CN116103508A - Device and method for leaching slag from reduced zinc - Google Patents

Device and method for leaching slag from reduced zinc Download PDF

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Publication number
CN116103508A
CN116103508A CN202310085154.4A CN202310085154A CN116103508A CN 116103508 A CN116103508 A CN 116103508A CN 202310085154 A CN202310085154 A CN 202310085154A CN 116103508 A CN116103508 A CN 116103508A
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reaction
zinc
slag
pipe
leaching
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CN202310085154.4A
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Inventor
王私富
朱北平
陶家荣
李鹏
夏永生
俞凌飞
胡智润
赵永喜
李云
冉厚建
张冯
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Yunxi Wenshan Zinc Indium Smelting Co ltd
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Yunxi Wenshan Zinc Indium Smelting Co ltd
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Priority to CN202310085154.4A priority Critical patent/CN116103508A/en
Publication of CN116103508A publication Critical patent/CN116103508A/en
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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
    • 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
    • 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
    • C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
    • 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
    • C22B3/02—Apparatus therefor
    • 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
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • 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
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • C22B58/00—Obtaining gallium or indium
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a device and a method for leaching slag by reducing zinc, wherein the device comprises the following steps: the reduction front groove is used for mixing the zinc leaching slag and the acid liquor; the reaction kettles are communicated with the pre-reduction groove through a first communication pipe, the reaction kettles are connected in series through slide pipes, the slide pipes are connected with the discharge holes of the reaction kettles, and the reaction kettles are provided with air inlets; and the flash tank is connected with the chute through a second communicating pipe and is provided with a flash tank delivery pipe. Therefore, the leaching rate of valuable metals in the zinc leaching slag can be improved, and the higher leaching rates of zinc, indium and copper are realized; the problems of difficult index monitoring, large index fluctuation, complex equipment mechanism, difficult maintenance and the like in the reduction leaching process are solved, the operation method is simplified, the industrial operation stability is improved, and the overhaul and maintenance frequency is greatly reduced.

Description

Device and method for leaching slag from reduced zinc
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a device and a method for reducing zinc leaching slag.
Background
Generally, zinc smelting systems have higher zinc content in generally leached zinc-containing materials, and common treatment methods include pyrogenic treatment or high-acid leaching and iron precipitation, and the following methods are summarized: the rotary kiln fuming method, the chlorofuming method, the hot acid leaching-hematite iron-precipitating method, the hot acid leaching-goethite iron-precipitating method and the hot acid leaching-iron alum iron-precipitating method are adopted, wherein the wet hot acid strengthening leaching is mostly adopted in the zinc smelting industry at present for saving energy, improving the operation environment and improving the recovery rate, and the hot acid leaching is an effective method for destroying zinc ferrite, but zinc, iron and indium enter a solution together in the hot acid leaching process of zinc leaching slag, and most of iron exists in a ferric ion form. Along with the dissolution of a large amount of iron compounds in leaching slag, a large amount of iron enters the solution in the form of ferric ions, in the subsequent iron separation process of the leaching solution, in order to avoid the entering of valuable metals such as zinc, indium, copper and the like into the slag in the iron precipitation process, the ferric ions in the leaching solution are usually required to be reduced into ferrous ions, and then copper and indium are recovered by a displacement method and a neutralization hydrolysis method, however, the prior art and equipment still have larger problems, such as complex equipment structure and lower leaching rate of zinc, indium and copper.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent.
In a first aspect of the invention, the invention provides a device for reducing zinc leach slag. The device comprises a reduction front groove, wherein the reduction front groove is used for mixing zinc leaching slag and acid liquor; the reaction kettles are communicated with the pre-reduction groove through a first communication pipe, the reaction kettles are connected in series through slide pipes, the slide pipes are connected with the discharge holes of the reaction kettles, and the reaction kettles are provided with air inlets; and the flash tank is connected with the chute through a second communicating pipe and is provided with a flash tank delivery pipe. Therefore, the device can improve the leaching rate of valuable metals in the zinc leaching slag, and realize higher leaching rates of zinc, indium and copper; at the same time, fe in the leaching solution 3+ Is reduced to Fe 2+ And Fe is added with 3+ The concentration of the zinc leaching residue is controlled in a reasonable range, so that the problems of difficult index monitoring, large index fluctuation, complex equipment mechanism, difficult maintenance and the like in the reduction leaching process are solved, the process method of the reduced zinc leaching residue can be simplified by a merchant, the industrial operation stability is improved, and the overhaul and maintenance frequency of the device is greatly reduced.
According to the embodiment of the invention, the chute is gradually inclined to the bottom of the reaction kettle in the arrangement direction of the pre-reduction tank, the reaction kettles and the flash tank.
According to the embodiment of the invention, the heights of the reaction kettles are sequentially reduced, and the height difference among a plurality of reaction kettles is 10-50 cm.
According to the embodiment of the invention, the slide pipe is provided with a plurality of sampling pipes, and the sampling pipes are arranged in one-to-one correspondence with the reaction kettles and are used for sampling liquid in the reaction kettles.
According to an embodiment of the present invention, the reduced zinc leach slag apparatus further includes: a zinc leaching slag feeding pipe connected with the first feed inlet of the reduction front tank; the acid liquor feeding pipe is connected with the second feed inlet of the reduction front tank through a third communicating pipe; and the heat exchanger is respectively connected with the acid liquor feeding pipe and the third communicating pipe.
According to the embodiment of the invention, the top of the reaction kettle is provided with a first exhaust pipe orifice, and the first exhaust pipe orifice is connected with the pre-reduction tank through a first exhaust gas collecting pipe; the side wall of the reaction kettle is provided with at least one steam pipe orifice.
According to the embodiment of the invention, the side wall of the reaction kettle is provided with a plurality of steam pipe orifices, and the steam pipe orifices are symmetrically distributed on the side wall of the reaction kettle.
According to the embodiment of the invention, the top of the flash tank is provided with a second exhaust pipe orifice, and the second exhaust pipe orifice is connected with the pre-reduction tank through a second exhaust gas collecting pipe.
According to an embodiment of the invention, the pre-reduction tank is provided with a first stirrer, a plurality of reaction kettles are provided with second stirrers, and the flash tank is provided with a third stirrer.
In another aspect of the present invention, the present invention provides a method of reducing zinc leaching slag, the method comprising: uniformly mixing zinc leaching residues and acid liquor in a reduction front tank to obtain a first mixed liquor; the first mixed liquid enters a plurality of reaction kettles through a first communication pipe, sulfur dioxide gas is introduced into the reaction kettles through air inlet pipe orifices of the reaction kettles, so that the zinc leaching slag, the acid liquor and the sulfur dioxide gas react for a certain time to obtain ore pulp products, wherein pressure difference exists among the reaction kettles; the reaction product enters the flash tank through the second communicating pipe and is output to the leaching liquid through the flash tank delivery pipe. Therefore, the method can improve the leaching rate of valuable metals in the zinc leaching slag,realizes higher leaching rate of zinc, indium and copper; at the same time, fe in the leaching solution 3+ Is reduced to Fe 2+ And Fe is added with 3+ The concentration of the water is controlled in a reasonable range, so that the problems of difficult monitoring of indexes, large index fluctuation, complex equipment mechanism, difficult maintenance and the like in the reduction leaching process are solved, the operation method is simplified, the industrial operation stability is improved, and the overhaul and maintenance frequency is greatly reduced.
According to the embodiment of the invention, before the acid liquor is mixed with the zinc leaching slag, the acid liquor is subjected to heating treatment in advance, and the acid liquor is heated to 70-90 ℃.
According to the embodiment of the invention, the solid-to-liquid ratio of the zinc leaching slag to the acid liquor is 6:1-10:1.
According to the embodiment of the invention, the reaction of the zinc leaching slag, the acid liquor and the sulfur dioxide gas in the reaction kettle meets at least one of the following conditions: the reaction temperature in the reaction kettle is 100-120 ℃; the reaction time in the reaction kettle is 1-4 h; the pressure in the reaction kettle is 0.01 Mpa-0.2 Mpa; the pressure difference among the reaction kettles is 0.005 Mpa-0.05 Mpa; fe in the supernatant of the ore pulp product 3+ The concentration is 0.5-2 g/L.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram of a reduced zinc leach slag apparatus according to one embodiment of the present invention;
FIG. 2 is a schematic diagram of a reduced zinc leach slag apparatus according to another embodiment of the present invention;
FIG. 3 is a schematic flow diagram of a method of reducing zinc leach slag according to one embodiment of the present invention.
Reference numerals illustrate:
1: a reduction front tank; 2: a reaction kettle; 3: a first communication pipe; 4: a chute; 5: a discharge port; 6: an air inlet; 7: a flash drum; 8: a second communicating pipe; 9: flash drum send-out pipe; 10: a sampling tube; 11: a zinc leaching slag feed pipe; 12: a first feed port; 13: an acid liquid feeding pipe; 14: a third communicating pipe; 15: a second feed inlet; 16: a heat exchanger; 17: a first exhaust nozzle; 18: a first exhaust gas collection pipe; 19: a steam pipe orifice; 20: a second exhaust nozzle; 21: a second exhaust gas collection pipe; 22: a first agitator; 23: a second stirrer; 24: a third agitator; 25: a feed pump; 26: an output pump; 27: and a transfer pump.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In one aspect of the invention, the invention provides a device for reducing zinc leaching slag. Referring to fig. 1, the apparatus includes a pre-reduction tank 1, the pre-reduction tank 1 being used for mixing zinc leaching slag and acid liquor; a plurality of serially connected inversesThe reaction kettles 2 are communicated with the reduction front groove 1 through a first communication pipe 3, a plurality of reaction kettles 2 connected in series are connected through slide pipes 4, the slide pipes 4 are connected with a discharge port 5 of each reaction kettle 2, and the reaction kettles 2 are provided with air inlets 6; the flash tank 7, the flash tank 7 is connected to the chute 4 through the second communication pipe 8, and the flash tank 7 has a flash tank feed pipe 9. Therefore, the device can improve the leaching rate of valuable metals in the zinc leaching slag, and realize higher leaching rates of zinc, indium and copper; at the same time, fe in the leaching solution 3+ Is reduced to Fe 2+ And Fe is added with 3+ The concentration of the zinc leaching residue is controlled in a reasonable range, so that the problems of difficult index monitoring, large index fluctuation, complex equipment mechanism, difficult maintenance and the like in the reduction leaching process are solved, the process method of the reduced zinc leaching residue can be simplified by a merchant, the industrial operation stability is improved, and the overhaul and maintenance frequency of the device is greatly reduced. In some embodiments, the device provided by the invention can be used for reducing zinc leaching residues, so that the leaching rates of zinc, indium and copper are respectively higher than 99%, 95% and 97%.
For easy understanding, the principle of the present application that the above advantageous effects can be achieved will be briefly described below:
the invention provides a device for reducing zinc leaching slag, which comprises the steps of firstly, mixing zinc leaching slag and acid liquor in a reduction tank 1, wherein the zinc leaching slag contains valuable metals such as zinc, indium, copper, iron and the like, and the acid liquor is waste electrolyte and other acid-containing solutions such as sulfuric acid in a zinc smelting wet system; then, after the mixed solution of the zinc leaching residues and the acid liquor is conveyed to the reaction kettles 2 through the feeding pump 25 on the first communication pipe 3, the mixed solution enters a plurality of reaction kettles 2 connected in series through the chute 4, sulfur dioxide gas enters the reaction kettles 2 through the air inlet 6 of each reaction kettles 2 and reacts with the mixed solution to obtain ore pulp products, and the process mainly generates zinc ferrite dissolution reaction, wherein the reaction equation is as follows: znFe (ZnFe) 2 O 4 +4H + +SO 2 ＝Zn 2+ +2Fe 2+ +SO 4 2- +2H 2 O, fe in the system 3+ Reduction to Fe 2+ Valuable metals such as zinc, indium, copper, iron and the like in the zinc leaching slag are dissolved out; finally, the ore pulp product enters through the chute 4 and the second communicating pipe 8In the flash tank 7, the flash tank 7 is heated to remove the sulfur dioxide, which is the waste gas in the pulp product, and then the final pulp product is output through the flash tank outlet pipe 9 and the pulp through the output pump 26 on the flash tank outlet pipe 9.
According to the embodiment of the invention, the air inlet 6 of the reaction kettle 2 is positioned at the bottom of the reaction kettle, and sulfur dioxide compressed gas is introduced into the reaction kettle through the air inlet 6, so that the sulfur dioxide gas and the mixed solution in the reaction kettle can be fully mixed, and the reaction efficiency of the reaction is improved.
According to the embodiment of the present invention, the reaction vessel 2 is a vertical reaction vessel, wherein the number of reaction vessels, the size of the reaction vessel, and the like are not limited, and can be flexibly set by a person skilled in the art according to actual requirements such as raw material consumption, yield, and the like.
According to the embodiment of the invention, referring to fig. 1, in the arrangement direction (X) of the pre-reduction tank 1, the plurality of reaction kettles 2 and the flash tank 7, the chute 4 gradually inclines towards the bottom of the reaction kettles 2, so that the mixed liquor of zinc leaching slag and acid liquor can flow from the first reaction kettles 2 to the last reaction kettles 2 in sequence along the inclination of the chute 4 in the X direction, and finally enter the flash tank 7. Wherein, the discharge gate that reation kettle 2 and elephant trunk 4 are connected sets up below the liquid level of mixed solution to establish pressure differential through static pressure, carry the ore pulp flow.
According to the embodiment of the invention, referring to fig. 1, the heights of the reaction kettles 2 are sequentially reduced in the X direction, and the height difference among the plurality of reaction kettles 2 is 10-50 cm, so that the chute inclination angle alpha is 10-30 degrees, and the inventor finds that the height difference of the reaction kettles 2 and the inclination of the chute 4 are kept in the range, so that the flow rate of ore pulp can be better ensured to be in an optimal state.
According to the embodiment of the invention, referring to fig. 1, a plurality of sampling pipes 10 are arranged on a chute 4, the plurality of sampling pipes 10 are arranged in one-to-one correspondence with a plurality of reaction kettles 2, and are used for sampling liquid in the reaction kettles 2 (namely, each reaction kettle is correspondingly provided with one sampling pipe so as to sample and detect ore pulp in each reaction kettle), wherein the sampling pipes 10 can be controlled by adopting manual or automatic valves, when the inclined chute 4 needs to be overhauled, a conveying pump on the chute 4 can be in a closed state, and ore pulp can also circulate through the sampling pipes 10 arranged on the reaction kettles 2, so that the process progress cannot be influenced.
According to an embodiment of the present invention, referring to fig. 1, the reduced zinc leach slag apparatus further includes: a zinc leaching slag feeding pipe 11, wherein the zinc leaching slag feeding pipe 11 is connected with a first feeding hole 12 of the pre-reduction tank 1; an acid liquor feed pipe 13, wherein the acid liquor feed pipe 13 is connected with a second feed inlet 15 of the reduction front tank 1 through a third communicating pipe 14; the heat exchanger 16, the heat exchanger 16 is connected with acidizing fluid inlet pipe 13 and third communicating pipe 14 respectively, and zinc leaches the sediment and flows into reduction front tank 1 through zinc leaches sediment inlet pipe 11 from first feed inlet 12, and the acidizing fluid flows into heat exchanger 16 through acidizing fluid inlet pipe 13, preheats in the heat exchanger 16, carries through delivery pump 27 on the third communicating pipe 14, flows into reduction front tank 1 from second feed inlet 15, so zinc leaches the sediment and mixes with the acidizing fluid in reduction front tank 1, and first agitator 22 stirs the mixed liquor and makes zinc leaches the sediment and mix evenly with the acidizing fluid.
According to the embodiment of the invention, referring to fig. 1, the top of the reaction kettle 2 is provided with a first exhaust pipe orifice 17, and the first exhaust pipe orifice 17 is connected with the pre-reduction tank 1 through a first exhaust gas collecting pipe 18, so that redundant sulfur dioxide gas in the reaction kettle 2 after the reaction is finished is discharged to the first exhaust gas collecting pipe 18 from the first exhaust pipe orifice 17 at the top of the reaction kettle 2 and is discharged into the pre-reduction tank 1 through the first exhaust gas collecting pipe 18, thereby not only avoiding the discharge of sulfur dioxide into the air to pollute the environment, but also enabling the continuous utilization of sulfur dioxide in the pre-reduction tank 1, and effectively reducing the cost.
In some embodiments of the present invention, referring to fig. 1, the sidewall of the reaction vessel 2 has at least one steam nozzle 19, so that a heating gas can be introduced into the reaction vessel 2 through the steam nozzle 19 to heat the mixed solution in the reaction vessel so that the reaction solution reaches a reaction temperature. In some embodiments, the reaction in the reaction vessel 2 requires that steam at 150-160 ℃ is introduced from the steam nozzle 19 on the side wall to heat the mixed solution, and the mixed solution is reacted under the stirring of the second stirrer 23.
According to the embodiment of the invention, referring to fig. 2, the side wall of the reaction kettle 2 is provided with a plurality of steam nozzles 19, and the steam nozzles 19 are symmetrically distributed on the side wall of the reaction kettle 2, so that the side wall of the reaction kettle 2 can be provided with the steam nozzles 19 which are symmetrically distributed, the steam inlet rate can be effectively improved, the heating uniformity is ensured, and meanwhile, the vibration of the reaction kettle 2 can be effectively reduced. The specific number of the steam nozzles 19 is not limited, and those skilled in the art can flexibly set according to actual requirements, where the steam nozzles 19 are not limited and are required to be symmetrically arranged on the side wall of the reaction kettle 2. In addition, the steam nozzle 19 is positioned above the liquid level of the mixed solution in the reaction kettle.
According to the embodiment of the invention, referring to fig. 1, the top of the flash tank 7 is provided with a second exhaust pipe orifice 20, the second exhaust pipe orifice 20 is connected with the pre-reduction tank 1 through a second exhaust gas collecting pipe 21, the ore pulp is stirred in the flash tank 7 by a third stirrer 24, generated exhaust gas or residual sulfur dioxide gas is discharged from the second exhaust pipe orifice 20 to the second exhaust gas collecting pipe 21 and then is conveyed into the pre-reduction tank 1 through the second exhaust gas collecting pipe 21, the discharge of sulfur dioxide into the air to pollute the environment is avoided, and the sulfur dioxide can be continuously utilized in the device, so that the cost can be effectively reduced.
In another aspect of the invention, the invention provides a method for reducing zinc leaching slag by using the device for reducing zinc leaching slag. The method comprises the following steps: uniformly mixing zinc leaching residues and acid liquor in a reduction front tank 1 to obtain a first mixed liquor; the first mixed solution enters a plurality of reaction kettles 2 through a first communication pipe 3, sulfur dioxide gas is introduced into the reaction kettles 2 through an air inlet pipe orifice 6 of the reaction kettles 2, so that zinc leaching residues, acid liquor and sulfur dioxide gas react for a certain time to obtain ore pulp products, wherein pressure difference exists among the plurality of reaction kettles 2; the reaction product enters the flash tank 7 through the second communicating pipe 8 and the leachate is output through the flash tank effluent pipe 9. Therefore, the method can improve the leaching rate of valuable metals in the zinc leaching slag, and realize higher leaching rates of zinc, indium and copper; at the same time, fe in the leaching solution 3+ Is reduced to Fe 2+ And Fe is added with 3+ The concentration of (2) is controlled in a reasonable range, and the reduction leaching process is solvedThe method has the advantages that the problems of difficult standard monitoring, large index fluctuation, complex equipment mechanism, difficult maintenance and the like are solved, the operation method is simplified, the industrial operation stability is improved, and the overhaul and maintenance frequency is greatly reduced. In some embodiments, the device provided by the invention can be used for reducing zinc leaching residues, so that the leaching rates of zinc, indium and copper are respectively higher than 99%, 95% and 97%.
The method of reducing zinc leaching residues according to the above embodiment of the present invention will be described in detail with reference to fig. 3.
S100: and uniformly mixing the zinc leaching slag and the acid liquor in the reduction front tank to obtain a first mixed liquor.
According to the embodiment of the invention, before the acid liquor is mixed with the zinc leaching slag, the acid liquor is subjected to heating treatment in the heat exchanger 16 in advance, and the acid liquor is heated to 70 ℃ -90 ℃ (such as 70 ℃, 75 ℃, 80 ℃, 85 ℃ and 90 ℃), and the inventor finds that the acid liquor preheating temperature can effectively remove impurities in the acid liquor within the range; the solid-liquid ratio of the zinc leaching slag and the acid liquor is 6:1-10:1 (such as 6:1, 7:1, 8:1, 9:1 and 10:1) and is uniformly mixed in the groove 1 before reduction to obtain a first mixed liquor.
The specific type of the acid solution and the concentration of the acid solution are not particularly required, and a person skilled in the art can flexibly select the acid solution according to practical situations, for example, the acid solution can be sulfuric acid, nitric acid or hydrochloric acid.
S200: the first mixed solution enters a plurality of reaction kettles 2 through a first communication pipe 3, and sulfur dioxide gas is introduced into the reaction kettles 2 through an air inlet pipe orifice 6 of the reaction kettles 2, so that zinc leaching residues, acid liquor and sulfur dioxide gas react for a certain time to obtain ore pulp products, wherein pressure difference exists among the plurality of reaction kettles 2.
In the steps, the reaction temperature in the reaction kettle 2 is 100-120 ℃ and the reaction time is 1-4 h, under the conditions, zinc leaching slag, acid liquor and sulfur dioxide gas can fully participate in the reaction, the generation of byproducts is reduced as much as possible, and the leaching rate of zinc, indium and copper is improved.
In the steps, the pressure in the reaction kettle is 0.01-0.2 Mpa, the pressure in the reaction kettle is controlled by the flow of the introduced sulfur dioxide gas, the pressure is favorable for improving the leaching rate of zinc, indium and copper, and if the sulfur dioxide is excessively introduced (the pressure is larger), the sulfur dioxide is relatively lost due to precipitation of part of valuable metals copper and indium.
In the above steps, the sulfur dioxide inflow of the plurality of reaction kettles 2 connected in series can be regulated, so that the overpressure in the reaction kettles is reduced in sequence in the X direction, and the pressure difference between the reaction kettles 2 is 0.005Mpa to 0.05Mpa, so that ore pulp conveying power is formed, and ore pulp can smoothly flow in a sealed system.
Further, after the mixed solution in the reaction kettle reacts for 1.5 to 2 hours, sampling analysis is carried out on the supernatant liquid in the monitoring ore pulp through a sampling tube 10 to control Fe 3+ Concentration is such that the supernatant of the pulp controls Fe 3+ The concentration is 0.5-2 g/L, thus controlling Fe by controlling the clear liquid on the ore pulp 3+ The concentration, the pressure in the reaction kettle and other parameters enable the dynamic change of the reaction overpressure to cooperatively regulate the reduction leaching of the zinc leaching slag, thereby ensuring the higher leaching rate of zinc, indium and copper.
S300: the reaction product enters the flash tank 7 through the second communicating pipe 8 and the leachate is output through the flash tank effluent pipe 9.
The following detailed description of embodiments of the invention is provided for the purpose of illustration only and is not to be construed as limiting the invention. In addition, all reagents employed in the examples below are commercially available or may be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
Example 1
The treatment objects are zinc leaching slag, mainly containing 23% of zinc, 35% of iron, 1.25% of copper and 0.08% of indium. The method adopts the device for leaching the slag from the reduced zinc shown in fig. 1, and comprises the following specific steps:
firstly, waste electrolyte in a zinc smelting wet method system is used as zinc leaching slag, an acid solution is preheated to 75 ℃ by a heat exchanger, then is uniformly mixed with zinc leaching slag bottom flow from a leaching system in a pre-reduction tank, and is conveyed into a vertical reaction kettle by a feed pump, zinc leaching slag and dilute sulfuric acid are introduced into sulfur dioxide compressed gas according to a liquid-solid ratio of 6:1 at a temperature of 110 ℃, and are reacted for 2.5h in the vertical reaction kettle with stirring, and after 1.5h of reaction, sampling analysis is carried out on pulp supernatant to control ferric ions at 0.5g/L. After the reaction kettles receive ore pulp, sulfur dioxide compressed gas is sequentially introduced into the plurality of reaction kettles connected in series, the reaction overpressure in the plurality of reaction kettles is controlled to be 0.01-0.2 Mpa, the plurality of vertical reaction kettles connected in series are controlled through sulfur dioxide introduction quantity, the overpressure is sequentially reduced, and the pressure difference between the kettles and the front of the kettles is controlled to be 0.005-0.05 Mpa so as to form ore pulp conveying power, so that ore pulp can smoothly flow in a sealed system.
Finally, the leaching rates of zinc, indium and copper by reduction leaching are respectively up to 99.1%, 95.3% and 97.2%.
Example 2
The treatment objects are zinc leaching slag, mainly containing 23% of zinc, 35% of iron, 1.25% of copper and 0.08% of indium. The method adopts the device for leaching the slag from the reduced zinc shown in fig. 1, and comprises the following specific steps:
firstly, waste electrolyte in a zinc smelting wet method system is used as zinc leaching slag, an acid solution is preheated to 90 ℃ by a heat exchanger, then is uniformly mixed with zinc leaching slag underflow from a leaching system in a pre-reduction tank, and is conveyed into a vertical reaction kettle by a pump, wherein the zinc leaching slag and dilute sulfuric acid are introduced into sulfur dioxide compressed gas according to a liquid-solid ratio of 10:1 at a temperature of 120 ℃, and are reacted for 4 hours in the vertical reaction kettle with stirring, and ferric ions are controlled at 0.5g/L by sampling analysis ore pulp supernatant after 1.5 hours of reaction through assay analysis. After the reaction kettles receive ore pulp, sulfur dioxide compressed gas is sequentially introduced into the plurality of reaction kettles connected in series, the reaction overpressure in the kettles is controlled to be 0.01-0.2 Mpa, the plurality of vertical reaction kettles connected in series are controlled through the sulfur dioxide introduction quantity, the overpressure is sequentially reduced, and the pressure difference between the kettles and the front of the kettles is controlled to be 0.005-0.05 Mpa so as to form ore pulp conveying power, so that the ore pulp can smoothly flow in a sealed system.
Finally, the leaching rates of zinc, indium and copper by reduction leaching are respectively up to 99.1%, 95.3% and 97.2%.
As can be seen from the above examples 1 and 2, the leaching rate of the reduction leached zinc, indium and copper can be greatly improved by the reduction zinc leaching slag device and the reduction method.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (13)

1. A reduced zinc leach slag apparatus, comprising:
the reduction front groove is used for mixing the zinc leaching slag and the acid liquor;
the reaction kettles are communicated with the pre-reduction groove through a first communication pipe, the reaction kettles are connected in series through slide pipes, the slide pipes are connected with the discharge holes of the reaction kettles, and the reaction kettles are provided with air inlets;
and the flash tank is connected with the chute through a second communicating pipe and is provided with a flash tank delivery pipe.
2. The apparatus for reducing zinc leaching slag according to claim 1, wherein the chute is gradually inclined toward the bottom of the reaction vessel in the direction of arrangement of the pre-reduction vessel, the plurality of reaction vessels, and the flash tank.
3. The reduced zinc leaching residue apparatus according to claim 2, wherein the height of the reaction kettles is sequentially reduced, and a height difference between the plurality of reaction kettles is 10 to 50 cm.
4. The reduced zinc leaching slag device according to claim 1, wherein a plurality of sampling pipes are arranged on the chute, and the sampling pipes are arranged in one-to-one correspondence with the reaction kettles and are used for sampling liquid in the reaction kettles.
5. The reduced zinc leach slag apparatus according to claim 1, further comprising:
a zinc leaching slag feeding pipe connected with the first feed inlet of the reduction front tank;
the acid liquor feeding pipe is connected with the second feed inlet of the reduction front tank through a third communicating pipe;
and the heat exchanger is respectively connected with the acid liquor feeding pipe and the third communicating pipe.
6. The reduced zinc leach slag apparatus according to claim 1, wherein a first vent pipe orifice is provided at a top of the reaction vessel, the first vent pipe orifice being connected to the pre-reduction tank by a first exhaust gas collection pipe; the side wall of the reaction kettle is provided with at least one steam pipe orifice.
7. The reduced zinc leach slag apparatus of claim 6, wherein the side wall of the reaction vessel has a plurality of steam nozzles, and the plurality of steam nozzles are symmetrically distributed on the side wall of the reaction vessel.
8. The reduced zinc leach slag apparatus according to claim 1, wherein a top of the flash drum has a second vent nozzle connected to the pre-reduction drum by a second flue gas collection pipe.
9. The reduced zinc leach slag apparatus according to claim 1, wherein the pre-reduction tank has a first stirrer, the plurality of reaction vessels has a second stirrer, and the flash tanks each have a third stirrer.
10. A method of reducing zinc leach slag using the reduced zinc leach slag apparatus according to any one of claims 1 to 9, comprising:
uniformly mixing zinc leaching residues and acid liquor in a reduction front tank to obtain a first mixed liquor;
the first mixed liquid enters a plurality of reaction kettles through a first communication pipe, sulfur dioxide gas is introduced into the reaction kettles through air inlet pipe orifices of the reaction kettles, so that the zinc leaching slag, the acid liquor and the sulfur dioxide gas react for a certain time to obtain ore pulp products, wherein pressure difference exists among the reaction kettles;
the reaction product enters the flash tank through the second communicating pipe and is output to the leaching liquid through the flash tank delivery pipe.
11. The method for reducing zinc leaching slag by a zinc leaching slag reducing device according to claim 10, wherein the acid liquor is heated to 70 ℃ to 90 ℃ in advance before being mixed with the zinc leaching slag.
12. The method for reducing zinc leaching residue by a zinc leaching residue reducing device according to claim 10, wherein the solid-to-liquid ratio of the zinc leaching residue to the acid solution is 6:1-10:1.
13. The method for reducing zinc leaching residue by a zinc leaching residue reducing device according to claim 10, wherein the reaction of the zinc leaching residue, the acid liquor and the sulfur dioxide gas occurring in the reaction kettle satisfies at least one of the following conditions:
the reaction temperature in the reaction kettle is 100-120 ℃;
the reaction time in the reaction kettle is 1-4 h;
the pressure in the reaction kettle is 0.01 Mpa-0.2 Mpa;
the pressure difference among the reaction kettles is 0.005 Mpa-0.05 Mpa;
fe in the supernatant of the ore pulp product 3+ The concentration is 0.5-2 g/L.
CN202310085154.4A 2023-01-29 2023-01-29 Device and method for leaching slag from reduced zinc Pending CN116103508A (en)

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CN202310085154.4A CN116103508A (en) 2023-01-29 2023-01-29 Device and method for leaching slag from reduced zinc

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Application Number Priority Date Filing Date Title
CN202310085154.4A CN116103508A (en) 2023-01-29 2023-01-29 Device and method for leaching slag from reduced zinc

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Publication Number Publication Date
CN116103508A true CN116103508A (en) 2023-05-12

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Country Link
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