类Fenton降解阿莫西林及固定化微生物降解甲基橙废水的研究
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摘要
随着抗生素和染料工业的发展,抗生素废水与染料废水成为了目前水体环境中备受关注的两类污染物,其共同特点是成分复杂、处理难度大,因此,开发新型有效的处理技术尤为重要。为了减少对机理研究的干扰,分别选取两类废水中的典型代表阿莫西林和甲基橙作为本文的目标降解物。旨在寻求高效的降解工艺,探讨两类废水的降解机理,以期为两类实际废水的有效治理提供基础数据、理论指导和应用参考。本研究主要包括以下几个方面的内容：
(1)电-Fe3+(EDTA)/H2O2处理阿莫西林废水的研究。试验结果表明,在初始中性条件下pH7.0(±0.1), EDTA和电流的引入使阿莫西林降解率和CODcr去除率分别得到提高。在电-Fe3+(EDTA)/H2O2体系中,阿莫西林降解率为86.0%, CODcr去除率为78.0%；在Fe3+(EDTA)/H2O2体系中,阿莫西林降解率为70.0%, CODcr去除率为64.0%；而在电-Fe3+/H2O2体系中,阿莫西林降解率仅为47.0%, CODcr去除率仅为33.0%。三个体系中生物可降解性(BOD5/CODcr)分别为0.12(电-Fe3+/H2O2),0.40(Fe3+(EDTA)/H2O2和0.48(电-Fe3+(EDTA)/H2O2)。结果表明,由于EDTA和电流的协同催化效应,提高了Fe3+的溶解性和循环利用的反应活性,从而提高了阿莫西林降解效率和生化性能,有效拓展了Fenton试剂的pH范围。此外,还探讨了H2O2和EDTA的作用机理,并利用红外光谱(Infrared spectra, IR)分析了阿莫西林可能的降解途径。
(2) UV-Fe3+(EDTA)/H2O2处理阿莫西林废水的研究。在初始中性条件下,相对于UV-Fe3+/H2O2体系,阿莫西林去除率从59.0%提高到100%,生物可降解性从0.25提高到0.45,CODcr去除率从43.0%提高到81.9%,而在Fe3+/H2O2体系中,阿莫西林和CODcr去除率仅为39.6%和31.3%。此外,针对UV-Fe3+(EDTA)/H2O2体系,探讨了H2O2和EDTA的作用机理以及阿莫西林的降解特性,并利用高效液相色谱-质谱联用技术(HPLC-MS)对其降解产物进行了分析,提出了阿莫西林降解途径。结果表明,在该体系中,EDTA既是催化剂也是反应物,避免了EDTA带来二次环境污染的可能性,有助于Fenton试剂在中性条件下去除废水中的阿莫西林。
(3)采用夹层培养法(菌株在固体培养基夹层中生长),从活性污泥中成功地分离了一株甲基橙降解菌株,经过菌落形态特征、细胞形态特征、生理生化特性实验、特征吸收光谱和分子生物学分析,初步鉴定为一株具有菌绿素a(bacteriochlorophylla)和类胡萝卜素(carotenoid)的新型戴尔福特菌属(Delfiiasp.),其基因库Genebank登录号为HQ659695。结果表明,菌株生长和降解试验的优化条件均为：pH7.0,光照强度3000lx,反应温度30℃,溶解氧浓度0—0.5mg/L在此条件下,通过96h的降解反应,甲基橙脱色率可以达到100%(甲基橙初始浓度≤500mg/L)。然而,随着甲基橙初始浓度的增加,对菌株的抑制作用增强,降解效率下降。
(4)为了提高菌株对高浓度甲基橙的降解性能,分别采用海藻酸钠,二氧化钛/海藻酸钠(TiO2/SA)以及硅藻土/海藻酸钠(Si/SA)三个固定化包埋体系对菌株进行固定,甲基橙初始浓度选为1000mg/L。试验结果表明,TiO2和硅藻土可以有效地提高固定化小球的机械强度和稳定性,从而有利于细菌的生长和保持稳定的连续降解性能,因此提高了脱色率和CODcr去除率。在海藻酸钠固定化体系中,脱色率和CODcr去除率分别为76.5%和35.6%,而在TiO2/SA和Si/SA固定化体系中脱色率和CODcr去除率分别达到100%和52.7%,100%和56.7%。此外,对Ti02/海藻酸钠(TiO2/SA)和硅藻土/海藻酸钠(Si/SA)固定化体系的降解机理进行了研究,分别提出了降解途径。在TiO2/SA固定化体系中,发现光化学催化和微生物降解作用协同于甲基橙的降解；在硅藻土/海藻酸钠(Si/SA)体系中,生物降解和化学吸附机理同时存在于降解过程中。由此可知,两个改进后的固定化体系均有效地提高了海藻酸钠固定化体系的性能。此外,试验结果还表明,降解过程中细菌本身固有的明亮颜色和固定化小球颜色变化可以定性地判断甲基橙的降解效率,为甲基橙提供了新的可视化降解途径。
本课题的研究分别为阿莫西林和甲基橙废水提出了新型有效的处理方法,同时为抗生素废水及偶氮型染料废水的研究提供了新的探索方向。研究结果丰富了现有的类Fenton和微生物固定化技术,并可能开发出简单的生化协同降解工艺,为难降解废水的处理提供了新的思路与方法。因此,具有重要的理论意义和应用前景。
With the development of antibiotics and dyes industries, antibiotics and dye wastewater have constructed two major pollution resources in the current water environment, which are difficult to handle due to the complicated ingredients and the toxic/refractory properties. Therefore, it is crucial to investigate novel and effective treatment technologies for the degradation of antibiotics and dyes wastewater. To reduce the interference in the study of the mechanisms, amoxicillin and methyl orange are selected as the model contaminations of antibiotics and dyes wastewater, respectively. It is expect to provide available references to theorey and application for the treatment of the real wastewater of antibiotics and dyes. The investigations are mainly involved in the following respects:
(1) Three oxidation processes for amoxicillin wastewater pretreatment such as Electro-Fe3+(EDTA)/H2O2(EDTA:ethylenediaminetetraacetic acid), Fe3+(EDTA)/H2O2and Electro-Fe3+/H2O2were simultaneously discussed at initial pH of7.0(±0.1). It was found that the above processes could achieve78.0%,64.0%,33.0%chemical oxygen demand (CODcr) removal, and86.0%,70.0%,47.0%amoxicillin degradation respectively. Moreover, the results of biodegradability (biological oxygen demand (BOD5)/CODcr ratio) showed that the Electro-Fe3+(EDTA)/H2O2process was a promising way to pretreat antibiotic wastewater due to the biodegradability of the effluent improved to0.48compared with the cases of Fe3+(EDTA)/H2O2(0.40) and Electro-Fe3+/H2O2process (0.12). Therefore, it was reasonable to note that EDTA and electricity showed synergetic effect on the oxidation process. Additionally, Infrared Spectra (IR) was applied to concisely propose a potential degradation way of amoxicillin. The characteristic changes of H2O2and EDTA in the oxidation process were also investigated in detail.
(2) Three oxidation processes of UV-Fe3+(EDTA)/H2O2(UV:ultraviolet light), UV-Fe3+/H2O2and Fe3+/H2O2were simultaneously investigated for the degradation of amoxicillin at initial pH of7.0(±0.1). The results indicated that,100%amoxicillin degradation and81.9%chemical oxygen demand (CODcr) removal could be achieved in the UV-Fe3+(EDTA)/H2O2process. The treatment efficiency of amoxicillin and CODcr removal were found to decrease to59.0%and43.0%in the UV-Fe3+/H2O2process;39.6%and31.3%in the Fe3+/H2O2process, respectively. Moreover, the results of biodegradability (biological oxygen demand (BOD5)/CODcr ratio) revealed that the UV-Fe3+(EDTA)/H2O2process was a promising strategy to degrade amoxicillin as the biodegradability of the effluent was improved to0.45, compared with the cases of UV-Fe3+/H2O2(0.25) and Fe3+/H2O2process (0.10). Therefore, it could be deduced that EDTA and UV light performed synergetic catalytic effect on the Fe3+/H2O2process, enhancing the treatment efficiency. Finally, the degradation mechanisms were investigated via UV-vis spectra, and High Performance Liquid Chromatography-Mass Spectra (HPLC-MS), and the degradation pathway of amoxicillin was further proposed.
(3) A novel species of methyl orange-biodegrading strain was successfully isolated by means of layer plating method. The identification and degradation characteristics of the strain were investigated as well. The strain showed biodegradability of methyl orange, which contains photosynthetic pigments bacteriochlorophyll a and carotenoid. Based on morphological and phylogenetic analysis, it could be deduced that strain might be a new genus of Delftia sp. The complete sequence of the strain had been deposited in the Gene Bank database under accession number HQ659695. The results showed that the conditions of both the growth of Delftia sp. and the biodegradation of methyl orange were optimized as pH of7.0, illumination intensity of3000lx, temperature of30℃, and dissovled oxygen (DO) of0-0.5mg/L. Under the optimal conditions,100%decolorization efficiency of methyl orange could be achieved when the initial concentration of methyl orange was lower than500mg/L. The results further revealed that the decolorization efficiency decreased when the concentration of methyl orange kept on increasing.
(4) To enhance the biodegradability of Delftia sp. STT01HQ659695for methyl orange of higher concentration, three immobilized systems were carried out namely sodium alginate immobilized system (SA), TiO2modified sodium alginate immobilized system (TiO2/SA) and diatomite modified sodium alginate immobilized system (Si/SA). In the SA system,76.5%decolorization and35.6%CODcr removal efficiencies were achieved when the initial concentration of methyl orange was1000mg/L. And the treatment efficiencies were improved to100%and52.7%in the TiO2/SA immobilized system, and100%and56.7%in the Si/SA immobilized system, respectively. The results revealed that TiO2and diatomite could markedly enhance the performances of the sodium alginate (SA) immobilized system, which were responsible for modifying mass transfer, mechanical strength and better stability of the immobilized pellets due to the more active biomass, enhancing the treatment efficiencies. It was found that TiO2photo-catalytic process involving hydroxyl radical or other activated media, together with the microbial process might simultaneously lead to the degradation of methyl orange; whereas both biodegradation and chemiadsorption were responsible for the removal of methyl orange simultaneously in the Si/SA immobilized system. The results further revealed that the intrinsic bright color of the immobilized pellets could also be ingeniously employed as an indicator for the degradation efficiency. This work not only affords a direct and visualization treatment effect for methyl orange but also opens a promising entry for developing novel immobilized techniques for the treatment of azo dye wastewater.
Moreover, the work provides novel treatment methods for the degradation of amoxicillin and methyl orange, which also offer a promising abiotic-biotic process for wastewater treatment. The results of this work enrich the current Fenton like process and microorganisms immobilization technology as well. Therefore, this study has both theoretical significance and wide foreground of application.
(1)电-Fe3+(EDTA)/H2O2处理阿莫西林废水的研究。试验结果表明,在初始中性条件下pH7.0(±0.1), EDTA和电流的引入使阿莫西林降解率和CODcr去除率分别得到提高。在电-Fe3+(EDTA)/H2O2体系中,阿莫西林降解率为86.0%, CODcr去除率为78.0%；在Fe3+(EDTA)/H2O2体系中,阿莫西林降解率为70.0%, CODcr去除率为64.0%；而在电-Fe3+/H2O2体系中,阿莫西林降解率仅为47.0%, CODcr去除率仅为33.0%。三个体系中生物可降解性(BOD5/CODcr)分别为0.12(电-Fe3+/H2O2),0.40(Fe3+(EDTA)/H2O2和0.48(电-Fe3+(EDTA)/H2O2)。结果表明,由于EDTA和电流的协同催化效应,提高了Fe3+的溶解性和循环利用的反应活性,从而提高了阿莫西林降解效率和生化性能,有效拓展了Fenton试剂的pH范围。此外,还探讨了H2O2和EDTA的作用机理,并利用红外光谱(Infrared spectra, IR)分析了阿莫西林可能的降解途径。
(2) UV-Fe3+(EDTA)/H2O2处理阿莫西林废水的研究。在初始中性条件下,相对于UV-Fe3+/H2O2体系,阿莫西林去除率从59.0%提高到100%,生物可降解性从0.25提高到0.45,CODcr去除率从43.0%提高到81.9%,而在Fe3+/H2O2体系中,阿莫西林和CODcr去除率仅为39.6%和31.3%。此外,针对UV-Fe3+(EDTA)/H2O2体系,探讨了H2O2和EDTA的作用机理以及阿莫西林的降解特性,并利用高效液相色谱-质谱联用技术(HPLC-MS)对其降解产物进行了分析,提出了阿莫西林降解途径。结果表明,在该体系中,EDTA既是催化剂也是反应物,避免了EDTA带来二次环境污染的可能性,有助于Fenton试剂在中性条件下去除废水中的阿莫西林。
(3)采用夹层培养法(菌株在固体培养基夹层中生长),从活性污泥中成功地分离了一株甲基橙降解菌株,经过菌落形态特征、细胞形态特征、生理生化特性实验、特征吸收光谱和分子生物学分析,初步鉴定为一株具有菌绿素a(bacteriochlorophylla)和类胡萝卜素(carotenoid)的新型戴尔福特菌属(Delfiiasp.),其基因库Genebank登录号为HQ659695。结果表明,菌株生长和降解试验的优化条件均为：pH7.0,光照强度3000lx,反应温度30℃,溶解氧浓度0—0.5mg/L在此条件下,通过96h的降解反应,甲基橙脱色率可以达到100%(甲基橙初始浓度≤500mg/L)。然而,随着甲基橙初始浓度的增加,对菌株的抑制作用增强,降解效率下降。
(4)为了提高菌株对高浓度甲基橙的降解性能,分别采用海藻酸钠,二氧化钛/海藻酸钠(TiO2/SA)以及硅藻土/海藻酸钠(Si/SA)三个固定化包埋体系对菌株进行固定,甲基橙初始浓度选为1000mg/L。试验结果表明,TiO2和硅藻土可以有效地提高固定化小球的机械强度和稳定性,从而有利于细菌的生长和保持稳定的连续降解性能,因此提高了脱色率和CODcr去除率。在海藻酸钠固定化体系中,脱色率和CODcr去除率分别为76.5%和35.6%,而在TiO2/SA和Si/SA固定化体系中脱色率和CODcr去除率分别达到100%和52.7%,100%和56.7%。此外,对Ti02/海藻酸钠(TiO2/SA)和硅藻土/海藻酸钠(Si/SA)固定化体系的降解机理进行了研究,分别提出了降解途径。在TiO2/SA固定化体系中,发现光化学催化和微生物降解作用协同于甲基橙的降解；在硅藻土/海藻酸钠(Si/SA)体系中,生物降解和化学吸附机理同时存在于降解过程中。由此可知,两个改进后的固定化体系均有效地提高了海藻酸钠固定化体系的性能。此外,试验结果还表明,降解过程中细菌本身固有的明亮颜色和固定化小球颜色变化可以定性地判断甲基橙的降解效率,为甲基橙提供了新的可视化降解途径。
本课题的研究分别为阿莫西林和甲基橙废水提出了新型有效的处理方法,同时为抗生素废水及偶氮型染料废水的研究提供了新的探索方向。研究结果丰富了现有的类Fenton和微生物固定化技术,并可能开发出简单的生化协同降解工艺,为难降解废水的处理提供了新的思路与方法。因此,具有重要的理论意义和应用前景。
With the development of antibiotics and dyes industries, antibiotics and dye wastewater have constructed two major pollution resources in the current water environment, which are difficult to handle due to the complicated ingredients and the toxic/refractory properties. Therefore, it is crucial to investigate novel and effective treatment technologies for the degradation of antibiotics and dyes wastewater. To reduce the interference in the study of the mechanisms, amoxicillin and methyl orange are selected as the model contaminations of antibiotics and dyes wastewater, respectively. It is expect to provide available references to theorey and application for the treatment of the real wastewater of antibiotics and dyes. The investigations are mainly involved in the following respects:
(1) Three oxidation processes for amoxicillin wastewater pretreatment such as Electro-Fe3+(EDTA)/H2O2(EDTA:ethylenediaminetetraacetic acid), Fe3+(EDTA)/H2O2and Electro-Fe3+/H2O2were simultaneously discussed at initial pH of7.0(±0.1). It was found that the above processes could achieve78.0%,64.0%,33.0%chemical oxygen demand (CODcr) removal, and86.0%,70.0%,47.0%amoxicillin degradation respectively. Moreover, the results of biodegradability (biological oxygen demand (BOD5)/CODcr ratio) showed that the Electro-Fe3+(EDTA)/H2O2process was a promising way to pretreat antibiotic wastewater due to the biodegradability of the effluent improved to0.48compared with the cases of Fe3+(EDTA)/H2O2(0.40) and Electro-Fe3+/H2O2process (0.12). Therefore, it was reasonable to note that EDTA and electricity showed synergetic effect on the oxidation process. Additionally, Infrared Spectra (IR) was applied to concisely propose a potential degradation way of amoxicillin. The characteristic changes of H2O2and EDTA in the oxidation process were also investigated in detail.
(2) Three oxidation processes of UV-Fe3+(EDTA)/H2O2(UV:ultraviolet light), UV-Fe3+/H2O2and Fe3+/H2O2were simultaneously investigated for the degradation of amoxicillin at initial pH of7.0(±0.1). The results indicated that,100%amoxicillin degradation and81.9%chemical oxygen demand (CODcr) removal could be achieved in the UV-Fe3+(EDTA)/H2O2process. The treatment efficiency of amoxicillin and CODcr removal were found to decrease to59.0%and43.0%in the UV-Fe3+/H2O2process;39.6%and31.3%in the Fe3+/H2O2process, respectively. Moreover, the results of biodegradability (biological oxygen demand (BOD5)/CODcr ratio) revealed that the UV-Fe3+(EDTA)/H2O2process was a promising strategy to degrade amoxicillin as the biodegradability of the effluent was improved to0.45, compared with the cases of UV-Fe3+/H2O2(0.25) and Fe3+/H2O2process (0.10). Therefore, it could be deduced that EDTA and UV light performed synergetic catalytic effect on the Fe3+/H2O2process, enhancing the treatment efficiency. Finally, the degradation mechanisms were investigated via UV-vis spectra, and High Performance Liquid Chromatography-Mass Spectra (HPLC-MS), and the degradation pathway of amoxicillin was further proposed.
(3) A novel species of methyl orange-biodegrading strain was successfully isolated by means of layer plating method. The identification and degradation characteristics of the strain were investigated as well. The strain showed biodegradability of methyl orange, which contains photosynthetic pigments bacteriochlorophyll a and carotenoid. Based on morphological and phylogenetic analysis, it could be deduced that strain might be a new genus of Delftia sp. The complete sequence of the strain had been deposited in the Gene Bank database under accession number HQ659695. The results showed that the conditions of both the growth of Delftia sp. and the biodegradation of methyl orange were optimized as pH of7.0, illumination intensity of3000lx, temperature of30℃, and dissovled oxygen (DO) of0-0.5mg/L. Under the optimal conditions,100%decolorization efficiency of methyl orange could be achieved when the initial concentration of methyl orange was lower than500mg/L. The results further revealed that the decolorization efficiency decreased when the concentration of methyl orange kept on increasing.
(4) To enhance the biodegradability of Delftia sp. STT01HQ659695for methyl orange of higher concentration, three immobilized systems were carried out namely sodium alginate immobilized system (SA), TiO2modified sodium alginate immobilized system (TiO2/SA) and diatomite modified sodium alginate immobilized system (Si/SA). In the SA system,76.5%decolorization and35.6%CODcr removal efficiencies were achieved when the initial concentration of methyl orange was1000mg/L. And the treatment efficiencies were improved to100%and52.7%in the TiO2/SA immobilized system, and100%and56.7%in the Si/SA immobilized system, respectively. The results revealed that TiO2and diatomite could markedly enhance the performances of the sodium alginate (SA) immobilized system, which were responsible for modifying mass transfer, mechanical strength and better stability of the immobilized pellets due to the more active biomass, enhancing the treatment efficiencies. It was found that TiO2photo-catalytic process involving hydroxyl radical or other activated media, together with the microbial process might simultaneously lead to the degradation of methyl orange; whereas both biodegradation and chemiadsorption were responsible for the removal of methyl orange simultaneously in the Si/SA immobilized system. The results further revealed that the intrinsic bright color of the immobilized pellets could also be ingeniously employed as an indicator for the degradation efficiency. This work not only affords a direct and visualization treatment effect for methyl orange but also opens a promising entry for developing novel immobilized techniques for the treatment of azo dye wastewater.
Moreover, the work provides novel treatment methods for the degradation of amoxicillin and methyl orange, which also offer a promising abiotic-biotic process for wastewater treatment. The results of this work enrich the current Fenton like process and microorganisms immobilization technology as well. Therefore, this study has both theoretical significance and wide foreground of application.
引文
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