UV/O_3降解水中新兴微污染物的特性与机理研究
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摘要
在工业迅速发展和人们生活水平普遍提高的今天,水环境污染受到了越来越多的关注,尤其是饮用水的卫生和安全问题。然而,传统的给水处理工艺对于近年来微污染水源中出现的一些新兴有机污染物如医药品和个人护理品(PPCPs)、内分泌干扰物(ECDs)和微囊藻毒素(MCs)等的处理能力有限,很难将其降解。另外,加强和推广污水的再生利用即中水回用是缓解我国水资源短缺压力的有效方法。而这两者均需要有效的深度处理技术来支撑。因此,研究简单、易行、经济的可用于饮用水及中水回用的深度处理技术是非常必要和有意义的,而臭氧和紫外联用技术(UV/O_3)正是可选的技术之一。
本文运用浓度去除率和生物毒性去除率两种评价指标对单独臭氧氧化工艺(O_3)、紫外辐射工艺(UV)和臭氧与紫外联用工艺(UV/O_3)降解几种典型的新兴有机物污染物的效能进行了评价和比较。并且考察了水质条件和操作参数对三种工艺降解污染物的效能的影响。同时,运用LC-TOF/MS和离子色谱等分析手段对降解过程中形成的中间产物进行了分析并提出了可能的降解途径。最后,基于非稳态的羟基自由基的假设结合半经验模型运用matlab建立了模拟天然水体本底的UV/O_3降解有机污染物的动力学模型。
臭氧化对目标污染物(磺胺甲基异恶唑(SMX)、佳乐麝香(HHCB)、双酚A(BPA)、微囊藻毒素LR(MC-LR))的浓度去除效果均令人满意,20min的去除率都能达到90%以上,二级反应速率常数在102~106 M-1·s-1数量级范围。而UV工艺仅仅对于光解活性较好的SMX和MC-LR(ФSMX=0.0263 mol·Einstein-1,ФMC-LR=0.041 mol·Einstein-1)的去除效果较好。而对于HHCB和BPA,由于量子产率和(或)吸光效率的低下导致二者20min的浓度去除率低于20%。
提高臭氧或紫外投量能够强化有机污染物的去除,而增加有机污染物的初始浓度则会导致降解效能的下降,这本质上是投配比(即臭氧或紫外投量与有机污染物的浓度比)决定了有机污染物的降解效能。对于O_3工艺,溶液的pH值能通过两方面影响有机污染的降解效能:一是pH的改变能够影响臭氧的直接反应和间接反应的贡献大小;二是pH的改变能够影响有机污染的离解状态从而影响其与臭氧分子的反应活性,尤其是那些与臭氧直接反应活性很高的有机物。对于UV工艺,pH值主要通过要影响有机物的离解状态进而影响其光解活性。重碳酸离子作为广为接受的羟基自由基捕获剂,其对臭氧氧化有机污染物的效能的影响分为两种情况:对于与臭氧反应活性相对较高的SMX、BPA和MC-LR,0～8mM的重碳酸根离子有利于水中臭氧残留的稳定,从而在一定程度上促进了三者的降解,而对于与臭氧反应活性相对较弱的HHCB,同样浓度范围的重碳酸根离子对其降解表现出了一定的抑制作用。重碳酸根离子的存在对四种目标有机物的UV降解基本上没有什么影响。当水体中存在0～5mg·L~(-1)的腐植酸时,其对四种目标有机物的臭氧氧化降解过程同样分为两种情况,对于与臭氧反应活性相对较高的SMX、BPA和MC-LR,腐植酸对他们的降解均表现除了不同程度的抑制作用;而对于与臭氧具有中等反应活性的HHCB,低浓度范围的腐植酸对其降解具有一定的促进作用,高浓度水平的腐植酸则表现出抑制作用。至于UV降解过程,考察浓度范围的腐植酸对四种目标有机物的降解均表现出了强化作用。操作参数和水质条件对UV/O_3工艺的影响类似于O_3工艺,但UV/O_3工艺抗水质波动的能力更强。需要说明的是,在考察的pH值范围(5.0～9.0)内,中性条件下的降解效能最好,这一点非常有利于其实际应用。
使用大型蚤活动抑制试验、费希尔弧菌毒性试验、酵母菌雌激素筛选测试(YES)和蛋白磷酸酶(PP2A)活性抑制试验等毒性评价手段对四种目标有机物在O_3、UV、和UV/O_3降解过程中的生物毒性进行了考察。通过对TOC去除率的考察和中间产物的定性分析,发现O_3和UV降解有机污染物的过程中产生了大量的中间产物,而这些产物部分保留或完全保留了母体分子的中的某些官能团结构。这些中间产物的积累导致了在O_3和UV降解有机污染物的过程中,浓度去除和毒性去除之间出现了偏离。而UV/O_3工艺由于能有效的减少中间产物的积累,所以其在有效降低污染物浓度的同时也能有效降其生物毒性。
在模拟天然水体本底条件下建立的UV/O_3体系的动力学模型能较好地预测模型化合物SMX的浓度变化,但是对体系中H_2O_2分解和积累在反应初期预测值不理想,另外模型对羟基自由基的浓度变化的预测值要较实测值低20%～35%。
With the rapid development and improvement of people’s living standard, the environmental pollution has been an issue of great concern, especially for the safety and sanitation of drinking water. However, there are no specific unites in the conventional drinking water treatment processes for the removal of emerging contaminants such as endocrine disrupting chemicals (ECDs), pharmaceutical and personal care products (PPCPs), microcystins (MCs) etc., so these emerging contaminants cannot be degraded by conventional drinking water treatment processes and then may enter into the drinking water . In addition, improving and promoting reclaimed water recycling is an effective method to relieve the stress of water source shortage. Based on the stated above, developing and designing efficient, easy, and economic advanced treatment technologies are in urgent need.
Degradation of target compounds by ozonation (O_3), UV photolysis (UV), and combined use of ozone and UV (UV/O_3) was investigated, and the efficiencies of biotoxicity removal were also evaluated. The influences of operational parameters and water qualities on the three processes were also investigated. Finally, assuming that hydroxyl radicals are in a unsteady state, a kinetic model for the UV/O_3 system, containing water simulating the natural water, was established with matlab.
Ozonation showed a satisfied performance on the removal of selected organic pollutants (sulfamethoxazole (SMX), galaxolide (HHCB), bisphenol A (BPA), and microcystin LR (MC-LR)), with removal rates over 90% in 20 min. The second-order rate constants of ozone with the four chemicals were on the order of 102~106 M-1·s-1 at neutral condition. The UV process only degraded SMX and MC-LR rapidly, but showed slow degradation rates for HHCB and BPA due to their low molar extinction coefficients and(or) quantum yields, with removal rates less than 20% in 20 min.
The influences of operational parameters and water qualities on the O_3 and UV processes were studied. Increasing the ozone or UV dose can improve the degradation of organic pollutants, while increase in the initial concentration of target compounds would worsen the degradation efficiency. Essentially, the ratio of ozone (UV) dose to concentration of target compounds determined the degradation efficiency. For O_3 process,the solution pH exerted effect on the degradation from two aspects. First, the solution pH can change the proportion of direct ozonation and indirect ozonation involved in the degradation process. Second, the solution pH can influence the dissociation state of target compounds which show different reactivity towards ozone, especially for the organic compounds with high reactivity towards ozone. As to UV process,the solution pH made its contribution mainly by changing the dissociation state of target compound. Bicarbonate ion, as a widely accepted hydroxyl radical quencher, showed different performance on different target compounds. For the compounds with high reactivity towards ozone such as SMX、BPA and MC-LR, the presence of bicarbonate ion in the range of 0～8 mM was favored to stabilize the aqueous ozone residual and thus benefit the removal of pollutants. However, when the pollutants reacted slowly with ozone, such as HHCB, the presence of bicarbonate ion would inhibit the degradation process. On the contrary, there was little effect in the presence of bicarbonate ion for UV process. Similar to the case of bicarbonate ion, the presence of humic acid (HA) in the range of 0～5 mg·L~(-1) showed different performance on different target compounds. To SMX, BPA, and MC-LR,HA was an inhibitor. In the case of HHCB, low level of HA promoted the degradation but the high level of HA suppressed the degradation. HA at all the concentration levels (0～5 mg·L~(-1)) improved the degradation efficiencies of target compounds. The influences of operational parameters and water qualities on the UV/O_3 process was similar to that on O_3 process, but the UV/O_3 process seemed to more resistant to fluctuation of water quality.one point should be mentioned, in the investigated pH range(5.0～9.0), best performance was obtained in the neutral condition, which was very advantageous to practical application.
The biotoxicity evolution of target compounds during the O_3, UV, and UV/O_3 processes was investigated with daphnia magna acute immobilisation test, vibrio fischeri toxicity test, yeast estrogen screen, and protein phosphatase 2A inhibition assay. Based on the results of TOC and intermidiates analysis, it can be concluded that a large amount of intermidiates were formed during the O_3 and UV processes. Unforunately, these intermidiates kept partial or intact functional groups contined in the parent moleceulars, which resulted in deviation between the concentration removal rates and biotoxicity rates. The UV/O_3process, with high mineralization ability, can effectively reduce the accumulation of intermidiates and thus decreased the biotoxicity meanwhile.
The established kinetic model for the UV/O_3 system, containing water simulating the natural water, can predict the concentration variation of SMX well, but yield a unsatisfied prediction for the decay and accumulation of H_2O_2 on the early stage of reaction. In addition, the model underestimated the concentration of hydroxyl concentration by 20%～35% compared to the experimental data.
本文运用浓度去除率和生物毒性去除率两种评价指标对单独臭氧氧化工艺(O_3)、紫外辐射工艺(UV)和臭氧与紫外联用工艺(UV/O_3)降解几种典型的新兴有机物污染物的效能进行了评价和比较。并且考察了水质条件和操作参数对三种工艺降解污染物的效能的影响。同时,运用LC-TOF/MS和离子色谱等分析手段对降解过程中形成的中间产物进行了分析并提出了可能的降解途径。最后,基于非稳态的羟基自由基的假设结合半经验模型运用matlab建立了模拟天然水体本底的UV/O_3降解有机污染物的动力学模型。
臭氧化对目标污染物(磺胺甲基异恶唑(SMX)、佳乐麝香(HHCB)、双酚A(BPA)、微囊藻毒素LR(MC-LR))的浓度去除效果均令人满意,20min的去除率都能达到90%以上,二级反应速率常数在102~106 M-1·s-1数量级范围。而UV工艺仅仅对于光解活性较好的SMX和MC-LR(ФSMX=0.0263 mol·Einstein-1,ФMC-LR=0.041 mol·Einstein-1)的去除效果较好。而对于HHCB和BPA,由于量子产率和(或)吸光效率的低下导致二者20min的浓度去除率低于20%。
提高臭氧或紫外投量能够强化有机污染物的去除,而增加有机污染物的初始浓度则会导致降解效能的下降,这本质上是投配比(即臭氧或紫外投量与有机污染物的浓度比)决定了有机污染物的降解效能。对于O_3工艺,溶液的pH值能通过两方面影响有机污染的降解效能:一是pH的改变能够影响臭氧的直接反应和间接反应的贡献大小;二是pH的改变能够影响有机污染的离解状态从而影响其与臭氧分子的反应活性,尤其是那些与臭氧直接反应活性很高的有机物。对于UV工艺,pH值主要通过要影响有机物的离解状态进而影响其光解活性。重碳酸离子作为广为接受的羟基自由基捕获剂,其对臭氧氧化有机污染物的效能的影响分为两种情况:对于与臭氧反应活性相对较高的SMX、BPA和MC-LR,0～8mM的重碳酸根离子有利于水中臭氧残留的稳定,从而在一定程度上促进了三者的降解,而对于与臭氧反应活性相对较弱的HHCB,同样浓度范围的重碳酸根离子对其降解表现出了一定的抑制作用。重碳酸根离子的存在对四种目标有机物的UV降解基本上没有什么影响。当水体中存在0～5mg·L~(-1)的腐植酸时,其对四种目标有机物的臭氧氧化降解过程同样分为两种情况,对于与臭氧反应活性相对较高的SMX、BPA和MC-LR,腐植酸对他们的降解均表现除了不同程度的抑制作用;而对于与臭氧具有中等反应活性的HHCB,低浓度范围的腐植酸对其降解具有一定的促进作用,高浓度水平的腐植酸则表现出抑制作用。至于UV降解过程,考察浓度范围的腐植酸对四种目标有机物的降解均表现出了强化作用。操作参数和水质条件对UV/O_3工艺的影响类似于O_3工艺,但UV/O_3工艺抗水质波动的能力更强。需要说明的是,在考察的pH值范围(5.0～9.0)内,中性条件下的降解效能最好,这一点非常有利于其实际应用。
使用大型蚤活动抑制试验、费希尔弧菌毒性试验、酵母菌雌激素筛选测试(YES)和蛋白磷酸酶(PP2A)活性抑制试验等毒性评价手段对四种目标有机物在O_3、UV、和UV/O_3降解过程中的生物毒性进行了考察。通过对TOC去除率的考察和中间产物的定性分析,发现O_3和UV降解有机污染物的过程中产生了大量的中间产物,而这些产物部分保留或完全保留了母体分子的中的某些官能团结构。这些中间产物的积累导致了在O_3和UV降解有机污染物的过程中,浓度去除和毒性去除之间出现了偏离。而UV/O_3工艺由于能有效的减少中间产物的积累,所以其在有效降低污染物浓度的同时也能有效降其生物毒性。
在模拟天然水体本底条件下建立的UV/O_3体系的动力学模型能较好地预测模型化合物SMX的浓度变化,但是对体系中H_2O_2分解和积累在反应初期预测值不理想,另外模型对羟基自由基的浓度变化的预测值要较实测值低20%～35%。
With the rapid development and improvement of people’s living standard, the environmental pollution has been an issue of great concern, especially for the safety and sanitation of drinking water. However, there are no specific unites in the conventional drinking water treatment processes for the removal of emerging contaminants such as endocrine disrupting chemicals (ECDs), pharmaceutical and personal care products (PPCPs), microcystins (MCs) etc., so these emerging contaminants cannot be degraded by conventional drinking water treatment processes and then may enter into the drinking water . In addition, improving and promoting reclaimed water recycling is an effective method to relieve the stress of water source shortage. Based on the stated above, developing and designing efficient, easy, and economic advanced treatment technologies are in urgent need.
Degradation of target compounds by ozonation (O_3), UV photolysis (UV), and combined use of ozone and UV (UV/O_3) was investigated, and the efficiencies of biotoxicity removal were also evaluated. The influences of operational parameters and water qualities on the three processes were also investigated. Finally, assuming that hydroxyl radicals are in a unsteady state, a kinetic model for the UV/O_3 system, containing water simulating the natural water, was established with matlab.
Ozonation showed a satisfied performance on the removal of selected organic pollutants (sulfamethoxazole (SMX), galaxolide (HHCB), bisphenol A (BPA), and microcystin LR (MC-LR)), with removal rates over 90% in 20 min. The second-order rate constants of ozone with the four chemicals were on the order of 102~106 M-1·s-1 at neutral condition. The UV process only degraded SMX and MC-LR rapidly, but showed slow degradation rates for HHCB and BPA due to their low molar extinction coefficients and(or) quantum yields, with removal rates less than 20% in 20 min.
The influences of operational parameters and water qualities on the O_3 and UV processes were studied. Increasing the ozone or UV dose can improve the degradation of organic pollutants, while increase in the initial concentration of target compounds would worsen the degradation efficiency. Essentially, the ratio of ozone (UV) dose to concentration of target compounds determined the degradation efficiency. For O_3 process,the solution pH exerted effect on the degradation from two aspects. First, the solution pH can change the proportion of direct ozonation and indirect ozonation involved in the degradation process. Second, the solution pH can influence the dissociation state of target compounds which show different reactivity towards ozone, especially for the organic compounds with high reactivity towards ozone. As to UV process,the solution pH made its contribution mainly by changing the dissociation state of target compound. Bicarbonate ion, as a widely accepted hydroxyl radical quencher, showed different performance on different target compounds. For the compounds with high reactivity towards ozone such as SMX、BPA and MC-LR, the presence of bicarbonate ion in the range of 0～8 mM was favored to stabilize the aqueous ozone residual and thus benefit the removal of pollutants. However, when the pollutants reacted slowly with ozone, such as HHCB, the presence of bicarbonate ion would inhibit the degradation process. On the contrary, there was little effect in the presence of bicarbonate ion for UV process. Similar to the case of bicarbonate ion, the presence of humic acid (HA) in the range of 0～5 mg·L~(-1) showed different performance on different target compounds. To SMX, BPA, and MC-LR,HA was an inhibitor. In the case of HHCB, low level of HA promoted the degradation but the high level of HA suppressed the degradation. HA at all the concentration levels (0～5 mg·L~(-1)) improved the degradation efficiencies of target compounds. The influences of operational parameters and water qualities on the UV/O_3 process was similar to that on O_3 process, but the UV/O_3 process seemed to more resistant to fluctuation of water quality.one point should be mentioned, in the investigated pH range(5.0～9.0), best performance was obtained in the neutral condition, which was very advantageous to practical application.
The biotoxicity evolution of target compounds during the O_3, UV, and UV/O_3 processes was investigated with daphnia magna acute immobilisation test, vibrio fischeri toxicity test, yeast estrogen screen, and protein phosphatase 2A inhibition assay. Based on the results of TOC and intermidiates analysis, it can be concluded that a large amount of intermidiates were formed during the O_3 and UV processes. Unforunately, these intermidiates kept partial or intact functional groups contined in the parent moleceulars, which resulted in deviation between the concentration removal rates and biotoxicity rates. The UV/O_3process, with high mineralization ability, can effectively reduce the accumulation of intermidiates and thus decreased the biotoxicity meanwhile.
The established kinetic model for the UV/O_3 system, containing water simulating the natural water, can predict the concentration variation of SMX well, but yield a unsatisfied prediction for the decay and accumulation of H_2O_2 on the early stage of reaction. In addition, the model underestimated the concentration of hydroxyl concentration by 20%～35% compared to the experimental data.
引文
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