室温芬顿试剂高级氧化技术条件选择及效果评价研究
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摘要
人类活动的不断增加、环境资源的不断改变,导致各类排放污水的复杂性不断增加,废水对环境所造成的影响也日益严重,与当前提倡的节能减排,建设资源节约型、环境友好型的人与自然和谐发展的社会理念相悖。Fenton试剂作为具有独特优势的一种高级氧化技术,近年来成为环境科学与工程领域的研究热点,也广泛地应用于各类废水处理实践中。但在实际的工程实践中,芬顿试剂的链反应的进行受到一系列因素的影响,导致存在着建设和运行成本较高或处理效率低等问题。因此系统分析这些影响因素及影响程度的大小,对芬顿试剂在工程实践中的应用有着重要的指导意义。
Fenton法处理含有羟基有机化合物的废水时存在明显的选择性。羟基取代基类型、羟基数量、羟基取代位置、主链链长及主链的饱和度对Fenton法处理效果均存在不同程度的影响。实验结果表明:一元酚羟基对Fenton反应有着促进作用,而一元醇羟基对其有强烈的抑制作用;当碳原子数相同而羟基数不同时,随羟基数量的增加其对Fenton反应的影响逐渐下降;饱和一元醇主链碳原子个数越多,则其对Fenton反应的抑制作用越明显;主链的不饱和度对Fenton反应的影响也是不同的,脂肪族不饱和羟基化合物的Fenton法处理效果很差,而对苯环类羟基化合物有着很好的氧化处理效果;链长与醇羟基个数都不同时,随主链的增长和羟基数量的增加,其对Fenton反应的抑制作用随之下降,表现出良好的氧化降解效果。
影响Fenton反应过程H_2O_2分解及其有效利用率的因素有很多,其中[Fe~(2+)]要求控制在3mmol/L以上。酚类体系H_2O_2的有效利用率不仅受H_2O_2浓度变化的影响,且受初始COD_(Cr)的影响。一般表现为随COD_(Cr)的增加,H_2O_2有效利用率迅速增加,当初始COD_(Cr)一定时,H_2O_2浓度在600和1800mg/L时,一元酚与二元酚体系的H_2O_2有效利用率均出现了两个峰值,前者的峰值分别为11.83和12.99gCOD_(Cr)/gH_2O_2,后者的峰值分别为9.01和11.95gCOD_(Cr)/gH_2O_2。而醇类体系H_2O_2的有效利用率受H_2O_2浓度的影响较大,但与初始COD_(Cr)的关系不明显。当H_2O_2浓度低于300mg/L时,乙醇比对照体系H_2O_2的分解率高1-3%,而有效利用率仅为0.6gCOD_(Cr)/gH_2O_2;随H_2O_2用量的继续增加,其有效利用率趋于0gCOD_(Cr)/gH_2O_2。而二元醇体系H_2O_2有效利用率与其浓度间呈“倒U”型规律,H_2O_2低于300mg/L时,其有效利用率仅为1.25gCOD_(Cr)/gH_2O_2;H_2O_2浓度在300-900mg/L之间时,其有效利用率可达8.96gCOD_(Cr)/gH_2O_2;其后随着H_2O_2的增加,有效利用率迅速下降到与乙醇体系相当。在混合体系中,醇羟基和酚羟基所占比例对H_2O_2有效利用率也有显著的影响,当乙醇比例小于60%时,H_2O_2有效利用率稳定在13.0gCOD_(Cr)/gH_2O_2;随乙醇比例的增加,其对H_2O_2的分解抑制效应表现出剂量依赖关系,H_2O_2有效利用率也逐渐下降到近于0gCOD_(Cr)/gH_2O_2,说明这部分H_2O_2并没有得以有效地分解用于氧化废水中的COD_(Cr),这在工程实践中应引起高度的重视。
芬顿氧化技术的选择性体现在不同体系中羟基自由基的不同产生量上。亚甲基蓝分光光度法测得的ΔA可直接反映出不同体系中产生的不同羟基自由基的量,而ΔA越大,羟基的生成量越大。氧化效果差的一元饱和醇(乙醇体系中),相同实验条件下其ΔA_(乙醇)仅为0.020,远远小于ΔA_(丙三醇)(1.000)、ΔA_(聚乙烯醇)(1.190)及ΔA_(苯酚)(1.200),ΔA_(丙三醇)又稍小于ΔA_(聚乙烯醇)及ΔA_(苯酚),因此我们可以明确判断出乙醇对羟基生成的抑制作用,亚甲基蓝分光光度法测定不同体系中的羟基自由基产生量可用来直接判断底物对芬顿试剂的抑制效应及抑制程度。脉冲式加温对室温下芬顿试剂的氧化效果有着促进作用,且加热频率越大,效果越明显。
The complexity of waste water is increasing and its harming to the environment is more and more serious because of the increasing of human activity and the ceaseless change of the environment resources,these object to the ideas of energy saving and emission reduction,environment amicably society and resources economizing society. The Fenton reagent is a unique superiority oxidation technology of kinds of advanced oxidation processes which is used in treating waste water widely and is a hot spot in environmental science and project research.But in the practice,there are high cost and low efficency in present processes because of the influencing of some factors to the Fenton reagent.So we need to analyse these factors and their influencing extents systematically which can do great benefit to the practice.
Fenton reagent was selective to the organic compounds with different kinds of hydroxyl such as the hydroxyl type,hydroxyl quantity,the hydroxyl position,the length of the chain and the chain's saturation.The experimental results indicated some concludes:the monohydric phenol hydroxyl can promote the Fenton reaction,but the monohydroxy-alcohol hydroxyl suppress it fiercely;when the hydroxy compounds had the same carbon but the hydroxy quantity,their effects wound unincreased as the hydroxy quantity increasing;to the saturated monohydroxy-alcohol,the suppression became more and more obviously while the carbons of the chain were increasing;the effects of the chain's unsaturation on Fenton reaction were different:the oxidized effects were very well for the hydroxyl compounds with the phenyl but the acyclic unsaturated compounds;when the length of the chain and the hydroxyl quantity were increasing,the suppression descended and the oxidized effects were well.
The free radical chain reaction in the Fenton reaction is influenced by many factors,[Fe2+] is required to control in 3mmol/L.In the phenol's system,the availably utilized ratios of H_2O_2 were not only influenced by its concentration but also the COD_(Cr) of this system.Generally,with the increasing of the COD_(Cr), the availably utilized ratios H_2O_2 were increasing.When the COD_(Cr) was constant and the concentration of H_2O_2 was from 600 to 1800mg/L,there were two peaks of H_2O_2’s availably utilized ratios in one phenol and dual phenol's systems respectively,the former peaks were 11.83 and 12.99gCOD_(Cr)/gH_2O_2,the latter peaks were 9.01 and 11.95gCOD_(Cr)/gH_2O_2.In the alcohol’s system,the availably utilized ratios of H_2O_2 were influenced by the concentration of H_2O_2 obviously,but not the system’s COD_(Cr).When the concentration of H_2O_2 was less than 300mg/L, the decomposition rate of H_2O_2 was higher by 1-3 percent in the ethanol than the control system,and the availably utilized ratios were only 0.6gCOD_(Cr)/gH_2O_2;with the increasing of H_2O_2,its availably utilized ratios tended to 0gCOD_(Cr)/gH_2O_2.In the system of 1,3 propanediol,the availably utilized ratios of H_2O_2 displayed a "inverted U",with its concentration increasing,when the concentration of H_2O_2 was less than 300mg/L,its availably utilized ratios were only 1.25gCOD_(Cr)/gH_2O_2; but the availably utilized ratios H_2O_2 could be up to 8.96gCOD_(Cr)/gH_2O_2 when the concentration H_2O_2 is 300-900mg/L,later it fell rapidly to the level of ethanol.In the mixed system,the availably utilized ratios of H_2O_2 was also influenced obiviously by the proportion of phenol and alcohol,when the proportion of ethanol was less than 60%,the H_2O_2’s availably utilized ratios stabilized in 13.0gCOD_(Cr)/gH_2O_2;and when its proportion surpassed 60%,it displayed the dosage dependent inhibitory action and the H_2O_2’s availably utilized ratios also tended to near 0gCOD_(Cr)/gH_2O_2,it was confirmed that this part of H_2O_2 could’t be decomposited effectivly for the oxidizition of COD_(Cr),consequently,we must pay more attention to it in engineering.
The selection of Fenton was expressed by the different hydroxyl radical quantity,and the hydroxyl radical quantity can be obtained by theΔA which was detected in the method based on its reaction with thiazine.the bigger was theΔA,the more was the hydroxyl radical quantity.Under the same experimental condition,ΔAethanol <<ΔA_(glycerol),ΔA_(polyvinyl alcohol_,ΔA_(phenol) andΔA_(glycerol) <ΔA_(polyvinyl alcohol),ΔA_(phenol).We can conclude that ethanol suppressed the oxidation of Fenton fiercely.So the thiazine spectrophotometric analysis can be used as an effective method which estimates the suppression and the extent of suppression of different organic compands.
The pulse warming can promote the oxidation effect of Fenton at room temperature,and the more increasing was the frequency,the more obvious was the promotion.
Fenton法处理含有羟基有机化合物的废水时存在明显的选择性。羟基取代基类型、羟基数量、羟基取代位置、主链链长及主链的饱和度对Fenton法处理效果均存在不同程度的影响。实验结果表明:一元酚羟基对Fenton反应有着促进作用,而一元醇羟基对其有强烈的抑制作用;当碳原子数相同而羟基数不同时,随羟基数量的增加其对Fenton反应的影响逐渐下降;饱和一元醇主链碳原子个数越多,则其对Fenton反应的抑制作用越明显;主链的不饱和度对Fenton反应的影响也是不同的,脂肪族不饱和羟基化合物的Fenton法处理效果很差,而对苯环类羟基化合物有着很好的氧化处理效果;链长与醇羟基个数都不同时,随主链的增长和羟基数量的增加,其对Fenton反应的抑制作用随之下降,表现出良好的氧化降解效果。
影响Fenton反应过程H_2O_2分解及其有效利用率的因素有很多,其中[Fe~(2+)]要求控制在3mmol/L以上。酚类体系H_2O_2的有效利用率不仅受H_2O_2浓度变化的影响,且受初始COD_(Cr)的影响。一般表现为随COD_(Cr)的增加,H_2O_2有效利用率迅速增加,当初始COD_(Cr)一定时,H_2O_2浓度在600和1800mg/L时,一元酚与二元酚体系的H_2O_2有效利用率均出现了两个峰值,前者的峰值分别为11.83和12.99gCOD_(Cr)/gH_2O_2,后者的峰值分别为9.01和11.95gCOD_(Cr)/gH_2O_2。而醇类体系H_2O_2的有效利用率受H_2O_2浓度的影响较大,但与初始COD_(Cr)的关系不明显。当H_2O_2浓度低于300mg/L时,乙醇比对照体系H_2O_2的分解率高1-3%,而有效利用率仅为0.6gCOD_(Cr)/gH_2O_2;随H_2O_2用量的继续增加,其有效利用率趋于0gCOD_(Cr)/gH_2O_2。而二元醇体系H_2O_2有效利用率与其浓度间呈“倒U”型规律,H_2O_2低于300mg/L时,其有效利用率仅为1.25gCOD_(Cr)/gH_2O_2;H_2O_2浓度在300-900mg/L之间时,其有效利用率可达8.96gCOD_(Cr)/gH_2O_2;其后随着H_2O_2的增加,有效利用率迅速下降到与乙醇体系相当。在混合体系中,醇羟基和酚羟基所占比例对H_2O_2有效利用率也有显著的影响,当乙醇比例小于60%时,H_2O_2有效利用率稳定在13.0gCOD_(Cr)/gH_2O_2;随乙醇比例的增加,其对H_2O_2的分解抑制效应表现出剂量依赖关系,H_2O_2有效利用率也逐渐下降到近于0gCOD_(Cr)/gH_2O_2,说明这部分H_2O_2并没有得以有效地分解用于氧化废水中的COD_(Cr),这在工程实践中应引起高度的重视。
芬顿氧化技术的选择性体现在不同体系中羟基自由基的不同产生量上。亚甲基蓝分光光度法测得的ΔA可直接反映出不同体系中产生的不同羟基自由基的量,而ΔA越大,羟基的生成量越大。氧化效果差的一元饱和醇(乙醇体系中),相同实验条件下其ΔA_(乙醇)仅为0.020,远远小于ΔA_(丙三醇)(1.000)、ΔA_(聚乙烯醇)(1.190)及ΔA_(苯酚)(1.200),ΔA_(丙三醇)又稍小于ΔA_(聚乙烯醇)及ΔA_(苯酚),因此我们可以明确判断出乙醇对羟基生成的抑制作用,亚甲基蓝分光光度法测定不同体系中的羟基自由基产生量可用来直接判断底物对芬顿试剂的抑制效应及抑制程度。脉冲式加温对室温下芬顿试剂的氧化效果有着促进作用,且加热频率越大,效果越明显。
The complexity of waste water is increasing and its harming to the environment is more and more serious because of the increasing of human activity and the ceaseless change of the environment resources,these object to the ideas of energy saving and emission reduction,environment amicably society and resources economizing society. The Fenton reagent is a unique superiority oxidation technology of kinds of advanced oxidation processes which is used in treating waste water widely and is a hot spot in environmental science and project research.But in the practice,there are high cost and low efficency in present processes because of the influencing of some factors to the Fenton reagent.So we need to analyse these factors and their influencing extents systematically which can do great benefit to the practice.
Fenton reagent was selective to the organic compounds with different kinds of hydroxyl such as the hydroxyl type,hydroxyl quantity,the hydroxyl position,the length of the chain and the chain's saturation.The experimental results indicated some concludes:the monohydric phenol hydroxyl can promote the Fenton reaction,but the monohydroxy-alcohol hydroxyl suppress it fiercely;when the hydroxy compounds had the same carbon but the hydroxy quantity,their effects wound unincreased as the hydroxy quantity increasing;to the saturated monohydroxy-alcohol,the suppression became more and more obviously while the carbons of the chain were increasing;the effects of the chain's unsaturation on Fenton reaction were different:the oxidized effects were very well for the hydroxyl compounds with the phenyl but the acyclic unsaturated compounds;when the length of the chain and the hydroxyl quantity were increasing,the suppression descended and the oxidized effects were well.
The free radical chain reaction in the Fenton reaction is influenced by many factors,[Fe2+] is required to control in 3mmol/L.In the phenol's system,the availably utilized ratios of H_2O_2 were not only influenced by its concentration but also the COD_(Cr) of this system.Generally,with the increasing of the COD_(Cr), the availably utilized ratios H_2O_2 were increasing.When the COD_(Cr) was constant and the concentration of H_2O_2 was from 600 to 1800mg/L,there were two peaks of H_2O_2’s availably utilized ratios in one phenol and dual phenol's systems respectively,the former peaks were 11.83 and 12.99gCOD_(Cr)/gH_2O_2,the latter peaks were 9.01 and 11.95gCOD_(Cr)/gH_2O_2.In the alcohol’s system,the availably utilized ratios of H_2O_2 were influenced by the concentration of H_2O_2 obviously,but not the system’s COD_(Cr).When the concentration of H_2O_2 was less than 300mg/L, the decomposition rate of H_2O_2 was higher by 1-3 percent in the ethanol than the control system,and the availably utilized ratios were only 0.6gCOD_(Cr)/gH_2O_2;with the increasing of H_2O_2,its availably utilized ratios tended to 0gCOD_(Cr)/gH_2O_2.In the system of 1,3 propanediol,the availably utilized ratios of H_2O_2 displayed a "inverted U",with its concentration increasing,when the concentration of H_2O_2 was less than 300mg/L,its availably utilized ratios were only 1.25gCOD_(Cr)/gH_2O_2; but the availably utilized ratios H_2O_2 could be up to 8.96gCOD_(Cr)/gH_2O_2 when the concentration H_2O_2 is 300-900mg/L,later it fell rapidly to the level of ethanol.In the mixed system,the availably utilized ratios of H_2O_2 was also influenced obiviously by the proportion of phenol and alcohol,when the proportion of ethanol was less than 60%,the H_2O_2’s availably utilized ratios stabilized in 13.0gCOD_(Cr)/gH_2O_2;and when its proportion surpassed 60%,it displayed the dosage dependent inhibitory action and the H_2O_2’s availably utilized ratios also tended to near 0gCOD_(Cr)/gH_2O_2,it was confirmed that this part of H_2O_2 could’t be decomposited effectivly for the oxidizition of COD_(Cr),consequently,we must pay more attention to it in engineering.
The selection of Fenton was expressed by the different hydroxyl radical quantity,and the hydroxyl radical quantity can be obtained by theΔA which was detected in the method based on its reaction with thiazine.the bigger was theΔA,the more was the hydroxyl radical quantity.Under the same experimental condition,ΔAethanol <<ΔA_(glycerol),ΔA_(polyvinyl alcohol_,ΔA_(phenol) andΔA_(glycerol) <ΔA_(polyvinyl alcohol),ΔA_(phenol).We can conclude that ethanol suppressed the oxidation of Fenton fiercely.So the thiazine spectrophotometric analysis can be used as an effective method which estimates the suppression and the extent of suppression of different organic compands.
The pulse warming can promote the oxidation effect of Fenton at room temperature,and the more increasing was the frequency,the more obvious was the promotion.
引文
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