kinetic equation, the rate constants were0.0836g-mg-1·min-1and0.4159g·mg-1·min-1, shows a stronger adsorption driving force of MWNTS/TiO2. This two kinds of equations are both following the Freundlich adsorption thermodynamics, and both be the spontaneous endothermic reaction. The strong adsorption of MWNTs and MWNTs/TiO2on trichlorobenzene base on the hydrophobic force, hydrogen bonding and the π electron conjugation between surface of MWNTs or MWNTs/TiO2and trichlorobenzene benzene. But it may be mainly through the effect of π electron conjugation achieved.
Using typical chlorobenzenes as the target removal, the experiments were studied for photocatalytic degradation and the synergistic reaction of MWNTs/TiO2, it was found that, the photocatalytic degradation rate constants of HCB and PeCB by MWNTs/TiO2were0.0664h-1and0.0670h-1, and this data significantly higher than other chlorobenzenes. However, the data of1,4-DCB was only0.0430h-1, which was the lowest in typical chlorobenzenes. Its typical chlorobenzenes1,2,4-TCB,1,2,4,5-TeCB, PeCB and HCB photocatalytic degradation of the main path are:1,2,4-TCB→1,4-DCB;1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;HCB→PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB. After composite the MWNTs and nano-Ti02, the result of removaling1,2,3-TCB has been markedly improved, which fully reflects that MWNTs/TiO2has the adsorption and photodegradation synergistic reaction. The solution temperature or pH values decreasing, will help MWNTs/TiO2to removal1,2,3-TCB; increasing the dosage of MWNTs/TiO2or the intensity of UV light will help MWNTs/TiO2to removal1,2,3TCB.
Therefore, using the adsorption and photodegradation synergistic reaction of the MWNTs/TiO2to removal chlorobenzene compounds speedy and completely will have a broad market prospect.
用优化后制备的MWNTs/TiO2与纳米Ti02对1,2,4-三氯苯进行光催化降解对比实验,结果发现此两种光催化降解均可用一级反应来描述。MWNTs/TiO2对1,2,4-三氯苯的光催化反应速率常数为0.0196h-1,比纳米TiO2提高了63.3%左右。用优化后制备的MWNTs/TiO2对甲基橙和1,2,4-三氯苯进行光催化降解对比实验,结果发现MWNTs/TiO2对甲基橙和1,2,4-三氯苯的光催化降解反应速率常数分别为0.0367h-1和0.0196h-1,比纳米TiO2分别提高了146%和63.3%左右。在实验室优化条件下制备的复合光催化剂对氯苯类化合物同样具有较好的光催化降解效果。
用MWNTs及MWNTs/TiO2对三氯苯进行吸附研究对比实验,结果表明：在相同条件下,MWNTs及MWNTs/TiO2对1,2,3-三氯苯的最大吸附量分别为71.8mg/g和3.0mg/g。MWNTs及MWNTs/TiO2对1,2,3-三氯苯的吸附动力学曲线基本一致,两种吸附反应均可用假二级动力学方程来描述,其速率常数分别为0.0836g·mg-1·min-1和0.4159g·mg-1·min-1,说明MWNTs/TiO2具有更强的吸附驱动力。两种吸附热力学均遵循Freundlich方程,且都为自发吸热反应。MWNTs及MWNTs/TiO2与三氯苯之间的强吸附作用力是由疏水作用、氢键作用和MWNTs及MWNTs/TiO2表面与三氯苯苯环之间的π电子共轭作用等共同作用的结果,但可能主要是通过π电子共轭作用而实现的。
以典型氯苯类化合物为目标去除物,研究MWNTs/TiO2对其光催化降解及协同作用,结果表明：MWNTs/TiO2对六氯苯和五氯苯的光催化降解速率常数分别为0.0664h-1和0.0670h-1,明显高于其它氯苯类化合物。而1,4-二氯苯的光催化降解反应速率常数仅为0.0430h-1,在典型氯苯类化合物中最小。典型氯苯类化合物1,2,4-三氯苯、1,2,4,5-四氯苯、五氯苯及六氯苯的主要光催化降解路径分别为：1,2,4-TCB→1,4-DCB;1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB; PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;HCB→PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB。将MWNTs和纳米TiO2复合之后,MWNTs/TiO2对1,2,3-TCB的去除效果得到明显提高,充分体现出其对氯苯类化合物的吸附与光降解协同作用。溶液中温度或pH值降低,将有利于MWNTs/TiO2对1,2,3-TCB去除；MWNTs/TiO2投加量增多或紫外光光强增大将提高MWNTs/TiO2对1,2,3-TCB去除率。
因此,利用MWNTs/TiO2对水中氯苯类化合物的吸附与光降解协同作用,快速、彻底去除该类有机化合物将具有广阔的市场应用前景。
In this research, using methyl orange as a model pollutant, the composite photocatalysts (MWNTs/TiO2) were optimized prepared by the Sol-Gel method. The results show that, photocatalytic activity of the composite photocatalysts was highest, which was calcinated at temperature of500℃for3h, when pH=3, pss dosage=5g/L and the amount of multi-walled carbon nanotubes was1.5%of nano-TiO2mass. The SEM images shows that nano-TiO2was evenly coated on the surface of the multi-walled carbon nanotubes after it was attached on mutil-walled carbon nanotubes. Its outer diameter was thickened from20-40nm to about60-80nm. It could be seen that MWNTS/TiO2contained Ti, C, O, Na and S elements, mainly to Ti, O and C elements based, via EDX. Determined by the surface analyzer, specific surface area of the purified MWNTs and the optimized MWNTs/TiO2were80.103m2/g and39.610m2/g respectively; MWNTs surface is mainly micro pore diameter range, and MWNTs/TiO2is mainly medium pore diameter range. Qualitative analysis by FTIR, it shows that the oxygen-containing functional groups of the purified MWNTs and optimized MWNTs/TiO2mainly existed on the surface are hydroxyl (-OH), carbonyl (-C=O), carboxyl (-COOH), etc. MWNTs has a strong absorption peak, while the absorption peak of MWNTS/TiO2has been reduced and weakened relatively.
Using the optimized prepared MWNTs/TiO2and nano-TiO2, the results of the comparative experiment revealed that both the photocatalytic degradation of1,2,4-trichlorobenzene can be used to describe by the first order reaction. The photocatalytic reaction rate constant of MWNTs/TiO2on1,2,4-trichlorobenzene was0.0196h-1, which was increased by about63.3%compared to that with nano-TiO2-The comparative experiments of photocatalytic degradation were studied, by the optimized MWNTs/TiO2on methyl orange and1,2,4-trichlorobenzene. The results were found that photocatalytic degradation reaction rate constants of MWNTs/TiO2on methyl orange and1,2,4-trichlorobenzene were0.0367h-1and0.0196h-1, which was increased by14.6%and63.3%compared to that with nano-TiO2respectively. Under optimal conditions the prepation of the composite photocatalyst had good photocatalytic degradation effects on chlorobenzenes.
The comparative experiments of the adsorption of trichlorobenzene by MWNTs and MWNTs/TiO2were studied, and the results showed that, under the same conditions, the maximum adsorption capacities of1,2,3-trichlorobenzene were71.8mg/g by MWNTs and3.0mg/g by MWNTs/TiO2. the adsorption kinetics curve of the adsorption of1,2,3-trichlorobenzene by MWNTs and MWNTs/TiO2was agreement, the two adsorption reaction can be used to describe by the pseudo second order kinetic equation, the rate constants were0.0836g-mg-1·min-1and0.4159g·mg-1·min-1, shows a stronger adsorption driving force of MWNTS/TiO2. This two kinds of equations are both following the Freundlich adsorption thermodynamics, and both be the spontaneous endothermic reaction. The strong adsorption of MWNTs and MWNTs/TiO2on trichlorobenzene base on the hydrophobic force, hydrogen bonding and the π electron conjugation between surface of MWNTs or MWNTs/TiO2and trichlorobenzene benzene. But it may be mainly through the effect of π electron conjugation achieved.
Using typical chlorobenzenes as the target removal, the experiments were studied for photocatalytic degradation and the synergistic reaction of MWNTs/TiO2, it was found that, the photocatalytic degradation rate constants of HCB and PeCB by MWNTs/TiO2were0.0664h-1and0.0670h-1, and this data significantly higher than other chlorobenzenes. However, the data of1,4-DCB was only0.0430h-1, which was the lowest in typical chlorobenzenes. Its typical chlorobenzenes1,2,4-TCB,1,2,4,5-TeCB, PeCB and HCB photocatalytic degradation of the main path are:1,2,4-TCB→1,4-DCB;1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB;HCB→PeCB→1,2,4,5-TeCB→1,2,4-TCB→1,4-DCB. After composite the MWNTs and nano-Ti02, the result of removaling1,2,3-TCB has been markedly improved, which fully reflects that MWNTs/TiO2has the adsorption and photodegradation synergistic reaction. The solution temperature or pH values decreasing, will help MWNTs/TiO2to removal1,2,3-TCB; increasing the dosage of MWNTs/TiO2or the intensity of UV light will help MWNTs/TiO2to removal1,2,3TCB.
Therefore, using the adsorption and photodegradation synergistic reaction of the MWNTs/TiO2to removal chlorobenzene compounds speedy and completely will have a broad market prospect.
引文
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