超重力强化臭氧高级氧化技术处理模拟苯酚废水的研究
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摘要
随着我国经济的迅猛发展和人民生活水平的提高,如何解决日益严峻的环境问题越来越成为全社会关注的焦点。有机废水污染是水环境日益恶化的重要原因之一,其中含酚废水是一类比较典型,且排放量和危害都较大的有机废水。化学氧化法预处理后接生物处理是一种经济高效的酚类废水处理方法。目前,臭氧高级氧化技术(如O3/H2O2工艺、均相催化臭氧化等)因其高氧化能力、无二次污染等优点被应用于水处理领域,但该类方法普遍存在臭氧在水中的溶解性差,利用效率低等缺陷。
本文引入超重力技术对臭氧高级氧化工艺进行强化,将其与O3/H2O2、 O3/Fe(Ⅱ)、O3/H2O2/Fe(Ⅱ)(O3/Fenton)三种高级氧化工艺结合,考察了超重力环境下操作条件对苯酚降解的影响规律,通过响应面实验设计方法对操作条件进行优化,比较了不同高级氧化工艺下羟基自由基相对浓度及苯酚的降解机理,为酚类废水的快速处理提供新的处理工艺,主要研究内容及成果总结如下：
(1)在使用旋转填充床作为反应器,以O3/Fe(Ⅱ)体系处理苯酚废水的单因素研究中发现,当超重力环境从2g(g为地球重力加速度)增加至175g时,O3和O3/Fe(Ⅱ)体系的传质系数提高了约1倍,苯酚降解率提高了约0.7倍。在酸性条件下,在O3体系中添加少量亚铁(0.4mM)即可提高苯酚降解率约10%。利用响应面法对操作条件进行进一步优化时发现,在亚铁浓度为0.58mM、臭氧浓度为60mg/L、液体流量为10L/h、旋转填充床转速为1500rpm时,03/Fe(Ⅱ)体系的苯酚降解率达70%；在亚铁浓度为0.5mM、臭氧浓度为30mg/L、液体流量为30L/h、旋转填充床转速为1500rpm时,03/Fe(Ⅱ)体系的臭氧利用率可达0.096mol/mol (phenol/O3)。苯酚溶液经过03/Fe(Ⅱ)体系处理之后可生化性指标(五日生物需氧量与化学需氧量之比,BOD5/COD)从处理前的0.2增加至0.56,大大高于生化处理所需的0.3。
(2)通过对旋转填充床强化03/H202体系降解苯酚废水的反应动力学研究发现,当超重力环境从8g增加至200g时,苯酚和COD降解的表观反应速率常数分别增加了1倍和0.6倍。研究表明,适宜的操作条件为：过氧化氢浓度为1.3mM、初始pH值为9、臭氧浓度为55mg/L、反应温度为25℃、转速为1000rpm,此时苯酚和COD降解率分别可达96%和75%。
(3)通过对超重力强化O3/Fenton (O3/Fe(II)/H2O2)体系处理苯酚废水的研究发现,苯酚降解率在O3/Fenton体系比03体系要高出大约20%,并且在过氧化氢浓度为1.4mM时达98%。当超重力环境从8g增加至200g时,03体系和O3/Fenton体系的苯酚降解率分别提高了0.6和0.3倍。在亚铁浓度为0.17mM、臭氧浓度为50mg/L、过氧化氢浓度为1.1mM、pH为6、旋转填充床转速为1000rpm时,O3/Fenton体系的苯酚降解率达98.6%, BOD5/COD值由0.2增加至0.58。
(4)通过比较O3、O3/Fe(Ⅱ)、O3/H2O2以及O3/Fenton四种氧化体系的羟基自由基浓度与臭氧浓度之比(羟基自由基相对浓度)发现,催化剂的加入可提高羟基自由基相对浓度,氧化性催化剂H2O2的加入能同时提高羟基自由基相对浓度及自由基总存在量∫[·OH]dt;还原性催化剂Fe(Ⅱ)的加入能提高羟基自由基相对浓度,但同时会消耗氧化剂并降低自由基总存在量∫[·OH]dt。O3/Fenton体系的羟基自由基相对浓度是O3体系的近80倍,其∫[·OH]dt提升约3倍。在臭氧浓度相同时,添加催化剂使之转变为高级氧化体系能显著提高氧化速率和降低选择性,对于羟基自由基浓度也有明显提升,高级氧化工艺的应用可提高水处理过程效率、减小水处理设施的体积。
(5)在pH=2时,在O3体系中添加Fe(Ⅱ)使部分苯酚降解中间产物苯醌被还原成对苯二酚,从而使对苯二酚在中间产物中所占比例上升；同时由于Fe(Ⅱ)加入使体系苯氧自由基等活跃的自由基增多,使O3/Fe(Ⅱ)体系中产生少量邻苯二甲酸二甲酯和一些聚合物。当pH在7左右时,与酸性条件下相比,O3体系中苯酚降解中间产物,中间产物浓度有明显下降,O3体系中只检测到残留的苯酚和少量的1,2-苯二酚、邻苯二甲酸二甲酯和乙酸苯酯；O3/Fenton体系中除了少量残留苯酚外几乎没有检测到中间产物,这表明苯酚在O3/Fenton体系降解相对更为彻底,产物大多为小分子有机酸等,这也解释了苯酚溶液经O3/Fenton体系处理后BOD5/COD值相对于O3体系有大幅提升的现象。
The organic wastewater becomes a big problem in petrochemical industry, printing and dyeing industry and pharmaceutical industry with the rapid development of China's economy. Phenolic wastewater is a typical organic wastewater with significant impact on environment. Chemical oxidation followed by biotreatment is an efficient method for phenolic wastewater treatment. Ozone-based advanced oxidation processes, such as O3/H2O2process and homogeneous catalytic ozonation, have been used in wastewater treatment field due to the high oxidizability and no secondary pollution. However, the low solubility and utilization rate of ozone limit the application of ozone-based advanced oxidation processes.
In this study, the high-gravity technology (rotating packed bed, RPB) was used to intensify the ozone-based advanced oxidation processes, including O3/H2O2, O3/Fe(II) and O3/H2O2/Fe(II)(O3/Fenton) processes. The effects of different operation conditions on phenol degradation were investigated and the operation conditions in high gravity environment were optimized using response surface method (RSM). The relative concentrations of hydroxyl radicals and phenol degradation mechanisms in different oxidation processes were compared, with an attempt to provide a new process for the rapid treatment of phenolic wastewater. This study has reached the following conclusions:
(1) Single-factor method was used to investigate the catalytic ozonation of phenol with O3/Fe(Ⅱ) process in RPB. In acidic environment, the phenol degradation rate in O3/Fe(Ⅱ) process was about10%higher than that in O3process. The mass transfer coefficient was doubled and the phenol degradation rate increased0.7times in O3and O3/Fe(Ⅱ) processes when the high gravity level in RPB increased from2g to175g. According to the result of the RSM experiments, the phenol degradation rate in O3Fe(Ⅱ) process reached70%at the Fe(Ⅱ) concentration of0.58mM, O3concentration of60mg/L, liquid flow rate of10L/h, rotating speed of1500rpm respectively. The ozone utilization rate of O3/Fe(Ⅱ) process reached0.096mol/mol (phenol/O3) at the Fe(Ⅱ) concentration of0.5mM, O3concentration of30mg/L, liquid flow rate of30L/h, rotating speed of1500rpm respectively. After the phenol solution was treated by O3/Fe(Ⅱ) process, the BOD5/COD value (biodegradability) of the phenol solution increased significantly from0.2to0.56which is much higher than the requirement of biochemical treatment (>0.3).
(2) The kinetics of the phenol degradation in O3/H2O2-RPB process was investigated in this study. The apparent reaction rate constant of phenol degradation and COD degradation increased1times and0.6times respectively when the high gravity level in RPB increased from8g to200g. Experimental results indicated that the phenol and COD removal rate reached96%and75%under the suitable operation conditions:H2O2concentration of1.3mM, O3concentration of60mg/L, initial pH of9, reaction temperature of25℃, and rotating speed of1500rpm.
(3) The ozonation of phenol in03/Fenton process intensified by an RPB was investigated in this study. It was found that the phenol degradation in03/Fenton process was about20%higher than that in O3process and reached98%at the H2O2concentration of1.4mM. The phenol degradation rate of O3and03/Fenton processes increased0.6times and0.3times respectively when the high gravity level in RPB increased from8g to200g. The phenol degradation rate in O3/Fenton process reached98.6%under the operation conditions:Fe(II) concentration of0.17mM, H2O2concentration of1.1mM, O3concentration of50mg/L, initial pH of6, and rotating speed of1000rpm. The BOD5/COD value of the phenol solution increased from0.2to0.58after the phenol solution was treated by03/Fenton process.
(4) The ratios of hydroxyl radicals concentration to ozone concentration (Ret) in O3, O3/Fe(II), O3/H2O2and03/Fenton processes were studied. It was found that the addition of catalyst could improve the formation of hydroxyl radicals; addition of H2O2and Fenton reagent could increase both the formation efficiency and amount of hydroxyl radicals, addition of Fe(II) could increase the formation efficiency of hydroxyl radicals but decrease oxidant amount (∫[·OH]dt) The Rct value in O3/Fenton process was about80times higher than that in O3process, but the total hydroxyl radical amount in03/Fenton process was only3times higher than that in O3process. Therefore, advanced oxidation processes have higher oxidation rate and low selectivity but could not increase the oxidation amount. The application of advanced oxidation processes will increase the treatment efficiency and decrease the equipment size in wastewater treatment.
(5) The addition of Fe(Ⅱ) increased the amount of hydroquinone in O3/Fe(Ⅱ) process due to the reduction of benzoquinone by Fe(Ⅱ) at pH=2. There were more free radicals such as phenoxy radicals in O3/Fe(Ⅱ) process leading to the formation of some dimethyl phthalate and polymers. The intermediates concentration in O3process was lower in neutral environment than that in acidic environment. Only residual phenol and a small amount of1,2-benzodiazepines, dimethyl phthalate, and phenylacetate were determined in O3process under neutral environment. A relatively thorough phenol degradation was attained in O3/Fenton process and most intermediates were degraded to small organic acids. So there were almost no intermediates found in O3/Fenton process. It also explained why phenol solution had a significantly higher BOD5/COD after treated by O3/Fenton process than by O3process.
本文引入超重力技术对臭氧高级氧化工艺进行强化,将其与O3/H2O2、 O3/Fe(Ⅱ)、O3/H2O2/Fe(Ⅱ)(O3/Fenton)三种高级氧化工艺结合,考察了超重力环境下操作条件对苯酚降解的影响规律,通过响应面实验设计方法对操作条件进行优化,比较了不同高级氧化工艺下羟基自由基相对浓度及苯酚的降解机理,为酚类废水的快速处理提供新的处理工艺,主要研究内容及成果总结如下：
(1)在使用旋转填充床作为反应器,以O3/Fe(Ⅱ)体系处理苯酚废水的单因素研究中发现,当超重力环境从2g(g为地球重力加速度)增加至175g时,O3和O3/Fe(Ⅱ)体系的传质系数提高了约1倍,苯酚降解率提高了约0.7倍。在酸性条件下,在O3体系中添加少量亚铁(0.4mM)即可提高苯酚降解率约10%。利用响应面法对操作条件进行进一步优化时发现,在亚铁浓度为0.58mM、臭氧浓度为60mg/L、液体流量为10L/h、旋转填充床转速为1500rpm时,03/Fe(Ⅱ)体系的苯酚降解率达70%；在亚铁浓度为0.5mM、臭氧浓度为30mg/L、液体流量为30L/h、旋转填充床转速为1500rpm时,03/Fe(Ⅱ)体系的臭氧利用率可达0.096mol/mol (phenol/O3)。苯酚溶液经过03/Fe(Ⅱ)体系处理之后可生化性指标(五日生物需氧量与化学需氧量之比,BOD5/COD)从处理前的0.2增加至0.56,大大高于生化处理所需的0.3。
(2)通过对旋转填充床强化03/H202体系降解苯酚废水的反应动力学研究发现,当超重力环境从8g增加至200g时,苯酚和COD降解的表观反应速率常数分别增加了1倍和0.6倍。研究表明,适宜的操作条件为：过氧化氢浓度为1.3mM、初始pH值为9、臭氧浓度为55mg/L、反应温度为25℃、转速为1000rpm,此时苯酚和COD降解率分别可达96%和75%。
(3)通过对超重力强化O3/Fenton (O3/Fe(II)/H2O2)体系处理苯酚废水的研究发现,苯酚降解率在O3/Fenton体系比03体系要高出大约20%,并且在过氧化氢浓度为1.4mM时达98%。当超重力环境从8g增加至200g时,03体系和O3/Fenton体系的苯酚降解率分别提高了0.6和0.3倍。在亚铁浓度为0.17mM、臭氧浓度为50mg/L、过氧化氢浓度为1.1mM、pH为6、旋转填充床转速为1000rpm时,O3/Fenton体系的苯酚降解率达98.6%, BOD5/COD值由0.2增加至0.58。
(4)通过比较O3、O3/Fe(Ⅱ)、O3/H2O2以及O3/Fenton四种氧化体系的羟基自由基浓度与臭氧浓度之比(羟基自由基相对浓度)发现,催化剂的加入可提高羟基自由基相对浓度,氧化性催化剂H2O2的加入能同时提高羟基自由基相对浓度及自由基总存在量∫[·OH]dt;还原性催化剂Fe(Ⅱ)的加入能提高羟基自由基相对浓度,但同时会消耗氧化剂并降低自由基总存在量∫[·OH]dt。O3/Fenton体系的羟基自由基相对浓度是O3体系的近80倍,其∫[·OH]dt提升约3倍。在臭氧浓度相同时,添加催化剂使之转变为高级氧化体系能显著提高氧化速率和降低选择性,对于羟基自由基浓度也有明显提升,高级氧化工艺的应用可提高水处理过程效率、减小水处理设施的体积。
(5)在pH=2时,在O3体系中添加Fe(Ⅱ)使部分苯酚降解中间产物苯醌被还原成对苯二酚,从而使对苯二酚在中间产物中所占比例上升；同时由于Fe(Ⅱ)加入使体系苯氧自由基等活跃的自由基增多,使O3/Fe(Ⅱ)体系中产生少量邻苯二甲酸二甲酯和一些聚合物。当pH在7左右时,与酸性条件下相比,O3体系中苯酚降解中间产物,中间产物浓度有明显下降,O3体系中只检测到残留的苯酚和少量的1,2-苯二酚、邻苯二甲酸二甲酯和乙酸苯酯；O3/Fenton体系中除了少量残留苯酚外几乎没有检测到中间产物,这表明苯酚在O3/Fenton体系降解相对更为彻底,产物大多为小分子有机酸等,这也解释了苯酚溶液经O3/Fenton体系处理后BOD5/COD值相对于O3体系有大幅提升的现象。
The organic wastewater becomes a big problem in petrochemical industry, printing and dyeing industry and pharmaceutical industry with the rapid development of China's economy. Phenolic wastewater is a typical organic wastewater with significant impact on environment. Chemical oxidation followed by biotreatment is an efficient method for phenolic wastewater treatment. Ozone-based advanced oxidation processes, such as O3/H2O2process and homogeneous catalytic ozonation, have been used in wastewater treatment field due to the high oxidizability and no secondary pollution. However, the low solubility and utilization rate of ozone limit the application of ozone-based advanced oxidation processes.
In this study, the high-gravity technology (rotating packed bed, RPB) was used to intensify the ozone-based advanced oxidation processes, including O3/H2O2, O3/Fe(II) and O3/H2O2/Fe(II)(O3/Fenton) processes. The effects of different operation conditions on phenol degradation were investigated and the operation conditions in high gravity environment were optimized using response surface method (RSM). The relative concentrations of hydroxyl radicals and phenol degradation mechanisms in different oxidation processes were compared, with an attempt to provide a new process for the rapid treatment of phenolic wastewater. This study has reached the following conclusions:
(1) Single-factor method was used to investigate the catalytic ozonation of phenol with O3/Fe(Ⅱ) process in RPB. In acidic environment, the phenol degradation rate in O3/Fe(Ⅱ) process was about10%higher than that in O3process. The mass transfer coefficient was doubled and the phenol degradation rate increased0.7times in O3and O3/Fe(Ⅱ) processes when the high gravity level in RPB increased from2g to175g. According to the result of the RSM experiments, the phenol degradation rate in O3Fe(Ⅱ) process reached70%at the Fe(Ⅱ) concentration of0.58mM, O3concentration of60mg/L, liquid flow rate of10L/h, rotating speed of1500rpm respectively. The ozone utilization rate of O3/Fe(Ⅱ) process reached0.096mol/mol (phenol/O3) at the Fe(Ⅱ) concentration of0.5mM, O3concentration of30mg/L, liquid flow rate of30L/h, rotating speed of1500rpm respectively. After the phenol solution was treated by O3/Fe(Ⅱ) process, the BOD5/COD value (biodegradability) of the phenol solution increased significantly from0.2to0.56which is much higher than the requirement of biochemical treatment (>0.3).
(2) The kinetics of the phenol degradation in O3/H2O2-RPB process was investigated in this study. The apparent reaction rate constant of phenol degradation and COD degradation increased1times and0.6times respectively when the high gravity level in RPB increased from8g to200g. Experimental results indicated that the phenol and COD removal rate reached96%and75%under the suitable operation conditions:H2O2concentration of1.3mM, O3concentration of60mg/L, initial pH of9, reaction temperature of25℃, and rotating speed of1500rpm.
(3) The ozonation of phenol in03/Fenton process intensified by an RPB was investigated in this study. It was found that the phenol degradation in03/Fenton process was about20%higher than that in O3process and reached98%at the H2O2concentration of1.4mM. The phenol degradation rate of O3and03/Fenton processes increased0.6times and0.3times respectively when the high gravity level in RPB increased from8g to200g. The phenol degradation rate in O3/Fenton process reached98.6%under the operation conditions:Fe(II) concentration of0.17mM, H2O2concentration of1.1mM, O3concentration of50mg/L, initial pH of6, and rotating speed of1000rpm. The BOD5/COD value of the phenol solution increased from0.2to0.58after the phenol solution was treated by03/Fenton process.
(4) The ratios of hydroxyl radicals concentration to ozone concentration (Ret) in O3, O3/Fe(II), O3/H2O2and03/Fenton processes were studied. It was found that the addition of catalyst could improve the formation of hydroxyl radicals; addition of H2O2and Fenton reagent could increase both the formation efficiency and amount of hydroxyl radicals, addition of Fe(II) could increase the formation efficiency of hydroxyl radicals but decrease oxidant amount (∫[·OH]dt) The Rct value in O3/Fenton process was about80times higher than that in O3process, but the total hydroxyl radical amount in03/Fenton process was only3times higher than that in O3process. Therefore, advanced oxidation processes have higher oxidation rate and low selectivity but could not increase the oxidation amount. The application of advanced oxidation processes will increase the treatment efficiency and decrease the equipment size in wastewater treatment.
(5) The addition of Fe(Ⅱ) increased the amount of hydroquinone in O3/Fe(Ⅱ) process due to the reduction of benzoquinone by Fe(Ⅱ) at pH=2. There were more free radicals such as phenoxy radicals in O3/Fe(Ⅱ) process leading to the formation of some dimethyl phthalate and polymers. The intermediates concentration in O3process was lower in neutral environment than that in acidic environment. Only residual phenol and a small amount of1,2-benzodiazepines, dimethyl phthalate, and phenylacetate were determined in O3process under neutral environment. A relatively thorough phenol degradation was attained in O3/Fenton process and most intermediates were degraded to small organic acids. So there were almost no intermediates found in O3/Fenton process. It also explained why phenol solution had a significantly higher BOD5/COD after treated by O3/Fenton process than by O3process.
引文
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