吹脱-MAP-两相厌氧联合工艺处理苯胺基乙腈生产废水试验研究
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摘要
苯胺基乙腈是一种染料中间体,在其生产过程中会产生含大量氨氮的高浓度有机废水。该废水成份复杂,可生化性低,是一种难生物降解的化工废水。为了除去该废水中的高浓度氨氮以利于后续生化处理,本研究采用吹脱-磷酸铵镁沉淀法(MAP)对废水进行脱氮预处理,然后将预处理后的废水进入两相厌氧反应器,考察两相厌氧工艺在处理该废水时的启动、分相特性,对两相厌氧动力学进行分析和研究,得到两相厌氧工艺处理苯胺基乙腈生产废水的动力学方程,同时对两相厌氧处理后的出水进行了好氧处理的可行性研究。此外,还对两相厌氧工艺中微生物种群多样性进行了分析。
苯胺基乙腈生产废水中的氨氮浓度高达7000mg/L~12000mg/L,若直接用MAP沉淀法处理会消耗大量化学药剂导致单位处理成本过高,并且处理效果不理想。对高浓度氨氮废水先进行吹脱可以降低氨氮浓度,同时还可以回收氨氮。经试验研究,吹脱法处理苯胺乙腈生产废水氨氮的最佳条件为:吹脱时间为180min,吹脱温度为70℃,气水比为2000:1,吹脱pH为11。吹脱出水的氨氮浓度为1000mg/L~1500mg/L,吹脱对废水的COD去除率为5.8%左右,废水颜色由吹脱前的亮棕色转为深黑色。
采用MgO和H_3PO_4作为MAP沉淀药剂,对吹脱出水进行正交试验得到MAP法去除氨氮的条件为:氧化镁与氨氮计量比为2.5:1,氨氮与磷酸计量比为1:1.2,反应pH为9.5。此时出水氨氮浓度为100mg/L~150mg/L,出水的残磷量为15~20mg/L,可以补充后续生化处理所需的磷元素。研究中发现生成物不易沉降,分析认为可能是废水中的疏水性物质附着于小颗粒沉淀表面,颗粒之间不易接触不能形成较密实的沉淀所致,研究中将药剂投加方式改为预配制糊状沉淀剂投加,该问题得到解决。
本研究利用重庆钢铁集团焦化厂废水处理站的兼氧污泥作为种泥进行接种,将未经氨氮预处理的原废水稀释后对污泥进行驯化。保持进水COD浓度为500mg/L,对污泥进行了12d的兼氧驯化和10d的厌氧适应驯化;污泥在22d内经历了底物类型与环境条件的变化,对苯胺基乙腈生产废水的降解作用逐渐增强,反应器在第22d对COD的去除率为50%左右。22d后反应器转入厌氧负荷驯化状态,在低负荷驯化段(进水COD=500~1000mg/L)反应器对COD的去除率为60%左右;在中负荷驯化段(进水COD=1000~2000mg/L)反应器对COD的去除率为80%左右;在高负荷驯化段(进水COD>2000mg/L)反应器对COD的去除率为80%左右,但随着进水浓度的继续增加,COD去除率下降至60%左右,此时进水中的氨氮浓度已达470mg/L以上,说明氨氮已对微生物产生抑制作用,所以后续工艺必须将废水中氨氮浓度降低再进入两相厌氧反应器。
分相研究中,向酸化反应器中投加2mol/LNa_2MoO_4做为甲烷菌抑制剂,连续投加3天。分相过程中,出水pH由8降至7,出水VFA由400mg/L升至800mg/L左右,出水碱度(以CaCO_3计)从800mg/L降至400mg/L左右。分相期间酸化反应器的COD去除率略有下降,但很快恢复正常。
用脱氮预处理的废水稀释后进行两相厌氧负荷试验,当进水COD浓度为7058mg/L时,两相厌氧反应器处理效率达到最高,COD去除率为55%,其中水解酸化反应器、一级产甲烷反应器、二级产甲烷反应器的去除率分别为11.1%、17.4%、25.1%。将两相厌氧处理出水稀释至COD浓度为1000mg/L进行好氧处理可行性研究,水力停留时间为16h,COD去除率为61.3%,色度去除率为76.1%。
以Nerfeld修正Monod方程作为两相厌氧工艺处理苯胺基乙腈生产废水动力学模型,通过Origin软件自定义曲线拟合得到产甲烷相一级、二级反应器及两相厌氧系统的动力学方程。利用PCR-TGGE技术对两相厌氧反应器内污泥进行了微生物菌群变化研究,通过接种污泥与不同反应器内驯化后的污泥对比得出以下结论:驯化过程极大改变了接种污泥的菌群丰度与结构,水解酸化反应器内1至4格污泥、两级产甲烷反应器内污泥与接种污泥的相似度分别为48.0%、48.2%、59.7%、56.8%和50.6%、50.2%;非公制多尺度分析(NMDS)表明水解酸化过程前期污泥结构差异较大,后期差异较小,两级产甲烷过程污泥差异相对较小。
N-Phenylglycinonitrile was a kind of dye intermediate which would produce a large number of wastewater of high concentration of COD and ammonia nitrogen in its production process. The wastewater was a kind of low biodegradability chemical wastewater with complex component. In order to remove high concentration of ammonia nitrogen in wastewater for the latter biological treatment, we used air-stripping and MAP as the pretreatment. The wastewater after pretreatment was pumped into two-phase anaerobic digester to study the feature of TPAD process in dealing with startup and phase splitted, and the kinetics equation was obtained after reaction kinetics analysis studied. The feasibility of treatment by actived sludge after anaerobic treatement and variation of bacterial community were also studied.
Concentration of Ammonia nitrogen in N-Phenylglycinonitrile wastewater was up to 7000mg/L~12000mg/L,if the MAP applied directly it would consume a large quantities of chemicals which could lead to high consumption in unit treatment, and the effect was not good enough. So MAP applied after the air-stripping process was feasible that could reduce concentraion of ammoina nitrogen to 1500mg/L~2000mg/L, and we could recovery tail gas. The best condition determined by the experiment was: air-stripping time=180min, temperature=70℃, gas-water ratio=2000:1, pH=11. Air-stripping would remove 5.8% COD, but the wastewater would get into darkness.
Using MgO and H_3PO_4 as the MAP agent, the optimal operation parameters of MAP was determined by orthogonal experiment: magnesium oxide and ammonia nitrogen stoichiometric ratio=2.5:1, ammonia nitrogen and phosphate ratio=1:1.2, reaction pH=9.5. Under the condition above, there would be 100mg/L~150mg/L NH_3-N and 15~20 mg/L phosphate remain in the wastewater. Experiments showed that the sediment was not easy to settle down for the reason that small particles of hyrophobic substances in wastewater attached to the sediments' surface, so that big particles of sediment was not easy to form for that they could not easily getting access from each other. But it would not occured after changing pre-prepared into paste precipitant dosage.
Acclimated seed sludge was from coking plant in Chongqing Steel Group which feeded with orginal wastewater. Holding influent COD concentration 500mg/L, we did a duration of 12 days’facultative anaerobic acclimation and 10 days’adaptive anaerobic acclimation. After sludge suffered changing of substrates and living environment, the degradation strengthened gradually, and the remove rate of COD reached 50%. Acclimation run into load anaerobic acclimation after 22 days, and in low load stage (COD=500~1000mg/L) , TPAD remove over 60% COD, in medium load stage (COD=1000~2000mg/L),the removal rate of COD was about 80%, in high load stage (COD>2000mg/L), removal rate was high as medium load stage at first, but it would drop down with the concentration increase, for the reason was the ammonia nitorgen concentration was up to 470 mg/L, and bacterias would get depressed. The ammonia nitrogen must be removed before wastewater pumped into TPAD.
Putting a dosage of 2mol/L Na2MoO4 as methanogens inhibitor lasted for 3 days. In this process, effluent pH drop down from 8 to 7, and VFA rised from 400mg/L to 800mg/L, alkalinity(CaCO_3) dropped from 800mg/L to 400mg/L. During these days, COD removal rate dropped down for a while, but it ran into normal quickly.
The TPAD reactor reached its highest condition when influent COD up to 7058 mg/L which was after ammonia nitrogen removing pretreatment. The COD removal rate was 55%, and the souring reactor could remove 11.1% COD, 1st methane reactor could remove 17.4% COD, 2st methane reactor could remove 25.1% COD. TPAD effluent was treated by actived sludge treatment to study the feasibility of aerobic treatment after diluting COD to 1000mg/L. When HRT was 16h, actived sludge treatment could remove 61.3% COD and 76.1% chroma.
We got N-Phenylglycinonitrile biodegradation dynamic model with 1st methane reactor, 2st methane reactor and TPAD reactor by curve fitting with Origin software custom fitted curve based on Nerfeld modified Monod equation. Research on bacterial community by contrasting acclimated sludge with seed sludge in different treatment unit with PCR-TGGE technique, we draw conclusion as follows: acclimating process could change bacterial diversity and community greatly, the dice coefficient between seed sludge and acclimated sludge was 48.0%、48.2%、59.7%、56.8% and 50.6%、50.2%, Analysis of NMDS showed there were differences in sludge of first steps of souring process, but less difference in the last steps, and more less differences between 1st methane sluge and 2st methane sludge.
苯胺基乙腈生产废水中的氨氮浓度高达7000mg/L~12000mg/L,若直接用MAP沉淀法处理会消耗大量化学药剂导致单位处理成本过高,并且处理效果不理想。对高浓度氨氮废水先进行吹脱可以降低氨氮浓度,同时还可以回收氨氮。经试验研究,吹脱法处理苯胺乙腈生产废水氨氮的最佳条件为:吹脱时间为180min,吹脱温度为70℃,气水比为2000:1,吹脱pH为11。吹脱出水的氨氮浓度为1000mg/L~1500mg/L,吹脱对废水的COD去除率为5.8%左右,废水颜色由吹脱前的亮棕色转为深黑色。
采用MgO和H_3PO_4作为MAP沉淀药剂,对吹脱出水进行正交试验得到MAP法去除氨氮的条件为:氧化镁与氨氮计量比为2.5:1,氨氮与磷酸计量比为1:1.2,反应pH为9.5。此时出水氨氮浓度为100mg/L~150mg/L,出水的残磷量为15~20mg/L,可以补充后续生化处理所需的磷元素。研究中发现生成物不易沉降,分析认为可能是废水中的疏水性物质附着于小颗粒沉淀表面,颗粒之间不易接触不能形成较密实的沉淀所致,研究中将药剂投加方式改为预配制糊状沉淀剂投加,该问题得到解决。
本研究利用重庆钢铁集团焦化厂废水处理站的兼氧污泥作为种泥进行接种,将未经氨氮预处理的原废水稀释后对污泥进行驯化。保持进水COD浓度为500mg/L,对污泥进行了12d的兼氧驯化和10d的厌氧适应驯化;污泥在22d内经历了底物类型与环境条件的变化,对苯胺基乙腈生产废水的降解作用逐渐增强,反应器在第22d对COD的去除率为50%左右。22d后反应器转入厌氧负荷驯化状态,在低负荷驯化段(进水COD=500~1000mg/L)反应器对COD的去除率为60%左右;在中负荷驯化段(进水COD=1000~2000mg/L)反应器对COD的去除率为80%左右;在高负荷驯化段(进水COD>2000mg/L)反应器对COD的去除率为80%左右,但随着进水浓度的继续增加,COD去除率下降至60%左右,此时进水中的氨氮浓度已达470mg/L以上,说明氨氮已对微生物产生抑制作用,所以后续工艺必须将废水中氨氮浓度降低再进入两相厌氧反应器。
分相研究中,向酸化反应器中投加2mol/LNa_2MoO_4做为甲烷菌抑制剂,连续投加3天。分相过程中,出水pH由8降至7,出水VFA由400mg/L升至800mg/L左右,出水碱度(以CaCO_3计)从800mg/L降至400mg/L左右。分相期间酸化反应器的COD去除率略有下降,但很快恢复正常。
用脱氮预处理的废水稀释后进行两相厌氧负荷试验,当进水COD浓度为7058mg/L时,两相厌氧反应器处理效率达到最高,COD去除率为55%,其中水解酸化反应器、一级产甲烷反应器、二级产甲烷反应器的去除率分别为11.1%、17.4%、25.1%。将两相厌氧处理出水稀释至COD浓度为1000mg/L进行好氧处理可行性研究,水力停留时间为16h,COD去除率为61.3%,色度去除率为76.1%。
以Nerfeld修正Monod方程作为两相厌氧工艺处理苯胺基乙腈生产废水动力学模型,通过Origin软件自定义曲线拟合得到产甲烷相一级、二级反应器及两相厌氧系统的动力学方程。利用PCR-TGGE技术对两相厌氧反应器内污泥进行了微生物菌群变化研究,通过接种污泥与不同反应器内驯化后的污泥对比得出以下结论:驯化过程极大改变了接种污泥的菌群丰度与结构,水解酸化反应器内1至4格污泥、两级产甲烷反应器内污泥与接种污泥的相似度分别为48.0%、48.2%、59.7%、56.8%和50.6%、50.2%;非公制多尺度分析(NMDS)表明水解酸化过程前期污泥结构差异较大,后期差异较小,两级产甲烷过程污泥差异相对较小。
N-Phenylglycinonitrile was a kind of dye intermediate which would produce a large number of wastewater of high concentration of COD and ammonia nitrogen in its production process. The wastewater was a kind of low biodegradability chemical wastewater with complex component. In order to remove high concentration of ammonia nitrogen in wastewater for the latter biological treatment, we used air-stripping and MAP as the pretreatment. The wastewater after pretreatment was pumped into two-phase anaerobic digester to study the feature of TPAD process in dealing with startup and phase splitted, and the kinetics equation was obtained after reaction kinetics analysis studied. The feasibility of treatment by actived sludge after anaerobic treatement and variation of bacterial community were also studied.
Concentration of Ammonia nitrogen in N-Phenylglycinonitrile wastewater was up to 7000mg/L~12000mg/L,if the MAP applied directly it would consume a large quantities of chemicals which could lead to high consumption in unit treatment, and the effect was not good enough. So MAP applied after the air-stripping process was feasible that could reduce concentraion of ammoina nitrogen to 1500mg/L~2000mg/L, and we could recovery tail gas. The best condition determined by the experiment was: air-stripping time=180min, temperature=70℃, gas-water ratio=2000:1, pH=11. Air-stripping would remove 5.8% COD, but the wastewater would get into darkness.
Using MgO and H_3PO_4 as the MAP agent, the optimal operation parameters of MAP was determined by orthogonal experiment: magnesium oxide and ammonia nitrogen stoichiometric ratio=2.5:1, ammonia nitrogen and phosphate ratio=1:1.2, reaction pH=9.5. Under the condition above, there would be 100mg/L~150mg/L NH_3-N and 15~20 mg/L phosphate remain in the wastewater. Experiments showed that the sediment was not easy to settle down for the reason that small particles of hyrophobic substances in wastewater attached to the sediments' surface, so that big particles of sediment was not easy to form for that they could not easily getting access from each other. But it would not occured after changing pre-prepared into paste precipitant dosage.
Acclimated seed sludge was from coking plant in Chongqing Steel Group which feeded with orginal wastewater. Holding influent COD concentration 500mg/L, we did a duration of 12 days’facultative anaerobic acclimation and 10 days’adaptive anaerobic acclimation. After sludge suffered changing of substrates and living environment, the degradation strengthened gradually, and the remove rate of COD reached 50%. Acclimation run into load anaerobic acclimation after 22 days, and in low load stage (COD=500~1000mg/L) , TPAD remove over 60% COD, in medium load stage (COD=1000~2000mg/L),the removal rate of COD was about 80%, in high load stage (COD>2000mg/L), removal rate was high as medium load stage at first, but it would drop down with the concentration increase, for the reason was the ammonia nitorgen concentration was up to 470 mg/L, and bacterias would get depressed. The ammonia nitrogen must be removed before wastewater pumped into TPAD.
Putting a dosage of 2mol/L Na2MoO4 as methanogens inhibitor lasted for 3 days. In this process, effluent pH drop down from 8 to 7, and VFA rised from 400mg/L to 800mg/L, alkalinity(CaCO_3) dropped from 800mg/L to 400mg/L. During these days, COD removal rate dropped down for a while, but it ran into normal quickly.
The TPAD reactor reached its highest condition when influent COD up to 7058 mg/L which was after ammonia nitrogen removing pretreatment. The COD removal rate was 55%, and the souring reactor could remove 11.1% COD, 1st methane reactor could remove 17.4% COD, 2st methane reactor could remove 25.1% COD. TPAD effluent was treated by actived sludge treatment to study the feasibility of aerobic treatment after diluting COD to 1000mg/L. When HRT was 16h, actived sludge treatment could remove 61.3% COD and 76.1% chroma.
We got N-Phenylglycinonitrile biodegradation dynamic model with 1st methane reactor, 2st methane reactor and TPAD reactor by curve fitting with Origin software custom fitted curve based on Nerfeld modified Monod equation. Research on bacterial community by contrasting acclimated sludge with seed sludge in different treatment unit with PCR-TGGE technique, we draw conclusion as follows: acclimating process could change bacterial diversity and community greatly, the dice coefficient between seed sludge and acclimated sludge was 48.0%、48.2%、59.7%、56.8% and 50.6%、50.2%, Analysis of NMDS showed there were differences in sludge of first steps of souring process, but less difference in the last steps, and more less differences between 1st methane sluge and 2st methane sludge.
引文
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