CN104611572A - Method for preparing copper sulfate through wet oxidation of copper concentrate - Google Patents

Method for preparing copper sulfate through wet oxidation of copper concentrate Download PDF

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Publication number
CN104611572A
CN104611572A CN201510016716.5A CN201510016716A CN104611572A CN 104611572 A CN104611572 A CN 104611572A CN 201510016716 A CN201510016716 A CN 201510016716A CN 104611572 A CN104611572 A CN 104611572A
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China
Prior art keywords
copper
reaction
sulfate
solution
wet oxidation
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CN201510016716.5A
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Chinese (zh)
Inventor
吴江渝
刘曙
张勇
谈华新
王西兵
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武汉工程大学
武汉钢铁集团矿业有限责任公司程潮铁矿
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Priority to CN201510016716.5A priority Critical patent/CN104611572A/en
Publication of CN104611572A publication Critical patent/CN104611572A/en

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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention relates to a method for preparing copper sulfate through wet oxidation of copper concentrate. The method comprises the following steps: (1) firstly, dispersing ground copper concentrate powder into a leaching solution, regulating a pH value to 1-2 by using dilute sulphuric acid, adding an oxidizer, and introducing air for leaching copper ions; (2) filtering a solution to obtain a filtrate containing copper ions, adding scrap iron to the filtrate to be used as a displacer, regulating the pH value of the obtained displacement liquid by using sulphuric acid, performing reaction, and performing constant temperature roasting to obtain copper oxide powder; (3) performing pickling reaction on the obtained copper oxide powder to prepare the copper sulfate. The method disclosed by the invention has the advantages that (1) the method is simple, the operation is easy, the energy consumption is low, and the leaching efficiency of copper in ores can reach 98% or more; (2) the purity of spongy copper can reach 90%; (3) the cyclic utilization during production is realized; (4) the leaching efficiency of copper oxide can reach 97% or more. The copper sulfate solution is concentrated and crystallized so as to obtain cupric sulfate pentahydrate crystals of which the purity can reach 97% or more.

Description

A kind of copper ore concentrates wet oxidation prepares the method for copper sulfate
Technical field
The present invention relates to a kind of method that copper ore concentrates wet oxidation prepares copper sulfate, belong to wet processes copper ore concentrates field.
Background technology
Cupric sulfate pentahydrate is important copper compound, and purposes is different with purity, and it all has been widely used in petrochemical complex, chemical industry, dyestuffs industries, coatings industry, electroplating industry, agricultural, medicine, food etc.The production of copper sulfate is mainly derived from selecting and purchasing and the smelting of copper mine.Along with the progress of science and technology, energy consumption, efficiency, environmental protection etc. require more and more higher, and this just makes existing copper sulfate production technique receive impact, finds new production method imperative.
The distinguishing feature of Mineral Resources in China is that low-grade, complicated refractory ore is in the majority.Tradition selecting and purchasing smelting process is when processing these low-grade complex Mineral resources, and efficiency is low, long flow path, cost are high, pollution is heavy.The development that these problems force mineral to process science and technology is faced with new challenges, and must strengthen fundamental research and new technology development.At present, the object of copper metallurgy industry is the Copper Ores based on copper glance mostly, and the abundantest Low-grade primary cooper sulfide ore of reserves due to leaching efficiency low, the production cycle is long, is difficult to large-scale application, and this is the bottleneck of industry development.
Copper-sulphide ores is with chalcopyrite (CuFeS 2) the most important, distribute the most extensive simultaneously, the slag produced in the process of large scale mining sulfide mineral and mine tailing, acidic mine waste water can be generated by rapid oxidation under the effect of microorganism, often there is stronger acidity, and be rich in vitriol and heavy metal, to the ecotope of mining area and surrounding area, there is very large harm, become one of environmental problem that people pay close attention to the most.
In recent years, along with the decline gradually of Copper Ores mining grade, the increase of difficult mining seam and fluctuating widely of the common concern to the environmental pollution that sulfurous gas causes, particularly copper valency make people more and more pay attention to hydrometallurgical technology.Chalcopyrite is the most frequently used raw material in copper smelt industry, therefore adopts hydrometallurgical technology process chalcopyrite to be the problem most with realistic meaning concerning metallargist.It is low that hydrometallurgical processes process chalcopyrite has operational cost, and oxidation rate is fast, and decompose sulfide thorough, environmental pollution is little, and the rate of recovery is advantages of higher comparatively.
Summary of the invention
Technical problem to be solved by this invention proposes a kind of method that copper ore concentrates wet oxidation prepares copper sulfate, and it is high that the method has cupric ion leaching yield, and product purity is high, and energy consumption is lower, the feature of easy handling.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of copper ore concentrates wet oxidation prepares the method for copper sulfate, includes following steps:
1) be first dispersed in infusion solution by the copper concentrate powder of milled, pulp density maintains 1% ~ 10%, by dilute sulphuric acid adjust ph 1 ~ 2, adds oxygenant, passes into air and carries out cupric ion Leaching reaction, air dividing potential drop 0.1 ~ 1MPa;
2) by step 1) solution obtain the filtrate of copper ions after filtration, add iron filings wherein as displacer, and regulate the pH value of gained displacement liquid with sulfuric acid, react, then be placed in retort furnace constant temperature calcining by cleaning, drying the copper sponge obtained, obtain cupric oxide powder;
3) cupric oxide powder obtained is carried out acid-leaching reaction and prepare copper sulfate.
By such scheme, the copper ore concentrates that described copper ore concentrates is produced for cheng chao Iron Mine.
By such scheme, step 1) described in oxygenant be ferric sulfate, add ferric sulfate amount meet Fe 3+/ Cu=1 ~ 3.
By such scheme, step 1) described in temperature of reaction be 70 ~ 100 DEG C, reaction times 1 ~ 5h.
By such scheme, step 2) described in iron filings add-on be 1 ~ 3 times of theoretical amount.
By such scheme, step 2) described in pH value be 1 ~ 3, temperature of reaction 30 ~ 60 DEG C, reaction times 1 ~ 5h.
By such scheme, step 2) described in calcination temperature 400 ~ 800 DEG C, reaction times 1 ~ 5h.
By such scheme, step 3) described in cupric oxide powder carry out acid-leaching reaction and prepare copper sulfate concrete steps and be: maintaining liquid-solid ratio in acid-leaching reaction system is 1:1 ~ 5:1, and adjust ph 1 ~ 3, temperature of reaction 70 ~ 100 DEG C, reaction times 1 ~ 5h; The cupric oxide leach liquor obtained filters, filtrate adds between vitriol oil control ph 2.5 ~ 3.0, evaporation concentration is carried out at 90 ~ 100 DEG C of temperature, stop transpiring moisture when epitaxial appears in solution surface and start whipping appts, control cooling rate and stirring velocity, namely solution obtain cupric sulfate pentahydrate crystal through concentrated, crystallization.
Compared with prior art, advantage of the present invention is:
1) with ferric ion and air for oxygenant carries out wet-leaching to copper ore concentrates, method is simple, and easily operate, energy consumption is low, and in ore, the leaching yield of copper can reach more than 98%;
2) be that copper sponge prepared by displacer with iron filings, method is simple, and by controlling permutizer condition, the rate of displacement of copper sponge can reach more than 95%, and copper sponge purity can reach 90%;
3), in the displacement liquid that copper sponge preparation obtains, main sulfur acid is ferrous, passes into air wherein, be oxidized by ferrous sulfate, obtain ferric ion solution, the leaching being circulated to the first step copper uses, effectively reduce discharging of waste liquid, achieve the recycle in production;
4) copper sponge produces cupric oxide through roasting oxidation, and cupric oxide acidleach obtains copper-bath, and the leaching yield of cupric oxide can reach more than 97%.Copper-bath, can obtain cupric sulfate pentahydrate crystal through concentrated, crystallization, its purity can reach more than 97%.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Wuhan iron & steel croup co. mining company cheng chao Iron Mine copper ore concentrates composition of ores is analyzed as follows:
Element term Fe S Cu Ag
Content (quality %) 48.55% 32.40% 13.92% 5.13%
Copper content about about 14% in cheng chao Iron Mine copper ore concentrates ore as can be seen from the table, Cu Concentrate Grade is not high not low yet, and the wet oxidation route of improvement can be adopted to process.
Embodiment 1:
1) be first dispersed in infusion solution by the wuhan iron & steel croup co. mining company cheng chao Iron Mine copper concentrate powder of milled, pulp density is 5%, and be 2 by dilute sulphuric acid regulator solution pH value, add ferric sulfate, wherein ferric sulfate consumption meets Fe 3+/ Cu=1.5, passes into air and carries out cupric ion leaching, air dividing potential drop 0.6MPa, temperature of reaction 90 DEG C, reaction times 2h.Cupric ion leaching yield is 98.1%.
2) solution after copper ore concentrates wet oxidation filters, and in gained filtrate, add iron filings as displacer, described iron filings add-on meets Fe/Cu 2+=2, be 2 by sulfuric acid regulation solution pH value, temperature of reaction 40 DEG C, reaction times 2h.Constantly stir in reaction process, until reaction terminates.Solution left standstill certain hour, after the foam copper precipitation of shape loose in solution, takes out throw out and washes, dries and namely obtain copper sponge.Copper sponge purity is 90.5%.
3) copper sponge cleaned, dry is placed in retort furnace constant temperature calcining, temperature of reaction 600 DEG C, reaction times 2h, obtains cupric oxide powder.
4) cupric oxide powder carries out acid-leaching reaction.Reaction system liquid-solid ratio 2:1, regulator solution pH value is 2, temperature of reaction 90 DEG C, reaction times 2h.Filtered by solution, filtrate pH value controls, between 2.5 ~ 3.0, at 90 DEG C, to carry out evaporation concentration, and stop transpiring moisture when epitaxial appears in solution surface and start stirring, solution obtains cupric sulfate pentahydrate product through condensing crystal.Cupric sulfate pentahydrate crystal purity is 97.3%.
Embodiment 2:
1) be first dispersed in infusion solution by the wuhan iron & steel croup co. mining company cheng chao Iron Mine copper concentrate powder of milled, pulp density 1%, be 2 by dilute sulphuric acid regulator solution pH value, add ferric sulfate, wherein ferric sulfate consumption meets Fe 3+/ Cu=1, passes into air and carries out cupric ion leaching, air dividing potential drop 0.1MPa, temperature of reaction 100 DEG C, reaction times 1h.Cupric ion leaching yield is 95.2%.
2) solution after copper ore concentrates wet oxidation filters, and in gained filtrate, add iron filings as displacer, described iron filings add-on meets Fe/Cu 2+=1, be 3 by sulfuric acid regulation solution pH value, temperature of reaction 30 DEG C, reaction times 1h.Constantly stir in reaction process, until reaction terminates.Solution left standstill certain hour, after the foam copper precipitation of shape loose in solution, takes out throw out and washes, dries and namely obtain copper sponge.Copper sponge purity is 88.2%.
3) copper sponge cleaned, dry is placed in retort furnace constant temperature calcining, temperature of reaction 800 DEG C, reaction times 1h, obtains cupric oxide powder.
4) cupric oxide powder carries out acid-leaching reaction.Reaction system liquid-solid ratio 1:1, regulator solution pH value is 3, temperature of reaction 70 DEG C, reaction times 1h.Filtered by solution, filtrate pH value controls, between 2.5 ~ 3.0, at 90 DEG C, to carry out evaporation concentration, and stop transpiring moisture when epitaxial appears in solution surface and start stirring, solution obtains cupric sulfate pentahydrate product through condensing crystal.Cupric sulfate pentahydrate crystal purity is 96.5%.
Embodiment 3:
1) be first dispersed in infusion solution by the wuhan iron & steel croup co. mining company cheng chao Iron Mine copper concentrate powder of milled, pulp density is 10%, and be 1 by dilute sulphuric acid regulator solution pH value, add ferric sulfate, wherein ferric sulfate consumption meets Fe 3+/ Cu=3, passes into air and carries out cupric ion leaching, air dividing potential drop 1MPa, temperature of reaction 90 DEG C, reaction times 5h.Cupric ion leaching yield is 97.4%.
2) solution after copper ore concentrates wet oxidation filters, and in gained filtrate, add iron filings as displacer, described iron filings add-on meets Fe/Cu 2+=3, be 1 by sulfuric acid regulation solution pH value, temperature of reaction 60 DEG C, reaction times 2h.Constantly stir in reaction process, until reaction terminates.Solution left standstill certain hour, after the foam copper precipitation of shape loose in solution, takes out throw out and washes, dries and namely obtain copper sponge.Copper sponge purity is 90.2%.
3) copper sponge cleaned, dry is placed in retort furnace constant temperature calcining, temperature of reaction 400 DEG C, reaction times 3h, obtains cupric oxide powder.
4) cupric oxide powder carries out acid-leaching reaction.Reaction system liquid-solid ratio 3:1, regulator solution pH value is 1, temperature of reaction 90 DEG C, reaction times 2h.Filtered by solution, filtrate pH value controls, between 2.5 ~ 3.0, at 100 DEG C, to carry out evaporation concentration, and stop transpiring moisture when epitaxial appears in solution surface and start stirring, solution obtains cupric sulfate pentahydrate product through condensing crystal.Cupric sulfate pentahydrate crystal purity is 97.0%.
Embodiment 4:
1) be first dispersed in infusion solution by the wuhan iron & steel croup co. mining company cheng chao Iron Mine copper concentrate powder of milled, pulp density is 7%, and be 1.5 by dilute sulphuric acid regulator solution pH value, add ferric sulfate, wherein ferric sulfate consumption meets Fe 3+/ Cu=2.5, passes into air and carries out cupric ion leaching, air dividing potential drop 0.4MPa, temperature of reaction 85 DEG C, reaction times 3h.Cupric ion leaching yield is 96.6%.
2) solution after copper ore concentrates wet oxidation filters, and in gained filtrate, add iron filings as displacer, described iron filings add-on meets Fe/Cu 2+=1.5, be 2 by sulfuric acid regulation solution pH value, temperature of reaction 50 DEG C, reaction times 3h.Constantly stir in reaction process, until reaction terminates.Solution left standstill certain hour, after the foam copper precipitation of shape loose in solution, takes out throw out and washes, dries and namely obtain copper sponge.Copper sponge purity is 86.8%.
3) copper sponge cleaned, dry is placed in retort furnace constant temperature calcining, temperature of reaction 700 DEG C, reaction times 2h, obtains cupric oxide powder.
4) cupric oxide powder carries out acid-leaching reaction.Reaction system liquid-solid ratio 2:1, regulator solution pH value is 1.5, temperature of reaction 90 DEG C, reaction times 1h.Filtered by solution, filtrate pH value controls, between 2.5 ~ 3.0, at 95 DEG C, to carry out evaporation concentration, and stop transpiring moisture when epitaxial appears in solution surface and start stirring, solution obtains cupric sulfate pentahydrate product through condensing crystal.Cupric sulfate pentahydrate crystal purity is 95.8%.

Claims (8)

1. copper ore concentrates wet oxidation prepares a method for copper sulfate, includes following steps:
1) be first dispersed in infusion solution by the copper concentrate powder of milled, pulp density maintains 1% ~ 10%, by dilute sulphuric acid adjust ph 1 ~ 2, adds oxygenant, passes into air and carries out cupric ion Leaching reaction, air dividing potential drop 0.1 ~ 1MPa;
2) by step 1) solution obtain the filtrate of copper ions after filtration, add iron filings wherein as displacer, and regulate the pH value of gained displacement liquid with sulfuric acid, react, then be placed in retort furnace constant temperature calcining by cleaning, drying the copper sponge obtained, obtain cupric oxide powder;
3) cupric oxide powder obtained is carried out acid-leaching reaction and prepare copper sulfate.
2. iron ore copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that the copper ore concentrates that described copper ore concentrates is produced for cheng chao Iron Mine.
3. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 1) described in oxygenant be ferric sulfate, add ferric sulfate amount meet Fe 3+/ Cu=1 ~ 3, molar ratio computing.
4. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 1) described in temperature of reaction be 70 ~ 100 DEG C, reaction times 1 ~ 5h.
5. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 2) described in iron filings add-on be 1 ~ 3 times of theoretical amount.
6. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 2) described in pH value be 1 ~ 3, temperature of reaction 30 ~ 60 DEG C, reaction times 1 ~ 5h.
7. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 2) described in calcination temperature 400 ~ 800 DEG C, reaction times 1 ~ 5h.
8. copper ore concentrates wet oxidation according to claim 1 prepares the method for copper sulfate, it is characterized in that step 3) described in cupric oxide powder carry out acid-leaching reaction and prepare copper sulfate concrete steps and be: maintaining liquid-solid ratio in acid-leaching reaction system is 1:1 ~ 5:1, and adjust ph 1 ~ 3, temperature of reaction 70 ~ 100 DEG C, reaction times 1 ~ 5h; The cupric oxide leach liquor obtained filters, filtrate adds between vitriol oil control ph 2.5 ~ 3.0, evaporation concentration is carried out at 90 ~ 100 DEG C of temperature, stop transpiring moisture when epitaxial appears in solution surface and start whipping appts, control cooling rate and stirring velocity, namely solution obtain cupric sulfate pentahydrate crystal through concentrated, crystallization.
CN201510016716.5A 2015-01-13 2015-01-13 Method for preparing copper sulfate through wet oxidation of copper concentrate CN104611572A (en)

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CN104911369A (en) * 2015-06-29 2015-09-16 郴州市金贵银业股份有限公司 Method for processing high-copper-silver smelting slag

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CN104911369A (en) * 2015-06-29 2015-09-16 郴州市金贵银业股份有限公司 Method for processing high-copper-silver smelting slag

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