US-Fenton法处理炸药废水的试验研究
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摘要
炸药废水是与炸药有关的产品在工业和军事生产、运输以及销毁过程中产生的废水，其成分复杂，所含污染物具有毒性，对人体和环境具有极大的危害。传统的水处理方法很难将污染物有效降解，近些年来未处理达标的炸药废水直接排放，引发各种环境问题，也引起了世界各国的广泛关注。寻求一种高效可行的处理方法是目前有效解决炸药废水污染问题的关键所在。US-Fenton法作为一种新兴的复合高级氧化技术，在水处理领域展现出广阔的发展前景。超声的空化作用、高温热解作用以及超临界水氧化作用对Fenton反应具有良好的促进作用，二者在有机物降解过程中相互协同，能有效降解传统方法难以降解的有机物。
本文在对实际炸药废水中有机污染物全面鉴定分析的基础上，选取TNT和DNAN为代表性污染物，将US-Fenton法引入炸药废水处理中，以实际炸药废水、TNT模拟废水和DNAN模拟废水为三种试验对象，通过室内试验对其处理效果及影响因素进行研究，并利用Batch和Semi-batch试验对TNT和DNAN的降解反应动力学进行了分析，通过GC-MS对中间产物进行了测定，明晰了TNT和DNAN的降解路径。论文的主要结论如下：
(1)以TOC去除率为主要参考指标，选取US-Fenton法为处理方法，并通过试验研究了反应条件对三种试验对象（实际炸药废水、TNT模拟废水和DNAN模拟废水）处理效果的影响，确定了三种废水的最佳处理条件，即：在pH=2，超声强度为300w/cm2， H_2O_2与Fe~(2+)摩尔浓度比为500：1，TOC初始浓度为42mg/L，处理时间为120min，温度为25时，实际炸药废水的处理效果相对较好，色度、TOC和COD的去除率分别达到86%、65%和84%；在pH=3，超声强度为300w/cm~2， H_2O_2与Fe~(~(2+))摩尔浓度比为10：1，TNT初始浓度为30mg/L，处理时间为300min，温度为25时，TNT模拟废水的处理效果相对较好，TNT、TOC和COD的去除率分别为99.9%、66.9%和81.2%；在pH=6，超声强度为300w/cm2， H_2O_2与Fe~(2+)摩尔浓度比为100：1，DNAN初始浓度为100mg/L，处理时间为300min，温度为25时，DNAN模拟废水的处理效果相对较好，DNAN、TOC和COD的去除率分别达到100%，73.8%和87.6%。
(2)利用Batch和Semi-batch试验分别对US-Fenton法降解TNT和DNAN的反应动力学进行了研究，结果表明，在Batch试验中，TNT和DNAN的降解反应属于二级反应，在Semi-batch试验中，TNT和DNAN的降解反应属于一级反应。
(3)基于US-Fenton法处理TNT降解机理的研究，初步得出了TNT降解的三种可能途径：一是OH首先将TNT中的甲基氧化，然后脱出羧基，生成TNB，TNB中的硝基进一步被OH氧化取代，生成三硝基苯酚、二硝基苯酚、硝基苯和苯酚，进而开环断键，通过水解和矿化作用，生成其他低分子酸(如草酸、甲酸)、CO_2、NO_3~-、H_2O等。二是TNT中的硝基先被还原成氨基，进而氨基被OH氧化脱去，之后甲基被氧化，生成苯酚，进而发生开环水解，有机物被进一步矿化，三是临位硝基先于甲基被氧化脱去，之后甲基被氧化成羧基，之后发生开环水解。
(4)通过对DNAN的US-Fenton法降解机理研究，揭示了DNAN降解的两种可能途径：其一是OH首先与DNAN发生脱硝基反应，生成2-羟基-4-硝基苯甲醚，4-羟基-2-硝基苯甲醚或是硝基苯甲醚，继而生成产物被进一步氧化，生成苯甲醚，之后苯甲醚被氧化成苯酚，进而开环断键，通过水解和矿化作用，生成低分子酸(如草酸、甲酸)、CO_2、NO_3~-、H_2O等。其二是DNAN中的硝基先被还原成氨基，进而氨基被OH氧化脱去，之后甲氧基被氧化，生成苯酚，进而发生开环水解，有机物被进一步矿化。
本研究将新兴的复合高级氧化技术US-Fenton法应用于炸药废水的处理，研究结果表明US-Fenton法处理炸药废水明显优于传统处理方法，能有效地降解炸药废水中的爆炸性有机物，因此，论文研究结果为炸药废水的处理和生态环境保护提供了科学依据。
Explosive wastewater generated from manufacturing, transporting, and demilitarizationin explosive industry and army ammunition plants contains rather complex chemicals, whichis toxic and harmful to both human beings and enviroment. Conventional wastewatertreatment processes are not effective in treating explosive wastewater. Due to discharge toenviroment before treatment, explosive wastewater has caused various enviromental troubles,which has become a world enviromental problem and focus of the people's concernrecently.Now the most important thing is to seek effective explosive wastewater treatmentmethods to sovle the problem.Combined ultrasound and Fenton (US-Fenton) process as anintergrated advanced oxidation technology showed vast potential for future development.Cavitation, pyrolysis, and supercritical water oxidation of ultrasound irradiation can improveFenton reaction and at the same time Fenton reaction can enhance the degradation effectiveof organic matter by ultrasound irradiation. Comparing with conventional wastewatertreatment process, US-Fenton process showed higher removal efficience in explosivewastewater treatment.
On the basis of real explosive wastewater physical and chemical charactors analysis,TNTand DNAN were selected as the representive explosive pollutants and US-Fenton process wasinvolved as the treatment method. Through a series of experiments, effect factors of realexplosive wastewater, TNT wastewater, and DNAN wastewater treatments were determined.Degradation kinetics of TNT and DNAN were detected in batch and semi-batch experiments.The degradation pathways of TNTand DNAN were gotten through determingintermedia byGC-MS.Main conclusionswere drawn based on the study presented herein:
(1) According to TOC removal efficience, US-Fenton process was chosen as thetreatment method. Effects of experimental conditions on real explosive wastewater, TNTwastewater, and DNAN wastewater treatment were determined and the optimal treatmentconditions were gotten. For real explosive wastewater, the optimal conditions were [TOC]0=420±20mg/L,[H_2O_2]/[Fe~(2+)]=500:1, pH=2,temperature=25, US intensity=300watts/cm2, and reaction time=120minutes. Under these conditions, color, TOC, and CODremoval were86,65, and84%, respectively; for TNT wastewater, the optimal conditionswere [TNT]0=30mg/L,[H_2O_2]/[Fe~(2+)]=10:1, pH=3, temperature=25, US intensity=300 watts/cm2, and reaction time=300minutes. TNT, TOC and COD removal were99.9,66.9,and81.2%, respectively; For DNANwastewaer,[DNAN]0=100mg/L,[H_2O_2]/[Fe~(2+)]=100:1,pH=6, temperature=25, US intensity=300watts/cm2, and reaction time=300minuteswere the optimal conditions and DNAN, TOC, and COD removal reached100,73.8, and87.6%, respectively.
(2) The degradation kinetics of TNT and DNAN were studied in batch and semi-batchexperiments. The results showed that both TNT and DNAN removals were pseudo-first-orderin batch experiment and in semi-batch experiment they were pseudo-second-order.
(3) Primarily proposed degradation pathways of TNT were determined through studyingthe degradation process. The first pathway was that methyl connected to benzene wasoxidated by OH to carboxyl and TNT became TNB. Subsequently, TNB was oxidatedfutherto trinitrophenol, dinitrophenol, nitrophenol, or phenol. At last, the ultimate products ofcarbon dioxide, nitrate ions and water were given by benzene ring open, hydrolysis, andmineralization; the second one was that nitro group was reduced to amino group firstly andthen cleaved from the benzene ring. Subsequently, methyl connected to benzene was oxidatedby OH to carboxyl and phenol was given; the third one was that p-nitro group was oxidatedby OH before methyl oxidation, and then methyl became carboxyl. Subsequently, benzenering open, hydrolysis, and mineralization happened and result in identical ultimate productsas mentioned.
(4) Through the study of DNAN degradation process, primarily proposed degradationpathways of DNAN were given.The first pathway was that DNAN reacted with OH togenerate2-hydroxy-4-nitroanisole,4-hydroxy-2-nitroanisole, or nitroanisole, which wereoxidated to anisole futher. Phenol as the oxidation production of anisole transformed tocarbon dioxide, nitrate ions and water through benzene ring open, hydrolysis, andmineralization; the second one was that nitro group was reduced to amino group firstly andthen cleaved from the benzene ring. Subsequently, methyl connected to benzene was oxidatedby OH to carboxyl. After that phenol was generated from benzoic acid, and then benzenering open, hydrolysis, and mineralization happened.
In this study, US-Fenton process was involved to treat explosive wastewater and showedhigher removal efficiency than conventional wastewater treatment processes. Explosivematter in the wastewater can be degraded well by US-Fenton process. Therefore this studyprovide scientific basis for explosive wastewater treatment and enviroment protection.
本文在对实际炸药废水中有机污染物全面鉴定分析的基础上，选取TNT和DNAN为代表性污染物，将US-Fenton法引入炸药废水处理中，以实际炸药废水、TNT模拟废水和DNAN模拟废水为三种试验对象，通过室内试验对其处理效果及影响因素进行研究，并利用Batch和Semi-batch试验对TNT和DNAN的降解反应动力学进行了分析，通过GC-MS对中间产物进行了测定，明晰了TNT和DNAN的降解路径。论文的主要结论如下：
(1)以TOC去除率为主要参考指标，选取US-Fenton法为处理方法，并通过试验研究了反应条件对三种试验对象（实际炸药废水、TNT模拟废水和DNAN模拟废水）处理效果的影响，确定了三种废水的最佳处理条件，即：在pH=2，超声强度为300w/cm2， H_2O_2与Fe~(2+)摩尔浓度比为500：1，TOC初始浓度为42mg/L，处理时间为120min，温度为25时，实际炸药废水的处理效果相对较好，色度、TOC和COD的去除率分别达到86%、65%和84%；在pH=3，超声强度为300w/cm~2， H_2O_2与Fe~(~(2+))摩尔浓度比为10：1，TNT初始浓度为30mg/L，处理时间为300min，温度为25时，TNT模拟废水的处理效果相对较好，TNT、TOC和COD的去除率分别为99.9%、66.9%和81.2%；在pH=6，超声强度为300w/cm2， H_2O_2与Fe~(2+)摩尔浓度比为100：1，DNAN初始浓度为100mg/L，处理时间为300min，温度为25时，DNAN模拟废水的处理效果相对较好，DNAN、TOC和COD的去除率分别达到100%，73.8%和87.6%。
(2)利用Batch和Semi-batch试验分别对US-Fenton法降解TNT和DNAN的反应动力学进行了研究，结果表明，在Batch试验中，TNT和DNAN的降解反应属于二级反应，在Semi-batch试验中，TNT和DNAN的降解反应属于一级反应。
(3)基于US-Fenton法处理TNT降解机理的研究，初步得出了TNT降解的三种可能途径：一是OH首先将TNT中的甲基氧化，然后脱出羧基，生成TNB，TNB中的硝基进一步被OH氧化取代，生成三硝基苯酚、二硝基苯酚、硝基苯和苯酚，进而开环断键，通过水解和矿化作用，生成其他低分子酸(如草酸、甲酸)、CO_2、NO_3~-、H_2O等。二是TNT中的硝基先被还原成氨基，进而氨基被OH氧化脱去，之后甲基被氧化，生成苯酚，进而发生开环水解，有机物被进一步矿化，三是临位硝基先于甲基被氧化脱去，之后甲基被氧化成羧基，之后发生开环水解。
(4)通过对DNAN的US-Fenton法降解机理研究，揭示了DNAN降解的两种可能途径：其一是OH首先与DNAN发生脱硝基反应，生成2-羟基-4-硝基苯甲醚，4-羟基-2-硝基苯甲醚或是硝基苯甲醚，继而生成产物被进一步氧化，生成苯甲醚，之后苯甲醚被氧化成苯酚，进而开环断键，通过水解和矿化作用，生成低分子酸(如草酸、甲酸)、CO_2、NO_3~-、H_2O等。其二是DNAN中的硝基先被还原成氨基，进而氨基被OH氧化脱去，之后甲氧基被氧化，生成苯酚，进而发生开环水解，有机物被进一步矿化。
本研究将新兴的复合高级氧化技术US-Fenton法应用于炸药废水的处理，研究结果表明US-Fenton法处理炸药废水明显优于传统处理方法，能有效地降解炸药废水中的爆炸性有机物，因此，论文研究结果为炸药废水的处理和生态环境保护提供了科学依据。
Explosive wastewater generated from manufacturing, transporting, and demilitarizationin explosive industry and army ammunition plants contains rather complex chemicals, whichis toxic and harmful to both human beings and enviroment. Conventional wastewatertreatment processes are not effective in treating explosive wastewater. Due to discharge toenviroment before treatment, explosive wastewater has caused various enviromental troubles,which has become a world enviromental problem and focus of the people's concernrecently.Now the most important thing is to seek effective explosive wastewater treatmentmethods to sovle the problem.Combined ultrasound and Fenton (US-Fenton) process as anintergrated advanced oxidation technology showed vast potential for future development.Cavitation, pyrolysis, and supercritical water oxidation of ultrasound irradiation can improveFenton reaction and at the same time Fenton reaction can enhance the degradation effectiveof organic matter by ultrasound irradiation. Comparing with conventional wastewatertreatment process, US-Fenton process showed higher removal efficience in explosivewastewater treatment.
On the basis of real explosive wastewater physical and chemical charactors analysis,TNTand DNAN were selected as the representive explosive pollutants and US-Fenton process wasinvolved as the treatment method. Through a series of experiments, effect factors of realexplosive wastewater, TNT wastewater, and DNAN wastewater treatments were determined.Degradation kinetics of TNT and DNAN were detected in batch and semi-batch experiments.The degradation pathways of TNTand DNAN were gotten through determingintermedia byGC-MS.Main conclusionswere drawn based on the study presented herein:
(1) According to TOC removal efficience, US-Fenton process was chosen as thetreatment method. Effects of experimental conditions on real explosive wastewater, TNTwastewater, and DNAN wastewater treatment were determined and the optimal treatmentconditions were gotten. For real explosive wastewater, the optimal conditions were [TOC]0=420±20mg/L,[H_2O_2]/[Fe~(2+)]=500:1, pH=2,temperature=25, US intensity=300watts/cm2, and reaction time=120minutes. Under these conditions, color, TOC, and CODremoval were86,65, and84%, respectively; for TNT wastewater, the optimal conditionswere [TNT]0=30mg/L,[H_2O_2]/[Fe~(2+)]=10:1, pH=3, temperature=25, US intensity=300 watts/cm2, and reaction time=300minutes. TNT, TOC and COD removal were99.9,66.9,and81.2%, respectively; For DNANwastewaer,[DNAN]0=100mg/L,[H_2O_2]/[Fe~(2+)]=100:1,pH=6, temperature=25, US intensity=300watts/cm2, and reaction time=300minuteswere the optimal conditions and DNAN, TOC, and COD removal reached100,73.8, and87.6%, respectively.
(2) The degradation kinetics of TNT and DNAN were studied in batch and semi-batchexperiments. The results showed that both TNT and DNAN removals were pseudo-first-orderin batch experiment and in semi-batch experiment they were pseudo-second-order.
(3) Primarily proposed degradation pathways of TNT were determined through studyingthe degradation process. The first pathway was that methyl connected to benzene wasoxidated by OH to carboxyl and TNT became TNB. Subsequently, TNB was oxidatedfutherto trinitrophenol, dinitrophenol, nitrophenol, or phenol. At last, the ultimate products ofcarbon dioxide, nitrate ions and water were given by benzene ring open, hydrolysis, andmineralization; the second one was that nitro group was reduced to amino group firstly andthen cleaved from the benzene ring. Subsequently, methyl connected to benzene was oxidatedby OH to carboxyl and phenol was given; the third one was that p-nitro group was oxidatedby OH before methyl oxidation, and then methyl became carboxyl. Subsequently, benzenering open, hydrolysis, and mineralization happened and result in identical ultimate productsas mentioned.
(4) Through the study of DNAN degradation process, primarily proposed degradationpathways of DNAN were given.The first pathway was that DNAN reacted with OH togenerate2-hydroxy-4-nitroanisole,4-hydroxy-2-nitroanisole, or nitroanisole, which wereoxidated to anisole futher. Phenol as the oxidation production of anisole transformed tocarbon dioxide, nitrate ions and water through benzene ring open, hydrolysis, andmineralization; the second one was that nitro group was reduced to amino group firstly andthen cleaved from the benzene ring. Subsequently, methyl connected to benzene was oxidatedby OH to carboxyl. After that phenol was generated from benzoic acid, and then benzenering open, hydrolysis, and mineralization happened.
In this study, US-Fenton process was involved to treat explosive wastewater and showedhigher removal efficiency than conventional wastewater treatment processes. Explosivematter in the wastewater can be degraded well by US-Fenton process. Therefore this studyprovide scientific basis for explosive wastewater treatment and enviroment protection.
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