CN108118158B - Method for extracting valuable metals from sulfide slag and blast furnace gas ash - Google Patents
Method for extracting valuable metals from sulfide slag and blast furnace gas ash Download PDFInfo
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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
- C22B7/02—Working-up flue dust
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- C22B1/02—Roasting processes
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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- C22B30/06—Obtaining bismuth
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Abstract
The invention discloses a method for extracting valuable metals from sulfide slag and blast furnace gas ash, which comprises the steps of taking sulfide slag and gas ash as raw materials, adding coke and/or coal powder, mixing and granulating, then roasting at low temperature, reselecting a roasted solid product to separate zinc sulfide ore and an arsenic-bismuth alloy, then separating the arsenic-bismuth alloy to obtain metal arsenic and bismuth, recovering mercury in roasted flue gas, smelting the final slag, and fusing the final slag with the existing smelting process to form closed cycle. The method has simple process and low energy consumption, realizes the low-temperature cooperative treatment of the sulfuric acid sludge and the gas generated by the ironmaking blast furnace, and greatly reduces the enterprise cost and the environmental pollution risk especially for the gas ash with high zinc content and the sulfide slag with high arsenic and mercury content; the method realizes the high-efficiency recovery of the metal zinc, arsenic, bismuth and mercury in the waste residue and the gas ash, is green and pollution-free in the whole technical process, and realizes the aim of clean production.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and relates to a method for extracting valuable metals from sulfide slag and blast furnace gas ash.
Background
The waste acid sulfide slag of a zinc smelting system is one of main dangerous wastes generated by heavy nonferrous metal smelteries, is a product after flue gas washing, and has high arsenic and mercury contents. At present, the sulfuration method is a main method for treating waste acid, part of sulfide generated by the sulfuration method is returned to a smelting system, and arsenic, mercury and the like circulate in the system; the other part is stably solidified and detoxified and then is buried, on one hand, valuable metals in sulfides are not recycled, which wastes arsenic and mercury resources, on the other hand, a large amount of land is occupied by stacking and burying, and the hidden danger of pollution to the environment is brought; some of the waste slag are even stolen, and arsenic and mercury are also key pollutants discharged by non-ferrous smelting waste slag.
On the other hand, the yield of steel in China reaches 8.08 hundred million tons in 2016, blast furnace gas ash is solid waste obtained by dust collection of raw gas produced by an iron-making blast furnace, the yield is about 4 percent of the iron yield, the quantity is considerable, and the yield per year reaches 3000 ten thousand tons. The main components of the composition are zinc oxide, iron and carbon, and a certain amount of chlorine fluoride is also contained. If the ecological environment is not reasonably disposed, the ecological environment including water, atmosphere and soil can be directly polluted and damaged greatly. Meanwhile, the blast furnace gas ash also contains a large amount of valuable metals such as zinc, silver, indium, germanium and the like, so that the blast furnace gas ash is not recycled, and secondary resource waste is caused. The conventional treatment method of a steel mill returns to a sintering process or participates in pelletizing, and both methods cannot comprehensively recover valuable metals in the steel mill, so that the metals are accumulated in a main process in a circulating manner, a blast furnace is prevented from running smoothly, and the treatment capacity is small; the conventional treatment method of the nonferrous industry is used as a burdening of an ISP (internet service provider) process to enter a lead-zinc smelting system, but the problems of high energy consumption and low-concentration sulfur dioxide of the ISP process cannot be solved well all the time. From the perspective of promoting the pollution prevention and control of heavy metals and the development of circular economy, an important development direction is how to recover valuable metals while performing harmless treatment on solid waste resources in a smelting process flow and realize the recycling of the solid waste.
In the chinese patent CN 101078053A, a rotary kiln is adopted for reduction and volatilization, so that valuable metals of indium, zinc, lead, bismuth and the like in gas ash enter into dust collection, neutral acid leaching and high-temperature strong acid leaching are performed on recovered smoke dust to separate zinc, lead and bismuth, and then extraction, back extraction and vacuum distillation impurity removal electrolysis are performed to obtain high-purity indium, which is a wet-fire combined process for recovering indium, zinc, lead and bismuth of high-value nonferrous metals, and the process is relatively long, and waste acid and wastewater in the process also needs special system treatment.
In the Chinese patent CN 102085526A, blast furnace gas ash is recovered by adopting a mineral separation method, the blast furnace gas ash is made into ore pulp, and the ore pulp is subjected to magnetic separation, gravity separation, strong magnetic separation and flotation, wherein the flotation comprises a product obtained by rough two times of fine scanning and is sent to be made into cemented filling products. The blast furnace gas ash is completely recycled without repeated discharge, and the whole method is separated circularly to achieve zero discharge.
In the chinese patent CN 102319617A, a combined process flow of flotation and carbon recovery and gravity-magnetic separation is adopted, gas ash is slurried, carbon concentrate is finally obtained through rough flotation-fine flotation, tailings of rough flotation and fine flotation are reselected to obtain reselected concentrate, and tailings of reselected tailings are subjected to weak magnetic separation to obtain weak magnetic separation concentrate and reselected concentrate, which are combined into final iron concentrate.
In Chinese patent CN 104911356A, blast furnace gas ash is comprehensively recovered by adopting a rotary kiln fuming enrichment technology, kiln tailings are treated and subjected to innocent treatment by utilizing a combined mineral separation technology and then stockpiled, and the problems of short kiln age, high energy consumption and low concentration SO in the iron vanadium slag treatment process are solved2The harm problem can also eliminate the difficult problems of poor iron selection effect and overhigh ZnO fluorine-containing chlorine in the gas ash recovery process.
In the Chinese patent CN 204738004U, an oxygen-enriched side-blown process is adopted to send blast furnace gas ash, limestone and coal into an oxygen-enriched side-blown furnace, smelted pig iron is discharged through a pig iron discharge port, slag is discharged through a siphon pool and is sent to a slag granulation system, and smelted flue gas is discharged from a flue and enters a flue gas purification system. The 2 nd to 4 th patents are all process researches carried out by taking iron and carbon as recovered products, and the process does not produce high-value nonferrous metals such as zinc, bismuth, lead and germanium in an enrichment way.
In the Chinese patent CN 105568002A, contaminated acid sulfide slag is added into copper electrolyte, bismuth and arsenic in the sulfide slag enter into solution, copper is enriched in the copper sulfide slag, the solution is evaporated to concentrate acid and then is cooled and crystallized to separate out a mixture of bismuth oxide and arsenic oxide, the bismuth in the mixture is extracted by selective leaching, and tail liquid returns to the solution rich in bismuth and arsenic for circulation. The method focuses on extracting bismuth and arsenic from the sulfide slag, and does not relate to enrichment extraction of mercury in the sulfide slag.
Disclosure of Invention
The invention aims to solve the problems that valuable metal resources are wasted due to the hidden danger of environmental pollution caused by the stacking and burying of the waste acid and sulfide slag of a zinc smelting system, and valuable metals in the traditional production process of blast furnace gas ash cannot be effectively recovered, the energy consumption is high, sulfur dioxide flue gas is treated and the like, and provides a method for extracting valuable metals from the sulfide slag and the blast furnace gas ash, which has the advantages of low energy consumption, small waste gas amount, high metal recovery rate and easiness in industrial production.
The invention provides a method for extracting valuable metals from sulfide slag and blast furnace gas ash, which takes sulfide slag and gas ash as raw materials, adds coke and/or coal powder, carries out low-temperature roasting after mixing and granulating, separates zinc sulfide ore and arsenic-bismuth alloy by gravity separation of roasted solid products, then separates arsenic-bismuth alloy to obtain metal arsenic and bismuth, recovers mercury in roasted flue gas, and finally carries out smelting to fuse with the current smelting process to form closed cycle.
Preferably, the mass ratio of the sulfide slag to the gas ash is 1 (1.4-1.7).
Preferably, the adding amount of the coke and/or the coal powder is 10-20% of the mass of the sulfide slag.
Preferably, clay is added as a binder in the mixing and granulating process, and the adding amount of the clay is 10-15% of the weight of the vulcanized slag.
Preferably, the low-temperature roasting temperature is 300-700 ℃, and the multi-phase reaction of zinc oxide in the gas ash and arsenic sulfide, mercury sulfide and bismuth sulfide in the sulfide slag is facilitated under the temperature condition, the sulfide state is converted into a metal state, a part of zinc oxide is converted into metal steam and then is recovered by condensation, and carbon dioxide and carbon monoxide gas are discharged.
Preferably, the low-temperature roasting time is 2-3 h.
Preferably, the sulfide slag is the sulfide slag after the acid treatment of the lead-zinc system.
Preferably, the gas ash is solid waste obtained by collecting dust from raw gas produced by an iron-making blast furnace.
Preferably, the arsenic-bismuth alloy adopts a vacuum separation method to obtain metal arsenic and metal bismuth.
Preferably, the mercury in the roasting flue gas is recovered by a deep cooling method or an adsorption method.
The method comprises the steps of carrying out gravity separation on the obtained zinc sulfide ore and arsenic-bismuth alloy, then carrying out flotation separation on the zinc sulfide ore to obtain zinc sulfide, obtaining metal arsenic and metal bismuth from the arsenic-bismuth alloy by adopting a vacuum separation method, and recycling mercury in the roasting flue gas by utilizing a cryogenic method or an adsorption method, wherein the gravity separation method, the flotation method, the vacuum separation method, the cryogenic method or the adsorption method are typical production processes, and technological parameters of the existing production practice can be used for reference.
The reaction temperature of the method is within the range of 300-700 ℃, and ZnO in the gas ash and As in the sulfide slag2S3Coke and/or coal fines mainly react as follows:
As2S3+ZnO+3C＝3ZnS(s)+As(s)+3CO(g) (1)
As2S3+3ZnO+3/2C＝3ZnS(s)+2As(s)+3/2CO2(g) (2)
in the invention, ZnO in the gas ash and HgS, coke and/or coal powder in the sulfide slag mainly react at the reaction temperature of 300-700 ℃ as follows:
HgS+ZnO+C＝Hg(g)+ZnS(s)+CO(g) (3)
2HgS+2ZnO+C＝2Hg(g)+2ZnS(s)+CO2(g) (4)
the reaction temperature of the method is 300-700 ℃, and ZnO in the gas ash and Bi in the sulfide slag2S3Coke and/or coal fines mainly react as follows:
Bi2S3+3ZnO+3C＝2Bi+3ZnS+3CO(g) (5)
Bi2S3+3ZnO+3C＝2Bi+3ZnS+3CO(g) (6)
compared with the prior art, the invention has the beneficial technical effects that:
1) the method has simple process and low energy consumption, realizes the low-temperature cooperative treatment of the waste acid sulfide slag and the gas generated by the ironmaking blast furnace, and greatly reduces the enterprise cost and the environmental pollution risk especially for the gas ash with high zinc content and the sulfide slag with high arsenic and mercury content.
2) The invention realizes the high-efficiency recovery of the metal zinc, arsenic, bismuth and mercury in the polluted sulfide slag and the gas ash, the whole technical process is green and pollution-free, and the aim of clean production is realized.
Drawings
FIG. 1 is a process flow diagram of the present invention for treating contaminated acid sulfide slag and blast furnace gas ash.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The blast furnace gas ash in the embodiment of the invention comprises the following main components (wt%): 26.32 percent of Zn, 23.17 percent of Fe, 0.02 percent of Cu0.02 percent of Cd, 0.03 percent of Co, 0.01 percent of As, 0.17 percent of Sb, 0.34 percent of F and 3.8 percent of Cl; main constituents (wt.%) of the sulphided slag (dry slag): 40.33 percent of S, 10.19 percent of As, 6.82 percent of Zns, 4.45 percent of Bi, 2.47 percent of Pb, 0.82 percent of Sb0.82 percent of Fe, 0.74 percent of Se, 0.63 percent of Cu, 0.16 percent of Ni and 0.15 percent of Hg.
Example 1
Weighing 500g of sulfide slag, 700g of gas ash, 50g of coke and 50g of clay respectively, mixing uniformly, granulating, transferring into a graphite crucible, placing into an electric furnace, roasting for 2.0h at 500 ℃, cooling to obtain 1203g of conversion product, passing flue gas in the whole roasting process through a condenser, wherein the product obtained by the condenser is 9.87g, performing gravity separation on the conversion product to obtain zinc sulfide ore and arsenic-bismuth alloy, performing flotation on the zinc sulfide ore to obtain zinc sulfide, obtaining metal arsenic and metal bismuth from the arsenic-bismuth alloy by adopting a vacuum separation method, and recovering mercury in the roasted flue gas by utilizing an adsorption method, wherein the specific process flow is shown in figure 1.
Analysis of the calcined product gave: the phase of arsenic is mainly metallic arsenic, accounting for 89.15% of the total arsenic; the phase of bismuth is mainly metal bismuth, and accounts for 96.71 percent of the total bismuth; the phase of zinc is mainly ZnS and accounts for 93.54 percent of the total zinc, and the phase of mercury in the smoke is metallic mercury and accounts for 97.87 percent of the total mercury.
Example 2
Weighing 500g of sulfide slag, 850g of gas ash, 100g of coal powder and 75g of clay respectively, uniformly mixing and granulating, transferring into a graphite crucible, putting into an electric furnace, roasting for 5 hours at 300 ℃, cooling to obtain 1326g of conversion product, allowing flue gas in the whole roasting process to pass through a condenser, allowing 17.05g of product obtained by the condenser, performing gravity separation on the conversion product to obtain zinc sulfide ore and arsenic-bismuth alloy, performing flotation on the zinc sulfide ore to obtain zinc sulfide, allowing the arsenic-bismuth alloy to obtain metal arsenic and metal bismuth by adopting a vacuum separation method, and recovering mercury in the roasted flue gas by using a cryogenic method, wherein the specific process flow is shown in figure 1.
Analysis of the calcined product gave: the phase of arsenic is mainly metallic arsenic, accounting for 70.71 percent of the total arsenic; the phase of bismuth is mainly metal bismuth, and accounts for 85.86% of the total bismuth; the zinc phase is mainly ZnS and accounts for 84.66% of the total zinc, the mercury phase in the smoke is metallic mercury and accounts for 73.2% of the total mercury, and the mercury oxide accounts for 4.1%.
Example 3
Weighing 500g of sulfide slag, 800g of gas ash, 80g of coke and 70g of clay respectively, mixing uniformly, granulating, transferring into a graphite crucible, placing into an electric furnace, roasting for 2.0h at 700 ℃, cooling to obtain 1237g of conversion product, passing the flue gas in the whole roasting process through a condenser, wherein the product obtained by the condenser is 22.17g, performing gravity separation on the conversion product to obtain zinc sulfide ore and arsenic-bismuth alloy, performing flotation on the zinc sulfide ore to obtain zinc sulfide, obtaining metal arsenic and metal bismuth from the arsenic-bismuth alloy by adopting a vacuum separation method, and recovering mercury in the roasted flue gas by utilizing an adsorption method, wherein the specific process flow is shown in figure 1.
Analysis of the calcined product gave: the phase of arsenic is mainly metallic arsenic, accounting for 90.15% of the total arsenic; the phase of bismuth is mainly metal bismuth, and accounts for 97.36 percent of the total bismuth; the zinc phase is mainly ZnS accounting for 96.75% of the total zinc, the mercury phase in the smoke is metal mercury accounting for 92.17% of the total mercury, the mercury oxide accounting for 5.70% of the total mercury, and the total mercury volatilization rate accounting for 97.87%.
Example 4
Weighing 500g of sulfide slag, 800g of gas ash, 80g of coke and 70g of clay respectively, uniformly mixing and granulating, transferring into a graphite crucible, putting into an electric furnace, roasting for 1.0h at 700 ℃, cooling to obtain 1220g of conversion product, allowing flue gas in the whole roasting process to pass through a condenser, allowing the product obtained by the condenser to be 23.05g, performing gravity separation on the conversion product to obtain zinc sulfide ore and arsenic-bismuth alloy, performing flotation on the zinc sulfide ore to obtain zinc sulfide, allowing the arsenic-bismuth alloy to obtain metal arsenic and metal bismuth by adopting a vacuum separation method, and recovering mercury in the roasted flue gas by using a cryogenic method, wherein the specific process flow is shown in figure 1.
Analysis of the calcined product gave: the phase of arsenic is mainly metallic arsenic, which accounts for 88.93% of the total arsenic; the phase of bismuth is mainly metal bismuth, and accounts for 96.69% of the total bismuth; the zinc phase is mainly ZnS and accounts for 95.32% of the total zinc, the mercury phase in the smoke is metallic mercury and accounts for 90.28% of the total mercury, and the mercury oxide accounts for 4.3%.
Example 5
Respectively weighing 500g of sulfide slag, 750g of gas ash, 60g of coal powder and 50g of clay, uniformly mixing and granulating, transferring into a graphite crucible, placing into an electric furnace, roasting for 4.0h at 600 ℃, cooling to obtain 1264g of conversion product, passing flue gas in the whole roasting process through a condenser, wherein the product obtained by the condenser is 12.27g, performing gravity separation on the conversion product to obtain zinc sulfide ore and arsenic-bismuth alloy, then performing flotation on the zinc sulfide ore to obtain zinc sulfide, obtaining metal arsenic and metal bismuth from the arsenic-bismuth alloy by adopting a vacuum separation method, and recovering mercury in the roasted flue gas by utilizing an adsorption method, wherein the specific process flow is shown in figure 1.
Analysis of the calcined product gave: the phase of arsenic is mainly metallic arsenic, which accounts for 88.16% of the total arsenic; the phase of bismuth is mainly metal bismuth, and accounts for 97.65 percent of the total bismuth; the zinc phase is mainly ZnS and accounts for 95.72% of the total zinc, the mercury phase in the smoke is metallic mercury and accounts for 95.31% of the total mercury, and the mercury oxide accounts for 4.18%.
Claims (5)
1. A method for extracting valuable metals from sulfide slag and blast furnace gas ash comprises the steps of taking sulfide slag and gas ash as raw materials, adding coke and/or coal powder, mixing and granulating, roasting at low temperature, cooling to obtain a conversion product, performing gravity separation on the conversion product to obtain zinc sulfide ore and an arsenic-bismuth alloy, separating the arsenic-bismuth alloy to obtain metal arsenic and bismuth, recovering mercury in roasted flue gas, and smelting the final slag;
the low-temperature roasting temperature is 600-700 ℃, and the low-temperature roasting time is 2-3 h;
the gas ash is solid waste obtained by collecting dust from raw gas produced by an iron-making blast furnace;
the sulfide slag is obtained after the acid treatment of a lead-zinc system;
the mass ratio of the sulfide slag to the gas ash is 1 (1.4-1.7).
2. The method for extracting valuable metals from the vulcanized slag and the blast furnace gas ash according to claim 1, wherein the addition amount of the coke and/or the pulverized coal is 10-20% of the mass of the vulcanized slag.
3. The method for extracting valuable metals from vulcanized slag and blast furnace gas ash as claimed in claim 1, wherein clay is added as a binder during the mixing and granulating process, wherein the amount of the added clay is 10-15% of the weight of the vulcanized slag.
4. The method for extracting valuable metals from sulfide slag and blast furnace gas ash as claimed in any one of claims 1 to 3, wherein the arsenic bismuth alloy is subjected to vacuum separation to obtain metallic arsenic and metallic bismuth.
5. The method for extracting valuable metals from sulfide slag and blast furnace gas ash as claimed in any one of claims 1 to 3, wherein mercury in the roasting flue gas is recovered by a cryogenic method or an adsorption method.
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