基于零价铁的复合污染土壤化学修复研究
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摘要
随着我国城市化的快速发展，化工厂关闭和搬迁产生大量污染场地，这些场地大多具有有机氯(Organochlorine Pesticides，OCPs)和重金属复合污染特征，对人体健康和生态环境构成严重威胁，亟需进行有效地修复。零价铁(Zero-valent iron，ZVI)已成功用于OCPs还原和重金属稳定化，但单纯ZVI技术的还原处理效率较低，污染物降解不彻底。基于ZVI的类Fenton氧化技术因能显著提高OCPs的降解速率和去除率而受到广泛关注，其中ZVI/EDTA/Air组成的ZEA类Fenton体系能快速有效地去除水溶液中的有机物和重金属，但国内外未见有ZEA体系对土壤中OCPs和复合污染土壤修复的研究报道。
本文以常见的滴滴涕(Dichlorodiphenyltrichloroethanes，DDT)和多氯联苯(Polychlorinated Biphenyl，PCB)作为OCPs的代表，Cu和Pb作为重金属的代表，系统研究了基于ZVI的复合污染土壤化学修复效率及作用机制，具体内容包括：（1）评估ZEA类Fenton氧化体系修复OCPs污染土壤的效果及作用机理。（2）研究ZEA类Fenton氧化体系同步修复PCB和重金属(Cu和Pb)复合污染土壤的效果及作用机理。（3）探索表面活性剂强化ZEA类Fenton氧化修复PCB和重金属(Cu和Pb)复合污染土壤的效果及作用机理。（4）考察亚临界水条件下ZVI对于PCB和重金属(Cu和Pb)复合污染土壤的修复效果及作用机理。本文得到如下结论：
（1）针对4,4’-DDE、2,4’-DDD、4,4’-DDD和4,4’-DDT的初始含量分别为4.6、82、295和987mg/kg的高浓度DDTs实际污染土壤，ZEA类Fenton氧化体系在常温常压和近中性条件下对土壤中DDTs具有很好的氧化降解效果。当ZVI和EDTA的初始浓度分别为5g/L和0.2mmol/L时，反应8h，初始土壤中4,4’-DDE、2,4’-DDD、4,4’-DDD、4,4’-DDT和总DDTs的去除率分别达到28.8%、68.8%、51.2%、50.3%和51.5%。初始EDTA和ZVI添加量对ZEA类Fenton氧化DDTs的效果有显著影响。过量的EDTA对ZEA类Fenton氧化效果具有抑制作用。EDTA在ZEA类Fenton氧化土壤中DDTs的同时自身也会被降解。同时ZEA类Fenton氧化体系对土壤pH和有机质含量的影响较小，优于传统Fenton体系。
（2）ZEA类Fenton氧化体系能同步修复PCB、Cu和Pb初始浓度分别为22.9、106.4和412.3mg/kg的复合污染土壤。当EDTA和ZVI浓度分别为1mol/L和5g/L时，PCB的去除率为68.6%，重金属Pb和Cu的稳定化率分别为82.3%和59.4%。初始EDTA浓度、ZVI添加量和体系pH对ZEA类Fenton氧化修复复合污染土壤的效果有显著影响，过量的EDTA会增加Pb的解吸，同时抑制类Fenton反应。酸性pH(2-3)不利于ZEA类Fenton氧化修复复合污染土壤。复合污染中重金属的存在对PCB的降解有抑制作用。在ZEA体系中通过调控EDTA的添加方式和Fe2+的含量有利于强化类Fenton氧化降解复合污染土壤中PCB。
（3）EDDS-皂素对于复合污染土壤中的Pb、Cu和PCB具有显著的协同解吸作用，当EDDS和皂素的浓度分别为10mmol/L和3000mg/L时，Pb、Cu和PCB的解吸率达到最大，分别为99.8%、85.7%和45.7%。皂素能够显著强化ZEA类Fenton氧化PCB的降解效果，PCB的实际降解率为85.6%，比不加皂素的单独ZEA类Fenton氧化体系的效率提高了24.8%。添加皂素后，ZEA类Fenton氧化体系对重金属稳定化的实验观测值提高，其效果主要来源于添加皂素对重金属的强化解吸作用将重金属转移到水相中。同时反应过程中EDDS和皂素逐渐被降解。
（4）亚临界水能显著强化ZVI还原降解复合污染土壤中的PCB，同时对复合污染土壤中重金属Cu和Pb具有很好的稳定化作用。当反应温度为180℃，ZVI的剂量为0.2g，土壤中PCB的实际降解率达到89.5%，重金属Cu和Pb的稳定化率分别为90.7%和96.4%。ZVI的剂量、初始pH和反应气氛对土壤中PCB的降解和重金属的稳定化效果有显著影响。随着ZVI剂量的增加，土壤中PCB的降解率和重金属的稳定化率会逐渐增加。碱性条件更有利于土壤中PCB的还原降解和重金属的稳定化。有氧环境对土壤中PCB的降解有抑制作用，但对重金属的稳定化有利。
With the development of urbanization in China, a large number of contaminated sitesare generated during the shutting down and demolition of chemical enterprises. Most ofthese contaminated sites contain both organochlorine pesticides (OCPs) and heavy metals,which pose great threat to public health and ecotope. So effecient remediationtechnologies for these composite contaminated soils are extremely urgent. Zero-valentiron (ZVI) has been successfully used for reduction of OCPs and stabilization of heavymetals, but sole ZVI technology was showed inefficient. Fenton-like systems based onZVI attract wide attentions for its significant enhancement on the degradation of OCPs. Anovel Fenton-like system formed by ZVI, EDTA and Air (ZEA) has been reportedefficient decomposition of chlorophenols and high removal of heavy metals from solution.However, there is a lack of knowledge about the efficiency on remediation of OCPs andcomposite contaminated soils by ZEA system.
In the present study, dichlorodiphenyltrichloroethanes (DDT) and polychlorinatedbiphenyl were chosen as the representative OCPs, and Cu and Pb were elected as thetypical heavy metals. We systematically investigate the chemical remediation of compositecontaminated soils based on ZVI. The main contents included:(1) evaluating theremediation efficiency for OCPs contaminated soil by ZEA system;(2) investigating themechanism for simultaneous degradation OCPs and removal of heavy metals in compositecontaminated soil was studied;(3) exploring the enhancement of ZEA system forremediation of composite contaminated soil by surfactant;(4) elucidating the remediationefficiency and mechanism for composite contaminated soil by ZVI in subcritical water.
In general, the main conclusions can be summarized as follows:
(1) DDTs in the actual contaminated soil containing4.6mg/kg4,4’-DDE,82mg/kg2,4’-DDD,295mg/kg4,4’-DDD and987mg/kg4,4’-DDT, could be effectively degradedby ZEA system at room temperature, ambient atmosphere pressure and near neutral pH.When initial concentration of EDTA and ZVI were0.2mmol/L and5g/L respectively, theremoval ratio of4,4’-DDE,2,4’-DDD,4,4’-DDD,4,4’-DDT and total amounts of DDTswere achieved28.8%,68.8%,51.2%,50.3%and51.5%respectively. The dosages ofEDTA and ZVI were the dominant factors influencing the removal of contaminants.Excessive amount of EDTA led to a negative effect on the degradation process.Meanwhile, EDTA was simultaneously degraded during the process. Negligible influences on soil pH and organic matter were observed after the treatment which was superior totradition Fenton system.
(2) The tested composite contaminated soil contained22.9mg/kg PCB,106.4mg/kgCu and412.3mg/kg Pb. Simultaneous remediation of PCB and heavy metals wereobserved in ZEA system. With the addition of EDTA and ZVI were1mol/L and5g/Lrespectively, the decomposition ratio of PCB was68.8%, and the stabilization of Cu andPb were82.3%and59.4%respectively. The initial concentration of EDTA, ZVI dosageand pH obviously influence the remediation of composite contaminated soil in ZEAsystem. Excessive amount of EDTA could enhance the desorption of Pb, but inhibit thedegradation of PCB. The removal ratio of PCB decreased in acidic condition (pH=2-3).The presence of heavy metals in composite contaminated soil showed negative influenceon PCB decomposition. Stepwise addition of EDTA and regeneration of Fe2+couldenhance the oxidation of PCB by ZEA system.
(3) Significant synergy on Pb, Cu and PCB desorption were achieved with the novelcombination of saponin and EDDS. The maximal desorption of Pb, Cu and PCB wereachieved99.8%,85.7%and45.7%, respectively, in the presence of10mmol/L EDDScombined with3000mg/L saponin. Compared with absence of saponin, the removal ratioof PCB increased24.8%with the addition of saponin, and the decomposition ratio wasachieved85.6%. The increases of desorption contributed to the enhancement of observedstabilization of heavy metals. In addition, EDTA and saponin were simultaneouslydegraded.
(4) Efficient reduction of PCB and stabilization of heavy metals by ZVI wereobtained in subcritical water. As the temperature was180oC and the dosage of ZVI was0.2g, the decomposition ratio of PCB was achieved85.6%, the stabilization ratios of Cuand Pb were attained90.7%and96.4%, respectively. The initial ZVI dosage, pH andreaction atmosphere obviously influence the remediation of composite contaminated soilby ZVI in subcritical water. As the increase of ZVI addition, the decomposition ratio ofPCB and stabilization ratio of heavy metals increased. High removal ratio of PCB andstabilization ratio of heavy metals occurred in basic condition. The presence of dissolvedoxygen inhibited the reduction of PCB, but enhanced the stabilization of heavy metals.
本文以常见的滴滴涕(Dichlorodiphenyltrichloroethanes，DDT)和多氯联苯(Polychlorinated Biphenyl，PCB)作为OCPs的代表，Cu和Pb作为重金属的代表，系统研究了基于ZVI的复合污染土壤化学修复效率及作用机制，具体内容包括：（1）评估ZEA类Fenton氧化体系修复OCPs污染土壤的效果及作用机理。（2）研究ZEA类Fenton氧化体系同步修复PCB和重金属(Cu和Pb)复合污染土壤的效果及作用机理。（3）探索表面活性剂强化ZEA类Fenton氧化修复PCB和重金属(Cu和Pb)复合污染土壤的效果及作用机理。（4）考察亚临界水条件下ZVI对于PCB和重金属(Cu和Pb)复合污染土壤的修复效果及作用机理。本文得到如下结论：
（1）针对4,4’-DDE、2,4’-DDD、4,4’-DDD和4,4’-DDT的初始含量分别为4.6、82、295和987mg/kg的高浓度DDTs实际污染土壤，ZEA类Fenton氧化体系在常温常压和近中性条件下对土壤中DDTs具有很好的氧化降解效果。当ZVI和EDTA的初始浓度分别为5g/L和0.2mmol/L时，反应8h，初始土壤中4,4’-DDE、2,4’-DDD、4,4’-DDD、4,4’-DDT和总DDTs的去除率分别达到28.8%、68.8%、51.2%、50.3%和51.5%。初始EDTA和ZVI添加量对ZEA类Fenton氧化DDTs的效果有显著影响。过量的EDTA对ZEA类Fenton氧化效果具有抑制作用。EDTA在ZEA类Fenton氧化土壤中DDTs的同时自身也会被降解。同时ZEA类Fenton氧化体系对土壤pH和有机质含量的影响较小，优于传统Fenton体系。
（2）ZEA类Fenton氧化体系能同步修复PCB、Cu和Pb初始浓度分别为22.9、106.4和412.3mg/kg的复合污染土壤。当EDTA和ZVI浓度分别为1mol/L和5g/L时，PCB的去除率为68.6%，重金属Pb和Cu的稳定化率分别为82.3%和59.4%。初始EDTA浓度、ZVI添加量和体系pH对ZEA类Fenton氧化修复复合污染土壤的效果有显著影响，过量的EDTA会增加Pb的解吸，同时抑制类Fenton反应。酸性pH(2-3)不利于ZEA类Fenton氧化修复复合污染土壤。复合污染中重金属的存在对PCB的降解有抑制作用。在ZEA体系中通过调控EDTA的添加方式和Fe2+的含量有利于强化类Fenton氧化降解复合污染土壤中PCB。
（3）EDDS-皂素对于复合污染土壤中的Pb、Cu和PCB具有显著的协同解吸作用，当EDDS和皂素的浓度分别为10mmol/L和3000mg/L时，Pb、Cu和PCB的解吸率达到最大，分别为99.8%、85.7%和45.7%。皂素能够显著强化ZEA类Fenton氧化PCB的降解效果，PCB的实际降解率为85.6%，比不加皂素的单独ZEA类Fenton氧化体系的效率提高了24.8%。添加皂素后，ZEA类Fenton氧化体系对重金属稳定化的实验观测值提高，其效果主要来源于添加皂素对重金属的强化解吸作用将重金属转移到水相中。同时反应过程中EDDS和皂素逐渐被降解。
（4）亚临界水能显著强化ZVI还原降解复合污染土壤中的PCB，同时对复合污染土壤中重金属Cu和Pb具有很好的稳定化作用。当反应温度为180℃，ZVI的剂量为0.2g，土壤中PCB的实际降解率达到89.5%，重金属Cu和Pb的稳定化率分别为90.7%和96.4%。ZVI的剂量、初始pH和反应气氛对土壤中PCB的降解和重金属的稳定化效果有显著影响。随着ZVI剂量的增加，土壤中PCB的降解率和重金属的稳定化率会逐渐增加。碱性条件更有利于土壤中PCB的还原降解和重金属的稳定化。有氧环境对土壤中PCB的降解有抑制作用，但对重金属的稳定化有利。
With the development of urbanization in China, a large number of contaminated sitesare generated during the shutting down and demolition of chemical enterprises. Most ofthese contaminated sites contain both organochlorine pesticides (OCPs) and heavy metals,which pose great threat to public health and ecotope. So effecient remediationtechnologies for these composite contaminated soils are extremely urgent. Zero-valentiron (ZVI) has been successfully used for reduction of OCPs and stabilization of heavymetals, but sole ZVI technology was showed inefficient. Fenton-like systems based onZVI attract wide attentions for its significant enhancement on the degradation of OCPs. Anovel Fenton-like system formed by ZVI, EDTA and Air (ZEA) has been reportedefficient decomposition of chlorophenols and high removal of heavy metals from solution.However, there is a lack of knowledge about the efficiency on remediation of OCPs andcomposite contaminated soils by ZEA system.
In the present study, dichlorodiphenyltrichloroethanes (DDT) and polychlorinatedbiphenyl were chosen as the representative OCPs, and Cu and Pb were elected as thetypical heavy metals. We systematically investigate the chemical remediation of compositecontaminated soils based on ZVI. The main contents included:(1) evaluating theremediation efficiency for OCPs contaminated soil by ZEA system;(2) investigating themechanism for simultaneous degradation OCPs and removal of heavy metals in compositecontaminated soil was studied;(3) exploring the enhancement of ZEA system forremediation of composite contaminated soil by surfactant;(4) elucidating the remediationefficiency and mechanism for composite contaminated soil by ZVI in subcritical water.
In general, the main conclusions can be summarized as follows:
(1) DDTs in the actual contaminated soil containing4.6mg/kg4,4’-DDE,82mg/kg2,4’-DDD,295mg/kg4,4’-DDD and987mg/kg4,4’-DDT, could be effectively degradedby ZEA system at room temperature, ambient atmosphere pressure and near neutral pH.When initial concentration of EDTA and ZVI were0.2mmol/L and5g/L respectively, theremoval ratio of4,4’-DDE,2,4’-DDD,4,4’-DDD,4,4’-DDT and total amounts of DDTswere achieved28.8%,68.8%,51.2%,50.3%and51.5%respectively. The dosages ofEDTA and ZVI were the dominant factors influencing the removal of contaminants.Excessive amount of EDTA led to a negative effect on the degradation process.Meanwhile, EDTA was simultaneously degraded during the process. Negligible influences on soil pH and organic matter were observed after the treatment which was superior totradition Fenton system.
(2) The tested composite contaminated soil contained22.9mg/kg PCB,106.4mg/kgCu and412.3mg/kg Pb. Simultaneous remediation of PCB and heavy metals wereobserved in ZEA system. With the addition of EDTA and ZVI were1mol/L and5g/Lrespectively, the decomposition ratio of PCB was68.8%, and the stabilization of Cu andPb were82.3%and59.4%respectively. The initial concentration of EDTA, ZVI dosageand pH obviously influence the remediation of composite contaminated soil in ZEAsystem. Excessive amount of EDTA could enhance the desorption of Pb, but inhibit thedegradation of PCB. The removal ratio of PCB decreased in acidic condition (pH=2-3).The presence of heavy metals in composite contaminated soil showed negative influenceon PCB decomposition. Stepwise addition of EDTA and regeneration of Fe2+couldenhance the oxidation of PCB by ZEA system.
(3) Significant synergy on Pb, Cu and PCB desorption were achieved with the novelcombination of saponin and EDDS. The maximal desorption of Pb, Cu and PCB wereachieved99.8%,85.7%and45.7%, respectively, in the presence of10mmol/L EDDScombined with3000mg/L saponin. Compared with absence of saponin, the removal ratioof PCB increased24.8%with the addition of saponin, and the decomposition ratio wasachieved85.6%. The increases of desorption contributed to the enhancement of observedstabilization of heavy metals. In addition, EDTA and saponin were simultaneouslydegraded.
(4) Efficient reduction of PCB and stabilization of heavy metals by ZVI wereobtained in subcritical water. As the temperature was180oC and the dosage of ZVI was0.2g, the decomposition ratio of PCB was achieved85.6%, the stabilization ratios of Cuand Pb were attained90.7%and96.4%, respectively. The initial ZVI dosage, pH andreaction atmosphere obviously influence the remediation of composite contaminated soilby ZVI in subcritical water. As the increase of ZVI addition, the decomposition ratio ofPCB and stabilization ratio of heavy metals increased. High removal ratio of PCB andstabilization ratio of heavy metals occurred in basic condition. The presence of dissolvedoxygen inhibited the reduction of PCB, but enhanced the stabilization of heavy metals.
引文
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