CN101760611A - Method for wet-method oxidative decomposition of metal sulfide ores - Google Patents
Method for wet-method oxidative decomposition of metal sulfide ores Download PDFInfo
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- CN101760611A CN101760611A CN201010300953A CN201010300953A CN101760611A CN 101760611 A CN101760611 A CN 101760611A CN 201010300953 A CN201010300953 A CN 201010300953A CN 201010300953 A CN201010300953 A CN 201010300953A CN 101760611 A CN101760611 A CN 101760611A
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- metal sulfide
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- oxidative decomposition
- sodium
- electrolytic solution
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Abstract
The invention provides a method for the wet-method oxidative decomposition of metal sulfide ores. The method comprises the following steps of: using chlorate electrolyte obtained by electrolyzing aqueous solution of sodium chloride as an oxidant, and performing oxidative decomposition of metal sulfide ores such as molybdenite, chalcopyrite, sphalerite, pyrite and the like under a condition of acid aqueous solution to obtain the corresponding aqueous solution of metallic salt. The chlorate electrolyte used by the method has the advantages of high oxidizing capability and low product cost, and solves the problems of safely storing, transporting and using the oxidant, so that the method is a novel high-efficiency and economic method for the wet-method oxidative decomposition of the metal sulfide ores.
Description
Technical field
The invention belongs to technical field of wet metallurgy, relate generally to a kind of method for wet-method oxidative decomposition of metal sulfide of novelty.
Background technology
Along with industrial expansion, higher-grade and easy to handle ore are fewer and feweri, owing to be subjected to the restriction of separation efficiency, only depend on single floatation process to be difficult to obtain qualified concentrate product.Therefore, the new eco-friendly high efficiency separation extraction process of exigence development.
In recent years, the research of the full wet processing of metal sulfide more and more comes into one's own, and oxygenant and method for oxidation are the core keys that metal sulfide oxygenolysis or oxidation are leached.For the oxygenant in the wet processing, on the one hand require to have the strong oxidizing property energy, on the other hand its source, price and aspect such as safe in utilization also there are certain requirement.
Oxymuriate is a kind of industrial widely used oxygenant.In acidic solution, oxymuriate and sulfuric acid or hydrochloric acid reaction generate ClO
2And thereby the Cl of nascent state has strong oxidizing property.The oxidation capacity of dioxide peroxide is 2.63 times of chlorine, has widespread use at aspects such as water treatment and paper pulp, textile bleaching, metallurgy.
Ren Yonggang as leaching agent, has carried out the leaching research of system with dioxide peroxide-sodium-chlor-water to the complicated gold sulphide concentrate after the roasting.Studies show that, liquid-solid ratio 2.5: 1, pH=2, sodium chloride concentration 1.0mol/L, 50 ℃ of temperature, under the condition of time 6h, the leaching yield of gold can reach 97.3%.Soak gold utensil with dioxide peroxide leaching yield height, fast, widely applicable, the environment amenable characteristics of speed are arranged.This technology for the comprehensive reutilization of complicated gold sulphide concentrate provide new approach (Ren Yonggang. dioxide peroxide leaches the experimental study of complicated gold sulphide concentrate. inorganic chemicals industry, 2006,38 (06): 46～48.).
Osmanli
Ucar carries out leaching experiment with sodium chlorate for zink sulphide under acidic conditions, zinc leaching rate up to 99.4% (
U.Kinetics of sphalerite dissolution by sodium chlorate inhydrochloric acid..Hydrometallurgy, 2008,95:39～43.).
Li Dongliang is by discovering, for oxidizing type of gold ore, liquid-solid ratio 3: 1, pH=3, NaCl concentration is 0.5mol/L, 40 ℃ of temperature, under the condition of time 10h, acid oxymuriate system obtains good leaching effect too, and gold leaching rate is up to 95.5%, and compare toxicological harmless, environmentally friendly (Li Dongliang with conventional cyaniding lixiviation process, Zhang Liang, Han Xuanli, Zhang Yinju. dioxide peroxide soaks golden experimental study [J]. Xi'an University of Architecture and Technology's journal, 2002,34 (2): 187～192.).
Above-mentioned studies show that, sodium chlorate are a kind of oxygenants efficiently, can be used for the wet method extract technology of multiple metalliferous mineral, but exist sodium chlorate price height, store and the not enough security problems of transportation.In order further to reduce metal sulfide extract technology production cost, solve the accumulating and the transportation safety problem of sodium chlorate oxygenant, the sodium chlorate electrolytic solution that the present invention uses the electrolytic chlorination natrium brine to generate, the wet oxidation that is directly used in sulphide oress such as molybdenum glance, chalcopyrite, zink sulphide and pyrite leaches.
Have not yet to see the direct chlorate electrolysis liquid that uses the electrolytic chlorination natrium brine to generate and be oxygenant, under the acidic aqueous solution condition, sulphide oress such as molybdenum glance, chalcopyrite, zink sulphide and pyrite are carried out the relevant report of oxygenolysis.
Summary of the invention
The metal sulfide method for wet-method oxidative decomposition that the purpose of this invention is to provide a kind of efficient economy, with the production cost of remarkable reduction sulphide ores wet method decomposition course, and the accumulating and the safe handling problem of solution oxygenant.
The method for wet-method oxidative decomposition of a kind of metal sulfide provided by the invention is, the sodium chlorate electrolytic solution that the electrolytic chlorination natrium brine is generated mixes with metal sulfide, under the acidic aqueous solution condition, metal sulfide carries out oxygenolysis with chlorate electrolysis liquid, generates the corresponding metal salt brine solution.
Because, the sodium chlorate electrolytic solution that the present invention directly generates the electrolytic chlorination natrium brine is as oxygenant, do not need operations such as refining, purification, crystallization, reciprocity metal sulfide carries out oxygenolysis under the acidic aqueous solution condition, generate the corresponding metal salt brine solution, greatly simplified processing step, reduced production cost, and solved the problem of the difficult accumulating of oxygenant effectively with safety.
In the method for the present invention, described sodium chlorate electrolytic solution is the electrolytic solution that contains sodium chlorate and sodium-chlor that adopts the electrolytic chlorination natrium brine to generate, electrolytic solution consist of sodium chlorate 50～750g/L, sodium-chlor 30～150g/L.
Preferable preparation technique condition of the present invention is: under 30～95 ℃ temperature, with the electrolysis in undivided cell of saturated sodium-chloride salt solution, the control output voltage is 3～5v during electrolysis, and anodic current density is 100～3000A/m
2, electrolyte ph is 6.5～7.5, electrolytic solution Na
2Cr
2O
7Concentration is 1～10g/L, volume current density 2～50A/L.Solution composition is sodium chlorate 200～750g/L after the electrolysis, sodium-chlor 70～150g/L.
In the method for the present invention, describedly in the technological process and the condition of under the acidic aqueous solution condition metal sulfide being carried out oxygenolysis be: metal sulfide carries out oxygenolysis with chlorate electrolysis liquid in the presence of sulfuric acid or hydrochloric acid, H
2SO
4Or the consumption of HCl is 1～5 times of the metal sulfide quality.The consumption of chlorate electrolysis liquid (calculating by the sodium chlorate butt) is 1～4 times of metal sulfide quality, and the solid masses percentage concentration of ore pulp is 1～40%, and temperature of reaction is 30 ℃～100 ℃, and the reaction times is 2～10 hours.
In the method for the present invention, described sodium chloride salt water concentration is greater than 30g/L, preferred saturated sodium-chloride salt solution.
In the method for the present invention, described acidic aqueous solution condition is meant H
2SO
4Or the HCl aqueous solution, H
2SO
4Or the consumption of HCl is 1～5 times of the metal sulfide quality.
The described metal sulfide of method of the present invention comprises zinc sulfide mineral, nickel sulfide ore and sulfurous iron ore such as copper sulfide minerals such as molybdenum glance, chalcopyrite, zink sulphide.
Method of the present invention is generally carried out under normal pressure.
In sum, utilize the electrolytic chlorination natrium brine to generate sodium chlorate electrolytic solution, the wet oxidation that is directly used in metal sulfide leaches, the metal sulfide wet method that is a kind of efficient economy is decomposed new technology, not only can reduce cost to a great extent, and can solve the accumulating and the safe handling problem of oxygenant.
Embodiment
The present invention is further specified by the following example, but is not subjected to the restriction of these embodiment.All umbers and percentage ratio all refer to quality except as otherwise herein provided among the embodiment.
Embodiment 1:
The molybdenum glance concentrate contains Mo40.22%.With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 1 part of brightness concentrated molybdenum ore, 2.2 parts of H
2SO
4, 6.5 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 99.79%.
Embodiment 2:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 1 part of brightness concentrated molybdenum ore (Mo40.22%, with embodiment 1), 4.5 parts of 37%HCl, 6.5 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer under 70 ℃ of conditions, Hangzhou instrucment and meter plant) reaction 10h, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 99.87%.
Embodiment 3:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.5v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 450g/L after the electrolysis, sodium-chlor 110g/L.Get 1 part of brightness concentrated molybdenum ore (Mo40.22% is with embodiment 1), 2.2 parts of H
2SO
4, 5.5 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 99.07%.
Embodiment 4:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 700A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 250g/L after the electrolysis, sodium-chlor 180g/L.Get 1 part of brightness concentrated molybdenum ore (Mo40.22% is with embodiment 1), 2.2 parts of H
2SO
4, 10 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 98.99%.
Embodiment 5:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 10 parts of molybdenum glances (Mo1.70%), 2.2 parts of H
2SO
4, 2.5 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 99.79%.
Embodiment 6:
With concentration is NaCl solution electrolysis in undivided cell of 250g/L, and the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 330g/L after the electrolysis, sodium-chlor 80g/L.Get 1 part of brightness concentrated molybdenum ore (Mo40.22% is with embodiment 1), 2.2 parts of H
2SO
4, 8.5 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Mo in the post analysis filtrate, the leaching yield of Mo is 98.94%.
Embodiment 7:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 1 part of brass concentrate (Cu23.22%), 2.5 parts of H
2SO
4, 7.0 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Cu in the post analysis filtrate, the leaching yield of Cu is 99.91%.
Embodiment 8:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 1 part and dodge zinc ore concentrate (Zn43.77%), 3.0 parts of H
2SO
4, 15 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Zn in the post analysis filtrate, the leaching yield of Zn is 98.49%.
Embodiment 9:
With the electrolysis in undivided cell of saturated NaCl solution, the control output voltage is 3.0v, and anodic current density is 1000A/m
2, electrolyte ph is 6.7, electrolytic solution Na
2Cr
2O
7Concentration is 3g/L, and solution composition is sodium chlorate 410g/L after the electrolysis, sodium-chlor 130g/L.Get 1 part of yellow iron ore concentrate (Fe44.01%), 3.1 parts of H
2SO
4, 10 parts of electrolytic solution and 20 parts of distilled water add in the 500ml round-bottomed flask, stir (JHS-1 type electronics constant speed stirrer, Hangzhou instrucment and meter plant) reaction 10h under 70 ℃ of conditions, filter the content of Fe in the post analysis filtrate, the leaching yield of Fe is 99.79%.
Claims (7)
1. the method for wet-method oxidative decomposition of a metal sulfide, it is characterized in that the sodium chlorate electrolytic solution that the electrolytic chlorination natrium brine is generated mixes with metal sulfide, under the acidic aqueous solution condition, the oxidized decomposition of metal sulfide generates the corresponding metal salt brine solution.
2. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 1, it is characterized in that: the consumption of chlorate electrolysis liquid, calculate by the sodium chlorate butt, be 1～4 times of metal sulfide quality, the solid masses percentage concentration of ore pulp is 1～40%, temperature of reaction is 30 ℃～100 ℃, and the reaction times is 2～10 hours.
3. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 1, it is characterized in that: described is in the presence of sulfuric acid or hydrochloric acid in the acidic aqueous solution condition, and the consumption of sulfuric acid or hydrochloric acid is 1～5 times of metal sulfide quality.
4. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 1, it is characterized in that: described sodium chlorate electrolytic solution is the electrolytic solution that contains sodium chlorate and sodium-chlor, electrolytic solution consist of sodium chlorate 50～750g/L, sodium-chlor 30～150g/L.
5. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 4 is characterized in that: electrolytic solution consist of sodium chlorate 200～750g/L, sodium-chlor 70～150g/L.
6. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 5, it is characterized in that: the electrolytic chlorination natrium brine is under 30～95 ℃ temperature, with the electrolysis in undivided cell of saturated sodium-chloride salt solution, the control output voltage is 3～5v during electrolysis, anodic current density is 100～3000A/m2, electrolyte ph is 6.5～7.5, and electrolytic solution Na2Cr2O7 concentration is 1～10g/L, volume current density 2～50A/L.
7. the method for wet-method oxidative decomposition of a kind of metal sulfide according to claim 1, it is characterized in that: described metal sulfide comprises zinc sulfide mineral, nickel sulfide ore or sulfurous iron ore such as copper sulfide minerals such as molybdenum glance, chalcopyrite, zink sulphide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776374A (en) * | 2011-05-09 | 2012-11-14 | 深圳市格林美高新技术股份有限公司 | Treatment method of nickel-cadmium slag |
| CN102918171A (en) * | 2010-07-28 | 2013-02-06 | 住友金属矿山株式会社 | Process for production of ferronickel smelting raw material from low grade lateritic nickel ore |
| CN104674025A (en) * | 2013-11-28 | 2015-06-03 | 韩国地质资源研究院 | Method of pre-treating molybdenite containing copper |
| CN107201531A (en) * | 2017-04-27 | 2017-09-26 | 新疆中泰化学阜康能源有限公司 | Highly acid light salt brine reclamation set after chlorate decomposer is decomposed in electrolysis process |
| CN108103310A (en) * | 2018-01-22 | 2018-06-01 | 东北大学 | A kind of chlorine dioxide method for pre-oxidizing containing sulfur gold ore |
| CN112442591A (en) * | 2019-08-30 | 2021-03-05 | 武汉理工大学 | Copper-nickel leaching and iron separation method for copper-nickel sulfide ore |
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2010
- 2010-01-30 CN CN201010300953A patent/CN101760611A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102918171A (en) * | 2010-07-28 | 2013-02-06 | 住友金属矿山株式会社 | Process for production of ferronickel smelting raw material from low grade lateritic nickel ore |
| CN102918171B (en) * | 2010-07-28 | 2014-03-12 | 住友金属矿山株式会社 | Process for production of ferronickel smelting raw material from low grade lateritic nickel ore |
| CN102776374A (en) * | 2011-05-09 | 2012-11-14 | 深圳市格林美高新技术股份有限公司 | Treatment method of nickel-cadmium slag |
| CN102776374B (en) * | 2011-05-09 | 2014-02-26 | 深圳市格林美高新技术股份有限公司 | Treatment method of nickel-cadmium slag |
| CN104674025A (en) * | 2013-11-28 | 2015-06-03 | 韩国地质资源研究院 | Method of pre-treating molybdenite containing copper |
| CN107201531A (en) * | 2017-04-27 | 2017-09-26 | 新疆中泰化学阜康能源有限公司 | Highly acid light salt brine reclamation set after chlorate decomposer is decomposed in electrolysis process |
| CN107201531B (en) * | 2017-04-27 | 2020-10-30 | 新疆中泰化学阜康能源有限公司 | Strong acid light salt water recycling device after chlorate decomposer decomposes in electrolysis process |
| CN108103310A (en) * | 2018-01-22 | 2018-06-01 | 东北大学 | A kind of chlorine dioxide method for pre-oxidizing containing sulfur gold ore |
| CN108103310B (en) * | 2018-01-22 | 2020-03-31 | 东北大学 | Chlorine dioxide pre-oxidation method for sulfur-containing gold ore |
| CN112442591A (en) * | 2019-08-30 | 2021-03-05 | 武汉理工大学 | Copper-nickel leaching and iron separation method for copper-nickel sulfide ore |
| CN112442591B (en) * | 2019-08-30 | 2023-10-20 | 武汉理工大学 | Copper-nickel leaching and iron separation method for copper-nickel sulfide ore |
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