负载型活性炭催化臭氧氧化有机物研究
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摘要
本研究首先对低温下制备的载铜及载镍活性炭催化剂(Cu/AC和Ni/AC)进行多种形式的表征,其次研究了Cu/AC和Ni/AC在催化臭氧化中对苯酚和草酸的降解效果。考察了催化剂投加量、初始溶液pH值、叔丁醇浓度、催化剂循环使用对催化臭氧化反应的影响,进而对非均相催化臭氧化苯酚和草酸降解性能和反应机理展开了初步研究。运用动力学理论对Cu/AC和Ni/AC催化臭氧化进行反应动力学研究,结合试验数据展开了两种催化剂催化臭氧化的对比研究。
Cu/AC和Ni/AC的XRD、SEM、BET及AAS表征结果显示:Cu/AC和Ni/AC中铜和镍几乎完全分别以CuO和NiO的棒状形式存于催化剂表面,且催化剂表面形貌发生了显著变化。与AC相比,Cu/AC的比表面积、微孔表面积及微孔体积分别减少了50.7%、62.9%、62.4%;Ni/AC则分别减少了47.9%、60.6%、60.7%,催化剂的平均孔径比AC略有增大。
在O_3/Cu/AC和O_3/Ni/AC氧化系统中,苯酚和草酸去除效果与催化剂投加量呈正相关关系,这主要是由于催化剂投加量的增多,引起臭氧分解成HO~·的效率和产量提高,最终增强了系统氧化能力;碱性条件下苯酚和草酸去除率明显高于酸性范围,这主要是由于臭氧的分解强烈受到溶液pH值的影响,它在碱性条件下主要分解生成HO~·。
叔丁醇试验表明O_3和O_3/AC过程主要是分子臭氧和活性炭吸附,O_3/Cu/AC和O_3/Ni/AC对苯酚和草酸的降解反应遵循HO~·机理,催化剂促进臭氧分解成一定量的HO~·。活性炭表面的碱性基团和弱碱性的金属氧化物使得催化臭氧化反应最终pH值比臭氧氧化略高。催化臭氧化过程中Cu~(2+)和Ni~(2+)析出浓度很小且析出率不到0.5%,这表明Cu/AC和Ni/AC在反应中稳定性较高且易于回收利用,反应为非均相催化臭氧化反应。
反应动力学及叔丁醇试验结果表明,O_3/Cu/AC比O_3/Ni/AC反应速率常数小,Ni/AC促进臭氧分解产生的HO~·比Cu/AC略多。催化作用的差别主要是单位质量的Ni/AC中金属负载量比Cu/AC多0.56mol·L~(-1),Ni/AC比表面积比Cu/AC大5%。O_3/Ni/AC体系中反应活性中心增多,且Ni/AC与臭氧接触面积增大,碰撞机会增多,臭氧分解成HO~·的生成量增大。
In this study, copper and nickel loaded activated carbon catalysts (termed Cu/AC and Ni/AC) which were prepared under low temperature were characterized in various forms, followed by studies of application in the ozonation of phenol and oxalic acid. The effects of catalyst dosage, initial pH, concentration of tert-butanol and catalyst recycling in the catalytic ozonation were studied; degradation and reaction mechanism of heterogeneous catalytic ozonation of phenol and oxalic acid were further investigaed. The kinetics studies of O_3/Cu/AC, O_3/Ni/AC and the comparison study of two catalysts in catalytic ozonation were carried out by kinetic theory and experimental data.
The XRD, SEM, BET and AAS characterization results of Cu/AC and Ni/AC showed that copper and nickel almost entirely in the form of rod-like structered CuO and NiO respectively loaded on the surface of Cu/AC and Ni/AC and both catalysts’surface morphologies were significantly changed. Compared with AC, the surface area, micropore surface area and pore volume of Cu/AC decreased by 50.7%, 62.9%, 62.4%; that of Ni/AC decreased by 47.9%, 60.6%, 60.7% and the average poresize of two catalysts slightly larger than that of AC.
In O_3/Cu/AC and O_3/Ni/AC oxidation system, the removals of phenol and oxalic acid were positively correlated with catalyst dosage, which was mainly due to the increase of catalyst dosage leads to higher ozone decomposition efficiency and finally enhanced the oxidation capacity of system; the removals of phenol and oxalic acid under alkaline condition significantly higher than that of acid one, which is because the decompositon of ozone strongly influenced by the pH value of solution and ozone was mainly decomposed into HO~·in alkaline condition.
The tert-butanol experiments showed that the processes of ozonation and O_3/AC mainly contained molecular ozone and activated carbon adsorption. The degradation of phenol and oxalic acid in O_3/Cu/AC and O_3/Ni/AC reactions follows the HO~·mechanism and catalysts promoted ozone decomposed into a certain amount of HO~·. The basic groups in activated carbon surface and the weak alkaline of metal oxides in Cu/AC and Ni/AC aroused the final pH values in catalytic ozonation slightly higher than that of ozonation. The leached Cu~(2+) and Ni~(2+) concentration in catalytic ozonation processes were very limited and the leaching rates were less than 0.5%, which indicating that Cu/AC and Ni/AC has high stability, easy to be recycled and the two catalytic reactions were heterogeneous catalytic ozonation.
Kinetic studies and tert-butanol experiments showed that the rate constant of O_3/Cu/AC is smaller than that of O_3/Ni/AC and Ni/AC promoted ozone decomposed into more HO~·than Cu/AC. The catalytic effect difference of Ni/AC and Cu/AC is mainly because the unit molar metal conccentration in Ni/AC is 0.56mol·L~(-1) larger than that of in Cu/AC and the BET of Ni/AC is 5% larger than Cu/AC. Therefore the reaction centers, exposure area and the collision of Ni/AC with ozone increased in O_3/Ni/AC system and the possibility and concentration of ozone decomposition into HO~·increased.
Cu/AC和Ni/AC的XRD、SEM、BET及AAS表征结果显示:Cu/AC和Ni/AC中铜和镍几乎完全分别以CuO和NiO的棒状形式存于催化剂表面,且催化剂表面形貌发生了显著变化。与AC相比,Cu/AC的比表面积、微孔表面积及微孔体积分别减少了50.7%、62.9%、62.4%;Ni/AC则分别减少了47.9%、60.6%、60.7%,催化剂的平均孔径比AC略有增大。
在O_3/Cu/AC和O_3/Ni/AC氧化系统中,苯酚和草酸去除效果与催化剂投加量呈正相关关系,这主要是由于催化剂投加量的增多,引起臭氧分解成HO~·的效率和产量提高,最终增强了系统氧化能力;碱性条件下苯酚和草酸去除率明显高于酸性范围,这主要是由于臭氧的分解强烈受到溶液pH值的影响,它在碱性条件下主要分解生成HO~·。
叔丁醇试验表明O_3和O_3/AC过程主要是分子臭氧和活性炭吸附,O_3/Cu/AC和O_3/Ni/AC对苯酚和草酸的降解反应遵循HO~·机理,催化剂促进臭氧分解成一定量的HO~·。活性炭表面的碱性基团和弱碱性的金属氧化物使得催化臭氧化反应最终pH值比臭氧氧化略高。催化臭氧化过程中Cu~(2+)和Ni~(2+)析出浓度很小且析出率不到0.5%,这表明Cu/AC和Ni/AC在反应中稳定性较高且易于回收利用,反应为非均相催化臭氧化反应。
反应动力学及叔丁醇试验结果表明,O_3/Cu/AC比O_3/Ni/AC反应速率常数小,Ni/AC促进臭氧分解产生的HO~·比Cu/AC略多。催化作用的差别主要是单位质量的Ni/AC中金属负载量比Cu/AC多0.56mol·L~(-1),Ni/AC比表面积比Cu/AC大5%。O_3/Ni/AC体系中反应活性中心增多,且Ni/AC与臭氧接触面积增大,碰撞机会增多,臭氧分解成HO~·的生成量增大。
In this study, copper and nickel loaded activated carbon catalysts (termed Cu/AC and Ni/AC) which were prepared under low temperature were characterized in various forms, followed by studies of application in the ozonation of phenol and oxalic acid. The effects of catalyst dosage, initial pH, concentration of tert-butanol and catalyst recycling in the catalytic ozonation were studied; degradation and reaction mechanism of heterogeneous catalytic ozonation of phenol and oxalic acid were further investigaed. The kinetics studies of O_3/Cu/AC, O_3/Ni/AC and the comparison study of two catalysts in catalytic ozonation were carried out by kinetic theory and experimental data.
The XRD, SEM, BET and AAS characterization results of Cu/AC and Ni/AC showed that copper and nickel almost entirely in the form of rod-like structered CuO and NiO respectively loaded on the surface of Cu/AC and Ni/AC and both catalysts’surface morphologies were significantly changed. Compared with AC, the surface area, micropore surface area and pore volume of Cu/AC decreased by 50.7%, 62.9%, 62.4%; that of Ni/AC decreased by 47.9%, 60.6%, 60.7% and the average poresize of two catalysts slightly larger than that of AC.
In O_3/Cu/AC and O_3/Ni/AC oxidation system, the removals of phenol and oxalic acid were positively correlated with catalyst dosage, which was mainly due to the increase of catalyst dosage leads to higher ozone decomposition efficiency and finally enhanced the oxidation capacity of system; the removals of phenol and oxalic acid under alkaline condition significantly higher than that of acid one, which is because the decompositon of ozone strongly influenced by the pH value of solution and ozone was mainly decomposed into HO~·in alkaline condition.
The tert-butanol experiments showed that the processes of ozonation and O_3/AC mainly contained molecular ozone and activated carbon adsorption. The degradation of phenol and oxalic acid in O_3/Cu/AC and O_3/Ni/AC reactions follows the HO~·mechanism and catalysts promoted ozone decomposed into a certain amount of HO~·. The basic groups in activated carbon surface and the weak alkaline of metal oxides in Cu/AC and Ni/AC aroused the final pH values in catalytic ozonation slightly higher than that of ozonation. The leached Cu~(2+) and Ni~(2+) concentration in catalytic ozonation processes were very limited and the leaching rates were less than 0.5%, which indicating that Cu/AC and Ni/AC has high stability, easy to be recycled and the two catalytic reactions were heterogeneous catalytic ozonation.
Kinetic studies and tert-butanol experiments showed that the rate constant of O_3/Cu/AC is smaller than that of O_3/Ni/AC and Ni/AC promoted ozone decomposed into more HO~·than Cu/AC. The catalytic effect difference of Ni/AC and Cu/AC is mainly because the unit molar metal conccentration in Ni/AC is 0.56mol·L~(-1) larger than that of in Cu/AC and the BET of Ni/AC is 5% larger than Cu/AC. Therefore the reaction centers, exposure area and the collision of Ni/AC with ozone increased in O_3/Ni/AC system and the possibility and concentration of ozone decomposition into HO~·increased.
引文
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