CN105779763A - Method for extracting zinc from high-cadmium zinc-contained mineral separation tailing water and preparing electric zinc - Google Patents
Method for extracting zinc from high-cadmium zinc-contained mineral separation tailing water and preparing electric zinc Download PDFInfo
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- CN105779763A CN105779763A CN201610359222.1A CN201610359222A CN105779763A CN 105779763 A CN105779763 A CN 105779763A CN 201610359222 A CN201610359222 A CN 201610359222A CN 105779763 A CN105779763 A CN 105779763A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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Abstract
The invention relates to a method for extracting zinc from high-cadmium zinc-contained mineral separation tailing water and preparing electric zinc. The method includes the following steps that (1) the high-cadmium zinc-contained mineral separation tailing water is filtered to remove suspended solid particles; (2) an organic phase is adopted for conducting two-stage counter-current extraction on aqueous phase feed liquid; (3) a sulfuric acid solution is used for conducting two-stage countercurrent washing on a loaded organic phase obtained after two-stage extraction; (4) a waste electrolyte is used for conducting reverse extraction on a washed organic phase; and (5) after strip liquor is subject to standing, ultrasonic treatment, air floatation treatment and activated carbon oil removing treatment, the oil content is controlled to be smaller than or equal to 1 mg/L, and then an electrodeposition process is executed to prepare the electric zinc. By means of the method, the problem of gypsum crystallization in the reverse extraction process is solved from a source, and stable running of the process is facilitated; and meanwhile, the process solves the problem in reusing of high-cadmium zinc-contained waste water, and is of great significance in perfecting and popularizing a process for treating lead and silver slag through a mineral separation method.
Description
Technical field
The invention belongs to electrolytic industry technical field, particularly to a kind of from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method.
Background technology
Adopting roasting, leaching, purification and electrodeposition process to process in the production process of zinc sulfide concentrates, lead contained in concentrate and silver are generally enriched in lead smelting gas (or being called hot acid leached mud).For Qian Xin joint enterprise, this lead smelting gas can be delivered to plumbous flow process of smelting as lead-containing material and carry out the recycling of valuable component；But for independent zinc abstraction enterprise, beneficiating method processes lead smelting gas and obtains silver preparation concentrate, it is possible to reclaiming silver-colored and plumbous more easily, its flow process is short, and cost of investment is low, has significant economic benefit.
Beneficiating method processes in the process of lead smelting gas, and water-soluble zinc contained in slag enters milltailings water therewith；Along with the reuse of milltailings water, in tailing water, zinc concentration can build up；Therefore, how to reclaim the water solublity zinc in milltailings water, and eliminate the water solublity zinc adverse effect to ore dressing recovery silver process index, be a problem demanding prompt solution.Solution to this problem, one to consider how the recovery valuable constituent zinc of economical rationality, also to avoid zinc recovering technique in tailing water reuse process that ore dressing carries the negative effect of silver flow process simultaneously.
For the zinc in recycle-water solution, alternative technique has the sedimentation method, absorption/ion exchange/membrane separation process, evaporative crystallization method and extraction etc.；Wherein the sedimentation method need to consume precipitant sodium hydroxide or sodium sulfide (CN201110446312), and it is relatively costly, and can cause sodium ion accumulation in loop tail mineral water；And adsorb/ion exchange/membrane separation process, evaporative crystallization method running cost high, without economic advantages；Comparatively speaking, adopting extracting process, the extractant especially with cation exchange property can realize the extraction of zinc ion, and and then can from strip liquor electrodeposition output electricity zinc；The raffinate formed after extracting containing zinc tailing water returns beneficiation flowsheet；The strip liquor that back extraction obtains carries out electrolytic deposition and produces electricity zinc, and the waste electrolyte that electrodeposition produces is for back extraction；This flow process can effectively realize the closed cycle of aqueous phase solution, has technical reasonability.
Extraction and recovery zinc-base this employing acidic organophosphorus extractant from solution at present, di-(2-ethylhexyl)phosphoric acid (trade name P204), such as Chinese patent CN101041520 and CN1837380；Owing to the chemical property of zinc and cadmium is close, usual association, process all kinds of slags that zinc sulfide concentrates process produces and zinc-containing water all in various degree containing inpurity cadmium, and other affects the impurity of zinc electrolysis deposition current efficiency；Before carrying out electrolytic deposition, all kinds of foreign ions in solution must carry out deep purifying, to ensure being normally carried out of electrowinning zinc；In production practices in common demands electrolyte Cd less than 2mg/L or lower；For extraction and recovery zinc, the zinc-containing solution for electrolysis needs also exist for purifying, to meet in electrolyte the requirement to impurity content.
The deep purifying of zinc-containing solution is generally adopted two kinds of methods, and one is zinc dust precipitation (zinc powder consumption is significantly larger than theoretical amount), then is increase washing section at extraction process to strengthen the washing elimination of foreign ion in load organic phases；As, in Chinese patent CN1837380, solution is 10.67g/L containing Zn, impurity Cd is 132.6mg/L；This solution adopts zinc dust precipitation elimination Cd, and zinc powder consumption is 1.5 ~ 4 times of theoretical amount；After displacement removes Cd, liquid adopts P204 to extract, and after three grades of extractions, two-stage washing impurity-removing, two-stage back extractions, after back extraction, liquid is 1.4mg/L containing Cd, can meet the requirement of electrowinning zinc；In the extraction production practices of Namibia SkorpionZn, its aqueous phase liquid is about 38g/L containing Zn, and impurity Cd is approximately 330mg/L, and its extracting operation condition is level Four extraction, three grades of washing impurity-removings, two-stage back extractions, containing Cd less than 0.01mg/L in the electrolyte obtained, to meet the requirement of electrowinning zinc；In washing impurity-removing process, aqueous phase generally uses containing zinc and the strip liquor containing aqueous acid and part peracid high zinc content；The content of impurity such as cadmium is more high, then the progression of corresponding washing impurity-removing requires more many, and requirement of strength is more big.
But the method for extraction and recovery zinc from the milltailings water of zinc hydrometallurgy lead smelting gas, there is presently no open report；Comparatively speaking, from lead smelting gas milltailings water, extraction and recovery zinc difficulty is bigger, and one is its foreign ion Cd content high (when Zn is 20g/L, Cd can reach about 1000mg/L)；Two is remain part beneficiation reagent in milltailings water；Three be adopt in Calx and time, extract particularly stripping process and the problem (as patent CN201310106110 adopts cooling down, the method adding crystal seed and active additive removes calcium) of gypsum crystallization easily occur；Therefore developing a kind of method reclaiming zinc in milltailings water high for Cd content is current urgent problem.
Summary of the invention
It is an object of the invention to provide a kind of from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method, utilize residual butyl black powder and Cd2+Mating capability is better than Zn2+Character, reduce Cd2+Extraction quantity in organic facies；Control the intensity of extracting zinc, adopt low-temperature extraction operation, it is suppressed that calcium enters organic facies, adjust Electrolytic conditions simultaneously, adopt the technical conditions of low temperature, low current density and low acid zinc ratio, it is ensured that the surface quality of the current efficiency of electrowinning zinc and electricity zinc and chemical composition, thus output qualified electricity zinc.
The method of the present invention sequentially includes the following steps:
1, pre-filtering: high cadmium is removed suspended solids containing zinc milltailings water filtration, it is thus achieved that aqueous phase liquid；Described high cadmium milltailings water containing zinc is containing zinc 15 ~ 25g/L, containing cadmium 750 ~ 1450mg/L, containing butyl black powder 150 ~ 220mg/L；
2, extract: adopt organic facies that aqueous phase liquid is carried out two-stage countercurrent extraction, it is thus achieved that load organic phases and raffinate；Organic facies is the P204 with sulfonated kerosene dilution, and wherein the volume ratio of P204 is 30 ~ 40%；The volume flow ratio of organic facies and aqueous phase liquid is (1.1 ~ 1.3): 1；
3, washing: the load organic phases after two-stage extraction is carried out two-stage countercurrent washing by the sulfuric acid solution adopting pH to be 2 ~ 3, it is thus achieved that cleaning mixture and washing organic facies；The volume flow ratio of sulfuric acid solution and load organic phases is (4 ~ 6): 1；
4, back extraction: adopt waste electrolyte that washing organic facies is carried out back extraction, it is thus achieved that strip liquor and blank organic facies；Described waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 50 ~ 55g/L, sulfur acid 145 ~ 150g/L；The flow volume ratio of washing organic facies and waste electrolyte is in (4 ~ 5): 1；
5, preparation electricity zinc: strip liquor, after standing, ultrasonic Treatment, air-flotation process and activated carbon deoiling treatment, controls oil content≤1mg/L, subsequently into electrodeposition operation, at low temperature 27 ~ 29 DEG C, low current density 400 ~ 500A/m2Carry out electrodeposition with low acid zinc than under 2.8 ~ 3.2 conditions, make electricity zinc.
In said method, the raffinate that step 2 obtains, after resin oil removing and two-stage activated carbon oil removing, controls oil content≤5mg/L therein, returns beneficiation flowsheet.
In said method, it is 9 ~ 10 to pH that cleaning mixture adds Calx pulp process, is then back to beneficiation flowsheet.
In said method, the strip liquor of step 4 is containing zinc 100 ~ 110g/L,Containing cadmium≤5mg/L.
Above-mentioned sour zinc ratio refers to H in electrolyte2SO4Mass ratio with Zn.
In said method, in step 2, the extraction yield of zinc is 45 ~ 55%.
Above-mentioned blank organic facies returns step 2 and uses as organic facies.
In said method, the waste electrolyte that electrodeposition produces returns step 4 and uses as waste electrolyte.
Principles of the invention and being characterized as being:
(1) extraction carries out in indoor, to aqueous phase liquid, organic facies and extraction cell body without extra heating measures, makes extraction system be naturally held in lower temperature range and carries out, and reduces the extraction of calcium；Extraction process is not neutralized, by the mating reaction of the butyl black powder of residual in aqueous phase liquid with cadmium so that zinc preferentially enters load organic phases；By the competition extraction of zinc with cadmium, calcium, reduce the content of major impurity cadmium and calcium in load organic phases further；
(2) two-stage countercurrent washing temperature is natural temperature, without additional heating measures；Removing, by washing, the aqueous phase liquid carried secretly on the one hand, strengthening load organic phases separates with the degree of depth containing cadma matter aqueous phase liquid, reduces foreign ion cadmium and is carried secretly the amount entering stripping section by physics；Utilize the feature that washing aqueous phase ionic strength is low, calcium dissolubility is big on the other hand, utilize the aqueous phase liquid washed that the calcium in load organic phases is removed, it is achieved the open circuit of low content calcium in load organic phases；
(3) raffinate returns beneficiation flowsheet through oil removing, it is achieved the reuse of water；Washings pulp processes and returns beneficiation flowsheet, it is achieved the reuse of water.
The present invention remains the mating reaction of beneficiation reagent butyl black powder and cadmium by utilizing in beneficiation wastewater, and the extraction conditions of moderate control zinc and extraction yield, extract in two-stage, two-stage washing, one-level back extraction process conditions under obtain the low cadmium strip liquor containing zinc；Extract relative to three grades (or the level Four) of current industrial use, for three grades of washings, two-stage stripping process, greatly reduce equipment investment, the indent amount of organic facies and power consumption, and by adjusting electrodeposition process parameter, qualified electricity zinc can be directly obtained, there is the superiority of Technological Economy in extraction and recovery zinc；Operated by low-temperature extraction, competing of zinc extracts the extraction effectively reducing calcium；Utilize water-washing process to realize the open circuit balance of calcium in load organic phases, from source, solve a difficult problem for gypsum crystallization in stripping process, be conducive to the stable of technique；This technique solves a reuse difficult problem for high cadmium zinc-containing water simultaneously, and to improving and promoting, beneficiating method process lead smelting gas technique is also significant.
Accompanying drawing explanation
Fig. 1 be the present invention from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method flow schematic diagram.
Detailed description of the invention
The equipment filtering employing in the embodiment of the present invention is filter press.
Calcium content≤the 100mg/L of strip liquor in the embodiment of the present invention.
The embodiment of the present invention stand for naturally placing clarification 4.0h, ultrasonic Treatment adopts the ultrasonic grease trap of XC-10CS-V type, process time 2.0h, air-flotation process adopts the bubble that compression air produces diameter about 30 μm by microporous pipe to carry out carrier band oil removing, and the oil removal by air bubbling time is 2.0h；During activated carbon deoiling treatment, activated carbon addition is that every cubic metre of strip liquor adds activated carbon 6kg, strip liquor and activated carbon mixing 30min, and after process, strip liquor oil-containing is less than 1mg/L.
In the embodiment of the present invention, resin oil removing adopts CN-01 resin column removing oil, and the raffinate time of staying in resin column is 2.0h, and after resin column removing oil, the oil content in raffinate is down to below 10ppm；The absorption oil removing of follow-up employing activated-charcoal column, the raffinate time of staying in activated-charcoal column is 30min, and the oil content of raffinate is reduced to below 5mg/L.
In the embodiment of the present invention, the electric zinc of preparation meets national standard GB/T 470-2008Zn99.95 zinc ingot metal standard.
The temperature that in the embodiment of the present invention, two-stage countercurrent extracts controls at 15 ~ 25 DEG C.
In the embodiment of the present invention, the temperature of two-stage countercurrent washing controls at 15 ~ 25 DEG C.
Embodiment 1
1, high cadmium is removed suspended solids containing zinc milltailings water filtration, it is thus achieved that aqueous phase liquid；Described high cadmium milltailings water containing zinc is containing zinc 20g/L, containing cadmium 1200mg/L, containing butyl black powder 180mg/L；Another cupric 0.5mg/L, cobalt 12mg/L, arsenic < 0.06mg/L, antimony < 0.1mg/L, ferrum < 1.0mg/L, calcium 2.3g/L；
2, adopt organic facies that aqueous phase liquid is carried out two-stage countercurrent extraction, it is thus achieved that load organic phases and raffinate；Organic facies is the P204 with sulfonated kerosene dilution, and wherein the volume ratio of P204 is 30%；The volume flow ratio of organic facies and aqueous phase liquid is 1.1:1；The extraction yield of zinc is 45%；
3, the load organic phases after two-stage extraction is carried out two-stage countercurrent washing by the sulfuric acid solution adopting pH to be 2 ~ 3, it is thus achieved that cleaning mixture and washing organic facies；The volume flow ratio of sulfuric acid solution and load organic phases is 4:1；
4, adopt waste electrolyte that washing organic facies is carried out back extraction, it is thus achieved that strip liquor and blank organic facies；Described waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 50g/L, sulfur acid 145g/L；The flow volume ratio of washing organic facies and waste electrolyte is at 4:1；Strip liquor is containing zinc 100g/L,Containing cadmium≤5mg/L；Blank organic facies returns step 2 and uses as organic facies；
5, strip liquor is after standing, ultrasonic Treatment, air-flotation process and activated carbon deoiling treatment, controls oil content≤1mg/L, subsequently into electrodeposition operation, at 27 DEG C, electric current density 400A/m2Carry out electrodeposition with acid zinc than under 2.8 conditions, make electricity zinc；The waste electrolyte that electrodeposition produces returns step 4；
Raffinate, after resin oil removing and two-stage activated carbon oil removing, controls oil content≤5mg/L therein, returns beneficiation flowsheet；
It is 9 ~ 10 to pH that cleaning mixture adds Calx pulp process, is then back to beneficiation flowsheet.
Embodiment 2
Method is with embodiment 1, and difference is in that:
(1) high cadmium milltailings water containing zinc is mainly composed of: containing zinc 25g/L, containing cadmium 1450mg/L, containing butyl black powder 220mg/L；
(2) volume ratio of P204 is 35%；The volume flow ratio of organic facies and aqueous phase liquid is 1.2:1；The extraction yield of zinc is 50%；
(3) sulfuric acid solution pH is 2 ~ 3；The volume flow ratio of sulfuric acid solution and load organic phases is 5:1；
(4) waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 55g/L, sulfur acid 150g/L；The flow volume ratio of washing organic facies and waste electrolyte is at 5:1；Strip liquor is containing zinc 110g/L,Containing cadmium≤5mg/L；
(5) at 29 DEG C, electric current density 500A/m2Electrodeposition is carried out than under 3.2 conditions with acid zinc.
Embodiment 3
Method is with embodiment 1, and difference is in that:
(1) high cadmium milltailings water containing zinc is mainly composed of: containing zinc 15g/L, containing cadmium 750mg/L, containing butyl black powder 150mg/L；
(2) volume ratio of P204 is 40%；The volume flow ratio of organic facies and aqueous phase liquid is 1.3:1；The extraction yield of zinc is 55%；
(3) sulfuric acid solution pH is 2 ~ 3；The volume flow ratio of sulfuric acid solution and load organic phases is 6:1；
(4) waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 52g/L, sulfur acid 148g/L；The flow volume ratio of washing organic facies and waste electrolyte is at 4.5:1；Strip liquor is containing zinc 105g/L,Containing cadmium≤5mg/L；
(5) at 28 DEG C, electric current density 450A/m2Electrodeposition is carried out than under 3.0 conditions with acid zinc.
Embodiment 4
Method is with embodiment 1, and difference is in that:
(1) high cadmium milltailings water containing zinc is mainly composed of: containing zinc 19g/L, containing cadmium 880mg/L, containing butyl black powder 170mg/L；
(2) volume ratio of P204 is 35%；The volume flow ratio of organic facies and aqueous phase liquid is 1.2:1；The extraction yield of zinc is 51%；
(3) sulfuric acid solution pH is 2 ~ 3；The volume flow ratio of sulfuric acid solution and load organic phases is 5:1；
(4) waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 53g/L, sulfur acid 146g/L；The flow volume ratio of washing organic facies and waste electrolyte is at 4.8:1；Strip liquor is containing zinc 108g/L,Containing cadmium≤5mg/L；
(5) at 28 DEG C, electric current density 400A/m2Electrodeposition is carried out than under 2.9 conditions with acid zinc.
Embodiment 5
Method is with embodiment 1, and difference is in that:
(1) high cadmium milltailings water containing zinc is mainly composed of: containing zinc 22g/L, containing cadmium 1340mg/L, containing butyl black powder 200mg/L；
(2) volume ratio of P204 is 35%；The volume flow ratio of organic facies and aqueous phase liquid is 1.2:1；The extraction yield of zinc is 53%；
(3) sulfuric acid solution pH is 2 ~ 3；The volume flow ratio of sulfuric acid solution and load organic phases is 5:1；
(4) waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 54g/L, sulfur acid 148g/L；The flow volume ratio of washing organic facies and waste electrolyte is at 4.6:1；Strip liquor is containing zinc 106g/L,Containing cadmium≤5mg/L；
(5) at 28 DEG C, electric current density 500A/m2Electrodeposition is carried out than under 3.1 conditions with acid zinc.
Claims (6)
1. one kind from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method, it is characterised in that sequentially include the following steps:
(1) pre-filtering: high cadmium is removed suspended solids containing zinc milltailings water filtration, it is thus achieved that aqueous phase liquid；Described high cadmium milltailings water containing zinc is containing zinc 15 ~ 25g/L, containing cadmium 750 ~ 1450mg/L, containing butyl black powder 150 ~ 220mg/L；
(2) extract: adopt organic facies that aqueous phase liquid is carried out two-stage countercurrent extraction, it is thus achieved that load organic phases and raffinate；Organic facies is the P204 with sulfonated kerosene dilution, and wherein the volume ratio of P204 is 30 ~ 40%；The volume flow ratio of organic facies and aqueous phase liquid is (1.1 ~ 1.3): 1；
(3) washing: the load organic phases after two-stage extraction is carried out two-stage countercurrent washing by the sulfuric acid solution adopting pH to be 2 ~ 3, it is thus achieved that cleaning mixture and washing organic facies；The volume flow ratio of sulfuric acid solution and load organic phases is (4 ~ 6): 1；
(4) back extraction: adopt waste electrolyte that washing organic facies is carried out back extraction, it is thus achieved that strip liquor and blank organic facies；Described waste electrolyte is the waste electrolyte of Zinc electrolysis, containing zinc 50 ~ 55g/L, sulfur acid 145 ~ 150g/L；The flow volume ratio of washing organic facies and waste electrolyte is in (4 ~ 5): 1；
(5) preparation electricity zinc: strip liquor, after standing, ultrasonic Treatment, air-flotation process and activated carbon deoiling treatment, controls oil content≤1mg/L, subsequently into electrodeposition operation, at low temperature 27 ~ 29 DEG C, low current density 400 ~ 500A/m2Carry out electrodeposition with low acid zinc than under 2.8 ~ 3.2 conditions, make electricity zinc.
2. according to claim 1 from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method, it is characterized in that raffinate that step (2) obtains is after resin oil removing and two-stage activated carbon oil removing, control oil content≤5mg/L therein, return beneficiation flowsheet.
3. according to claim 1 from high cadmium containing zinc milltailings water extracts zinc the method preparing electricity zinc, it is characterised in that it is 9 ~ 10 that described cleaning mixture adds that Calx pulp processes to pH, is then back to beneficiation flowsheet.
4. according to claim 1 from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method, it is characterised in that the strip liquor of step (4) is containing zinc 100 ~ 110g/L,Containing cadmium≤5mg/L.
5. according to claim 1 from high cadmium containing zinc milltailings water extract zinc and prepare electricity zinc method, it is characterised in that in step (2), the extraction yield of zinc is 45 ~ 55%.
6. according to claim 1 from high cadmium containing zinc milltailings water extracts zinc the method preparing electricity zinc, it is characterised in that described blank organic facies returns step 2 and uses as organic facies.
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| CN112195344A (en) * | 2020-10-18 | 2021-01-08 | 赤峰中色锌业有限公司 | Method for extracting and recovering zinc from high leaching residue flotation tailing water |
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