CN110669928B - Method for selectively removing zinc from zinc-containing copper concentrate by using oxidizing gas - Google Patents
Method for selectively removing zinc from zinc-containing copper concentrate by using oxidizing gas Download PDFInfo
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- CN110669928B CN110669928B CN201910986756.0A CN201910986756A CN110669928B CN 110669928 B CN110669928 B CN 110669928B CN 201910986756 A CN201910986756 A CN 201910986756A CN 110669928 B CN110669928 B CN 110669928B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/045—Leaching using electrochemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0002—Preliminary treatment
- C22B15/0004—Preliminary treatment without modification of the copper constituent
- C22B15/0008—Preliminary treatment without modification of the copper constituent by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for selectively removing zinc from zinc-containing copper concentrate by using oxidizing gas, which comprises the steps of mixing zinc-containing copper concentrate powder with water to obtain different ore pulp concentrations, then introducing a gas oxidant, then adjusting the pH value of the ore pulp, stirring and leaching the obtained ore pulp at a certain temperature, controlling the oxidation-reduction potential of a leaching system, selectively removing zinc, and then obtaining high-grade copper concentrate. According to the invention, zinc is preferentially leached by adopting different gas oxidant leaching methods, the grade of copper ore is greatly improved, the problem that the copper and zinc are difficult to separate at present is solved, the leaching solution can be used as a production raw material of metal zinc, the production process is simplified, the production cost is reduced, unnecessary energy waste is reduced, the removed zinc can be used as a production raw material of metal zinc in the solution, the existing mineral resources are utilized to the maximum extent, the harm to the environment is reduced, and the economic benefit is increased. The method is clean, simple and easy to operate, and is suitable for large-scale popularization and application.
Description
Technical Field
The invention relates to efficient separation and extraction of metal copper and metal zinc in a copper-zinc mixed ore in the fields of hydrometallurgy and mineral processing, in particular to a method for selectively removing zinc from zinc-containing copper concentrate by using oxidizing gas to obtain leachate containing zinc ions and copper concentrate.
Background
With the development of the mining industry in China, single easily-processed ores are reduced day by day, the contradiction of resource constraint is highlighted day by day, and the comprehensive development and reasonable utilization of complex common and associated ores become the inevitable trend of resource exploitation in China. Copper ore is the most common associated ore, and is often associated with a plurality of metal elements such as lead, zinc and the like, and the impurity metal elements and the copper element are embedded with each other. In the flotation process, copper and zinc minerals are densely symbiotic and difficult to dissociate, so that the separation is difficult. Even if the grinding fineness reaches the condition of monomer dissociation, the ore particles are too fine due to over grinding, the flotation rate is greatly reduced, and copper ions in the ore pulp activate the zinc blende, so that the surface of the zinc blende and the surface of the chalcopyrite have similar floatability, and the copper and zinc are difficult to separate by a flotation method. Therefore, the content of lead and zinc in the copper concentrate is relatively high, which not only causes the waste of zinc resources, but also reduces the taste of the copper concentrate and seriously influences the market price of the copper concentrate. Therefore, the development of a method capable of effectively separating copper and zinc has wide industrial application prospect.
The current methods for smelting copper from copper ores or copper concentrates are numerous and include mainly the pyrogenic process and the wet process in summary. The main method for producing copper is the pyrometallurgical method, and 80% of the primary copper production in the world is produced by pyrometallurgical method at present, especially copper sulphide ore, which is basically treated by pyrometallurgical method. However, when the zinc content in the copper minerals exceeds 15%, slag is easily formed to block the feed inlet in the smelting process, and the furnace temperature cannot be controlled and cannot enter a closed blast furnace for smelting. Therefore, the research on the removal of zinc in copper minerals is a problem to be solved urgently, some researchers research the removal of zinc in copper minerals, namely, copper-zinc bulk concentrates are obtained through flotation, and then two-stage countercurrent oxygen pressure acid leaching is carried out on the bulk concentrates, so that the separation of copper and zinc is realized; and according to the characteristics that the copper-lead-zinc sulphide ore is closely symbiotic and the lead-zinc ore is embedded with fine granularity, an equal-floatable process is adopted, firstly, copper and lead ores and part of easily-floated zinc ores float, copper, lead and zinc concentrates are sequentially separated after the mixed concentrate is reground, and the zinc ores with poor flotability are separately separated from the mixed-floated tailings, so that the copper, lead and zinc ores are effectively separated. In Japan, copper-zinc concentrate is roasted by sulfated boiling layer to generate copper sulfate and zinc sulfate from copper and zinc sulfides, and copper and zinc can be obtained by electrolysis. Direct pyrometallurgy of copper, lead, zinc, iron and other mixed sulfur concentrates has also been studied to open up a way for direct smelting. The patent (CN 106884184A) discloses a device for separating and removing lead and zinc from polymetallic copper sulfide ores, which is also designed and constructed according to the electrolysis principle so as to remove lead and zinc impurities in the copper sulfide ores through electrolysis. The method mainly realizes the removal of lead and zinc by controlling reaction conditions, and the adopted device is a conventional electrolysis device. The method improves the grade of the copper concentrate to a certain extent, but the methods have the following defects:
(1) large-scale pressurizing equipment, electrolytic cells and heating equipment need to be constructed;
(2) the hydrochloric acid in the electrolyte solution is extremely volatile, so that the waste of resources is caused;
(3) the production process is increased, so that the production cost of the copper concentrate is improved;
(4) the conventional flotation reagent has poor selectivity and large consumption, and has great pollution to the environment in the lead and zinc removing process.
Disclosure of Invention
The invention aims to solve the problems of complicated separation process, heavy pollution, high cost, difficult recovery of removed zinc and the like of copper and zinc sulfide minerals in zinc-containing minerals in the prior art, provides a method capable of selectively removing zinc from zinc-containing copper concentrate minerals efficiently to obtain required high-grade copper concentrate, and is beneficial to further recycling of zinc resources. The zinc contained in the minerals is selectively removed by using a leaching process, so that the high-efficiency separation of copper and zinc is realized, the influence of the zinc on the subsequent processing and smelting of copper concentrate is avoided, and the zinc is convenient to recycle. In order to solve the problems of complex dezincification process, high production cost, great environmental pollution and the like, the invention provides a new idea of dezincification by using oxidizing gas, and aims to realize selective leaching of zinc in the leaching process and further realize high-efficiency separation of zinc and copper. The method can effectively reduce the content of zinc in the copper concentrate.
In order to achieve the above object, the present invention provides a method for selectively dezincifying a zinc-containing copper concentrate using an oxidizing gas, comprising the steps of:
(1) pretreating zinc-containing copper concentrate;
(2) preparing the zinc-containing copper concentrate after pretreatment into ore pulp;
(3) introducing a gas oxidant into the ore pulp, and stirring and leaching;
(4) carrying out solid-liquid separation on the leached ore pulp to obtain low-zinc high-grade copper concentrate and a zinc-containing solution;
(5) recovering zinc from the zinc-containing solution.
Preferably, in the step (1), the zinc content of the zinc-containing copper concentrate is 8.6-20.5%.
Preferably, the pretreatment method is to regrind the concentrate to-200 meshes.
Preferably, in the step (2), the pulp concentration is less than or equal to 35 percent.
Preferably, in step (3), the gaseous oxidant is one or more of ozone, chlorine, pure oxygen, nitrous oxide, and nitrogen trifluoride.
Preferably, in the step (3), the pH value of the ore pulp is adjusted to be less than or equal to 5.0 during agitation leaching.
Preferably, in the step (3), the ore pulp is stirred and leached at the temperature of 20-75 ℃.
More preferably, in the step (3), the stirring speed is 10 to 680 rpm.
Preferably, in the step (3), the potential of a leaching system in the agitation leaching process is controlled to be 250-850 mV relative to a saturated silver/silver chloride electrode.
Preferably, in the step (3), the stirring leaching time is more than or equal to 0.4 hour.
Compared with the prior art, the invention has the following advantages: 1. the method can remove the zinc in the zinc-containing copper minerals efficiently and selectively, the removal rate can reach more than 80 percent at most, and the loss rate of the copper is less than 5 percent; 2. the production cost of the copper concentrate is reduced, and the selective separation of zinc in the zinc-containing copper concentrate can be realized without constructing large-scale pressurizing equipment, electrolytic cells and heating equipment; 3. the zinc-containing mineral is selectively dezincified before being processed by the gas oxidant directly, so that unnecessary energy waste is reduced, the removed zinc can be used as a production raw material of metal zinc in the solution, and the existing mineral resources are utilized to the maximum extent; 4. the reagents used in the process of removing the zinc can be recycled, and the method is environment-friendly.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further described in detail with the specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; and mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 3-9%. And introducing gas oxidant ozone into the ore pulp, stirring and leaching, adjusting the pH value of the ore pulp to 1.1-1.7 in the leaching process, controlling the stirring speed to be 150-200 rpm, the leaching temperature to be 35-40 ℃, controlling the potential of a leaching system to be 300-350 mv relative to a saturated silver/silver chloride electrode, and the leaching time to be 2-5 hours. Filtering the leached ore pulp to obtain low-zinc high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 87.6-89.4%.
Example 2
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; and mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 5-10%. Introducing a gas oxidant pure oxygen, adjusting the pH value of the ore pulp to 1.0-2.0, controlling the stirring speed to be 100-200 rpm, controlling the temperature to be 35-40 ℃, controlling the system potential to be 250-300 mv relative to the saturated silver/silver chloride electrode, and controlling the leaching time to be 2-5 hours. Filtering the leached ore pulp to obtain low-zinc high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 81.6-85.6%.
Example 3
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 8-13%, and introducing a gaseous oxidant chlorine Cl2Adjusting the pH value of the ore pulp to 2.0-2.5, controlling the stirring speed to 200-250 rpm, and controlling the temperatureThe temperature is 40-45 ℃, the potential of the system is controlled to be 400-450 mv relative to the saturated silver/silver chloride electrode, and the leaching time is 2-4 hours. Filtering the leached ore pulp to obtain low-zinc high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 84.6% -88.2%.
Example 4
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 10-15%, and introducing a gas oxidant nitric oxide N2And O, adjusting the pH value of the ore pulp to 2.5-3.5, controlling the stirring speed to be 400-500 rpm, controlling the temperature to be 35-40 ℃, controlling the system potential to be 500-550 mv relative to the saturated silver/silver chloride electrode, and leaching for 2-6 hours. Filtering the leached ore pulp to obtain high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 84.6% -88.3%.
Example 5
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 15-20%, and introducing a gas oxidant nitrous oxide N2And O, adjusting the pH value of the ore pulp to 1.5-2.0, controlling the stirring speed to be 600-650 rpm, controlling the temperature to be 50-60 ℃, controlling the system potential to be 600-650 mv relative to the saturated silver/silver chloride electrode, and leaching for 2-3 hours. Filtering the leached ore pulp to obtain high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 83.6% -88.6%.
Example 6
Pressing the zinc-containing copper mineral with oxygenAnd performing acid leaching and other traditional beneficiation methods to obtain zinc-containing copper concentrate, wherein the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 10-20%, and introducing a gas oxidant, namely nitrogen trifluoride NF3Adjusting the pH value of the ore pulp to 2.0-3.0, controlling the stirring speed to 300-400 rpm, controlling the temperature to 50-60 ℃, controlling the system potential to be 500-650 mv relative to the saturated silver/silver chloride electrode, and leaching for 1-3 hours. Filtering the leached ore pulp to obtain high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 84.6% -88.3%.
Example 7
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 10-15%, and introducing a gaseous oxidant chlorine Cl2Adjusting the pH value of the ore pulp to 1.0-1.5, controlling the stirring speed to be 500-600 rpm, controlling the temperature to be 50-60 ℃, controlling the system potential to be 600-750 mv relative to the saturated silver/silver chloride electrode, and leaching for 5-8 hours. Filtering the leached ore pulp to obtain high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 80.6% -88.3%.
Example 8
The zinc-containing copper ore is treated by the traditional beneficiation methods such as oxygen pressure acid leaching and the like to obtain zinc-containing copper concentrate, and the zinc content of the zinc-containing copper concentrate is 8.6-20.5%. Crushing and grinding the zinc-copper concentrate, and screening to obtain zinc-copper containing concentrate powder with the granularity of 200 meshes; mixing the zinc-copper concentrate powder with water to obtain ore pulp, wherein the concentration of the ore pulp is 15-20%, introducing a gas oxidant ozone, adjusting the pH of the ore pulp to 1.5-2.5, controlling the stirring speed to be 500-600 rpm, controlling the temperature to be 55-65 ℃, controlling the system potential to be 400-550 mv relative to the saturated silver/silver chloride electrode, and controlling the leaching time to be 5-10 hours. Filtering the leached ore pulp to obtain high-grade copper concentrate and zinc-containing filtrate after selective dezincification; and recovering the filtrate to obtain a high-zinc product. Through detection, the removal rate of zinc can reach 80.5% -87.5%.
While there have been shown and described the fundamental principles and principal features of the invention and advantages thereof, it will be understood by those skilled in the art that the invention is not limited by the foregoing examples, which are provided for illustration of the principles of the invention, but is susceptible to various changes and modifications without departing from the spirit and scope of the invention, such as various minerals containing zinc. Such changes and modifications are intended to be included within the scope of the claimed invention, which is defined by the appended claims and their equivalents.
Claims (1)
1. A process for the selective dezincification of a zinc-bearing copper concentrate using an oxidizing gas, comprising the steps of:
(1) pretreating zinc-containing copper concentrate;
(2) preparing the zinc-containing copper concentrate after pretreatment into ore pulp;
(3) introducing a gas oxidant into the ore pulp, and stirring and leaching;
(4) carrying out solid-liquid separation on the leached ore pulp to obtain low-zinc high-grade copper concentrate and a zinc-containing solution;
(5) recovering zinc from the zinc-containing solution;
in the step (1), the zinc content of the zinc-copper containing concentrate is 8.6-20.5%; in the step (1), the pretreatment method comprises the steps of regrinding the concentrate to-200 meshes; in the step (2), the concentration of the ore pulp is less than or equal to 35 percent; in the step (3), the gas oxidant is one or more of ozone, chlorine, pure oxygen, nitrous oxide and nitrogen trifluoride; in the step (3), the pH value of the ore pulp is adjusted to be less than or equal to 5.0 during agitation leaching; in the step (3), stirring and leaching the ore pulp at the temperature of 20-75 ℃; in the step (3), the stirring speed is 10-680 rpm; in the step (3), the potential of a leaching system in the stirring leaching process is controlled to be 250-850 mV relative to a saturated silver/silver chloride electrode; in the step (3), the stirring leaching time is more than or equal to 0.4 hour.
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Non-Patent Citations (1)
| Title |
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| "铜锌硫精矿常压选择性浸出探索性试验";有色冶金专业73级结业小组;《西安建筑科技大学学报(自然科学版)》;19771231(第02期);正文第119-125页 * |
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