高级氧化工艺降解水溶液中氯贝酸的影响因素及机理研究
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摘要
药物及个人护理产品(Pharmaceuticals and personal care products, PPCPs)是一类普遍存在于环境中的微量有机污染物,其浓度常在ng/L-μg/L水平。由于个人和畜牧业中大量而频繁的使用,导致其在环境中形成假性持续性现象。众多的研究结果表明,在低浓度药物中长期暴露是导致微生态动植物基因改变、造成细菌耐药性及形成水环境中内分泌干扰作用的重要原因。由于PPCPs在污水厂中不能完全被去除,导致其通过污水排放或污水回用进入到自然环境当中,因此,有必要寻求一种高效经济的新工艺或新技术以提高PPCPs的去除效率。
本论文以目前发现的在环境中存在最为持久的药物之一氯贝酸(降血脂药物的有效成分及代谢产物)为研究对象,比较了同样条件ultraviolet (UV)、vacuum ultraviolet (VUV)、UV/H2O2、VUV/H2O2工艺的降解效果,考察了H202投加量、氯贝酸初始浓度、溶液初始pH值、阴离子(Cl-、SO42-、NO3-、HCO3-)和有机质(腐殖酸)等的影响。以UV/H2O2工艺为对象,主要研究了温度在氯贝酸去除过程中所起的作用。研究了夏季及冬季solar/TiO2、solar/ZnO工艺对氯贝酸的去除,考察了温度、太阳光照强度、外加氧化剂H202、有机物质、NO3-、HCO3等因素的影响。最后通过GC-MS分析鉴定氯贝酸在不同工艺中的降解中间产物,并利用发光菌毒性试验对处理前后反应溶液毒性变化进行了评价。主要研究结论如下：
(1) UV、UV/H2O2、VUV、VUV/H2O2工艺降解氯贝酸过程遵循准一级反应动力学模型。氯贝酸在UV/H2O2、VUV/H2O2工艺中可通过直接光降解和·OH间接氧化去除,并以后者为主,而在VUV工艺中则是以直接光解为主。UV工艺中因不产生自由基,故氯贝酸的去除仅是直接光氧化作用的结果,其中溶液过酸或过碱均不利于氯贝酸的光解过程。当有腐殖酸有机质(20 mg/L)存在时可严重抑制氯贝酸的光降解。在UV工艺中,阴离子对氯贝酸降解有促进作用；其他工艺中均表现为基本无作用或有明显的抑制作用,且Cl-、SO42对降解过程的影响比NO3-、HCO3小。污水厂出水中复杂的成分可严重抑制氯贝酸的降解,与超纯水体系相比,表观速率常数降低1.8-4.9倍。四种工艺中,VUV/H2O2是去除超纯水及污水中氯贝酸最有效的工艺。同样达到99%以上去除率,VUV/H2O2、VUV、UV/H2O2、UV工艺去除污水中氯贝酸所需时间分别为40、80、80、240 min。
(2)在考察温度对UV/H2O2降解氯贝酸过程的影响时发现,升高温度(10℃—30℃)均能大大强化超纯水及污水厂二级处理出水中氯贝酸的去除效果。当氯贝酸初始浓度为10 mg/L时,同样达到99%以上的去除率,T1 (9.0-11.5℃)、T2 (19.0-21.0℃)、T3 (29.0-30.0℃)条件下污水中氯贝酸降解所需的反应时间分别为80、40、15 min。添加腐殖酸抑制了超纯水中氯贝酸的降解,且温度越低,影响越显著。低温条件下无论是低浓度还是高浓度,HC03-均表现为明显的抑制效应；当温度升高后,抑制作用减弱,且低浓度的抑制效应可忽略。三个温度条件下高浓度的NO3-均明显抑制了氯贝酸的降解,且随着温度的升高,抑制作用减弱；而T1(9.0-11.5℃)时低浓度N03-没有明显影响,但随着温度升高,表现出略微的促进作用。
(3)夏季及冬季氯贝酸在solar/TiO2、solar/ZnO工艺中的降解效果差异很大。两种阴离子(N03-和HC03-)的投加均抑制了氯贝酸的光催化降解过程,在高浓度HCO3-(0.1 mol/L)存在时尤为明显。夏季时,在solar/TiO2工艺中加入0.5 mg/L的腐殖酸能略微促进氯贝酸的降解,而冬季时,腐殖酸(20 mg/L)的投加严重抑制了氯贝酸的去除过程。在solar/ZnO工艺中,投加20 mg/L的腐殖酸同样起到严重抑制作用,但抑制程度在两个季节没有明显差别。在solar/TiO2工艺中,H202的添加没有明显促进氯贝酸的降解；而在solar/ZnO工艺中,添加100 mg/L H2O2则明显抑制了氯贝酸的去除。污水厂出水中氯贝酸的光催化降解速率常数明显低于超纯水体系。
(4)通过GC-MS分析,鉴定出了UV、UV/H2O2、VUV、VUV/H2O2、solar/TiO2工艺降解氯贝酸过程中产生的11种中间产物,其中只有3种化合物在以往文献中报道过。结合氯贝酸降解过程中溶解性有机碳(DOC)、Cl以及特征紫外吸光度(SUVA254)的变化情况,可推断在solar/TiO2工艺中首先发生的是苯环开环反应,而其他工艺中首先发生的是脱氯过程,且芳香类中间产物在溶液中存在累积现象。明亮发光杆菌毒性试验结果初步表明,溶液毒性增强主要是由芳香类中间产物引起的,而solar/TiO2工艺中的开环反应是降低毒性的一条有效途径。
Pharmaceuticals and personal care products (PPCPs) have been frequently detected at ng/L-μg/L levels (trace concentration) worldwide in the environment. Due to the large consumption of human and veterinary medicines, these compounds can be persistent in aquatic environment. Numerous researches showed that the long-term exposure to low concentration of pharmaceutical compounds has been regarded as the main reason to the change of genes in aquatic organisms, development of bacterial resistance to antibiotics and formation of endocrine disruption. Because of their incomplete removal in WWTPs, PPCPs can enter the aquatic environment through the discharge or reuse of wastewater treatment plants (WWTP) effluents, therefore, it is necessary to explore some new ways to promote their removal efficiency.
Clofibric acid (CA) is a metabolite of several lipid regulators consumed by human beings suffered angiocardiopathy problems and is believed as one of the most persistent pharmaceuticals in the environment. CA removal performances under the same experimental conditions by ultraviolet (UV), vacuum ultraviolet (VUV), UV/H2O2 and VUV/H2O2 processes were compared in this study. The influences of various factors including H2O2 amount, initial CA concentration, initial solution pH, anions (Cl-,SO42-, NO3-, HCO3-) and organic matters (humic acid, HA) on CA degradation were performed. In addition, the effect of temperature on CA removal was specially investigated in UV/H2O2 process. The performance of CA degradation in solar/TiO2 and solar/ZnO processes was studied in summer and winter seasons and the effects of temperature, solar light intensity, NO3- and HCO3-, HA and H2O2 on CA photo-catalysis were evaluated. Finally the intermediates in CA degradation during UV, UV/H2O2, VUV, VUV/H2O2 and solar/TiO2 processes were identified by GC-MS and the toxicity of these by-products also assessed. The key findings were summarized as below.
(1) All the experimental data well fitted the pseudo-first-order kinetic model. Direct oxidation was the main process in VUV irradiation despite the slight generation of hydroxyl radicals (·OH). In contrast, indirect oxidation of CA by generated OH was the main CA degradation mechanism in UV/H2O2 and VUV/H2O2. CA photodegradation was negatively influenced in both low and high pH conditions. The addition of 20 mg/L HA could significantly inhibit CA degradation, whereas anions (1.0×10-3 and 0.1 mol L-1) showed inhibitive or insignificant effects on CA degradation in all processes except in UV irradiation where they could increase the apparent reaction rate constants. The effects of Cl- and SO42-were less obvious than NO3- and HCO3- anions.The degradation rate decreased 1.8-4.9 folds when these processes were applied to real WWTP effluent due to the complex constituents. In all of the four, VUV/H2O2 showed the most effective process and the CA removal efficiency reached over 99% after 40 min in contrast to 80min in both UV/H2O2 and VUV processes and 240 min in UV process.
(2) Higher temperature (10℃-30℃) would favor CA degradation in UV/H2O2 process. When using a real WWTP effluent spiked with 10 mg/L CA over 99% of CA removal could be achieved under T3 (29.0-30.0℃) within only 15 min compared with 40 and 80 min under T2 (19.0-21.0℃) and T1 (9.0-11.5℃), respectively. HA had negative effect on CA degradation in Milli-Q water and this effect was much more apparent under low temperature condition. In addition, the inhibitive effect on CA degradation at both lower and higher concentrations of bicarbonate was observed, and this inhibitive effect was much more apparent at higher bicarbonate concentration and lower temperature condition. On the other hand, at higher nitrate concentration the inhibitive effect on CA degradation under three temperature ranges was observed, and with the temperature increase this negative effect was apparently weakened. However, at lower nitrate concentration a slightly positive effect on CA degradation was found under T2 and T3 conditions.
(3) Significant difference in CA degradation in two seasons was observed both in solar/TiO2 and solar/ZnO processes. The two anions (NO3- and HCO3-) adversely affected CA degradation, particularly at high HCO3- concentration. CA degradation slightly increased with 0.5 mg L-1 HA in solar/TiO2 in summer, but significantly inhibited in winter at 20 mg L-1 HA. However, the inhibitive effect of 20 mg L-1 HA on CA removal in solar/ZnO had no remarkable difference in two seasons. The degradation in solar/TiO2/H2O2 was similar to that in solar/TiO2, but inhibited obviously in solar/ZnO/H2O2. When applying photo-catalytic process into WWTP effluent degradation rates were apparently lower comparing to Milli-Q water.
(4) Eleven intermediates were detected by GC/MS, of which only three compounds have been reported before by other researchers. Combining with the evolution of the dissolved organic carbon (DOC), Cl- and specific ultraviolet absorption at 254 nm (SUVA254), it could be proposed that cleavage of aromatic ring followed by dechlorination was the mechanism in solar/TiO2 process, while dechlorination happening first and aromatic intermediates accumulated in other processes. The acute toxicity was evaluated by means of P. phosphoreum (T3, spp.) bioassay. It was believed that aromatic intermediates enhanced the solution toxicity and the ring-opening pathway in solar/TiO2 process could reduce the acute toxicity.
本论文以目前发现的在环境中存在最为持久的药物之一氯贝酸(降血脂药物的有效成分及代谢产物)为研究对象,比较了同样条件ultraviolet (UV)、vacuum ultraviolet (VUV)、UV/H2O2、VUV/H2O2工艺的降解效果,考察了H202投加量、氯贝酸初始浓度、溶液初始pH值、阴离子(Cl-、SO42-、NO3-、HCO3-)和有机质(腐殖酸)等的影响。以UV/H2O2工艺为对象,主要研究了温度在氯贝酸去除过程中所起的作用。研究了夏季及冬季solar/TiO2、solar/ZnO工艺对氯贝酸的去除,考察了温度、太阳光照强度、外加氧化剂H202、有机物质、NO3-、HCO3等因素的影响。最后通过GC-MS分析鉴定氯贝酸在不同工艺中的降解中间产物,并利用发光菌毒性试验对处理前后反应溶液毒性变化进行了评价。主要研究结论如下：
(1) UV、UV/H2O2、VUV、VUV/H2O2工艺降解氯贝酸过程遵循准一级反应动力学模型。氯贝酸在UV/H2O2、VUV/H2O2工艺中可通过直接光降解和·OH间接氧化去除,并以后者为主,而在VUV工艺中则是以直接光解为主。UV工艺中因不产生自由基,故氯贝酸的去除仅是直接光氧化作用的结果,其中溶液过酸或过碱均不利于氯贝酸的光解过程。当有腐殖酸有机质(20 mg/L)存在时可严重抑制氯贝酸的光降解。在UV工艺中,阴离子对氯贝酸降解有促进作用；其他工艺中均表现为基本无作用或有明显的抑制作用,且Cl-、SO42对降解过程的影响比NO3-、HCO3小。污水厂出水中复杂的成分可严重抑制氯贝酸的降解,与超纯水体系相比,表观速率常数降低1.8-4.9倍。四种工艺中,VUV/H2O2是去除超纯水及污水中氯贝酸最有效的工艺。同样达到99%以上去除率,VUV/H2O2、VUV、UV/H2O2、UV工艺去除污水中氯贝酸所需时间分别为40、80、80、240 min。
(2)在考察温度对UV/H2O2降解氯贝酸过程的影响时发现,升高温度(10℃—30℃)均能大大强化超纯水及污水厂二级处理出水中氯贝酸的去除效果。当氯贝酸初始浓度为10 mg/L时,同样达到99%以上的去除率,T1 (9.0-11.5℃)、T2 (19.0-21.0℃)、T3 (29.0-30.0℃)条件下污水中氯贝酸降解所需的反应时间分别为80、40、15 min。添加腐殖酸抑制了超纯水中氯贝酸的降解,且温度越低,影响越显著。低温条件下无论是低浓度还是高浓度,HC03-均表现为明显的抑制效应；当温度升高后,抑制作用减弱,且低浓度的抑制效应可忽略。三个温度条件下高浓度的NO3-均明显抑制了氯贝酸的降解,且随着温度的升高,抑制作用减弱；而T1(9.0-11.5℃)时低浓度N03-没有明显影响,但随着温度升高,表现出略微的促进作用。
(3)夏季及冬季氯贝酸在solar/TiO2、solar/ZnO工艺中的降解效果差异很大。两种阴离子(N03-和HC03-)的投加均抑制了氯贝酸的光催化降解过程,在高浓度HCO3-(0.1 mol/L)存在时尤为明显。夏季时,在solar/TiO2工艺中加入0.5 mg/L的腐殖酸能略微促进氯贝酸的降解,而冬季时,腐殖酸(20 mg/L)的投加严重抑制了氯贝酸的去除过程。在solar/ZnO工艺中,投加20 mg/L的腐殖酸同样起到严重抑制作用,但抑制程度在两个季节没有明显差别。在solar/TiO2工艺中,H202的添加没有明显促进氯贝酸的降解；而在solar/ZnO工艺中,添加100 mg/L H2O2则明显抑制了氯贝酸的去除。污水厂出水中氯贝酸的光催化降解速率常数明显低于超纯水体系。
(4)通过GC-MS分析,鉴定出了UV、UV/H2O2、VUV、VUV/H2O2、solar/TiO2工艺降解氯贝酸过程中产生的11种中间产物,其中只有3种化合物在以往文献中报道过。结合氯贝酸降解过程中溶解性有机碳(DOC)、Cl以及特征紫外吸光度(SUVA254)的变化情况,可推断在solar/TiO2工艺中首先发生的是苯环开环反应,而其他工艺中首先发生的是脱氯过程,且芳香类中间产物在溶液中存在累积现象。明亮发光杆菌毒性试验结果初步表明,溶液毒性增强主要是由芳香类中间产物引起的,而solar/TiO2工艺中的开环反应是降低毒性的一条有效途径。
Pharmaceuticals and personal care products (PPCPs) have been frequently detected at ng/L-μg/L levels (trace concentration) worldwide in the environment. Due to the large consumption of human and veterinary medicines, these compounds can be persistent in aquatic environment. Numerous researches showed that the long-term exposure to low concentration of pharmaceutical compounds has been regarded as the main reason to the change of genes in aquatic organisms, development of bacterial resistance to antibiotics and formation of endocrine disruption. Because of their incomplete removal in WWTPs, PPCPs can enter the aquatic environment through the discharge or reuse of wastewater treatment plants (WWTP) effluents, therefore, it is necessary to explore some new ways to promote their removal efficiency.
Clofibric acid (CA) is a metabolite of several lipid regulators consumed by human beings suffered angiocardiopathy problems and is believed as one of the most persistent pharmaceuticals in the environment. CA removal performances under the same experimental conditions by ultraviolet (UV), vacuum ultraviolet (VUV), UV/H2O2 and VUV/H2O2 processes were compared in this study. The influences of various factors including H2O2 amount, initial CA concentration, initial solution pH, anions (Cl-,SO42-, NO3-, HCO3-) and organic matters (humic acid, HA) on CA degradation were performed. In addition, the effect of temperature on CA removal was specially investigated in UV/H2O2 process. The performance of CA degradation in solar/TiO2 and solar/ZnO processes was studied in summer and winter seasons and the effects of temperature, solar light intensity, NO3- and HCO3-, HA and H2O2 on CA photo-catalysis were evaluated. Finally the intermediates in CA degradation during UV, UV/H2O2, VUV, VUV/H2O2 and solar/TiO2 processes were identified by GC-MS and the toxicity of these by-products also assessed. The key findings were summarized as below.
(1) All the experimental data well fitted the pseudo-first-order kinetic model. Direct oxidation was the main process in VUV irradiation despite the slight generation of hydroxyl radicals (·OH). In contrast, indirect oxidation of CA by generated OH was the main CA degradation mechanism in UV/H2O2 and VUV/H2O2. CA photodegradation was negatively influenced in both low and high pH conditions. The addition of 20 mg/L HA could significantly inhibit CA degradation, whereas anions (1.0×10-3 and 0.1 mol L-1) showed inhibitive or insignificant effects on CA degradation in all processes except in UV irradiation where they could increase the apparent reaction rate constants. The effects of Cl- and SO42-were less obvious than NO3- and HCO3- anions.The degradation rate decreased 1.8-4.9 folds when these processes were applied to real WWTP effluent due to the complex constituents. In all of the four, VUV/H2O2 showed the most effective process and the CA removal efficiency reached over 99% after 40 min in contrast to 80min in both UV/H2O2 and VUV processes and 240 min in UV process.
(2) Higher temperature (10℃-30℃) would favor CA degradation in UV/H2O2 process. When using a real WWTP effluent spiked with 10 mg/L CA over 99% of CA removal could be achieved under T3 (29.0-30.0℃) within only 15 min compared with 40 and 80 min under T2 (19.0-21.0℃) and T1 (9.0-11.5℃), respectively. HA had negative effect on CA degradation in Milli-Q water and this effect was much more apparent under low temperature condition. In addition, the inhibitive effect on CA degradation at both lower and higher concentrations of bicarbonate was observed, and this inhibitive effect was much more apparent at higher bicarbonate concentration and lower temperature condition. On the other hand, at higher nitrate concentration the inhibitive effect on CA degradation under three temperature ranges was observed, and with the temperature increase this negative effect was apparently weakened. However, at lower nitrate concentration a slightly positive effect on CA degradation was found under T2 and T3 conditions.
(3) Significant difference in CA degradation in two seasons was observed both in solar/TiO2 and solar/ZnO processes. The two anions (NO3- and HCO3-) adversely affected CA degradation, particularly at high HCO3- concentration. CA degradation slightly increased with 0.5 mg L-1 HA in solar/TiO2 in summer, but significantly inhibited in winter at 20 mg L-1 HA. However, the inhibitive effect of 20 mg L-1 HA on CA removal in solar/ZnO had no remarkable difference in two seasons. The degradation in solar/TiO2/H2O2 was similar to that in solar/TiO2, but inhibited obviously in solar/ZnO/H2O2. When applying photo-catalytic process into WWTP effluent degradation rates were apparently lower comparing to Milli-Q water.
(4) Eleven intermediates were detected by GC/MS, of which only three compounds have been reported before by other researchers. Combining with the evolution of the dissolved organic carbon (DOC), Cl- and specific ultraviolet absorption at 254 nm (SUVA254), it could be proposed that cleavage of aromatic ring followed by dechlorination was the mechanism in solar/TiO2 process, while dechlorination happening first and aromatic intermediates accumulated in other processes. The acute toxicity was evaluated by means of P. phosphoreum (T3, spp.) bioassay. It was believed that aromatic intermediates enhanced the solution toxicity and the ring-opening pathway in solar/TiO2 process could reduce the acute toxicity.
引文
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