CN103074499B - Method for producing high-quality copper sulfate through low-pressure oxygen leaching of copper slag - Google Patents
Method for producing high-quality copper sulfate through low-pressure oxygen leaching of copper slag Download PDFInfo
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Abstract
The invention relates to a method for producing high-quality copper sulfate through low-pressure oxygen leaching of copper slag. A copper-bearing material with metallic copper or cuprous oxide content greater than 15wt% serves as a raw material, and the method comprises the steps of copper slag or spongy copper slag pickling of zinc hydrometallurgy. A dilute sulphuric acid solution is adopted for low-pressure oxygen leaching of the raw material, an obtained leachate is subjected to combined crystallization including cooling crystallization and salting-out crystallization, a copper sulfate crystal is obtained after liquid-solid separation, and dried after multistage washing, and copper sulfate meeting requirements of above a premium grade specified in YS/T 94-2007 is obtained.
Description
Technical field
The present invention relates to a kind of copper ashes Low Pressure Oxygen and soak the method for producing high-quality copper sulfate, belong to technical field of wet metallurgy.
Background technology
The method of the copper ashes material production copper sulfate of known employing containing metal copper or Red copper oxide is: 1) copper ashes leaches: copper ashes is directly or indirectly leached with dilute sulphuric acid, filtration obtains copper-bath, comprises high-temperature roasting-conventional lixiviation process, oxygenant or catalyst dissolution method, liquid-phase air oxidation, oxygen pressure lixiviation process, stores up oxidation---conventional lixiviation process.2) leach liquor crystallization: make copper with cupric sulfate pentahydrate form crystallization from solution, comprise condensing crystal method, crystallisation by cooling method, salting-out crystallization method.3) copper sulfate removal of impurities: comprise that thick copper sulfate crystal dissolves removal of impurities, copper sulfate leaching liquid purification and impurity removal again.Known copper ashes is produced copper sulfate method in Table 1.
The known copper ashes of table 1 is produced copper sulfate method relative merits
Mono-kind of patent documentation < < leaches by copper-contained material strengthening the condition adopting in the processing method > > that produces copper sulfate: (1) strengthening is leached: after copper-contained material copper ashes is pulverized with sulphuric acid soln containing sour 160g/l～200g/l, the oxygen of 90% above purity or oxygen-rich air successively add in autoclave, under the leaching pressure process condition of the extraction temperatures of 60 ℃～150 ℃ and 1.0Mpa～1.4Mpa, after in autoclave, through certain hour, strengthening is leached, leach the copper in copper ashes, obtain leach liquor, (2) clarification leach liquor: when leach liquor temperature adds flocculation agent during at 60 ℃～80 ℃, clarify siphon supernatant liquor after 1～5 hour, centrifuging underflow, (3) condensing crystal: the solution after supernatant liquor and underflow filtration is squeezed into thickener, 80 ℃ ± 5 ℃ of temperature controls concentrate, the process of heating fills into supernatant liquor constant volume, when proportion reaches 1.30～1.45, calcium magnesium is removed in press filtration, solution after press filtration proceeds to thickener again and continues to be concentrated into after weighing more than 1.45 solution is proceeded to crystallizer tank, and it is concentrated that 20～35 ℃ of temperature controls carry out crystallization, filtration and secondary crystal, obtains and leach mother liquor, (4) when leaching mother solution C zn
2+, Ccu
2+when reaching certain ratio, mother liquor open circuit is returned into Zn system, reclaim zinc, cadmium.The method leaching efficiency is high, but adopt oxygen to press, leaches---and condensing crystal is produced copper sulfate, exists and leaches pressure too high (1.0～1.4MPa), the concentrated large shortcoming of energy consumption.
Patent documentation < < copper-contained material is exempted from the condition adopting in the method > > of Evaporation preparation copper sulfate: the sulphuric acid soln that (1) is 50～350g/L using concentration is as leaching agent, at 70～100 ℃, by solid-to-liquid ratio, be that 1: 3～8 pairs copper-contained materials leach 0.5～3 hour, obtain slip; (2) slip after the leaching of step (1) gained is filtered at 70～100 ℃, obtain respectively leach liquor and leached mud; (3) step (2) gained leach liquor is adopted to conventional crystallisation by cooling, then through centrifugation, obtain copper sulfate and crystalline mother solution.The method needed copper ashes to store up for some time before leaching, and made itself and the abundant catalytic oxidation of air, and needs are certain stores up place and antiseep facility.
The condition adopting in the production method > > of a patent documentation < < high-purity sulphuric acid copper: A. gets technical grade copper sulfate and is dissolved in ultrapure water, be warmed up to 40-70 ℃, drip sulphur acid for adjusting pH to 1.0-2.0, add hydrogen peroxide under after stirring and dissolving; B. 1:2.5-4.5 in mass ratio of bodied ferric sulfate and ventilation breather are mixed and made into precipitation and complexation agent, by 0.5-2.5% of solution weight, precipitation and complexation agent is joined in above-mentioned insulation solution, the gac that adds again solution weight 0.5-2.5%, stir 3-7 hours, cool to room temperature, standing over night; C. will after above-mentioned solution coarse filtration, use the micro-pore-film filtration of 0.2 μ m, filtrate condensing crystal obtains high-purity sulphuric acid copper again.
Mono-kind of patent documentation < < improves the condition adopting in the production method > > of copper sulfate grade: A, copper sulfate is mixed with to volumn concentration is 30%～50% copper-bath; B, add oxygenant, oxidation time is 10min～40min, and described oxygenant is the mixture of hydrogen peroxide and ammonium persulphate, and the weight percentage of described hydrogen peroxide is 2%～15%, and the weight percentage of ammonium persulphate is 0.05%～0.15%; C, add precipitation agent, under continuous agitation condition, after reaction 0.5h～1h, filter, temperature of reaction and filtration temperature are 25 ℃～55 ℃; Described precipitation agent is the mixture of sodium carbonate and sodium oxalate, and the weight percentage of described sodium carbonate is 3%～7%, and the weight percentage of sodium oxalate is 3%～17%; D, described step C filter the filtrate obtaining and evaporate, and the solution proportion after evaporation is 1.06g/cm3～1.59 g/cm3; E, condensing crystal, the type of cooling adopts gradient cooling cooling, and cooling temperature is at 10 ℃～35 ℃; F, the cooling fluid of described step e is carried out to suction filtration, the suction filtration time is 25min～35min.The copper sulfate product of producing reaches the requirement of industry standard YS/T94-2007 seconds.
Above-mentioned two kinds are removed the impurity method after dissolving by copper sulfate, although can access the copper sulfate product of higher degree, all need to add cleaner, the problem that process is complicated, production cost is high.
Summary of the invention
Object of the present invention is intended to overcome the deficiency of known copper ashes leaching and copper sulfate impurity-removing method, provides a kind of copper ashes Low Pressure Oxygen to soak the method for producing high-quality copper sulfate.The cupric of take is greater than the metallic copper of 15wt% or the copper-contained material of Red copper oxide is raw material, the pickling copper ashes or the sponge copper ashes that comprise zinc hydrometallurgy, adopting dilution heat of sulfuric acid to carry out Low Pressure Oxygen to raw material soaks, the leach liquor obtaining carries out co-crystallization, comprise crystallisation by cooling and salting-out crystallization, after liquid-solid separation, obtain copper sulfate crystal, this crystal is carried out to multistage washing and by super-dry, obtain the above copper sulfate product requiring of YS/T94-2007 top grade product
The present invention implements by following steps
(1) Low Pressure Oxygen soaks: the dilution heat of sulfuric acid that is 100～200g/l by sulfur acid and raw material are 3～12m according to liquid-solid ratio
3/ t mixes, blast oxygen or oxygen-rich air, at 70～85 ℃ of temperature, oxygen partial pressure, be not less than 0.08MPa, total pressure not under the condition higher than 0.3MPa, leach 2～4 hours, and control terminal pH value 1～3, obtain leaching feed liquid, at 80～90 ℃, to leaching feed liquid, filter, obtain respectively leach liquor and leached mud;
(2) co-crystallization: by the leach liquor crystallisation by cooling of step (1) gained, clarified separation goes out a mother liquor of 10%～30% and carries out innoxious open circuit processing, to adding in remaining slurry 98% vitriol oil to make it contain acid, be to carry out salting-out crystallization after 100～200g/l, liquid-solid separation obtains copper sulfate crystal and secondary mother liquid;
(3) multistage washing: the copper sulfate crystal of step (2) gained is carried out to 2～6 grades of washings, and last step washs with clear water, and liquid-solid ratio is 0.8～1.7m
3/ t, the copper/saturated copper sulphate solution that the washing before last step produces with one-level washing is thereafter as washings, and liquid-solid ratio is 1～2m
3/ t, the washing of every one-level is first by copper sulfate crystal and washings mixing post-heating to 70～90 ℃, wait copper sulfate to dissolve completely after crystallisation by cooling again, liquid-solid copper sulfate crystal and the washings isolated.Last step washing gained copper sulfate crystal is final copper sulfate product after super-dry, packing.
Described raw material is that cupric is greater than the metallic copper of 15wt% or the copper-contained material of Red copper oxide, comprises pickling copper ashes or the sponge copper ashes of zinc hydrometallurgy;
Described step (1) gained leached mud returns to other and smelts flow process, for reclaiming other valuable metals;
Described step (2) crystallisation by cooling and salting-out crystallization terminal temperature are 5～30 ℃;
Described step (2) gained secondary mother liquid returns to step (1) and recycles as leaching agent;
Described step (3), when washing first, is washed with clear water, and liquid-solid ratio is 0.8～1.7m
3/ t;
Liquid-solid separate mode in described step (2), (3) is centrifugation or filtration;
The 1st grade of described step (3) washing gained copper/saturated copper sulphate washings returns to Low Pressure Oxygen and soaks as leaching agent and recycle.
Tool of the present invention has the following advantages and effect:
(1), without high-temperature roasting or store up, without adding oxygenant or catalyzer, adopt lower pressure to reach direct
The object that leaches copper ashes, leaching yield reaches more than 95%.
(2) without condensing crystal, crystallisation by cooling is combined with salting-out crystallization and use raising percent crystallization in massecuite to reach more than 76%,
Copper sulfate saving per ton concentrates energy consumption 490kgce/t.
(3) without adding cleaner, product purity is high, can reach the above requirement of YS/T94-2007 top grade product.
Accompanying drawing explanation
Fig. 1 process flow sheet of the present invention.
The multistage washing process schema of Fig. 2 step of the present invention (3) (the 3 grades of washings of take are example).
Embodiment
embodiment 1
(1) copper ashes 1t zinc hydrometallurgy being produced is as being willing to material, copper mainly exists with Red copper oxide form, and the mass percent of its main chemical is Cu 25.0wt%, Pb 20.0 wt %, Zn 4.8 wt % are 4m with containing sour 135g/l dilution heat of sulfuric acid according to liquid-solid ratio
3/ t mixing is encased in 5m
3pressurized vessel in, at 80 ℃, blast volume oxygen level and be 99.5% oxygen, keeping oxygen partial pressure in pressurized vessel is 0.2Mpa, total pressure 0.25MPa, extraction time 2 hours, terminal pH value 2.0, obtains leaching feed liquid, uses Filter Press at 80 ℃, obtain respectively leach liquor and leached mud, leached mud gives other to smelt flow process and reclaims other valuable metals.Leaching yield is 95.6%.
(2) leach liquor of step (1) gained is joined to 4m
3crystallization kettle, to passing into cooling circulating water in the cooling jacket of crystallization kettle, carry out crystallisation by cooling, 25 ℃ of crystallisation by cooling terminal temperatures, clarified separation goes out a mother liquor of 25% and carries out innoxious open circuit processing, to residue slurry, add 98% vitriol oil to make it contain salting-out crystallization after sour 127g/l, 25 ℃ of salting-out crystallization terminal temperatures, obtain copper sulfate crystal and secondary mother liquid with drier centrifugation, and gained secondary mother liquid returns to step (1) and recycles as leaching agent.Percent crystallization in massecuite 76.5%.
(3) copper sulfate crystal of step (2) gained is carried out to 4 grades of washings, the 4th grade is washed with clear water, and liquid-solid ratio is 1m
3/ t, the 1st, 2,3 grades of washings use the copper/saturated copper sulphate solution of the generation of one-level washing thereafter as washings, and liquid-solid ratio is 1.2m
3/ t, clear water when washing first, the washing of every one-level is at 5m by copper sulfate crystal and washings
3rinse bath in mix post-heating to 80 ℃, after dissolving completely Deng copper sulfate crystal, to the spiral coil cooling tube in rinse bath, pass into cooling circulating water again and carry out crystallisation by cooling, crystallisation by cooling terminal temperature is 25 ℃, with drier centrifugation, go out copper sulfate crystal and washings, the 1st grade of washing gained copper/saturated copper sulphate washings returns to step (1) and recycles as leaching agent, and the 4th grade of washing gained copper sulfate crystal is final copper sulfate product after super-dry, packing.The purity of gained copper sulfate product is: Cu
2sO
4.5H
2o 99.02%, Zn 0.002%, Cd 0.0004%, Co 0.0006%, Ni 0.0003%, Fe 0.002%, As 0.0005%, Sb < 0.001%, Ca 0.0008%, Pb < 0.001%, Bi < 0.001%, Cl < 0.001% and water-insoluble 0.005%.Reach YS/T94-2007 top grade product specification of quality.
embodiment 2
(1) 100g sponge copper ashes is expected for being willing to, copper mainly exists with metallic copper form, and the mass percent of its main chemical is Cu 75.4wt%, Zn 10.2 wt %, and Pb 1.5 wt % are 10m with containing sour 160g/l dilution heat of sulfuric acid according to liquid-solid ratio
3/ t mixing is encased in the pressurized vessel of 2L, at 75 ℃, blast volume oxygen level and be 30% oxygen-rich air, keeping oxygen partial pressure in pressurized vessel is 0.08Mpa, total pressure 0.3MPa, leach 4 hours, terminal pH value 1.5, obtains leaching feed liquid, vacuum filtration at 85 ℃, obtain respectively leach liquor and leached mud, leached mud returns to other smelting flow processs and reclaims other valuable metals.Leaching yield 95.8%.
(2) the beaker splendid attire with 800ml by the leach liquor of step (1) gained, standing crystallisation by cooling, 18 ℃ of crystallisation by cooling terminal temperatures, clarified separation goes out 16% mother liquor and carries out innoxious open circuit processing, to residue slip, add 98% vitriol oil to make it contain salting-out crystallization after sour 130g/l, 18 ℃ of salting-out crystallization terminal temperatures, vacuum filtration obtains copper sulfate crystal and secondary mother liquid, and gained secondary mother liquid returns to step (1) and recycles as leaching agent.Percent crystallization in massecuite 78.0%.
The copper sulfate crystal of step (2) gained is carried out to 3 grades of washings, and 3rd level washs with clear water, and liquid-solid ratio is 1.2m
3/ t, the 1st, 2 grades of washings use the copper/saturated copper sulphate solution of the generation of one-level washing thereafter as washings, and liquid-solid ratio is 1.5m
3/ t, clear water when washing first, the washing of every one-level is that crystal is mixed to post-heating to 85 ℃ with washings in the beaker of 500ml, standing crystallisation by cooling again after dissolving completely in copper sulfate, crystallisation by cooling terminal temperature is 18 ℃, isolated by vacuum filtration goes out copper sulfate crystal and washings, and the 1st grade of washing gained copper/saturated copper sulphate washings returns to step (1) and recycle as leaching agent, and 3rd level washing gained copper sulfate crystal is final copper sulfate product after super-dry, packing.The purity of gained copper sulfate product is: Cu
2sO
4.5H
2o 99.10%, Zn0.001%, Cd0.0002%, Co0.0005%, Ni0.0002%, Fe0.001%, As0.0003%, Sb < 0.001%, Ca0.0007%, Pb < 0.001%, Bi < 0.001%, Cl < 0.001% and water-insoluble 0.004%.Reach YS/T94-2007 top grade product specification of quality.
Claims (3)
1. a copper ashes Low Pressure Oxygen soaks the method for producing high-quality copper sulfate, cupric is greater than to the zinc hydrometallurgy pickling copper ashes of 15wt% or sponge copper ashes as raw material, through Low Pressure Oxygen, soak, co-crystallization, comprise crystallisation by cooling and salting-out crystallization, described salting-out crystallization, the secondary mother liquid that liquid-solid separation obtains returns to Low Pressure Oxygen and soaks as leaching agent and recycle, carry out again multistage washing, in described multistage washing the 1st grade washing gained copper/saturated copper sulphate washings returns to Low Pressure Oxygen and soaks as leaching agent and recycle, last step washing gained copper sulfate crystal is through super-dry, after packing, be copper sulfate product,
It is characterized in that:
It is by sulfur acid, to be 100～200g/l dilution heat of sulfuric acid is that 3～12m3/t mixes with raw material according to liquid-solid ratio that described Low Pressure Oxygen soaks, blast oxygen or oxygen-rich air, at 70～85 ℃ of temperature, oxygen partial pressure, be not less than 0.08MPa, total pressure not under the condition higher than 0.3MPa, leach 2～4 hours, and control terminal pH value 1～3, obtain leaching feed liquid, at 80～90 ℃, to leaching feed liquid, filter, obtain respectively leach liquor and leached mud;
Described co-crystallization is Low Pressure Oxygen to be soaked to the leach liquor crystallisation by cooling of gained, clarified separation goes out a mother liquor of 10%～30% and carries out innoxious open circuit processing, to adding in remaining slurry 98% vitriol oil to make it contain acid, be to carry out salting-out crystallization after 100～200g/l, liquid-solid separation obtains copper sulfate crystal and secondary mother liquid;
Described multistage washing is that the copper sulfate crystal of gained is carried out to 2～6 grades of washings, and last step washs with clear water, and liquid-solid ratio is 0.8～1.7 m
3/ t, the copper/saturated copper sulphate solution that the washing before last step produces with one-level washing is thereafter as washings, and liquid-solid ratio is 1～2 m
3/ t, the washing of every one-level is first by copper sulfate crystal and washings mixing post-heating to 70～90 ℃, wait copper sulfate to dissolve completely after crystallisation by cooling again, liquid-solid copper sulfate crystal and the washings isolated.
2. copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate and it is characterized in that: described crystallisation by cooling and salting-out crystallization terminal temperature are 5～30 ℃.
3. copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate and it is characterized in that: in described multistage washing, when washing first, with clear water, wash, liquid-solid ratio is 0.8～1.7 m
3/ t.
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| CN104131171B (en) * | 2014-07-28 | 2017-02-15 | 蒙自矿冶有限责任公司 | Method for producing copper sulfate pentahydrate by combination of zinc and copper systems based on chlorine removal as link |
| CN104711431B (en) * | 2015-03-27 | 2017-09-26 | 云南驰宏锌锗股份有限公司 | A kind of method that copper dross slag produces copper sulphate |
| CN104846204B (en) * | 2015-06-10 | 2017-05-31 | 云南驰宏锌锗股份有限公司 | A kind of method that copper is efficiently leached under zinc abstraction copper ashes normal pressure |
| CN104911369B (en) * | 2015-06-29 | 2017-05-10 | 郴州市金贵银业股份有限公司 | Method for processing high-copper-silver smelting slag |
| CN107140675B (en) * | 2017-07-06 | 2019-05-14 | 华南理工大学 | A kind of energy-saving copper sludge recycling prepares the device of copper sulphate |
| CN111011395A (en) * | 2019-12-20 | 2020-04-17 | 武汉昊泽环保科技有限公司 | Bactericide for industrial sewage treatment and processing method thereof |
| CN114107670B (en) * | 2021-11-24 | 2023-07-25 | 白银有色集团股份有限公司 | Method for recycling copper sulfate crystals from waste copper slag |
| CN115927847A (en) * | 2022-11-03 | 2023-04-07 | 核工业北京化工冶金研究院 | Method for leaching beryllium in bertrandite-type beryllium ore |
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| JPS6035415B2 (en) * | 1982-10-20 | 1985-08-14 | 日本鉱業株式会社 | Separation method for copper and arsenic |
| CN1168662C (en) * | 2001-09-03 | 2004-09-29 | 贾荣宝 | Wet low-temperature oxidation and decomposition process of producing active copper oxide |
| CN1255561C (en) * | 2003-11-13 | 2006-05-10 | 河北科技大学 | Method for preparing copper sulfate using copper concentrate |
| CN102633293B (en) * | 2012-05-04 | 2014-07-02 | 昆明理工大学 | Method for refining multistage circulation evaporation-free copper sulfate |
| CN102876903A (en) * | 2012-10-08 | 2013-01-16 | 来宾华锡冶炼有限公司 | Direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues |
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