基于磷酸铵镁结晶法的氨氮回收技术过程研究
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摘要
氨氮污染已经成为我国地表水的主要污染源,作为“十二·五”期间节能减排战略中新增的约束性指标,氨氮废水处理技术的理论研究与技术应用具有巨大的市场潜力和产业化应用前景。磷酸铵镁结晶法,通过向废水中投加镁盐和磷酸盐与废水中的氨氮反应生成磷酸铵镁沉淀,可快速高效去除回收废水中氨氮。目前,磷酸铵镁结晶法已经成为氨氮废水处理与氨氮资源回收的热点研究技术之一。
但是,磷酸铵镁结晶法氨氮回收技术过程中的参数调控、化学污泥利用,结晶反应装备等问题是制约该技术推广应用的主要影响因素。本论文以“基于磷酸铵镁结晶法的氨氮回收技术过程研究”为题,针对目前技术过程中的技术瓶颈——参数调控、化学污泥、结晶反应装备,采用精准沉淀反应调控、PHREEQC建模优化、响应面智能化评估、磷酸铵镁热解脱氨、化学药剂循环沉氨、U型流向路线设计、一体化连续流控制等技术路线,开展磷酸铵镁结晶法反应参数优化研究、热力学建模评估技术研究、磷酸铵镁碱促热解循环沉氨技术研究、一体化新型结晶器研制等系列研究,为实施磷酸铵镁结晶法回收氨氮技术过程提供依据。主要研究成果如下：
(1)优化了磷酸铵镁结晶法氨氮回收技术过程工艺参数
对磷酸铵镁结晶法回收氨氮的参数调控情况,磷酸铵镁结晶动力学反应,化学污泥表征进行重点研究,结果表明：最佳的反应pH值范围为9.0-10.5；最佳的Mg2+:NH4+:PO43-范围为1.1-1.2:1:1; MgCl2·6H2O和Na2HPO4·12H2O沉淀剂组合沉氨效果最好；干扰离子Ca2+、CO32-、K+,离子强度,以及温度会影响磷酸铵镁结晶回收氨氮效果；磷酸铵镁结晶的动力学反应过程符合一级反应动力学；X射线衍射分析和傅里叶变换红外光谱分析表明磷酸铵镁是沉淀产物的主要成分,扫描电子显微镜及能谱分析表明沉淀产物为不规则形态表面粗糙晶体。
(2)建立了磷酸铵镁结晶法的热力学评估预测模型
开发单因素仿真模拟与多因素评估的磷酸铵镁结晶模型,对于参数调控优化的理论研究与工程应用具有预测评估作用,结果表明：磷酸铵镁饱和溶解指数值与pH值呈现多项式关系,分别与镁氮比(Mg/N)、初始氮浓度(CN)、磷氮比(P/N)呈现对数关系,随Mg/N、CN、P/N的增加而增加,分别随钙氮比(Ca/N)、碳酸根氮比(C032-/N)增加而降低,随离子强度增加而降低,随温度变化而变化；响应面优化法(RSM)分析认为pH、Mg/N、CN、Ca/N、(Mg/N)×(CO32-/N)、(pH)2、(Mg/N)2、以及(CN)2是磷酸铵镁结晶的相对显著影响因子；实验证明热力学建模有效预测磷酸铵镁结晶法回收氨氮效率变化趋势。
(3)解析了化学沉氨碱促热解循环沉氨技术
利用磷酸铵镁热解脱氨及化学药剂循环沉氨的技术路线,开展磷酸铵镁碱促热解循环沉氨技术研究,结果表明：当热解温度为110℃,热解时间为3小时,OH":NH4+为2：1时,磷酸铵镁碱促热解脱氨效率大于90%,脱出氨氮可采用硫酸进行资源化回收；热解产物循环沉氨最佳pH值为9.5；只添加磷酸铵镁热解产物循环作沉淀剂时,沉氨效率随循环次数增加而下降,每次循环添加磷酸铵镁热解产物基础上投加MgCl2·6H2O和Na2HPO4·12H2O作为补充,沉氨效率不随循环次数增加而下降；使用预制磷酸铵镁作为晶种材料的加晶种技术可提高热解产物循环沉氨效率。
(4)研制出了一体化连续流机械搅拌式结晶器
开展一体化新型磷酸铵镁结晶器的研制,设计一体化连续流机械搅拌式结晶器(CSCSR),并对其运行情况进行研究,结果表明：采用U型流向路线设计,基于磷酸铵镁结晶原理进行模块分区研制CSCSR,在初始pH值为11.0、Mg/N为1：1、HRT为1.5h、Ca/N为0：1时,氨氮去除率达到91.08%；RSM分析认为Mg/N、Ca/N为CSCSR运行的显著影响因子。
One of the major environmental concerns associated with surface water environment is related to the pollution of ammonium nitrogen. Now, ammonium nitrogen is used as an additional controlled indicator for energy saving and emission reduction strategy of "12Five Year Plan". As a result, the technology for ammonium nitrogen removal will show great market potential and industrial applications prospects. Ammonium nitrogen removal by adding magnesium salt and phosphate to form magnesium ammonium phosphate hexahydrate (MAP) crystallization is a useful method. Recently, MAP precipitation of ammonium has been studied widely.
However, the problem, parameter controlled, magnesium ammonium phosphate disposal, and crystallized-settled reactor designed, that hamper the wide application of MAP precipitation. In the present research of "Ammonium Nitrogen Recovery from Wastewater by Magnesium Ammonium Phosphate Crystallization", the problem, parameter controlled, magnesium ammonium phosphate disposal, and crystallized-settled reactor designed, that was investigated by the method of extract precipitation reaction control, PHREEQC thermodynamic modeling, response surface methodology evaluation, magnesium ammonium phosphate pyrogenation, chemical precipitation pyrogenation recycle, U-shape flow course design, and continuous stirred crystallized-settled reactor control. The research of MAP precipitation parameter control technology, thermodynamic modeling assessment technology, chemical precipitation recycle technology, and continuous stirred crystallized-settled reactor function technology, were examined. The main results are as follows:
(1) Ammonium nitrogen recovery from wastewater by MAP precipitation
Taking into account the problem of parameter controlled, ammonium nitrogen recovery from wastewater by MAP precipitation was investigated and the following conclusions could be obtained. When MgCl2·6H2O and Na2HPO4·12H2O were employed, the optimum pH was9.0-10.5and the molar ratio of Mg2+:NH4+:PO43-was controlled at1.1-1.2:1:1in order to recovery ammonium effectively and avoid higher concentration of PO43-in the effluent. MgCl2·6H2O plus Na2HPO4·12H2O was the most efficient for ammonium removal. The interfering ions of Ca+, CO32-, and K+could obviously affect ammonium nitrogen recovery efficiency. The ionic strength, and temperature could also affect ammonium nitrogen recovery efficiency. The kinetics experiment showed that the rate of reaction was closer to the first order kinetic model. Fourier transform infrared spectroscopy and X-ray diffraction analysis indicated that MAP was the main composition of the precipitates. Scanning electron microscopy with energy dispersive X-ray analysis indicated that the unshaped crystal was coarse and its size was irregular, the surface composition of the precipitates contains a great deal of O, P, Mg.
(2) Thermodynamic modeling assessment for ammonium nitrogen recovery by MAP precipitation
Thermodynamic modeling was developed for predicting ammonium nitrogen recovery from wastewater by MAP precipitation. Response surface methodology (RSM) was applied to assist in understanding the relative significance of reaction factors and the interactive effects of solution conditions. The following conclusions were drawn. The saturation index (SI) of MAP followed a polynomial function of pH. The SI of MAP increased and followed a logarithmic function of the concentration of magnesium, ammonium, and phosphate, respectively. The SI of MAP decreased with an increase in the concentration of calcium, carbonate, respectively. The SI of MAP decreased with an increase in ionic strength. Temperature could obviously affect the SI of MAP. The RSM analysis indicated that the factors pH, Mg/N, CN, Ca/N,(Mg/N) x (CO32-/N),(pH)2,(Mg/N), and (Cn)2were significant. Thermodynamic modeling was validated by comparing it with the case study.
(3) Ammonium nitrogen removal by chemical precipitation recycle technology
Taking into account the problem of magnesium ammonium phosphate disposal, chemical precipitation recycle technology (CPRT) for ammonium nitrogen removal from wastewater was examined. The pyrolysate resulting from magnesium ammonium phosphate pyrogenation in sodium hydroxide solution was recycled for ammonium nitrogen removal from wastewater, and the following conclusions were drawn. The MAP pyrolysate could be produced at the optimal condition of a hydroxyl to ammonium molar ratio of2:1, a heating temperature of110℃, and a heating time of3h. The pyrolysate could be recycled as a magnesium and phosphate source at an optimum pH of9.5. When the recycle times were increased, the ammonium nitrogen removal ratio gradually decreased if the pyrolysate was used without supplementation. When the recycle times were increased, the ammonium nitrogen removal efficiency was not decreased if the added pyrolysate was supplemented with MgCl2-6H2O plus Na2HPO4·12H2O during treatment. A high ammonium nitrogen removal ratio was obtained by using pre-formed MAP as seeding material.
(4) New continuous crystallization reactor designed for ammonium nitrogen recovery as MAP precipitation
Taking into account the problem of crystallized-settled reactor, a new continuous crystallization reactor was designed for ammonium nitrogen recovery as MAP precipitation. The reactor practical operation was studied, and the following conclusions were drawn. A continuous stirred crystallized-settled reactor (CSCSR), adopted U-shaped flow course design, consists of column coagulation implement, filler baffle-wall, taper stabilization implement, and settlement tank. The ammonium nitrogen recovery efficiency was91.08%at the condition of pH11.0, Mg/N1:1, HRT1.5h, and Ca/N0:1. The RSM analysis indicated that the factors Mg/N, and Ca/N were significant.
但是,磷酸铵镁结晶法氨氮回收技术过程中的参数调控、化学污泥利用,结晶反应装备等问题是制约该技术推广应用的主要影响因素。本论文以“基于磷酸铵镁结晶法的氨氮回收技术过程研究”为题,针对目前技术过程中的技术瓶颈——参数调控、化学污泥、结晶反应装备,采用精准沉淀反应调控、PHREEQC建模优化、响应面智能化评估、磷酸铵镁热解脱氨、化学药剂循环沉氨、U型流向路线设计、一体化连续流控制等技术路线,开展磷酸铵镁结晶法反应参数优化研究、热力学建模评估技术研究、磷酸铵镁碱促热解循环沉氨技术研究、一体化新型结晶器研制等系列研究,为实施磷酸铵镁结晶法回收氨氮技术过程提供依据。主要研究成果如下：
(1)优化了磷酸铵镁结晶法氨氮回收技术过程工艺参数
对磷酸铵镁结晶法回收氨氮的参数调控情况,磷酸铵镁结晶动力学反应,化学污泥表征进行重点研究,结果表明：最佳的反应pH值范围为9.0-10.5；最佳的Mg2+:NH4+:PO43-范围为1.1-1.2:1:1; MgCl2·6H2O和Na2HPO4·12H2O沉淀剂组合沉氨效果最好；干扰离子Ca2+、CO32-、K+,离子强度,以及温度会影响磷酸铵镁结晶回收氨氮效果；磷酸铵镁结晶的动力学反应过程符合一级反应动力学；X射线衍射分析和傅里叶变换红外光谱分析表明磷酸铵镁是沉淀产物的主要成分,扫描电子显微镜及能谱分析表明沉淀产物为不规则形态表面粗糙晶体。
(2)建立了磷酸铵镁结晶法的热力学评估预测模型
开发单因素仿真模拟与多因素评估的磷酸铵镁结晶模型,对于参数调控优化的理论研究与工程应用具有预测评估作用,结果表明：磷酸铵镁饱和溶解指数值与pH值呈现多项式关系,分别与镁氮比(Mg/N)、初始氮浓度(CN)、磷氮比(P/N)呈现对数关系,随Mg/N、CN、P/N的增加而增加,分别随钙氮比(Ca/N)、碳酸根氮比(C032-/N)增加而降低,随离子强度增加而降低,随温度变化而变化；响应面优化法(RSM)分析认为pH、Mg/N、CN、Ca/N、(Mg/N)×(CO32-/N)、(pH)2、(Mg/N)2、以及(CN)2是磷酸铵镁结晶的相对显著影响因子；实验证明热力学建模有效预测磷酸铵镁结晶法回收氨氮效率变化趋势。
(3)解析了化学沉氨碱促热解循环沉氨技术
利用磷酸铵镁热解脱氨及化学药剂循环沉氨的技术路线,开展磷酸铵镁碱促热解循环沉氨技术研究,结果表明：当热解温度为110℃,热解时间为3小时,OH":NH4+为2：1时,磷酸铵镁碱促热解脱氨效率大于90%,脱出氨氮可采用硫酸进行资源化回收；热解产物循环沉氨最佳pH值为9.5；只添加磷酸铵镁热解产物循环作沉淀剂时,沉氨效率随循环次数增加而下降,每次循环添加磷酸铵镁热解产物基础上投加MgCl2·6H2O和Na2HPO4·12H2O作为补充,沉氨效率不随循环次数增加而下降；使用预制磷酸铵镁作为晶种材料的加晶种技术可提高热解产物循环沉氨效率。
(4)研制出了一体化连续流机械搅拌式结晶器
开展一体化新型磷酸铵镁结晶器的研制,设计一体化连续流机械搅拌式结晶器(CSCSR),并对其运行情况进行研究,结果表明：采用U型流向路线设计,基于磷酸铵镁结晶原理进行模块分区研制CSCSR,在初始pH值为11.0、Mg/N为1：1、HRT为1.5h、Ca/N为0：1时,氨氮去除率达到91.08%；RSM分析认为Mg/N、Ca/N为CSCSR运行的显著影响因子。
One of the major environmental concerns associated with surface water environment is related to the pollution of ammonium nitrogen. Now, ammonium nitrogen is used as an additional controlled indicator for energy saving and emission reduction strategy of "12Five Year Plan". As a result, the technology for ammonium nitrogen removal will show great market potential and industrial applications prospects. Ammonium nitrogen removal by adding magnesium salt and phosphate to form magnesium ammonium phosphate hexahydrate (MAP) crystallization is a useful method. Recently, MAP precipitation of ammonium has been studied widely.
However, the problem, parameter controlled, magnesium ammonium phosphate disposal, and crystallized-settled reactor designed, that hamper the wide application of MAP precipitation. In the present research of "Ammonium Nitrogen Recovery from Wastewater by Magnesium Ammonium Phosphate Crystallization", the problem, parameter controlled, magnesium ammonium phosphate disposal, and crystallized-settled reactor designed, that was investigated by the method of extract precipitation reaction control, PHREEQC thermodynamic modeling, response surface methodology evaluation, magnesium ammonium phosphate pyrogenation, chemical precipitation pyrogenation recycle, U-shape flow course design, and continuous stirred crystallized-settled reactor control. The research of MAP precipitation parameter control technology, thermodynamic modeling assessment technology, chemical precipitation recycle technology, and continuous stirred crystallized-settled reactor function technology, were examined. The main results are as follows:
(1) Ammonium nitrogen recovery from wastewater by MAP precipitation
Taking into account the problem of parameter controlled, ammonium nitrogen recovery from wastewater by MAP precipitation was investigated and the following conclusions could be obtained. When MgCl2·6H2O and Na2HPO4·12H2O were employed, the optimum pH was9.0-10.5and the molar ratio of Mg2+:NH4+:PO43-was controlled at1.1-1.2:1:1in order to recovery ammonium effectively and avoid higher concentration of PO43-in the effluent. MgCl2·6H2O plus Na2HPO4·12H2O was the most efficient for ammonium removal. The interfering ions of Ca+, CO32-, and K+could obviously affect ammonium nitrogen recovery efficiency. The ionic strength, and temperature could also affect ammonium nitrogen recovery efficiency. The kinetics experiment showed that the rate of reaction was closer to the first order kinetic model. Fourier transform infrared spectroscopy and X-ray diffraction analysis indicated that MAP was the main composition of the precipitates. Scanning electron microscopy with energy dispersive X-ray analysis indicated that the unshaped crystal was coarse and its size was irregular, the surface composition of the precipitates contains a great deal of O, P, Mg.
(2) Thermodynamic modeling assessment for ammonium nitrogen recovery by MAP precipitation
Thermodynamic modeling was developed for predicting ammonium nitrogen recovery from wastewater by MAP precipitation. Response surface methodology (RSM) was applied to assist in understanding the relative significance of reaction factors and the interactive effects of solution conditions. The following conclusions were drawn. The saturation index (SI) of MAP followed a polynomial function of pH. The SI of MAP increased and followed a logarithmic function of the concentration of magnesium, ammonium, and phosphate, respectively. The SI of MAP decreased with an increase in the concentration of calcium, carbonate, respectively. The SI of MAP decreased with an increase in ionic strength. Temperature could obviously affect the SI of MAP. The RSM analysis indicated that the factors pH, Mg/N, CN, Ca/N,(Mg/N) x (CO32-/N),(pH)2,(Mg/N), and (Cn)2were significant. Thermodynamic modeling was validated by comparing it with the case study.
(3) Ammonium nitrogen removal by chemical precipitation recycle technology
Taking into account the problem of magnesium ammonium phosphate disposal, chemical precipitation recycle technology (CPRT) for ammonium nitrogen removal from wastewater was examined. The pyrolysate resulting from magnesium ammonium phosphate pyrogenation in sodium hydroxide solution was recycled for ammonium nitrogen removal from wastewater, and the following conclusions were drawn. The MAP pyrolysate could be produced at the optimal condition of a hydroxyl to ammonium molar ratio of2:1, a heating temperature of110℃, and a heating time of3h. The pyrolysate could be recycled as a magnesium and phosphate source at an optimum pH of9.5. When the recycle times were increased, the ammonium nitrogen removal ratio gradually decreased if the pyrolysate was used without supplementation. When the recycle times were increased, the ammonium nitrogen removal efficiency was not decreased if the added pyrolysate was supplemented with MgCl2-6H2O plus Na2HPO4·12H2O during treatment. A high ammonium nitrogen removal ratio was obtained by using pre-formed MAP as seeding material.
(4) New continuous crystallization reactor designed for ammonium nitrogen recovery as MAP precipitation
Taking into account the problem of crystallized-settled reactor, a new continuous crystallization reactor was designed for ammonium nitrogen recovery as MAP precipitation. The reactor practical operation was studied, and the following conclusions were drawn. A continuous stirred crystallized-settled reactor (CSCSR), adopted U-shaped flow course design, consists of column coagulation implement, filler baffle-wall, taper stabilization implement, and settlement tank. The ammonium nitrogen recovery efficiency was91.08%at the condition of pH11.0, Mg/N1:1, HRT1.5h, and Ca/N0:1. The RSM analysis indicated that the factors Mg/N, and Ca/N were significant.
引文
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