零价金属强化氧化工艺去除水中邻苯二甲酸二丁酯的研究
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摘要
随着水环境污染的加重,水中的微量有机污染物种类越来越多,尤其是邻苯二甲酸酯类物质(PAEs),在水环境中已经达到普遍检出的水平,成为一类最普遍的污染物。这类物质具有致癌、致畸、致突变的活性,对人体健康危害极大,引起全球性关注并被很多国家列为优先控制污染物。常规给水处理工艺对这类有机物的去除效率十分有限,已经不能满足日益提高的水质标准的要求,开发新的水处理工艺以控制饮用水中的PAEs成为当前迫切需要解决的问题。
本文以邻苯二甲酸二丁酯(DBP)为主要目标污染物,从强化臭氧氧化的角度考虑,通过对比试验筛选能够高效去除水中DBP的方法,综合考察了各种金属氧化物、活性炭、过氧化氢、零价金属等物质对臭氧氧化DBP的强化作用,最后找出能够经济高效地强化去除水中PAEs等微量有机污染物的零价金属强化氧化工艺,主要工作与研究成果如下:
制备了多种催化剂,并考察了不同种类催化剂存在条件下对臭氧去除水中DBP的影响规律。研究发现,α-FeOOH、γ-Fe2O3、Mn3O4具有一定的强化臭氧去除DBP能力,但强化效果最佳的催化剂γ-Fe2O3对DBP的去除率也只有60.7%;过氧化氢能够大幅度的强化臭氧去除DBP,去除率可达90%以上;纳米TiO2对臭氧氧化DBP的强化效果较好,负载型的纳米二氧化钛强化臭氧氧化对DBP的去除率可达80%以上;活性炭具有一定的强化臭氧氧化去除DBP的能力,但与过氧化氢联用时并没有体现出协同作用。研究发现,零价铁、零价锌对臭氧氧化去除DBP具有良好的强化作用,反应过程中对DBP的去除率可高达90%以上;值得注意的是,在酸性条件下零价铁和零价铜具有强化水中溶解氧去除DBP的能力,臭氧在氧化反应过程中并不是必需的氧化剂。
在零价铁强化臭氧氧化DBP过程中,DBP去除效果受零价铁投量、有机物浓度、溶液pH值等因素的影响,不同pH值条件下对DBP的氧化机理有所差别;中性条件下,零价铁对臭氧的强化作用受叔丁醇的影响,反应过程遵循羟基自由基机理;排除了反应过程中其他铁氧化物的强化作用,认为强化臭氧氧化DBP效率的提高主要是基于零价铁本身的强化能力;水质条件及水中常见阴阳离子、有机物等对零价铁强化臭氧氧化具有一定影响。
零价锌对臭氧氧化DBP具有良好的强化能力,在所选择的实验条件下,当零价锌投量为0.05g/L时即可高效的强化臭氧去除DBP;零价锌投量增大有利于DBP的去除,DBP初始浓度对其去除效率影响不大,溶液pH值影响零价锌强化臭氧氧化的效果。值得注意的是,零价锌强化臭氧氧化过程不受水中碳酸根的影响,叔丁醇存在时对氧化过程的抑制作用也不完全,因此认为该反应过程不完全遵循羟基自由基机理;反应过程中零价锌本身对臭氧的强化起主要作用,但重复利用后效果更好,说明反应过程中零价锌生成了强化活性更高的物质;不同水质对零价锌强化臭氧氧化DBP的效率影响较小,但一些阳离子如钠离子、铵离子、铁离子及低浓度腐殖酸存在可以加快DBP的去除。
在酸性条件下,零价铜具有良好的强化氧化去除水中多种有机物的能力,其强化氧化效果随溶液pH值降低、零价铜投量增加而提高,有机物的去除效率受有机物初始浓度的影响较小;零价铜强化氧化去除水中有机物的过程,排除了吸附、氧化铜以及铜离子的作用,并且能够达到降低TOC、矿化有机物的效果;零价铜强化氧化的反应机理受溶液中酸的影响,用硫酸调pH值时,溶解氧对于零价铜强化氧化去除有机物并不是必需的,反应遵循羟基自由基作用机理;而用盐酸调pH值时,溶解氧对于零价铜强化氧化去除有机物是必需的,反应过程不受羟基自由基抑制剂叔丁醇的影响;水质条件对零价铜强化氧化的效果影响较大,铁离子的加入能加快DBP的去除,而甲醛的加入对DBP的去除起反作用;零价铜重复使用后强化氧化效率提高,反应过程中有铜离子溶出。
零价铁、零价锌强化臭氧氧化工艺可用于实际水源水的处理,提高原水中DOC的去除率,处理后UV254降低,氨氮浓度升高,强化臭氧氧化对分子量为1000～10000之间的有机物的去除效果明显;零价铜强化氧化对原水中的DOC有一定去除,对分子量为1750和3800附近的有机物的去除比较明显;零价铁、零价锌强化臭氧氧化也可以用于废水的处理,在一定程度上提高臭氧去除COD的效率。
With the increasing pollution of water environment, more and more micro-organic pollutants are found in water, especially phthalate acid esters(PAEs), which has been detected widely in water environment and become a kind of prevalent pollutants. PAEs are cancerogenic, teratogenic and mutagenic, which are seriously harmful to human health. PAEs have been listed as the priority pollutants by many countries and widely concerned all over the world. The improvement of drinking water standards and the low removal efficiency of PAEs by conventional water treatment technology make it urgent to develop new water treatment processes and control PAEs in drinking water.
Dibutyl phthalate (DBP) was chosen as a main target pollutant in this experiment which aimed at improving ozonation by the presence of metal oxides, activated carbon, hydrogen peroxide and zero valent metals. The objective of this work is to find a method which is high efficiency, simple and low cost to remove PAEs from drinking water. Results and conclusions include:
Several metal oxides were prepared by different methods, andα-FeOOH,γ-Fe2O3, Mn3O4 were found to have the ability of improving DBP removal efficiency in ozonation, and the best removal efficiency was 60.7% when usingγ-Fe2O3 as the catalyst. Removal efficiency of DBP in ozonation could be enhanced greatly by adding hydrogen peroxide and more than 90% of DBP could be removed. Nanosized titanium dioxide (TiO2) had good performance to improve ozonation efficiency, and the removal efficiency of DBP could reach 80% at least by using supported nanosized TiO2. DBP removal efficiency could also be enhanced to some extent by adding activated carbon into ozonation process, but coupling use of activated carbon and hydrogen peroxide did not show synergistic effect. Zero valent iron (ZVI) and zero valent zinc (ZVZ) had excellent ability to improve ozonation efficiency, and the DBP removal efficiency was more than 90% in the experimental conditions. In acidic condition, DBP could be removed by the presence of ZVI and zero valent copper (ZVC),and ozone was not necessary to present in these two processes.
DBP removal efficiency in the enhanced ozonation by using ZVI was influenced by ZVI dose, DBP concentration and pH. Under different pH conditions, the oxidation mechanisms of DBP were different. Under neutral condition,the ability of improving ozonation efficiency by the presence of ZVI was influenced by the addition of tert-butyl alcohol,which means that the reaction follow hydroxyl radical mechanism. The improvement of DBP ozonation was due to mainly the acceleration effect of ZVI itself, rather than other oxide species. DBP removal efficiency in the enhanced ozonation process using ZVI was influenced by water quality condition, and cations, anions, organic compounds in water to some extents.
ZVZ had good ability to improve the ozonation efficiency of DBP, and 0.05g/L dose of ZVZ was enough to remove DBP effectively under experimental conditions. DBP removal efficiency was enhanced from the increase of ZVZ dose and pH value of the solution, and the DBP initial concentration had little influence on its removal efficiency. The efficiency of ZVZ enhanced ozonation was not inhibited by the presence of carbonate. It is also found that the inhibition of tert-butyl alcohol on this process was uncompleted, so the reaction did not follow hydroxyl radical mechanism entirely. ZVZ itself played the major role in improving ozonation process, but better efficiency was achieved after ZVZ was reused, which means that there are some species with higher activity on improving ozonation during the reaction. Under different water quality conditions, DBP removal efficiency was changed little,but some cations such as Na+, NH4+, Fe2+ and low concentration of humic acid could accelerate the removal of DBP.
Under acidic condition, Zero valent copper (ZVC) had good ability to remove organic compounds from water by using dissolved oxygen. The oxidation efficiency was increased with the decrease of solution pH and the increase of ZVC dose. The initial concentration of organic compounds had a little influence on the removal efficiency. The experiment results excluded the improving effect achieved by the adsorption of ZVC, the presence of copper oxide and copper ion in the ZVC enhanced oxidation process. The TOC was decreased and mineralization was achieved in the oxidation of DEP by the presence of ZVC under acid condition. The reaction mechanism of copper enhanced oxidation process was different when using different type of acids in the experiment. When the solution pH was adjusted by sulfuric acid, dissolved oxygen was not necessary to present for ZVC enhanced oxidation process and the reaction was affected by the presence of tert-butyl alcohol, which means that the reaction follow hydroxyl radical mechanism. When pH was adjusted using hydrochloric acid, dissolved oxygen was necessary to present for the enhanced removal of organic compounds, and the reaction was not influenced by the presence of hydroxyl radical inhibitor-tert butyl alcohol. The efficiency of ZVC enhanced oxidation process was greatly influenced by the water quality condition, and the addition of iron ion could speed up the removal of DBP,but the addition of methanal inhibit the removal of DBP. After ZVC was reused, its ability of improving the oxidation process increased, and copper ion was released in the reaction process.
ZVI and ZVZ enhanced ozonation can be used in the treatment of source water. The TOC and UV254 were reduced in ZVI and ZVZ enhanced ozonation process and ammonia nitrogen concentration was increased. Organic compounds with a molecular weight of 1000～10000 was removed obviously in ZVI and ZVZ enhanced ozonation process, and Organic compounds with a molecular weight about 1750 and 3800 was removed obviously in ZVC enhanced oxidation process under acidic condition. ZVI and ZVZ enhanced ozonation process could also be used in the treatment of wastewater to increase the removal efficiency of COD.
本文以邻苯二甲酸二丁酯(DBP)为主要目标污染物,从强化臭氧氧化的角度考虑,通过对比试验筛选能够高效去除水中DBP的方法,综合考察了各种金属氧化物、活性炭、过氧化氢、零价金属等物质对臭氧氧化DBP的强化作用,最后找出能够经济高效地强化去除水中PAEs等微量有机污染物的零价金属强化氧化工艺,主要工作与研究成果如下:
制备了多种催化剂,并考察了不同种类催化剂存在条件下对臭氧去除水中DBP的影响规律。研究发现,α-FeOOH、γ-Fe2O3、Mn3O4具有一定的强化臭氧去除DBP能力,但强化效果最佳的催化剂γ-Fe2O3对DBP的去除率也只有60.7%;过氧化氢能够大幅度的强化臭氧去除DBP,去除率可达90%以上;纳米TiO2对臭氧氧化DBP的强化效果较好,负载型的纳米二氧化钛强化臭氧氧化对DBP的去除率可达80%以上;活性炭具有一定的强化臭氧氧化去除DBP的能力,但与过氧化氢联用时并没有体现出协同作用。研究发现,零价铁、零价锌对臭氧氧化去除DBP具有良好的强化作用,反应过程中对DBP的去除率可高达90%以上;值得注意的是,在酸性条件下零价铁和零价铜具有强化水中溶解氧去除DBP的能力,臭氧在氧化反应过程中并不是必需的氧化剂。
在零价铁强化臭氧氧化DBP过程中,DBP去除效果受零价铁投量、有机物浓度、溶液pH值等因素的影响,不同pH值条件下对DBP的氧化机理有所差别;中性条件下,零价铁对臭氧的强化作用受叔丁醇的影响,反应过程遵循羟基自由基机理;排除了反应过程中其他铁氧化物的强化作用,认为强化臭氧氧化DBP效率的提高主要是基于零价铁本身的强化能力;水质条件及水中常见阴阳离子、有机物等对零价铁强化臭氧氧化具有一定影响。
零价锌对臭氧氧化DBP具有良好的强化能力,在所选择的实验条件下,当零价锌投量为0.05g/L时即可高效的强化臭氧去除DBP;零价锌投量增大有利于DBP的去除,DBP初始浓度对其去除效率影响不大,溶液pH值影响零价锌强化臭氧氧化的效果。值得注意的是,零价锌强化臭氧氧化过程不受水中碳酸根的影响,叔丁醇存在时对氧化过程的抑制作用也不完全,因此认为该反应过程不完全遵循羟基自由基机理;反应过程中零价锌本身对臭氧的强化起主要作用,但重复利用后效果更好,说明反应过程中零价锌生成了强化活性更高的物质;不同水质对零价锌强化臭氧氧化DBP的效率影响较小,但一些阳离子如钠离子、铵离子、铁离子及低浓度腐殖酸存在可以加快DBP的去除。
在酸性条件下,零价铜具有良好的强化氧化去除水中多种有机物的能力,其强化氧化效果随溶液pH值降低、零价铜投量增加而提高,有机物的去除效率受有机物初始浓度的影响较小;零价铜强化氧化去除水中有机物的过程,排除了吸附、氧化铜以及铜离子的作用,并且能够达到降低TOC、矿化有机物的效果;零价铜强化氧化的反应机理受溶液中酸的影响,用硫酸调pH值时,溶解氧对于零价铜强化氧化去除有机物并不是必需的,反应遵循羟基自由基作用机理;而用盐酸调pH值时,溶解氧对于零价铜强化氧化去除有机物是必需的,反应过程不受羟基自由基抑制剂叔丁醇的影响;水质条件对零价铜强化氧化的效果影响较大,铁离子的加入能加快DBP的去除,而甲醛的加入对DBP的去除起反作用;零价铜重复使用后强化氧化效率提高,反应过程中有铜离子溶出。
零价铁、零价锌强化臭氧氧化工艺可用于实际水源水的处理,提高原水中DOC的去除率,处理后UV254降低,氨氮浓度升高,强化臭氧氧化对分子量为1000～10000之间的有机物的去除效果明显;零价铜强化氧化对原水中的DOC有一定去除,对分子量为1750和3800附近的有机物的去除比较明显;零价铁、零价锌强化臭氧氧化也可以用于废水的处理,在一定程度上提高臭氧去除COD的效率。
With the increasing pollution of water environment, more and more micro-organic pollutants are found in water, especially phthalate acid esters(PAEs), which has been detected widely in water environment and become a kind of prevalent pollutants. PAEs are cancerogenic, teratogenic and mutagenic, which are seriously harmful to human health. PAEs have been listed as the priority pollutants by many countries and widely concerned all over the world. The improvement of drinking water standards and the low removal efficiency of PAEs by conventional water treatment technology make it urgent to develop new water treatment processes and control PAEs in drinking water.
Dibutyl phthalate (DBP) was chosen as a main target pollutant in this experiment which aimed at improving ozonation by the presence of metal oxides, activated carbon, hydrogen peroxide and zero valent metals. The objective of this work is to find a method which is high efficiency, simple and low cost to remove PAEs from drinking water. Results and conclusions include:
Several metal oxides were prepared by different methods, andα-FeOOH,γ-Fe2O3, Mn3O4 were found to have the ability of improving DBP removal efficiency in ozonation, and the best removal efficiency was 60.7% when usingγ-Fe2O3 as the catalyst. Removal efficiency of DBP in ozonation could be enhanced greatly by adding hydrogen peroxide and more than 90% of DBP could be removed. Nanosized titanium dioxide (TiO2) had good performance to improve ozonation efficiency, and the removal efficiency of DBP could reach 80% at least by using supported nanosized TiO2. DBP removal efficiency could also be enhanced to some extent by adding activated carbon into ozonation process, but coupling use of activated carbon and hydrogen peroxide did not show synergistic effect. Zero valent iron (ZVI) and zero valent zinc (ZVZ) had excellent ability to improve ozonation efficiency, and the DBP removal efficiency was more than 90% in the experimental conditions. In acidic condition, DBP could be removed by the presence of ZVI and zero valent copper (ZVC),and ozone was not necessary to present in these two processes.
DBP removal efficiency in the enhanced ozonation by using ZVI was influenced by ZVI dose, DBP concentration and pH. Under different pH conditions, the oxidation mechanisms of DBP were different. Under neutral condition,the ability of improving ozonation efficiency by the presence of ZVI was influenced by the addition of tert-butyl alcohol,which means that the reaction follow hydroxyl radical mechanism. The improvement of DBP ozonation was due to mainly the acceleration effect of ZVI itself, rather than other oxide species. DBP removal efficiency in the enhanced ozonation process using ZVI was influenced by water quality condition, and cations, anions, organic compounds in water to some extents.
ZVZ had good ability to improve the ozonation efficiency of DBP, and 0.05g/L dose of ZVZ was enough to remove DBP effectively under experimental conditions. DBP removal efficiency was enhanced from the increase of ZVZ dose and pH value of the solution, and the DBP initial concentration had little influence on its removal efficiency. The efficiency of ZVZ enhanced ozonation was not inhibited by the presence of carbonate. It is also found that the inhibition of tert-butyl alcohol on this process was uncompleted, so the reaction did not follow hydroxyl radical mechanism entirely. ZVZ itself played the major role in improving ozonation process, but better efficiency was achieved after ZVZ was reused, which means that there are some species with higher activity on improving ozonation during the reaction. Under different water quality conditions, DBP removal efficiency was changed little,but some cations such as Na+, NH4+, Fe2+ and low concentration of humic acid could accelerate the removal of DBP.
Under acidic condition, Zero valent copper (ZVC) had good ability to remove organic compounds from water by using dissolved oxygen. The oxidation efficiency was increased with the decrease of solution pH and the increase of ZVC dose. The initial concentration of organic compounds had a little influence on the removal efficiency. The experiment results excluded the improving effect achieved by the adsorption of ZVC, the presence of copper oxide and copper ion in the ZVC enhanced oxidation process. The TOC was decreased and mineralization was achieved in the oxidation of DEP by the presence of ZVC under acid condition. The reaction mechanism of copper enhanced oxidation process was different when using different type of acids in the experiment. When the solution pH was adjusted by sulfuric acid, dissolved oxygen was not necessary to present for ZVC enhanced oxidation process and the reaction was affected by the presence of tert-butyl alcohol, which means that the reaction follow hydroxyl radical mechanism. When pH was adjusted using hydrochloric acid, dissolved oxygen was necessary to present for the enhanced removal of organic compounds, and the reaction was not influenced by the presence of hydroxyl radical inhibitor-tert butyl alcohol. The efficiency of ZVC enhanced oxidation process was greatly influenced by the water quality condition, and the addition of iron ion could speed up the removal of DBP,but the addition of methanal inhibit the removal of DBP. After ZVC was reused, its ability of improving the oxidation process increased, and copper ion was released in the reaction process.
ZVI and ZVZ enhanced ozonation can be used in the treatment of source water. The TOC and UV254 were reduced in ZVI and ZVZ enhanced ozonation process and ammonia nitrogen concentration was increased. Organic compounds with a molecular weight of 1000～10000 was removed obviously in ZVI and ZVZ enhanced ozonation process, and Organic compounds with a molecular weight about 1750 and 3800 was removed obviously in ZVC enhanced oxidation process under acidic condition. ZVI and ZVZ enhanced ozonation process could also be used in the treatment of wastewater to increase the removal efficiency of COD.
引文
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