CN101209853A - Method for preparing cupric sulfate from spongy copper and copper-containing acid pickle - Google Patents
Method for preparing cupric sulfate from spongy copper and copper-containing acid pickle Download PDFInfo
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- CN101209853A CN101209853A CNA2007103038072A CN200710303807A CN101209853A CN 101209853 A CN101209853 A CN 101209853A CN A2007103038072 A CNA2007103038072 A CN A2007103038072A CN 200710303807 A CN200710303807 A CN 200710303807A CN 101209853 A CN101209853 A CN 101209853A
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Abstract
The invention relates to a method for preparing copper sulfate by adopting sponge cooper and the waste acid liquid containing cooper as raw materials. The invention is characterized in that (1) sponge cooper and the cooper containing waste acid liquid, after acid adjustment, are emulsified and mixed; then leaching reaction is carried out; (2) the leached liquid is extracted by using P204, and then cooper and nickel are separated from part of impurities; (3) under the help of sulphuric acid, reverse extraction is carried out to the extraction liquid P204, the oil in the reverse extract liquid and extraction raffinate is removed; (4) cooper sulphate solution, after oil removal and purification, is concentrated by steam, crystallized and dried; then the final product cooper sulphate crystal is obtained. The method of the invention has the advantages of good separation effect of cooper and nickel, being capable of fully making use of nonferrous smelting intermediate residue with complex components and the waste acid liquid containing cooper to produce high quality cooper sulphate and reclaim valuable metal nickel, thus achieving resources comprehensive utilization.
Description
Technical field
A kind of is the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, relates to a kind of method of utilizing copper nickel is smelted and refining is produced copper sponge and copper-containing waste acid liquid for feedstock production copper sulfate.
Background technology
At present, producing the main production technique of copper sulfate has: 1. be raw material with purple composition brass, with the dilute sulphuric acid leaching, again the solution concentration crystallization obtained copper sulfate after being sintered into cupric oxide; This method technical process complexity, labour intensity is big, the energy consumption height; 2. produced the production technique of copper sulfate by copper-sulphide ores, comprise processes such as breeze roasting, the leaching of calcining copper, crystallisation by cooling, the total recovery of copper sulfate can reach more than 96%; 3. with delafossite wet method direct production copper sulfate process, be specially adapted to delafossite wet production copper sulfate and byproduct thereof based on chalcopyrite, ventilation breather or cupric oxide---copper sponge and ferrous sulfate.Its characteristics with breeze add dilute sulphuric acid at normal temperatures in the acidolysis reaction leaching ore deposit copper, iron be copper sulfate, ferrous solution, transfer PH to remove iron ion in the solution with lime white again, getting purified copper-bath, is the copper sulfate product through concentrated, crystallization, drying, and copper recovery can reach 60%～80%.The method that also has other technologies is as sulfuric acid process, chemical condensing crystal method, copper scrap method, electrolytic process, white matte method, cupric oxide method etc.These technology major parts are very ripe, but certain limitation is all arranged, and are suitable for a certain specific raw material and condition.
The copper sponge that copper nickel is smelted and refining is produced be a kind of impurity composition extremely complexity and content high contain copper ashes, contain plurality of impurities such as arsenic, nickel, iron, manganese, zinc, be the intermediates of smelting and refining process impurity open circuit institute output, because the impurity component that contains is many, so can't return the original system recycle, otherwise will cause the pernicious internal recycle of whole production system.And the spent acid solution that copper nickel is smelted and refining is produced comprises the Lix984 copper sulfate strip liquor of cobalt system, the acidic solution of multiple cupric such as copper melting wet dust collector liquid and a large amount of impurity, acid concentration is about 150g/l, because these spent acid contain valuable metal and various heavy metal ion such as a large amount of copper, nickel, acid concentration is higher again, used so both can't continue to return in smelting and the rectification systems, also can't directly discharge.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively overcome copper sponge and copper-containing waste acid liquid dopant species complexity and the big shortcoming of foreign matter content that copper nickel is smelted and refining is produced, and effective various valuable metals of comprehensive reutilization provide a kind of method of utilizing copper nickel is smelted and refining is produced copper sponge and copper-containing waste acid liquid for feedstock production copper sulfate.
The objective of the invention is to be achieved through the following technical solutions.
A kind of is the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that its step comprises:
(1) copper sponge and copper-containing waste acid liquid are carried out acid adjustment after emulsification mix, leach reaction;
(2) will leach back liquid P
204Collection copper makes copper separate with partial impurities with nickel;
(3) with P
204Get liquid sulfuric acid back extraction, with strip liquor and raffinate oil removing;
(4) to extracting except that the copper-bath after the oil purification concentrates at steam, crystallization, drying makes copper sulfate crystal.
Of the present invention a kind of be the method for feedstock production copper with copper sponge and copper-containing waste acid liquid, it is characterized in that described copper-containing waste acid liquid comprises that copper smelts wet dust collector liquid, the anode sludge and reclaim copper nickel solution and electrolysis peracid copper sulfate solution behind the selenium.
Of the present invention a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described copper sponge and copper-containing waste acid liquid carrying out after the acid adjustment emulsification, to mix the solid-to-liquid ratio (weight ratio) that leaches reaction be 1: 3, leaches to contain H in mixing
2SO
4Amount is 120～140g/l, and extraction temperature is 65 ℃～83 ℃, leaches terminal point H
2SO
4Be 20～35g/l;
Of the present invention a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that it is through floating of high-pressure injector blended that described copper sponge and copper-containing waste acid liquid carry out after the acid adjustment that emulsification mixes.
Of the present invention a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described P
204Strip liquor and raffinate carry out the Cu in the strip liquor after the oil removing
2+Be 70～100g/l, Fe
2+≤ 0.01g/l, Ni
2+≤ 0.05g/l, PH:2.0～3.0, oil content≤5 * 10
-3Mg/l; P after the oil removing
204Raffinate specification of quality: Cu
2+≤ 0.05g/l, oil content≤10
-2Mg/l.
Of the present invention a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described extraction is 0.2～0.4MPa except that the copper-bath after the oil purification at the vapor pressure of steam concentration process, vacuum tightness is that 0.02～0.05MPa. evaporation terminal point density is 1.48～1.52 * 10
3Kg/m
3, cool 25～35 ℃, after the liquid-solid separation of vacuum filtration, obtain copper sulfate crystal.
Of the present invention a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described leaching back liquid P
204Extraction realizes the separation of copper and mickel, partial impurities, adds yellow soda ash in the raffinate behind the collection copper and gets Ni
2(OH)
2CO
3Precipitation, reaction end PH:8.0～8.5, the reaction end temperature: 50～60 ℃, supernatant liquor contains Ni
2+≤ 0.03g/l, slag liquid Separation and Recovery nickel.
Method of the present invention based on principle be under suitable temperature, following phase reaction: 2Cu+2H takes place in elemental copper in the copper sponge and sulfuric acid, airborne oxygen
2SO
4+ O
2=2CuSO
4+ 2H
2O; Simultaneously, following reaction: CuO+H takes place in copper that exists with oxidizing substance in the copper sponge and sulfuric acid
2SO
4=CuSO
4+ H
2O, after the reaction, the copper that exists with simple substance and oxidised form in the copper sponge enters in the infusion solution, and the copper that exists with sulphided form enters into leached mud.Leach back liquid and contain about sour 20g/l, cupric is about 90g/l, for reaching P
204To the extraction process technical requirements, need neutralize and fall acid and dilution.Neutralizing agent is a yellow soda ash.Reaction equation is: Na
2CO
3+ H
2SO
4=Na
2SO
4+ H
2O+CO
2↑; Thinner is a water, and dilution back liquid composition requires: Cu
2+: 58～65g/l, PH:1.0～2.0.
After the copper sponge acidleach, main impurity element is a nickel, can reach copper nickel by extraction and separate, because P
204The order that extracts various metals is: H
+＞Fe
3+＞Zn
2+＞Ca
2+＞Mn
2+＞Co
2+＞Ni
2+P
204Selectivity to copper and mickel is good, and P
204Be easy to and the water layering; Be convenient to recycling.So extraction agent is elected P as
204(chemical name is a di-(2-ethylhexyl)phosphoric acid, is a kind of organic monoacid) is because extraction constantly discharges H
+(Me
N++ (HR)=MeRn+nH
+), for keeping extraction process PH balance, be to P
204Carry out extracting again after the saponification.React as follows: HR+NaOH=NaR+H
2O; NNaR+Me
N+=MeRn+nNa
+The whole displacements of soda soap are converted into Copoloid, pass through 1.0mol/lH again
2SO
4Washing, the small part nickel soap in the Copoloid is replaced into water, and Copoloid is through 2.0mol/lH
2SO
4Back extraction obtains purified copper sulfate strip liquor, reaches copper nickel and separates.For the P of impurity (as iron, zinc, manganese etc.) that made load
204Holomorphosis, with the salt acid elution back extraction of 6mol/l, its reaction equation is: MeR+nHCl=MeCln+n (HR).P
204Nickel in the single nickel salt raffinate, available industrial sodium carbonate precipitates: 2Na
2CO
3+ 2NiSO
4+ H
2O=Ni
2(OH)
2CO
3+ 2Na
2SO
4+ CO
2↑.Adopt the churned mechanically mode of steam heating in reactive tank, nickel to be precipitated on the technology,, reach the purpose that reclaims nickel after filter-press residues liquid separates.
Method of the present invention, employing be multi-stage counter current extraction, equipment can provide excellent contact chance and mechanical separation for two liquid phases for mixing the clarification extraction box, the throughput ratio of two liquid phases can in very large range change.And be easy to go into operation and stop work unlikely damage quality product.
In order to obtain purified strip liquor and raffinate, must carry out oil removing.Pass through ultrasonic wave oil removing, oil removal by air bubbling and fibrous nodules oil removing successively.Ultrasonic wave is meant that frequency is higher than the sound wave of 20kHz.The ultrasonic wave oil removing mainly is to carry out breakdown of emulsion and remove most of suspension oil, dispersed oil in the solution.Oil removal by air bubbling is to utilize efficient dissolved air release, in solution, produce the trickle bubble of sufficient amount, suspended particles (suspension elaioleucite) adhere to mutually in trickle bubble and the solution, form global density " bubble-particle " complex body less than solution, make suspended particles float to the solution face with bubble.But the strong adsorptivity degree of depth of fibrous nodules is removed the oil content in the solution, makes in the solution oleaginousness less than 10
-3Mg/l.
Method of the present invention, can effectively utilize copper sponge and the copper-containing waste acid liquid that copper nickel is smelted and refining is produced is that feedstock production goes out high-quality copper sulfate, and be reached for the purpose that impurity formation is opened a way in smelting and the refining process, can reach the rational distribution of resources and obtain the certain economic environmental benefit.
Embodiment
A kind of is the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, and its step comprises:
(1) copper sponge and copper-containing waste acid liquid are carried out acid adjustment after high-pressure injector carries out emulsification mixes, leach reaction; The solid-to-liquid ratio (weight ratio) that leaches reaction is 1: 3, contains H in the liquid before leaching
2SO
4Amount is 120～140g/l, and extraction temperature is 65 ℃～83 ℃, leaches terminal point and contains H
2SO
4Be 20～35g/l;
(2) will leach back liquid P
204Collection copper makes copper separate with partial impurities with nickel;
(3) with P
204Extraction liquid sulfuric acid back extraction is with strip liquor and raffinate oil removing; Cu in the strip liquor after the oil removing
2+Be 70～100g/l, Fe
2+≤ 0.01g/l, Ni
2+≤ 0.05g/l, PH:2.0～3.0, oil content≤5 * 10
-3Mg/l; P after the oil removing
204Raffinate specification of quality: Cu
2+≤ 0.05g/l, oil content≤10
-2Mg/l;
(4) steam concentrates, crystallization except that the copper-bath after the oil purification carries out to extraction, and drying makes copper sulfate crystal; The vapor pressure of steam concentration process is 0.2～0.4MPa, and vacuum tightness is 0.02～0.05MPa.Evaporation terminal point density is 1.48～1.52 * 10
3Kg/m
3, cool 25～35 ℃, after the liquid-solid separation of vacuum filtration, obtain copper sulfate crystal.
Embodiment 1
(the molten bronze, brass or copper ware with separate unit 2t/d is an example)
The dried copper sponge that will contain Cu:62.6%, Ni:3.2%, Fe:0.05%, Pb:0.02%, Ca:0.32%, As:0.35%, Sb:0.026%, Bi:0.019%, S:2.5%, Cl:2.2% is milled to-10 orders (being equivalent to 0.016mm) and accounts for 90%, add continuously with the speed of screw feeder, pump into and contain Cu with 220kg/h
2+: 32g/l contains H
2SO
4: liquid before the leaching of 120g/l, with 0.65m
3The speed of/h adds molten bronze, brass or copper ware continuously.Temperature of reaction is controlled at about 80 ℃.Leach to such an extent that contain Cu continuously
2+: 97g/l, H
2SO
4: the leach liquor 0.65m of 26g/l
3/ h.After a press filtration, add Na to liquid in-out
2CO
3Acid falls in neutralization, and process temperature is controlled at 40～70 ℃, PH:2.0.After the secondary press filtration, thin up is to containing Cu
2+: 63g/l contains Ni
2+: 20g/l, again through after three press filtrations, adopt extraction agent P
204Carry out multi-stage counter current extraction and oil removing, must contain Cu
2+: 93g/l, Fe
2+: 0.006g/l, Ni
2+: 0.01g/l, oil content: 3 * 10
-3Mg/l, the strip liquor of PH:2.6.Must contain Cu
2+: 0.035g/l, oil content: 5 * 10
-3The raffinate of mg/l.Strip liquor carries out economic benefits and social benefits vacuum-evaporation after the oil removing, and density reaches 1.48 * 10
3Kg/m
3The time, transfer to the crystallizer crystallisation by cooling terminal temperature: 32 ℃.Carry out to contain Cu:98.13% and the qualified plating grade bluestone crystal of other elements after centrifugal and dry.
Embodiment 2
(the molten bronze, brass or copper ware with separate unit 2t/d is an example)
The dried copper sponge that will contain Cu:60.5%, Ni:3.5%, Fe:0.06%, Pb:0.02%, Ca:0.13%, As:0.4%, Sb:0.024%, Bi:0.025%, S:2.8%, Cl:2.3% is milled to-10 orders (being equivalent to 0.016mm) and accounts for 90%, add continuously with the speed of screw feeder, pump into and contain Cu with 230kg/h
2+: 38g/l contains H
2SO
4: liquid before the leaching of 130g/l, with 0.7m
3The speed of/h adds molten bronze, brass or copper ware continuously.Temperature of reaction is controlled at about 83 ℃.Leach to such an extent that contain Cu continuously
2+: 95g/l, H
2SO
4: the leach liquor 0.7m of 32g/l
3/ h.After a press filtration, add Na to liquid in-out
2CO
3Acid falls in neutralization, and process temperature is controlled at 40～70 ℃, PH:1.6.After the secondary press filtration, thin up is to containing Cu
2+: 62g/l contains Ni
2+: 18g/l, again through after three press filtrations, adopt extraction agent P
204Carry out multi-stage counter current extraction and oil removing, must contain Cu
2+: 90g/l, Fe
2+: 0.008g/l, Ni
2+: 0.03g/l, oil content: 3 * 10
-3Mg/l, the strip liquor of PH:2.5.Must contain Cu
2+: 0.07g/l, oil content: 7 * 10
-3The raffinate of mg/l.Strip liquor carries out economic benefits and social benefits vacuum-evaporation after the oil removing, and density reaches 1.5 * 10
3Kg/m
3The time, transfer to the crystallizer crystallisation by cooling terminal temperature: 35 ℃.Carry out to contain Cu:98.86% and the qualified plating grade bluestone crystal of other elements after centrifugal and dry.
Embodiment 3
(the molten bronze, brass or copper ware with separate unit 2t/d is an example)
The dried copper sponge that will contain Cu:62.3%, Ni:3.1%, Fe:0.05%, Pb:0.03%, Ca:0.16%, As:0.56%, Sb:0.027%, Bi:0.029%, S:3.3%, Cl:2.4% is milled to-10 orders (being equivalent to 0.016mm) and accounts for 90%, add continuously with the speed of screw feeder, pump into and contain Cu with 250kg/h
2+: 32g/l contains H
2SO
4: liquid before the leaching of 140g/l, with 0.8m
3The speed of/h adds molten bronze, brass or copper ware continuously.Temperature of reaction is controlled at about 78 ℃.Leach to such an extent that contain Cu continuously
2+: 96g/l, H
2SO
4: the leach liquor 0.8m of 28g/l
3/ h.After a press filtration, add Na to liquid in-out
2CO
3Acid falls in neutralization, and process temperature is controlled at 40～70 ℃, PH:1.5.After the secondary press filtration, thin up is to containing Cu
2+: 60g/l contains Ni
2+: 17g/l, again through after three press filtrations, adopt extraction agent P
204Carry out multi-stage counter current extraction and oil removing, must contain Cu
2+: 86g/l, Fe
2+: 0.006g/l, Ni
2+: 0.02g/l, oil content: 2 * 10
-3Mg/l, the strip liquor of PH:2.8.Obtain containing Cu
2+: 0.04g/l, oil content: 7 * 10
-3The raffinate of mg/l.Strip liquor carries out economic benefits and social benefits vacuum-evaporation after the oil removing, and density reaches 1.52 * 10
3Kg/m
3The time, transfer to the crystallizer crystallisation by cooling terminal temperature: 30 ℃.Carry out to contain Cu:98.23% and the qualified plating grade bluestone crystal of other elements after centrifugal and dry.
Claims (7)
1. one kind is the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that its step comprises:
(1) copper sponge and copper-containing waste acid liquid are carried out acid adjustment after emulsification mix, leach reaction;
(2) will leach back liquid P
204Collection copper makes copper separate with partial impurities with nickel;
(3) with P
204Get liquid sulfuric acid back extraction, with strip liquor and raffinate oil removing;
(4) to extracting except that the copper-bath after the oil purification concentrates at steam, crystallization, drying makes copper sulfate crystal.
2. according to claim 1 a kind of be the method for feedstock production copper with copper sponge and copper-containing waste acid liquid, it is characterized in that described copper-containing waste acid liquid comprises that copper smelts wet dust collector liquid, the anode sludge and reclaim copper nickel solution and electrolysis peracid copper sulfate solution behind the selenium.
3. according to claim 1 a kind of be the method for feedstock production copper with copper sponge and copper-containing waste acid liquid, it is characterized in that described copper sponge and copper-containing waste acid liquid carrying out after the acid adjustment emulsification, to mix the solid-liquid weight ratio that leaches reaction be 1: 3, contains H in the liquid before leaching
2SO
4Amount is 120～140g/l, and extraction temperature is 65 ℃～83 ℃, leaches terminal point and contains H
2SO
4Be 20～35g/l.
4. according to claim 1 a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that it is through floating of high-pressure injector blended that described copper sponge and copper-containing waste acid liquid carry out after the acid adjustment that emulsification mixes.
5. according to claim 1 a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described P
204Strip liquor and raffinate carry out the Gu in the strip liquor after the oil removing
2+Be 70～100g/l, Fe
2+≤ 0.01g/l, Ni
2+≤ 0.05g/l, PH:2.0～3.0, oil content≤5 * 10
-3Mg/l; P after the oil removing
204Raffinate specification of quality: Cu
2+≤ 0.05g/l, oil content≤10
-2Mg/l.
6. according to claim 1 a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described extraction is 0.2～0.4MPa except that the copper-bath after the oil purification at the vapor pressure of steam concentration process, vacuum tightness is that 0.02～0.05MPa. evaporation terminal point density is 1.48～1.52 * 10
3Kg/m
3, cool 25～35 ℃, after the liquid-solid separation of vacuum filtration, obtain copper sulfate crystal.
7. according to claim 1 a kind of be the method for feedstock production copper sulfate with copper sponge and copper-containing waste acid liquid, it is characterized in that described leaching back liquid P
204Extraction realizes the separation of copper and mickel, partial impurities, adds yellow soda ash in the raffinate behind the collection copper and obtains Ni
2(OH)
2CO
3Precipitation, reaction end PH:8.0～8.5, the reaction end temperature: 50～60 ℃, supernatant liquor contains Ni
2+≤ 0.03g/l, slag liquid Separation and Recovery nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007103038072A CN101209853B (en) | 2007-12-25 | 2007-12-25 | Method for preparing cupric sulfate from spongy copper and copper-containing acid pickle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007103038072A CN101209853B (en) | 2007-12-25 | 2007-12-25 | Method for preparing cupric sulfate from spongy copper and copper-containing acid pickle |
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| Publication Number | Publication Date |
|---|---|
| CN101209853A true CN101209853A (en) | 2008-07-02 |
| CN101209853B CN101209853B (en) | 2010-07-21 |
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|---|---|---|---|
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| CN102145908A (en) * | 2011-02-24 | 2011-08-10 | 山东三丰集团股份有限公司 | Aluminum sulfate filter-pressing and deslagging process |
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| CN101974689A (en) * | 2010-09-26 | 2011-02-16 | 金川集团有限公司 | Method for processing material containing copper |
| CN102145908A (en) * | 2011-02-24 | 2011-08-10 | 山东三丰集团股份有限公司 | Aluminum sulfate filter-pressing and deslagging process |
| CN102732729A (en) * | 2012-06-27 | 2012-10-17 | 金川集团有限公司 | Method for removing nickel and copper from high nickel copper anode mud |
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| CN103866139A (en) * | 2012-12-18 | 2014-06-18 | 宁波金田铜业(集团)股份有限公司 | Method for evaporation-free preparation of zinc sulfate from brass slag material |
| CN103924085A (en) * | 2014-03-25 | 2014-07-16 | 宁波金田铜业(集团)股份有限公司 | Method for recovering copper zinc nickel from heavy metal sludge by using copper smelting waste acid |
| CN105039695A (en) * | 2014-12-16 | 2015-11-11 | 铜陵翔宇商贸有限公司 | Extraction method of extracting copper sulfate from waste copper liquid |
| CN105039695B (en) * | 2014-12-16 | 2017-06-13 | 安徽格太信控科技有限公司 | The extracting process of copper sulphate is extracted from waste copper liquid |
| CN107460341A (en) * | 2017-08-04 | 2017-12-12 | 俞振元 | The method that recovery prepares cupric sulfate purified from copper containing scrap |
| WO2020211757A1 (en) * | 2019-04-16 | 2020-10-22 | 中国恩菲工程技术有限公司 | Method for recovering copper from phosphoric acid extractant-containing solution |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101209853B (en) | 2010-07-21 |
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