CN109321755B - Method for removing arsenic from copper smelting smoke dust - Google Patents

Method for removing arsenic from copper smelting smoke dust Download PDF

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CN109321755B
CN109321755B CN201811422941.9A CN201811422941A CN109321755B CN 109321755 B CN109321755 B CN 109321755B CN 201811422941 A CN201811422941 A CN 201811422941A CN 109321755 B CN109321755 B CN 109321755B
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arsenic
copper smelting
smoke dust
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smelting
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CN109321755A (en
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彭兵
朱顺
刘恢
梁彦杰
陈玉洁
姚文明
王忠兵
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Central South University
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/04—Obtaining arsenic
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/02—Working-up flue dust
    • 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

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Abstract

The invention discloses a method for removing arsenic from copper smelting smoke dust. The method can realize the high-efficiency removal of arsenic at a lower roasting temperature compared with the conventional arsenic removal method by a pyrogenic process, has the removal rate of more than 88 percent, is simple to operate, has mild conditions and low energy consumption, and can treat the arsenic in the copper smelting smoke dust on a large scale.

Description

Method for removing arsenic from copper smelting smoke dust
Technical Field
The invention relates to a method for removing arsenic from copper smelting smoke dust, which utilizes pyrite as an arsenic removal additive to improve the arsenic removal rate of the arsenic-containing copper smelting smoke dust and realize the high-efficiency separation and recovery of arsenic from complex arsenic-containing materials, and belongs to the field of pyrometallurgy of nonferrous metals.
Background
The global copper industry is rapidly developed, according to the statistical data released by the world metal statistical institute (WBMS)2015 at 2, 15 and the global refined copper yield of 2015 is 2288.3 ten thousand tons, the refined copper still needs to be supplied and demanded, and the refined copper yield of China still keeps steadily increasing in the coming years. Arsenic-containing smoke dust generated in the copper smelting process is an important raw material for recovering gold and silver and various valuable metals; however, due to the existence of arsenic, both in the pyrometallurgical and wet recovery processes, the treatment process brings great pollution to the environment, the flow becomes complicated, the quality of other products used comprehensively is affected, and in addition, the continuous improvement of the current environmental protection requirements, the dearsenification of smelting smoke dust is more and more emphasized.
The common arsenic-containing smoke dust dearsenization methods at present comprise three methods, namely a pyrogenic method, a wet method and a pyrogenic-wet method combination. The dearsenization by a wet process refers to the treatment of an aqueous solution containing a dearsenization agent at a temperature within 100 ℃ so that arsenic enters the solution in the form of arsenic acid (salt) or arsenous acid (salt) to be separated from solid materials, wherein common leaching agents comprise an acid leaching agent, an alkali leaching agent, an inorganic salt leaching agent and the like. Wet dearsenization and fire-wet combined dearsenization have been widely noticed and studied by scholars at home and abroad in recent years, but have a series of disadvantages: the process is long, secondary pollution is easy to generate, the arsenic removal cost is high, and the process is not suitable for treating large-batch smoke dust. Compared with wet dearsenification and combined dearsenification by a pyrometallurgical method and a wet pyrometallurgical method, the method has the advantages of simplicity and convenience, no need of adding extra production equipment and processes, capability of directly returning the dearsenified materials to a molten pool smelting system, and high economic benefit. Additives which are commonly added in the fire roasting dearsenification reported in the literature at present comprise coke, alkaline substances, oxides, sulfates and the like, the addition of the coke for dearsenification needs to be carried out at the temperature of 1100 ℃, the requirement on equipment is high, the energy consumption is high, and other valuable metals can volatilize along with the addition of the coke; adding alkaline matter for roasting to convert arsenic-containing compound into arsenate, and performing wet dearsenification and arsenic stabilization treatment subsequently, but the process is complex, the process flow is long, and the method is not suitable for industrial production.
Disclosure of Invention
Aiming at the defects of high pollution, high energy consumption, high cost, potential safety hazard and the like in the dearsenization technology of complex arsenic-containing materials in the prior art, the invention aims to provide a method for realizing the efficient removal of arsenic in copper smelting smoke dust at low temperature by using pyrite as a dearsenization additive. The method has simple process and low energy consumption, can effectively solve the technical problem of dearsenification treatment of arsenic-containing smoke dust in copper smelting, and meets the application requirement of industrial production.
The invention provides a method for removing arsenic from copper smelting smoke dust, which comprises the steps of mixing arsenic-containing smoke dust in copper smelting with a material containing ferric sulfide, placing the mixture in a protective atmosphere, and roasting at the temperature of 500-1000 ℃ to remove arsenic in the arsenic-containing smoke dust in copper smelting in the form of arsenic oxide.
The invention has the technical key point that the arsenic-containing smoke dust produced in the copper smelting and the iron sulfide-containing materials are subjected to solid-phase reaction under a proper temperature condition, so that heavy metals such as copper, lead, zinc and the like in the arsenic-containing smoke dust produced in the copper smelting are effectively fixed, simultaneously arsenic is selectively converted into volatile arsenic trioxide, and the volatilization and recovery of the arsenic trioxide are realized. In the presence of iron sulfide, at a temperature of 500-1000 ℃ (preferably 550-700 ℃), and under inert atmosphere conditions, arsenic-containing smoke dust in copper smelting mainly undergoes the following main reactions:
As2O3(s)＝As2O3(g)↑；
As2O5+S＝As2O3(g)↑+SO2↑；
1.455Me3(AsO4)2+3FeS2＝4.364MeS+Fe3O4+1.455As2O3↑+1.636SO2↑；
from the above reactions it can be seen that lead and zinc are mainly converted to stable metal sulphides, enriched in the slag phase, while iron is converted to magnetite, the slag phase can be returned directly to the smelting system, while arsenic is converted to arsenic trioxide, which can be recovered by cooling.
The invention uses the material containing ferric sulfide as the arsenic removing additive, compared with the existing arsenic removing agents such as coke, the roasting temperature is greatly reduced, and the invention is beneficial to reducing energy consumption.
In the preferred scheme, the roasting temperature is 500-1000 ℃, and is preferably controlled at 550-700 ℃.
In the preferable scheme, the mass of the pyrite is 20-50% of that of the arsenic-containing smoke dust in the copper smelting, and the pyrite and the arsenic-containing smoke dust in the copper smelting are in favor of selectively converting arsenic into As by selecting a proper proportion2O3。
In the preferred scheme, the arsenic-containing smoke dust and the pyrite in the copper smelting process are dried, then are crushed to the particle size of less than 2mm, and are uniformly mixed.
In a preferred scheme, the roasting process comprises the following steps: placing a mixed material of arsenic-containing smoke dust and a material containing ferric sulfide in copper smelting in a furnace, introducing nitrogen and/or argon as a protective gas, raising the temperature to 500-1000 ℃ at a heating rate of 10-40 ℃/min, and roasting for 10-60 min
In the preferred scheme, volatile matters generated in the roasting process are cooled to recover arsenic trioxide, tail gas is absorbed by alkaline solution, and slag generated in the roasting process returns to a smelting system.
The method for removing arsenic from arsenic-containing smoke dust in copper smelting comprises the following steps:
1) drying the copper smelting smoke dust and the pyrite, crushing until the particle size is smaller than 2mm, and uniformly mixing the arsenic-containing smoke dust in the copper smelting and the pyrite according to the addition of 20-50% of the pyrite to obtain a mixed material;
2) and (2) putting the mixed material obtained in the step 1) into a furnace, introducing nitrogen gas into the furnace for roasting, controlling the temperature at 500-1000 ℃, roasting for 10-60 min, and enabling arsenic to be separated from smoke dust in the form of arsenic oxide at the heating rate of 10-40 ℃/min, directly returning roasting residues to a smelting system for circulation, and absorbing tail gas by using an alkali solution.
Compared with the prior art, the technical scheme of the invention has the following technical effects:
1. the invention adopts the material containing iron sulfide (such as pyrite) as the dearsenifying additive of the arsenic-containing smoke dust in the copper smelting, not only realizes dearsenification at lower temperature, but also greatly improves the dearsenification rate of the arsenic, which is up to more than 88 percent. Compared with the existing dearsenifying process of arsenic-containing smoke dust in copper smelting, the method has the advantages of low energy consumption, good dearsenifying effect, no secondary pollution and obvious technical advantages,
2. the invention selectively converts the arsenic-containing smoke dust in copper smelting into arsenic trioxide, is beneficial to the recovery of arsenic and realizes the recycling of arsenic oxide.
3. The method has the advantages of simple process flow, flexible operation, low energy consumption, contribution to reducing the production cost of enterprises and good economic and social benefits.
Drawings
FIG. 1 is an XRD (X-ray diffraction) pattern of a volatile product in the dearsenification process of arsenic-containing smoke dust in copper smelting.
Detailed Description
The following examples or embodiments are intended to further illustrate the present invention and are not intended to limit the scope of the claims.
Example 1
The embodiment selects the electric dust collection for smelting in a certain copper smelting plant in Hunan province, the main element composition of the electric dust collection is shown in Table 1, the additive is pyrite, and the specific implementation steps are as follows:
TABLE 1 composition of main elements (%) -for electric smelting dust collection in certain copper smeltery of Hunan province
Figure BDA0001880917440000041
The method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 30% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature at 700 ℃, the roasting time at 60min and the heating rate at 20 ℃/min, digesting the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis to obtain the roasted residue with the As content of 1.61% and the arsenic removal rate of 92.28%. The XRD pattern of the calcined volatile is shown in FIG. 1, and from FIG. 1 it can be seen that arsenic is totally converted to arsenic trioxide for removal.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.
Example 2
The embodiment selects the electric dust collection for smelting in a certain copper smelting plant in Hunan province, the main element composition of the electric dust collection is shown in Table 2, the additive is pyrite, and the specific implementation steps are as follows:
TABLE 2 composition of main elements (%) -for electric smelting dust collection in certain copper smeltery of Hunan province
Figure BDA0001880917440000042
The method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 30% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature at 700 ℃, the roasting time at 5min, setting the heating rate at 20 ℃/min to digest the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis, so that the content of As in the roasted residue is 3.23%, and the arsenic removal rate is 69.73%.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.
Example 3
The embodiment selects the electric dust collection for smelting in a certain copper smelting plant in Hunan province, the main element composition of the electric dust collection is shown in Table 3, the additive is pyrite, and the specific implementation steps are as follows:
TABLE 3 composition of main elements (%) -for electric smelting dust collection in certain copper smeltery of Hunan province
Figure BDA0001880917440000051
The method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 30% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature at 400 ℃, the roasting time at 60min and the heating rate at 20 ℃/min, digesting the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis to obtain the roasted residue with the As content of 14.75% and the arsenic removal rate of 22.18%.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.
Example 4
The embodiment selects the electric dust collection for smelting in a certain copper smelting plant in Hunan province, the main element composition of the electric dust collection is shown in Table 4, the additive is pyrite, and the specific implementation steps are as follows:
table 4 composition table of major elements (%) -of electric dust collection for smelting in copper smelter of Hunan province
Figure BDA0001880917440000052
The method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 10% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature at 700 ℃, the roasting time at 60min and the heating rate at 20 ℃/min, digesting the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis to obtain the roasted residue with the As content of 11.05% and the arsenic removal rate of 48.49%.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.
Example 5
The embodiment selects a certain copper smelting plant in Hunan province for smelting electric dust collection, the additive is pyrite, and the specific implementation steps are as follows:
the method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 60% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature to be 550 ℃, the roasting time to be 40min, and the heating rate to be 20 ℃/min, digesting the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis, so As to obtain the roasted residue with the As content of 2.33% and the arsenic removal rate of 81.83%.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.
Example 6
The embodiment selects a certain copper smelting plant in Hunan province for smelting electric dust collection, the additive is pyrite, and the specific implementation steps are as follows:
the method comprises the following steps: respectively taking the copper smelting electric dust collection and the pyrite, drying at low temperature, crushing until the particle size is less than 2mm, and uniformly mixing the copper smelting smoke dust and the pyrite according to the addition of 28% of the pyrite to obtain a mixed material.
Step two: weighing 5g of the mixture in a canoe crucible, placing the canoe crucible in a tube furnace for roasting, setting the roasting temperature to be 550 ℃, the roasting time to be 40min, and the heating rate to be 20 ℃/min, digesting the roasted sample, and sending the digested sample to an inductively coupled plasma emission spectrometer (ICP-OES) for analysis, so that the content of As in the roasting residue is 1.55%, and the arsenic removal rate is 94.68%.
Step three: and tail gas enters a tail gas absorption device, so that the pollution to the environment is reduced.

Claims (3)

1. A method for removing arsenic from copper smelting smoke dust is characterized by comprising the following steps: mixing the arsenic-containing smoke dust in copper smelting with a material containing ferric sulfide, placing the mixture in a protective atmosphere, heating to 550-700 ℃ at a heating rate of 10-40 ℃/min, and roasting for 40-60 min to remove arsenic in the arsenic-containing smoke dust in copper smelting in the form of arsenic oxide; the mass of the material containing the ferric sulfide is 20-50% of that of the arsenic-containing smoke dust generated in the copper smelting process; the material containing the iron sulfide is pyrite.
2. The method for removing arsenic from copper smelting dust according to claim 1, wherein the method comprises the following steps: the arsenic-containing smoke dust and the iron sulfide-containing materials in the copper smelting process are dried and then crushed to the particle size of less than 2 mm.
3. The method for removing arsenic from copper smelting dust according to claim 1, wherein: volatile matters generated in the roasting process are cooled to recover arsenic trioxide, tail gas is absorbed by alkaline solution, and slag generated in the roasting process returns to a smelting system.
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CN110218871A (en) * 2019-05-21 2019-09-10 铜仁学院 A method of arsenic-selective recycles in flue dust containing arsenical copper
CN110669941A (en) * 2019-09-19 2020-01-10 云南锡业研究院有限公司 Method for selectively removing arsenic and recovering valuable metal from white smoke
CN111235397A (en) * 2020-03-10 2020-06-05 云南锡业研究院有限公司 Process for efficiently treating copper smelting smoke dust
CN111996383B (en) * 2020-08-25 2022-01-25 中南大学 Method for separating arsenic from copper slag by matching high-arsenic materials
CN112251609B (en) * 2020-11-03 2022-02-01 云南省生态环境科学研究院 Method for resource utilization of copper smelting smoke dust
CN113526548B (en) * 2021-07-13 2022-07-22 广西凯玺有色金属有限公司 Process method for clean disposal of high-arsenic hazardous waste
CN114752754B (en) * 2022-04-26 2023-04-25 昆明理工大学 Method for removing arsenic from black copper mud
CN115354146B (en) * 2022-08-11 2023-04-07 红河砷业有限责任公司 Method for strengthening white smoke dearsenification by triple process superposition
CN115679109B (en) * 2022-11-14 2024-04-09 中南大学 Method for selectively recycling heavy metals in copper smelting smoke dust

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CN106367602B (en) * 2016-09-13 2018-07-24 昆明理工大学 A kind of method that high-arsenic antimony flue dust vulcanization detaches arsenic and recycles antimony
CN107779607B (en) * 2017-11-01 2019-06-28 紫金铜业有限公司 A kind of method of the high arsenic smoke dust low cost dearsenification of Copper making

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