CN106435192B - Removal and the method for recycling copper in a kind of ammonium magnesium phosphate sludge - Google Patents
Removal and the method for recycling copper in a kind of ammonium magnesium phosphate sludge Download PDFInfo
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- CN106435192B CN106435192B CN201610822711.6A CN201610822711A CN106435192B CN 106435192 B CN106435192 B CN 106435192B CN 201610822711 A CN201610822711 A CN 201610822711A CN 106435192 B CN106435192 B CN 106435192B
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- sludge
- copper
- ammonium
- magnesium phosphate
- ammonium magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses removals in a kind of ammonium magnesium phosphate sludge and the method for recycling copper, belong to city domestic sewage and Industrial Wastewater Treatment and recycling field.The low-concentration heavy metal contained in sewage can cause gained ammonium magnesium phosphate sludge heavy-metal exceeded, for ammonium magnesium phosphate sludge is enable to be directly applied to farmland as fertilizer.The method of the present invention is：Concentrated ammonia liquor and ammonium salt are added in the ammonium magnesium phosphate sludge containing copper, is filtered by vacuum after oscillation mixing, fully reaction, filter residue dries in the shade as purified ammonium magnesium phosphate, and the filtrate of separation of solid and liquid is by electrolysis, recyclable elemental copper, electrolyte can be mixed with cupric ammonium magnesium phosphate, and realization recycles.Copper content reaches in this method makes that treated ammonium magnesium phosphate sludge《Pollutant catabolic gene standard in agricultural sludge》(GB4282‑84)；Simple process is easy to operate；Solve the problems, such as because Cu in waste water there are due to reduce ammonium magnesium phosphate sewage sludge quality；Copper can also be recycled after isolation with simple substance form；Ammonia leaching solution can be recycled, and save reagent cost.
Description
Technical field
The invention belongs to city domestic sewage and Industrial Wastewater Treatment and recycling fields, are in particular a kind of
The method that copper removal is removed from cupric ammonium magnesium phosphate sludge.
Background technology
Nitrogenous and phosphorus-containing wastewater directly can lead to body eutrophication, national " 13 " planning to natural water discharge
It clearly proposes to reach to substantially eliminate bad this target of V water body in major river valley, the important indicator ammonia nitrogen as earth's surface water monitoring
It is imperative with the limiting emission of phosphorus and improvement.There is non-renewable phosphor resource, it is estimated that its reserves is only capable of maintaining people
Class develops 100 years or so, and ammoniomagnesium phosphate crystal technology (MAP) precipitates the nitrogen in removal waste water by adding magnesium salts reagent
And phosphorus, precipitated product can be recycled as excellent slow release fertilizer, the application of the technology is closed increasingly by domestic and international researcher
Note.
Poultry manure waste water, landfill leachate containing high ammonia or high phosphorus, semiconductor waste water, anaerobic fermentation supernatant, saponification
Waste water, piggery wastewater and coking wastewater etc. usually contain heavy metal ion, wherein copper concentration range from 1-500mg/L etc.,
When recycling nitrogen phosphorus using ammoniomagnesium phosphate crystal method, for needing to effectively remove heavy metal copper during fertilizer, to meet《Agricultural dirt
Pollutant catabolic gene standard in mud》(GB4282-84).Using the such waste water of ammoniomagnesium phosphate crystal process, when a huge sum of money in waste water
When belonging to 8 times of a concentration of national secondary discharge standard, in ammonium magnesium phosphate sludge nickel, lead, cadmium, copper it is 115 times about exceeded respectively, 15
Again, 68 times and 1.5 times.(the composition of sediment and influence [J] chemistry works of crystalline form that Huang Ying heavy metals recycle guanite method
Journey and equipment, 2008 (3))
There are two types of the current methods that heavy metal is avoided to influence ammoniomagnesium phosphate crystal technique：A kind of is first by the weight in waste water
Metal ion removes, then carries out ammonium magnesium phosphate reaction, and pharmacy cuprammonium such as can be generated in pharmaceutical industry, Fu Luofen production processes gives up
Water has been reported and is first removed Cu in waste water with iron filings and lime, uses ammoniomagnesium phosphate crystal method afterwards by ammonia nitrogen removal.But due to preceding
Hold treatment effect it is limited, during iron reduction copper removal be not thorough, into magnesium ammonium phosphate sediment process before still have copper residual, tie
Copper is with ammonium magnesium phosphate co-precipitation during crystalline substance, leads in sludge that copper is exceeded to become solid waste, can not be directly applied to as fertilizer
Farmland.Another kind is without front-end processing, directly carries out magnesium ammonium phosphate sediment reaction to the waste water of the heavy metal containing high concentration,
Difficult point is that processing cost is high and sludge cannot effective reuse.Magnesium ammonium phosphate sediment is used if any scholar- pyrolysis deamination-acid
Dissolving-electrodeposition technology processing cuprammonium waste water simultaneously recycles copper, and precipitating sludge sub-prime treatment process is numerous and diverse, needs high warm
Solution.
Invention content
1st, technical problems to be solved by the inivention
For using in precipitated product after the ammoniomagnesium phosphate crystal method high ammonia nitrogen copper-containing wastewater of processing or high ammonia nitrogen phosphorus-containing wastewater
Copper excessive problem, the present invention are provided in a kind of sludge from ammonium magnesium phosphate and go the method for copper removal, and copper is recycled, soaked using ammonia
Method removes copper, and precipitated product reaches copper content limit value (GB4282-84, alkali in national regulation using in farmland standard after making processing
Property soil 500mg/Kg dewatered sludges).
2nd, technical solution
A kind of method that copper removal is removed in ammonium magnesium phosphate sludge from cupric, step are：
(1) the cupric ammonium magnesium phosphate that cupric high phosphate or high ammonia-nitrogen wastewater obtain after ammoniomagnesium phosphate crystal process
Sludge first using copper content in ICP or atomic absorption method analysis dewatered sludge, controls dewatered sludge copper content<30g/kg (wet muds
80%) moisture content is no more than, the ammonium hydroxide of 0.3g copper-contained sludges input 3-9ml 8mol/L is formed ammonia with 2.4-7.2mmol ammonium salts
In leaching extraction atmosphere；
(2) 2-4h is mixed in cupric magnesium ammonium phosphate and ammonia leaching solution, and 20-60 DEG C of temperature, speed of agitator is in 200-500r/
Min stands 0.5h afterwards, vacuum filtration；
(3) sludge after filtering, copper content are less than 500mg/Kg；
(4) filtrate in step (2) carries out electrodeposition Copper treatment, electro-deposition voltage 2.2V, current density 200A/m2, temperature
40℃.Filtrate blue shoal until blue disappear after electro-deposition 0.5h again, terminate electro-deposition；
(5) ammonia leaching solution reuse：Electrolyte is as in the substitute of ammonium hydroxide and ammonium salt input step (1) in above-mentioned steps (4)
Ammonia leaching reactor, control reuse ammonia leaching solution quality and dewatered sludge mass ratio (liquid-solid ratio)=(10-30):1, it recycles.
The magnesium ammonium phosphate sediment from livestock-raising waste water, electroplating wastewater, nonferrous metallurgy waste water, landfill leachate,
The waste water such as anaerobic supernatant gained after ammoniomagnesium phosphate crystal process precipitates.It is found in this seminar studies for a long period of time, copper
Mainly it is present in sludge in the form of the compound states such as cupric phosphate and Kocide SD, and the compound of copper is mainly attached to ammonium magnesium phosphate
Plane of crystal is without entering ammonium magnesium phosphate crystals, it means that directly can effectively go sludge progress copper leaching process
Except the copper in sludge, without sludge is dehydrated, desiccation, the complicated processes such as grinds sludge internal copper is exposed again
Carry out leaching process.
Copper content is no more than 30g/kg in above method processing magnesium ammonium phosphate sediment.
Key reaction occurs after magnesium ammonium phosphate sediment is mixed with ammonia leaching solution in step (2) is：
Copper is shifted from solid phase to liquid phase, so as to fulfill the removal of copper.
Sludge in step (3) after filters uses XRD characterization to show that sludge main ingredient for ammonium magnesium phosphate, meets after handling
The using in farmland standard (GB4282-84, basic soil 500mg/Kg dewatered sludge) of national regulation
3rd, advantageous effect
Invention provides a kind of method that copper removal is removed in sludge from ammonium magnesium phosphate, using technical solution provided by the invention,
With following remarkable result：
(1) copper content reaches in the ammonium magnesium phosphate sludge that makes that treated《Pollutant catabolic gene standard in agricultural sludge》
(GB4282-84)；The sludge that can be collected to sedimentation basin is directly carried out except Copper treatment, consumed energy process without sludge dewatering, desiccation etc.,
Greatly simplify technological process.
(2) solve the problems, such as because Cu in waste water there are due to reduce ammonium magnesium phosphate sewage sludge quality, cupric can be effectively removed
Copper in ammonium magnesium phosphate sludge reduces heavy metal and recycles process risk in later stage sludge.
(3) ammonia leaching copper will not lead to the dissolving or decomposition of ammonium magnesium phosphate used by, and XRD characterization result also indicates that place
Sludge main ingredient is ammonium magnesium phosphate after reason；Copper can also be recycled after isolation with simple substance form, and the copper after recycling can be directly as
Industrial production raw material realize the recycling of polluter.
(4) ammonia leaching solution can be recycled, and need to only consume a small amount of chemical reagent, save reagent cost.With the phosphoric acid delivered
Ammonium magnesium technique the relevant technologies compare, and the present invention has the advantage for significantly reducing cost.Such as pungent grasp clear etc. removes cuprammonium pharmacy waste water
It in copper deamination experimental pretreatment, needs first first to be removed Cu in waste water with iron filings and lime, uses ammoniomagnesium phosphate crystal method afterwards by ammonia
Nitrogen removes, and the ammonium magnesium phosphate sludge finally obtained is still difficult to as Fertilizer application.Under comparing, using the invention without locating in advance
Copper removal is managed, can directly carry out ammoniomagnesium phosphate crystal reaction, then cupric ammonium magnesium phosphate sludge is carried out again except Copper treatment, handles it
Ammonium magnesium phosphate can be used as fertilizer to sell afterwards, while ammonia leaching solution is through can be recycled after electrodeposition cement copper, copper removal process energy consumption and
Supplies consumption is extremely low, and cost advantage is apparent.
(5) suitable application area is in the high waste water of the nitrogen and phosphorus contents such as breeding wastewater, landfill leachate and copper content.
Description of the drawings
Fig. 1 is pure phosphoric acid ammonium magnesium (MAP pure) and ammonia leaching treated ammonium magnesium phosphate sludge XRD diffraction peak figures, before ammonia leaching
Sludge prepare respectively from copper initial concentration be 20mg/L (MAP-Cu-20) and 100mg/L (MAP-Cu-100) simulated wastewater.
Fig. 2 is scanning electron microscope phenogram, and sample is respectively：(a) pure phosphoric acid ammonium magnesium, (b) from copper initial concentration be 20mg/L
Simulated wastewater in the sludge (MAP-Cu-20) for preparing, (c) is prepared from simulated wastewater that copper initial concentration is 100mg/L
Sludge (MAP-Cu-100), (d) soak treated MAP-Cu-20 sludge with ammonia of the present invention, and (e) soaks that treated with ammonia of the present invention
MAP-Cu-100 sludge.
Fig. 3 is the influence of copper content in sludge after liquid-solid ratio soaks ammonia.
Fig. 4 is the influence of copper content in sludge after ammonia density soaks ammonia
Fig. 5 is the influence that ammonia-ammonium system that different ammonium salts are formed and ammonia ammonium compare copper content in sludge after ammonia soaks
Fig. 6 is the influence of copper content in sludge after ammonia leaching temperature soaks ammonia
Fig. 7 is present invention process flow chart.
Specific embodiment
Embodiment 1：
The waste water of certain copper content 20mg/L, ammonia-nitrogen content 333mg/L, by n (N)：n(P):N (Mg)=1:1:1 ratio adds
Enter phosphate and magnesium salts, pH value is adjusted to 9.5 with sodium hydroxide carries out ammonium magnesium phosphate reaction, stirs 1 hour, it is heavy to be obtained by filtration
It forms sediment.After testing, copper content is 2920mg/kg in sediment.It is《Pollutant catabolic gene standard in agricultural sludge》(GB4282-84) in
6 times of copper limit value.Ammonium carbonate is added in the concentrated ammonia liquor of 8-12mol/L and ammonia leaching solution is made, control ammonium salt is with ammonium hydroxide molar ratio
(0.5-2):1.Ammonia leaching solution is mixed with magnesium ammonium phosphate sediment, liquid-solid ratio 18：1, oscillation leaching, 2h are carried out in closed container
Filtering is taken out afterwards, measures after ammonia leaching that copper content is 296mg/kg in ammonium magnesium phosphate sludge.Copper in treated ammonium magnesium phosphate sludge
Content reaches《Pollutant catabolic gene standard in agricultural sludge》(GB4282-84), XRD characterization result prove ammonia leaching after precipitate mainly into
Part is ammonium magnesium phosphate, can be sold as fertilizer.
Embodiment 2：
The waste water of certain copper content 100mg/L, ammonia-nitrogen content 333mg/L, by n (N)：n(P):N (Mg)=1:1:1 ratio
Phosphate and magnesium salts are added in, pH value is adjusted to 9.5 with sodium hydroxide carries out ammonium magnesium phosphate reaction, stirs 1 hour, it is heavy to be obtained by filtration
It forms sediment.After testing, copper content is 17849mg/kg in sediment.It is《Pollutant catabolic gene standard in agricultural sludge》(GB4282-84)
18 times of middle copper limit value.Ammonium sulfate is added in the concentrated ammonia liquor of 8-12mol/L and ammonia leaching solution is made, control ammonium salt and ammonium hydroxide molar ratio
For (0.5-2):1.Ammonia leaching solution is mixed with magnesium ammonium phosphate sediment, liquid-solid ratio 16：1, oscillation leaching is carried out in closed container,
Filtering is taken out after 2h, it is 396mg/kg to measure copper content in precipitation.Copper content reaches in treated ammonium magnesium phosphate sludge《It is agricultural
Pollutant catabolic gene standard in sludge》(GB4282-84), precipitation main ingredient is ammonium magnesium phosphate after XRD characterization result proves ammonia leaching,
It can sell as fertilizer.
Embodiment 3：
The waste water of certain copper content 100mg/L, phosphorus content 737mg/L, by n (N)：n(P):N (Mg)=1:1:1 ratio adds
Enter phosphate and magnesium salts, pH is adjusted to 10 with sodium hydroxide carries out ammonium magnesium phosphate reaction, stirs 1h, precipitation is obtained by filtration.Through inspection
It surveys, copper content is 17602mg/kg in sediment.It is《Pollutant catabolic gene standard in agricultural sludge》(GB4282-84) copper limit value in
35 times.Ammonium carbonate is added in the concentrated ammonia liquor of 8-12mol/L and ammonia leaching solution is made, control ammonium salt is (0.5- with ammonium hydroxide molar ratio
2):1.Ammonia leaching solution is mixed with magnesium ammonium phosphate sediment, liquid-solid ratio 10：1, oscillation leaching is carried out in closed container, is taken after 2h
Go out filtering, it is 410mg/L to measure copper content in precipitation.Copper content reaches in treated ammonium magnesium phosphate sludge《In agricultural sludge
Pollutant catabolic gene standard》(GB4282-84), precipitation main ingredient is ammonium magnesium phosphate after XRD characterization result proves ammonia leaching, can conduct
Fertilizer sells.
Embodiment 4：
Certain copper content is the ammonium magnesium phosphate sludge of 694mg/kg.Copper content is《Pollutant catabolic gene standard in agricultural sludge》
(GB4282-84) 1.4 times of copper limit value in.Ammonium acetate is added in the concentrated ammonia liquor of 8-12mol/L and ammonia leaching solution is made, control ammonium salt
It is (0.5-2) with ammonium hydroxide molar ratio:1.Ammonia leaching solution is mixed with magnesium ammonium phosphate sediment, liquid-solid ratio 30：1, in closed container
Oscillation leaching is carried out, filtering is taken out after 2h, it is 366mg/L to measure copper content in precipitation.Copper in treated ammonium magnesium phosphate sludge
Content reaches《Pollutant catabolic gene standard in agricultural sludge》(GB4282-84), XRD characterization result prove ammonia leaching after precipitate mainly into
Part is ammonium magnesium phosphate, can be sold as fertilizer.
Claims (4)
1. going the method for copper removal in a kind of ammonium magnesium phosphate sludge from cupric, step is
（1）The cupric ammonium magnesium phosphate that cupric high phosphate or high ammonia-nitrogen wastewater obtain after ammoniomagnesium phosphate crystal process is dirty
Mud forms ammonia leaching according to ammonium hydroxide and the 2.4-7.2mmol ammonium salts of every 0.2-0.4g copper-contained sludges input 3-9ml 8mol/L and extracts
In atmosphere；
（2）2-4h is mixed in cupric magnesium ammonium phosphate sludge and ammonia leaching solution, and 20-60 DEG C of temperature, speed of agitator is in 200-500r/
0.5h is stood after min, fully reaction, is filtered by vacuum；
（3）Sludge after filter, copper content are less than 500mg/Kg；
（4）By step（2）In filtrate carry out electrodeposition Copper treatment, filtrate blue shoal until blue disappear after electro-deposition again
0.5h terminates electro-deposition；
（5）Ammonia leaching solution reuse：Above-mentioned steps（4）Middle electrolyte puts into step as the substitute of ammonium hydroxide and ammonium salt（1）In ammonia
Reactor is soaked, control reuse ammonia leaching solution quality is 10-30 with dewatered sludge mass ratio:1, it recycles.
2. the method for copper removal is gone in a kind of ammonium magnesium phosphate sludge from cupric according to claim 1, it is characterised in that step
（1）Middle control dewatered sludge copper content<30g/kg, wet mud moisture content are no more than 80%.
3. the method for copper removal is gone in a kind of ammonium magnesium phosphate sludge from cupric according to claim 1 or 2, it is characterised in that step
Suddenly（4）In electro-deposition voltage 1-3V, current density 100-300A/m2, 30-50 DEG C of temperature.
4. the method for copper removal is gone in a kind of ammonium magnesium phosphate sludge from cupric according to claim 1 or 2, it is characterised in that step
Suddenly（4）In use XRD characterization show processing after sludge main ingredient for ammonium magnesium phosphate, meet the using in farmland mark of national regulation
It is accurate.
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| CN109201722A (en) * | 2017-07-04 | 2019-01-15 | 江西盖亚环保科技有限公司 | A method of strengthening Pb, As, Cu, Cd, Zn heavy-metal contaminated soil regulation effect |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623924A (en) * | 2003-12-04 | 2005-06-08 | 中国科学院生态环境研究中心 | Process for removing ammonia of treating waste water containing high contentrition ammonia |
| CN1884116A (en) * | 2006-07-10 | 2006-12-27 | 同济大学 | Method for processing refuse-burning fly-ash by using magnesium ammonium phosphate sedimentation sludge |
| CN103466770A (en) * | 2013-09-27 | 2013-12-25 | 中南大学 | Copper ammonia complexation wastewater treatment method |
| CN203529996U (en) * | 2013-09-27 | 2014-04-09 | 中南大学 | Cuprammouium complexing wastewater treatment device |
| CN105152716A (en) * | 2015-09-05 | 2015-12-16 | 山东红日阿康化工股份有限公司 | Treating technology for acid liquor generated during phosphorus ore dressing process by acid method as well as ore-dressing process and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19829799C2 (en) * | 1998-07-03 | 2001-03-29 | Fraunhofer Ges Forschung | Process for recycling manure |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623924A (en) * | 2003-12-04 | 2005-06-08 | 中国科学院生态环境研究中心 | Process for removing ammonia of treating waste water containing high contentrition ammonia |
| CN1884116A (en) * | 2006-07-10 | 2006-12-27 | 同济大学 | Method for processing refuse-burning fly-ash by using magnesium ammonium phosphate sedimentation sludge |
| CN103466770A (en) * | 2013-09-27 | 2013-12-25 | 中南大学 | Copper ammonia complexation wastewater treatment method |
| CN203529996U (en) * | 2013-09-27 | 2014-04-09 | 中南大学 | Cuprammouium complexing wastewater treatment device |
| CN105152716A (en) * | 2015-09-05 | 2015-12-16 | 山东红日阿康化工股份有限公司 | Treating technology for acid liquor generated during phosphorus ore dressing process by acid method as well as ore-dressing process and application |
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