催化湿式氧化—好氧颗粒污泥处理高浓度制药废水研究
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摘要
制药废水是一种高浓度、难降解的工业废水,具有毒性强、常规生物法难以处理等特点,直接排放将对水体环境造成严重危害。因此,本文在“十一五”国家水专项浑河流域水体污染控制研究课题支持下,开展了针对东北制药总厂磷霉素钠制药废水的催化湿式氧化预处理—磷酸铵镁沉淀法除磷—好氧颗粒污泥集成工艺试验研究。
催化湿式氧化降解磷霉素钠过程中,磷霉素钠原水残留的WO3-和P043-(氧化磷霉素钠右盐生成),可与黄连素制药废水中Cu2+(脱铜反应生成)可形成均相杂多酸盐催化剂·-Cu2+[PxWmOy]q-。在250℃、1.4MPa初始氧分压条件下,磷霉素钠和黄连素混合制药废水中COD(121081mgL-1), TOC(5823mgL-1)去除率分别可达41.1%、43.0%,同时95%的有机磷被转化为P043-,70%的有机氮被转化为NH4+,出水可生化性明显提高。该过程中磷霉素钠右盐可被氧化成丙醇、丙酸,拆分剂苯乙胺被氧化成苯甲酸,达到了“以废治废”,解除原水有机磷毒性目的。整个催化氧化过程以Cu2+[PxWmOy]q-催化氧化、羟基自由基反应为主。出水中Cu2+[PxWmOy]q可大量过饱和析出、易分离,可缓解以往湿式氧化存在的重金属二次污染问题。对析出的Cu2+[PxWmOy]q进行TGA、 IR、XRD、XRF分析,结果表明该催化剂具有较高的热稳定性,结构近似P4Ws032,氧化还原性可调范围较大,且对污泥中微生物毒性较低。
磷酸铵镁盐(MgNH4PO4,MAP,矿物学名：鸟粪石)沉淀法可同时去除湿式氧化出水中NH4-、PO43-,但杂质离子Cu2+可通过进入晶格或吸附作用,影响磷酸铵镁盐结晶。在Cu2+低浓度存在条件下,湿式氧化出水中P043-可被去除48%,被去除的部分可结晶成鸟粪石。
将磷酸铵镁沉淀得到的不纯沉淀物—鸟粪石,作为生物载体培养好氧颗粒污泥强化最终二级生物处理单元。启动初期,鸟粪石可通过固体表面作用、Mg2+压缩污泥双电层、游离氨浓度刺激AOB富集等作用,刺激污泥多糖产量由28.4mgg-1MLVSS增加至42.2mgg-1MLVSS,有效的加速了颗粒化进程,30天即可培养出尺寸为700～1100μm的成熟颗粒污泥。通过扫描电镜、荧光原位杂交技术,证实了颗粒内部主要由AOB构成,NOB、PAO种群数量较小。对于具有生物毒性的制药废水,该好氧颗粒污泥单元在短水力停留时间条件下,可去除90%以上COD以及70%以上的NH4+-N。颗粒污泥亚硝化作用明显,NO2--N/(NO2--N+NO3--N)稳定期平均值为89%,表明鸟粪石载体培养是一种有效的业硝化好氧颗粒污泥培养方法。
Pharmaceutical wastewater often contains high concentration non-biodegradable organic compounds, the discharge of toxic substances not degraded in pharmaceutical wastewater cause serious detrimental effect to the natural environment. Therefore, supported by the "Eleventh Five-Year" National Water Pollution Control Projects (Hun river in Liaoning province, China), we were committed to investigate the integration process in treating fosfomycin pharmaceutical wastewater from Northeast General Pharmaceutical Factory, using catalytic wet air oxidation (CWAO) and aerobic granular sludge which used struvite granule formed by precipitative phosphate removal.
In CWAO treatment of fosfomycin pharmaceutical wastewater, WO3-and PO43-(converted from fosfomycin calt oxidation) in fosfomycin wastewater and Cu2+(generated from decoppering) in berberine pharmaceutical wastewater could form Cu2+[PxWmOy]q-, namely polyoxometalates (POMs). At250℃and1.4MPa initial oxygen pressure,41%and43%of COD (chemical oxygen demand, the initial COD of mixed streams was121081mgL-1) and TOC (total organic carbon, the value of mixed streams was5823mgL-1) removal can be easily realized, meanwhile,95%organophosphorus and70%organic amine were converted to PO43-and NH4+,respectively. The biodegradability of wastewater was enhanced by the CWAO treatment. In addition, fosfomycin was incompletely oxidized to propionic acid or propanol, and the resolving agent phenethylamine was oxidized to benzoic acid. Noteworthy, reusing these active ions and detoxicating organophosphorus simultaneously, satisfies the demand of "treating wastes with other wastes". Both the hydroxyl radical reaction and catalytic oxidation play crucial roles in the CWAO process. Supersaturated precipitate Cu2+[PxWmOy]q-can be easily separated from the effluent, which can reduce secondary pollution caused by heavy metal ions used in CWAO. Characterizations(e.g., TGA, IR, XRD, XRF) and analysis of Cu2+[PxWmOy]q-showed that it was similar to P4W8O32in structure, and had high thermal stability, low microbial toxicity, and adjustable acid-base and redox properties.
NH4+and PO43-in CWAO effluent can been removed simultaneously using precipitation method by forming magnesium ammonium phosphate (MgNH4PO4, MAP, struvite). Cu2+impurities can affect crystallization by entering into the crystal lattice or adsorbing on struvite surface. When Cu2+concentration was low,48%of PO43-was removed in the form of struvite.
Struvite was reused as a carrier to cultivate aerobic granules and enhance the biological treatment. In start-up period, its addition stimulated polysaccharides generation (42.2mgg-1MLVSS versus28.4mgg-1MLVSS in sludge without it), which possibly caused accelerated granulation via the solid surface effect, compressed "double layer" effect by Mg2+and enriched ammonia-oxidizing bacteria (AOB) by free ammonia. The size of mature granules ranged from700to1100μm after30days cultivation. According to SEM and FISH analysis, AOB was found as the dominate strains over nitrite-oxidizing bacteria (NOB) and polyphosphate accumulating bacteria (PAO). Although the CWAO treated pharmaceutical wastewater contains toxic substance, the removal of90%COD and more than70%NH4+-N, was achieved the granule has significant nitrification effect, the average value of stable accumulation of nitrite was89%[NO2--N:(NO2--N+NO3--N)] in this biological treatment unit. This emphasizes that adding struvite as a new-type carrier can effectively promote the formation of partial nitrification granular sludge, and the new granular cultivation method is effective for cultivating nitrification granular sludge.
催化湿式氧化降解磷霉素钠过程中,磷霉素钠原水残留的WO3-和P043-(氧化磷霉素钠右盐生成),可与黄连素制药废水中Cu2+(脱铜反应生成)可形成均相杂多酸盐催化剂·-Cu2+[PxWmOy]q-。在250℃、1.4MPa初始氧分压条件下,磷霉素钠和黄连素混合制药废水中COD(121081mgL-1), TOC(5823mgL-1)去除率分别可达41.1%、43.0%,同时95%的有机磷被转化为P043-,70%的有机氮被转化为NH4+,出水可生化性明显提高。该过程中磷霉素钠右盐可被氧化成丙醇、丙酸,拆分剂苯乙胺被氧化成苯甲酸,达到了“以废治废”,解除原水有机磷毒性目的。整个催化氧化过程以Cu2+[PxWmOy]q-催化氧化、羟基自由基反应为主。出水中Cu2+[PxWmOy]q可大量过饱和析出、易分离,可缓解以往湿式氧化存在的重金属二次污染问题。对析出的Cu2+[PxWmOy]q进行TGA、 IR、XRD、XRF分析,结果表明该催化剂具有较高的热稳定性,结构近似P4Ws032,氧化还原性可调范围较大,且对污泥中微生物毒性较低。
磷酸铵镁盐(MgNH4PO4,MAP,矿物学名：鸟粪石)沉淀法可同时去除湿式氧化出水中NH4-、PO43-,但杂质离子Cu2+可通过进入晶格或吸附作用,影响磷酸铵镁盐结晶。在Cu2+低浓度存在条件下,湿式氧化出水中P043-可被去除48%,被去除的部分可结晶成鸟粪石。
将磷酸铵镁沉淀得到的不纯沉淀物—鸟粪石,作为生物载体培养好氧颗粒污泥强化最终二级生物处理单元。启动初期,鸟粪石可通过固体表面作用、Mg2+压缩污泥双电层、游离氨浓度刺激AOB富集等作用,刺激污泥多糖产量由28.4mgg-1MLVSS增加至42.2mgg-1MLVSS,有效的加速了颗粒化进程,30天即可培养出尺寸为700～1100μm的成熟颗粒污泥。通过扫描电镜、荧光原位杂交技术,证实了颗粒内部主要由AOB构成,NOB、PAO种群数量较小。对于具有生物毒性的制药废水,该好氧颗粒污泥单元在短水力停留时间条件下,可去除90%以上COD以及70%以上的NH4+-N。颗粒污泥亚硝化作用明显,NO2--N/(NO2--N+NO3--N)稳定期平均值为89%,表明鸟粪石载体培养是一种有效的业硝化好氧颗粒污泥培养方法。
Pharmaceutical wastewater often contains high concentration non-biodegradable organic compounds, the discharge of toxic substances not degraded in pharmaceutical wastewater cause serious detrimental effect to the natural environment. Therefore, supported by the "Eleventh Five-Year" National Water Pollution Control Projects (Hun river in Liaoning province, China), we were committed to investigate the integration process in treating fosfomycin pharmaceutical wastewater from Northeast General Pharmaceutical Factory, using catalytic wet air oxidation (CWAO) and aerobic granular sludge which used struvite granule formed by precipitative phosphate removal.
In CWAO treatment of fosfomycin pharmaceutical wastewater, WO3-and PO43-(converted from fosfomycin calt oxidation) in fosfomycin wastewater and Cu2+(generated from decoppering) in berberine pharmaceutical wastewater could form Cu2+[PxWmOy]q-, namely polyoxometalates (POMs). At250℃and1.4MPa initial oxygen pressure,41%and43%of COD (chemical oxygen demand, the initial COD of mixed streams was121081mgL-1) and TOC (total organic carbon, the value of mixed streams was5823mgL-1) removal can be easily realized, meanwhile,95%organophosphorus and70%organic amine were converted to PO43-and NH4+,respectively. The biodegradability of wastewater was enhanced by the CWAO treatment. In addition, fosfomycin was incompletely oxidized to propionic acid or propanol, and the resolving agent phenethylamine was oxidized to benzoic acid. Noteworthy, reusing these active ions and detoxicating organophosphorus simultaneously, satisfies the demand of "treating wastes with other wastes". Both the hydroxyl radical reaction and catalytic oxidation play crucial roles in the CWAO process. Supersaturated precipitate Cu2+[PxWmOy]q-can be easily separated from the effluent, which can reduce secondary pollution caused by heavy metal ions used in CWAO. Characterizations(e.g., TGA, IR, XRD, XRF) and analysis of Cu2+[PxWmOy]q-showed that it was similar to P4W8O32in structure, and had high thermal stability, low microbial toxicity, and adjustable acid-base and redox properties.
NH4+and PO43-in CWAO effluent can been removed simultaneously using precipitation method by forming magnesium ammonium phosphate (MgNH4PO4, MAP, struvite). Cu2+impurities can affect crystallization by entering into the crystal lattice or adsorbing on struvite surface. When Cu2+concentration was low,48%of PO43-was removed in the form of struvite.
Struvite was reused as a carrier to cultivate aerobic granules and enhance the biological treatment. In start-up period, its addition stimulated polysaccharides generation (42.2mgg-1MLVSS versus28.4mgg-1MLVSS in sludge without it), which possibly caused accelerated granulation via the solid surface effect, compressed "double layer" effect by Mg2+and enriched ammonia-oxidizing bacteria (AOB) by free ammonia. The size of mature granules ranged from700to1100μm after30days cultivation. According to SEM and FISH analysis, AOB was found as the dominate strains over nitrite-oxidizing bacteria (NOB) and polyphosphate accumulating bacteria (PAO). Although the CWAO treated pharmaceutical wastewater contains toxic substance, the removal of90%COD and more than70%NH4+-N, was achieved the granule has significant nitrification effect, the average value of stable accumulation of nitrite was89%[NO2--N:(NO2--N+NO3--N)] in this biological treatment unit. This emphasizes that adding struvite as a new-type carrier can effectively promote the formation of partial nitrification granular sludge, and the new granular cultivation method is effective for cultivating nitrification granular sludge.
引文
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