CN102260000B - Process for treating and recycling ammonium chloride rare earth wastewater - Google Patents
Process for treating and recycling ammonium chloride rare earth wastewater Download PDFInfo
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- CN102260000B CN102260000B CN 201110207191 CN201110207191A CN102260000B CN 102260000 B CN102260000 B CN 102260000B CN 201110207191 CN201110207191 CN 201110207191 CN 201110207191 A CN201110207191 A CN 201110207191A CN 102260000 B CN102260000 B CN 102260000B
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Abstract
The invention relates to a process for treating and recycling ammonium chloride rare earth wastewater. The ammonium chloride wastewater is completely recycled by diethyl phthalate (DEP), so that the ammonium chloride wastewater discharged in a rare earth smelting process can be completely recycled; dielectrophoresis is used for reinforcing the treatment efficiency of a membrane in DEP microfiltration and DEP nanofiltration, and compared with the conventional process in which high energy consumption is caused because clear water is needed to be introduced under high pressure for frequent backwashing and membrane filtration is forced to be stopped, the process has the advantages that: the work continuity and high efficiency of the membrane are achieved and energy consumption is low in the DEP microfiltration and the DEP nanofiltration; a nanofiltration membrane is adopted, so that ammonium ions and chlorine ions in ammonium chloride are selectively separated from the wastewater and enriched; compared with a process for treating industrial wastewater through a reverse osmosis membrane and electrodialysis, the process has the advantage that: osmotic pressure required by the nanofiltration membrane is low, so that the energy requirement and treating cost are reduced; chlorine, hydrogen and ammonia water are generated by electrolyzing high-concentration ammonium chloride solution, and the hydrogen and the chlorine are introduced into a hydrogen chlorine fuel cell to release electric energy so as to partially compensate electricity consumption in the whole separation and recoveryprocess; meanwhile, dilute hydrochloric acid is generated after reaction in the fuel cell is finished, and is recycled together with the ammonia water generated in the electrolysis process.
Description
Technical field
The invention belongs to environmental technology field, relate to rare-earth smelting factory ammonium chloride and be master's wastewater treatment and reclaim the active substance recycle, especially a kind of ammonium chloride RE waste water is handled and is recycled technology.
Background technology
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, also can cause great harm to human and vegeto-animal existence and health.The ammonium chloride that contains high density in the ammonium chloride waste-water that rare-earth smelting factory is discharged, its concentration are more than several thousand times of emission standard requirement.Though can adopt several different methods handles; But the biological oxidation process that adopts at present usually can't concentration of treatment be higher than the ammonium chloride waste-water of 0.5g/L; And the stripping stripping is sent out and is needed chemical agent to adjust pH value, and the ammonium salt residue behind the stripping is too high, still has secondary pollution problems.Ion exchange method can be used for handling, but needs frequent regeneration, so improved processing cost greatly.Many producers adopt fresh water towards rare but waste water reaches emission standard, but so not only make environmental pollution, and have wasted water resources and ammonium salt in a large number.Distillation also is being used the concentrated ammonium salt to extract water, but distil process needs lot of energy, and can not and recycle in rare-earth smelting technology the decomposition of the ammonium chloride in the waste water.The common ground of the above technology is: processing power is low, processing efficiency low (being mostly batch processed), and energy consumption is big, and the resource regeneration rate is extremely low.
In addition, the synthetic of the integrated electrodialysis process of reverse osmosis membrane also once was suggested as handling the effective scheme that ammonia nitrogen water pollutes.Yet technical process that is proposed 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 film pressure in the reverse osmosis membrane technology; This means that also its requirement to water pump in the technology is high and consume the more energy, and electrodialytic technique needs the very high energy equally, and; Still contain other elements in the ammonium chloride liquid concentrator after the processing, and be unfavorable for that waste recovery utilizes again.
Through retrieval, do not find the publication document identical as yet with present patent application.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, provide the ammonium chloride RE waste water of the good with low cost and good environmental protection of a kind of treatment effect to handle and recycle technology.
The present invention realizes that the technical scheme of purpose is following:
A kind of ammonium chloride RE waste water is handled and is recycled technology, and it is characterized in that: step is following:
⑴ the suspension liquid after sedimentation is handled is input in the DEP micro-filtration, and it is 1 to 2bar that work is pressed, the solid particulate that shifts out in the suspension liquid to be contained, and liquid concentrator re-circulates in the sedimentation, and the liquid of the outstanding absurd creature of the no solid after the processing inputs in the DEP nanofiltration group;
⑵ be input to DEP-DEEP-BED micro-filtration art breading through the spissated kerosene emulsification that contains solid particulate after repeatedly circulating and the kerosene emulsification separated from suspension liquid, and the water purification after the processing inputs in the DEP nanofiltration group;
⑶ in DEP nanofiltration group; The ammonium chloride of the liquid of the outstanding absurd creature of no solid is concentrated, thereby contained ammonium radical ion in the waste water is shifted out, and the liquid of removing the ammonium radical ion is used for process water; The ammonium chloride liquid concentrator will be input to electrolyzer, and the required pressure of nanofiltration work is 5 to 6bar;
⑷ in electrolyzer, and the ammonium chloride liquid concentrator is through electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm
2, the ammoniacal liquor that electrolysis produces is that rare-earth smelting uses, the chlorine of generation and hydrogen input fuel cell are used for generating;
⑸ chlorine that electrolysis produces 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 WV of said 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 recycling fully of ammonium chloride waste-water, and the ammonium chloride waste-water of rare-earth smelting technology discharging will be recycled fully, realizes zero release, low cost, less energy-consumption.The DEP sedimentation process has improved settled efficient and working range.In DEP micro-filtration and DEP nanofiltration, dielectrophoresis all is used for the processing efficiency of reinforced film.Need the high energy consumption and the compelled stopper film filteration of high pressure input clear water 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 kerosene emulsification is enhanced can be through DEP-DEEP-BED micro-filtration technology rich long-pending and reclaim and be used for rare-earth smelting technology in its concentration.Adopt nf membrane ammonium ion in the ammonium chloride and cl ions selectivity to be separated from waste water and rich amassing to reach the selective separation ammonium chloride waste-water.Compare with reverse osmosis membrane and electrodialysis process trade effluent energy consumption, owing to the cost that has reduced demands for energy and processing is forced down in the required infiltration of nf membrane.Electrolysis high strength ammonium-chloride solution produces chlorine, hydrogen and ammoniacal liquor; Hydrogen and chlorine are imported in the hydrogen-chlorine fuel cell to discharge the power consumption that electric energy partly compensates whole process for separating and recovering; Simultaneously after the reaction of fuel cell, produce Hydrogen chloride, its with electrolysis process in the ammoniacal liquor that produces is same is recovered utilization.
2, the present invention can adopt continuous processing treatment of high concentration ammonium chloride waste-water; Can effectively improve efficient that permeable membrane handles and prolong permeable membrane duration of service to reduce cost and to improve processing efficiency; Reasonably optimizing uses permeable membrane to reduce energy consumption; The selectivity richness is long-pending and separate effective constituent in the waste water, and according to industrial specific requirement, effective constituent is processed required chemical substance in the suitable waste water; The gas that utilizes technical process to produce is processed fuel cell and is replenished as electric energy for technology, and the medelling continuous processing can be optimized the composition technical process to the requirement of recycling composition according to different content ammonium chloride and different industry.
Description of drawings
Fig. 1 is a DEP processor structure synoptic diagram involved in the present invention;
Fig. 2 recycles artwork for ammonium chloride waste-water of the present invention.
Embodiment
Through accompanying drawing specific embodiment is made further detailed description to the present invention below, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
A kind of ammonium chloride RE waste water is handled and is recycled technology, and concrete steps and working conditions are following:
⑴ the suspension liquid after sedimentation is handled is input in the DEP micro-filtration, and it is 1 to 2bar that work is pressed, the solid particulate that is contained to shift out in the suspension liquid, and liquid concentrator re-circulates in the sedimentation, and the liquid of the outstanding absurd creature of the no solid after handling inputs in the DEP nanofiltration group;
⑵ will be input to DEP-DEEP-BED micro-filtration art breading through the spissated kerosene emulsification that contains solid particulate after repeatedly circulating and the kerosene emulsification will be separated from suspension liquid.The principle of work of DEP-DEEP-BED micro-filtration technology is similar with the DEP micro-filtration with structure, and working conditions is identical with the DEP micro-filtration, and the water purification after the processing inputs in the DEP nanofiltration group;
⑶ in DEP nanofiltration group; The ammonium chloride of the liquid of the outstanding absurd creature of no solid will be concentrated, thereby contained ammonium radical ion in the waste water is shifted out, and the liquid of removing the ammonium radical ion can be used for process water; And the ammonium chloride liquid concentrator will be input to electrolyzer, and the required pressure of nanofiltration work is 5 to 6bar;
⑷ in electrolyzer, and the ammonium chloride liquid concentrator is through electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm2.The ammoniacal liquor that electrolysis produces can be rare-earth smelting and uses, and the chlorine that produces can be imported fuel cell with hydrogen and is used for generating electricity; Different with the electrolysis treatment amount according to different ammonium chloride concentrations, parameter also changes to some extent.
⑸ chlorine that electrolysis produces 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 technologies do not have specified otherwise all at normal temperature, and normal pressure is work down, does not have other specific working conditions requirement.Dielectrophoresis (DEP) WV 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 through the dielectrophoresis technology to strengthen its settling efficiency and sedimentation process range (promptly increase can handle particle size scope to 10 micron).Participate in Fig. 1, the dielectrophoresis force that the asymmetric electric field through electrode 1 produces has strengthened the kinetic energy that particulate moves downward, to have improved settled efficient and working range.
The waste water of handling 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 use of dielectrophoresis force to reduce permeable membrane 2 because solid and the problem of liquid particle attached to film obstruction that causes on the film and the decline of filtration treatment amount.Especially the kerosene emulsification that in rare-earth smelting technology, uses, still part is present in the waste water.Because filter the high pressure that is applied, 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 the work-ing life of permeable membrane, filtration area reduces, the also corresponding decline of treatment capacity, thus cause the raising greatly of processing cost.Because the negative dielectrophoresis character that in water, shown 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 kerosene emulsification is caused.The waste water that filters the no suspended solid that produces will be pumped to next processing links, and liquid concentrator will be recycled and can DEP sedimentation link further handle.Because kerosene emulsification contained concentration in raw wastewater is lower, through after certain continuous circular treatment, its concentration will be enhanced can be through DEP-DEEP-BED micro-filtration technology rich long-pending and reclaim and be used for rare-earth smelting technology.And the waste water of the no suspended solid of crossing through DEP-DEEP-BED micro-filtration art breading will together pump into next processing links with the same waste water that produces in the DEP micro-filtration technology: multiple DEP nanofiltration technique.
Because contained ammonium chloride exceeds several thousand times (about 4000) than value up to standard in the raw wastewater, so adopt multiple DEP nanofiltration technique so that the ammonium chloride solution height concentrates simultaneously that the ammonium chloride concentration in the waste water is up to standard so that recycle in the rare-earth smelting technology.Adopt nf membrane to reach the purpose of selective separation here.Because the fenestra of nf membrane only allows monovalent ion to pass through, so can ammonium ion in the ammonium chloride and cl ions selectivity be separated from waste water and rich amassing.In addition, compare with the reverse osmosis membrane and the required energy of electrodialysis process trade effluent, owing to the cost that has reduced demands for energy and processing is forced down in the required infiltration of nf membrane.In the nanofiltration membrane separation technology of routine; The fenestra of nf membrane is stopped up in crystallization that produces owing to the concentration difference of nf membrane both sides and fouling meeting; So; Dielectrophoresis force is used that remove may be attached to the crystal fine particle in the fenestra on the film or even, to guarantee the real work area and the processing efficiency of nf membrane.In DEP micro-filtration and DEP nanofiltration, dielectrophoresis all is used for the processing efficiency of reinforced film.Need the high energy consumption and the compelled stopper film filteration of high pressure input clear water 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 strength ammonium-chloride solution that behind above-mentioned waste water treatment process, is produced will be imported into electrolyzer.In electrolyzer,, and produce the gas mixture of ammonia and hydrogen at negative electrode because the electrochemical anode that acts on produces chlorine.The hydroxide ion reaction of in water, understanding in rapid and the water owing to ammonia forms ammoniacal liquor, so the electrolytic chlorination ammonium will produce three kinds of products: hydrogen, ammoniacal liquor, and chlorine.Hydrogen and chlorine are imported in the hydrogen-chlorine fuel cell to discharge the power consumption that electric energy partly compensates whole process for separating and recovering; Simultaneously after the reaction of fuel cell, produce Hydrogen chloride, the ammoniacal liquor that produces in itself and the electrolysis process is both the indispensable raw material of rare-earth smelting technology.
So, all will be recycled from the ammonium chloride waste-water of rare-earth smelting technology discharging fully, realize zero release, low cost, less energy-consumption.
Explain below 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 the liquid of no suspension solid phase.In conventional micro-filtration, owing to be used in the high osmotic pressure in the micro-filtration, particulate will be easy to permeate in the fenestra attached to perhaps being trapped on the permeable membrane, thereby cause water purification production output to descend, and separation efficiency reduces, results such as the working life minimizing of permeable membrane.Therefore, conventional micro-filtration technology is used the work-ing life of high-frequency and high-voltage back flushing the prolongation with the method that will shift out attached to the particulate on permeable membrane permeable membrane.Yet when using back flushing, micro-filtration technology must stop, so, although back flushing can also can't keep separation efficiency and water purifying production output in the working hour of improving permeable membrane to a certain degree.In addition, the required HPP of back flushing expends very big electric weight, thereby has improved the running cost of micro-filtration technology.
Similarly; In the nanofiltration technique; Since the concentration difference at the permeable membrane two ends, thus the institute's saliniferous moment concentration raising in the liquid of handling caused, because under certain envrionment conditions; The solubleness of this salt in water is certain, thus the xln of this salt will be separated out and can attached on the permeable membrane or be trapped in the infiltration fenestra in.Along with the input of more saline solution, so thereby this salt gets xln can progressively grow up fenestra is stopped up.Thereby the working area that has so not only reduced nf membrane reduces separation efficiency, the decline of turnout, and as do not handle and will and can't work whole nanofiltration technique stagnation.Same back-flushing method often is used and washes fenestra.Its drawback is as implied above.In addition; Also often adopt the adding chemical agent to shift out relevant salt in the industry 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 technology to cooperate and generation damages to nf membrane through regular meeting, and the pollution that possibly cause environment.
Thereby DEP micro-filtration involved in the present invention and nanofiltration are to use the dielectrophoresis force that acts on the particulate to make particulate or salt crystal reached the generation that nothing is blocked 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 receives and pushed away electrode surface, thereby and by current take away reach particulate can't be near the effect of permeable membrane.So structure can guarantee micro-filtration and nanofiltration continuous firing, does not have stifled film phenomenon and takes place, and improves the working efficiency and the work-ing life of permeable membrane.
Claims (2)
1. an ammonium chloride RE waste water is handled and is recycled technology, and it is characterized in that: step is following:
⑴ the suspension liquid after sedimentation is handled is input in the DEP micro-filtration, and it is 1 to 2bar that work is pressed, the solid particulate that shifts out in the suspension liquid to be contained, and liquid concentrator re-circulates in the sedimentation, and the liquid of the outstanding absurd creature of the no solid after the processing inputs in the DEP nanofiltration group;
⑵ be input to DEP-DEEP-BED micro-filtration art breading through the spissated kerosene emulsification that contains solid particulate after repeatedly circulating and the kerosene emulsification separated from suspension liquid, and the water purification after the processing inputs in the DEP nanofiltration group;
⑶ in DEP nanofiltration group; The ammonium chloride of the liquid of the outstanding absurd creature of no solid is concentrated, thereby contained ammonium radical ion in the waste water is shifted out, and the liquid of removing the ammonium radical ion is used for process water; The ammonium chloride liquid concentrator will be input to electrolyzer, and the required pressure of nanofiltration work is 5 to 6bar;
⑷ in electrolyzer, and the ammonium chloride liquid concentrator is through electrochemical reaction and by electrolysis, its electrolysis voltage is 2 to 3V, and electrolytic current density is 0.3-1A/cm
2, the ammoniacal liquor that electrolysis produces is that rare-earth smelting uses, the chlorine of generation and hydrogen input fuel cell are used for generating;
⑸ chlorine that electrolysis produces 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. ammonium chloride RE waste water according to claim 1 is handled and recycled technology, it is characterized in that: the WV of said DEP micro-filtration and nanofiltration exchanges 200V, 100kHz.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108706687A (en) * | 2018-05-30 | 2018-10-26 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of enzymatic amoxicillin production waste water reclaiming recovery process |
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| CN103463986B (en) * | 2013-09-10 | 2015-08-19 | 内蒙古天一环境技术有限公司 | The dull and stereotyped permeable membrane device of a kind of dielectrophoresis |
| 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 |
| CN103463984B (en) * | 2013-09-10 | 2015-05-13 | 内蒙古天一环境技术有限公司 | Dielectrophoresis hollow fiber membrane assembly |
| CN103480277B (en) * | 2013-10-09 | 2015-07-01 | 内蒙古天一环境技术有限公司 | Dielectrophoresis flat permeable membrane component |
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| CN107162120B (en) * | 2017-06-27 | 2020-12-22 | 包头稀土研究院 | Purification and utilization method of rare earth carbonate precipitation wastewater |
| CN110467205A (en) * | 2019-08-22 | 2019-11-19 | 四川思达能环保科技有限公司 | Lithium salt solution processing system |
| CN115627487A (en) * | 2022-10-31 | 2023-01-20 | 西南石油大学 | Solar power generation and water electrolysis combined hydrogen production and building environment dehumidification system |
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| US20100187178A1 (en) * | 2003-01-29 | 2010-07-29 | Molycorp Minerals, Llc | Process for removing and sequestering contaminants from aqueous streams |
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| CN1504413A (en) * | 2002-12-03 | 2004-06-16 | 杨文斌 | Reclamation process for waste water of rare earth extraction separation |
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Effective date of registration: 20150907 Address after: 010011 the Inner Mongolia Autonomous Region Ruyi Development Zone, Hohhot city building, No. 1207 Patentee after: INNER MONGOLIA TIANYI ENVIRONMENTAL TECHNOLOGY Co.,Ltd. Address before: 010070, Zhongsheng building, Ruyi development area, the Inner Mongolia Autonomous Region, Hohhot 1207 Patentee before: Inner Mongolia Institute of Technology Dielectrophoresis Applications |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121212 Termination date: 20210722 |