CN109928542A - A kind of integrated apparatus and method for realizing ammonium magnesium phosphate efficient crystallization and separation of solid and liquid - Google Patents

A kind of integrated apparatus and method for realizing ammonium magnesium phosphate efficient crystallization and separation of solid and liquid Download PDF

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CN109928542A
CN109928542A CN201910232535.4A CN201910232535A CN109928542A CN 109928542 A CN109928542 A CN 109928542A CN 201910232535 A CN201910232535 A CN 201910232535A CN 109928542 A CN109928542 A CN 109928542A
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crystallization
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liquid
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郝瑞霞
李鹏
李嘉雯
孙彤
武旭源
李宏康
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Beijing University of Technology
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Abstract

A kind of integrated apparatus that realizing ammonium magnesium phosphate efficient crystallization and separation of solid and liquid and method belong to sewage recycling processing technology field.Hybrid reaction crystal region is connected with intake pump;Solid-liquid displacement zone is set to inner cylinder between outer cylinder;Buffer area is in hybrid reaction crystal region lower part;MAP sludge area is set in the cone of reactor bottom, and its bottom connects large aperture valve;Exhalant region is arranged in reactor head, and the mode of overflow is taken to be discharged.Reactor operation operation includes crystallization reaction and separation of solid and liquid process.Reactor assembly takes Quick mechanical agitating mode to accelerate crystallization reaction, to improve reactor for treatment ability;The deflector type continuous flow processing mode for taking Inlet and outlet water in the same direction simultaneously extends the flow path of material in the reactor, keeps crystallization reaction and separation of solid and liquid process more abundant;By the way that inclined plate is arranged, it can be achieved that high efficient solid and liquid separation, the loss and secondary pollution of MAP when avoiding water outlet in solid-liquid displacement zone.

Description

一种实现磷酸铵镁高效结晶及固液分离的一体化装置及方法A kind of integrated device and method for realizing high-efficiency crystallization and solid-liquid separation of magnesium ammonium phosphate

技术领域technical field

本发明涉及污水资源化处理技术领域。主要是实现磷酸铵镁(MAP)高效结晶及固液分离的一体化装置及方法。The invention relates to the technical field of sewage resource treatment. It is mainly an integrated device and method for realizing high-efficiency crystallization and solid-liquid separation of magnesium ammonium phosphate (MAP).

背景技术Background technique

在污水资源化处理领域中,磷酸铵镁结晶法作为一种氮磷废水处理工艺,以其可同步回收污水中的氮磷资源等优点,在氮磷废水资源化处理领域受到了越来越多学者的青睐。反应器是MAP结晶技术的核心装置,是将MAP结晶技术与工程应用紧密联系的纽带,反应器的研究与应用能够加快实现MAP氮磷回收技术产业化,从而实现环境与经济的可持续发展。目前,国内外学者在MAP结晶反应器的理论研究和工程试验方面已开展了一些工作,但是现有的MAP结晶反应器仍然存在固液分离不彻底、氨磷回收率不理想等诸多问题,限制了该技术的工程推广应用。In the field of wastewater resource treatment, magnesium ammonium phosphate crystallization, as a nitrogen and phosphorus wastewater treatment process, has received more and more favored by scholars. The reactor is the core device of MAP crystallization technology, and it is the link that closely links MAP crystallization technology with engineering applications. The research and application of the reactor can accelerate the industrialization of MAP nitrogen and phosphorus recovery technology, so as to realize the sustainable development of the environment and economy. At present, scholars at home and abroad have carried out some work in the theoretical research and engineering experiments of MAP crystallization reactors, but the existing MAP crystallization reactors still have many problems such as incomplete solid-liquid separation and unsatisfactory ammonia phosphorus recovery rate. The engineering popularization and application of this technology.

MAP结晶反应器的设计主要依据结晶反应动力学和反应器流态调控两个要素,既要使得溶液充分混合反应生成晶体并稳定成长,还要保证高效快速的固液分离与结晶回收。因此结晶反应和固液分离两大过程是目前MAP结晶反应器设计重点考虑方面。目前MAP结晶反应器主要分为三种:气动搅拌式、流化床式和机械搅拌式三种类型。气动搅拌式属于间歇运行,需要定期停止曝气来收集MAP晶体,因此废水处理能力比较低;流化床式要保持晶体处于流化状态,耗能相当大;而机械搅拌式具有结构简单、操作便捷、处理性能稳定高效等优点,但是机械搅拌式反应器存在紊流状态下结晶反应与层流状态下的固液分离之间的流态调控问题,尤其是当搅拌速度增加时,虽然能够促进混合过程、缩短结晶反应时间、提高废水处理能力,但是反应器内过高的紊流程度不利于MAP晶体成长与固液分离,容易导致晶体流失及二次污染。有文献报道了李秋成等人通过增加贴壁式沉淀器来提高固液分离效果的方法。该方法为减少混合结晶器紊流流态对沉淀区的扰动,贴壁式沉淀器是与混合结晶器下部一映射面为长方形的小口相连,这样虽然在一定程度上提高了固液分离的效果,但是这种设计存在一定的局限性:(1)反应器物料流态不连续、流动路径不流畅,在混合结晶器与沉淀器连接处容易产生壅水现象,导致废水处理能力降低;(2)流态的变化使得MAP晶体易于在连接处析出结垢,从而发生堵塞,对排泥和出水均会产生不利影响;(3)反应器这种组合形式也不利于工程应用。The design of the MAP crystallization reactor is mainly based on two elements: the kinetics of the crystallization reaction and the control of the flow state of the reactor. It is necessary to make the solution fully mix and react to generate crystals and grow stably, and to ensure efficient and rapid solid-liquid separation and crystallization recovery. Therefore, the two major processes of crystallization reaction and solid-liquid separation are the key considerations in the design of the current MAP crystallization reactor. At present, MAP crystallization reactors are mainly divided into three types: pneumatic stirring, fluidized bed and mechanical stirring. Pneumatic stirring type belongs to intermittent operation, and needs to stop aeration regularly to collect MAP crystals, so the wastewater treatment capacity is relatively low; fluidized bed type needs to keep crystals in a fluidized state, and consumes a lot of energy; while mechanical stirring type has simple structure, easy operation It has the advantages of convenience, stable and efficient processing performance, etc., but the mechanically stirred reactor has the problem of fluid regulation between the crystallization reaction under turbulent flow and the solid-liquid separation under laminar flow, especially when the stirring speed increases, although it can promote The mixing process can shorten the crystallization reaction time and improve the wastewater treatment capacity. However, the excessive turbulence in the reactor is not conducive to the growth of MAP crystals and the separation of solid and liquid, and it is easy to cause crystal loss and secondary pollution. Some literatures reported that Li Qiucheng et al. improved the solid-liquid separation effect by adding a wall-mounted precipitator. In this method, in order to reduce the disturbance of the turbulent flow state of the mixed crystallizer to the precipitation zone, the wall-mounted settler is connected to a small port with a rectangular mapping surface at the lower part of the mixed crystallizer, which improves the effect of solid-liquid separation to a certain extent. However, this design has certain limitations: (1) The material flow of the reactor is discontinuous and the flow path is not smooth, and the phenomenon of backwater is likely to occur at the connection between the mixing crystallizer and the settler, resulting in a reduction in the wastewater treatment capacity; (2) ) The change of flow state makes the MAP crystal easy to precipitate and scale at the connection, so as to cause blockage, which will have an adverse effect on both sludge discharge and effluent; (3) The combination of the reactor is also not conducive to engineering applications.

因此,研发出一种实现MAP高效结晶及固液分离的一体化装置及方法,对MAP结晶法的工程应用具有积极的促进作用。本发明得到了国家自然科学基金项目的大力支持。Therefore, an integrated device and method for realizing high-efficiency crystallization and solid-liquid separation of MAP have been developed, which has a positive effect on the engineering application of MAP crystallization method. The invention has been greatly supported by the National Natural Science Foundation of China.

发明内容SUMMARY OF THE INVENTION

本发明设计一种实现MAP高效结晶及固液分离的一体化装置及方法。The present invention designs an integrated device and method for realizing high-efficiency crystallization and solid-liquid separation of MAP.

发明的目的是为了克服目前MAP结晶反应器废水处理能力低、MAP晶体固液分离不彻底、氨磷回收率低等技术难题,设计一种实现磷酸铵镁高效结晶及固液分离的一体化装置及方法,实现MAP结晶技术在氨磷废水处理中的工程应用。The purpose of the invention is to design an integrated device for realizing high-efficiency crystallization of magnesium ammonium phosphate and solid-liquid separation in order to overcome the technical problems such as low wastewater treatment capacity of MAP crystallization reactor, incomplete solid-liquid separation of MAP crystals, and low ammonia phosphorus recovery rate. And the method realizes the engineering application of MAP crystallization technology in ammonia phosphorus wastewater treatment.

本发明的具体技术方案为:The specific technical scheme of the present invention is:

一种实现磷酸铵镁高效结晶及固液分离的一体化装置,其包括混合反应结晶区、固液分离区、缓冲区、MAP污泥区、出水区五部分组成。所述混合反应结晶区与进水泵相连;所述固液分离区设置于内筒与外筒之间;所述缓冲区在混合反应结晶区下部;所述MAP污泥区设置于反应器底部的圆锥体中,且其底部连接大孔径阀门;所述出水区设置在反应器顶部,采取溢流的方式出水。反应器采取进出水同向的折流式连续流处理方式,延长物料在反应器中的流动路径,使结晶反应和固液分离过程更加充分。An integrated device for realizing high-efficiency crystallization and solid-liquid separation of magnesium ammonium phosphate, comprising five parts: a mixed reaction crystallization zone, a solid-liquid separation zone, a buffer zone, a MAP sludge zone, and a water outlet zone. The mixing reaction crystallization zone is connected with the inlet water pump; the solid-liquid separation zone is arranged between the inner cylinder and the outer cylinder; the buffer zone is at the lower part of the mixing reaction crystallization zone; the MAP sludge zone is arranged at the bottom of the reactor. The bottom of the cone is connected with a large-diameter valve; the water outlet area is arranged on the top of the reactor, and the water is discharged by means of overflow. The reactor adopts a baffled continuous flow treatment method with the same direction of inlet and outlet water, which prolongs the flow path of materials in the reactor, and makes the crystallization reaction and solid-liquid separation process more sufficient.

进一步地,反应器为套筒式,内筒为混合反应结晶区。Further, the reactor is a sleeve type, and the inner cylinder is a mixed reaction crystallization zone.

作为优选,所述的混合反应结晶区设置在内筒,采用机械搅拌的方式使结晶更加充分,并在内筒下侧设置环式V型固液两相分离器,它的结构是在圆柱上下面对称贯通切割两个圆台,切面为两个顶点相对的V字型。这样既有利于将晶体和液体进行初步分离,也避免了混合反应区的液体快速直接进入固液分离区,有效避免紊流、短流等不利影响。Preferably, the mixing reaction crystallization zone is set in the inner cylinder, and the crystallization is made more fully by means of mechanical stirring, and a ring-type V-shaped solid-liquid two-phase separator is set on the lower side of the inner cylinder, and its structure is on the cylinder The two circular truncated cones are cut through symmetrically below, and the cut surface is a V shape with two opposite vertices. This not only facilitates the preliminary separation of the crystal and the liquid, but also prevents the liquid in the mixed reaction zone from entering the solid-liquid separation zone quickly and directly, and effectively avoids adverse effects such as turbulent flow and short flow.

作为优选,所述的缓冲区设置在混合反应结晶区与MAP污泥区之间,设置缓冲区一方面可以有效避免混合反应区的水流快速直接进入MAP污泥区,水流扰动过强,使沉下的晶体颗粒重新被水流冲起,导致出水带走大量晶体等不良影响;另一方面晶体也可以在此继续生长,并利用重力作用使之发生沉降。Preferably, the buffer zone is set between the mixed reaction crystallization zone and the MAP sludge zone. On the one hand, setting the buffer zone can effectively prevent the water flow in the mixed reaction zone from entering the MAP sludge zone quickly and directly. The lower crystal particles are washed up again by the water flow, which causes the effluent to take away a large number of crystals and other adverse effects; on the other hand, the crystals can also continue to grow here, and use gravity to cause them to settle.

作为优选,所述的MAP污泥区采用圆锥体是为了收集MAP晶体,使晶体更容易滑落到底部,并在底部设置大孔径阀门,方便定期排出晶体,不易堵塞管道。Preferably, the MAP sludge area adopts a cone to collect MAP crystals, so that the crystals can more easily slide to the bottom, and a large-diameter valve is set at the bottom to facilitate regular discharge of crystals and not easily block the pipeline.

进一步地,所述的固液分离区设置在内筒与外筒之间,将混合反应结晶区与固液分离区分隔开来,避免了快速混合反应区紊流流态对固液分离区的扰动影响。Further, the solid-liquid separation zone is arranged between the inner cylinder and the outer cylinder to separate the mixing reaction crystallization zone and the solid-liquid separation zone, so as to avoid the effect of the turbulent flow state of the rapid mixing reaction zone on the solid-liquid separation zone. disturbance effect.

作为优选,所述的固液分离区利用斜板沉淀水力学原理,在其下部增添斜板。增添斜板后会强化沉淀效果,实现泥水高效分离,提高出水水质,极大降低出水中MAP的含量。Preferably, the solid-liquid separation zone utilizes the principle of sloping plate precipitation hydraulics, and a sloping plate is added to its lower part. The addition of the inclined plate will strengthen the sedimentation effect, realize the efficient separation of mud and water, improve the quality of the effluent, and greatly reduce the content of MAP in the effluent.

作为优选,所述的出水区采用溢流方式进行出水,有利于保持水流的均匀性。Preferably, the water outlet area adopts an overflow mode to discharge water, which is beneficial to maintain the uniformity of the water flow.

本发明反应器混合反应区的圆柱形内筒高径比为1.8~2.5:1,环式V型固液两相分离器位于内筒最下侧,高度占内筒高的1/7~1/5,母线与内筒壁夹角为30°~45°,内筒与外筒横截面积之比为3~4:1,固液分离区的斜板与内筒底部的距离为内筒高度的1/6~1/5,斜板倾斜角度为45°~60°,长度为内筒与外筒间距的0.75~1.5,斜板间距为1.5~2.5cm,出水口与斜板的距离为内筒高度的1/3~1/2。The height-diameter ratio of the cylindrical inner cylinder in the mixing reaction zone of the reactor of the present invention is 1.8-2.5:1, the annular V-shaped solid-liquid two-phase separator is located at the lowermost side of the inner cylinder, and the height accounts for 1/7-1 of the height of the inner cylinder. /5, the angle between the busbar and the inner cylinder wall is 30°~45°, the ratio of the cross-sectional area of the inner cylinder and the outer cylinder is 3~4:1, the distance between the inclined plate of the solid-liquid separation zone and the bottom of the inner cylinder is the inner cylinder 1/6~1/5 of the height, the inclination angle of the inclined plate is 45°~60°, the length is 0.75~1.5 of the distance between the inner cylinder and the outer cylinder, the distance between the inclined plates is 1.5~2.5cm, and the distance between the water outlet and the inclined plate It is 1/3 to 1/2 of the height of the inner cylinder.

本发明运行操作方法:The operating method of the present invention:

a.反应。通过泵抽吸磷、铵废水于内筒,控制起始浓度n(PO4 3-):n(NH4 +)在1~15:1之间,并同时通过泵抽吸镁源及反应所需要的碱液于内筒中,控制n(Mg2+):n(PO4 3-)在1~2.5:1,控制水力停留时间在0.25h~3h,开启搅拌器,转速在100r/min~350r/min,并通过pH计控制反应pH值在8~10,进行结晶反应。a. Reaction. Phosphorus and ammonium waste water is pumped into the inner cylinder by pump, and the initial concentration n(PO 4 3- ): n(NH 4 + ) is controlled between 1 and 15:1, and the magnesium source and the reaction chamber are simultaneously pumped by pump. The required lye is placed in the inner cylinder, control n(Mg 2+ ): n(PO 4 3- ) at 1~2.5:1, control the hydraulic retention time at 0.25h~3h, turn on the agitator, and rotate the speed at 100r/min~ 350r/min, and the pH value of the reaction was controlled at 8-10 by a pH meter, and the crystallization reaction was carried out.

作为优选,水力停留时间在0.5h~1h,这样既可以使废水处理量在一个较大的范围,也可以避免因为流速过高,造成紊流、短流的不利影响。Preferably, the hydraulic retention time is 0.5h to 1h, which can not only make the wastewater treatment amount in a larger range, but also avoid the adverse effects of turbulent flow and short flow due to the high flow rate.

作为优选,转速在250r/min~350r/min,因为高转速能够促进混合过程、缩短结晶反应时间、提高废水处理能力。Preferably, the rotation speed is 250r/min~350r/min, because high rotation speed can promote the mixing process, shorten the crystallization reaction time, and improve the wastewater treatment capacity.

作为优选,pH值控制在9.5(±0.2),这样有利于提高氮磷的回收率。Preferably, the pH value is controlled at 9.5 (±0.2), which is beneficial to improve the recovery rate of nitrogen and phosphorus.

b.沉淀。废水在反应后携带晶体首先进入缓冲区,沉降的晶体会落在MAP污泥区,未沉降的晶体会随着废水进入固液分离区,最后进入出水区,出水中氨氮的回收率达到80%以上,磷的回收率达到95%以上,出水浊度在5NTU以下。沉淀在底部污泥区的MAP晶体定期开启阀门排出。b. Precipitation. After the reaction, the wastewater carries crystals into the buffer zone first, the settled crystals will fall in the MAP sludge zone, and the unsettled crystals will enter the solid-liquid separation zone with the wastewater, and finally enter the effluent zone. The recovery rate of ammonia nitrogen in the effluent reaches 80%. Above, the recovery rate of phosphorus reaches more than 95%, and the turbidity of the effluent is below 5NTU. The MAP crystals deposited in the sludge area at the bottom are discharged by opening the valve regularly.

本发明一种实现MAP高效结晶及固液分离的装置及方法所带来有益的技术效果体现在:The beneficial technical effects brought by a device and method for realizing high-efficiency crystallization and solid-liquid separation of MAP of the present invention are reflected in:

1.本发明反应器装置中,将反应区和沉淀区集中于同一个反应器中,主体为套筒式,内筒为反应区,外筒经沉淀后出水,这种一体式反应器具有结构紧凑,设备简化等优点,利于实际工程应用。1. In the reactor device of the present invention, the reaction zone and the precipitation zone are concentrated in the same reactor, the main body is a sleeve type, the inner cylinder is the reaction zone, and the outer cylinder discharges water after precipitation. This integrated reactor has a structure. The advantages of compactness and simplification of equipment are beneficial to practical engineering applications.

2.本发明反应器装置中,在固液分离区增添斜板的设计,一方面,增加了水流断面的湿周,从而减少了沉淀区的水力半径,减小了雷诺数,提高了水流的稳定性,另一方面,加大固液之间的速度梯度从而实现流动固液之间的分离,当颗粒沉至斜板表面时便被沉淀下来,沉淀下来的晶体颗粒沿斜板表面下滑而自动排出,从而保证出水澄清实现高效固液分离,保证出水水质,减少出水时MAP晶体的流失,从而避免了二次污染与晶体的浪费。当水力停留时间大于0.25h、转速在250r/min~350r/min范围时,本发明反应器出水浊度比对照组出水浊度下降99%以上。2. In the reactor device of the present invention, the design of adding a sloping plate in the solid-liquid separation zone, on the one hand, increases the wet circumference of the water flow section, thereby reducing the hydraulic radius of the precipitation zone, reducing the Reynolds number, and improving the water flow. Stability, on the other hand, increase the velocity gradient between solid and liquid to achieve separation between flowing solid and liquid. When the particles sink to the surface of the inclined plate, they will be precipitated, and the precipitated crystal particles will slide down the surface of the inclined plate. Automatic discharge, so as to ensure the clarification of the effluent to achieve high-efficiency solid-liquid separation, to ensure the quality of the effluent, and to reduce the loss of MAP crystals in the effluent, thereby avoiding secondary pollution and crystal waste. When the hydraulic retention time is greater than 0.25h and the rotation speed is in the range of 250r/min to 350r/min, the turbidity of the effluent of the reactor of the present invention is reduced by more than 99% compared with the turbidity of the effluent of the control group.

3.本发明反应器装置中,在混合反应结晶区下方设置环式V型两相固液分离器,这样既有利于将晶体和液体进行初步分离,也避免了混合反应区的液体快速直接进入固液分离区,有效避免紊流、短流等不利影响。3. In the reactor device of the present invention, a ring-type V-type two-phase solid-liquid separator is arranged below the mixed reaction crystallization zone, which is not only conducive to the preliminary separation of the crystal and the liquid, but also avoids the rapid and direct entry of the liquid in the mixed reaction zone. The solid-liquid separation zone can effectively avoid adverse effects such as turbulent flow and short flow.

4.本发明反应器装置采取进出水同向的折流式连续流处理方式,延长物料在反应器中的流动路径,使结晶反应和固液分离过程更加充分。当氨氮浓度大于200mg/L、无机磷浓度大于400mg/L时,氮磷的回收率可以分别达到80%、95%以上。4. The reactor device of the present invention adopts a baffled continuous flow treatment method with the same direction of inlet and outlet water, which prolongs the flow path of materials in the reactor, and makes the crystallization reaction and solid-liquid separation process more sufficient. When the ammonia nitrogen concentration is greater than 200 mg/L and the inorganic phosphorus concentration is greater than 400 mg/L, the recovery rate of nitrogen and phosphorus can reach 80% and 95%, respectively.

5.本发明反应器装置功能分区明确,有效地调控了混合结晶反应与固液分离过程的流态变化,可以在较高搅拌速度下(250r/min~350r/min)实现快速混合结晶反应过程,从而提高反应器处理能力;同时也避免了水流对固液分离的扰动,提高了出水水质和MAP回收效率。5. The functional division of the reactor device of the present invention is clear, which effectively regulates the fluid state change of the mixed crystallization reaction and the solid-liquid separation process, and can realize the rapid mixed crystallization reaction process at a relatively high stirring speed (250r/min~350r/min). , thereby improving the processing capacity of the reactor; at the same time, it also avoids the disturbance of the water flow to the solid-liquid separation, and improves the effluent quality and MAP recovery efficiency.

附图说明Description of drawings

图1本发明MAP结晶反应器装置结构示意图。图中,1-氮磷废水进水泵;2-镁源进水泵;3-碱液进水泵;4-机械搅拌器;5-pH计;6-内筒壁;7-外筒壁;8-斜板;9-环式V型固液两相分离器;10-出水口;11-圆锥形泥斗;12-MAP晶体排出阀门;I-混合反应结晶区;II-缓冲区;III-MAP污泥区;IV-固液分离区;V-出水区。Fig. 1 is a schematic diagram of the structure of the MAP crystallization reactor device of the present invention. In the figure, 1- nitrogen and phosphorus wastewater feed pump; 2- magnesium source feed pump; 3- lye feed pump; 4- mechanical stirrer; 5- pH meter; 6- inner cylinder wall; 7- outer cylinder wall; 8- Inclined plate; 9-ring V-type solid-liquid two-phase separator; 10-water outlet; 11-conical mud hopper; 12-MAP crystal discharge valve; I-mixed reaction crystallization zone; II-buffer zone; III-MAP Sludge area; IV-solid-liquid separation area; V-outlet area.

图2本发明MAP结晶反应器实现结晶及固液分离示意图;Fig. 2 realizes crystallization and solid-liquid separation schematic diagram of MAP crystallization reactor of the present invention;

图3环式V型固液两相分离器立体图及剖面图;Figure 3 is a perspective view and a cross-sectional view of a ring-type V-shaped solid-liquid two-phase separator;

图4固液分离区斜板装置立体图和俯视图;4 is a perspective view and a top view of the inclined plate device in the solid-liquid separation zone;

图5本发明MAP结晶反应器出水氮磷的回收率;Fig. 5 recovery rate of effluent nitrogen and phosphorus of MAP crystallization reactor of the present invention;

图6本发明MAP结晶反应器与未加斜板的对照组MAP结晶反应器出水浊度对比图。Fig. 6 is a graph comparing the turbidity of the effluent from the MAP crystallization reactor of the present invention and the MAP crystallization reactor of the control group without the inclined plate.

具体实施方式Detailed ways

实施例1Example 1

如附图1所示,本发明MAP结晶反应器装置包括:1-氮磷废水进水泵;2-镁源进水泵;3-碱液进水泵;4-机械搅拌器;5-pH计;6-内筒壁;7-外筒壁;8-斜板;9-环式V型固液两相分离器;10-出水口;11-圆锥形泥斗;12-MAP晶体排出阀门;I-混合反应结晶区;II-缓冲区;III-MAP污泥区;IV-固液分离区;V-出水区。混合反应结晶区(I)与氮磷废水进水泵(1)、镁源进水泵(2)、碱液进水泵(3)相连,并在其内部设有机械搅拌器(4)和pH计(5),缓冲区(II)与混合反应结晶区(I)相连,设置在混合反应结晶区(I)下部,环式V型固液两相分离器(9)与内筒壁(6)相连,处于混合反应结晶区(I)下侧,缓冲区(II)上侧,MAP污泥区(III)与缓冲区(II)相连,设置在主体底部的圆锥体(11)中,且其底部连接大孔径阀门(12);固液分离区(IV)位于内筒壁(6)与外筒壁(7)之间,其下侧放置斜板(8),出水区(V)与固液分离区(IV)相连,设置在主体顶部,采取溢流方式出水。As shown in accompanying drawing 1, the MAP crystallization reactor device of the present invention includes: 1- nitrogen and phosphorus waste water feed pump; 2- magnesium source feed pump; 3- lye feed pump; 4- mechanical stirrer; 5- pH meter; 6- - inner cylinder wall; 7- outer cylinder wall; 8- inclined plate; 9- ring V-type solid-liquid two-phase separator; 10- water outlet; 11- conical mud hopper; 12- MAP crystal discharge valve; I- Mixed reaction crystallization zone; II-buffer zone; III-MAP sludge zone; IV-solid-liquid separation zone; V-water outlet zone. The mixed reaction crystallization zone (1) is connected with the nitrogen and phosphorus waste water feed pump (1), the magnesium source feed pump (2), and the lye feed water pump (3), and is provided with a mechanical stirrer (4) and a pH meter ( 5), the buffer zone (II) is connected with the mixed reaction crystallization zone (I), and is arranged at the bottom of the mixed reaction crystallization zone (I), and the ring-type V-type solid-liquid two-phase separator (9) is connected with the inner cylinder wall (6) , located on the lower side of the mixed reaction crystallization zone (I) and on the upper side of the buffer zone (II), the MAP sludge zone (III) is connected to the buffer zone (II), and is arranged in the cone (11) at the bottom of the main body, and its bottom The large-diameter valve (12) is connected; the solid-liquid separation zone (IV) is located between the inner cylinder wall (6) and the outer cylinder wall (7), and a sloping plate (8) is placed on the underside, and the water outlet zone (V) is separated from the solid-liquid The separation area (IV) is connected and set on the top of the main body, and the water is discharged by means of overflow.

该反应器整体容积为12.4L,内筒高径比为2:1,环式V型固液两相分离器(9)位于内筒最下侧,其高度占内筒高度的1/6,环式V型固液两相分离器(9)上侧母线与内筒壁(6)夹角为45°,外筒与内筒的横截面积比为3.24:1,固液分离区(IV)的斜板(8)倾斜角度为60°,斜板长度与内筒和外筒间距的4/5,板间距1.5cm,出水区(V)与斜板(8)的距离为内筒高度的1/2。The overall volume of the reactor is 12.4L, the height-diameter ratio of the inner cylinder is 2:1, the annular V-shaped solid-liquid two-phase separator (9) is located on the lowermost side of the inner cylinder, and its height accounts for 1/6 of the height of the inner cylinder, The angle between the upper busbar of the ring-type V-shaped solid-liquid two-phase separator (9) and the inner cylinder wall (6) is 45°, the cross-sectional area ratio of the outer cylinder and the inner cylinder is 3.24:1, and the solid-liquid separation zone (IV ) of the inclined plate (8) with an inclination angle of 60°, the length of the inclined plate is 4/5 of the distance between the inner cylinder and the outer cylinder, the plate spacing is 1.5cm, and the distance between the water outlet (V) and the inclined plate (8) is the height of the inner cylinder 1/2 of .

实施例2Example 2

本发明中磷酸铵镁结晶回收氮磷的操作方法:通过泵(1)抽吸n(PO4 3-):n(NH4 +)为1:1的磷、铵混合废水于内筒混合反应结晶区(I),并同时通过泵(2,3)抽吸镁源及反应所需要的碱液于内筒混合反应结晶区(I)中,控制n(Mg2+):n(PO4 3-)在1:1,控制进水流量在24.8L/h,开启搅拌器(4),转速在350r/min,并通过pH计(5)控制反应pH值在9.5(±0.2),进行结晶反应。废水在反应后携带晶体首先进入缓冲区(II),沉降的晶体落在MAP污泥区(III),固定每隔0.5h在MAP污泥区(III)底部的排泥阀(12)排出1L高浓度晶体混合液,未沉降的晶体会随着废水进入固液分离区(IV),最后进入出水区(V)。出水后每隔半个小时测一次出水中磷、铵的浓度和出水浊度,连续运行4个小时。In the present invention, the operation method for recovering nitrogen and phosphorus by crystallization of magnesium ammonium phosphate: sucking the phosphorus and ammonium mixed waste water with n(PO 4 3- ):n(NH 4 + ) of 1:1 through the pump (1) and mixing and reacting in the inner cylinder Crystallization zone (I), and simultaneously through pump (2, 3) suction magnesium source and lye required for reaction in inner cylinder mixing reaction crystallisation zone (I), control n(Mg 2+ ): n(PO 4 3- ) At 1:1, control the influent flow at 24.8L/h, turn on the stirrer (4), rotate the speed at 350r/min, and control the reaction pH at 9.5 (±0.2) by the pH meter (5), carry out Crystallization reaction. After the reaction, the wastewater carries crystals into the buffer zone (II) first, and the settled crystals fall in the MAP sludge zone (III), and the sludge discharge valve (12) at the bottom of the MAP sludge zone (III) is fixed every 0.5h to discharge 1L High-concentration crystal mixed liquid, unsettled crystals will enter the solid-liquid separation zone (IV) along with the wastewater, and finally enter the effluent zone (V). After effluent, the concentration of phosphorus and ammonium in effluent and turbidity of effluent were measured every half an hour, and the operation continued for 4 hours.

作为对照,在相同条件下,反应装置换成在固液分离区没有安装斜板的反应器,出水后每隔半个小时测一次浊度,连续测4个小时。As a control, under the same conditions, the reaction device was replaced with a reactor without a sloping plate in the solid-liquid separation zone, and the turbidity was measured every half an hour after the water was discharged, and the measurement was continued for 4 hours.

本发明MAP结晶反应器装置在此条件下氮磷回收率如图5所示,可以看出,氮的回收率平均在80%以上,磷的回收率在95%以上。浊度对比图如图6所示,可以看出来,本发明装置出水浊度与对照组相比,可以减少平均99%以上,出水浊度平均在5NTU以下。因此,本发明装置可以实现高效结晶及固液分离。The recovery rate of nitrogen and phosphorus in the MAP crystallization reactor device of the present invention is shown in Figure 5. It can be seen that the recovery rate of nitrogen is above 80% on average, and the recovery rate of phosphorus is above 95%. The turbidity comparison chart is shown in Figure 6. It can be seen that the turbidity of the effluent of the device of the present invention can be reduced by an average of more than 99% compared with the control group, and the turbidity of the effluent is below 5 NTU on average. Therefore, the device of the present invention can realize high-efficiency crystallization and solid-liquid separation.

需要说明的是,以上所述的实施例仅用于解释本发明,并不用于限定本发明。凡采取等同替换或等效替换的方式取得的技术方案,均在本发明的保护范围。It should be noted that the above-mentioned embodiments are only used to explain the present invention, and are not used to limit the present invention. All technical solutions obtained by means of equivalent replacement or equivalent replacement are within the protection scope of the present invention.

Claims (5)

1.一种实现磷酸铵镁高效结晶及固液分离的一体化装置,其特征在于,包括混合反应结晶区、缓冲区、MAP污泥区、固液分离区、出水区;主体为套筒式,圆柱形内筒高径比为1.8~2.5:1,内筒与外筒横截面积之比为3~4:1;所述混合反应结晶区在内筒中,与氨磷废水进水泵、镁源进水泵、碱液进水泵相连,并在混合反应结晶区内部设有机械搅拌器和pH计;所述缓冲区与混合反应结晶区相连,设置在混合反应结晶区下部;所述MAP污泥区与缓冲区相连,设置在缓冲区下部;所述固液分离区位于内筒与外筒之间;所述出水区与固液分离区相连,设置在固液分离区上部。1. an integrated device that realizes high-efficiency crystallization of magnesium ammonium phosphate and solid-liquid separation, is characterized in that, comprises mixed reaction crystallization zone, buffer zone, MAP sludge zone, solid-liquid separation zone, water outlet zone; Main body is a sleeve type , the height-diameter ratio of the cylindrical inner cylinder is 1.8 to 2.5:1, and the ratio of the cross-sectional area of the inner cylinder to the outer cylinder is 3 to 4:1; The source inlet water pump and the lye inlet water pump are connected, and a mechanical stirrer and a pH meter are arranged inside the mixed reaction crystallization zone; the buffer zone is connected with the mixed reaction crystallization zone, and is arranged at the lower part of the mixed reaction crystallization zone; the MAP sludge The solid-liquid separation zone is connected with the buffer zone and is arranged at the lower part of the buffer zone; the solid-liquid separation zone is located between the inner cylinder and the outer cylinder; the water outlet zone is connected with the solid-liquid separation zone and is arranged at the upper part of the solid-liquid separation zone. 2.按照权利要求1所述的磷酸铵镁高效结晶及固液分离反应器装置,其特征在于,所述的混合反应结晶区下侧、缓冲区上侧设有环式V型固液两相分离器;环式V型固液两相分离器的结构是在圆柱上下面对称贯通切割两个圆台,切面为两个顶点相对的V字型环式V型固液两相分离器,高度占内筒高的1/7~1/5,母线与内筒壁夹角为30°~45°。2. according to the high-efficiency crystallization of magnesium ammonium phosphate and solid-liquid separation reactor device according to claim 1, it is characterized in that, described mixed reaction crystallization zone lower side, buffer zone upper side are provided with ring type V-type solid-liquid two-phase Separator; The structure of the ring-type V-type solid-liquid two-phase separator is to symmetrically cut two circular tables on the upper and lower sides of the cylinder, and the cut surface is a V-shaped ring-type V-type solid-liquid two-phase separator with two opposite vertices. The height of the inner cylinder is 1/7~1/5, and the angle between the busbar and the inner cylinder wall is 30°~45°. 3.按照权利要求1所述的磷酸铵镁高效结晶及固液分离反应器装置,其特征在于,所述的固液分离区下侧设有斜板;斜板与内筒底部的距离为内筒高度的1/6~1/5,斜板倾斜角度为45°~60°,长度为内筒与外筒间距的0.75~1.5,斜板间距为1.5~2.5cm,出水口与斜板的距离为内筒高度的1/3~1/2。3. according to the high-efficiency crystallization of magnesium ammonium phosphate and solid-liquid separation reactor device according to claim 1, it is characterized in that, described solid-liquid separation zone lower side is provided with inclined plate; 1/6~1/5 of the height of the cylinder, the inclined angle of the inclined plate is 45°~60°, the length is 0.75~1.5 of the distance between the inner cylinder and the outer cylinder, the distance between the inclined plates is 1.5~2.5cm, and the distance between the water outlet and the inclined plate is 1/6~1/5. The distance is 1/3 to 1/2 of the height of the inner cylinder. 4.一种实现磷酸铵镁高效结晶及固液分离的方法,其特征在于,通过泵抽吸磷、铵废水于内筒,控制起始浓度n(PO4 3-):n(NH4 +)在1~15:1之间,并同时通过泵抽吸镁源及反应所需要的碱液于内筒中,控制n(Mg2+):n(PO4 3-)在1~2.5:1,控制水力停留时间为0.25h~3h,开启搅拌器,转速在100r/min~350r/min,并通过pH计控制反应pH值在8~10之间,进行结晶反应;废水在反应后携带晶体首先进入缓冲区,沉降的晶体落在MAP污泥区,并定期开启阀门,排出MAP晶体,未沉降的晶体会随着废水进入固液分离区,最后进入出水区,溢流出水。4. a method for realizing high-efficiency crystallization of magnesium ammonium phosphate and solid-liquid separation, it is characterized in that, by pumping phosphorus, ammonium waste water in inner cylinder, control initial concentration n(PO 4 3- ): n(NH 4 + ) is between 1~15:1, and at the same time, the magnesium source and the lye required for the reaction are pumped into the inner cylinder through the pump, and the n(Mg 2+ ): n(PO 4 3- ) is controlled at 1~2.5: 1 , control the hydraulic retention time to be 0.25h ~ 3h, turn on the stirrer, the rotating speed is 100r/min ~ 350r/min, and control the pH value of the reaction to be between 8 and 10 through the pH meter, and carry out the crystallization reaction; the wastewater carries crystals after the reaction First enter the buffer zone, the settled crystals fall into the MAP sludge zone, and the valve is opened regularly to discharge the MAP crystals. The unsettled crystals will enter the solid-liquid separation zone along with the wastewater, and finally enter the water outlet zone, overflowing the water. 5.根据权利要求4所述的方法,其特征在于,转速能达到250r/min~350r/min。5. The method according to claim 4, wherein the rotational speed can reach 250r/min~350r/min.
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