类Fenton高级氧化技术处理染料废水的研究
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摘要
随着染料工业的迅速发展,染料废水成为环境问题中的一个重要课题。为了有效地降解染料废水中的有机污染物,本文利用Fenton反应对染料废水进行降解。Fenton氧化技术是现在水处理中重要的高级氧化技术,可以降解水中大多数有毒有害物质。本文利用孔雀石绿和罗丹明B两种染料为研究对象进行Fenton反应,得出一些创新性的结论：(1)首先利用Salen配体与铁离子形成铁配体络合物,用它作为Fenton反应的催化剂进行Fenton反应处理染料废水,而且配体加入量为铁离子十分之一时,达到较好的脱色率：(2)首次采用固体废料石墨尾矿作为多相Fenton反应的催化剂对染料废水进行脱色降解；(3)对铁配体Fenton反应对染料废水的脱色动力学进行了研究,得出动力学方程和动力学参数；
在铁配体Fenton反应研究中,用四种不同的处理方法对孔雀石绿和罗丹明B的脱色效果进行比较,可以得出不同处理方法对孔雀石绿和罗丹明B分子的去除率的大小顺序为：铁配体Fenton反应>Fe3+/H2O2反应体系>双氧水单独氧化>铁配体单独作用。通过实验得出铁配体降解孔雀石绿溶液的反应条件,在孔雀石绿初始浓度为100mg/L的溶液中,铁配体加入量为35μmol/L,双氧水加入量为10mmol/L, Salen配体与铁离子摩尔比值采用1：10,反应温度为20℃,得出的去除率为97.95%；铁配体降解罗丹明B溶液的反应条件,在罗丹明B初始浓度为100mg/L的溶液中,铁配体加入量为40μmol/L,双氧水加入量为15mmol/L, Salen配体与铁离子摩尔比值采用1：10,反应温度为20℃,得出的脱色率率为98.06%。
对孔雀石绿和罗丹明B不同降解方法和不同影响因素对铁配体Fenton反应的动力学进行了研究,各反应均符合假一级反应动力学。铁配体Fenton反应中活性氧化物种分析得出,反应中存在羟基自由基和中间价态铁物种两种活性氧化物种。孔雀石绿和罗丹明B在铁配体Fenton反应中TOC去除率分别为54.35%和58.39%,孔雀石绿和罗丹明B没有完全降解,通过GC-MS产物分析得出,孔雀石绿的可能的降解产物为N,N-二甲基甲酰胺,戊二醛,3-羟甲基戊二醛,3-二苯甲叉基-戊二醛,3-二苯羟甲基-戊二醛,甲酸和2-烯戊二酸；罗丹明B可能的降解产物为乙二胺,戊二醛,3-羟甲基戊二醛,3-二苯甲叉基-戊二醛,3-二苯羟甲基-戊二醛,甲酸和2-烯戊二酸。对孔雀石绿和罗丹明B的铁配体Fenton反应的反应活化能进行计算表明,铁配体Fenton反应中的活化能低于Fe3+/H2O2反应体系,铁配体能有效的提高Fenton反应速率,是一种有效的催化剂。
通过对石墨尾矿XRD、EDS和比表面积表征分析得出,石墨尾矿中含有铁的氧化物可以作为Fenton反应催化剂,石墨尾矿具有的孔洞结构对染料分子具有一定的吸附性能。
相同反应条件下,石墨尾矿多相Fenton反应对孔雀石绿和罗丹明B脱色效果优于石墨尾矿单独吸附作用和双氧水单独氧化作用。由实验得出孔雀石绿石墨尾矿多相Fenton反应的反应条件为：孔雀石绿初始浓度为100mg/L时,石墨尾矿投加量为5g/L,双氧水投加量为4g/L时石墨尾矿多相Fenton反应对孔雀石绿的最大脱色率为99.51%。罗丹明B石墨尾矿多相Fenton反应的反应条件为,罗丹明B初始浓度为100mg/L时,石墨尾矿投加量为50g/L,双氧水投加量为10g/L时脱色率为93.39%。
对石墨尾矿多相Fenton反应降解孔雀石绿和罗丹明B的机理进行研究表明,石墨尾矿多相Fenton反应中存在Fenton反应和吸附作用两种作用。石墨尾矿多相Fenton反应对孔雀石绿和罗丹明B的TOC去除率分别为60.38%和49.02%。孔雀石绿和罗丹明B溶液石墨尾矿多相Fenton反应后,溶液中的铁离子浸出量为0.2309mg/L和0.4824mg/L,溶液中含有的铁离子量达到国家《污水综合排放标准》(GB8978-1996),石墨尾矿是铁离子较好的载体。通过对溶液中铁离子浸出量的分析,推导出石墨尾矿多相Fenton反应可能的反应路径。
With the development of dye industry, the dye wastewater has become one of the important fields in the enrironmental problems. In order to make the dye wastewater have higher degradation and supply an effective treatment method, the Fenton reaction on the degradation of dye wastewater was studied. The Fenton reaction whicn can decompose most organics was an important advaced oxidation technology in water treatment. However, it still has many shortcomings. In order to improve the efficiency of Fenton reaction, improvement was studied on the degradation of malachite green and rhodamine B. The optimum condition and the mechanism of [Fe(Ⅲ)-salen]Cl complex Fenton reaction and the graphite tailing Fenton reaction were investigated.
The different treatment on malachite green and rhodamine B was compared. The decolorization order of the methods was [Fe(Ⅲ)-salen]Cl complex Fenton reaction> Fe3+/H2O2system> H2O2alone>[Fe(Ⅲ)-salen]Cl complex alone.
The optimum condition of malachite green degradation in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was that:the concentration of the [Fe(Ⅲ)-salen]Cl complex was35μmol/L, the concentration of H2O2was10mmol/L, the molar ratio of Fe(Ⅲ) to salen ligand was1:10, the initial concentration of malachite green was100mg/L and the reaction temperature was20℃. The decolorization of malachite green under the optimum condition was97.95%. The optimum condition of rhodamine B degradation in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was that:the concentration of the [Fe(Ⅲ)-salen]Cl complex was40μmol/L,the concentration of H2O2was15mmol/L, the molar ratio of Fe(Ⅲ) to salen ligand was1:10, the initial concentration of rhodamine B was100mg/L and the reaction temperature was20℃. The decolorization of rhodamine B under the optimum condition was97.95%.
The pseudo-first order reaction kinetics in different treatment was compared and they all obeyed pseudo-first order equation. The hydroxyl radical and the Fe(Ⅳ) species were the active oxidation species. The TOC removal rate of malachite grren and rhodamine B in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was54.35%and58.39%. According to the GC-MS analyse, the possible degradation intermediates of malachite green were dimethylform amide, glutaraldehyde,3-(hydroxymethyl) pentanedial,3-(diphenylmethylene) pentanedial,3-(hydroxydiphenylmethyl) pentanedial, formic acid and (2)-pent-2-enedioic acid. The possible degradation intermediates of rhodamine B were ethanediamine, glutaraldehyde,3-(hydroxymethyl) pentanedial,3-(diphenylmethylene) pentanedial,3-(hydroxydiphenylmethyl) pentanedial, formic acid and (2)-pent-2-enedioic acid. The pseudo-activated energy of malachite green and rhodamine B was calculated by the related kinetic constants.
The GT used in this study was characterized by X-ray diffraction (XRD), Energy dispersive spectrometry (EDS) and Brunauer-Emmett-Teller (BET) method. The mesoporous structure of the GT made it as an absorbent and the encapsulated Fe2O3in GT was able to initiate the Fenton reaction.
The decolorization in graphite taling Fenton-like reaction was much higher than in graphite tailing adsorption and the hydroxyl peroxide alone. The optimum condition of malachite green degradation in graphite taling Fenton-like reaction was that:the initial concentration of malachite green was100mg/L, the concentration of H2O2and graphite tailing was4g/L and5g/L. The decolorization of malachite green under the optimum condition was99.51%. The optimum condition of rhodamine B degradation in graphite taling Fenton-like reaction was that:the initial concentration of rhodamine B was100mg/L, the concentration of H2O2and graphite tailing was10g/L and50g/L. The decolorization of malachite green under the optimum condition was93.39%.
According to the mechanism of degradation of malachite green and rhodamine B in graphite tailing Fenton-like process, the graphite has the adsoption and Fenton reaction. The reaction solution has the active oxidation speciey-hydroxyl radical. The TOC remevol rate of Malachite Green and Rhodamine B was60.38%and49.02%. The malachite green and rhodamine B molecules were not mineralized completely and they were oxidized to low melocule organics.
After the degradation of malachite green and rhodamine B in the graphite tailing Fenton-like process, the iron ion leaching was detected. Depending on the results of Atomic Absorption Spectrophotometer, the concentration of the iron ions in malachite geen and rhodamine B solution was about0.2309mg/L and0.4824mg/L and the release of the iron ions from GT to the solution could be ignored. So it can be concluded that the Fenton oxidation process is mainly due to the heterogeneous effect of the catalyst and not to the leaching of iron ions.The leached iron ions in the solution can be discharged accodingto the standard of the watswater discharge in our country. The possible degradation process was that the encapsulated Fe2O3in GT was the Fenton reaction site of the catalyst. And the heterogeneous Fenton reaction process may be that the malachite green and rhodamine B molecules in the solution contacted with encapsulated Fe2O3in GT, were oxidized first by H2O2. With the movement of malachite green and rhodamine B molecules, other molecules touched the catalysis center again and they are degraded at the first.
在铁配体Fenton反应研究中,用四种不同的处理方法对孔雀石绿和罗丹明B的脱色效果进行比较,可以得出不同处理方法对孔雀石绿和罗丹明B分子的去除率的大小顺序为：铁配体Fenton反应>Fe3+/H2O2反应体系>双氧水单独氧化>铁配体单独作用。通过实验得出铁配体降解孔雀石绿溶液的反应条件,在孔雀石绿初始浓度为100mg/L的溶液中,铁配体加入量为35μmol/L,双氧水加入量为10mmol/L, Salen配体与铁离子摩尔比值采用1：10,反应温度为20℃,得出的去除率为97.95%；铁配体降解罗丹明B溶液的反应条件,在罗丹明B初始浓度为100mg/L的溶液中,铁配体加入量为40μmol/L,双氧水加入量为15mmol/L, Salen配体与铁离子摩尔比值采用1：10,反应温度为20℃,得出的脱色率率为98.06%。
对孔雀石绿和罗丹明B不同降解方法和不同影响因素对铁配体Fenton反应的动力学进行了研究,各反应均符合假一级反应动力学。铁配体Fenton反应中活性氧化物种分析得出,反应中存在羟基自由基和中间价态铁物种两种活性氧化物种。孔雀石绿和罗丹明B在铁配体Fenton反应中TOC去除率分别为54.35%和58.39%,孔雀石绿和罗丹明B没有完全降解,通过GC-MS产物分析得出,孔雀石绿的可能的降解产物为N,N-二甲基甲酰胺,戊二醛,3-羟甲基戊二醛,3-二苯甲叉基-戊二醛,3-二苯羟甲基-戊二醛,甲酸和2-烯戊二酸；罗丹明B可能的降解产物为乙二胺,戊二醛,3-羟甲基戊二醛,3-二苯甲叉基-戊二醛,3-二苯羟甲基-戊二醛,甲酸和2-烯戊二酸。对孔雀石绿和罗丹明B的铁配体Fenton反应的反应活化能进行计算表明,铁配体Fenton反应中的活化能低于Fe3+/H2O2反应体系,铁配体能有效的提高Fenton反应速率,是一种有效的催化剂。
通过对石墨尾矿XRD、EDS和比表面积表征分析得出,石墨尾矿中含有铁的氧化物可以作为Fenton反应催化剂,石墨尾矿具有的孔洞结构对染料分子具有一定的吸附性能。
相同反应条件下,石墨尾矿多相Fenton反应对孔雀石绿和罗丹明B脱色效果优于石墨尾矿单独吸附作用和双氧水单独氧化作用。由实验得出孔雀石绿石墨尾矿多相Fenton反应的反应条件为：孔雀石绿初始浓度为100mg/L时,石墨尾矿投加量为5g/L,双氧水投加量为4g/L时石墨尾矿多相Fenton反应对孔雀石绿的最大脱色率为99.51%。罗丹明B石墨尾矿多相Fenton反应的反应条件为,罗丹明B初始浓度为100mg/L时,石墨尾矿投加量为50g/L,双氧水投加量为10g/L时脱色率为93.39%。
对石墨尾矿多相Fenton反应降解孔雀石绿和罗丹明B的机理进行研究表明,石墨尾矿多相Fenton反应中存在Fenton反应和吸附作用两种作用。石墨尾矿多相Fenton反应对孔雀石绿和罗丹明B的TOC去除率分别为60.38%和49.02%。孔雀石绿和罗丹明B溶液石墨尾矿多相Fenton反应后,溶液中的铁离子浸出量为0.2309mg/L和0.4824mg/L,溶液中含有的铁离子量达到国家《污水综合排放标准》(GB8978-1996),石墨尾矿是铁离子较好的载体。通过对溶液中铁离子浸出量的分析,推导出石墨尾矿多相Fenton反应可能的反应路径。
With the development of dye industry, the dye wastewater has become one of the important fields in the enrironmental problems. In order to make the dye wastewater have higher degradation and supply an effective treatment method, the Fenton reaction on the degradation of dye wastewater was studied. The Fenton reaction whicn can decompose most organics was an important advaced oxidation technology in water treatment. However, it still has many shortcomings. In order to improve the efficiency of Fenton reaction, improvement was studied on the degradation of malachite green and rhodamine B. The optimum condition and the mechanism of [Fe(Ⅲ)-salen]Cl complex Fenton reaction and the graphite tailing Fenton reaction were investigated.
The different treatment on malachite green and rhodamine B was compared. The decolorization order of the methods was [Fe(Ⅲ)-salen]Cl complex Fenton reaction> Fe3+/H2O2system> H2O2alone>[Fe(Ⅲ)-salen]Cl complex alone.
The optimum condition of malachite green degradation in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was that:the concentration of the [Fe(Ⅲ)-salen]Cl complex was35μmol/L, the concentration of H2O2was10mmol/L, the molar ratio of Fe(Ⅲ) to salen ligand was1:10, the initial concentration of malachite green was100mg/L and the reaction temperature was20℃. The decolorization of malachite green under the optimum condition was97.95%. The optimum condition of rhodamine B degradation in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was that:the concentration of the [Fe(Ⅲ)-salen]Cl complex was40μmol/L,the concentration of H2O2was15mmol/L, the molar ratio of Fe(Ⅲ) to salen ligand was1:10, the initial concentration of rhodamine B was100mg/L and the reaction temperature was20℃. The decolorization of rhodamine B under the optimum condition was97.95%.
The pseudo-first order reaction kinetics in different treatment was compared and they all obeyed pseudo-first order equation. The hydroxyl radical and the Fe(Ⅳ) species were the active oxidation species. The TOC removal rate of malachite grren and rhodamine B in [Fe(Ⅲ)-salen]Cl complex Fenton reaction was54.35%and58.39%. According to the GC-MS analyse, the possible degradation intermediates of malachite green were dimethylform amide, glutaraldehyde,3-(hydroxymethyl) pentanedial,3-(diphenylmethylene) pentanedial,3-(hydroxydiphenylmethyl) pentanedial, formic acid and (2)-pent-2-enedioic acid. The possible degradation intermediates of rhodamine B were ethanediamine, glutaraldehyde,3-(hydroxymethyl) pentanedial,3-(diphenylmethylene) pentanedial,3-(hydroxydiphenylmethyl) pentanedial, formic acid and (2)-pent-2-enedioic acid. The pseudo-activated energy of malachite green and rhodamine B was calculated by the related kinetic constants.
The GT used in this study was characterized by X-ray diffraction (XRD), Energy dispersive spectrometry (EDS) and Brunauer-Emmett-Teller (BET) method. The mesoporous structure of the GT made it as an absorbent and the encapsulated Fe2O3in GT was able to initiate the Fenton reaction.
The decolorization in graphite taling Fenton-like reaction was much higher than in graphite tailing adsorption and the hydroxyl peroxide alone. The optimum condition of malachite green degradation in graphite taling Fenton-like reaction was that:the initial concentration of malachite green was100mg/L, the concentration of H2O2and graphite tailing was4g/L and5g/L. The decolorization of malachite green under the optimum condition was99.51%. The optimum condition of rhodamine B degradation in graphite taling Fenton-like reaction was that:the initial concentration of rhodamine B was100mg/L, the concentration of H2O2and graphite tailing was10g/L and50g/L. The decolorization of malachite green under the optimum condition was93.39%.
According to the mechanism of degradation of malachite green and rhodamine B in graphite tailing Fenton-like process, the graphite has the adsoption and Fenton reaction. The reaction solution has the active oxidation speciey-hydroxyl radical. The TOC remevol rate of Malachite Green and Rhodamine B was60.38%and49.02%. The malachite green and rhodamine B molecules were not mineralized completely and they were oxidized to low melocule organics.
After the degradation of malachite green and rhodamine B in the graphite tailing Fenton-like process, the iron ion leaching was detected. Depending on the results of Atomic Absorption Spectrophotometer, the concentration of the iron ions in malachite geen and rhodamine B solution was about0.2309mg/L and0.4824mg/L and the release of the iron ions from GT to the solution could be ignored. So it can be concluded that the Fenton oxidation process is mainly due to the heterogeneous effect of the catalyst and not to the leaching of iron ions.The leached iron ions in the solution can be discharged accodingto the standard of the watswater discharge in our country. The possible degradation process was that the encapsulated Fe2O3in GT was the Fenton reaction site of the catalyst. And the heterogeneous Fenton reaction process may be that the malachite green and rhodamine B molecules in the solution contacted with encapsulated Fe2O3in GT, were oxidized first by H2O2. With the movement of malachite green and rhodamine B molecules, other molecules touched the catalysis center again and they are degraded at the first.
引文
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