混凝—水解/好氧MBBR-Fenton法处理抗生素发酵废水研究
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摘要
对于多数制药企业来说,高浓度制药废水因其成分复杂、有机物含量高、色度深、可生化性差,难以被微生物降解,采用单一的水处理技术往往难以达到理想的效果。因此,当前急需开发一套对这类废水行之有效的处理新工艺,使其满足越来越严格的排放标准。本文根据哈尔滨某制药厂某车间排放的抗生素发酵废水水质(COD为14700~17600mg·L~(-1);BOD5/COD为0.25~0.26),研究采用混凝-水解酸化/好氧移动床生物膜-Fenton法来处理该废水。
首先进行了混凝法处理高浓度制药废水的实验研究。根据抗生素发酵废水中胶体的带电性质,选用和比较了六种混凝剂的处理效果;并对筛选出的混凝剂PFS从pH值、投加量、搅拌时间和沉淀时间等几方面考察了其对COD去除效果的影响;采用SEM、TEM、FT-IR以及XRD等对筛选出的混凝剂进行形貌表征,初步探讨了混凝剂形貌与混凝机理之间的联系;通过对混凝后絮体形貌的观测,研究了混凝的分形维数与絮体沉降性能的关系;通过考察不同粒径颗粒物的分布,研究了不同粒径颗粒的沉降速率对固液分离的影响。得出混凝最佳工艺参数如下: PFS最优投加量为135.26mg/gCOD,废水初始pH为4.0左右,快速搅拌(300r·min~(-1))时间为1min,慢速搅拌(50r·min~(-1))时间为12min,沉降时间为60min。在最优混凝工艺条件下,废水经过混凝处理后COD和SS去除率分别达到62.2%和88.2%,有机负荷大大降低,但B/C仅仅由0.25提高至0.28。
研究了水解酸化-好氧MBBR法处理抗生素发酵废水工艺。包括水解酸化-好氧MBBR反应器的启动研究;水解酸化反应器的pH、HRT和OLR等工艺参数进行了优化;好氧反应器的HRT、曝气量和OLR等工艺参数进行了优化;水解酸化-好氧MBBR反应器内微生物相表征及生物膜形貌的表征。采用SEM对水解酸化菌和好氧菌的生物相进行了表征;采用电子显微镜对好氧反应器内悬浮填料的生物膜厚度进行了测定,并采用计算流体力学软件Fluent对填料内部流化状态进行了数值模拟,初步探讨了悬浮填料内部流场分布与生物膜厚度的关系。实验结果表明,在抗生素废水进水COD浓度为6000～7000mg·L~(-1)条件下,经水解-好氧MBBR串联工艺处理,COD总去除率可达93.09%,最终出水COD浓度为449.3mg·L~(-1)。水解酸化反应哈尔滨工业大学工学博士学位论文器进水pH在5.5～7.0范围内,适宜水解酸化菌生存,有利于水解反应进行。在pH为6.5时,水解效果最高,VFA产量达到741.12mg·L~(-1),水解酸化率为11.4%,水解段COD去除率为15.38%。在HRT为12h,水解段效果最佳,VFA产量高达931.75mg·L~(-1),水解酸化率为14.33%,COD去除率为26.59%,B/C由0.28提升到0.40,有利于后段处理。进水pH和HRT对生物系统处理效果影响很大,但对水解发酵类型和酸化产物影响较小。本试验中,水解出水中VFA均以乙酸为主,丙酸次之,丁酸、戊酸产量较低。好氧MBBR反应器在HRT为12h,好氧段效果最佳,COD去除率为89.6%;当曝气量为1.5m3·h-1时,好氧段效果最佳,COD去除率为91%。水解酸化-好氧MBBR适宜的有机负荷率应为13kgCOD·(m3·d)-1。生物膜生物相分析表明,水解酸化细菌主要为杆菌呈长杆状;好氧菌多为球状菌和短杆菌。好氧生物膜厚度要比水解酸化生物膜厚度厚的多,好氧生物膜平均生物膜厚度为1.0~1.2mm,且厚度不均匀。填料内流速分布与生物膜厚度分布一致,因此生物膜厚度的分布可以通过Fluent软件进行模拟预测。
研究了移动床生物膜处理抗生素发酵废水的好氧生化动力学,建立了新模型,即S=(S0-Sn)exp(-K2Xt)+Sn。通过不同初始浓度和不同填料填充比下的实验数据模拟结果表明该模型能够描述生物膜法处理抗生素发酵废水的生物降解过程,其动力学参数K2能够直观地反映底物的降解速率,Sn可以作为抗生素发酵废水的可生化性和可降解程度的评价指标。
研究了不同类型Fenton体系对抗生素发酵废水的处理效果。对经典Fenton工艺的初始Fe2+浓度、H2O2浓度、pH、反应时间、沉淀pH、载气以及H2O2等操作参数进行了优化;研究了Fenton过程的反应动力学;通过采用EPR法对不同Fenton体系的羟基自由基进行了测定;进行了Fenton连续流实验,并给出整个工艺不同工段进出水水质的比较分析;最后对不同组合工艺进行了比较与评价。通过实验研究得出Fenton工艺的最佳工艺参数如下:废水初始pH为3.0、初始Fe2+浓度为60.8mg·L~(-1)、H2O2投加量为1/2理论投加量(Qth),以空气为载气,反应3h,然后调节废水至7.0沉降出水,其中Fe2+和H2O2在反应开始1h内平均分三次投加。在该工艺条件下,COD去除率可达80.0%。本文最后通过对三种不同组合工艺的比较,给出了不同组合工艺的适用范围。对于本实验所处理抗生素发酵废水应采用PFS混凝-水解酸化/好氧MBBR-Fenton法处理较为适宜。
As for most pharmaceutical enterprises, high concentration pharmaceutical wastewater is one kind of refractory industry wastewater due to the complicated components, high quantity organic compounds, deep color and low biodegradability. Furthermore, it is difficult to biodegrade the antibiotic wastewater and single wastewater treatment has been imperfect. Hence, it is imperative to develop a series effective new process for wastewater treatment, which can meet the increasing strict discharge standards. The combined coagulation-hydrolysis/oxidation MBBR-Fenton process was adopted for the treatment of high concentration antibiotic fermentation wastewater which was originated from a workshop of some pharmaceutical factory of Harbin (COD 14700~17600mg·L~(-1); BOD5/COD ratio 0.25~0.26).
According to colloid charge charactes in antibiotic fermentation wastewater, the coagulation efficiencies of six kinds of selected coagulants were compared. The results indicated that Polyferric Sulfate (PFS) was the best compared to the others, so it was chosen as the coagulant for the pharmaceutical wastewater. The effects of PFS dosage, initial pH, strring time and settling time in coagulation process were investigated. The relationship between PFS coagulation mechanisms and PFS modalities were discussed by SEM, TEM, FT-IR and XRD characterization of PFS. The effects of the fractal dimension of PFS floccules and the distribution of different size particles after coagulation to sedimentation performances were also studied. The optimal operational parameters of coagulation were determined as follows: PFS dosage of 135.26mg/gCOD, initial pH of 4.0 around, high speed agitation of 300r·min-1 with 1min, low speed agitation of 50r·min-1 with 12min and sedimentation time of 60min. After coagulation, 62.2% COD and 88.2% SS removal were achieved, and the organic load was evidently decreased, but B/C ratio only increased from 0.25 to 0.28.
Hydrolysis/aerobic MBBR were applied to treat antibiotic fermentation wastewater, and the correlative operational parameters were investigated. The start of hydrolysis/aerobic MBBR was studied. On the one hand, the pH,HRT and OLR of hydrolysis MBBR were optimized; On the other hand, the HRT, aeration rate and OLR of aerobic MBBR were also optimized. The microorganisms and biofilms which were in hydrolysis/aerobic MBBR were observed. Hydrolysis/acidification bacteria and aerobic bacteria were characterized by SEM. The thickness of biofilm that was in aerobic MBBR carries was measured, and then flow status which was inside carries were simulated by the computed fluid dynamics software Fluent. The simulated results were used to analyze the relationship between distributions of flow field and distributions of biofilm thickness. The experimental results showed when COD of influent were 6000~7000mg·L~(-1), the COD removal efficiency could reach 93.09% after series hydrolysis/oxidation MBBR treatment. And the final COD of effluent was 449.3mg·L~(-1). In addition, when the pH was in 5.5-7.0 range, the hydrolysis/acidification bacteria were suitable to survive, i.e., it would be good at hydrolysis reaction. At pH 6.5, the hydrolysis efficiency was upmost, and the VFAs production could reach 741.12mg·L~(-1) accompanying with 11.4% acidification degree and 15.38% of COD removal. At HRT 12h,the hydrolysis efficiency was optimum, and B/C was improved from 0.28 to 0.40 accompanying with 931.75mg·L~(-1) of VFAs, 14.33% acidification degree and 26.59% of COD removal, which were very benefit for the latter biological treatment. Although the pH and HRT were influenced the treatment efficiency, the type of hydrolysis was not changed basically. Acetate was the main composition of VFAs. The Propionate was the second, butyrate and valerate were lowest. At HRT 12h of aerobic MBBR, the COD removal efficiency could reach 89.6%. At aeration rate 1.5m~3·h~(-1), the COD removal efficiency could reach 91%. The feasible OLR of whole MBBR process was 13kgCOD·(m3·d)~(-1). The results of biofilm measures showed hydrolysis/acidification bacteria mainly were bacilli. From the observations by SEM, some fields mainly contained zoogloea; some fields mainly contained filamentous bacteria. Aerobic bacteria mainly were cocci and short bacilli. From the observations by SEM, some fields mainly contained short bacilli; some fields mainly contained cocci; in addition, some fields mainly contained bacilli and cocci. The experimental results showed the thickness of aerobic biofilms was thicker than hydrolysis/acidification biofilm. The thickness of aerobic biofilms was 1.0~1.2mm and was asymemetry. The simulated results showed the distributions of flow filed of inside carriers in accordance with thickness of biofilms. Hence, it could use the Fluent-software to simulate the distributions of thickness of biofilms.
Batch tests were carried out to investigate the COD degradation kinetics of antibiotic fermentation wastewater by aerobic MBBR and a modified bio-kinetic model was set up to describe the biological reaction, that is, S=(S0-Sn)exp(-K2Xt)+Sn. The experimental results obtained from different initial concentration and different bio-carrier volume showed that the model could well describe the biodegradation of antibiotic fermentation wastewater, and the kinetic parameter K2 could be used as indicator of degradation rate and Sn could be used to estimate the biodegradability of antibiotic fermentation wastewater.
The oxidation effects of three kinds of Fenton systems were compared. The effect of initial Fe2+ dosage, pH, reaction time, agitation time, the sedimentation pH, carrier gas and manner of H2O2 addition were investigated. The kinetics of Fenton process was also studied. The hydroxyl radical of Fenton system were measured by EPR. The continuous running experiments were conducted, and the qualities of influent and effluent in different process were analyzed. The different combined processes were compared and estimated. The Optimum conditions of Fenton process for treating the effluent of coagulation were determined as: adjusting initial pH of wastewater about 3.0, controlling initial Fe2+ concentration of 60.8mg·L~(-1), adding half the stoichiometric calculated quantities (Qth) of H2O2, using air as carrier gas, reacting for 1h, pH was then adjusted to 7.0, in which Fe2+ and H2O2 were added every 20 minutes during the first hour of reaction. Under these conditions, 80% of COD removal was obtained. Finally,the application ranges of different combined processes were given by comparisons. It was feasible to apply coagulation-hydrolysis/aerobic MBBR-Fenton process to treat antibiotic fermentation wastewater.
首先进行了混凝法处理高浓度制药废水的实验研究。根据抗生素发酵废水中胶体的带电性质,选用和比较了六种混凝剂的处理效果;并对筛选出的混凝剂PFS从pH值、投加量、搅拌时间和沉淀时间等几方面考察了其对COD去除效果的影响;采用SEM、TEM、FT-IR以及XRD等对筛选出的混凝剂进行形貌表征,初步探讨了混凝剂形貌与混凝机理之间的联系;通过对混凝后絮体形貌的观测,研究了混凝的分形维数与絮体沉降性能的关系;通过考察不同粒径颗粒物的分布,研究了不同粒径颗粒的沉降速率对固液分离的影响。得出混凝最佳工艺参数如下: PFS最优投加量为135.26mg/gCOD,废水初始pH为4.0左右,快速搅拌(300r·min~(-1))时间为1min,慢速搅拌(50r·min~(-1))时间为12min,沉降时间为60min。在最优混凝工艺条件下,废水经过混凝处理后COD和SS去除率分别达到62.2%和88.2%,有机负荷大大降低,但B/C仅仅由0.25提高至0.28。
研究了水解酸化-好氧MBBR法处理抗生素发酵废水工艺。包括水解酸化-好氧MBBR反应器的启动研究;水解酸化反应器的pH、HRT和OLR等工艺参数进行了优化;好氧反应器的HRT、曝气量和OLR等工艺参数进行了优化;水解酸化-好氧MBBR反应器内微生物相表征及生物膜形貌的表征。采用SEM对水解酸化菌和好氧菌的生物相进行了表征;采用电子显微镜对好氧反应器内悬浮填料的生物膜厚度进行了测定,并采用计算流体力学软件Fluent对填料内部流化状态进行了数值模拟,初步探讨了悬浮填料内部流场分布与生物膜厚度的关系。实验结果表明,在抗生素废水进水COD浓度为6000～7000mg·L~(-1)条件下,经水解-好氧MBBR串联工艺处理,COD总去除率可达93.09%,最终出水COD浓度为449.3mg·L~(-1)。水解酸化反应哈尔滨工业大学工学博士学位论文器进水pH在5.5～7.0范围内,适宜水解酸化菌生存,有利于水解反应进行。在pH为6.5时,水解效果最高,VFA产量达到741.12mg·L~(-1),水解酸化率为11.4%,水解段COD去除率为15.38%。在HRT为12h,水解段效果最佳,VFA产量高达931.75mg·L~(-1),水解酸化率为14.33%,COD去除率为26.59%,B/C由0.28提升到0.40,有利于后段处理。进水pH和HRT对生物系统处理效果影响很大,但对水解发酵类型和酸化产物影响较小。本试验中,水解出水中VFA均以乙酸为主,丙酸次之,丁酸、戊酸产量较低。好氧MBBR反应器在HRT为12h,好氧段效果最佳,COD去除率为89.6%;当曝气量为1.5m3·h-1时,好氧段效果最佳,COD去除率为91%。水解酸化-好氧MBBR适宜的有机负荷率应为13kgCOD·(m3·d)-1。生物膜生物相分析表明,水解酸化细菌主要为杆菌呈长杆状;好氧菌多为球状菌和短杆菌。好氧生物膜厚度要比水解酸化生物膜厚度厚的多,好氧生物膜平均生物膜厚度为1.0~1.2mm,且厚度不均匀。填料内流速分布与生物膜厚度分布一致,因此生物膜厚度的分布可以通过Fluent软件进行模拟预测。
研究了移动床生物膜处理抗生素发酵废水的好氧生化动力学,建立了新模型,即S=(S0-Sn)exp(-K2Xt)+Sn。通过不同初始浓度和不同填料填充比下的实验数据模拟结果表明该模型能够描述生物膜法处理抗生素发酵废水的生物降解过程,其动力学参数K2能够直观地反映底物的降解速率,Sn可以作为抗生素发酵废水的可生化性和可降解程度的评价指标。
研究了不同类型Fenton体系对抗生素发酵废水的处理效果。对经典Fenton工艺的初始Fe2+浓度、H2O2浓度、pH、反应时间、沉淀pH、载气以及H2O2等操作参数进行了优化;研究了Fenton过程的反应动力学;通过采用EPR法对不同Fenton体系的羟基自由基进行了测定;进行了Fenton连续流实验,并给出整个工艺不同工段进出水水质的比较分析;最后对不同组合工艺进行了比较与评价。通过实验研究得出Fenton工艺的最佳工艺参数如下:废水初始pH为3.0、初始Fe2+浓度为60.8mg·L~(-1)、H2O2投加量为1/2理论投加量(Qth),以空气为载气,反应3h,然后调节废水至7.0沉降出水,其中Fe2+和H2O2在反应开始1h内平均分三次投加。在该工艺条件下,COD去除率可达80.0%。本文最后通过对三种不同组合工艺的比较,给出了不同组合工艺的适用范围。对于本实验所处理抗生素发酵废水应采用PFS混凝-水解酸化/好氧MBBR-Fenton法处理较为适宜。
As for most pharmaceutical enterprises, high concentration pharmaceutical wastewater is one kind of refractory industry wastewater due to the complicated components, high quantity organic compounds, deep color and low biodegradability. Furthermore, it is difficult to biodegrade the antibiotic wastewater and single wastewater treatment has been imperfect. Hence, it is imperative to develop a series effective new process for wastewater treatment, which can meet the increasing strict discharge standards. The combined coagulation-hydrolysis/oxidation MBBR-Fenton process was adopted for the treatment of high concentration antibiotic fermentation wastewater which was originated from a workshop of some pharmaceutical factory of Harbin (COD 14700~17600mg·L~(-1); BOD5/COD ratio 0.25~0.26).
According to colloid charge charactes in antibiotic fermentation wastewater, the coagulation efficiencies of six kinds of selected coagulants were compared. The results indicated that Polyferric Sulfate (PFS) was the best compared to the others, so it was chosen as the coagulant for the pharmaceutical wastewater. The effects of PFS dosage, initial pH, strring time and settling time in coagulation process were investigated. The relationship between PFS coagulation mechanisms and PFS modalities were discussed by SEM, TEM, FT-IR and XRD characterization of PFS. The effects of the fractal dimension of PFS floccules and the distribution of different size particles after coagulation to sedimentation performances were also studied. The optimal operational parameters of coagulation were determined as follows: PFS dosage of 135.26mg/gCOD, initial pH of 4.0 around, high speed agitation of 300r·min-1 with 1min, low speed agitation of 50r·min-1 with 12min and sedimentation time of 60min. After coagulation, 62.2% COD and 88.2% SS removal were achieved, and the organic load was evidently decreased, but B/C ratio only increased from 0.25 to 0.28.
Hydrolysis/aerobic MBBR were applied to treat antibiotic fermentation wastewater, and the correlative operational parameters were investigated. The start of hydrolysis/aerobic MBBR was studied. On the one hand, the pH,HRT and OLR of hydrolysis MBBR were optimized; On the other hand, the HRT, aeration rate and OLR of aerobic MBBR were also optimized. The microorganisms and biofilms which were in hydrolysis/aerobic MBBR were observed. Hydrolysis/acidification bacteria and aerobic bacteria were characterized by SEM. The thickness of biofilm that was in aerobic MBBR carries was measured, and then flow status which was inside carries were simulated by the computed fluid dynamics software Fluent. The simulated results were used to analyze the relationship between distributions of flow field and distributions of biofilm thickness. The experimental results showed when COD of influent were 6000~7000mg·L~(-1), the COD removal efficiency could reach 93.09% after series hydrolysis/oxidation MBBR treatment. And the final COD of effluent was 449.3mg·L~(-1). In addition, when the pH was in 5.5-7.0 range, the hydrolysis/acidification bacteria were suitable to survive, i.e., it would be good at hydrolysis reaction. At pH 6.5, the hydrolysis efficiency was upmost, and the VFAs production could reach 741.12mg·L~(-1) accompanying with 11.4% acidification degree and 15.38% of COD removal. At HRT 12h,the hydrolysis efficiency was optimum, and B/C was improved from 0.28 to 0.40 accompanying with 931.75mg·L~(-1) of VFAs, 14.33% acidification degree and 26.59% of COD removal, which were very benefit for the latter biological treatment. Although the pH and HRT were influenced the treatment efficiency, the type of hydrolysis was not changed basically. Acetate was the main composition of VFAs. The Propionate was the second, butyrate and valerate were lowest. At HRT 12h of aerobic MBBR, the COD removal efficiency could reach 89.6%. At aeration rate 1.5m~3·h~(-1), the COD removal efficiency could reach 91%. The feasible OLR of whole MBBR process was 13kgCOD·(m3·d)~(-1). The results of biofilm measures showed hydrolysis/acidification bacteria mainly were bacilli. From the observations by SEM, some fields mainly contained zoogloea; some fields mainly contained filamentous bacteria. Aerobic bacteria mainly were cocci and short bacilli. From the observations by SEM, some fields mainly contained short bacilli; some fields mainly contained cocci; in addition, some fields mainly contained bacilli and cocci. The experimental results showed the thickness of aerobic biofilms was thicker than hydrolysis/acidification biofilm. The thickness of aerobic biofilms was 1.0~1.2mm and was asymemetry. The simulated results showed the distributions of flow filed of inside carriers in accordance with thickness of biofilms. Hence, it could use the Fluent-software to simulate the distributions of thickness of biofilms.
Batch tests were carried out to investigate the COD degradation kinetics of antibiotic fermentation wastewater by aerobic MBBR and a modified bio-kinetic model was set up to describe the biological reaction, that is, S=(S0-Sn)exp(-K2Xt)+Sn. The experimental results obtained from different initial concentration and different bio-carrier volume showed that the model could well describe the biodegradation of antibiotic fermentation wastewater, and the kinetic parameter K2 could be used as indicator of degradation rate and Sn could be used to estimate the biodegradability of antibiotic fermentation wastewater.
The oxidation effects of three kinds of Fenton systems were compared. The effect of initial Fe2+ dosage, pH, reaction time, agitation time, the sedimentation pH, carrier gas and manner of H2O2 addition were investigated. The kinetics of Fenton process was also studied. The hydroxyl radical of Fenton system were measured by EPR. The continuous running experiments were conducted, and the qualities of influent and effluent in different process were analyzed. The different combined processes were compared and estimated. The Optimum conditions of Fenton process for treating the effluent of coagulation were determined as: adjusting initial pH of wastewater about 3.0, controlling initial Fe2+ concentration of 60.8mg·L~(-1), adding half the stoichiometric calculated quantities (Qth) of H2O2, using air as carrier gas, reacting for 1h, pH was then adjusted to 7.0, in which Fe2+ and H2O2 were added every 20 minutes during the first hour of reaction. Under these conditions, 80% of COD removal was obtained. Finally,the application ranges of different combined processes were given by comparisons. It was feasible to apply coagulation-hydrolysis/aerobic MBBR-Fenton process to treat antibiotic fermentation wastewater.
引文
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4 I. Arslan-Alaton, S. Dogruel. Pre-treatment of Penicillin Formulation Effluent by Advanced Oxidation Processes. Journal of Hazardous Materials. 2004, 112(1-2): 105~113
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