CN101628761A - Treatment method of nickel-cobalt-manganese wastewater generated in waste and old battery treatment process - Google Patents
Treatment method of nickel-cobalt-manganese wastewater generated in waste and old battery treatment process Download PDFInfo
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Abstract
The invention discloses a treatment method of nickel-cobalt-manganese wastewater generated in waste and old battery treatment process and the wastewater mainly contains metal ions such as ions of nickel, cobalt, manganese, copper and the like and little organic matter which is insoluble in water. The invention is mainly characterized in that first the wastewater is treated by stepwise coagulation-sedimentation treatment, then sand filtration-carbon filtration-ion-exchange deep purification treatment is performed, the effluent quality reaches the first-class standard of National Discharge Standards and also corresponds to the demand of industrial production water and the effluent can be reused in production for recycling. The invention facilitates the reuse of nickel-cobalt-manganese wastewater, is characterized by low cost, high metal recovery, large treating capacity, reasonable process flow, simple operation, stable operation, easy execution in industry and the like and is an effective way for the treatment of nickel-cobalt-manganese wastewater generated in waste and old battery recovery process.
Description
Technical field
The invention belongs to the hydrometallurgy field, relate to the nickel cobalt manganese wastewater treatment method that produces in a kind of old and useless battery treatment process.
Background technology
In recent years, along with lithium ion battery, nickel metal hydride battery consumption increase rapidly, the lithium ion battery of scrapping, nickel metal hydride battery quantity significantly increase progressively year by year.Contain a large amount of valuable metals in these old and useless batterys, as nickel, cobalt, copper, aluminium, iron, lithium etc., therefore reclaiming old and useless battery can not only produce huge economic benefit, and can reduce objectionable impurities in the battery, as the pollution to environment such as lithium hexafluoro phosphate, alleviate China's strategic resource cobalt metal shortage, for a long time according to the nervous situation of anti-import, and promote China's battery industry Sustainable development, realize the industrial ecology circulation of battery industry.
At present, hydrometallurgical processes is adopted in the recovery of waste and old lithium ion battery, nickel metal hydride battery usually.Refuse battery through peeling, shell, after the pre-treatment such as fragmentation, sorting, isolated electrode materials through alkali molten-acidleach-P204 abstraction impurity removal-P507 extracting and separating nickel cobalt-crystallization treatment technology reclaims and obtains cobalt chloride and single nickel salt.In the treating processes, acidleach, extraction workshop section can produce the waste water of a large amount of nickeliferous, cobalts, manganese, copper, if not treated, directly discharging not only causes the loss of valuable metal, also will introduce secondary pollution, and the destruction ecotope is detrimental to health directly or indirectly.Therefore must be to the nickel cobalt manganese that produces in the old and useless battery treatment process
Waste waterCarry out resource utilization, harmless treatment.
Because it is emerging industry that old and useless battery reclaims industry; do not design at present the water technology that meets the sector waste water characteristic rationally simple, with low cost, that processing efficiency is high as yet; each middle-size and small-size old and useless battery reclaims enterprise the nickel cobalt manganese waste water that produces in the removal process is adopted the pre-treatment of accent PH-precipitation more; after just directly discharging after the simple filter just of PP cotton or macropore filter screen; just usually also can residual minor amount of nickel cobalt manganese in the water of filter back etc. metal ion; promptly introduce secondary pollution, caused the loss of valuable metal again.Large-lot producer adopts ultrafiltration-reverse osmosis process that initial filter water is done further processing usually, and gained water quality can reach the domestic water standard.Though ultrafiltration and reverse osmosis treatment effect are good, processing speed is slow, and (every permeable membrane is per hour handled wastewater flow rate and is no more than 0.45m
3), film cost height, fenestra easily stops up and causes inefficacy, life-span is shorter, and can't regenerate, and can only change, generally have only large-lot producer just to possess these economic strengths, medium and small sized enterprises are difficult to bear, and can only directly discharge or only carry out filter back discharging just after pre-treatment, so promptly introduce secondary pollution to environment, cause wastewater quality not meet the industrial process waters standard again and be difficult to Returning utilization again, greatly caused water resource waste.
Summary of the invention
Technical problem to be solved by this invention provides the nickel cobalt manganese wastewater treatment method that produces in a kind of old and useless battery treatment process.This method is with low cost, metal recovery rate is high, and effluent quality reaches the primary standard in the national sewage comprehensive emission standard, also meets the industrial process waters requirement, has improved wastewater recycle rate.
For achieving the above object, technical scheme of the present invention is:
The nickel cobalt manganese wastewater treatment method that produces in a kind of old and useless battery treatment process is characterized in that, may further comprise the steps:
1) for the first time coagulation-sedimentation is handled: add alkali lye to nickel cobalt manganese waste water and transfer PH to 8.5～9.8, add coagulating agent then in the waste water and nickel in the waste water, cobalt are precipitated with the form of nickel, cobalt insolubles separate out, No. 1 supernatant liquor of gained enters treatment step 2);
2) coagulation-sedimentation processing for the second time: in No. 1 supernatant liquor, add alkali lye, after fully reacting, add coagulating agent and make manganese, copper in the waste water separate out, get No. 2 supernatant liquors with manganese, copper insolubles form precipitation;
3) sand filtration-charcoal filter is handled: No. 2 supernatant liquors of gained are adjusted back pH value to 8.1～8.5 with sulphuric acid soln; Carry out sand filtration-charcoal filter processing through sand filtration unit and charcoal filter unit successively then, remove suspended substance, oily substance and metal remained ion in the waste water; Gained filtrate enters step 4);
4) deep purifying is handled: adopt ion-exchange to carry out deep purifying to described filtrate and handle, remove metal remained ion in the waste water, make effluent quality reach the industry emission standard.
Described old and useless battery is lithium ion battery, nickel metal hydride battery.
Alkali lye described in the step 1) is the sodium hydroxide saturated solution, and described nickel, cobalt insolubles are the oxyhydroxide of nickel, cobalt.
Step 2) alkali lye described in is saturated solution of sodium carbonate, and the molar mass of the yellow soda ash of adding is manganese in the waste water, the total molar mass of copper 1.0～1.2 times; Described manganese, copper insolubles are manganese, copper carbonic acid thing.
Step 1), 2) in the coagulating agent described in, be flocculation agent with the polymerize aluminum chloride, consumption is 0.5～1g/L, and polyacrylamide is a coagulant aids, and consumption is 0.5g～1g/L, and operation is at room temperature carried out.
The concentration of sulphuric acid soln described in the step 3) is 4～6mol/L.
Sand filtration unit in the step 3), quartz sand filler height are 1400～2000mm, and the operation flow velocity is 6～8m/h.
Charcoal described in step 3) filter unit, the high granular size of charcoal filter tower bottom filling 200～300mm be the quartz sand of 1～10mm as supporting layer, load the high granular gac of 1000～1500mm on the quartz sand layer as filtering layer, flow velocity is 8～15m/h.
The ion-exchange unit that is used for ion exchange treatment in the step 4) adopts slightly acidic Na type ion exchange resin, and the resin extender height is 1500～2000mm, twin columns series connection, operation flow velocity 10～15m/h.
Nickel, cobalt insolubles that step 1) is produced form the dewatered sludge recovery after press filtration, the filtrate of gained is returned in the nickel cobalt manganese waste water in the step 1) and handled after the press filtration; Step 2) manganese of Chan Shenging, copper insolubles form dewatered sludge and reclaim after press filtration, and the filtrate of gained is returned step 2 after the press filtration) in No. 1 supernatant liquor in handle.
Nickel cobalt manganese waste water is after collecting among the present invention, earlier through substep coagulation-sedimentation pre-treatment, promptly add saturated sodium hydroxide solution and transfer pH value, stir through air blast, behind the thorough mixing, waste water imports in the coagulation reaction tank, through adding coagulating agent nickel, cobalt is separated out with the hydroxide form precipitation, goes into the tube settler solid-liquid separation then; Supernatant liquor is gone into the comprehensive adjustment pond No. 2, adds saturated solution of sodium carbonate, and air blast imports No. 2 coagulation reaction tank after stirring thorough mixing, through adding coagulating agent manganese, copper is separated out with carbonic acid thing form precipitation, after go into the tube settler solid-liquid separation, supernatant liquor is gone into PH and is adjusted back the pond; Readjustment PH is after sand filtration-charcoal is filtered processing, after the processing of ion-exchange deep purifying.Effluent quality reaches industry emission standard and industrial process waters standard, thereby realizes above purpose.
Among the present invention, in the nickel cobalt manganese waste water of processing, nickel≤1g/L, cobalt≤1g/L, copper≤7g/L, manganese≤5g/L, iron≤0.02g/L, and contain a small amount of water-fast organism.
Among the present invention, because of adopting acidulous cation resin in the postorder purification process [ion-exchange process for deeper purifying], it is bigger that the disassociation of its cation exchange groups is influenced by pH value, therefore regulate waste water PH earlier, add the sodium hydroxide saturated solution to nickel cobalt manganese waste water, through thorough mixing reaction and aeration, with oxidation
Waste waterMiddle reducing substances, stripping is removed volatile material, and metal ion is wherein separated out with the hydroxide form precipitation, and this operation can at room temperature be carried out;
Among the present invention, adopt to add the coagulating agent accelerate precipitation, lock out operation can carry out at normal temperatures; In the coagulating agent that polymerize aluminum chloride and polyacrylamide are formed, flocculant poly aluminum chloride consumption 0.5g～1g/L, coagulant aids polyacrylamide consumption is 0.5g～1g/L.Wadding grain fully reacts with flocculation agent in coagulation reaction tank, and the reaction times is 15～30min, after go into tube settler and carry out solid-liquid separation, No. 1 supernatant liquor.In order to increase desilting area, shorten sedimentation time, establish the inclined tube filler in the settling region, divide into sludge bucket.Mud at the bottom of the pond enters mud collection mud sump by bottom tube.
Among the present invention, add saturated solution of sodium carbonate to No. 1 supernatant liquor, stir the thorough mixing reaction through air blast, metal ion is wherein separated out with carbonic acid thing form precipitation, and this operation can at room temperature be carried out; After turbidity is imported in No. 2 coagulation reaction tank, add the coagulating agent accelerate precipitation, identical when coagulating agent composition and consumption and heavy nickel, cobalt, the coagulating time is 15～30min,, after go into tube settler and carry out solid-liquid separation, get No. 2 supernatant liquors, aforesaid operations all carries out at normal temperatures.No. 2 supernatant liquor is gone into PH readjustment pond.Various concentration of metal ions all can be reduced to below the 3mg/L in the nickel cobalt manganese waste water after substep coagulation-sedimentation is handled.
Among the present invention, adopt the sulphuric acid soln of 4～6mol/L to transfer No. 2 supernatant liquor PH to 8.1～8.5, after go into sand filtration-charcoal filter-ion exchange treatment unit.
Among the present invention, adopt the quartz sand filtration device as just filtering treatment facility, to remove suspended substance, the organic residue in the waste water.Operate under the room temperature and carry out, the operation flow velocity is 6～8m/h, and delivery turbidity is less than 1.Strainer is a filler with refining quartz sand, and packed height is 1400mm, is specially from top to bottom:
Quartz sand 0.4-0.6mm 700mm
Quartz sand 0.6-1.2mm 200mm
Quartz sand 1.2-2.0mm 200mm
Supporting layer 3.0-5.0mm 300mm
Among the present invention, adopt activated charcoal filter further to handle filtrate just, with the turbidity in the reduction water, chlorine residue etc., flow velocity is 8～15m/h, and delivery turbidity is 0.According to the characteristics of this waste water, the design of filter leaching material is specially from top to bottom:
Gac 20～40 order 1500mm
Quartz sand 1～2mm 50mm
Quartz sand 2～3mm 100mm
Gravel～10mm 150mm
Among the present invention, adopt slightly acidic Na type ion exchange resin to carry out the ion-exchange process for deeper purifying, the resin extender height is 1500mm, twin columns series connection, operation flow velocity 10～15m/h.
Among the present invention, sludge dewatering system comprises: mud dosing pond, spiral pump, medicine system, pressure filter.Mud in the mud collection mud sump is promoted to mud dosing pond by the mud lift pump, after add a certain amount of polyacrylamide medicament, stir the back and squeeze into pressure filter by spiral pump and carry out processed.
Among the present invention behind the ion-exchange deep purifying discharge water water quality: PH ≈ 8.0, total nickel＜0.3mg/L, total manganese＜0.2mg/L, total copper＜0.2mg/L, cobalt, iron all are lower than detectability, water quality reaches primary standard in the national sewage comprehensive emission standard (GB8978-1996), and the industrial process waters standard.
The beneficial effect that the present invention has:
The present invention has realized that discharge water water quality reaches primary standard in the national sewage comprehensive emission standard to the processing of the nickel cobalt manganese waste water of waste and old lithium ion battery removal process generation.This waste water treatment process adopts the filter of lower-cost sand filtration, charcoal, ion-exchange treatment process to substitute expensive ultrafiltration, reverse osmosis operation, overcome in the conventional processes because of introducing ultrafiltration, reverse osmosis operation to cause processing cost high and do not adopt ultrafiltration, reverse osmosis operation to cause again that suspended substance in the discharge water is many, the awkward predicament of the difficult removal of heavy metal ion.It is short that this waste water treatment process has flow process, good work environment, with low cost, the metal recovery rate advantages of higher, day output is big, technical process is reasonable, operation is simple and easy, stable, implement easily, the effective way of the nickel cobalt manganese wastewater treatment that a kind of waste and old lithium ion battery removal process produces is provided.
Description of drawings
Fig. 1 is recovery process figure of the present invention;
Fig. 2 is detailed recovery process figure of the present invention.
Embodiment
Further set forth the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process of the present invention below in conjunction with specific embodiment.
Embodiment 1
In the original nickel cobalt manganese waste water: PH ≈ 6.5, total nickel are that 493.98mg/L, total cobalt are that 115.79mg/L, total manganese are that 1000mg/L, total copper are that 5000mg/L, total iron are 1.14mg/L.
The nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process comprises following step of carrying out continuously:
(1) nickel cobalt manganese waste water is through substep coagulation-sedimentation pre-treatment: add saturated sodium hydroxide solution and regulate waste water pH value to 9.5, after 0.5h is stirred in air blast, waste water is imported in the coagulation reaction tank, add appropriate coagulant, add 500g polymerize aluminum chloride, 600g polyacrylamide in every cube of nickel cobalt manganese waste water, air blast stirring reaction 0.5h, the back is squeezed into tube settler with pump with muddy liquid, carry out settlement separate, get No. 1 supernatant liquor, mud enters mud collection mud sump by bottom tube, gets heavy metal residue nickeliferous, cobalt after press filtration.No. 1 supernatant liquor is gone into the comprehensive adjustment pond No. 2, enters next step coagulation-sedimentation and handles.
(2) in No. 1 supernatant liquor, add saturated solution of sodium carbonate, 0.5h is stirred in air blast, in No. 2 coagulation reaction tank of waste water importing, add coagulating agent, add 500g polymerize aluminum chloride, 600g polyacrylamide in every cube of waste water, air blast stirring reaction 0.5h, the back is squeezed into tube settler with pump No. 2 with muddy liquid, and is settlement separate, gets No. 2 supernatant liquors, mud enters mud collection mud sump No. 2 by bottom tube, must contain the metallic residue of manganese, copper after press filtration.No. 2 supernatant liquor is adjusted back waste water PH to 8.1 with the sulfuric acid of 6mol/L.
(3) heavy metal sewage sludge is handled: by the mud lift pump mud in the mud collection mud sump is promoted to mud dosing pond, adds a certain amount of polyacrylamide, go into pressure filter after the stirring and carry out processed.The gained dewatered sludge is recycled, and pressing filtering liquid goes back to the comprehensive adjustment pond.
Adopt flame atomic absorption spectrometry detect in No. 2 supernatant liquors each concentration of metal ions all less than 3mg/L, nickel: 2.1mg/L, cobalt: 1.7mg/L, copper: 2.6mg/L, manganese: 1.8mg/L, iron: 0.5mg/L wherein.
(4) sand filtration-charcoal filter is handled: No. 2 supernatant liquors of step (2) gained PH=8.1 are carried out sand filtration-charcoal filter processing successively, not only can remove suspended substance, oily substance basically, remaining a small amount of heavy metal ion in can also active adsorption filtrate reduces wherein the light metal positively charged ion greatly (as Na
+, Mg
2+Ion) and negatively charged ion (as Cl
-, SO4
2-Ion) concentration, the quartz sand and the gac that use in above-mentioned sand filtration and the charcoal filter after use for some time absorption property descends, can regularly carry out back flushing to them and handle, and can recover its absorption property fully basically.Recoil water can adopt the ion exchange tower water outlet, by back flushing the adsorptive on the adsorption medium is washed, and backwashing water returns the comprehensive adjustment pond, recycles.
(5) the ion-exchange deep purifying is handled
Adopt ion-exchange that waste water is carried out deep purifying among the present invention and handle, reclaim and remove
Waste waterIn residual Determination of Trace Nickel, cobalt, manganese, copper, ferrous metal ion.Adopt slightly acidic Na ion exchange resin, twin columns series connection, operation flow velocity 10～15m/h.
Adopt flame atomic absorption spectrometry detect in the ion exchange tower water outlet each concentration of metal ions less than 1mg/L, nickel: 0.2mg/L, copper: 0.1mg/L, manganese: 0.1mg/L wherein, cobalt, iron are lower than detectability, delivery turbidity is 0, effluent quality reaches the industry emission standard, also meets the industrial process waters standard.
Waste water is after the present invention handles, water quality is higher, can reach the standard of water of productive use, though may being slightly poorer than the ultrafiltration that some large-lot producer are at present adopted, the water quality after handling adds reverse-osmosis treated, but the present invention has given up ultra-filtration membrane and the reverse osmosis membrane that involves great expense, adopted dog-cheap by contrast sand filtration and charcoal filter treatment process, and particularly quartz sand and gac can also be regenerated, saved processing cost greatly, medium and small sized enterprises also have the ability to adopt the present invention, so range of application of the present invention is wider compared to existing technology; Secondly, the processing speed of sand filtration and activated carbon filtration is very fast (is 1.4m * 0.79m when filling the sand-bed filter volume of expiring quartz sand for example
2, the charcoal filter volume of filling full gac is 1.4m * 0.79m
2, per hour handle wastewater flow rate and be about 30m
3), the treatment capacity of its unit time is much larger than the capacity of ultra-filtration membrane and reverse-osmosis treated.The present invention administers the terminal ion-exchange deep purifying that adopts of technology, has guaranteed effluent quality more.
Above-mentioned each enforcement only is explanation technical conceive of the present invention and characteristics; its objective is and allow the personage that is familiar with this art can understand the present invention and implemented; can not limit protection scope of the present invention with this; all equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process is characterized in that, may further comprise the steps:
1) for the first time coagulation-sedimentation is handled: add alkali lye to nickel cobalt manganese waste water and transfer PH to 8.5～9.8, add coagulating agent then in the waste water and nickel in the waste water, cobalt are precipitated with the form of nickel, cobalt insolubles separate out, No. 1 supernatant liquor of gained enters treatment step 2);
2) coagulation-sedimentation processing for the second time: in No. 1 supernatant liquor, add alkali lye, after fully reacting, add coagulating agent and make manganese, copper in the waste water separate out, get No. 2 supernatant liquors with manganese, copper insolubles form precipitation;
3) sand filtration-charcoal filter is handled: No. 2 supernatant liquors of gained are adjusted back pH value to 8.1～8.5 with sulphuric acid soln; Carry out sand filtration-charcoal filter processing through sand filtration unit and charcoal filter unit successively then, remove suspended substance, oily substance and metal remained ion in the waste water; Gained filtrate enters step 4);
4) deep purifying is handled: adopt ion-exchange to carry out deep purifying to described filtrate and handle, remove metal remained ion in the waste water, make effluent quality reach the industry emission standard.
2. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1 is characterized in that described old and useless battery is lithium ion battery, nickel metal hydride battery.
3. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: the alkali lye described in the step 1) is the sodium hydroxide saturated solution, described nickel, cobalt insolubles are the oxyhydroxide of nickel, cobalt.
4. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: step 2) described in alkali lye be saturated solution of sodium carbonate, the molar mass of the yellow soda ash of adding is manganese in the waste water, the total molar mass of copper 1.0～1.2 times; Described manganese, copper insolubles are manganese, copper carbonic acid thing.
5. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: in the coagulating agent step 1), 2), with the polymerize aluminum chloride is flocculation agent, consumption is 0.5～1g/L, polyacrylamide is a coagulant aids, consumption is 0.5g～1g/L, and operation is at room temperature carried out.
6. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: the concentration of sulphuric acid soln described in the step 3) is 4～6mol/L.
7. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: sand filtration unit in the step 3), quartz sand filler height are 1400～2000mm, the operation flow velocity is 6～8m/h.
8. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: the charcoal filter unit described in the step 3), the high granular size of charcoal filter tower bottom filling 200～300mm is that the quartz sand of 1～10mm is as supporting layer, load the high granular gac of 1000～1500mm on the quartz sand layer as filtering layer, flow velocity is 8～15m/h.
9. according to the nickel cobalt manganese wastewater treatment method that produces in each described old and useless battery treatment process of claim 1～8, it is characterized in that: the ion-exchange unit that is used for ion exchange treatment in the step 4), adopt slightly acidic Na type ion exchange resin, the resin extender height is 1500～2000mm, the twin columns series connection, operation flow velocity 10～15m/h.
10. the nickel cobalt manganese wastewater treatment method that produces in the old and useless battery treatment process according to claim 1, it is characterized in that: nickel, cobalt insolubles that step 1) is produced form the dewatered sludge recovery after press filtration, and the filtrate of gained is returned in the nickel cobalt manganese waste water in the step 1) and handled after the press filtration; Step 2) manganese of Chan Shenging, copper insolubles form dewatered sludge and reclaim after press filtration, and the filtrate of gained is returned step 2 after the press filtration) in No. 1 supernatant liquor in handle.
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