纳米水合二氧化锰氧化水中典型有机污染物的效能研究
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摘要
锰元素是自然界中丰度较高的金属元素之一，它的氧化物不仅参与了自然环境中许多有机、无机成分的迁移转化，还在水质净化过程中发挥着重要作用。在水处理中，二氧化锰一般通过高锰酸盐的氧化还原原位产生，它不仅对高锰酸盐的氧化具有重要意义，自身还具有许多重要的除污染特性。磺胺和溴酚类化合物在水体中频繁检出，两类化合物与二氧化锰反应的特征官能团不同，分别为芳胺基和酚羟基。本文通过硫代硫酸钠还原高锰酸钾制得纳米水合二氧化锰（nHMO），模拟水处理中原位产生的二氧化锰，进而研究其对目标物的催化氧化特性。
本文中制得的nHMO粒径分布在24.4~91.2nm之间，能够稳定存在40天以上。不同制备浓度、温度和混合方式对产生的nHMO的粒径均有影响，从而影响它的氧化活性。对混方式制得的nHMO比滴加方式制得的nHMO平均粒径小18.41nm。当pH为7.3时，前者氧化SMZ的效率要高出后者28%。制备液浓度越低、温度越高，制得的nHMO的平均粒径越小，它的氧化活性越高。
为了考察nHMO的氧化活性，本文选取了磺胺二甲嘧啶（SMZ）、磺胺甲噻唑（SMZO）、磺胺甲噁唑（SMX）三种具有芳胺结构的药物进行研究。nHMO氧化三种磺胺的能力依次为：SMZ>SMX>SMZO。相比其它常见的二价阳离子，锰离子对nHMO的氧化抑制最明显，当pH为6.0时，5μM锰离子就使SMZ的去除率下降22%。低浓度的磷酸根对SMZ的去除率影响较小，但是腐殖酸以及高浓度的磷酸根都表现出一定的抑制作用。nHMO氧化三种有机物的动力学曲线均不符合假一级动力学，反应后期存在明显的自抑制现象。本文通过引入两个动力学参数Sr和k，分别表示二氧化锰氧化有机物的活性位点数和基于该值的反应速率常数，建立了nHMO氧化SMZ的动力学模型。该模型能够很好的拟合整个氧化过程，其中，随着SMZ初始浓度的增加，Sr值增加，k值减小；随着nHMO浓度的增加，Sr值增加，k值增加；pH值的增加导致Sr值和k值均降低。
为了研究nHMO氧化卤代酚类有机物过程中的脱卤现象，本文选取了三种溴酚进行了研究。nHMO氧化三种溴酚的能力依次为：4-溴酚（4-BrP）>2-溴酚（2-BrP）>3-溴酚（3-BrP），氧化过程中的脱溴能力也遵循相同的次序。假一级条件下，nHMO氧化4-BrP的反应速率常数随着溴酚浓度的增加保持不变，表明表面络合物的电子转移是该氧化过程中的速控步骤。nHMO氧化溴酚过程中的脱溴指数（DN）随着pH的升高而逐渐减小，表明nHMO氧化溴酚的过程不仅仅遵循有机自由基耦合的机理。氮气曝气对溴酚的氧化及溴离子的释放均有一定的抑制作用，且pH5.0时的抑制效果比pH4.0时更明显。nHMO氧化溴酚的过程中，nHMO颗粒粒径不断增大，溴酚和nHMO初始浓度越大、pH越低，颗粒粒径增大的幅度越大。氧化过程中产生的锰离子大部分吸附在二氧化锰表面，溶液中锰离子浓度很低。
鉴于nHMO的氧化活性和它的纳米粒径相关，本文还研究了nHMO氧化过程中的凝聚现象。锰离子引发的nHMO凝聚具有较低的临界浓度，在10-5M级别。随着pH值的升高，相同锰离子浓度引起的凝聚速率增大，因而引起扩散凝聚的临界浓度降低。nHMO氧化有机物过程中的凝聚速率主要取决于与有机物的反应速率，pH值升高，氧化速率降低，凝聚速率减慢。nHMO的氧化凝聚对氧化效能的影响很大，投加少量高锰酸钾可以有效控制nHMO氧化过程中的凝聚。nHMO/少量高锰酸钾组合体系氧化初始浓度为2.5~16.8μM的双酚A（BPA）时，自抑制现象消失，其假一级速率常数分别与nHMO单独氧化时初始阶段的速率常数一致，表明高锰酸钾在该体系中主要起氧化锰离子和维持nHMO纳米粒径的作用；而在氧化4-硝基酚（4-NP）时，高锰酸钾主要参与表面络合物的电子转移过程，从而强化4-NP的氧化去除，该组合体系主要表现为二氧化锰催化高锰酸钾氧化4-NP。
二氧化锰对高锰酸钾氧化除污染具有非常重要的催化作用，本文选取了双键类污染物卡马西平（CMZ）以及酚类污染物双酚A（BPA）、苯酚（Phen）、2-氯酚（2-CP）、2,4-二氯酚（2,4-DCP）、2,4,6-三氯酚（2,4,6-TCP）等目标物，研究了高锰酸钾氧化以两种有机物形成的复合污染过程中nHMO和其它中间态锰物种的重要作用。在弱酸性条件下，CMZ能够促进Phen的氧化去除而自身不受影响；酚类化合物的氧化去除则表现为互相促进，且反应慢的酚的氧化去除受到的促进更大，nHMO的催化作用是造成这些现象的主导原因。弱碱性条件下，CMZ和Phen复合时，二者的氧化去除均不受影响；酚类污染物之间复合时，表现为与高锰酸钾反应速率常数较低的酚的氧化去除受到抑制，而反应速率常数较大的酚的氧化去除受到的影响很小。竞争动力学的研究表明，这种抑制作用主要是两种酚类污染物竞争了体系中除高锰酸钾及nHMO以外的其它氧化活性物种所致。由于CMZ的氧化机制和Phen不同，二者不存在竞争作用，因而二者的共存对各自的氧化均不构成影响。
Manganese is one of the most abundant elements in the nature. Its oxide not onlyparticipates in the migration and transformation of organic and inorganic compounds inthe environment，but also plays an important role on water purification. In watertreatment processes, manganese dioxide is usually in situ generated by thepermanganate oxidation, which is significant to the oxidation. Furthermore, it alsoshows an excellent performance on the removal of pollutants. Sulfonamides andbromophenols frequently occur in natural waters whose reactive functional groupstoward manganese dioxide are aromatic amine and phenolic hydroxyl group,respectively. In this paper, nanoscale hydrous manganese dioxide (nHMO) is generatedby the reduction of permanganate by thiosulfate to mimic the in situ generated one, andthe oxidative or catalytic behaviors are investigated.
The particle size of nHMO is distributed between24.4-91.2nm, and its reactivitykeeps almost the same for40days. The preparation concentration, temperature andmixing approach can affect the particle size of nHMO, and thus change its reactivity.The average size of nHMO formed by mixing two reactants instantaneously is18.41nmsmaller than by titrating thiosulfate into permanganate. The removal efficiency of SMZat pH7.3by the former one is higher than that by the latter one by28%. Both lowpreparation concentration and high temperature facilitate the small particle size and highoxidative reactivity of nHMO.
Sulfamethazine (SMZ), sulfamethizole (SMZO) and sulfamethoxazole (SMX) areemployed to study the oxidative reactivity of nHMO. The reactivity of nHMO towardthree compounds is in the order of SMZ> SMX> SMZO. The inhibition of manganeseion on the oxidation by nHMO is more significant than other common divalent ions, sothat the removal of SMZ decreases by22%in the presence of5μM manganese ion atpH6.0. Both phosphate in high concentration and humic acid inhibit the oxidationprocess, but phosphate in low concentration has little effect on it. Oxidative kinetics ofthree compounds deviates from the pseudo first-order kinetic curve, with a plateau inthe later stage. Two kinetic parameters Srand k, which represent the number of reactivesites of nHMO and the reaction rate constant based on the reactive sites, respectively,are introduced to fit the whole oxidation curve of SMZ. Increasing the initial concentration of SMZ, the value of Srincreases, while the value of k decreases. Both thevalues of Srand k increase when increasing the initial concentration of nHMO, butdecrease when increasing the solution pH.
Three bromophenols are selected to study the dehalogenation during the reactionbetween nHMO and halophenols. Both the oxidative reactivity and debrominationcapability are in the order of4-bromophenol (4-BrP)>2-bromophenol (2-BrP)>3-bromophenol (3-BrP). The pseudo first-order rate constants are almost the same fordifferent initial concentration of4-BrP, which indicates the rate-determining step of thereaction between nHMO and4-bromophenol (4-BrP) is electron transfer of surfacecomplex. The debromination number (DN) decreases while pH increases, whichindicates there are still other pathways in addition to the mechanism of oxidativecoupling during the oxidation of bromophenols by nHMO. The reaction rate anddebromination capability decrease under nigrogen atomosphere, and the inhibition at pH5.0is larger than pH4.0. During the oxidation of4-BrP, the particle size of nHMOkeeps increasing. Both high initial concentration of the reactants and low pH facilitatethe particle growth. The concentration of manganese ion released to the solution is verylow compared with the removal of bromophenols, which indicates that most ofmanganese ion adsorbs on to the surface of manganese dioxide.
In view of the relationship between the reactivity and particle size of nHMO, theaggregation of nHMO during the oxidation has been studied. The critical coagulationconcentration of manganese ion is relatively low for aggregation of nHMO, which is inthe order of magnitude of10-5M. Higher pH leads to the higher aggregation rate andlower critical coagulation concentration. Aggregation rate induced by the oxidation oforganic compounds depends on its oxidation rate. The increase of pH decreasesoxidation rate of organic compounds, and hence decreases the aggregation rate ofnHMO. Since oxidative aggregation strongly affects the oxidation efficiency,permanganate is employed to effectively maintain the particle size of nHMO andalleviate the aggregation. When oxidizing bisphenol A (BPA) by nHMO and tracepermanganate together, the pseudo first-order rate constant is the same with that at theinitial phase of the oxidation by nHMO, which indicates that the important role ofpermanganate is to oxidize the manganese ion and keep the particle size of nHMOconstant. When oxidizing4-nitrophenol (4-NP) by the same system, the removal of4-NP is improved due to the participation of permanganate in the electron transfer of the surface complex. In this case, nHMO exhibits the catalytic capability towardspermanganate.
Because of the catalytic effect of manganese oxide on permanganate oxidation,carbamazepine (CMZ) with double bond and phenols like bisphenol A (BPA), phenol(Phen),2-chlorophenol (2-CP),2,4-dichlorophenol (2,4-DCP) and2,4,6-trichlorophenol(2,4,6-TCP) are chosen to study the role of nHMO and other reactive manganeseintermediates during the simultaneous oxidation of two pollutants by permanganate.Under weakly acidic conditions, CMZ can accelerate the oxidation of Phen while theoxidation of itself keeps unchanged. Phenols can enhance their oxidation mutually, andthe oxidation of the pollutant with a smaller reaction constant is accelerated more. Thecatalytic effect of nHMO is the main reason for the phenomena under weakly acidicconditions. Under weakly alkaline conditions, the coexistence of CMZ and Phen haslittle effect on the oxidation of each other, while the coexsitence of phenols exhibitsdifferent that the oxidation of phenolic pollutant with smaller rate constant is inhibitedbut almost unchanged for the other. The competitive kinetics shows that two phenolicpollutants may compete for a new reactive intermediate in the oxidation rather thanpermanganate and manganese dioxide. Since the mechanism of the oxidation of CMZ isdifferent with that of Phen, CMZ and Phen do not compete for the same reactiveintermediate so that oxidation of Phen is not inhibited.
本文中制得的nHMO粒径分布在24.4~91.2nm之间，能够稳定存在40天以上。不同制备浓度、温度和混合方式对产生的nHMO的粒径均有影响，从而影响它的氧化活性。对混方式制得的nHMO比滴加方式制得的nHMO平均粒径小18.41nm。当pH为7.3时，前者氧化SMZ的效率要高出后者28%。制备液浓度越低、温度越高，制得的nHMO的平均粒径越小，它的氧化活性越高。
为了考察nHMO的氧化活性，本文选取了磺胺二甲嘧啶（SMZ）、磺胺甲噻唑（SMZO）、磺胺甲噁唑（SMX）三种具有芳胺结构的药物进行研究。nHMO氧化三种磺胺的能力依次为：SMZ>SMX>SMZO。相比其它常见的二价阳离子，锰离子对nHMO的氧化抑制最明显，当pH为6.0时，5μM锰离子就使SMZ的去除率下降22%。低浓度的磷酸根对SMZ的去除率影响较小，但是腐殖酸以及高浓度的磷酸根都表现出一定的抑制作用。nHMO氧化三种有机物的动力学曲线均不符合假一级动力学，反应后期存在明显的自抑制现象。本文通过引入两个动力学参数Sr和k，分别表示二氧化锰氧化有机物的活性位点数和基于该值的反应速率常数，建立了nHMO氧化SMZ的动力学模型。该模型能够很好的拟合整个氧化过程，其中，随着SMZ初始浓度的增加，Sr值增加，k值减小；随着nHMO浓度的增加，Sr值增加，k值增加；pH值的增加导致Sr值和k值均降低。
为了研究nHMO氧化卤代酚类有机物过程中的脱卤现象，本文选取了三种溴酚进行了研究。nHMO氧化三种溴酚的能力依次为：4-溴酚（4-BrP）>2-溴酚（2-BrP）>3-溴酚（3-BrP），氧化过程中的脱溴能力也遵循相同的次序。假一级条件下，nHMO氧化4-BrP的反应速率常数随着溴酚浓度的增加保持不变，表明表面络合物的电子转移是该氧化过程中的速控步骤。nHMO氧化溴酚过程中的脱溴指数（DN）随着pH的升高而逐渐减小，表明nHMO氧化溴酚的过程不仅仅遵循有机自由基耦合的机理。氮气曝气对溴酚的氧化及溴离子的释放均有一定的抑制作用，且pH5.0时的抑制效果比pH4.0时更明显。nHMO氧化溴酚的过程中，nHMO颗粒粒径不断增大，溴酚和nHMO初始浓度越大、pH越低，颗粒粒径增大的幅度越大。氧化过程中产生的锰离子大部分吸附在二氧化锰表面，溶液中锰离子浓度很低。
鉴于nHMO的氧化活性和它的纳米粒径相关，本文还研究了nHMO氧化过程中的凝聚现象。锰离子引发的nHMO凝聚具有较低的临界浓度，在10-5M级别。随着pH值的升高，相同锰离子浓度引起的凝聚速率增大，因而引起扩散凝聚的临界浓度降低。nHMO氧化有机物过程中的凝聚速率主要取决于与有机物的反应速率，pH值升高，氧化速率降低，凝聚速率减慢。nHMO的氧化凝聚对氧化效能的影响很大，投加少量高锰酸钾可以有效控制nHMO氧化过程中的凝聚。nHMO/少量高锰酸钾组合体系氧化初始浓度为2.5~16.8μM的双酚A（BPA）时，自抑制现象消失，其假一级速率常数分别与nHMO单独氧化时初始阶段的速率常数一致，表明高锰酸钾在该体系中主要起氧化锰离子和维持nHMO纳米粒径的作用；而在氧化4-硝基酚（4-NP）时，高锰酸钾主要参与表面络合物的电子转移过程，从而强化4-NP的氧化去除，该组合体系主要表现为二氧化锰催化高锰酸钾氧化4-NP。
二氧化锰对高锰酸钾氧化除污染具有非常重要的催化作用，本文选取了双键类污染物卡马西平（CMZ）以及酚类污染物双酚A（BPA）、苯酚（Phen）、2-氯酚（2-CP）、2,4-二氯酚（2,4-DCP）、2,4,6-三氯酚（2,4,6-TCP）等目标物，研究了高锰酸钾氧化以两种有机物形成的复合污染过程中nHMO和其它中间态锰物种的重要作用。在弱酸性条件下，CMZ能够促进Phen的氧化去除而自身不受影响；酚类化合物的氧化去除则表现为互相促进，且反应慢的酚的氧化去除受到的促进更大，nHMO的催化作用是造成这些现象的主导原因。弱碱性条件下，CMZ和Phen复合时，二者的氧化去除均不受影响；酚类污染物之间复合时，表现为与高锰酸钾反应速率常数较低的酚的氧化去除受到抑制，而反应速率常数较大的酚的氧化去除受到的影响很小。竞争动力学的研究表明，这种抑制作用主要是两种酚类污染物竞争了体系中除高锰酸钾及nHMO以外的其它氧化活性物种所致。由于CMZ的氧化机制和Phen不同，二者不存在竞争作用，因而二者的共存对各自的氧化均不构成影响。
Manganese is one of the most abundant elements in the nature. Its oxide not onlyparticipates in the migration and transformation of organic and inorganic compounds inthe environment，but also plays an important role on water purification. In watertreatment processes, manganese dioxide is usually in situ generated by thepermanganate oxidation, which is significant to the oxidation. Furthermore, it alsoshows an excellent performance on the removal of pollutants. Sulfonamides andbromophenols frequently occur in natural waters whose reactive functional groupstoward manganese dioxide are aromatic amine and phenolic hydroxyl group,respectively. In this paper, nanoscale hydrous manganese dioxide (nHMO) is generatedby the reduction of permanganate by thiosulfate to mimic the in situ generated one, andthe oxidative or catalytic behaviors are investigated.
The particle size of nHMO is distributed between24.4-91.2nm, and its reactivitykeeps almost the same for40days. The preparation concentration, temperature andmixing approach can affect the particle size of nHMO, and thus change its reactivity.The average size of nHMO formed by mixing two reactants instantaneously is18.41nmsmaller than by titrating thiosulfate into permanganate. The removal efficiency of SMZat pH7.3by the former one is higher than that by the latter one by28%. Both lowpreparation concentration and high temperature facilitate the small particle size and highoxidative reactivity of nHMO.
Sulfamethazine (SMZ), sulfamethizole (SMZO) and sulfamethoxazole (SMX) areemployed to study the oxidative reactivity of nHMO. The reactivity of nHMO towardthree compounds is in the order of SMZ> SMX> SMZO. The inhibition of manganeseion on the oxidation by nHMO is more significant than other common divalent ions, sothat the removal of SMZ decreases by22%in the presence of5μM manganese ion atpH6.0. Both phosphate in high concentration and humic acid inhibit the oxidationprocess, but phosphate in low concentration has little effect on it. Oxidative kinetics ofthree compounds deviates from the pseudo first-order kinetic curve, with a plateau inthe later stage. Two kinetic parameters Srand k, which represent the number of reactivesites of nHMO and the reaction rate constant based on the reactive sites, respectively,are introduced to fit the whole oxidation curve of SMZ. Increasing the initial concentration of SMZ, the value of Srincreases, while the value of k decreases. Both thevalues of Srand k increase when increasing the initial concentration of nHMO, butdecrease when increasing the solution pH.
Three bromophenols are selected to study the dehalogenation during the reactionbetween nHMO and halophenols. Both the oxidative reactivity and debrominationcapability are in the order of4-bromophenol (4-BrP)>2-bromophenol (2-BrP)>3-bromophenol (3-BrP). The pseudo first-order rate constants are almost the same fordifferent initial concentration of4-BrP, which indicates the rate-determining step of thereaction between nHMO and4-bromophenol (4-BrP) is electron transfer of surfacecomplex. The debromination number (DN) decreases while pH increases, whichindicates there are still other pathways in addition to the mechanism of oxidativecoupling during the oxidation of bromophenols by nHMO. The reaction rate anddebromination capability decrease under nigrogen atomosphere, and the inhibition at pH5.0is larger than pH4.0. During the oxidation of4-BrP, the particle size of nHMOkeeps increasing. Both high initial concentration of the reactants and low pH facilitatethe particle growth. The concentration of manganese ion released to the solution is verylow compared with the removal of bromophenols, which indicates that most ofmanganese ion adsorbs on to the surface of manganese dioxide.
In view of the relationship between the reactivity and particle size of nHMO, theaggregation of nHMO during the oxidation has been studied. The critical coagulationconcentration of manganese ion is relatively low for aggregation of nHMO, which is inthe order of magnitude of10-5M. Higher pH leads to the higher aggregation rate andlower critical coagulation concentration. Aggregation rate induced by the oxidation oforganic compounds depends on its oxidation rate. The increase of pH decreasesoxidation rate of organic compounds, and hence decreases the aggregation rate ofnHMO. Since oxidative aggregation strongly affects the oxidation efficiency,permanganate is employed to effectively maintain the particle size of nHMO andalleviate the aggregation. When oxidizing bisphenol A (BPA) by nHMO and tracepermanganate together, the pseudo first-order rate constant is the same with that at theinitial phase of the oxidation by nHMO, which indicates that the important role ofpermanganate is to oxidize the manganese ion and keep the particle size of nHMOconstant. When oxidizing4-nitrophenol (4-NP) by the same system, the removal of4-NP is improved due to the participation of permanganate in the electron transfer of the surface complex. In this case, nHMO exhibits the catalytic capability towardspermanganate.
Because of the catalytic effect of manganese oxide on permanganate oxidation,carbamazepine (CMZ) with double bond and phenols like bisphenol A (BPA), phenol(Phen),2-chlorophenol (2-CP),2,4-dichlorophenol (2,4-DCP) and2,4,6-trichlorophenol(2,4,6-TCP) are chosen to study the role of nHMO and other reactive manganeseintermediates during the simultaneous oxidation of two pollutants by permanganate.Under weakly acidic conditions, CMZ can accelerate the oxidation of Phen while theoxidation of itself keeps unchanged. Phenols can enhance their oxidation mutually, andthe oxidation of the pollutant with a smaller reaction constant is accelerated more. Thecatalytic effect of nHMO is the main reason for the phenomena under weakly acidicconditions. Under weakly alkaline conditions, the coexistence of CMZ and Phen haslittle effect on the oxidation of each other, while the coexsitence of phenols exhibitsdifferent that the oxidation of phenolic pollutant with smaller rate constant is inhibitedbut almost unchanged for the other. The competitive kinetics shows that two phenolicpollutants may compete for a new reactive intermediate in the oxidation rather thanpermanganate and manganese dioxide. Since the mechanism of the oxidation of CMZ isdifferent with that of Phen, CMZ and Phen do not compete for the same reactiveintermediate so that oxidation of Phen is not inhibited.
引文
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