CN102260002B - Process for treating and recycling rare earth wastewater containing high-concentration sodium chloride and ammonium chloride - Google Patents
Process for treating and recycling rare earth wastewater containing high-concentration sodium chloride and ammonium chloride Download PDFInfo
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- CN102260002B CN102260002B CN 201110207198 CN201110207198A CN102260002B CN 102260002 B CN102260002 B CN 102260002B CN 201110207198 CN201110207198 CN 201110207198 CN 201110207198 A CN201110207198 A CN 201110207198A CN 102260002 B CN102260002 B CN 102260002B
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Abstract
The invention relates to a process for treating and recycling rare earth wastewater containing high-concentration sodium chloride and ammonium chloride. In the process, DEP (dielectrophoresis) is adopted to completely recycle sodium chloride wastewater, so that the sodium chloride wastewater discharged in a rare earth smelting process is completely recycled, and the settlement efficiency and working scope are improved by a DEP settlement process. During DEP microfiltration and DEP nanofiltration, the dielectrophoresis is used to enhance the treatment efficiency of membranes; and compared with the high energy consumption for high-pressure clean water input and the forced stopping of the membrane filtration effect in the traditional frequent backwashing process, the working continuity and efficiency of the membranes and low energy consumption can be guaranteed by DEP microfiltration and DEP nanofiltration. Compared with the energy consumption in industrial wastewater treatment by electrodialysis and reverse osmosis membrane, the energy demand and treatment cost are reduced because the osmotic pressure required for nanofiltration is low; and the high-concentration sodium chloride and ammonium chloride solutions are electrolyzed to generate chlorine, hydrogen and concentrated sodium chloride solution, then the hydrogen and chlorine are input into a hydrogen-chloride fuel cell to release the electric energy part for compensating the electric power consumption in the separation and recycling process, simultaneously diluted hydrochloric acid is generated after the reaction of the fuel cell, and the ammonia water and high-concentration sodium chloride solution produced in the electrolysis process are input into an osmotic pressure electric generating set for generating electricity.
Description
Technical field
The invention belongs to environmental technology field, relate to for rare-earth smelting factory sodium-chlor for leading and containing behavior of high-strength ammonium and the wastewater treatment of emulsification thing and reclaim the active substance recycle, process and reclaim the energy additional or power supply for the energy that produces, especially a kind of waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth utilizes technique.
Background technology
The sodium-chlor that in the sewage that rare-earth smelting factory discharges, contains high density, not only contaminate environment, and waste resource.And also contain ammonium chloride and emulsification thing in the waste water, wherein ammonia nitrogen is the important pollutent of polluted-water, and the ammonia-nitrogen content in the water body exceeds standard and not only destroys ecotope and also can cause great harm to human and vegeto-animal existence and health.And high density like this and the complicated waste water of composition, treatment process now can't reach the standard of discharging, also can't be with resource recycling.
The problem of exist actually is that if only contain the sodium-chlor of high density in the waste water, method commonly used is to obtain the crystal settling of sodium-chlor by evaporative crystallization.This technique can reduce process costs by optimization, but energy consumption is large.And produce desired substance because sodium-chlor is not rare-earth smelting factory, invest huge and the huge multipole evaporation technology and be not suitable for the local principle of processing and reclaiming the use resource of consuming energy.
In addition, contain high strength ammonium-chloride in the ammonium chloride waste-water that rare-earth smelting factory discharges, its concentration is that existing treatment process consists essentially of following several respects more than the desired hundred times of emission standard: 1, biological oxidation process can't concentration for the treatment of be higher than the ammonium chloride waste-water of 0.5g/L; 2, the stripping stripping is sent out needs chemical agent adjustment pH value, and the ammonium salt residue behind the stripping is too high, still has secondary pollution problems; 3, ion exchange method can be used for processing, but needs frequent regeneration, so greatly improved processing cost; 4, many producers also adopt fresh water to rush rare but waste water reaches emission standard, but so not only make environmental pollution, and have wasted in a large number water resources and ammonium salt; 5, distillation also concentrates ammonium salt being used to extract water, but distil process needs a large amount of energy, and the ammonium chloride in the waste water can not be decomposed and recycle in rare-earth smelting technique.The common ground of the above technique is: processing power is low, processing efficiency low (mostly being batch processed), and energy consumption is large, and the resource regeneration rate is extremely low.
In addition, the synthetic effective scheme that pollutes as processing ammonia nitrogen water that also once was suggested of the integrated electrodialysis process of reverse osmosis membrane.Yet the technical process that proposes and patented invention do not take into full account the complicacy of the contained material of ammonia nitrogen waste water.For example, often contain water/oily emulsification and other suspended substances in the ammonium chloride waste-water that behind rare-earth smelting, discharges, and these materials can not only shorten the water treatment efficiency of reverse osmosis membrane and the work-ing life that can reduce permeable membrane.In addition, because exigent permeable membrane pressure in the reverse osmosis membrane technique, this means that also its requirement to water pump in the technique is high and consumes the more energy.Electrodialytic technique needs the very high energy equally.And, still contain other elements in the ammonium chloride concentrated solution after the processing, and be unfavorable for the waste recovery recycling.
By retrieval, not yet find the publication document identical with present patent application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide the waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth good with low cost and good environmental protection of a kind for the treatment of effect to utilize technique.
The present invention realizes that the technical scheme of purpose is as follows:
A kind of waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth utilizes technique, and step is as follows:
(1) the waste water suspension liquid after natural subsidence is processed is input in the DEP micro-filtration, it is 1 to 2bar that work is pressed, isolate solid particulate contained in the suspension liquid, this concentrated solution re-circulates in the sedimentation, and the liquid without the outstanding absurd creature of solid that obtains inputs in the DEP nanofiltration group;
(2) through behind the settling circulation repeatedly, contained emulsification thing will be input to DEP-DEEP-BED micro-filtration art breading in the solid particulate, and the emulsification thing is separated from suspension liquid, and the water purification after the processing inputs in the DEP nanofiltration group;
(3) in DEP nanofiltration group, the sodium chloride and the ammonium chloride that hang the liquid of absurd creature without solid are concentrated, contained ammonium radical ion in the waste water is shifted out, the liquid of removing the ammonium radical ion can be used for process water, sodium chloride and ammonium chloride concentrated solution will be input to electrolyzer, and the required pressure drop of nanofiltration work is 5 to 6bar;
(4) in electrolyzer, sodium chloride and ammonium chloride concentrated solution are by electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm
2, the high dense saline solution that electrolysis produces is input to the osmotic pressure power station and is used for generating electricity, and the chlorine that produces and hydrogen input fuel cell are used for generating;
(5) chlorine of electrolysis generation and hydrogen are inputing to hydrogen chlorine fuel cell through after the drying treatment, and the direct current that fuel cell produces is connected to the grid through overcommutation electric energy supplement is provided, and the hydrogenchloride that fuel cell reaction generates is used for rare-earth smelting.
And the operating voltage of described DEP micro-filtration and nanofiltration exchanges 200V, 100kHz.
Advantage of the present invention and positively effect are:
1, the present invention adopts DEP to carry out the fully recycling of sodium chloride waste water, and the sodium chloride waste water of rare-earth smelting technique discharging will be recycled fully, realizes zero release, low cost, less energy-consumption.The DEP sedimentation process has improved efficient and the working range of sedimentation.In DEP micro-filtration and DEP nanofiltration, dielectrophoresis all is used for the processing efficiency of reinforced film, need the high energy consumption of high input voltage clear water and be forced to the stopper film filteration to compare with traditional frequent back flushing, the continuity of DEP micro-filtration and the work of DEP nanofiltration permission film and high efficiency and energy consumption are low.The emulsification thing is raised in its concentration can be by DEP-DEEP-BED micro-filtration technique and rich long-pending and reclaim and be used for rare-earth smelting technique, adopts nanofiltration membrane will wherein sodium ion, ammonium ion and chlorion selectivity to separate from waste water and rich long-pending to reach selective separation sodium-chlor and ammonium chloride waste-water.Compare with reverse osmosis membrane and electrodialysis process trade effluent energy consumption, owing to the demand that reduced the energy and the cost of processing are forced down in the required infiltration of nanofiltration membrane, electrolysis high density chlorination sodium and ammonium chloride solution produce chlorine, hydrogen and ammoniacal liquor and sodium-chlor concentrated solution, hydrogen and chlorine are imported in the hydrogen-chlorine fuel cell to discharge the power consumption of the whole process for separating and recovering of electric energy partial-compensation, simultaneously after the reaction of fuel cell, produce dilute hydrochloric acid, and the ammoniacal liquor that in electrolysis process, produces and the generating of sodium-chlor highly concentrated solution input osmotic pressure generating set.
2, the present invention can process high density chlorination sodium and ammonium chloride waste-water continuously, improve efficient that permeable membrane processes and prolong permeable membrane duration of service to reduce cost and to improve processing efficiency, reasonably optimizing uses permeable membrane to reduce energy consumption, selectivity is rich long-pending and separate effective constituent in the waste water, according to industrial specific requirement, effective constituent is made required chemical substance in the applicable waste water, the gas fuel made battery that utilizes technical process to produce replenishes as electric energy for technique, the medelling continuous processing can be optimized the composition technical process from ammonium chloride and different industry to the requirement of recycling composition according to different content sodium-chlor, and concentrated high density saline solution is used for the osmotic pressure generating after processing.
Description of drawings
Fig. 1 is DEP processor structure schematic diagram involved in the present invention;
Fig. 2 is that the present invention contains high density chlorination sodium and ammonium chloride rare earth wastewater is processed the recycling artwork.
Embodiment
The invention will be further described to specific embodiment below by accompanying drawing, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
A kind of waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth utilizes technique, and concrete steps and working conditions are as follows:
(1) the waste water suspension liquid after natural subsidence is processed is input in the DEP micro-filtration, it is 1 to 2bar that work is pressed, to isolate solid particulate contained in the suspension liquid, concentrated solution re-circulates in the sedimentation, and resulting liquid without the outstanding absurd creature of solid inputs in the DEP nanofiltration group after processing;
(2) through behind the settling circulation repeatedly, contained emulsification thing will be input to DEP-DEEP-BED micro-filtration art breading in the solid particulate, and the emulsification thing is separated from suspension liquid.The principle of work of DEP-DEEP-BED micro-filtration technique is similar to the DEP micro-filtration to structure, and working conditions is identical with the DEP micro-filtration, and the water purification after the processing inputs in the DEP nanofiltration group;
(3) in DEP nanofiltration group, the sodium chloride and the ammonium chloride that hang the liquid of absurd creature without solid will be concentrated, thereby contained ammonium radical ion in the waste water is shifted out, the liquid of removing the ammonium radical ion can be used for process water, and sodium chloride and ammonium chloride concentrated solution will be input to electrolyzer, and the required pressure drop of nanofiltration work is 5 to 6bar;
(4) in electrolyzer, sodium chloride and ammonium chloride concentrated solution are by electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm2.The high dense saline solution that electrolysis produces can be input to the osmotic pressure power station and be used for generating electricity, and the chlorine that produces and hydrogen can be inputted fuel cell for generating, and is different with the electrolysis treatment amount from ammonium chloride concentration according to different sodium chlorides, and parameter also changes to some extent;
(5) chlorine of electrolysis generation and hydrogen are inputing to hydrogen chlorine fuel cell through after the drying treatment, and the direct current that fuel cell produces can be connected to the grid through overcommutation electric energy supplement is provided, and the hydrogenchloride that fuel cell reaction generates can be used for rare-earth smelting.
All techniques, are worked under the normal pressure all at normal temperature without specified otherwise, there is no specific other working conditions requirement.Dielectrophoresis (DEP) operating voltage exchanges 200V 100kHz.
Principle of work of the present invention is:
At first sedimentation separates greater than 10 microns solia particles diameter ammonium chloride waste-water from waste water through DEP.This sedimentation process by the dielectrophoresis technology to strengthen its settling efficiency and sedimentation process range (namely increase can process particle size scope to 10 micron).Referring to Fig. 1, the dielectrophoresis force that the asymmetric electric field by electrode 1 produces has strengthened the kinetic energy that particulate moves downward, with efficient and the working range that has improved sedimentation.
The waste water of processing through sedimentation is imported into the technical process of DEP micro-filtration to remove all solids suspended substance in the waste water.In this link, the film that causes on the film stops up and the problem of filtration treatment amount decline because solid and liquid particle are attached to reduce permeable membrane 2 in the use of dielectrophoresis force.Especially the emulsification thing that uses in rare-earth smelting technique, still part is present in the waste water.Because filter the high pressure that applies, the kerosene oil droplet in these emulsifications is very easy to block the permeable membrane fenestra and causes the film latch up phenomenon that can't reverse.So, descend to the work-ing life of permeable membrane, and filtration area reduces, and treatment capacity is corresponding decline also, thereby cause the greatly raising of processing cost.Because the negative dielectrophoresis character that in water, shows of kerosene oil droplet, and by dielectrophoresis force to the direction motion of permeable membrane surface opposite, and postpone water (flow) direction and discharge membrane module, so solved the problems referred to above that the emulsification thing causes.Filter the waste water without suspended solid that produces and to be pumped to next processing links, and concentrated solution will be recycled and can DEP sedimentation link further process.Because emulsification thing contained concentration in raw wastewater is lower, after processing through certain continuous circulation, its concentration will be raised to can be by DEP-DEEP-BED micro-filtration technique and rich long-pending and reclaim and be used for rare-earth smelting technique.And will together pump into next processing links through what DEP-DEEP-BED micro-filtration art breading was crossed with the same waste water that produces in the DEP micro-filtration technique without the waste water of suspended solid: multiple DEP nanofiltration technique.
Because sodium-chlor and ammonium chloride content contained in the raw wastewater are high, so adopt multiple DEP nanofiltration technique so that the waste water height is concentrated up to standard in order to recycle in the rare-earth smelting technique with the salt concn in the waste water simultaneously.Adopt nanofiltration membrane to reach the purpose of selective separation here.Because the fenestra of nanofiltration membrane only allows monovalent ion to pass through, so can be with the sodium ion in the waste water, ammonium ion separates from waste water with the chlorion selectivity and is rich long-pending.In addition, with the required energy of reverse osmosis membrane and electrodialysis process trade effluent relatively, owing to the demand that reduced the energy and the cost of processing are forced down in the required infiltration of nanofiltration membrane.In the nanofiltration membrane separation technique of routine, the crystallization that produces owing to the concentration difference of nanofiltration membrane both sides and fouling meeting are with the Pore Blocking of nanofiltration membrane, so, dielectrophoresis force is used to remove and may be attached on the film or the crystal fine particle in the fenestra even, to guarantee real work area and the processing efficiency of nanofiltration membrane.In DEP micro-filtration and DEP nanofiltration, dielectrophoresis all is used for the processing efficiency of reinforced film.Need the high energy consumption of high input voltage clear water and be forced to the stopper film filteration to compare with traditional frequent back flushing, the continuity of DEP micro-filtration and the work of DEP nanofiltration permission film and high efficiency and energy consumption are low.
The high density chlorination sodium and the ammonium chloride solution that produce behind above-mentioned waste water treatment process will be imported into electrolyzer.In electrolyzer, because the electrochemical anode that acts on produces chlorine, and produce the gas mixture of ammonia and hydrogen at negative electrode.Owing to ammonia can be rapidly in water with water in the hydroxide ion reaction forms ammoniacal liquor, so the electrolytic chlorination ammonium will produce three kinds of products: hydrogen, ammoniacal liquor, and chlorine reaches the sodium chloride solution that concentrates.Hydrogen and chlorine are imported in the hydrogen-chlorine fuel cell to discharge the power consumption of the whole process for separating and recovering of electric energy partial-compensation, produce dilute hydrochloric acid simultaneously after the reaction of fuel cell.The high strong solution of remaining ammoniacal liquor and sodium-chlor will be imported into the osmotic pressure power station and be used for generating.
So, all will be recycled fully from the ammonium chloride waste-water of rare-earth smelting technique discharging, realize zero release, low cost, less energy-consumption.
The following describes and relate to micro-filtration of the present invention and nanofiltration.
Micro-filtration is used for liquid-solid separation, and the particulate in the suspension liquid is shifted out to obtain liquid without the suspension solid phase.In conventional micro-filtration, owing to the high osmotic pressure that is used in the micro-filtration, particulate will be easy to be attached on the permeable membrane or be trapped in the infiltration fenestra, thereby cause water purification to produce production declining, and separation efficiency reduces, the results such as the working life minimizing of permeable membrane.Therefore, the method that shifts out with the particulate that will be attached on the permeable membrane with the high-frequency and high-voltage back flushing of conventional micro-filtration technique prolongs the work-ing life of permeable membrane.Yet when using back flushing, micro-filtration technique must stop, so, although back flushing can in the working hour of improving to a certain degree permeable membrane, also can't keep the production output of separation efficiency and water purification.In addition, the required high-pressure pump of back flushing expends very large electric weight, thereby has improved the running cost of micro-filtration technique.
Similarly, in the nanofiltration technique, because the concentration difference at the permeable membrane two ends, thereby cause the moment concentration of the institute's saliferous in the liquid of processing to improve, because under certain envrionment conditions, the solubleness of this salt in water is certain, so the xln of this salt will separate out and can be attached on the permeable membrane or be trapped in the infiltration fenestra.Along with the input of more saline solution, so thereby this salt gets xln can progressively grow up Pore Blocking.Thereby the working area that has so not only reduced nanofiltration membrane reduces separation efficiency, the decline of turnout, and as do not process and will and can't work whole nanofiltration technique stagnation.Same back-flushing method often is used to wash fenestra.Its drawback is as implied above.In addition; the industrial adding chemical agent that also often adopts shifts out relevant salt to reduce the generation of this situation; yet so processing has not only improved the running cost of nanofiltration; and the medicament that adds will need other technique to cooperate and often can produce infringement to nanofiltration membrane, and the pollution that may cause environment.
DEP micro-filtration involved in the present invention and nanofiltration are to use the dielectrophoresis force that acts on the particulate that thereby particulate or salt crystal are being reached without the generation of blocking up the film phenomenon near moving apart permeable membrane before the permeable membrane.Its structure is that interdigital electrode is installed in permeable membrane below, because the effect of the negative dielectrophoresis force that particulate is subject to pushed away from electrode surface, thereby and is taken away the effect that particulate can't close permeable membrane that reaches by current.So structure can guarantee micro-filtration and nanofiltration continuous firing, occurs without stifled film phenomenon, improves working efficiency and the work-ing life of permeable membrane.
Claims (2)
1. a waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth utilizes technique, and it is characterized in that: step is as follows:
(1) the waste water suspension liquid after natural subsidence is processed is input in the DEP micro-filtration, it is 1 to 2bar that work is pressed, isolate solid particulate contained in the suspension liquid, this concentrated solution re-circulates in the sedimentation, and the liquid without the outstanding absurd creature of solid that obtains inputs in the DEP nanofiltration group;
(2) through behind the settling circulation repeatedly, contained emulsification thing will be input to DEP-DEEP-BED micro-filtration art breading in the solid particulate, and the emulsification thing is separated from suspension liquid, and the water purification after the processing inputs in the DEP nanofiltration group;
(3) in DEP nanofiltration group, the sodium chloride and the ammonium chloride that hang the liquid of absurd creature without solid are concentrated, contained ammonium radical ion in the waste water is shifted out, the liquid of removing the ammonium radical ion can be used for process water, sodium chloride and ammonium chloride concentrated solution will be input to electrolyzer, and the required pressure drop of nanofiltration work is 5 to 6bar;
(4) in electrolyzer, sodium chloride and ammonium chloride concentrated solution are by electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm
2, the high dense saline solution that electrolysis produces is input to the osmotic pressure power station and is used for generating electricity, and the chlorine that produces and hydrogen input fuel cell are used for generating;
(5) chlorine of electrolysis generation and hydrogen are inputing to hydrogen chlorine fuel cell through after the drying treatment, and the direct current that fuel cell produces is connected to the grid through overcommutation electric energy supplement is provided, and the hydrogenchloride that fuel cell reaction generates is used for rare-earth smelting.
2. the waste water treatment and reclamation that contains high density chlorination sodium and ammonium chloride rare earth according to claim 1 utilizes technique, it is characterized in that: the operating voltage of described DEP micro-filtration and nanofiltration exchanges 200V, 100kHz.
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| CN103463985B (en) * | 2013-09-10 | 2015-07-01 | 内蒙古天一环境技术有限公司 | Osmosis membrane assembly for dielectrophoresis forward-osmosis flat plate |
| CN103463987B (en) * | 2013-09-10 | 2015-07-01 | 内蒙古天一环境技术有限公司 | Method for strengthening filter capacity of osmotic membrane through dielectrophoresis technology |
| CN104071941B (en) * | 2014-06-24 | 2016-03-02 | 燕山大学 | In a kind of recovering rare earth ammonium salt waste water, ammonium chloride prepares the method for agrochemical |
| CN115259119B (en) * | 2022-07-06 | 2024-02-27 | 北京水木方科技有限公司 | Method for continuously preparing battery-grade ferric phosphate by using ferrous chloride |
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| CN101088935A (en) * | 2007-06-26 | 2007-12-19 | 张凌云 | RE waste water treating complete circulation process |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
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| CN101088935A (en) * | 2007-06-26 | 2007-12-19 | 张凌云 | RE waste water treating complete circulation process |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
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