CN101914681A - Pollution-free method for treating copper, lead and silver-containing material - Google Patents
Pollution-free method for treating copper, lead and silver-containing material Download PDFInfo
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- CN101914681A CN101914681A CN2010102370325A CN201010237032A CN101914681A CN 101914681 A CN101914681 A CN 101914681A CN 2010102370325 A CN2010102370325 A CN 2010102370325A CN 201010237032 A CN201010237032 A CN 201010237032A CN 101914681 A CN101914681 A CN 101914681A
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- silver
- copper
- lead
- nitric acid
- hydrogen peroxide
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- Y02P10/20—Recycling
Abstract
The invention relates to a pollution-free method for treating a copper, lead and silver-containing material. The method comprises the following steps of: performing crushing or spray fragmenting on the copper, lead and silver-containing material; adding hydrogen peroxide into salpeter solution for oxidation leaching; washing leached residue, and recycling other precious metals; adding sodium chloride, sodium sulphide and sodium carbonate into leachate sequentially to recycle three valuable metals, namely sliver, lead and copper respectively; regulating the pH of the solution with nitric acid; evaporating the solution to crystallize a sodium nitrate product; and absorbing water vapor containing nitric oxide generated in all the processes with aqueous solution containing the hydrogen peroxide, and returning to the oxidation leaching process to realize non pollution and zero release in the whole process of production. The method greatly reduces nitric acid consumption, and the leaching rates of copper, lead and silver all reach over 98 percent.
Description
Technical field the present invention relates to hydrometallurgy process in the field of metallurgy, the Wet-process metallurgy method of the plumbous silver-colored material of particularly pollution-free Treatment of Copper.
Background technology is because the mutual associations of metal such as copper, lead and silver in the non-ferrous metal mineral, in addition, these metals are used with again in industrial use mutually, so no matter be the Metal smelting process, or waste residue, scrap or the alloy type material of metals such as just inevitable output cupric, lead and silver in other production process, so copper, lead and silver-containing material is a kind of important secondary nonferrous metal resource, be necessary the comprehensive valuable metal that reclaims wherein.Treatment process about cupric argentalium material mainly contains: the direct dissolution method of nitric acid, sulfuric acid oxidation dissolution method and vacuum distillation method etc.Because three kinds of metals such as copper, lead and silver can both be dissolved in the nitric acid, handle this type of material so generally adopt the direct dissolving method of nitric acid, but in the nitric acid dissolve process, can produce a large amount of oxynitride inevitably, administer nitrogen oxides pollution in the nitric acid leaching process so study a lot of methods, obtained certain effect.In order to reduce the treatment capacity of nitric acid dissolve process material, Li Hui proposes the copper bismuth silver alloy earlier through the sulfuric acid oxidation dissolved copper, uses nitric acid dissolve silver again, and substep has reclaimed the method for copper and silver.Patent 200910095112.9 proposes to handle lead bronze bismuth gold and silver multicomponent alloy with vacuum distillation method, with lead and bismuth volatilization, copper, gold and silver further is enriched in the slag, and it is short not only to have shortened technical process, and has improved metal recovery rate.The Chinese patent electricity asks 200810222385.0 to disclose " reclaiming the method for silver-bearing copper in the yellow gold waste material " in addition, Chinese patent ZL97107236 discloses " reducing the method for nitrogen oxides emission in the course of preparing nitrate ", the Chinese patent electricity asks 200910095112. to disclose a kind of method of separating multi-element alloy of lead, bismuth, gold, silver and copper, Li Hui is 1996, and (6): 32～34 " coloured mining and metallurgy " also delivered " reclaiming the research of copper silver from copper bismuth silver alloy scrap ".But there is following shortcoming in the method for the plumbous silver-colored material of these Treatment of Copper:
(1) the direct dissolving method of nitric acid, dissolution process produces a large amount of oxynitride, shortcoming such as have that environmental pollution is serious, operating environment difference and nitric acid consumption are big, and existing oxynitride improvement method all belongs to end treatment fails to prevent from the source generation of oxynitride;
(2) sulfuric acid oxidation dissolution method combines with the nitric acid dissolve method, realizes that the substep of copper and silver separates, owing to the influence of lead, causes that copper leaching rate is low, the oxygenant utilization ratio is low, wastewater flow rate is big, also has the problem of nitrogen oxides pollution;
(3) vacuum distillation method is though there are shortcomings such as equipment requirements height, energy consumption height, cost height and Production Flow Chart be long in effective metal such as separation of lead and copper silver.
Summary of the invention the purpose of this invention is to provide a kind ofly can reclaim valuable metal in the copper, lead and silver-containing material effectively, and the free of contamination Wet-process metallurgy method of process.
The technical solution used in the present invention is in order to achieve the above object: after fragmentation of copper, lead and silver-containing material process or the spraying fragmentation, adding hydrogen peroxide oxidation in salpeter solution leaches, other precious metal is reclaimed in leached mud washing back, leach liquor adds sodium-chlor successively, sodium sulfate and yellow soda ash reclaim silver respectively, lead and three kinds of valuable metals of copper, solution is adjusted pH with nitric acid, evaporative crystallization output SODIUMNITRATE product then, the water vapor of the nitrogen-containing oxide of output in each operation, with returning the oxidation leaching process after the aqueous solution absorption that contains hydrogen peroxide, realize the pollution-free and zero release of whole process of production.
Concrete technological process and processing parameter are as follows:
1 fragmentation or fragmentation
Pending copper, lead and silver-containing material is broken or be broken into and be fit to the granularity handled, material can be powdery, bulk and alloy, is the sieve of 44～420um for powdery and blocky material employing cylindrical mill crusher machine to granularity 100% mistake aperture, and can cross the aperture to granularity 100% with the fragmentation of high-temperature spray equipment for alloy material be the sieve of 74～250um.
2 pollution-free oxidations are leached
The mixing solutions of preparation nitric acid and hydrogen peroxide, the volumetric concentration of nitric acid and hydrogen peroxide is respectively 5.0～20% and 2.5～30% in the control mixing solutions, get this liquor capacity 40～80% and be to add material fragmentation or fragmentation after at 3～6: 1 by liquid-solid ratio L/Kg, keep 60～90 ℃ of temperature of reaction and the slow mixing solutions that adds remaining nitric acid for preparing and hydrogen peroxide, nitrogenfree oxide produces in the reaction process, reaction 2～8h after-filtration, other precious metals are reclaimed in leached mud washing back.The chemical reaction that takes place in the oxidation leaching process is as follows:
2Ag+2HNO
3+H
2O
2＝2AgNO
3+2H
2O (1)
Me+2HNO
3++ H
2O
2=Me (NO
3)
2+ 2H
2(Me is Cu to O, Pb) (2)
3 silver medals, lead and copper reclaim step by step
Character according to each metal-salt, add sodium-chlor, sodium sulfate and yellow soda ash successively and reclaim metals such as silver, lead and copper in the nitric acid leach liquor respectively, remain 60～95 ℃ of solution temperatures and time 1～4h, the sodium-chlor add-on is that 0.50～0.60 times of silver content, sodium sulfate add-on are 0.55～0.60 times, yellow soda ash add-on control pH value of solution=10～12 of lead content, after-filtration is finished in each reaction, difference output silver chloride slag, sulfuric acid lead skim and copper ashes, the chemical reaction of generation is as follows respectively:
AgNO
3+NaCl＝AgCl↓+NaNO
3 (3)
Pb(NO
3)
2+Na
2SO
4＝PbSO
4↓+2NaNO
3 (4)
2Cu(NO
3)
2+Na
2CO
3+H
2O＝CuCO
3·Cu(OH)
2↓+2NaNO
3+CO
2↑?(5)
4 SODIUMNITRATE reclaim
After the nitric acid leach liquor reclaimed valuable metal, the pH of solution was 10～12, for the qualified SODIUMNITRATE product of output, at first is neutralized to pH value of solution to 7～9 with nitric acid, and then concentrate, decolouring and crystallisation by cooling output SODIUMNITRATE product, the chemical reaction of generation is:
Na
2CO
3+2HNO
3＝NaNO
3+H
2O+CO
2↑ (6)
The recycling of 5 low-concentration nitrogen oxides
The water vapor that contains low-concentration nitrogen oxide of each operation output, the aqueous solution that employing contains hydrogen peroxide absorbs, keep in the absorption liquid that the hydrogen peroxide volumetric concentration is 2.5～25.0%, 25～55 ℃ of temperature, when hydrogen peroxide volumetric concentration in the absorption liquid is reduced to 0.5% when following, absorption liquid returns the oxidation leaching process.The chemical reaction that takes place in the absorption process is:
2NO+3H
2O
2＝2HNO
3+2H
2O (7)
NO+H
2O
2＝NO
2+H
2O (8)
2NO
2+H
2O
2＝2HNO
3 (9)
Described nitric acid, hydrogen peroxide, sodium-chlor, sodium sulfate and yellow soda ash are technical grade reagent.
The treatment process of the present invention and traditional copper, lead and silver-containing material relatively, have the following advantages: 1, adopt nitric acid system to add hydrogen peroxide oxidation and leach, nitric acid consumption reduces significantly, copper, lead and silver-colored leaching yield all reach more than 98%, and production process does not have yellow oxynitride and produces, and has solved the problem of environmental pollution of nitric acid leaching process from the source; 2, the oxidation leaching process of nitric acid system is not introduced foreign ion, after leach liquor reclaims copper, lead and silver respectively, can concentrate output technical grade SODIUMNITRATE product, the discharging of having stopped nitrogenous effluent; 3, the water vapor that contains low-concentration nitrogen oxide of production process output adopts the aqueous solution that contains hydrogen peroxide to absorb the back Returning utilization, has improved operating environment greatly; 4, labour intensity of the present invention is low, the treatment time short, good operational environment.
The present invention is applicable to the material of the plumbous silver of Treatment of Copper, can be powdery, bulk or alloy, its main component is (%): Cu4.0～75, Pb5～35, Ag0.2～30 and Au0.01～15 by weight percentage, also is suitable for handling the zinc dust precipitation slag of prussiate system output.
Description of drawings
Fig. 1: process flow diagram of the present invention.
Embodiment
Embodiment 1:
It is the sieve of 150um that block copper, lead and silver-containing slag is crossed the aperture with the cylindrical mill crusher machine to granularity 100%, and its main component is (%): Cu35.50, Pb15.65, Ag12.40 and Au0.18 by weight percentage.Technical grade nitric acid, content 65%; The technical grade hydrogen peroxide, content 27.5%, sodium-chlor, yellow soda ash and SODIUMNITRATE are technical grade reagent.
Each 200ml of the nitric acid of mentioned component and hydrogen peroxide and 165ml, water is made into the 1000ml mixing solutions, get the 800ml mixing solutions, the copper, lead and silver-containing material that adds the mentioned component of 200g after levigate while stirring, solution temperature is rapidly increased to about 75 ℃, slowly add remaining 200ml mixing solutions then, control temperature of reaction system at 85 ℃ by the flow velocity size, solution to be mixed adds and continues to stir the 2h after-filtration, leach liquor volume 1100ml, its main component is (g/L): Cu63.80, Pb28.10 and Ag22.35, leached mud washing back oven-dried weight 4.5g, its main component is (%): Cu0.10 by weight percentage, Pb0.12, Ag0.05 and Au8.10.
Reclaim each valuable metal from the nitric acid leach liquor, keep 80 ℃ of solution temperatures, add 13.5g sodium-chlor and react the 2h filtration, the silver chloride pulp water is washed the back oven dry, the heavy 33.15g of silver chloride slag.Solution after the precipitated silver keeps temperature to add 19g sodium sulfate down for 80 ℃, reaction 2h after-filtration, and the lead sulfate pulp water is washed the back oven dry, the heavy 46.25g of sulfuric acid lead skim.Solution behind the precipitation lead at first is warming up to 95 ℃, and then adjusts pH value of solution=11.5 with yellow soda ash, reaction 2h after-filtration, copper ashes washing back oven dry, the heavy 148.50g of copper ashes.Nitric acid leach liquor behind the precipitated copper is neutralized to pH=8 with nitric acid, concentrates, decolouring and crystallisation by cooling the SODIUMNITRATE weight 235.8g of output then; The water vapor that contains low-concentration nitrogen oxide of each operation output is that 7.5% hydrogen peroxide solution absorbs with volumetric concentration, keeps temperature of reaction to be lower than 45 ℃, and when the hydrogen peroxide volumetric concentration was lower than 0.5% in the absorption liquid, absorption liquid returned the dosing of oxidation leaching process.
Embodiment 2:
It is the sieve of 75um that the copper, lead and silver-containing alloy is crossed the aperture with the fragmentation of high-temperature spray equipment to granularity 100%, and its main component is (%): Cu52.80, Pb19.80, Ag9.70 and Ni8.65 by weight percentage.Technical grade nitric acid, content 65%; The technical grade hydrogen peroxide, content 27.5%, sodium-chlor, yellow soda ash and SODIUMNITRATE are technical grade reagent.
Each 850ml of the nitric acid of mentioned component and hydrogen peroxide and 730ml, water is made into the 3000ml mixing solutions, get the 2000ml mixing solutions, the copper, lead and silver-containing alloy that adds the mentioned component after 500g atomizes while stirring, solution temperature is rapidly increased to about 80 ℃, slowly add remaining 1000ml mixing solutions then, control temperature of reaction system at 85 ℃ by the flow velocity size, solution to be mixed adds and continues to stir the 3h after-filtration, leach liquor volume 3400ml, its main component is (g/L): Cu75.43, Pb29.50 and Ag15.28, leached mud washing back oven-dried weight 12.50g, its main component is (%): Cu0.20 by weight percentage, Pb0.12, Ag0.08 and Ni0.05.
Reclaim each valuable metal from the nitric acid leach liquor, keep 80 ℃ of solution temperatures, add 27.5g sodium-chlor and react the 2h filtration, the silver chloride pulp water is washed the back oven dry, the heavy 65.32g of silver chloride slag.Solution after the precipitated silver keeps temperature to add 68g sodium sulfate down for 80 ℃, reaction 2h after-filtration, and the lead sulfate pulp water is washed the back oven dry, the heavy 144.80g of sulfuric acid lead skim.Solution behind the precipitation lead at first is warming up to 95 ℃, and then adjusts pH value of solution=12 with yellow soda ash, reaction 2h after-filtration, copper ashes washing back oven dry, the heavy 625.8g of copper ashes.Nitric acid leach liquor behind the precipitated copper is neutralized to pH=8 with nitric acid, concentrates, decolouring and crystallisation by cooling the SODIUMNITRATE weight 1100.5g of output then; The water vapor that contains low-concentration nitrogen oxide of each operation output is that 10.0% hydrogen peroxide solution absorbs with volumetric concentration, keeps temperature of reaction to be lower than 45 ℃, and when the hydrogen peroxide volumetric concentration was lower than 0.5% in the absorption liquid, absorption liquid returned the dosing of oxidation leaching process.
Claims (2)
1. the method for the plumbous silver-colored material of pollution-free Treatment of Copper is characterized in that concrete steps are as follows:
(1) fragmentation or fragmentation
Pending copper, lead and silver-containing material is broken or be broken into and be fit to the granularity handled, material is powdery, bulk or alloy, is the sieve of 44～420um for powdery and blocky material employing cylindrical mill crusher machine to granularity 100% mistake aperture, and crossing aperture with the fragmentation of high-temperature spray equipment to granularity 100% for alloy material is the sieve of 74～250um;
(2) pollution-free oxidation is leached
The mixing solutions of preparation nitric acid and hydrogen peroxide, the volumetric concentration of nitric acid and hydrogen peroxide is respectively 5.0～20% and 2.5～30% in the control mixing solutions, get this liquor capacity 40～80% and be to add fragmentation that step (1) obtain or material fragmentation after at 3～6: 1 by liquid-solid ratio L/Kg, keep 60～90 ℃ of temperature of reaction, the mixing solutions that slowly adds remaining nitric acid for preparing and hydrogen peroxide, reaction 2～8h after-filtration, other precious metals are reclaimed in leached mud washing back;
(3) silver, lead and copper reclaim step by step
Character according to each metal-salt, add sodium-chlor, sodium sulfate and yellow soda ash successively and reclaim silver, lead and copper in the nitric acid leach liquor respectively, remain 60～95 ℃ of solution temperatures, time 1～4h, the sodium-chlor add-on is that 0.50～0.60 times of silver content, sodium sulfate add-on are 0.55～0.60 times, yellow soda ash add-on control pH value of solution=10～12 of lead content, after-filtration is finished in each reaction, respectively output silver chloride slag, sulfuric acid lead skim and copper ashes;
(4) SODIUMNITRATE reclaims
After the nitric acid leach liquor reclaimed valuable metal, the pH of solution was 10～12, is neutralized to pH value of solution to 7～9 with nitric acid, and then concentrate, decolouring and crystallisation by cooling output SODIUMNITRATE product;
(5) recycling of low-concentration nitrogen oxide
The water vapor that contains low-concentration nitrogen oxide of each operation output, the aqueous solution that employing contains hydrogen peroxide absorbs, keep in the absorption liquid that the hydrogen peroxide volumetric concentration is 2.5～25.0%, 25～55 ℃ of temperature, when hydrogen peroxide volumetric concentration in the absorption liquid is reduced to 0.5% when following, absorption liquid returns the oxidation leaching process.
2. the method for the plumbous silver-colored material of pollution-free Treatment of Copper according to claim 1, it is characterized in that: described nitric acid, hydrogen peroxide, sodium-chlor, sodium sulfate and yellow soda ash are technical grade reagent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363839A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Process for recovering silver, lead and bismuth from silver-bearing soot comprehensively |
| CN104789771A (en) * | 2015-05-06 | 2015-07-22 | 昆明贵益金属材料有限公司 | Valuable metal separation method for complex copper, lead, zinc and silver mixed concentrates |
| CN104911366A (en) * | 2015-05-11 | 2015-09-16 | 湖南众兴环保科技有限公司 | Method for recovering valuable metals from silver-bismuth slag through using aqua regia |
| CN113308609A (en) * | 2021-05-26 | 2021-08-27 | 江苏北矿金属循环利用科技有限公司 | Method for clean recovery and resource utilization of spent silver-containing waste catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4108639A (en) * | 1976-07-09 | 1978-08-22 | Johns-Manville Corporation | Process for recovering platinum group metals from ores also containing nickel, copper and iron |
| CN101353727A (en) * | 2008-09-18 | 2009-01-28 | 西部金属材料股份有限公司 | Method for reclaiming silver and copper in silver-copper alloy scrap |
| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
-
2010
- 2010-07-27 CN CN2010102370325A patent/CN101914681B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4108639A (en) * | 1976-07-09 | 1978-08-22 | Johns-Manville Corporation | Process for recovering platinum group metals from ores also containing nickel, copper and iron |
| CN101353727A (en) * | 2008-09-18 | 2009-01-28 | 西部金属材料股份有限公司 | Method for reclaiming silver and copper in silver-copper alloy scrap |
| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363839A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Process for recovering silver, lead and bismuth from silver-bearing soot comprehensively |
| CN104789771A (en) * | 2015-05-06 | 2015-07-22 | 昆明贵益金属材料有限公司 | Valuable metal separation method for complex copper, lead, zinc and silver mixed concentrates |
| CN104911366A (en) * | 2015-05-11 | 2015-09-16 | 湖南众兴环保科技有限公司 | Method for recovering valuable metals from silver-bismuth slag through using aqua regia |
| CN113308609A (en) * | 2021-05-26 | 2021-08-27 | 江苏北矿金属循环利用科技有限公司 | Method for clean recovery and resource utilization of spent silver-containing waste catalyst |
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