CN103805776A - Method of separating and enriching copper and zinc from copper and zinc containing wastes - Google Patents
Method of separating and enriching copper and zinc from copper and zinc containing wastes Download PDFInfo
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Abstract
The invention belongs to the field of nonferrous metal recovery and solid wastes recycle, and relates to a method of separating and enriching copper and zinc from copper and zinc containing wastes. The method comprises the following steps: (1) preparing strong alkali leaching liquor; (2) adding particles of the copper and zinc containing wastes into the strong alkali leaching liquor prepared by the step (1), and heating by microwaves; (3) purifying impurities in the leaching liquor by a separant to obtain electrolyte; (4) electrolyzing the purified electrolyte in the sep (3) by a pulse power supply to obtain zinc powder; and (5) recovering copper enriched in leaching residues. The method is environment-friendly and easy to operate on a large scale. The leaching liquor is heated by microwaves, and the zinc copper ratio in the extractum is increased, so that over 98% of copper is enriched in residues. The leaching liquor is electrolyzed by introducing a pulse technology, so that the grade and specific surface area of zinc powder are improved, and the morphological control means of the product are enriched. Impurities are removed by means of self-generated high activity dendritic zinc powder which is fewer in use level, the reaction effect is superior to that of conventional zinc powder, and the self-generated zinc powder is recycled.
Description
Technical field
The invention belongs to non-ferrous metal and reclaim and reclamation of solid wastes field, relate to a kind of from cupric zinc refuse the method for separation and concentration copper, zinc.
Background technology
China is the production and consumption big country of non-ferrous metal, and along with domestic economy high speed development, the contradiction of domestic shortage of mineral resources also becomes increasingly conspicuous.In recent years, constantly make great efforts under promotion in national policy guiding and industry self, China's nonferrous metal industry is rapidly developed, domestic reclaimed copper year utilization exceeded 2,000,000 tons, secondary aluminum and exceed 3,000,000 tons, secondary metal annual production and broken through 6,000,000 tons.Multiple workshop sections by-product waste residue of secondary metal recovery process, useless dirt ash, as dirt ash of the collections such as electric furnace ash, converter slag, smelting slag, electric precipitator etc., and this type of lime-ash, along with the expansion annual production cumulative year after year of secondary metal industry size, has exceeded 100,000 tons/year.In these solid waste, contain plurality of heavy metal, belong to harmful waste, its processing cost, storage cost, transportation cost are all higher than Ordinary solid waste; But it contains zinc, lead, copper, aluminium etc., has again potential utility value.The technical process of therefore developing a kind of simple environmental protection is reclaimed respectively metal and is had significant environmental benefit and economic benefit from these industrial residues.
The technique that Chinese patent CN1450182A-method with zinc oxide ore production high purity metal zinc and CN1482263A-propose from the method for zinc oxide ore production high-purity zinc has promoted the scale operation of alkaline process electrolytic zinc powder technique, but the zinc powder particle diameter that this flow process is produced is large, and skewness, subsequent machining cost is high, technology difficulty is large; Mono-kind of patent applied for 201210249664.2-adds mono-kind of the method for aluminum contained compound alkali lye electrolytic preparation super-fine zinc dust and 201210034534.7-and adds lead-containing compounds alkali lye to prepare the method for super-fine zinc dust be to utilize the polarized action of additive to increase zinc powder specific surface area, the zinc powder that electrolysis goes out is dendroid pattern, be applicable to the additive that displacer in hydrometallurgy and part chemicals are produced, but process control is comparatively complicated.The method of a Chinese invention patent CN102181886A-Direct Electrolysis production 1-dimention nano zinc flake from strong base solution has realized the zinc flake of thickness in 100nm, but in technical process, need to add exhibiting high surface promoting agent, increased bath voltage and energy consumption.
Chinese invention patent CN101012514A (a kind of use is produced the method for metallic lead and zinc containing lead-zinc residue or lead-zinc) has proposed by the method containing lead-zinc residue or low-grade zinc oxide ore production metallic lead and zinc, technique is simple, raw material sources are extensive, production cost is low, can comprehensive reutilization metal.But this flow process does not propose the removal technique of remaining Pb after electrolysis deleading, also potentially harmful substance Sb in solution is not carried out to respective handling simultaneously.Chinese invention patent CN102234821A (from the method containing reclaiming the ultra-fine lead powder of preparation and pure lead pig zinc ingot metal smelting charge of lead and zinc) provides a kind of with the method containing reclaiming the ultra-fine lead powder of preparation or pure lead pig zinc ingot metal in smelting charge of lead and zinc; this technological operation convenience, environmental friendliness, applicable large-scale production; but the current density that its electrolytic zinc process is used is too low; be difficult to like this to get surface-area large, and the zinc powder being evenly distributed.Chinese invention patent CN102409180A (a kind of metallurgical technology that reclaims copper-lead zinc-tin metal from copper slag) is mainly for conventional copper metallurgy industrial residue, useless lime-ash significant difference in its raw material composition and this technique, and these process using two steps dechlorinate, purification cost is high, and pickling link also can cause a certain amount of zinc loss.
Summary of the invention
The object of the invention is to defect for overcoming prior art provide a kind of from cupric zinc refuse the method for separation and concentration copper, zinc; the simple environmental protection of the method is easy to mass-producing operation; and make full use of self-made products and introduce pulsed technique in electrolysis link and improve zinc powder quality, having realized making full use of of refuse.
For achieving the above object, the present invention is by the following technical solutions:
A method for separation and concentration copper, zinc from cupric zinc refuse, the process of the method is simple, and step comprises:
(1) prepare leaching liquid with highly basic;
(2) the leaching liquid microwave heating leaching cupric zinc industrial waste particle making by step (1);
(3) obtain electrolytic solution with the impurity in separating agent purifying step (2) gained leach liquor;
(4) with the electrolytic solution after pulse power electrolysis step (3) purification, obtain zinc powder;
(5) reclaim the copper that leaches enrichment in residue.
In the present invention, the particle of cupric zinc refuse is from the useless lime-ash of regenerated metal industry by-product etc.
In described step (1), highly basic is NaOH or KOH, and wherein, the content of NaOH in leaching liquid is 150-250g/L; The content of KOH in leaching liquid is 250-420g/L.
In described step (2), the particle diameter of cupric zinc industrial waste particle is less than 1mm.
In described step (2), the liquid-solid ratio of leaching liquid and industrial waste particle is 8:1-12:1, utilizes 600-800W microwave heating, heating cycle 2-4 time, and single loop continues 10-50S.
The 1.2-2 that in described step (3), the addition of separating agent is leaded molar content in described industrial waste doubly.
Separating agent in described step (3) is sulfur-based compound, based on solubility product principle, to purify the impurity in leach liquor, generates sulfide precipitation, and wherein sulfur-based compound is sodium sulphite or potassium sulphide.
Separating agent in described step (3) is zinc powder, to replace the impurity in leach liquor; The preferred dendritic zinc powder of this zinc powder, this dendritic zinc powder can adopt the self-produced dendritic zinc powder of step of the present invention (4) electrolysis, the dendritic zinc powder that also can adopt market to buy.
Impurity in described step (3) comprises lead, copper, antimony.
When antimony content in described step (3) electrolytic solution is greater than 1mg/L, add anion surfactant, the negative effect that declines and zinc powder is bubbled with the current efficiency that suppresses to cause due to antimony, wherein, anion surfactant is one or more the mixing in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate or sodium laurylsulfonate, enters next step when antimony content concentration exceedes after 5mg/L needs active zinc powder and sulfur-based compound to coordinate deep purifying.
In described step (4), electrolytic zinc-coated steel sheet is stainless steel plate, and interpole gap is 1-10cm, and whole electrolytic process carries out in a groove, electrolyte temperature 15-80 ℃, and electrolysis time is 60-120min.
The ON time T of the pulse power in described step (4)
onfor 10-20ms, turn-off time T
offbe made as 5-30ms, peak current density is made as 1000-1800A/m
2.
Described step (5) leaches the copper of enrichment in residue and reclaims with ammonia leaching process, or as the raw material of copper smelting by pyrometallurgy.
Tool of the present invention has the following advantages:
(1) utilize strong base solution can directly realize on the one hand separating of copper and zinc, because alkaline electrolyte is better than acid electrolyte to the tolerance of chlorine, reduced purification cost on the other hand.
(2) utilize microwave selective heating, improved zinc-copper ratio in extract, make to exceed in 98% copper enrichment and slag.
(3) introduce pulsed technique electrolysis leach liquor, improved zinc powder grade and specific surface area, enriched product morphology control means, the zinc powder making is dendrite more, active in conventional zinc powder.
(4) utilize the dendritic zinc powder removal of impurities of self-produced high reactivity, consumption is few, and reaction effect is better than conventional zinc powder, and has realized the recycle of self-produced zinc powder.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 gained zinc powder.
Fig. 2 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 2 gained zinc powders.
Fig. 3 is the scanning electron microscope (SEM) photograph of conventional DC electrolysis zinc powder.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but the invention is not restricted to embodiment.
Embodiment 1
Reclaim factory's industrial waste as raw material take Zhejiang copper scrap, it forms as table 1
Table 1
| Composition | Zn | Cu | Pb | Al | Cl |
| Content (%) | 40.21 | 9.53 | 4.62 | 2.58 | 8.47 |
(1) prepare leaching liquid with distilled water, NaOH, NaOH concentration is 250g/L;
(2) cupric zinc industrial waste is sieved and be levigately less than 1mm to grain diameter, add in the leaching liquid of step (1), liquid-solid ratio is 8:1, microwave power is 600W, microwave heating leaching circulation 4 times, and the single cycle time is 30s, 99.3% bronze medal is stayed in slag, and the leaching yield of zinc is 87.2%;
(3) in step (2) gained leach liquor, add separating agent sodium sulphite, addition is leaded molar content in industrial waste 1.2 times, based on solubility product principle, to purify the residual impurity such as copper, lead of leach liquor, generate sulfide precipitation.In leach liquor after purification, zinc content is 40g/L, and copper, lead content are all less than 50mg/L, obtain electrolytic solution;
(4) gained electrolytic solution enters pulse electrolysis groove, by ON time T
onbe designed to 15ms, turn-off time T
offbe made as 5ms, peak current density is made as 1800A/m
2, electrolyte temperature is 80 ℃, interpole gap is 10cm, electrolysis time 60min, products therefrom be grain diameter 35.3 μ m left and right even zinc powder;
(5) copper that leaches enrichment in residue reclaims with ammonia leaching process.
When the present embodiment electrolytic zinc powder, record current efficiency and be greater than 80%, Fig. 1 is the scanning electron microscope (SEM) photograph of electrolysis gained zinc powder, and it shows that zinc powder is dendrite more, contrasts with Fig. 3, adopt the zinc powder dendrite rate of pulsed current electrolysis higher, and the activity of dendritic zinc powder is better than conventional zinc powder.The size distribution of the present embodiment gained zinc powder is in table 2, it shows that prepared zinc powder exceedes 50% particle and is less than 46.85 μ m, specific surface area median size D[3,2] be 35.3 μ m, length mean diameter is 8.82um, and even particle distribution (index of conformity is 0.518), the large (169.8m of specific surface area
2/ kg).
Table 2
| Sreen analysis | Mean value (um) | D10(um) | D50(um) | D90(um) |
| Length mean diameter, D[1,0] | 8.82 | 1.58 | 12.44 | 27.56 |
| Surface area mean diameter, D[2,0] | 14.67 | ? | ? | ? |
| Specific surface area mean diameter, D[3,2] | 35.33 | 18.90 | 46.85 | 97.12 |
| Volume mean diameter, D[3,0] | 50.15 | ? | ? | ? |
The dendritic zinc powder that this enforcement is made joins in the step (3) of embodiment 2 and embodiment 3, replace sodium sulphite as impurity such as the copper-leads in separating agent purifying and replacing leach liquor, the zinc powder making due to pulse electrolysis is dendrite, its activity is higher, therefore its reaction effect is better than adding conventional zinc powder, and realize the recycle of self-produced zinc powder.
Embodiment 2
Take Yunnan smeltery industrial waste as raw material, it forms as table 3
Table 3
| Composition | Zn | Cu | Pb | Sb | Al |
| Content (%) | 31.08 | 8.79 | 6.53 | 0.26 | 7.61 |
(1) prepare leaching liquid with distilled water, NaOH, NaOH concentration is 150g/L;
(2) cupric zinc industrial waste is sieved and be levigately less than 1mm to grain diameter, add in the leaching liquid of step (1), liquid-solid ratio is 12:1, microwave power is 800W microwave heating leaching circulation 2 times, the single cycle time is 50s, and 98.4% bronze medal is stayed in slag, and the leaching yield of zinc is 85.5%;
(3) in step (2) gained leach liquor, the dendritic zinc powder that adds embodiment 1 to make, addition is leaded molar content in industrial waste 1.5 times, to replace the impurity such as copper residual in leach liquor, lead, antimony.In leach liquor after purification, recording zinc content is 30g/L, and copper, lead content are all less than 50mg/L, and antimony content is 3mg/L, add sodium lauryl sulphate, making its concentration is 10mg/L, and the negative effect that declines and zinc powder is bubbled with the current efficiency that suppresses to cause due to antimony, obtains electrolytic solution;
(4) gained electrolytic solution enters pulse electrolysis groove, by ON time T
onbe designed to 20ms, turn-off time T
offbe made as 30ms, peak current density is made as 1000A/m
2, electrolyte temperature is 15 ℃, and interpole gap is 1cm, and electrolysis time is 120min, and products therefrom is that grain diameter is the even zinc powder of 42.8 μ m left and right.
(5) copper that leaches enrichment in residue reclaims with pyrogenic process.
When the present embodiment electrolytic zinc powder, record current efficiency and be greater than 85%, Fig. 2 is the scanning electron microscope (SEM) photograph of electrolysis gained zinc powder, and it shows that gained zinc powder is dendrite more, contrasts with Fig. 3, adopt the zinc powder dendrite rate of pulsed current electrolysis higher, and the activity of dendritic zinc powder is better than conventional zinc powder.The size distribution of the present embodiment gained zinc powder is in table 4, the zinc powder that its demonstration makes exceedes 50% particle and is less than 60.15 μ m, specific surface area median size D[3,2] be 42.83 μ m, length mean diameter is 10.04um, and even particle distribution (index of conformity is 0.794), the large (140.3m of specific surface area
2/ kg).
Table 4
| Sreen analysis | Mean value (um) | D10(um) | D50(um) | D90(um) |
| Length mean diameter, D[1,0] | 10.04 | 1.57 | 10.92 | 25.16 |
| Surface area mean diameter, D[2,0] | 15.36 | ? | ? | ? |
| Specific surface area mean diameter, D[3,2] | 42.83 | 21.70 | 60.15 | 155.54 |
| Volume mean diameter, D[3,0] | 52.84 | ? | ? | ? |
Embodiment 3
Take Jiangxi Metallurgical Factory industrial waste as raw material, it forms as table 5
Table 5
| Composition | Zn | Cu | Pb | Al | Cl |
| Content (%) | 52.11 | 6.25 | 5.78 | 1.32 | 6.50 |
(1) prepare leaching liquid with distilled water, NaOH, NaOH concentration is 190g/L;
(2) cupric zinc industrial waste is sieved and be levigately less than 1mm to grain diameter, add in the leaching liquid of step (1), liquid-solid ratio is 10:1, microwave power is 700W microwave heating leaching circulation 3 times, the single cycle time is 10s, and 99.6% bronze medal is stayed in slag, and the leaching yield of zinc is 88.5%;
(3) in step (2) gained leach liquor, the dendritic zinc powder that adds embodiment 1 to make, addition is leaded molar content in industrial waste 2 times, to replace the impurity such as copper, lead residual in leach liquor.In leach liquor after purification, zinc content is 44g/L, and copper, lead content are all less than 50mg/L, obtain electrolytic solution;
(4) gained electrolytic solution enters pulse electrolysis groove, by ON time T
onbe designed to 10ms, turn-off time T
offbe made as 15ms, peak current density is made as 1400A/m
2, electrolyte temperature is 45 ℃, and interpole gap is 5cm, and electrolysis time is 90min, and products therefrom is the even zinc powder of grain diameter in 36 μ m left and right;
(5) copper that leaches enrichment in residue reclaims with pyrogenic process.
When the present embodiment electrolytic zinc powder, record current efficiency and be greater than 92%, show that according to obtained zinc powder electron-microscope scanning figure gained zinc powder is dendrite more, activity is better than conventional zinc powder.The size distribution of the present embodiment gained zinc powder is in table 6, it shows that gained zinc powder exceedes 50% particle and is less than 50.93 μ m, specific surface area median size D[3,2] be 36.72 μ m, length mean diameter is 15.29um, and even particle distribution (index of conformity is 0.625), the large (162.6m of specific surface area
2/ kg).
Table 6
| Sreen analysis | Mean value (um) | D10(um) | D50(um) | D90(um) |
| Length mean diameter, D[1,0] | 15.29 | 5.67 | 22.78 | 53.23 |
| Surface area mean diameter, D[2,0] | 18.35 | ? | ? | ? |
| Specific surface area mean diameter, D[3,2] | 36.72 | 17.44 | 50.93 | 101.06 |
| Volume mean diameter, D[3,0] | 49.31 | ? | ? | ? |
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. a method for separation and concentration copper, zinc from cupric zinc refuse, is characterized in that: comprise the steps:
(1) prepare highly basic leaching liquid;
(2) particle of cupric zinc refuse is joined in the highly basic leaching liquid that step (1) makes to microwave heating;
(3) obtain electrolytic solution with the impurity in separating agent purifying step (2) gained leach liquor;
(4) with the electrolytic solution after pulse power electrolysis step (3) purification, obtain zinc powder;
(5) reclaim the copper that leaches enrichment in residue.
2. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 1, is characterized in that: in described step (1), highly basic is NaOH or KOH, wherein, the content of NaOH in leaching liquid is 150-250g/L; The content of KOH in leaching liquid is 250-420g/L.
3. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 1, is characterized in that: in described step (2), the particle diameter of cupric zinc waste particles is less than 1mm.
According to described in claim 1 or 3 from cupric zinc refuse the method for separation and concentration copper, zinc, it is characterized in that: in described step (2), the liquid-solid ratio of leaching liquid and cupric zinc waste particles is 8:1-12:1, utilizes 600-800W microwave heating, heating cycle 2-4 time, single loop continues 10-50s.
5. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 1, is characterized in that: the impurity in described step (3) comprises lead, copper, antimony.
According to described in claim 1 or 5 from cupric zinc refuse the method for separation and concentration copper, zinc, it is characterized in that: in described step (3) addition of separating agent be plumbous molar content in described cupric zinc waste particles 1.2-2 doubly; Described separating agent is zinc powder or sulfur-based compound.
7. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 6, is characterized in that: the preferred dendritic zinc powder of described zinc powder; Described sulfur-based compound is sodium sulphite or potassium sulphide.
8. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 5, it is characterized in that: when the antimony content in described step (3) electrolytic solution is greater than 1mg/L, add anion surfactant, described anion surfactant is one or more the mixing in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate or sodium laurylsulfonate.
9. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 1, it is characterized in that: in described step (4), electrolytic zinc-coated steel sheet is stainless steel plate, interpole gap is 1-10cm, whole electrolytic process carries out in a groove, electrolyte temperature 15-80 ℃, electrolysis time is 60-120min;
The ON time T of the pulse power in described step (4)
onfor 10-20ms, turn-off time T
offbe made as 5-30ms, peak current density is made as 1000-1800A/m
2.
10. the method for separation and concentration copper, zinc from cupric zinc refuse according to claim 1, is characterized in that: the copper ammonia leaching process that described step (5) leaches enrichment in residue reclaims, or as the raw material of copper smelting by pyrometallurgy.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114134538A (en) * | 2021-12-08 | 2022-03-04 | 昆明理工恒达科技股份有限公司 | Zinc electrodeposition system suitable for high current density |
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Patent Citations (5)
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|---|---|---|---|---|
| WO2009050334A1 (en) * | 2007-10-16 | 2009-04-23 | Outotec Oyj | Method for the hydrometallurgical processing of sulphidic material containing zinc and copper |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114134538A (en) * | 2021-12-08 | 2022-03-04 | 昆明理工恒达科技股份有限公司 | Zinc electrodeposition system suitable for high current density |
| CN114134538B (en) * | 2021-12-08 | 2024-03-26 | 昆明理工恒达科技股份有限公司 | Zinc electrowinning system suitable for high current density |
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