CN103074499A - 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 the copper sulfate method and is seen Table 1.
The known copper ashes of table 1 is produced copper sulfate method relative merits
The condition that adopts in the patent documentation " a kind of processing method of copper-contained material strengthen to leach being produced copper sulfate ": (1) is strengthened and is leached: after the copper-contained material copper ashes is pulverized with contain the sulphuric acid soln of sour 160g/l～200g/l, oxygen or the oxygen-rich air of 90% above purity successively adds in the autoclave, under the leaching pressure process condition of 60 ℃～150 ℃ extraction temperatures and 1.0Mpa～1.4Mpa, after the process certain hour is strengthened leaching in autoclave, leach the copper in the copper ashes, obtain leach liquor; (2) clarification leach liquor: when the leach liquor temperature adds flocculation agent during at 60 ℃～80 ℃, clarify siphon supernatant liquor after 1～5 hour, the centrifuging underflow; (3) condensing crystal: the solution after supernatant liquor and the underflow filtration is squeezed into thickener, 80 ℃ ± 5 ℃ of temperature controls concentrate, the process of heating fills into the supernatant liquor constant volume, when proportion reaches 1.30～1.45, calcium magnesium is removed in press filtration, solution after the press filtration changes thickener over to again and continues to be concentrated into after weighing more than 1.45 and change solution over to crystallizer tank, and it is concentrated that 20～35 ℃ of temperature controls carry out crystallization, filtration and secondary crystal, obtains to leach mother liquor; (4) when leaching mother solution C zn
2+, Ccu
2+When reaching certain ratio, the mother liquor open circuit is returned into Zn system, reclaim zinc, cadmium.The method leaching efficiency is high, leaches but adopt oxygen to press---condensing crystal is produced copper sulfate, exist leach pressure too high (1.0～1.4MPa), the concentrated large shortcoming of energy consumption.
The condition that adopts in the patent documentation " non-evaporating method for preparing copper sulfate of a kind of copper-contained material ": (1) is that the sulphuric acid soln of 50～350g/L is as leaching agent with concentration, under 70～100 ℃, be that 1: 3～8 pairs copper-contained materials leached 0.5～3 hour by solid-to-liquid ratio, obtain slip; (2) slip after the leaching of step (1) gained is filtered under 70～100 ℃, obtain respectively leach liquor and leached mud; (3) step (2) gained leach liquor is adopted conventional crystallisation by cooling, again through centrifugation, namely obtain copper sulfate and crystalline mother solution.The method needed copper ashes is stored 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 that adopts in the patent documentation " a kind of production method of high-purity sulphuric acid copper ": A. gets technical grade copper sulfate and is dissolved in the ultrapure water, is warmed up to 40-70 ℃, drips sulphur acid for adjusting pH to 1.0-2.0, the lower hydrogen peroxide that adds after the stirring and dissolving; B. the in mass ratio 1:2.5-4.5 with bodied ferric sulfate and ventilation breather is mixed and made into the precipitation and complexation agent, by 0.5-2.5% of solution weight the precipitation and complexation agent joined in the above-mentioned insulation solution, the gac that adds again solution weight 0.5-2.5%, stirred 3-7 hours, cool to room temperature, hold over night; C. will use the micro-pore-film filtration of 0.2 μ m after the mentioned solution coarse filtration, the filtrate condensing crystal obtains high-purity sulphuric acid copper again.
The condition that adopts in the patent documentation " a kind of production method that improves the copper sulfate grade ": A, copper sulfate is mixed with volumn concentration is 30%～50% copper-bath; B, adding 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, adding precipitation agent under continuous agitation condition, behind reaction 0.5h～1h, filter, and temperature of reaction and filtration temperature are 25 ℃～55 ℃; Described precipitation agent is the mixture of yellow soda ash and sodium oxalate, and the weight percentage of described yellow soda ash is 3%～7%, and the weight percentage of sodium oxalate is 3%～17%; D, described step C filter the filtrate that obtains and evaporate, and the solution proportion after the evaporation is 1.06g/cm3～1.59 g/cm3; E, condensing crystal, the type of cooling adopt the gradient cooling cooling, and cooling temperature is at 10 ℃～35 ℃; F, the cooling fluid of described step e is carried out 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 with the impurity method of copper sulfate after except dissolving, 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
Purpose 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.Take cupric greater than the copper-contained material of the metallic copper of 15wt% or Red copper oxide as raw material, the pickling copper ashes or the sponge copper ashes that comprise zinc hydrometallurgy, adopting dilution heat of sulfuric acid that raw material is carried out Low Pressure Oxygen soaks, the leach liquor that obtains carries out co-crystallization, comprise crystallisation by cooling and salting-out crystallization, obtain copper sulfate crystal after the liquid-solid separation, this crystal is carried out multistage washing namely get the above copper sulfate product that requires of YS/T94-2007 top grade product by super-dry
The present invention implements by following steps
(1) Low Pressure Oxygen soaks: be that dilution heat of sulfuric acid and the raw material of 100～200g/l is 3～12m according to liquid-solid ratio with sulfur acid
3/ t mixes, blast oxygen or oxygen-rich air, be not less than under the condition that 0.08MPa, total pressure be not higher than 0.3MPa at 70～85 ℃ of temperature, oxygen partial pressure, leached 2～4 hours, and control terminal point pH value 1～3, obtain leaching feed liquid, under 80～90 ℃, filter leaching feed liquid, obtain respectively leach liquor and leached mud;
(2) co-crystallization: with the leach liquor crystallisation by cooling of step (1) gained, clarified separation goes out a mother liquor of 10%～30% to carry out innoxious open circuit and processes, adding 98% vitriol oil in the remaining slurry, to make it contain acid be to carry out salting-out crystallization behind 100～200g/l, and 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 2～6 grades of washings, and last step washs with clear water, and liquid-solid ratio is 0.8～1.7m
3Washing before the/t, last step uses the copper/saturated copper sulphate solution of thereafter one-level washing generation as washings, and liquid-solid ratio is 1～2m
3/ t, the washing of every one-level is first with copper sulfate crystal and washings mixing post-heating to 70～90 ℃, wait copper sulfate to dissolve fully 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 be cupric greater than the metallic copper of 15wt% or the copper-contained material of Red copper oxide, comprise pickling copper ashes or the sponge copper ashes of zinc hydrometallurgy;
Described step (1) gained leached mud returns other and smelts flow process, is used 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 step (1) and recycles as leaching agent;
Described step (3) is washed with clear water when washing first, 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 Low Pressure Oxygen and soaks as leaching agent and recycle.
The present invention has following advantage and effect:
(1) need not high-temperature roasting or store up, need not to add oxygenant or catalyzer, adopt lower pressure to reach direct
Leach the purpose of copper ashes, leaching yield reaches more than 95%.
(2) need not condensing crystal, crystallisation by cooling and salting-out crystallization united to use improve percent crystallization in massecuite and reach more than 76%,
Copper sulfate saving per ton concentrates energy consumption 490kgce/t.
(3) need not to add cleaner, product purity is high, can reach the above requirement of YS/T94-2007 top grade product.
Description of drawings
Fig. 1 process flow sheet of the present invention.
The multistage washing process schema of Fig. 2 step of the present invention (3) (take 3 grades of washings as example).
Embodiment
Embodiment 1
(1) copper ashes that the 1t zinc hydrometallurgy is produced is as being willing to material, copper mainly exists with the 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, under 80 ℃, blast the volume oxygen level and be 99.5% oxygen, keep that oxygen partial pressure is 0.2Mpa in the pressurized vessel, total pressure 0.25MPa, extraction time 2 hours, terminal point pH value 2.0 obtains leaching feed liquid, at 80 ℃ of lower Filter Press of using, 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 with step (1) gained joins 4m
3Crystallization kettle, pass into cooling circulating water in the cooling jacket of crystallization kettle and carry out crystallisation by cooling, 25 ℃ of crystallisation by cooling terminal temperatures, clarified separation goes out a mother liquor of 25% to carry out innoxious open circuit and processes, adding 98% vitriol oil to the residue slurry makes it contain salting-out crystallization behind the sour 127g/l, 25 ℃ of salting-out crystallization terminal temperatures obtain copper sulfate crystal and secondary mother liquid with the drier centrifugation, and the gained secondary mother liquid returns step (1) and recycles as leaching agent.Percent crystallization in massecuite 76.5%.
(3) copper sulfate crystal with step (2) gained carries out 4 grades of washings, and the 4th grade with clear water washing, and liquid-solid ratio is 1m
3/ t, the copper/saturated copper sulphate solution of the 1st, 2,3 grade of thereafter one-level washing of washing usefulness generation is as washings, and liquid-solid ratio is 1.2m
3/ t uses clear water when washing first, the washing of every one-level is at 5m with copper sulfate crystal and washings
3Rinse bath in mix post-heating to 80 ℃, after dissolving fully Deng copper sulfate crystal, spiral coil cooling tube in the rinse bath passes into cooling circulating water and carries out crystallisation by cooling again, the crystallisation by cooling terminal temperature is 25 ℃, go out copper sulfate crystal and washings with the drier centrifugation, the 1st grade of washing gained copper/saturated copper sulphate washings returns 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 the requirement of YS/T94-2007 top grade product quality.
Embodiment 2
(1) 100g sponge copper ashes is expected that for being willing to copper mainly exists with the metallic copper form, 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, under 75 ℃, blast the volume oxygen level and be 30% oxygen-rich air, keep that oxygen partial pressure is 0.08Mpa in the pressurized vessel, total pressure 0.3MPa, leached 4 hours, terminal point pH value 1.5 obtains leaching feed liquid, at 85 ℃ of lower vacuum filtrations, obtain respectively leach liquor and leached mud, leached mud returns other smelting flow processs and reclaims other valuable metals.Leaching yield 95.8%.
(2) with the leach liquor of step (1) the gained beaker splendid attire with 800ml, leave standstill crystallisation by cooling, 18 ℃ of crystallisation by cooling terminal temperatures, clarified separation goes out 16% mother liquor and carries out innoxious open circuit processing, adding 98% vitriol oil to the residue slip makes it contain salting-out crystallization behind the sour 130g/l, 18 ℃ of salting-out crystallization terminal temperatures, vacuum filtration obtains copper sulfate crystal and secondary mother liquid, and the gained secondary mother liquid returns step (1) and recycles as leaching agent.Percent crystallization in massecuite 78.0%.
The copper sulfate crystal of step (2) gained is carried out 3 grades of washings, and 3rd level washs with clear water, and liquid-solid ratio is 1.2m
3/ t, the copper/saturated copper sulphate solution of the 1st, 2 grade of thereafter one-level washing of washing usefulness generation is as washings, and liquid-solid ratio is 1.5m
3/ t, when washing first, use clear water, the washing of every one-level is that crystal and washings are mixed post-heating to 85 ℃ in the beaker of 500ml, leave standstill again crystallisation by cooling after dissolving fully in copper sulfate, the 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 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 the requirement of YS/T94-2007 top grade product quality.
Claims (7)
1. a copper ashes Low Pressure Oxygen soaks the method for producing high-quality copper sulfate, and it is characterized in that: it is implemented according to the following steps,
(1) Low Pressure Oxygen soaks: with sulfur acid be the dilution heat of sulfuric acid of 100～200g/l and raw material according to liquid-solid ratio be 3～
12m
3/ t mixes, blast oxygen or oxygen-rich air, be not less than under the condition that 0.08MPa, total pressure be not higher than 0.3MPa at 70～85 ℃ of temperature, oxygen partial pressure, leached 2～4 hours, and control terminal point pH value 1～3, obtain leaching feed liquid, under 80～90 ℃, filter leaching feed liquid, obtain respectively leach liquor and leached mud;
(2) co-crystallization: with the leach liquor crystallisation by cooling of step (1) gained, clarified separation goes out 10%～30%
Mother liquor carries out innoxious open circuit to be processed, and adding 98% vitriol oil in the remaining slurry, to make it contain acid be to carry out salting-out crystallization behind 100～200g/l, and 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 2～6 grades of washings, and last step washs with clear water, and liquid-solid ratio is 0.8～1.7m
3Washing before the/t, last step uses the copper/saturated copper sulphate solution of thereafter one-level washing generation as washings, and liquid-solid ratio is 1～2m
3/ t, the washing of every one-level is first with copper sulfate crystal and washings mixing post-heating to 70～90 ℃, Deng copper sulfate dissolve fully after crystallisation by cooling again, liquid-solid copper sulfate crystal and the washings isolated, last step washing gained copper sulfate crystal is the copper sulfate product after super-dry, packing.
2. a kind of copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate, it is characterized in that: described raw material be cupric greater than the metallic copper of 15wt% or the copper-contained material of Red copper oxide, comprise pickling copper ashes or the sponge copper ashes of zinc hydrometallurgy.
3. a kind of 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 ℃.
4. a kind of copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate, it is characterized in that: described salting-out crystallization, the secondary mother liquid that liquid-solid separation obtains return Low Pressure Oxygen and soak as leaching agent and recycle.
5. a kind of copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate, and it is characterized in that: when washing first, wash with clear water in the described multistage washing, liquid-solid ratio is 0.8～1.7m
3/ t.
6. a kind of copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate, and it is characterized in that: the liquid-solid separate mode in described co-crystallization and the multistage washing is centrifugation or filtration.
7. a kind of copper ashes Low Pressure Oxygen according to claim 1 soaks the method for producing high-quality copper sulfate, it is characterized in that: the 1st grade of washing gained copper/saturated copper sulphate washings in the described multistage washing returns Low Pressure Oxygen and soaks as leaching agent and recycle.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131171A (en) * | 2014-07-28 | 2014-11-05 | 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 |
| CN104711431A (en) * | 2015-03-27 | 2015-06-17 | 云南驰宏锌锗股份有限公司 | Method for producing copper sulfate from copper scum |
| CN104846204A (en) * | 2015-06-10 | 2015-08-19 | 云南驰宏锌锗股份有限公司 | Method of efficiently leaching copper from zinc smelting copper slag at atmosphere pressure |
| CN104911369A (en) * | 2015-06-29 | 2015-09-16 | 郴州市金贵银业股份有限公司 | Method for processing high-copper-silver smelting slag |
| CN107140675A (en) * | 2017-07-06 | 2017-09-08 | 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 |
| CN114107670A (en) * | 2021-11-24 | 2022-03-01 | 白银有色集团股份有限公司 | Method for recovering 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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| 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 |
| CN114107670A (en) * | 2021-11-24 | 2022-03-01 | 白银有色集团股份有限公司 | Method for recovering 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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