CN103570158B - A kind of recovering rare earth from Rare Earth Production waste water and the method for ammonia nitrogen qualified discharge - Google Patents
A kind of recovering rare earth from Rare Earth Production waste water and the method for ammonia nitrogen qualified discharge Download PDFInfo
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- CN103570158B CN103570158B CN201310547708.4A CN201310547708A CN103570158B CN 103570158 B CN103570158 B CN 103570158B CN 201310547708 A CN201310547708 A CN 201310547708A CN 103570158 B CN103570158 B CN 103570158B
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Abstract
The invention provides a kind of method of recovering rare earth from Rare Earth Production waste water and ammonia nitrogen qualified discharge, the method mainly comprises the steps such as the wastewater repurification after Rare Earth Production purification of waste water, rare earth recovery, rare earth recovery and NH_3-N treating.The present invention adopts ion exchange resin to reclaim to have the rare earth of high economic worth, is then directly processed by the ammonia nitrogen waste water of ammonia nitrogen gas-liquid separation membrane to the various concentration in factory effluent.This technological process is simple, cost is low, invest little, treatment effect is obvious, can ensure ammonia nitrogen emission compliance completely, ammonia nitrogen absorption liquid can also recycle in rare earth mining process, not having secondary pollution problem, is a kind of method of efficient from Rare Earth Production waste water, economic recovery rare earth and process ammonia nitrogen.
Description
Technical field
The present invention is specifically related to a kind of method of recovering rare earth from Rare Earth Production waste water and ammonia nitrogen qualified discharge, belongs to mineral wealth recovery and utilization technology field.
Background technology
Rare-earth mineral can produce a large amount of waste water containing high added value rare earth element and high ammonia-nitrogen content in leaching, the course of processing.The ammonia nitrogen in waste water content that China's rare-earth trade is directly discharged every year is 100-2000mg/L, exceeds discharging standards tens times to hundreds of times.The direct discharge of these waste water causes the loss in vain of high added value rare earth element on the one hand; On the other hand, these high ammonia-nitrogen wastewaters directly enter water body, will cause body eutrophication, reduce water body ornamental value, and the NO3-N and NO2-N that oxidation generates also can cause permanent injury to the hydrobiont even health of the mankind.On November 24th, 2011, China national Environmental Protection Department is issued in 14 provincial 84 Rare Earth Enterprises in the whole nation, only has 15 enterprise wastewater ammonia-nitrogen contents to meet environmental requirement.Therefore, how to facilitate, economically the valency rare earth element recovery that has in Rare Earth Production process discharge waste water is come, and standard ammonia-nitrogen content being reduced to country's permission has become one of Rare Earth Production enterprise of China difficult problem anxious to be resolved.
The method of recovering rare earth and process ammonia nitrogen is varied, and treatment process respectively has feature.Liu Huanchang etc. utilize sodium bicarbonate to do precipitation agent from rare earth containing zeolite mother liquor, precipitate and isolate rare earth compound (201210251397.2).Liu little Nan utilizes cheap lime to make precipitation agent, and rare earth ion is separated from waste water with precipitation of hydroxide (201010570069.X).The method process RE waste water of Zhong Huayun calcium hydroxide precipitation and P507 organic extraction, reclaims rare earth (201010294998.2) wherein.Blow-off method and ion-exchange denitrification method are combined by Zhou Kanggen, blow-off method process high strength ammonia nitrogen solution, ion exchange resin treatment low concentration ammonia nitrogen solution (201010546175.4).The people such as Zhou Jicheng carry out removal of ammonia and nitrogen at microwave field irradiation, and the ammonia nitrogen waste water adding modified activated carbon forms liquid-solid mixed solution at microwave field irradiation removal of ammonia and nitrogen (201010517621.9).The people such as Xie Yu utilize biological process to process ammonia nitrogen waste water, carry out the oxidizing reaction of ammonia due to the existence of oxygen on granule sludge top layer, granule interior is because utilize the oxidation products of ammonia to carry out anti-nitration reaction under anoxia condition, thus realize single-stage biological nitrogen removal, achieve Simultaneous Nitrification and denitrification, reach higher denitrification percent (200710191587.9).The people such as Lv Lufeng utilize precipitator method process ammonia nitrogen, ammonia nitrogen waste water is divided into two portions, wherein add magnesium salts precipitation agent in a part of waste water, phosphoric acid precipitates agent is added in another part waste water, two portions waste water is mixed, the pH value regulating the rear waste water of mixing is 8 ~ 10, is precipitated the supernatant liquid (200610144220.7) of thing ammonium magnesium phosphate and removal of ammonia and nitrogen after sedimentation.Reverse osmosis membrane separation, ion-exchange and traditional stripping process combine use by Dai Yongqi, the ammonia nitrogen waste water (200910029777.X) of process different concns.
In summary, current rare earth reclaims and processes in the technological method of ammonia nitrogen, mainly with the precipitator method and absorption method the most common, on treatment process, major part be all be separated use, do not process ammonia nitrogen waste water at recovering rare earth simultaneously, major part is all that these technology often exist complex process, and processing cost is high for the multiple method compound use of different concns ammonia nitrogen waste water, investment is large, the problems such as effect is undesirable.
Summary of the invention
Reclaim and is separated with process ammonia nitrogen technique for overcoming prior art middle-weight rare earths, method complexity, the defect that processing cost is high, effect is undesirable, the invention provides a kind of new recovering rare earth from Rare Earth Production waste water and the method for ammonia nitrogen qualified discharge.The method cost is low, invests little, and process is simple, and treatment effect is obvious, and ammonia nitrogen absorption liquid can also recycle in rare earth mining process, does not have secondary pollution problem.
Realize a kind of method that technical scheme that the object of the invention adopts is recovering rare earth from Rare Earth Production waste water and ammonia nitrogen qualified discharge, specifically adopt following steps:
(1) purification of waste water, rare earth are reclaimed: Rare-earth Mine factory effluent is injected rare earth retrieving arrangement with 1000-3000L/h flow velocity, after quartz sand, manganese sand, activated charcoal filter, enter the rare earth that ion exchange resin is housed to reclaim in post and carry out rare earth recovery, hydrochloric acid soln is used to carry out desorption process to the ion exchange resin after absorption, desorbed solution enters rare earth collection box, reclaims rare earth;
(2) rare earth reclaim after wastewater repurification: the waste water after rare earth reclaims is flowed into flocculation tanks, adds sedimentation after flocculation agent, enter NH_3-N treating water tank through filter;
(3) NH_3-N treating: the pH value of waste water in NH_3-N treating water tank is regulated and remains on 11 ~ 13, ammonia nitrogen absorption liquid pH value is regulated and remains on 1 ~ 3 simultaneously; With ammonia nitrogen gas-liquid separation film device, cyclic absorption process is carried out to the waste water that pH value is adjusted in the NH_3-N treating water tank of 11 ~ 13, in cyclic absorption treating processes, waste water injects the flow velocity of ammonia nitrogen gas-liquid separation film device is 600-1000L/h, and ammonia nitrogen degassing film external and internal pressure difference remains within the scope of 0.02-0.08MPa;
(4) treat that in the waste water in NH_3-N treating water tank, ammonia nitrogen concentration is down to below national regulations value, stop wastewater treatment circulation, waste water is discharged through water shoot.
Further being defined as flocculation agent used to technique scheme is polymeric flocculant or inorganic flocculating agent, can select polymerize aluminum chloride or polyacrylamide.The pH value of waste water in NH_3-N treating water tank regulates and remains on 11-13 by step (3) sodium hydroxide, potassium hydroxide or calcium hydroxide; With the sulfuric acid of 1-6mol/L or nitric acid, ammonia nitrogen absorption liquid pH value is regulated and remains on 1-3.Described in step (1), ion exchange resin is strong acid type, weak-type or chelating ion exchange resin.
As shown from the above technical solution, the present invention adopts ion exchange resin to reclaim to have the rare earth of high economic worth, is then directly processed by the ammonia nitrogen waste water of ammonia nitrogen gas-liquid separation membrane to the various concentration in factory effluent.This technological process is simple, cost is low, invest little, treatment effect is obvious, rare earth yield is up to more than 90%, ammonia nitrogen concentration in waste discharge after all process is reduced to below 10mg/L, have even lower than 2mg/L, ammonia nitrogen removal frank is up to more than 98%, can ensure ammonia nitrogen emission compliance completely, ammonia nitrogen absorption liquid sea can recycle in rare earth mining process, do not have secondary pollution problem, visible the present invention is a kind of method of efficient from Rare Earth Production waste water, economic recovery rare earth and process ammonia nitrogen.
Accompanying drawing explanation
Accompanying drawing is recovering rare earth from Rare Earth Production waste water provided by the invention and the process flow sheet of the method for ammonia nitrogen qualified discharge.
Embodiment
Recovering rare earth from Rare Earth Production the waste water provided by the invention and method of ammonia nitrogen qualified discharge is mainly divided into three parts as shown in drawings, Rare Earth Production purification of waste water part, rare earth recovery part and NH_3-N treating part, specific embodiment refers to following embodiment.
Embodiment 1
Get Rare Earth Production waste water, recording got waste water Rare-Earth Content is 200mg/L, ammonia nitrogen concentration is 500mg/L, this for 1000L Rare Earth Production waste water is injected rare earth retrieving arrangement with 1000L/h flow velocity, pass through quartz sand, after manganese sand and activated carbon filtration tank, entering the rare earth that strong acid ion exchange resin is housed reclaims in post, the water reclaimed through rare earth flows into flocculation tanks, with polyacrylamide flocculant, flocculating settling process is carried out to waste water, waste water after flocculation treatment through filter laggard enter NH_3-N treating water tank, add sodium hydroxide while stirring and wastewater pH is adjusted to 12, inject ammonia nitrogen gas-liquid separation film device with the treated liquid pipeline of 600L/h flow velocity and carry out ammonia nitrogen circular treatment, simultaneously, absorption liquid pH value sulfuric acid in ammonia nitrogen respiratory box is adjusted to 2, inject ammonia nitrogen gas-liquid separation film device through absorption liquid pipeline and carry out ammonia nitrogen cyclic absorption, and ensure that degassing film external and internal pressure difference is for 0.05MPa, ammonia nitrogen in waste water concentration through circular treatment is reduced to 2.96mg/L, ammonia nitrogen removal frank is 99.41%, reaches ammonia nitrogen concentration in rare-earth industry pollutant emission standard (GB26451-2011) and is less than the regulation of 15mg/L.Use 2mol/L hydrochloric acid soln to carry out desorption process to the strong acid ion exchange resin after absorption, desorbed solution enters rare earth collection box, and rare earth yield is 92.50%.
Embodiment 2
Get Rare Earth Production waste water, recording got waste water Rare-Earth Content is 20mg/L, ammonia nitrogen concentration is 2000mg/L, this for 1000L Rare Earth Production waste water is injected rare earth retrieving arrangement with 2000L/h flow velocity, pass through quartz sand, after manganese sand and activated carbon filtration tank, entering the rare earth that weak acid ion exchange resin is housed reclaims in post, the water reclaimed through rare earth flows into flocculation tanks, with flocculant of polymeric aluminium chloride, flocculating settling process is carried out to waste water, waste water after flocculation treatment through filter laggard enter NH_3-N treating water tank, add calcium hydroxide while stirring and wastewater pH is adjusted to 13, inject ammonia nitrogen gas-liquid separation film device with the treated liquid pipeline of 1000L/h flow velocity and carry out ammonia nitrogen circular treatment, simultaneously, absorption liquid pH value sulfuric acid in ammonia nitrogen respiratory box is adjusted to 1, inject ammonia nitrogen gas-liquid separation film device through absorption liquid pipeline and carry out ammonia nitrogen cyclic absorption, and ensure that degassing film external and internal pressure difference is for 0.08MPa, ammonia nitrogen in waste water concentration through circular treatment is reduced to 8.66mg/L, ammonia nitrogen removal frank is 99.57%, reaches ammonia nitrogen concentration in rare-earth industry pollutant emission standard (GB26451-2011) and is less than the regulation of 15mg/L.Use 1mol/L hydrochloric acid soln to carry out desorption process to the weak acid ion exchange resin after absorption, desorbed solution enters rare earth collection box, and rare earth yield is 93.60%.
Embodiment 3
Get Rare Earth Production waste water, recording got waste water Rare-Earth Content is 200mg/L, ammonia nitrogen concentration is 100mg/L, this for 1000L Rare Earth Production waste water is injected rare earth retrieving arrangement with 3000L/h flow velocity, pass through quartz sand, after manganese sand and activated carbon filtration tank, entering the rare earth that chelating ion exchange resin is housed reclaims in post, the water reclaimed through rare earth flows into flocculation tanks, with polyaluminum sulfate aluminium flocculating agent, flocculating settling process is carried out to waste water, waste water after flocculation treatment through filter laggard enter NH_3-N treating water tank, add sodium hydroxide while stirring and wastewater pH is adjusted to 11, inject ammonia nitrogen gas-liquid separation film device with the treated liquid pipeline of 800L/h flow velocity and carry out ammonia nitrogen circular treatment, simultaneously, absorption liquid pH value nitric acid in ammonia nitrogen respiratory box is adjusted to 3, inject ammonia nitrogen gas-liquid separation film device through absorption liquid pipeline and carry out ammonia nitrogen cyclic absorption, and ensure that degassing film external and internal pressure difference is for 0.02MPa, ammonia nitrogen in waste water concentration through circular treatment is reduced to 1.08mg/L, ammonia nitrogen removal frank is 98.92%, reaches ammonia nitrogen concentration in rare-earth industry pollutant emission standard (GB26451-2011) and is less than the regulation of 15mg/L.Use 2mol/L hydrochloric acid soln to carry out desorption process to the chelating ion exchange resin after absorption, desorbed solution enters rare earth collection box, and rare earth yield is 90.30%.
Embodiment 4
Get Rare Earth Production waste water, recording got waste water Rare-Earth Content is 100mg/L, ammonia nitrogen concentration is 600mg/L, this for 1000L Rare Earth Production waste water is injected rare earth retrieving arrangement with 1000L/h flow velocity, pass through quartz sand, after manganese sand and activated carbon filtration tank, entering the rare earth that strong acid ion exchange resin is housed reclaims in post, the water reclaimed through rare earth flows into flocculation tanks, with polyaluminum sulfate aluminium flocculating agent, flocculating settling process is carried out to waste water, waste water after flocculation treatment through filter laggard enter NH_3-N treating water tank, add sodium hydroxide while stirring and wastewater pH is adjusted to 12, inject ammonia nitrogen gas-liquid separation film device with the treated liquid pipeline of 900L/h flow velocity and carry out ammonia nitrogen circular treatment, simultaneously, absorption liquid pH value nitric acid in ammonia nitrogen respiratory box is adjusted to 2, inject ammonia nitrogen gas-liquid separation film device through absorption liquid pipeline and carry out ammonia nitrogen cyclic absorption, and ensure that degassing film external and internal pressure difference is for 0.06MPa, ammonia nitrogen in waste water concentration through circular treatment is reduced to 6.08mg/L, ammonia nitrogen removal frank is 98.99%, reaches ammonia nitrogen concentration in rare-earth industry pollutant emission standard (GB26451-2011) and is less than the regulation of 15mg/L.Use 2mol/L hydrochloric acid soln to carry out desorption process to the strong acid ion exchange resin after absorption, desorbed solution enters rare earth collection box, and rare earth yield is 90.82%.
Claims (7)
1. recovering rare earth and a method for ammonia nitrogen qualified discharge from Rare Earth Production waste water, is characterized in that comprising the steps:
(1) purification of waste water, rare earth are reclaimed: Rare-earth Mine factory effluent is injected rare earth retrieving arrangement with 1000-3000L/h flow velocity, after quartz sand, manganese sand, activated charcoal filter, enter the rare earth that ion exchange resin is housed to reclaim in post and carry out rare earth recovery, hydrochloric acid soln is used to carry out desorption process to the ion exchange resin after absorption, desorbed solution enters rare earth collection box, reclaims rare earth;
(2) rare earth reclaim after wastewater repurification: the waste water after rare earth reclaims is flowed into flocculation tanks, adds sedimentation after flocculation agent, enter NH_3-N treating water tank through filter;
(3) NH_3-N treating: the pH value of waste water in NH_3-N treating water tank is regulated and remains on 11 ~ 13, ammonia nitrogen absorption liquid pH value is regulated and remains on 1 ~ 3 simultaneously; With ammonia nitrogen gas-liquid separation film device, cyclic absorption process is carried out to the waste water that pH value is adjusted in the NH_3-N treating water tank of 11 ~ 13, in cyclic absorption treating processes, waste water injects the flow velocity of ammonia nitrogen gas-liquid separation film device is 600-1000L/h, and ammonia nitrogen degassing film external and internal pressure difference remains within the scope of 0.02-0.08MPa;
(4) treat that in the waste water in NH_3-N treating water tank, ammonia nitrogen concentration is down to below national regulations value, stop wastewater treatment circulation, waste water is discharged through water shoot.
2. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 1, is characterized in that: flocculation agent used is polymeric flocculant.
3. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 2, is characterized in that: flocculation agent used is polymerize aluminum chloride or polyacrylamide.
4. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 1, is characterized in that: flocculation agent used is inorganic flocculating agent.
5. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 1, is characterized in that: the pH value of waste water in NH_3-N treating water tank regulates and remains on 11-13 by step (3) sodium hydroxide, potassium hydroxide or calcium hydroxide.
6. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 1, is characterized in that: ammonia nitrogen absorption liquid pH value regulates and remains on 1-3 by sulfuric acid or the nitric acid of step (3) 1-6mol/L.
7. recovering rare earth and the method for ammonia nitrogen qualified discharge from Rare Earth Production waste water according to claim 1, is characterized in that: described in step (1), ion exchange resin is strong acid type, weak-type or chelating ion exchange resin.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105174551A (en) * | 2015-10-12 | 2015-12-23 | 厦门星富环保科技有限公司 | High-concentration ammonia-nitrogen wastewater recycling technology |
| CN105293772B (en) * | 2015-11-17 | 2017-12-29 | 中国地质大学（武汉） | Rare earth selects the recovery of smelting waste water middle rare earth and ammonia nitrogen resource utilization method |
| JP6592386B2 (en) * | 2016-03-09 | 2019-10-16 | オルガノ株式会社 | Method and apparatus for treating ammonia-containing wastewater |
| CN106145443A (en) * | 2016-07-29 | 2016-11-23 | 乐山东承新材料有限公司 | A kind of processing method of Rare Earth Production waste water |
| CN106186492A (en) * | 2016-08-24 | 2016-12-07 | 国家海洋局天津海水淡化与综合利用研究所 | The ammonia nitrogen removal of a kind of embrane method high-concentration ammonia nitrogenous wastewater and ammonium salt enrichment method |
| CN107487903A (en) * | 2017-09-30 | 2017-12-19 | 重庆融极环保工程有限公司 | The recovery method of ammonia nitrogen in a kind of livestock breeding wastewater |
| CN108715496B (en) * | 2018-06-07 | 2019-03-22 | 全南县新资源稀土有限责任公司 | A method of recycling ammonia from Rare Earth Separation waste liquid |
| CN109097566A (en) * | 2018-09-17 | 2018-12-28 | 江西理工大学 | A method of the recovering rare earth from weathered superficial leaching rare-earth ore |
| CN110171906B (en) * | 2019-06-13 | 2020-01-07 | 江西挺进环保科技有限公司 | Drainage-type rare earth mine tail water treatment system and treatment process |
| CN114873832A (en) * | 2021-02-05 | 2022-08-09 | 三达膜科技（厦门）有限公司 | Treatment method of high-ammonia nitrogen wastewater with unbalanced nutrient source |
| CN114457234A (en) * | 2021-07-23 | 2022-05-10 | 江西离子型稀土工程技术研究有限公司 | Rare earth impurity removal and enrichment ion exchange system and process method |
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