CN101824541B - Treatment method of wet method zinc smelting by-products - Google Patents
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Abstract
The invention discloses a treatment method of wet method zinc smelting by-products, which comprises the following steps: firstly, using a sulfuric acid solution for leaching heat treated copper-cadmium slag or copper-rich slag; then, using an organic solvent extraction method for extracting copper and cadmium at the same time from leach liquor to obtain copper-cadmium-rich organic phase zinc-sulfate-containing faffinate; using sulphuric acid for carrying out back extraction on the copper-cadmium-rich organic phase to obtain a mixed solution of copper sulfate and cadmium sulfate; then, adding a proper amount of organic precipitant into the mixed solution to obtain a mixture of organic precipitates of the copper and the cadmium; separating and washing the copper and cadmium precipitates; and adding a reducing agent solution for carrying out reduction reaction to respectively obtain sheet type copper powder and organic cadmium products. The invention realizes the value adding utilization of wet method zinc smelting by-products, reduces the treatment cost of the zinc smelting by-products, and reaches the goals of discharge reduction and yield improvement.
Description
Technical field
The present invention relates to a kind of treatment process of zinc hydrometallurgy by product, belong to nonferrous metal resource comprehensive utilization and environmental protection technical field.Be particularly related to a kind of from the zinc hydrometallurgy process copper-cadmium slag of output or the incrementization of copper ashes utilize method.
Technical background
In recent years, China's zinc metallurgy industrial development is rapid, and output occupies the first in the world for years, and wherein the output of zinc hydrometallurgy accounts for more than 70% of zinc ultimate production.In the zinc hydrometallurgy process, in order to obtain high-quality metallic zinc, and, reduce power consumption in order to improve current efficiency, before electrolysis, need the foreign ion Cu in the electrolytic solution, Cd, Ni, purifications such as Co are removed.The general two sections method of replacement of zinc powder that adopt are removed Cu in the industrial production, Cd and Ni, and Co, output contains the copper-cadmium slag and the nickel cobalt slag of a large amount of metallic zinc respectively.Usually contain Cu 1.5%～5% in the copper-cadmium slag, Zn 28%～50%, and Cd 5%～10%.If main valuable metal is all recycled in the copper-cadmium slag, for enterprise will produce huge economic benefit and solve stack and transport process in the environmental problem that produced, so it is significant to reclaim in the copper-cadmium slag valuable metal.In recent years, researchist's key issue that valuable metal reclaims in the copper-cadmium slag has proposed technological methods such as pressurized acid leaching method, ammonia leaching process, microbial leaching method.The pressurized acid leaching method is carried out under High Temperature High Pressure, to having relatively high expectations of equipment, is unfavorable for industrialized widespread use; Ammonia leaching process and microbial leaching method etc. then are difficult to be connected with existing copper-cadmium slag system for handling.The large-scale zinc of present domestic part smeltery only carries out roughing out to copper-cadmium slag, and Tathagata punch refinery at first leaches zinc, cadmium, leaches rear filtrate and send the production of cadmium recovery process thick cadmium, and the copper ashes of Jin Chuing is not directly sold.Also contain cadmium about 3% and about 20% zinc in the copper ashes, the recovery of subsequent copper is brought disadvantageous effect.Also have producer that copper-cadmium slag is directly sent into rotary kiln and handle, the cadmium volatilization enters zinc oxide fumes.When leaching zinc oxide fumes, cadmium dissolves again, and cadmium does not obtain reclaiming in this process, just at system's internal recycle, repeats consumption acid, and the consumption zinc powder increases the cost of producing zinc per ton.As a whole, contain the existing complex treatment process of zinc copper-cadmium slag or copper ashes, long processing period, needed chemical feedstocks kind and equipment are many, and middle by-product secondary material is many, and the zinc consumption amount is big, the cumulative metallic zinc is many in the Production Flow Chart, and can only produce thick level such as copper, zinc, cadmium product.If these zinc metallurgy intermediate products can be used, prepare the flake copper of high added value, organic cadmium, organic zinc product, then can realize the increment utilization of zinc hydrometallurgy by product, reduce the processing cost of zinc smelting byproducts, realize reducing discharging increasing income.
Summary of the invention
The treatment process that the purpose of this invention is to provide a kind of zinc hydrometallurgy by product, with zinc hydrometallurgy intermediate product copper-cadmium slag or copper ashes is raw material, the fine product of preparation copper, cadmium, zinc, realize the increment utilization of zinc hydrometallurgy by product, reduce the processing cost of zinc smelting byproducts, reach the purpose that reduction of discharging increases income.
The objective of the invention is to realize by following scheme:
A kind of treatment process of zinc hydrometallurgy by product: the copper-cadmium slag or the rich copper ashes that at first leach output in the zinc hydrometallurgy process with sulphuric acid soln, use method while extracting copper and cadmium from leach liquor of organic extraction then, and obtain the mixing solutions of copper sulfate and Cadmium Sulphate with the sulfuric acid back extraction, in mixing solutions, add organic precipitant, obtain the mixture of copper, cadmium organic deposition; After separating this copper, cadmium throw out and washing, add reductant solution and carry out reduction reaction, obtain flake copper and organic cadmium product respectively.
Specifically may further comprise the steps:
(1) copper-cadmium slag or rich copper ashes earlier in air atmosphere under 250～300 ℃ of temperature thermal treatment 1～6h;
(2) copper-cadmium slag after the thermal treatment or rich copper ashes join in the sulphuric acid soln, carry out agitation leach; Wherein temperature of reaction is 10～90 ℃, and the solid-liquid mass volume ratio is 1: 2～7g/ml, and sulfuric acid concentration is 1mol/L～8mol/L, extraction time 2～10h;
(3) leach liquor being filtered, is extraction agent with two (2-ethylhexyl) phosphorodithioic acid-trioctylamine, and sulfonated kerosene is thinner extracting copper and cadmium, and the volume ratio of sulfonated kerosene and two (2-ethylhexyl) phosphorodithioic acid-trioctylamine is 1: 3-6; Leach liquor compares 4～8 with organic extractant during extraction: 1, and 10～40 ℃ of extraction temperature, extraction progression is 1～4; Aqueous sulfuric acid with 100～200g/L is a strip liquor, back extraction copper, cadmium from rich copper, rich cadmium organic phase, strip liquor and organic phase be in a ratio of 1: 1～5, back extraction progression is 1～4,10～40 ℃ of back extraction temperature;
(4) add organic precipitant in the copper sulfate that after back extraction, obtains, the Cadmium Sulphate mixing solutions, obtain being in copper, the cadmium organic deposition on upper strata; Temperature of reaction is 10～50 ℃, and the add-on of organic precipitant is 1～3 times of Theoretical Mass;
(5) method of toppling is separated above-mentioned copper, cadmium organic deposition, stirs reduction reaction with adding reductant solution behind the distilled water wash, reduction reaction time 0.5～3h, and the add-on of reductive agent is 1～3 times of Theoretical Mass; Separation and washing are in organic cadmium on upper strata, obtain organic cadmium product after the drying; The solution that separates behind organic cadmium adopts filtration method that the copper powder that restores in the solution is separated, and the washing drying obtains flake copper.
Described organic precipitant is sodium oleate, stearic acid, sodium stearate, erucic acid sodium, the mixture of one or more in the cetoleic acid sodium.
Described reductive agent is one or more of formaldehyde, glucose, xitix, hydrazine hydrate, sodium borohydride, hypophosphite.
Zinciferous raffinate changes electric Zn system over to and obtains electric zinc or add organic precipitant obtaining organic zinc.
Advantage of the present invention and positively effect are:
(1) with two (2-ethylhexyl) phosphorodithioic acid-trioctylamine common extracting copper and cadmium from leach liquor, obtain the mixing organic phase of copper and cadmium, realized that not only copper, cadmium separate with other foreign metal ionic in the leach liquor, but also can realize synchronously separating of copper, cadmium and zinc, simplified subsequent processes.
(2), obtain the mixed solution of copper sulfate and Cadmium Sulphate, for the purified organic copper of subsequent preparation, organic cadmium product create conditions with sulfuric acid while back extraction copper and cadmium.
(3) organic copper, cadmium mixture washing back add reductant solution and stir reduction reaction, can obtain flake copper and organic cadmium product, realize the increment utilization of copper, cadmium in the copper-cadmium slag.At present, flake copper is widely used in electrically conducting coating, conductive resin and electrocondution slurry etc.As the copper powder of conductive filler material, its pattern has a significant impact the electroconductibility of electro-conductive material and the character of made electrocondution slurry.Spherical conductive filler material mainly is a contact, and laminal filler mainly is the face contact, helps the conduction of electric charge, and smooth surface, can increase contact area, helps the raising of electroconductibility.And organic cadmium, organic zinc product such as cadmium stearate, Zinic stearas etc. are widely used in the stablizer of polyvinyl chloride; As the lubricant of styrene resin, resol, amine resin and releasing agent, as raw material of the flatting agent of stablizer, paint and the enamel of the polishing agent of the softening lubricant of rubber item, textiles, igelite and makeup, flour or the like, market is boundless.
(4) adopt to add the measure that organic precipitant obtains organic zinc in the raffinate, other foreign metal ion isolation in zinc and the raffinate also can be able to be obtained the higher organic zinc product of added value.
(5) the present invention first extraction treatment is obtained copper and cadmium the mixing organic phase method and add organic precipitant and the method for reductive agent combines in the process field that is applied to zinc hydrometallurgy by product, be the completely new approach that a cover is particularly suitable for the processing of zinc hydrometallurgy by product.The fine product that not only prepares copper, cadmium, zinc: flake copper, organic cadmium, organic zinc product; Its added value than general method prepare all high, realized the increment utilization of zinc hydrometallurgy by product; And reduced the processing cost of zinc smelting byproducts, and need not complicated steps such as electrolysis, only need simply to add organic precipitant and reductive agent gets final product, operate very simply, and the reaction times is short, the degree of purity of production height, do not produce pollutent and waste water, reached the purpose that reduction of discharging increases income.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention,
Fig. 2 is the SEM figure that adopts the flake copper that the present invention obtains,
Fig. 3 is the XRD figure spectrum that adopts the flake copper that the present invention obtains.
Embodiment
Below in conjunction with specific embodiment embodiment of the present invention is described further.
Embodiment one
Present embodiment provides a kind of treatment process of zinc hydrometallurgy by product, with the copper-cadmium slag after the sulphuric acid soln leaching thermal treatment, use method while extracting copper and cadmium from leach liquor of organic solvent extraction then, obtain the raffinate of rich copper, cadmium organic phase and sulfur acid zinc.Rich copper, cadmium organic phase obtain the mixing solutions of copper sulfate and Cadmium Sulphate earlier with the sulfuric acid back extraction, add an amount of organic precipitant then in mixing solutions, obtain the mixture of copper, cadmium organic deposition.After separating this copper, cadmium throw out and washing, add reductant solution and carry out reduction reaction, obtain flake copper and organic cadmium product respectively.The raffinate of sulfur acid zinc then adds organic precipitant and obtains organic zinc.
Specifically comprise: (its major ingredient is (%): Cu3.81, Zn39.43, Cd8.78 to get copper-cadmium slag 500g, Pb1.78, Fe 1.28, As0.079, Co0.124, Ni0.067), thermal treatment 3h under 280 ℃ temperature pours into after the cooling in the 3L beaker, and the sulphuric acid soln 1L that adds 4mol/L carries out agitation leach, 60 ℃ of extraction temperatures, extraction time 4h.After the cooling leach liquor is filtered, add two (2-ethylhexyl) phosphorodithioic acid-trioctylamine as extraction agent in filtrate, sulfonated kerosene is thinner extracting copper and cadmium, and leach liquor is compared 5: 1 with organic extractant during extraction; Wherein the volume ratio of sulfonated kerosene and two (2-ethylhexyl) phosphorodithioic acid-trioctylamine is 1: 5.30 ℃ of extraction temperature; The two-stage extraction.Aqueous sulfuric acid with 120g/L is a strip liquor, back extraction copper, cadmium from rich copper, rich cadmium organic phase, strip liquor and organic phase be in a ratio of 1: 5, three grades of back extractions, 30 ℃ of back extraction temperature.Obtain adding in copper sulfate, the cadmium sulfate solution sodium oleate of 40g after the back extraction to back extraction, stirring reaction 30min under 30 ℃ of conditions, treat that lower leaf obviously will float over afterwards the cupric oleate on upper strata, the cadmium oleate mixture adopts the method for toppling to separate, behind this mixture of 200ml distilled water wash, the sodium hypophosphite 300ml that adds 80g/L stirs reduction 30min.Separate and washing floats over behind the cadmium oleate of upper strata dry 8h under 50 ℃ of conditions, obtain cadmium oleate (purity 99.9%) product, and the residual solution of separating behind the cadmium oleate adopts the method for filtration washing to obtain flake copper (purity 99.9%) (Fig. 2, shown in Figure 3).And add the 20g sodium stearate in the raffinate of above-mentioned sulfur acid zinc solution, and stirring reaction 30min, temperature of reaction is 30 ℃.Obtain Zinic stearas product (purity 99.5%) afterwards.
Embodiment two
Present embodiment provides a kind of treatment process of zinc hydrometallurgy by product, at first with copper ashes thermal treatment in rotary kiln of one of hydrometallurgy by product, use method while extracting copper and cadmium from leach liquor of organic solvent extraction then, obtain the raffinate of rich copper, cadmium organic phase and sulfur acid zinc.Rich copper, cadmium organic phase obtain the mixing solutions of copper sulfate and Cadmium Sulphate earlier with the sulfuric acid back extraction, add an amount of organic precipitant then in mixing solutions, obtain the mixture of copper, cadmium organic deposition.After separating this copper, cadmium throw out and washing, add reductant solution and carry out reduction reaction, obtain flake copper and organic cadmium product respectively.The raffinate of sulfur acid zinc then adds organic precipitant and obtains organic zinc.
Specifically comprise: get copper-cadmium slag 1000g, its major ingredient is (%): Cu17.09, Zn13.74, Cd4.83, Pb9.34, Fe 2.28, As0.39, Co0.11, Ni 0.21, thermal treatment 6h under the temperature about 300 ℃, pour into after the cooling in the 5L beaker, the sulphuric acid soln 2L that adds 5mol/L carries out agitation leach, 70 ℃ of extraction temperatures, extraction time 2h.After reaction finishes cooled leach liquor is filtered, add two (2-ethylhexyl) phosphorodithioic acid-trioctylamine as extraction agent in filtrate, sulfonated kerosene is thinner extracting copper and cadmium, and leach liquor is compared 8: 1 with organic extractant during extraction; Wherein the volume ratio of sulfonated kerosene and two (2-ethylhexyl) phosphorodithioic acid-trioctylamine is 1: 4.Three grades of extractions, 30 ℃ of extraction temperature; Aqueous sulfuric acid with 200g/L is a strip liquor, back extraction copper, cadmium from rich copper, rich cadmium organic phase, strip liquor and organic phase be in a ratio of 1: 4,30 ℃ of back extraction temperature.Three grades of back extractions.The sodium stearate that in obtaining copper sulfate, Cadmium Sulphate mixing solutions, adds 80g after the back extraction, stirring reaction 30min postcooling under 50 ℃ of conditions, treat that lower leaf obviously will float over afterwards the copper stearate on upper strata, the cadmium mixture adopts the method for toppling to separate, behind this mixture of 600ml distilled water wash, the sodium borohydride 500ml that adds 90g/L stirs reduction 60min.Separate and washing floats over behind the cadmium stearate of upper strata dry 8h under 50 ℃ of conditions, obtain cadmium stearate product (99.9%), and the residual solution of separating behind the cadmium stearate adopts the method for filtration washing to obtain flake copper (99.9%).And in the raffinate of above-mentioned sulfur acid zinc solution, add the 30g sodium oleate, and stirring reaction 40min, temperature of reaction is 50 ℃.Obtain zinc oleate (99.5%) product afterwards.
Embodiment three
Present embodiment provides a kind of treatment process of zinc hydrometallurgy by product, at first with copper-cadmium slag thermal treatment in rotary kiln of one of hydrometallurgy by product, use method while extracting copper and cadmium from leach liquor of organic solvent extraction then, obtain the raffinate of rich copper, cadmium organic phase and sulfur acid zinc.Rich copper, cadmium organic phase obtain the mixing solutions of copper sulfate and Cadmium Sulphate earlier with the sulfuric acid back extraction, add an amount of organic precipitant then in mixing solutions, obtain the mixture of copper, cadmium organic deposition.After separating this copper, cadmium throw out and washing, add reductant solution and carry out reduction reaction, obtain flake copper and organic cadmium product respectively.The raffinate of sulfur acid zinc then adds organic precipitant and obtains organic zinc.
Specifically comprise: get copper-cadmium slag 5000g, its major ingredient is (%): Cu10.12, Zn9.22, Cd3.56, Pb6.14, Fe 3.02, As0.44, Co0.27, Ni 0.23, thermal treatment 5h under the temperature about 270 ℃, pour into after the cooling in the 50L reactor, the sulphuric acid soln 20L that adds 6mol/L carries out agitation leach, 80 ℃ of extraction temperatures, extraction time 2.5h.After reaction finishes cooled leach liquor is filtered, add two (2-ethylhexyl) phosphorodithioic acid-trioctylamine as extraction agent in filtrate, sulfonated kerosene is thinner extracting copper and cadmium, and leach liquor is compared 6: 1 with organic extractant during extraction; Wherein the volume ratio of sulfonated kerosene and two (2-ethylhexyl) phosphorodithioic acid-trioctylamine is 1: 5.Three grades of extractions, 25 ℃ of extraction temperature; Aqueous sulfuric acid with 200g/L is a strip liquor, back extraction copper, cadmium from rich copper, rich cadmium organic phase, strip liquor and organic phase be in a ratio of 1: 5,25 ℃ of back extraction temperature.Three grades of back extractions.The erucic acid sodium that in obtaining copper sulfate, Cadmium Sulphate mixing solutions, adds 800g after the back extraction, stirring reaction 30min postcooling under 40 ℃ of conditions, treat that lower leaf obviously will float over afterwards the erucic acid copper on upper strata, the cadmium mixture adopts the method for toppling to separate, behind this mixture of 6L distilled water wash, the hydrazine hydrate 1000ml that adds 100g/L stirs reduction 60min.Separate and washing floats over behind the erucic acid cadmium of upper strata dry 10h under 40 ℃ of conditions, obtain erucic acid cadmium product (99.5%), and the residual solution of separating behind the erucic acid cadmium adopts the method for filtration washing to obtain flake copper (99.9%).And in the raffinate of above-mentioned sulfur acid zinc solution, add 300g cetoleic acid sodium, and stirring reaction 60min, temperature of reaction is 40 ℃.Obtain cetoleic acid zinc (99.5%) product afterwards.
The above; be specific embodiments of the invention only, protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (3)
1. the treatment process of a zinc hydrometallurgy by product, it is characterized in that: the copper-cadmium slag or the rich copper ashes that at first leach output in the zinc hydrometallurgy process with sulphuric acid soln, use method while extracting copper and cadmium from leach liquor of organic extraction then, and obtain the mixing solutions of copper sulfate and Cadmium Sulphate with the sulfuric acid back extraction, in mixing solutions, add organic precipitant, obtain the mixture of copper, cadmium organic deposition; After separating this copper, cadmium throw out and washing, add reductant solution and carry out reduction reaction, obtain flake copper and organic cadmium product respectively; Zinciferous raffinate changes electric Zn system over to and obtains electric zinc or add organic precipitant obtaining organic zinc;
Specifically may further comprise the steps:
(1) copper-cadmium slag or rich copper ashes earlier in air atmosphere under 250～300 ℃ of temperature thermal treatment 1～6h;
(2) copper-cadmium slag after the thermal treatment or rich copper ashes join in the sulphuric acid soln, carry out agitation leach; Wherein temperature of reaction is 10～90 ℃, and the solid-liquid mass volume ratio is 1: 2～7g/ml, and sulfuric acid concentration is 1mol/L～8mol/L, extraction time 2～10h;
(3) leach liquor being filtered, is extraction agent with two (2-ethylhexyl) phosphorodithioic acid-trioctylamine, and sulfonated kerosene is thinner extracting copper and cadmium, and the volume ratio of sulfonated kerosene and two (2-ethylhexyl) phosphorodithioic acid-trioctylamine is 1: 3-6; Leach liquor compares 4～8 with organic extractant during extraction: 1, and 10～40 ℃ of extraction temperature, extraction progression is 1～4; Aqueous sulfuric acid with 100～200g/L is a strip liquor, back extraction copper, cadmium from rich copper, rich cadmium organic phase, strip liquor and organic phase be in a ratio of 1: 1～5, back extraction progression is 1～4,10～40 ℃ of back extraction temperature;
(4) add organic precipitant in the copper sulfate that after back extraction, obtains, the Cadmium Sulphate mixing solutions, obtain being in copper, the cadmium organic deposition on upper strata; Temperature of reaction is 10～50 ℃, and the add-on of organic precipitant is 1～3 times of Theoretical Mass;
(5) method of toppling is separated above-mentioned copper, cadmium organic deposition, stirs reduction reaction with adding reductant solution behind the distilled water wash, reduction reaction time 0.5～3h, and the add-on of reductive agent is 1～3 times of Theoretical Mass; Separation and washing are in organic cadmium on upper strata, obtain organic cadmium product after the drying; The solution that separates behind organic cadmium adopts filtration method that the copper powder that restores in the solution is separated, and the washing drying obtains flake copper.
2. the treatment process of zinc hydrometallurgy by product according to claim 1 is characterized in that, described organic precipitant is sodium oleate, stearic acid, sodium stearate, erucic acid sodium, the mixture of one or more in the cetoleic acid sodium.
3. the treatment process of zinc hydrometallurgy by product according to claim 1 is characterized in that, described reductive agent is one or more of formaldehyde, glucose, xitix, hydrazine hydrate, sodium borohydride, hypophosphite.
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| CN105779763B (en) * | 2016-05-27 | 2017-07-04 | 赤峰中色锌业有限公司 | Zinc and the method for preparing electric zinc are extracted from cadmium milltailings containing zinc water high |
| CN109722547B (en) * | 2019-03-11 | 2020-11-03 | 福州大学 | Method for recovering copper from copper smelting slag and preparing phenylaminoarsonate |
| CN112126795A (en) * | 2020-10-18 | 2020-12-25 | 赤峰中色锌业有限公司 | Method for recovering zinc from clean liquid poor copper slag |
| CN113337723A (en) * | 2021-06-10 | 2021-09-03 | 广东先导稀材股份有限公司 | Method for separating and extracting silver, palladium, copper and germanium from silver separating slag |
| CN115141940B (en) * | 2022-07-14 | 2023-10-24 | 赛恩斯环保股份有限公司 | Method for separating zinc and cadmium from sulfuric acid medium |
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| JP特开平6-240373A 1994.08.30 |
| 袁贵有.从铜镉渣中回收镉的试验研究.《有色金属再生与利用》.2006,(第12期),21-22. * |
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