纳滤—厌氧氨氧化—高级氧化工艺深度处理干法腈纶废水研究
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摘要
腈纶生产过程中产生的废水成分复杂,生物降解性差,对环境造成危害较大,是目前废水处理领域的一大难题。以抚顺石化腈纶厂为例,现有处理工艺不能满足处理要求,经过二级生化处理后的尾水中仍含有较高浓度难降解有机物,氨氮和总氮浓度也较高且缺少可被反硝化利用的碳源。面对日益严格的污水排放要求,选择经济有效的后续深度处理工艺是腈纶生产企业的迫切需求。
本研究中,通过对现有污水处理工艺中重要处理单元的水样进行全分析,分析难降解污染物组成,了解各污染物在生物处理工艺过程中的迁移和转化规律。经过现有厌氧-好氧过程处理后,干法腈纶废水(DAFW)中的腈类和酚类可以被生物降解,丙烯腈等含氮有机物降解过程中释放出氨氮,造成生化出水氨氮浓度大幅度升高；而残留的烷烃和腈类低聚物为难以降解的有机物,造成生化出水COD难以达到排放标准。针对腈纶废水氨氮浓度高和COD难以生物降解的特点,并对比多种工艺对腈纶废水的处理效果,提出了“纳滤-亚硝化／厌氧氨氧化-非均相电催化”为主体的深度处理工艺,并通过小试和中试实验验证了工艺的可行性。
实验结果表明,纳滤不但可以有效截留腈纶废水二级生化尾水中的难降解有机物,还可以通过电荷平衡作用同时去除氨氮,使出水基本达到排放标准,同时经纳滤浓缩后可有效减少后续工艺处理水量。温度和TMP等参数均可影响纳滤产水效果,在跨膜压差为0.45-0.6MPa、温度为30-35℃并采用二级过滤的条件下,产水COD和氨氮分别为32mg／L和17mg／L。中试实验中,进水SS严重影响纳滤装置的稳定运行。增加预处理装置去除SS后连续运行时,跨膜压差变化不大,虽然缓慢增加,但始终在0.75MPa以下,说明纳滤系统处理腈纶废水二级生化出水时膜污染较轻。采用物理方法和化学方法对纳滤膜进行清洗和维护,可以有效的减轻膜污染和膜运行阻力。
应用纳滤膜对腈纶废水二级生化尾水分离浓缩后,浓水再分别由亚硝化/厌氧氨氧化(anammox)和非均相电催化工艺进行脱氮除碳。实验采用膜生物反应器来实现亚硝化过程,利用其对微生物的高效截留作用,延长系统中微生物的污泥停留时间,强化亚硝化反应。对比中试和小试实验表明,采用硝化污泥作为优势菌种启动,可以较快的实现完全亚硝化。处理实际废水时NH4+-N去除率和NO2--N/NOX--N比率分别为85%和80%。投加KClO3可以有效控制出水N03--N浓度,并且HRT的缩短有助于强化控制效果。系统稳定运行时N03--N的转化率可以维持在较低水平,基本稳定在30mg/L以下。Anammox批式和小试连续实验表明,anammox工艺处理腈纶废水时其反应速率略有降低,但对厌氧氨氧化菌没有急性毒性和累积抑制作用。中试实验采用高纯度anammox菌接种的生物膜法,并用立体帘式结构无纺布填料进行挂膜,可以实现低接种菌量下的anammox反应器快速启动。在人工培养阶段,运行稳定后NH4+-N和N02--N的去除率分别可以达到90%和95%。与小试实验相比,中试实验处理实际废水时氨氮去除率和总氮去除率均有所下降,分别为85%和73%。现场实验中anammox菌对温度和SS较敏感,并且anammox菌属呈现多样化,由接种时的单一B. anammoxidans sp.转变成Kuenenia sp.为优势菌属,说明在处理腈纶废水的环境下,更有利于Kuenenia sp.的生长。
本实验构建非均相电催化体系,在控制反应时间3h、反应槽压4V,H202的投加量为3mL并采用分段投加方式时,对腈纶废水纳滤浓缩后的浓水处理效果最佳,COD可降解到85mg/L左右,去除率可达到83%。
小试和中试实验结果表明,通过本方案设计工艺对腈纶废水进行深度处理,可以同时有效去除废水中的难降解有机物和NH4+-N。并通过简单成本估算,本方案工艺工程建设总投资为1723万元,吨水运行费用为4.56元,环境效益可观,为实际工程应用提供理论依据和技术支持。
The wastewater from acrylic fiber production process presents significant harms to the enviroment because of its complex components and poor bio-degradation. Nowadays, it is a difficult problem in wastewater treatment field. Illustrated by the example of Fushun acrylic fiber factory of petrochemical company, the present wastewater treatment process could not satisfy the requirement of wastewater discharge standard. After secondary biotreatment process, the concentrations of COD and NH4+-N in effluent are still very high, and there is nearly no removal of TN due to the lack of available organic carbon source for denitrification. In order to meet the more stringent requirement of wastewater discharge standard, it is urgent for related enterprise to find an economical and effective advanced treatment process.
In this study, complete water quality analysis of the important unit samples in present treatment process was carried out, in order to analyze the composition of refractory organic pollutants and investigate the transformation discipline of each kind of pollutant. After the anaerobic and aerobic biological treatment process, most of nitriles and phenols in dry-spun acrylic fiber wastewater (DAFW) could be biodegraded, and some nitrogenous organic compounds such as acrylonitrile degraded and formed ammonia which resulted in a high ammonium concentration in effluent. The composition of residual refractory organic compounds was alkanes and oligomers, which made the effluent COD concentration higher than the discharge standard. According to the characteristics of DAFW and comparison of the effects of several treatment processes, a new advanced treatment process was proposed which integrated nanofiltration, nitritation, anaerobic ammonia oxidation (anammox) and electro-heterogeneous catalytic oxidation. The feasibility of this process was investigated both in lab-scale and pilot-scale
Experimental results showed that refractory organic matter remained in biochemical effluent was retained effectively and the ammonia nitrogen was also removed by the charge balance in the nanofiltration process simultaneously. The effluent basically met the discharge standard. Furthermore the treatment quantity of the subsequent process was reduced significantly by nanofiltration concentration process. The permeate quality of nanofiltration process was affected by operational parameters such as temperature and Trans-Membrane Pressure (TMP). After two stage filtration, COD and ammonia nitrogen concentration of the permeate were32mg/L and17mg/L under TMP of0.45-0.6MPa and the temperature between30-35℃. The pilot test indicated that the SS concentration of the influent had a critical influence on the stable operation of nanofiltration device. After using the pretreatment device to remove SS of the influent, the TMP was always below0.75MPa though it increased slowly during continuous operation. The membrane fouling was lighter when nanofiltration process was sued for advanced treatment of DAFW. The membrane pollution and running resistance could be effectively reduced by cleaning and maintaining nanofiltration membrane with physical and chemical method.
After the nanofiltration process, nitritation/anammox and electro-heterogeneous catalytic oxidation were chosen to remove carbon and nitrogen from the nanofiltration concentrated liquid. The membrane bioreactor was used to realize the nitratation process, for its efficient microbial entrapment effect and longer sludge retention time. Compared with lab experiments, results of pilot tests indicate that the nitritation process could start up quickly when seeding mature nitrifying bacteria. The NHLt+-N removal efficiency and the ratio of NO2--N/NOX--N were85%and0.8, respectively. The addition of KClO3could control NO3--N concentration of the MBR effluent effectively, which could be enhanced with the shorter HRT. The conversion of NO3--N was maintained at relatively low level and the concentration of NO3--N was basically below30mg/L under stable operation period.
The batch and continuous test results of anammox process showed that anammox reaction rate decreased slightly when treating DAFW, but there was no acute toxicity and cumulative inhibition to the anammox bacteria. Fast start-up of anammox reactor with low inoculation sludge was achieved by seeding of high purity anammox bacteria and the utilization of non-woven fabric of cubic stereo shade structure as biofilm carrier. In the artificial culture stage, the removal efficiencies of NH4+-N and NO2--N were maintained at90%and95%, respectively. When treating actual wastewater, anammox bacteria were sensitive to temperature and SS. During the period of stable operation, the removal efficiencies of NH4+-N and TN decreased to85%and73%, respectively. The anammox bacteria genus has diversified, which transformed from single B. Anammoxidans sp. in inoculum to Kuenenia sp. as the predominate bacteria in reactor, which indicated that the condition of treating DAFW benefited the growth of the Kuenenia sp.
The COD removal of nanofiltration concentrated water was achieved by electro-heterogeneous catalytic oxidation process. The COD concentration was decreased to85mg/L and the COD removal efficiency was83%under the operation condition of reaction time3h, voltage4V and H2O2dosage of3mL.
Results of the pilot and lab tests showed that the refractory organic pollutants and NH4+-N in DAFW could be removed effectively by application of the advanced treatment process. Simple cost estimation showed that engineering construction total investment of this process was17.23million RMB and operation cost was4.56yuan/ton.
本研究中,通过对现有污水处理工艺中重要处理单元的水样进行全分析,分析难降解污染物组成,了解各污染物在生物处理工艺过程中的迁移和转化规律。经过现有厌氧-好氧过程处理后,干法腈纶废水(DAFW)中的腈类和酚类可以被生物降解,丙烯腈等含氮有机物降解过程中释放出氨氮,造成生化出水氨氮浓度大幅度升高；而残留的烷烃和腈类低聚物为难以降解的有机物,造成生化出水COD难以达到排放标准。针对腈纶废水氨氮浓度高和COD难以生物降解的特点,并对比多种工艺对腈纶废水的处理效果,提出了“纳滤-亚硝化／厌氧氨氧化-非均相电催化”为主体的深度处理工艺,并通过小试和中试实验验证了工艺的可行性。
实验结果表明,纳滤不但可以有效截留腈纶废水二级生化尾水中的难降解有机物,还可以通过电荷平衡作用同时去除氨氮,使出水基本达到排放标准,同时经纳滤浓缩后可有效减少后续工艺处理水量。温度和TMP等参数均可影响纳滤产水效果,在跨膜压差为0.45-0.6MPa、温度为30-35℃并采用二级过滤的条件下,产水COD和氨氮分别为32mg／L和17mg／L。中试实验中,进水SS严重影响纳滤装置的稳定运行。增加预处理装置去除SS后连续运行时,跨膜压差变化不大,虽然缓慢增加,但始终在0.75MPa以下,说明纳滤系统处理腈纶废水二级生化出水时膜污染较轻。采用物理方法和化学方法对纳滤膜进行清洗和维护,可以有效的减轻膜污染和膜运行阻力。
应用纳滤膜对腈纶废水二级生化尾水分离浓缩后,浓水再分别由亚硝化/厌氧氨氧化(anammox)和非均相电催化工艺进行脱氮除碳。实验采用膜生物反应器来实现亚硝化过程,利用其对微生物的高效截留作用,延长系统中微生物的污泥停留时间,强化亚硝化反应。对比中试和小试实验表明,采用硝化污泥作为优势菌种启动,可以较快的实现完全亚硝化。处理实际废水时NH4+-N去除率和NO2--N/NOX--N比率分别为85%和80%。投加KClO3可以有效控制出水N03--N浓度,并且HRT的缩短有助于强化控制效果。系统稳定运行时N03--N的转化率可以维持在较低水平,基本稳定在30mg/L以下。Anammox批式和小试连续实验表明,anammox工艺处理腈纶废水时其反应速率略有降低,但对厌氧氨氧化菌没有急性毒性和累积抑制作用。中试实验采用高纯度anammox菌接种的生物膜法,并用立体帘式结构无纺布填料进行挂膜,可以实现低接种菌量下的anammox反应器快速启动。在人工培养阶段,运行稳定后NH4+-N和N02--N的去除率分别可以达到90%和95%。与小试实验相比,中试实验处理实际废水时氨氮去除率和总氮去除率均有所下降,分别为85%和73%。现场实验中anammox菌对温度和SS较敏感,并且anammox菌属呈现多样化,由接种时的单一B. anammoxidans sp.转变成Kuenenia sp.为优势菌属,说明在处理腈纶废水的环境下,更有利于Kuenenia sp.的生长。
本实验构建非均相电催化体系,在控制反应时间3h、反应槽压4V,H202的投加量为3mL并采用分段投加方式时,对腈纶废水纳滤浓缩后的浓水处理效果最佳,COD可降解到85mg/L左右,去除率可达到83%。
小试和中试实验结果表明,通过本方案设计工艺对腈纶废水进行深度处理,可以同时有效去除废水中的难降解有机物和NH4+-N。并通过简单成本估算,本方案工艺工程建设总投资为1723万元,吨水运行费用为4.56元,环境效益可观,为实际工程应用提供理论依据和技术支持。
The wastewater from acrylic fiber production process presents significant harms to the enviroment because of its complex components and poor bio-degradation. Nowadays, it is a difficult problem in wastewater treatment field. Illustrated by the example of Fushun acrylic fiber factory of petrochemical company, the present wastewater treatment process could not satisfy the requirement of wastewater discharge standard. After secondary biotreatment process, the concentrations of COD and NH4+-N in effluent are still very high, and there is nearly no removal of TN due to the lack of available organic carbon source for denitrification. In order to meet the more stringent requirement of wastewater discharge standard, it is urgent for related enterprise to find an economical and effective advanced treatment process.
In this study, complete water quality analysis of the important unit samples in present treatment process was carried out, in order to analyze the composition of refractory organic pollutants and investigate the transformation discipline of each kind of pollutant. After the anaerobic and aerobic biological treatment process, most of nitriles and phenols in dry-spun acrylic fiber wastewater (DAFW) could be biodegraded, and some nitrogenous organic compounds such as acrylonitrile degraded and formed ammonia which resulted in a high ammonium concentration in effluent. The composition of residual refractory organic compounds was alkanes and oligomers, which made the effluent COD concentration higher than the discharge standard. According to the characteristics of DAFW and comparison of the effects of several treatment processes, a new advanced treatment process was proposed which integrated nanofiltration, nitritation, anaerobic ammonia oxidation (anammox) and electro-heterogeneous catalytic oxidation. The feasibility of this process was investigated both in lab-scale and pilot-scale
Experimental results showed that refractory organic matter remained in biochemical effluent was retained effectively and the ammonia nitrogen was also removed by the charge balance in the nanofiltration process simultaneously. The effluent basically met the discharge standard. Furthermore the treatment quantity of the subsequent process was reduced significantly by nanofiltration concentration process. The permeate quality of nanofiltration process was affected by operational parameters such as temperature and Trans-Membrane Pressure (TMP). After two stage filtration, COD and ammonia nitrogen concentration of the permeate were32mg/L and17mg/L under TMP of0.45-0.6MPa and the temperature between30-35℃. The pilot test indicated that the SS concentration of the influent had a critical influence on the stable operation of nanofiltration device. After using the pretreatment device to remove SS of the influent, the TMP was always below0.75MPa though it increased slowly during continuous operation. The membrane fouling was lighter when nanofiltration process was sued for advanced treatment of DAFW. The membrane pollution and running resistance could be effectively reduced by cleaning and maintaining nanofiltration membrane with physical and chemical method.
After the nanofiltration process, nitritation/anammox and electro-heterogeneous catalytic oxidation were chosen to remove carbon and nitrogen from the nanofiltration concentrated liquid. The membrane bioreactor was used to realize the nitratation process, for its efficient microbial entrapment effect and longer sludge retention time. Compared with lab experiments, results of pilot tests indicate that the nitritation process could start up quickly when seeding mature nitrifying bacteria. The NHLt+-N removal efficiency and the ratio of NO2--N/NOX--N were85%and0.8, respectively. The addition of KClO3could control NO3--N concentration of the MBR effluent effectively, which could be enhanced with the shorter HRT. The conversion of NO3--N was maintained at relatively low level and the concentration of NO3--N was basically below30mg/L under stable operation period.
The batch and continuous test results of anammox process showed that anammox reaction rate decreased slightly when treating DAFW, but there was no acute toxicity and cumulative inhibition to the anammox bacteria. Fast start-up of anammox reactor with low inoculation sludge was achieved by seeding of high purity anammox bacteria and the utilization of non-woven fabric of cubic stereo shade structure as biofilm carrier. In the artificial culture stage, the removal efficiencies of NH4+-N and NO2--N were maintained at90%and95%, respectively. When treating actual wastewater, anammox bacteria were sensitive to temperature and SS. During the period of stable operation, the removal efficiencies of NH4+-N and TN decreased to85%and73%, respectively. The anammox bacteria genus has diversified, which transformed from single B. Anammoxidans sp. in inoculum to Kuenenia sp. as the predominate bacteria in reactor, which indicated that the condition of treating DAFW benefited the growth of the Kuenenia sp.
The COD removal of nanofiltration concentrated water was achieved by electro-heterogeneous catalytic oxidation process. The COD concentration was decreased to85mg/L and the COD removal efficiency was83%under the operation condition of reaction time3h, voltage4V and H2O2dosage of3mL.
Results of the pilot and lab tests showed that the refractory organic pollutants and NH4+-N in DAFW could be removed effectively by application of the advanced treatment process. Simple cost estimation showed that engineering construction total investment of this process was17.23million RMB and operation cost was4.56yuan/ton.
引文
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