介孔生物填料流化床和蒙脱石吸附混凝工艺脱氮除酚效能
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摘要
焦化废水是一种典型的难降解高酚、高氨氮工业废水,对环境污染严重,而且对人类危害较大。虽然现有的处理方法对废水中的酚、氰、BOD_5具有一定的处理效果,但COD、氨氮及色度等指标一般难以满足排放要求,是我国河流污染的重要污染源之一。本文针对焦化废水处理工艺的研究现状,提出了介孔生物填料流化床与改性蒙脱石吸附混凝的组合工艺,系统地研究了该组合工艺中的介孔生物填料和改性蒙脱石单独对模拟配水及焦化废水中有机物的去除能力及其脱氮性能,进行了组合工艺的小试和实际应用研究,为焦化废水污染问题的解决提供一个可行的方案。
分别以高浓度苯酚配水和实际焦化废水为研究对象,对介孔生物填料流化床对废水的处理性能进行了研究。结果表明,当HRT为20h,pH在6.6~8.1的范围内,溶解氧在1.8~3.7 mg/L之间时,介孔生物填料流化床反应器可对1000~1500mg/L左右的苯酚溶液和COD为1700~4200mg/L的焦化废水进行有效的降解,苯酚去除率可达99.9%以上,COD去除率在80%左右,NH_4~+-N去除率在70%左右,而且该介孔生物填料流化床具有较强的抗冲击能力和自我恢复能力,并在反应器中发现有同步硝化反硝化作用(SND)的存在。正交试验表明对反应器处理效果影响因素的重要性依次为HRT>DO>进水COD浓度>pH值。而且通过两级介孔生物填料流化床的联用,可以明显提高进水氨氮的负荷,并获得良好的处理效果,出水COD和氨氮已接近排放标准,当保证COD/NH_4~+-N在10以上时,COD去除率可达到95%以上,NH_4~+-N去除率也可达到90%以上,TN去除率可达80%左右。
根据生化反应不能完全对焦化废水处理达标的特点,以十六烷基三甲基溴化铵为有机改性剂,Na_2CO_3为钠化剂,分别采用普通加热法和微波辐射法制备出两种有机改性蒙脱石和钠化改性蒙脱石,并以苯酚和氯化铵模拟废水为目标,对其吸附性能进行了研究。结果表明,微波有机改性蒙脱石在投量为20 g/L,吸附时间为30 min,pH不大于10的条件下,对苯酚的吸附去除效果最好,去除率可达80.7%;而钠化改性蒙脱石在投量为10 g/L,吸附时间为30 min,pH在7~9之间的条件下,对氨氮的吸附效果最好,其去除率为60%以上。两种吸附材料的吸附过程均可用Freundlich吸附等温方程进行很好地描述。根据吸附热力学函数和动力学的分析,初步判断微波有机改性土在吸附苯酚的过程中主要以物理吸附为主,而钠化蒙脱石的吸附过程主要以化学吸附为主,两种吸附材料的吸附反应均符合二级吸附反应模型,吸附过程活化能分别为2.589和1.613 kJ/mol。将按照质量比为有机蒙脱石:钠基蒙脱石:聚合氯化铝=20:20:1混合而制成的改性蒙脱石复合吸附混凝剂用于焦化废水的深度处理可达到较好的处理效果,当投量为30g/L时,吸附混凝时间为30min时,COD、氨氮去除率和脱色率分别可达84.8%、78.2%和96%。
论文对介孔生物填料物化的性能进行了研究,结果表明,介孔生物填料表面有大量的负电荷,主要以有机成分为主,含量约为81.6%。而且该填料对反应器中的氧传递起到了促进作用,能够提高反应器中氧总转移系数约10%左右。同时该生物填料对苯酚的吸附作用较小,这表明反应器对苯酚的去除效果中,微生物的降解起到了主要作用,而填料的吸附在其中只占很小的部分。通过对改性蒙脱石表面和结构的表征研究了其改性前后形貌和结构上的变化。结果表明,改性没有改变蒙脱石的基本构型。和原土相比,微波有机改性蒙脱石层间距增加,而比表面积减小;钠化改性蒙脱石的层间距和比表面积都降低。根据表征结果可以推测出OMt中CTA~+的排列方式主要是以紧密的单层CTA~+ M型平卧和单层吸附水分子结合的形式为主;而M-OMt中CTA~+主要以34.1°的倾斜角度呈较稀疏的形式排列,这正是微波有机改性蒙脱石获得较好吸附性能的原因。
论文还对该组合工艺的运行效能进行了实际应用研究,结果表明,该组合工艺完全可以满足高浓度焦化废水的处理要求,其出水COD、氨氮和总酚的平均值分别为20.56,9.55和0.12 mg/L,远低于国家一级排放标准的要求。通过水质分析发现,该组合工艺对焦化废水中的难降解的杂环化合物等有良好的去除效果,出水主要以烷烃为主。而且该组合工艺运行稳定,能够耐受较大的有机负荷,具有较强的抗冲击能力。本论文为焦化废水严重污染问题的解决提供了一个可行的方案和翔实的数据支持,具有重要的理论意义和实际应用价值。
Coking wastewater is a kind of typical trouble industrial wastewater with high concentration of phenols and NH_4~+-N, which could pollute environment seriously and do harm to human health heavily. Though the effect there was on the treatment of phenol, cyanogens and BOD5 in this wastewater by the existent treatment methods, the effluent COD, NH_4~+-N and colority couldn’t meet the discharge standard, which has been one of the main pollution sources of river in our country. In this paper, according to the research situation of treatment process of coking wastewater, the combination process of biological fluid-bed packed with new mesoporous biological carriers and adsorption coagulation with modification montmorillonite was proposed. Organic compound and nitrogen removal performance of mesoporous biological carriers and modification montmorillonite were investigated in the treatment of simulated wastewater and coking wastewater, and both lab-scale and practical application studies were conducted. This combination process will be a feasible scheme to solve the problem of the coking wastewater pollution.
High concentration phenol and coking wastewater was regarded as research object, and the organic compound and nitrogen removal performance of fluid-bed packed with mesoporous biological carriers were researched. The results showed that there were good effect on the phenol solution of 1000~1500mg/L and coking wastewater with COD of 1700~4200mg/L in this fluid-bed reactor, the removal efficiency of phenol, COD and NH_4~+-N was above 99.9%, 80% and 70%, respectively, when HRT was 20 h, pH was 6.6~8.1 and DO was 1.8~3.7 mg/L. And this fluid-bed reactor packed with mesoporous biological carriers had the stronger impact resistance and self recovery capability. And it also was found that there was phenomenon of simultaneous nitrification and denitrification (SND) in the reactor. Orthogonal experiment results indicated that the importance of influence factors on treatment effect of this fluid-bed reactor was HRT > DO >influent COD concentration > pH. Furthermore, combination of two stage fluid-bed reactor could evidently improve the loading of influent NH_4~+-N and obtain good treatment effect, effluent COD and NH_4~+-N had been close to the discharge standard. When the ratio of COD/NH_4~+-N was above 10, the removal efficiency of COD, NH_4~+-N and TN was above 95%, 90% and 80%, respectively.
Because the effluent quality of biological fluid-bed reactor to coking wastewater couldn’t completely meet discharge standard, organic modification montmorillonite and Na-montmorillonite were prepared by common heating method and microwave irradiation using cetyltrimethyl ammonium bromide(CTAB) as organic modifier and Na2CO3 as sodium agent, and the adsorption of simulation phenol and NH4Cl wastewater on these materials was investigated. The results indicated that the adsorption effect of phenol on organic modification montmorillonite by microwave irradiation (M-OMt) was the best, the removal efficiency was 80.7%, when the dosage of this montmorillonite was 20 g/L, adsorption time was 30 min, pH was lower than 10. And the adsorption effect of NH_4~+-N on Na-montmorillonite (Mt(Na)) was the best, the removal efficiency was above 60%, when the dosage of this montmorillonite was 10 g/L, adsorption time was 30 min, pH was 7~9. The adsorption processes of the two montmorillonite materials both were in conformity with Freundlich isothermal adsorption equation. According to the analysis of adsorption thermodynamics and dynamics, it was preliminarily ascertained that the main mechanism of phenoladsorption was physical sorption for M-OMt, and the main mechanism of NH_4~+-N adsorption was chemical sorption for Mt (Na). The adsorption kinetics for two montmorillonite materials could be well described by the pseudo-second order kinetics model, and the adsorption activity energy was 2.589 and 1.613 kJ/mol, respectively. The composite adsorption coagulants prepared with M-OMt : Mt (Na) : polyaluminum chloride = 20 : 20 : 1 (mass ratio) was used to deeply treat coking wastewater, and the treatment effect was also investigation. The results showed that the removal efficiency of COD, NH_4~+-N and colority was 84.8%, 78.2% and 96%, respectively, when the dosage was 30 g/L, adsorption time was 30min.
Physical and chemical performance of new mesoporous biological carrierswere investigated, the results showed that there were lots of negative charges on the surface of mesoporous biological carriers that was mainly composed oforganic substance with about 81.6% amount. The existence of this biological carrier in the fluid-bed reactor accelerated the process of oxygen transfer, which could improve the oxygen transfer coefficient to about 10%. And the adsorption of phenol on this biological carrier was very low, which indicated that the removal efficiency of phenol in the fluid-bed reactor mainly caused by the degradation of microorganism, not by the adsorption of biological carriers. The change of appearance and structure of montmorillonite before and after modification was also characterized. The results showed that comparison with raw montmorillonite, the interlayer spacing of M-OMt was increased and the specific surface area was decreased; the interlayer spacing and specific surface area of Mt (Na) were all decreased. And the basic raw structure of montmorillonite wasn’t changed after modification. The characteristic results also indicated that the arrangement of CTAB cations in OMt was the close M-type lateral-monolayer combined with the monolayer adsorbed water molecule, however, CTAB in M-OMt was arranged in the form of the orderly and loose inclination angle of 34.1o.
The practical application was carried out to verify the operation efficiency of this combination process. The results indicated that this combination process could completely meet the treatment requirement of high concentration coking wastewater, the effluent of COD, NH_4~+-N and total phenol was 20.56, 9.55 and 0.12 mg/L, respectively, which was lower than the GradeΙof Wastewater Discharge Standard. According to the analysis of water quality, it was found that there were excellent removal effect of nondigradation heterocyclic compounds in coking wastewater on the combination process, and the main residual organic compounds were alkanes in the effluent of this combination process. And the treatment efficiency of the process was stable, and the combination process could tolerate the bigger organic loading and hydraulic impact. Work of this dissertation has great theoretical and practical value as it provided a feasible technology and enough data basis to solve the problem of the gasification wastewater contamination.
分别以高浓度苯酚配水和实际焦化废水为研究对象,对介孔生物填料流化床对废水的处理性能进行了研究。结果表明,当HRT为20h,pH在6.6~8.1的范围内,溶解氧在1.8~3.7 mg/L之间时,介孔生物填料流化床反应器可对1000~1500mg/L左右的苯酚溶液和COD为1700~4200mg/L的焦化废水进行有效的降解,苯酚去除率可达99.9%以上,COD去除率在80%左右,NH_4~+-N去除率在70%左右,而且该介孔生物填料流化床具有较强的抗冲击能力和自我恢复能力,并在反应器中发现有同步硝化反硝化作用(SND)的存在。正交试验表明对反应器处理效果影响因素的重要性依次为HRT>DO>进水COD浓度>pH值。而且通过两级介孔生物填料流化床的联用,可以明显提高进水氨氮的负荷,并获得良好的处理效果,出水COD和氨氮已接近排放标准,当保证COD/NH_4~+-N在10以上时,COD去除率可达到95%以上,NH_4~+-N去除率也可达到90%以上,TN去除率可达80%左右。
根据生化反应不能完全对焦化废水处理达标的特点,以十六烷基三甲基溴化铵为有机改性剂,Na_2CO_3为钠化剂,分别采用普通加热法和微波辐射法制备出两种有机改性蒙脱石和钠化改性蒙脱石,并以苯酚和氯化铵模拟废水为目标,对其吸附性能进行了研究。结果表明,微波有机改性蒙脱石在投量为20 g/L,吸附时间为30 min,pH不大于10的条件下,对苯酚的吸附去除效果最好,去除率可达80.7%;而钠化改性蒙脱石在投量为10 g/L,吸附时间为30 min,pH在7~9之间的条件下,对氨氮的吸附效果最好,其去除率为60%以上。两种吸附材料的吸附过程均可用Freundlich吸附等温方程进行很好地描述。根据吸附热力学函数和动力学的分析,初步判断微波有机改性土在吸附苯酚的过程中主要以物理吸附为主,而钠化蒙脱石的吸附过程主要以化学吸附为主,两种吸附材料的吸附反应均符合二级吸附反应模型,吸附过程活化能分别为2.589和1.613 kJ/mol。将按照质量比为有机蒙脱石:钠基蒙脱石:聚合氯化铝=20:20:1混合而制成的改性蒙脱石复合吸附混凝剂用于焦化废水的深度处理可达到较好的处理效果,当投量为30g/L时,吸附混凝时间为30min时,COD、氨氮去除率和脱色率分别可达84.8%、78.2%和96%。
论文对介孔生物填料物化的性能进行了研究,结果表明,介孔生物填料表面有大量的负电荷,主要以有机成分为主,含量约为81.6%。而且该填料对反应器中的氧传递起到了促进作用,能够提高反应器中氧总转移系数约10%左右。同时该生物填料对苯酚的吸附作用较小,这表明反应器对苯酚的去除效果中,微生物的降解起到了主要作用,而填料的吸附在其中只占很小的部分。通过对改性蒙脱石表面和结构的表征研究了其改性前后形貌和结构上的变化。结果表明,改性没有改变蒙脱石的基本构型。和原土相比,微波有机改性蒙脱石层间距增加,而比表面积减小;钠化改性蒙脱石的层间距和比表面积都降低。根据表征结果可以推测出OMt中CTA~+的排列方式主要是以紧密的单层CTA~+ M型平卧和单层吸附水分子结合的形式为主;而M-OMt中CTA~+主要以34.1°的倾斜角度呈较稀疏的形式排列,这正是微波有机改性蒙脱石获得较好吸附性能的原因。
论文还对该组合工艺的运行效能进行了实际应用研究,结果表明,该组合工艺完全可以满足高浓度焦化废水的处理要求,其出水COD、氨氮和总酚的平均值分别为20.56,9.55和0.12 mg/L,远低于国家一级排放标准的要求。通过水质分析发现,该组合工艺对焦化废水中的难降解的杂环化合物等有良好的去除效果,出水主要以烷烃为主。而且该组合工艺运行稳定,能够耐受较大的有机负荷,具有较强的抗冲击能力。本论文为焦化废水严重污染问题的解决提供了一个可行的方案和翔实的数据支持,具有重要的理论意义和实际应用价值。
Coking wastewater is a kind of typical trouble industrial wastewater with high concentration of phenols and NH_4~+-N, which could pollute environment seriously and do harm to human health heavily. Though the effect there was on the treatment of phenol, cyanogens and BOD5 in this wastewater by the existent treatment methods, the effluent COD, NH_4~+-N and colority couldn’t meet the discharge standard, which has been one of the main pollution sources of river in our country. In this paper, according to the research situation of treatment process of coking wastewater, the combination process of biological fluid-bed packed with new mesoporous biological carriers and adsorption coagulation with modification montmorillonite was proposed. Organic compound and nitrogen removal performance of mesoporous biological carriers and modification montmorillonite were investigated in the treatment of simulated wastewater and coking wastewater, and both lab-scale and practical application studies were conducted. This combination process will be a feasible scheme to solve the problem of the coking wastewater pollution.
High concentration phenol and coking wastewater was regarded as research object, and the organic compound and nitrogen removal performance of fluid-bed packed with mesoporous biological carriers were researched. The results showed that there were good effect on the phenol solution of 1000~1500mg/L and coking wastewater with COD of 1700~4200mg/L in this fluid-bed reactor, the removal efficiency of phenol, COD and NH_4~+-N was above 99.9%, 80% and 70%, respectively, when HRT was 20 h, pH was 6.6~8.1 and DO was 1.8~3.7 mg/L. And this fluid-bed reactor packed with mesoporous biological carriers had the stronger impact resistance and self recovery capability. And it also was found that there was phenomenon of simultaneous nitrification and denitrification (SND) in the reactor. Orthogonal experiment results indicated that the importance of influence factors on treatment effect of this fluid-bed reactor was HRT > DO >influent COD concentration > pH. Furthermore, combination of two stage fluid-bed reactor could evidently improve the loading of influent NH_4~+-N and obtain good treatment effect, effluent COD and NH_4~+-N had been close to the discharge standard. When the ratio of COD/NH_4~+-N was above 10, the removal efficiency of COD, NH_4~+-N and TN was above 95%, 90% and 80%, respectively.
Because the effluent quality of biological fluid-bed reactor to coking wastewater couldn’t completely meet discharge standard, organic modification montmorillonite and Na-montmorillonite were prepared by common heating method and microwave irradiation using cetyltrimethyl ammonium bromide(CTAB) as organic modifier and Na2CO3 as sodium agent, and the adsorption of simulation phenol and NH4Cl wastewater on these materials was investigated. The results indicated that the adsorption effect of phenol on organic modification montmorillonite by microwave irradiation (M-OMt) was the best, the removal efficiency was 80.7%, when the dosage of this montmorillonite was 20 g/L, adsorption time was 30 min, pH was lower than 10. And the adsorption effect of NH_4~+-N on Na-montmorillonite (Mt(Na)) was the best, the removal efficiency was above 60%, when the dosage of this montmorillonite was 10 g/L, adsorption time was 30 min, pH was 7~9. The adsorption processes of the two montmorillonite materials both were in conformity with Freundlich isothermal adsorption equation. According to the analysis of adsorption thermodynamics and dynamics, it was preliminarily ascertained that the main mechanism of phenoladsorption was physical sorption for M-OMt, and the main mechanism of NH_4~+-N adsorption was chemical sorption for Mt (Na). The adsorption kinetics for two montmorillonite materials could be well described by the pseudo-second order kinetics model, and the adsorption activity energy was 2.589 and 1.613 kJ/mol, respectively. The composite adsorption coagulants prepared with M-OMt : Mt (Na) : polyaluminum chloride = 20 : 20 : 1 (mass ratio) was used to deeply treat coking wastewater, and the treatment effect was also investigation. The results showed that the removal efficiency of COD, NH_4~+-N and colority was 84.8%, 78.2% and 96%, respectively, when the dosage was 30 g/L, adsorption time was 30min.
Physical and chemical performance of new mesoporous biological carrierswere investigated, the results showed that there were lots of negative charges on the surface of mesoporous biological carriers that was mainly composed oforganic substance with about 81.6% amount. The existence of this biological carrier in the fluid-bed reactor accelerated the process of oxygen transfer, which could improve the oxygen transfer coefficient to about 10%. And the adsorption of phenol on this biological carrier was very low, which indicated that the removal efficiency of phenol in the fluid-bed reactor mainly caused by the degradation of microorganism, not by the adsorption of biological carriers. The change of appearance and structure of montmorillonite before and after modification was also characterized. The results showed that comparison with raw montmorillonite, the interlayer spacing of M-OMt was increased and the specific surface area was decreased; the interlayer spacing and specific surface area of Mt (Na) were all decreased. And the basic raw structure of montmorillonite wasn’t changed after modification. The characteristic results also indicated that the arrangement of CTAB cations in OMt was the close M-type lateral-monolayer combined with the monolayer adsorbed water molecule, however, CTAB in M-OMt was arranged in the form of the orderly and loose inclination angle of 34.1o.
The practical application was carried out to verify the operation efficiency of this combination process. The results indicated that this combination process could completely meet the treatment requirement of high concentration coking wastewater, the effluent of COD, NH_4~+-N and total phenol was 20.56, 9.55 and 0.12 mg/L, respectively, which was lower than the GradeΙof Wastewater Discharge Standard. According to the analysis of water quality, it was found that there were excellent removal effect of nondigradation heterocyclic compounds in coking wastewater on the combination process, and the main residual organic compounds were alkanes in the effluent of this combination process. And the treatment efficiency of the process was stable, and the combination process could tolerate the bigger organic loading and hydraulic impact. Work of this dissertation has great theoretical and practical value as it provided a feasible technology and enough data basis to solve the problem of the gasification wastewater contamination.
引文
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