鸟粪石沉淀法去除和回收废水中氨氮和磷的实验研究
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摘要
氮磷是导致水体富营养化的关键因素，磷是一种不可再生的宝贵资源。随着污染物排放标准的日趋严格以及磷资源的日益匮乏，废水脱氮除磷技术以及磷资源化回收技术的研究与开发无疑具有重要意义。鸟粪石沉淀法可同时去除和回收废水中的氨氮和磷，回收产物可作为一种高效缓释肥，具有广阔的开发应用前景。
本文首先采用鸟粪石沉淀法对两种高浓度实际工业废水进行脱氮除磷处理，考察了各因素对氨氮和磷的去除和回收效果的影响，得出了最佳工艺条件；为降低药剂消耗，降低处理成本，采用以废治废的新思路，将两种废水混合后进行处理，考察了各因素对混合废水脱氮除磷效果的影响，得出了混合废水处理的最佳工艺条件；结合扫描电镜、X射线衍射、化学分析等方法对沉淀产物的结构形态、组成成分以及沉淀产物中重金属元素的含量等进行了分析；探讨了鸟粪石沉淀法的反应机理；最后对鸟粪石沉淀法去除和回收氨氮和磷的环境效益和经济效益进行了分析。论文主要结论如下：
（1）采用鸟粪石沉淀法去除和回收PO_4~(3-)-P含量为5399.83~5475.62mg·L~(-1)的高浓度含磷废水中的磷，在pH=9.5，n(Mg):n(N):n(P)=1.25:1.05:1，搅拌速率为200r·min-1左右，反应20min，沉淀20min的条件下，废水中PO_4~(3-)-P的去除率为99.96%，处理出水中PO_4~(3-)-P的残留量为2.20mg·L~(-1)，NH_4~+-N的残留量为213.14mg·L~(-1)。
（2）采用鸟粪石沉淀法去除和回收NH_4~+-N含量为562.97~677.28mg·L~(-1)的高浓度氨氮废水中的氨氮，在pH=9.5，n(Mg):n(P):n(N)=1.15:0.95:1，搅拌速率为150r·min-1左右，反应20min，沉淀20min的条件下，废水中NH_4~+-N的去除率为94.14%，处理出水中NH_4~+-N的残留量为38.21mg·L~(-1)，PO_4~(3-)-P的残留量为49.43mg·L~(-1)。
（3）处理PO_4~(3-)-P含量为7374.53mg·L~(-1)的高浓度含磷废水与NH_4~+-N含量为717.47mg·L~(-1)的高浓度氨氮废水的混合废水时，在高浓度含磷废水与高浓度氨氮废水按体积比为1:4.5混合，pH=9.5，n(Mg):n(P)=1.2:1，搅拌速率为200r·min-1左右，反应20min，沉淀20min的条件下，混合废水中PO_4~(3-)-P的去除率为99.64%，NH_4~+-N的去除率为88.62%，处理出水中PO_4~(3-)-P的残留量为4.86mg·L~(-1)，NH_4~+-N的残留量为70.76mg·L~(-1)。
（4）最佳工艺条件下得到的沉淀产物的扫描电镜结果显示沉淀产物为斜方晶体，X射线衍射分析结果表明沉淀产物的主要成分为MgNH_4PO_4·6H_2O，其N、P、Mg含量与鸟粪石理论值较为接近，沉淀产物中的重金属元素含量符合《肥料中砷、镉、铅、铬、汞生态指标》（GB/T23349-2009）相关要求，可作为缓释肥加以回收利用。
（5）实验研究和理论分析结果表明，反应物摩尔配比和pH值对鸟粪石沉淀法从废水中去除和回收氨氮和磷的效果有很大影响。
（6）鸟粪石沉淀法能有效的去除和回收废水中的氨氮和磷，具有较好的环境效益和经济效益；采用以废治废的新思路处理高浓度氮磷废水可大大节约药剂费用，是一种技术可行，经济合理的方法，具有很好的开发应用前景。
Nitrogen and phosphorus are key factors leading to the eutrophication of water bodies, andphosphorus is also a precious non-renewable resources. With the increasingly stringentpollutant discharge standards and the growing scarcity of phosphorus resources, the researchand development of the technology for the removal of nitrogen and phosphorus fromwastewater and the resource recycling technology of phosphorus is undoubtedly important. Thestruvite precipitation method can simultaneously remove and recover ammonia nitrogen andphosphorus from wastewater, and the products recovered can be used as a kind of high efficientslow-release fertilizer, therefore it has a wide prospect for development and application.
In this thesis, the removal of ammonia nitrogen and phosphorus from two kinds of highconcentration practical industrial wastewater by struvite precipitation method was firstlystudied. The influences of factors on the ammonia nitrogen and phosphorus removal andrecovery efficiency were investigated respectively, and the optimal process conditions wereobtained. In order to reduce the chemical consumption and the treatment cost, the new idea thatusing waste to treat waste was used. The two kinds of wastewater were mixed, and then weretreated by using the same method. The influences of factors on mixed wastewater treatmentwere also investigated, and the best process conditions for mixed wastewater were obtained.The structure, constituent and heavy metals content of the precipitates were analyzed byscanning electron microscope, X-ray diffraction, chemical analysis and other methods. Thereaction mechanism of the struvite precipitation method was also discussed. Finally, analyseswere conducted on the environmental and economic benefits of removal and recovery ammonianitrogen and phosphorus from wastewater by struvite precipitation method. The mainconclusions of the thesis were as follows:
(1) Phosphorus was removed and recovered from high concentration phosphorus-containing wastewater that the concentration of PO_4~(3-)-P is5399.83~5475.62mg·L~(-1)by struviteprecipitation method, while pH=9.5, n(Mg):n(N):n(P)=1.25:1.05:1,stirring speed was about200r·min-1, reaction time was20min, precipitation time was20min, the removal rate of PO_4~(3-)-P was99.96%, the concentration of PO_4~(3-)-P in the treated water was2.20mg·L~(-1),and the concentrationof NH_4~+-N in the treated water was213.14mg·L~(-1).
(2) Ammonia nitrogen was removed and recovered from high ammonia nitrogen contentwastewater that the concentration of NH_4~+-N is562.97~677.28mg·L~(-1)by struvite precipitationmethod, while pH=9.5, n(Mg):n(P):n(N)=1.15:0.95:1, stirring speed was about150r·min-1,reaction time was20min, precipitation time was20min, the removal rate of NH_4~+-N was94.14%, the concentration of NH_4~+-N in the treated water was38.21mg·L~(-1), the concentrationof PO_4~(3-)-P in the treated water was49.43mg·L~(-1).
(3) When treating the mixed wastewater containing high concentration phosphorus-containing wastewater that the concentration of PO_4~(3-)-P is7374.53mg·L~(-1)and high ammonianitrogen content wastewater that the concentration of NH_4~+-N is717.47mg·L~(-1), while highconcentration phosphorus-containing wastewater and high ammonia nitrogen content waste-water were mixed1:4.5by volume, pH=9.5, n(Mg):n(P)=1.2:1, stirring speed was about200r·min-1, reaction time was20min, precipitation time was20min, the removal rate of PO_4~(3-)-Pwas99.64%, the removal rate of NH_4~+-N was88.62%, the concentration of PO_4~(3-)-P in thetreated water was4.86mg·L~(-1), and the concentration of NH_4~+-N in the treated water was70.76mg·L~(-1).
(4) The result of scanning electron microscope of the precipitates obtained under theoptimal process conditions indicated that the precipitates had rhombic structure. X-raydiffraction analysis results showed that the precipitates were mainly composed ofMgNH4PO4·6H2O.And the content of N, P and Mg were close to the theoretical content ofstruvite. The content of heavy metals elements in the precipitates was consistent with therequirements of the ecological index of arsenic, cadmium, lead, chromium and mercury forfertilizers(GB/T23349-2009). And it can be recycled as slow-release fertilizer.
(5) The result of experiment research and theoretical analysis indicated that the reactantmolar ratio and pH had a great influence on the effects of removal and recovery ammonianitrogen and phosphorus from wastewater by struvite precipitation method.
(6) The struvite precipitation method can effectively remove and recover ammonianitrogen and phosphorus from wastewater.It has better economic and environmental benefits. Itcan greatly reduce the chemical agent costs by use the new idea that using waste to treat waste,it is a technically feasible and economically reasonable method, and has great development andapplication prospect.
本文首先采用鸟粪石沉淀法对两种高浓度实际工业废水进行脱氮除磷处理，考察了各因素对氨氮和磷的去除和回收效果的影响，得出了最佳工艺条件；为降低药剂消耗，降低处理成本，采用以废治废的新思路，将两种废水混合后进行处理，考察了各因素对混合废水脱氮除磷效果的影响，得出了混合废水处理的最佳工艺条件；结合扫描电镜、X射线衍射、化学分析等方法对沉淀产物的结构形态、组成成分以及沉淀产物中重金属元素的含量等进行了分析；探讨了鸟粪石沉淀法的反应机理；最后对鸟粪石沉淀法去除和回收氨氮和磷的环境效益和经济效益进行了分析。论文主要结论如下：
（1）采用鸟粪石沉淀法去除和回收PO_4~(3-)-P含量为5399.83~5475.62mg·L~(-1)的高浓度含磷废水中的磷，在pH=9.5，n(Mg):n(N):n(P)=1.25:1.05:1，搅拌速率为200r·min-1左右，反应20min，沉淀20min的条件下，废水中PO_4~(3-)-P的去除率为99.96%，处理出水中PO_4~(3-)-P的残留量为2.20mg·L~(-1)，NH_4~+-N的残留量为213.14mg·L~(-1)。
（2）采用鸟粪石沉淀法去除和回收NH_4~+-N含量为562.97~677.28mg·L~(-1)的高浓度氨氮废水中的氨氮，在pH=9.5，n(Mg):n(P):n(N)=1.15:0.95:1，搅拌速率为150r·min-1左右，反应20min，沉淀20min的条件下，废水中NH_4~+-N的去除率为94.14%，处理出水中NH_4~+-N的残留量为38.21mg·L~(-1)，PO_4~(3-)-P的残留量为49.43mg·L~(-1)。
（3）处理PO_4~(3-)-P含量为7374.53mg·L~(-1)的高浓度含磷废水与NH_4~+-N含量为717.47mg·L~(-1)的高浓度氨氮废水的混合废水时，在高浓度含磷废水与高浓度氨氮废水按体积比为1:4.5混合，pH=9.5，n(Mg):n(P)=1.2:1，搅拌速率为200r·min-1左右，反应20min，沉淀20min的条件下，混合废水中PO_4~(3-)-P的去除率为99.64%，NH_4~+-N的去除率为88.62%，处理出水中PO_4~(3-)-P的残留量为4.86mg·L~(-1)，NH_4~+-N的残留量为70.76mg·L~(-1)。
（4）最佳工艺条件下得到的沉淀产物的扫描电镜结果显示沉淀产物为斜方晶体，X射线衍射分析结果表明沉淀产物的主要成分为MgNH_4PO_4·6H_2O，其N、P、Mg含量与鸟粪石理论值较为接近，沉淀产物中的重金属元素含量符合《肥料中砷、镉、铅、铬、汞生态指标》（GB/T23349-2009）相关要求，可作为缓释肥加以回收利用。
（5）实验研究和理论分析结果表明，反应物摩尔配比和pH值对鸟粪石沉淀法从废水中去除和回收氨氮和磷的效果有很大影响。
（6）鸟粪石沉淀法能有效的去除和回收废水中的氨氮和磷，具有较好的环境效益和经济效益；采用以废治废的新思路处理高浓度氮磷废水可大大节约药剂费用，是一种技术可行，经济合理的方法，具有很好的开发应用前景。
Nitrogen and phosphorus are key factors leading to the eutrophication of water bodies, andphosphorus is also a precious non-renewable resources. With the increasingly stringentpollutant discharge standards and the growing scarcity of phosphorus resources, the researchand development of the technology for the removal of nitrogen and phosphorus fromwastewater and the resource recycling technology of phosphorus is undoubtedly important. Thestruvite precipitation method can simultaneously remove and recover ammonia nitrogen andphosphorus from wastewater, and the products recovered can be used as a kind of high efficientslow-release fertilizer, therefore it has a wide prospect for development and application.
In this thesis, the removal of ammonia nitrogen and phosphorus from two kinds of highconcentration practical industrial wastewater by struvite precipitation method was firstlystudied. The influences of factors on the ammonia nitrogen and phosphorus removal andrecovery efficiency were investigated respectively, and the optimal process conditions wereobtained. In order to reduce the chemical consumption and the treatment cost, the new idea thatusing waste to treat waste was used. The two kinds of wastewater were mixed, and then weretreated by using the same method. The influences of factors on mixed wastewater treatmentwere also investigated, and the best process conditions for mixed wastewater were obtained.The structure, constituent and heavy metals content of the precipitates were analyzed byscanning electron microscope, X-ray diffraction, chemical analysis and other methods. Thereaction mechanism of the struvite precipitation method was also discussed. Finally, analyseswere conducted on the environmental and economic benefits of removal and recovery ammonianitrogen and phosphorus from wastewater by struvite precipitation method. The mainconclusions of the thesis were as follows:
(1) Phosphorus was removed and recovered from high concentration phosphorus-containing wastewater that the concentration of PO_4~(3-)-P is5399.83~5475.62mg·L~(-1)by struviteprecipitation method, while pH=9.5, n(Mg):n(N):n(P)=1.25:1.05:1,stirring speed was about200r·min-1, reaction time was20min, precipitation time was20min, the removal rate of PO_4~(3-)-P was99.96%, the concentration of PO_4~(3-)-P in the treated water was2.20mg·L~(-1),and the concentrationof NH_4~+-N in the treated water was213.14mg·L~(-1).
(2) Ammonia nitrogen was removed and recovered from high ammonia nitrogen contentwastewater that the concentration of NH_4~+-N is562.97~677.28mg·L~(-1)by struvite precipitationmethod, while pH=9.5, n(Mg):n(P):n(N)=1.15:0.95:1, stirring speed was about150r·min-1,reaction time was20min, precipitation time was20min, the removal rate of NH_4~+-N was94.14%, the concentration of NH_4~+-N in the treated water was38.21mg·L~(-1), the concentrationof PO_4~(3-)-P in the treated water was49.43mg·L~(-1).
(3) When treating the mixed wastewater containing high concentration phosphorus-containing wastewater that the concentration of PO_4~(3-)-P is7374.53mg·L~(-1)and high ammonianitrogen content wastewater that the concentration of NH_4~+-N is717.47mg·L~(-1), while highconcentration phosphorus-containing wastewater and high ammonia nitrogen content waste-water were mixed1:4.5by volume, pH=9.5, n(Mg):n(P)=1.2:1, stirring speed was about200r·min-1, reaction time was20min, precipitation time was20min, the removal rate of PO_4~(3-)-Pwas99.64%, the removal rate of NH_4~+-N was88.62%, the concentration of PO_4~(3-)-P in thetreated water was4.86mg·L~(-1), and the concentration of NH_4~+-N in the treated water was70.76mg·L~(-1).
(4) The result of scanning electron microscope of the precipitates obtained under theoptimal process conditions indicated that the precipitates had rhombic structure. X-raydiffraction analysis results showed that the precipitates were mainly composed ofMgNH4PO4·6H2O.And the content of N, P and Mg were close to the theoretical content ofstruvite. The content of heavy metals elements in the precipitates was consistent with therequirements of the ecological index of arsenic, cadmium, lead, chromium and mercury forfertilizers(GB/T23349-2009). And it can be recycled as slow-release fertilizer.
(5) The result of experiment research and theoretical analysis indicated that the reactantmolar ratio and pH had a great influence on the effects of removal and recovery ammonianitrogen and phosphorus from wastewater by struvite precipitation method.
(6) The struvite precipitation method can effectively remove and recover ammonianitrogen and phosphorus from wastewater.It has better economic and environmental benefits. Itcan greatly reduce the chemical agent costs by use the new idea that using waste to treat waste,it is a technically feasible and economically reasonable method, and has great development andapplication prospect.
引文
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