CN101481806A - Method for desulphurization of copper sulfur ore - Google Patents
Method for desulphurization of copper sulfur ore Download PDFInfo
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- CN101481806A CN101481806A CNA2009100762220A CN200910076222A CN101481806A CN 101481806 A CN101481806 A CN 101481806A CN A2009100762220 A CNA2009100762220 A CN A2009100762220A CN 200910076222 A CN200910076222 A CN 200910076222A CN 101481806 A CN101481806 A CN 101481806A
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Abstract
The invention discloses a method for removing sulfur in a copper sulfide ore. The method comprises steps that a fused salt electrolysis process is used for removing the sulfur in the copper sulfide core by using the copper sulfide ore as cathode and fused salt as electrolyte. The fused salt comprise the following two fused salts which are alkaline earth metal chloride fused salt (1) and the blended fused salt of the alkaline earth metal chloride and alkali chloride. In the fused salt electrolysis process, the electrolytic temperature ranges from 700 to 1000 DEG C and the decomposition voltage is 1.6-3.2V. In the method, only the fused salt medium is used for electrolysis and no any waste residue is discharged; and SO2 or CO2 gas is not discharged in the treatment process; the melting temperature of the fused salt can be reduced by using the blended fused salts of CaCl2-NaCl/LiCI with low cost, thus reducing the reaction temperature (working temperature is under 1000 DEG C), further reducing the energy consumption. Compared with the traditional complicated copper smelting technique with long flow, the method causes that not only the active constituents of iron, sulfur can be fully used, but also no waste residue is discharged; the method has no atmospheric pollution, has short process flow, little pollution and low energy consumption.
Description
Technical field
The present invention relates to a kind of method of desulphurization of copper sulfur ore.
Background technology
Traditional from ore the process more complicated of copper smelting.With the chalcopyrite is example, at first washed ore, flux (Wingdale, sand etc.) and fuel (coke, charcoal or hard coal) is mixed, and drops in " airtight " blast furnace, carries out melting about 1000 ℃.So a part of sulphur becomes SO in the ore
2(being used to make sulfuric acid), impurity such as most arsenic, antimony become As
2O
3, Sb
2O
3Deng volatile matter and be removed: 2CuFeS
2+ O
2=Cu
2S+2FeS+SO
2↑.The sulfide of part iron changes oxide compound into: 2FeS+3O
2=2FeO+2SO
2↑.Cu
2S just is fused together with remaining FeS etc. and forms so-called " matte " (mainly by Cu
2S and FeS are lysigenous mutually, and its copper factor is between 20%～50%, and the sulfur-bearing rate is between 23%～27%), FeO is with SiO
2Form slag: FeO+SiO
2=FeSiO
3Slag float over molten matte above, separate easily can be so as to removing a part of impurity.Then, matte is moved in the converter, add and to blast air blow (1100～1300 ℃) behind the flux (quartz sand).At this moment, the FeS in the matte changes FeO earlier into, follows flux in conjunction with slagging, then Cu
2S just changes Cu into
2O, Cu
2O is with Cu
2The S reaction generates blister copper (copper content is about 98.5%), 2Cu
2S+3O
2=2Cu
2O+2SO
2↑, 2Cu
2O+Cu
2S=6Cu+SO
2↑, again blister copper is moved into reverberatory furnace, add flux (quartz sand), bubbling air makes the oxidation of impurities in the blister copper, forms slag and removes with flux.After impurity removes to a certain degree, spray into heavy oil again, the reducing gas such as carbon monoxide that produced by heavy oil combustion make Red copper oxide at high temperature be reduced to copper.
By above copper smelting process as can be seen, the smelting process temperature is higher, and chalcopyrite (CuFeS
2) in component Fe, finally be to be present in not obtain in the slag utilizing, and S is with SO
2Form is overflowed.Copper slag pollutes surrounding environment, and SO
2The effusion of gas is if deal with improperly also and will cause severe contamination to atmosphere.Explore the new copper metallurgical method of new green non-pollution zero release, it is urgently necessary to replace traditional technology, also conforms to the sustainable society development strategy.
Summary of the invention
The method that the purpose of this invention is to provide a kind of desulphurization of copper sulfur ore.
The method of desulphurization of copper sulfur ore provided by the present invention comprises: with copper sulphur ore deposit is that negative electrode, fused salt are ionogen, the step that adopts fused salt electrolysis process that desulfurization is carried out in copper sulphur ore deposit.
In the described fused salt electrolysis process, the fused salt that is adopted can be following two kinds: 1) alkaline earth metal chloride fused salt, 2) fused salt mixt of alkaline earth metal chloride and alkali metal chloride, described alkaline earth metal chloride specifically can be MgCl
2, CaCl
2Or BaCl
2, described alkali metal chloride specifically can be LiCl, NaCl or KCl.
Consider any in general preferred following three kinds of fused salts: 1) calcium chloride fused salt, 2 from cost factor) mole fused salt mixts such as calcium chloride and sodium-chlor, 3) mole fused salt mixts such as calcium chloride and lithium chloride.
In the described fused salt electrolysis process, electrolysis temperature needs specifically to can be 700-1000 ℃ on the temperature of fusion of fused salt that the present invention adopts; Electrolysis voltage need be lower than the decomposition voltage of fused salt that the present invention adopts, and is higher than the decomposition voltage of institute's sulfur compound in the copper sulphur ore deposit simultaneously, specifically can be 1.6-3.2V.
The preparation method of described negative electrode comprises: the agglomerating step is carried out in described copper sulphur ore deposit under the condition of starvation.Described agglomerating temperature is 300-800 ℃, and the described agglomerating time is 1-6 hour.Anticathode copper sulphur ore deposit is carried out sintering and is helped to improve negative electrode intensity, microstructure and porosity or the like, and the desulfuration efficiency of fused salt electrolysis process is had important raising effect.
The preparation method of described negative electrode also comprises: before sintering is carried out in described copper sulphur ore deposit, under 4-20MPa pressure described copper sulphur ore deposit is pressed into sheet or tabular step.Porosity and intensity in order to strengthen compressing tablet during compacting can be added binding agent in copper sulphur breeze end, as polyoxyethylene glycol, wherein, the quality of binding agent is the 1%-5% of copper sulphur mineral amount.
Copper sulphur of the present invention ore deposit comprises copper glance (Cu
2S), covellite (CuS), chalcopyrite (CuFeS
2) and purple copper (Cu
5FeS
4) etc.
When described copper sulphur ore deposit is specially copper glance (Cu
2S) or during covellite (CuS), the electrode preparation of copper glance or covellite can be carried out according to the method described above.
When described copper sulphur ore deposit is specially chalcopyrite (CuFeS
2) or purple copper (Cu
5FeS
4) time, the preparation method of described negative electrode also comprises: with described copper sulphur ore deposit be pressed into sheet or tabular before, under the condition of 300-800 ℃ of starvation, copper sulphur ore deposit heating 1-12 hour (that is: is made CuFeS
2Or Cu
5FeS
4Fully be decomposed into Cu
2The time of S and FeS) step.
With the chalcopyrite is that following decomposition reaction: 2CuFeS can take place example
2=Cu
2S+2FeS+S is because the S boiling point is lower, by the recyclable S that obtains of corresponding condensing equipment.Powder after the chalcopyrite heating is mainly Cu
2S and FeS.Similarly, the decomposition reaction of purple copper is: 2Cu
5FeS
4=5Cu
2S+2FeS+S also can reclaim by corresponding condensing equipment and obtain S.
When the present invention adopts fused salt electrolysis process that desulfurization is carried out in copper sulphur ore deposit, with copper sulphur ore deposit is negative electrode, anode can adopt graphite (or inert anode, as alloy anode, the stannic oxide anode, sintering metal anode and cerium oxide coated anode etc.), electrolytic reaction takes place under certain voltage, can obtain sulphur at the anode place, obtain copper or copper iron mixed powder at the negative electrode place.
Because anode material graphite (C) generates CS with S
2Perhaps the thermodynamic tendency of CS gas is less, and carbon anode hardly can loss in electrolytic process.In addition, different with some other electric deoxidation process, adopt method of the present invention that desulfurization is carried out in copper sulphur ore deposit, even electrolysis time is very long, the coming off also seldom of carbon dust, thus can not cause the microcell short circuit, current efficiency is higher, and can not pollute cathode product (copper or copper iron mixed powder).Anode can not discharge SO
2Perhaps CO
2Gas, but in the fused salt electrolysis process, obtain most sulphur by the condenser collection.
After electrolytic reaction finishes, the negative electrode oven dry is broken, and water, acetone (to copper glance or covellite) supersound washing or use ethanol, acetone (to chalcopyrite or purple copper) supersound washing successively successively, collect the powder that obtains, be copper powder or copper iron mixed powder after the desulfurization.The separation of copper iron mixed powder can be adopted several different methods, and for example wet extraction separates, and mixed powder is dissolved in the dilute sulphuric acid, and following reaction: Fe+H will take place
2SO
4=FeSO
4+ H
2,, can filter and be separated because copper powder does not react with dilute sulphuric acid.Copperas solution can obtain FeSO at-10～20 ℃ of following crystallisation by cooling
47H
2O, i.e. green vitriol also can heat and obtains other molysite products.Thereby make the copper iron component in the raw ore all obtain effective complete utilization, do not have waste residue to produce.
The use of the invention fused salt electrolysis process desulfurization is carried out in copper sulphur ore deposit, sulphur is separated, because SO has been avoided in the intervention that completely cut off oxidizing atmosphere with metal component
2Discharging, reduced possible pollution, thereby realized the complete utilization of three kinds of active principle copper, iron and sulphur in the copper sulphur ore deposit first air, be a kind of new copper metallurgical technology of green non-pollution zero release.The inventive method is only carried out electrolysis by fused-salt medium, without any the discharging of waste residue, and does not discharge SO in the treating processes
2Perhaps CO
2Gas uses cheap CaCl
2-NaCl/LiCl fused salt mixt can reduce the fused salt melt temperature, thereby reduces temperature of reaction (working temperature is below 1000 ℃), has further reduced energy consumption.Compare with traditional long flow path and complicated copper smelting technology, can not only make full use of active principle iron, sulphur does not discharge residue, no topsoil, and also technical process is short, pollutes less, and energy consumption is low.
Description of drawings
Fig. 1 removes the sulphur in the chalcopyrite and the schema of separating copper iron for adopting the inventive method.
Fig. 2 is that copper glance electrode among the embodiment 1 is before electrolytic reaction and 20 hours photo of electrolysis.
Fig. 3 composes for the XRD figure of the cathode product that the copper glance electrolysis different time among the embodiment 1 obtains, wherein: (a) be not electrolytic negative electrode, (b) be the cathode product of electrolysis 2h, (c) be the cathode product of electrolysis 6h, (d) be the cathode product of electrolysis 2h.
The SEM photo of the cathode product that Fig. 4 obtained for the copper glance electrolysis among the embodiment 1 in 24 hours.
Fig. 5 composes for the XRD figure of the cathode product that the copper glance electrolysis among the embodiment 2 obtained in 20 hours.
The cathode product that Fig. 6 obtains for the chalcopyrite electrolysis different time among the embodiment 4 and the XRD figure spectrum of anodic product, wherein: (a) be raw material powder, (b) for the cathode product of electrolysis 10h, (c) be the cathode product of electrolysis 24h, (d) be the anodic product of electrolysis 24h.
Embodiment
Embodiment 1, utilize method of the present invention to remove the sulphur in the copper glance and reclaim sulphur, copper
With copper glance (Cu
2S) (99.5%, Alfa-Aesar, catalog number (Cat.No.): 14718, the about 10 μ m of mean particle size), do not add binding agent, compression moulding is cylindric compressing tablet under 6Mpa pressure, and wherein, the diameter of cylindric compressing tablet is 16mm, and thickness is between the 3mm, the about 3g of quality.Cylindric compressing tablet sintering under 300 ℃ of argon gas atmosphere protections was obtained the cylindric compressing tablet of porous in 2 hours.In fused-salt bath, with graphite rod (the about 4mm of diameter) as anode, the cylindric compressing tablet of porous is as porous cathode, the mixture (mol ratio 1:1) of pure Calcium Chloride Powder Anhydrous of operational analysis (quality percentage composition〉99%) and sodium-chlor (quality percentage composition〉99%) is as molten salt system, at voltage is 2.8V, temperature is under 800 ℃ the condition, electrolysis 2～24 hours.In the electrolysis implementation process, pneumatic outlet is connected with condenser, can collects corresponding anode product elemental sulfur.Electrolytic reaction also can be collected part sulphur at the boiler tube cold zone after finishing.After electrolytic reaction finishes, use the distilled water flushing porous cathode, then use washing with acetone, with the porous cathode fragmentation, promptly obtain about 2.4g copper powder after the oven dry.
Before electrolytic reaction and the photo contrast (see figure 2) of electrolysis after 20 hours, can obviously observe the metalluster that porous cathode after the electrolysis presents copper by porous cathode.
Fig. 3 is the XRD figure spectrum of cathode product behind the copper glance electrolysis different time.As seen from the figure, copper glance (Cu
2S) the CaS intermediate product can occur in the electrolytic process, and along with the prolongation of electrolysis time, intermediate product CaS is reduced gradually, can obtain purified copper behind electrolysis 24h.The existence of minute quantity Red copper oxide in some electrolysate (as Fig. 3 (b)) may be that subsequent laundering process causes.
(acceleration voltage of Electronic Speculum is 20kv to the SEM photo of the cathode product that Fig. 4 obtains after 24 hours for the copper glance electrolysis, magnification is 3000 times), X-ray energy spectrum confirms that copper content is about 98.93%, all the other are a small amount of Ca (0.37%), Na (0.38%), Cl (0.33%) etc.
In sum, the XRD of powder (X-ray diffraction) result proves cupric and intermediate product sulfurated lime etc. in the product, and corresponding SEM (scanning electron microscope) and EDS (X-ray energy spectrum) result have also confirmed to utilize this method can obtain copper.
Embodiment 2, utilize method of the present invention to remove the sulphur in the copper glance and reclaim sulphur, copper
With copper glance (Cu
2S) powder (99.5%, Alfa-Aesar, catalog number (Cat.No.): 14718, about 10 μ m of mean particle size), not adding binding agent, is powder pressing forming cylindric compressing tablet under 6Mpa pressure, wherein, the diameter of cylindric compressing tablet is 16mm, and thickness is 2.8mm, the about 2.72g of quality.Cylindric compressing tablet sintering under 300 ℃ of argon gas atmosphere protections was obtained the cylindric compressing tablet of porous in 2 hours.In fused-salt bath, with graphite rod (the about 4mm of diameter) as anode, the cylindric compressing tablet of porous is as porous cathode, the mixture (mol ratio 1:1) of pure Calcium Chloride Powder Anhydrous of operational analysis (quality percentage composition〉99%) and lithium chloride (quality percentage composition〉99%) is as molten salt system, at voltage is 2.2V, temperature is under 800 ℃ the condition, electrolysis 20 hours.In the electrolysis implementation process, pneumatic outlet is connected with condenser, can collects corresponding anode product elemental sulfur.After electrolytic reaction finished, the boiler tube cold zone also can be collected part sulphur.After electrolytic reaction finishes, use the distilled water flushing porous cathode earlier, then use washing with acetone, with the porous cathode fragmentation, promptly obtain about 2.17g copper powder after the oven dry.
The XRD spectra of the cathode product that Fig. 5 obtained for the copper glance electrolysis in 20 hours, result prove that the product principal crystalline phase is a copper.
Embodiment 3, utilize method of the present invention to remove the sulphur in the copper glance and reclaim sulphur, copper
With copper glance (Cu
2S) powder (99.5%, Alfa-Aesar, catalog number (Cat.No.): 14718, about 10 μ m of mean particle size), adding about 0.1g poly(oxyethylene glycol) 400 binding agent, is powder pressing forming cylindric compressing tablet under 4Mpa pressure, wherein, the diameter of cylindric compressing tablet is 16mm, and thickness is 3.84mm, the about 3.12g of quality.Cylindric compressing tablet sintering under 300 ℃ of argon gas atmosphere protections was obtained the cylindric compressing tablet of porous in 2 hours.In fused-salt bath, with graphite rod (the about 4mm of diameter) as anode, the cylindric compressing tablet of porous is as porous cathode, the mixture (mol ratio 1:1) of pure Calcium Chloride Powder Anhydrous of operational analysis (quality percentage composition〉99%) and sodium-chlor (quality percentage composition〉99%) is as molten salt system, at voltage is 2.8V, temperature is under 800 ℃ the condition, electrolysis 12 hours.In the electrolysis implementation process, pneumatic outlet is connected with condenser, can collects corresponding anode product elemental sulfur.After electrolytic reaction finished, the boiler tube cold zone also can be collected part sulphur.After electrolytic reaction finishes, use the distilled water flushing porous cathode, then use washing with acetone, with the porous cathode fragmentation, promptly obtain about 2.5g copper powder after the oven dry.
Embodiment 4, utilize method of the present invention to remove the sulphur in the chalcopyrite and reclaim sulphur, copper and iron
Present embodiment can remove sulphur in the chalcopyrite and the schema of separating copper iron is operated according to Fig. 1.
With chalcopyrite (CuFeS
2) powder (purchases the Outokumpu company in Finland; for than the simple brass breeze; chemical analysis results is as shown in table 1), be crushed into the powder that mean particle size is 10 μ m, 800 ℃ of sintering are 6 hours under argon gas atmosphere protection; then the powder behind the sintering is not added binding agent; compression moulding is cylindric compressing tablet under 6Mpa pressure, and wherein, the diameter of cylindric compressing tablet is 16mm; thickness is 3mm, the about 3g of quality.Again cylindric compressing tablet sintering under 800 ℃ of argon gas atmosphere protections was obtained the cylindric compressing tablet of porous in 2 hours.In fused-salt bath, with graphite rod (the about 4mm of diameter) as anode, the cylindric compressing tablet of porous is as porous cathode, the mixture (mol ratio 1:1) of pure Calcium Chloride Powder Anhydrous of operational analysis (quality percentage composition〉99%) and sodium-chlor (quality percentage composition〉99%) is as molten salt system, at voltage is 2.8V, temperature is that electrolysis did not wait in 12～24 hours under 800 ℃ the condition.In the electrolysis implementation process, pneumatic outlet is connected with condenser, can collects corresponding anode product elemental sulfur.After electrolytic reaction finished, the boiler tube cold zone also can be collected part sulphur.After electrolytic reaction finishes, use the ethanol ultrasonic irrigation earlier, then use washing with acetone, with the electrode fragmentation, promptly obtain about 2.4g copper iron mixed powder after the oven dry.
Fig. 6 is the XRD figure spectrum of cathode product and anodic product behind the chalcopyrite electrolysis different time.As seen from the figure, similar with the copper glance electrolysis, also the CaS intermediate product can occur in the chalcopyrite electrolytic process, and along with the prolongation of electrolysis time, intermediate product CaS is reduced gradually, can obtain purified copper iron mixture behind electrolysis 24h.Repeatedly after the electrolysis, the anodic product of collecting in the condenser is analyzed, the confirmation product is a sulphur, shown in Fig. 6 (d).
Adopt wet extraction separating copper iron mixed powder, mixed powder is dissolved in the dilute sulphuric acid, fully after the reaction, filter, collect filter residue and filtrate, filter residue is copper powder, and filtrate is copperas solution.The copperas solution of collecting can be obtained FeSO at-10～20 ℃ of following crystallisation by cooling
47H
2O (green vitriol).Thereby make the copper iron component in the chalcopyrite all obtain effective complete utilization, do not have waste residue to produce.
Table 1, raw material chalcopyrite efflorescence component list
| Yellow ingot metal breeze end | Cu | Fe | S | Cr | Si | Al | Ca | Pb | Zn | Mg |
| Quality percentage composition (%) | 26.3 | 27.7 | 39.6 | 0.2 | 1.6 | 0.3 | 0.3 | 0.6 | 2.4 | 1.0 |
Claims (10)
1, a kind of method of desulphurization of copper sulfur ore comprises: with copper sulphur ore deposit is that negative electrode, fused salt are ionogen, the step that adopts fused salt electrolysis process that desulfurization is carried out in copper sulphur ore deposit.
2, method according to claim 1 is characterized in that: described fused salt is following two kinds of fused salts: 1) alkaline earth metal chloride fused salt, 2) fused salt mixt of alkaline earth metal chloride and alkali metal chloride; Described alkaline earth metal chloride is selected from MgCl
2, CaCl
2Or BaCl
2, described alkali metal chloride is selected from LiCl, NaCl or KCl.
3, method according to claim 2 is characterized in that: described fused salt is a kind of in following three kinds of fused salts: 1) calcium chloride fused salt, 2) mole fused salt mixts such as calcium chloride and sodium-chlor, 3) mole fused salt mixts such as calcium chloride and lithium chloride.
4, method according to claim 3 is characterized in that: the electrolysis temperature in the described fused salt electrolysis process is 700-1000 ℃.
5, method according to claim 3 is characterized in that: the electrolysis voltage in the described fused salt electrolysis process is 1.6-3.2V.
6, according to arbitrary described method among the claim 1-5, it is characterized in that: the preparation method of described negative electrode comprises: the agglomerating step is carried out in described copper sulphur ore deposit under the condition of starvation.
7, method according to claim 6 is characterized in that: described agglomerating temperature is 300-800 ℃, and the described agglomerating time is 1-6 hour.
8, according to claim 6 or 7 described methods, it is characterized in that: the preparation method of described negative electrode also comprises: before sintering is carried out in described copper sulphur ore deposit, under 4-20MPa pressure described copper sulphur ore deposit is pressed into sheet or tabular step.
9, according to arbitrary described method among the claim 1-8, it is characterized in that: described copper sulphur ore deposit comprises copper glance, covellite, chalcopyrite and purple copper.
10, method according to claim 9, it is characterized in that: described copper sulphur ore deposit is chalcopyrite and purple copper, the preparation method of described negative electrode also comprises: with described copper sulphur ore deposit be pressed into sheet or tabular before, under the condition of 300-800 ℃ of starvations, make copper sulphur ore deposit be decomposed into the step of Cu2S and FeS.
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Cited By (5)
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| CN102995066A (en) * | 2011-09-09 | 2013-03-27 | 河北联合大学 | Molten salt electrochemical reduction method for removing sulfide inclusions on solid steel surface |
| CN106422716A (en) * | 2016-08-25 | 2017-02-22 | 昆明理工大学 | Method and device for removing SO2 in flue gas with copper extracting tailings and recycling copper extracting tailings |
| CN108505070A (en) * | 2018-04-23 | 2018-09-07 | 东北大学 | A method of extracting oxygen and metal from lunar soil lunar rock |
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN111349503A (en) * | 2020-04-02 | 2020-06-30 | 北京科技大学 | Petroleum coke electrochemical desulfurization method |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102995066A (en) * | 2011-09-09 | 2013-03-27 | 河北联合大学 | Molten salt electrochemical reduction method for removing sulfide inclusions on solid steel surface |
| CN106422716A (en) * | 2016-08-25 | 2017-02-22 | 昆明理工大学 | Method and device for removing SO2 in flue gas with copper extracting tailings and recycling copper extracting tailings |
| CN106422716B (en) * | 2016-08-25 | 2023-07-21 | 昆明理工大学 | SO in copper extraction tailings desorption flue gas 2 And resource method and device |
| CN108505070A (en) * | 2018-04-23 | 2018-09-07 | 东北大学 | A method of extracting oxygen and metal from lunar soil lunar rock |
| CN108505070B (en) * | 2018-04-23 | 2019-07-16 | 东北大学 | A method of extracting oxygen and metal from lunar soil lunar rock |
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN110565120B (en) * | 2019-10-18 | 2021-09-07 | 东北大学 | Method for removing and recovering copper from copper-containing iron liquid |
| CN111349503A (en) * | 2020-04-02 | 2020-06-30 | 北京科技大学 | Petroleum coke electrochemical desulfurization method |
| CN111349503B (en) * | 2020-04-02 | 2021-05-25 | 北京科技大学 | Petroleum coke electrochemical desulfurization method |
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