CN112063849A - Method for recovering zinc from blast furnace gas mud - Google Patents
Method for recovering zinc from blast furnace gas mud Download PDFInfo
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- CN112063849A CN112063849A CN202010349231.9A CN202010349231A CN112063849A CN 112063849 A CN112063849 A CN 112063849A CN 202010349231 A CN202010349231 A CN 202010349231A CN 112063849 A CN112063849 A CN 112063849A
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- blast furnace
- zinc
- gas mud
- furnace gas
- hydrogen bond
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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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- 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
-
- 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
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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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 recovering zinc in blast furnace gas mud, belonging to the field of comprehensive utilization of metallurgical solid waste. The method of the invention comprises the following steps: and (3) enabling the hydrogen bond donor and the hydrogen bond acceptor to be in a molar ratio of 1-2: 1-4, uniformly mixing, and stirring at 60-80 ℃ for 12-24 hours to obtain a leaching agent; according to the liquid-solid ratio of 10-20: mixing 1mL/g of gas mud with the leaching agent, and leaching for 10-30 hours under the conditions of stirring rotation speed of 200-500 revolutions/minute and temperature of 323-373K to obtain ore pulp; directly carrying out electrodeposition on the ore pulp to obtain zinc; the electrodeposition adopts a three-electrode system and a potentiostatic method for deposition; the temperature of the electrodeposition is 323-373K; the hydrogen bond donor is at least one of choline chloride or betaine hydrochloride; the hydrogen bond acceptor is an amide compound. The invention has short process flow, eliminates the influence of other metal impurities in the gas mud and has low energy consumption. The recovery rate of zinc in the gas mud is high.
Description
Technical Field
The invention relates to a method for recovering zinc in blast furnace gas mud, belonging to the field of comprehensive utilization of metallurgical solid waste.
Background
The blast furnace gas mud is dust discharged along with blast furnace gas generated in the iron making process of iron and steel enterprises, mainly contains valuable elements such as iron, carbon, zinc and the like, and has the value and the potential of comprehensive recycling. According to statistics, the generated amount of the blast furnace gas mud is about 4% of the iron output, the zinc content in the gas mud is between 4% and 10%, the zinc content in part of enterprises can reach more than 13%, the Chinese crude steel output in 2018 reaches 9.283 hundred million t, and the gas mud output can reach more than 3700 million t through calculation. Taking an iron-making plant producing 1000 million tons per year as an example, 40 million tons of gas mud solid waste has a zinc content of 1.6-4.0 million tons and an industrial value of 2.72-6.8 million yuan (2020 zinc price: 1# zinc, 1.7 million yuan/t). The blast furnace gas mud exists in the form of waste in iron and steel enterprises, which not only causes serious environmental pollution, but also has the problems of resource waste and land occupation. At present, the mode of recovering zinc resources from blast furnace gas mud is mainly to smelt the sintered agglomerates again and recycle the sintered agglomerates, but the blast furnace gas mud is directly sintered and recycled, so that the air permeability of sintered furnace materials is influenced, the dezincification capability is poor, the accumulation of zinc is easy to cause the nodulation on the upper part of a blast furnace, and the service life of the blast furnace is influenced. At present, the blast furnace gas mud pyrogenic process treatment technology which is applied industrially comprises an OXY-CUP process, a rotary kiln process, a rotary hearth furnace process and the like, but has the obvious problems of overlarge one-time investment, low production rate, overhigh cost, overhigh energy consumption and the like. Therefore, the zinc-containing resource in the gas mud is recycled, so that the waste is changed into valuable, the method has great significance for recycling the solid waste resource, and the method has great significance for realizing the resource optimization configuration and the economic sustainable development of the iron and steel enterprises. Therefore, finding a technological means capable of realizing high recovery rate of zinc in gas mud, short flow, low cost and low pollution is a development direction of the gas mud zinc extraction technology in the future.
The invention provides a novel process for leaching blast furnace gas mud and recovering zinc through electrodeposition, which takes the blast furnace gas mud generated in the blast furnace ironmaking process as a raw material and aims at solving the problems of long process flow, high production cost, serious equipment corrosion, difficult separation of impurities and the like in the process of extracting metal zinc from the gas mud. The process takes the eutectic solvent dissolved with the gas mud as the electrolyte, zinc is electrodeposited in a three-electrode system, the production flow is obviously shortened, the production cost and the equipment requirement are reduced, the influence of other metal impurities is eliminated, and the energy consumption is reduced.
Disclosure of Invention
The invention provides a method for recovering zinc in blast furnace gas mud, which aims to shorten the process for extracting metal zinc from the blast furnace gas mud.
In order to solve the problems, the method for recovering zinc from blast furnace gas mud comprises the following steps:
(1) and (3) enabling the hydrogen bond donor and the hydrogen bond acceptor to be in a molar ratio of 1-2: 1-4, uniformly mixing, and stirring at 60-80 ℃ for 12-24 hours to obtain a leaching agent;
(2) according to the liquid-solid ratio of 10-20: mixing 1mL/g of gas mud with the leaching agent, and leaching for 10-40 h under the conditions of stirring speed of 200-500 rpm and temperature of 323-373K to obtain ore pulp;
(3) directly carrying out electrodeposition on the ore pulp obtained in the step (2) to obtain zinc; the electrodeposition adopts a three-electrode system and a potentiostatic method for deposition; the temperature of the electrodeposition is 323-373K;
the hydrogen bond donor is at least one of choline chloride or betaine hydrochloride;
the hydrogen bond acceptor is an amide compound.
The liquid-solid ratio is 10-20: the unit of 1 is a volume-to-mass ratio mL/g.
Preferably, the hydrogen bond donor in step (1) is choline chloride.
Preferably, the hydrogen bond acceptor in step (1) is at least one of formamide, acrylamide, acetamide or urea.
Preferably, the recovered blast furnace gas mud of step (1) has a particle size of 74 μm or less.
Preferably, the temperature in the step (2) is 323-343K.
Preferably, the deposition time of the electrodeposition in the step (2) is 1-24 h.
Preferably, the deposition time of the electrodeposition in the step (2) is 1-12 h.
Preferably, the three-electrode system in step (3) is: the cathode is a red copper sheet; the auxiliary electrode is a platinum column; the reference electrode was Ag/AgCl.
Preferably, the surface of the red copper sheet in the step (3) is polished to be bright and is washed by deionized water and absolute ethyl alcohol.
Preferably, the deposition potential deposited by the potentiostatic method in the step (3) is determined by performing cyclic voltammetry on the eutectic solvent-blast furnace gas mud, and the deposition potential deposited by the potentiostatic method in the step (3) is determined between the initial reduction potential and the peak potential of zinc (II) by analyzing the reduction peak of zinc (II).
Has the advantages that:
the method for recovering zinc from blast furnace gas mud has the technical effects that:
1. the method adopts the eutectic solvent to leach the gas mud and the electrodeposition process to prepare the metal zinc, has the advantages of short process flow, difficult corrosion on equipment, low equipment requirement, environmental friendliness and the like compared with the traditional process, and realizes the comprehensive utilization of the gas mud;
2. the eutectic solvent used in the invention belongs to a green chemical solvent, and compared with functional ionic liquids such as imidazole, pyrrole and the like, the eutectic solvent has the advantages of simple synthesis and low price.
3. The method of the invention eliminates the influence of other metal impurities in the gas mud and reduces the energy consumption.
4. By adopting the process conditions of the invention, the leaching rate of zinc in the gas mud is high, and the recovery rate is high.
Drawings
FIG. 1 is a cyclic voltammogram of example 1 after leaching of blast furnace gas sludge with a eutectic solvent;
fig. 2 is an SEM image of the zinc deposition layer obtained in example 1;
fig. 3 is an EDS spectrum of the zinc deposition layer obtained in example 1.
Detailed Description
The method for recovering zinc from blast furnace gas mud comprises the following steps:
(1) and (3) enabling the hydrogen bond donor and the hydrogen bond acceptor to be in a molar ratio of 1-2: 1-4, uniformly mixing, and stirring at 60-80 ℃ for 12-24 hours to obtain a leaching agent;
(2) according to the liquid-solid ratio of 10-20: mixing 1mL/g of gas mud with the leaching agent, and leaching for 10-40 h under the conditions of stirring speed of 200-500 rpm and temperature of 323-373K to obtain ore pulp;
(3) directly carrying out electrodeposition on the ore pulp obtained in the step (2) to obtain zinc; the electrodeposition adopts a three-electrode system and a potentiostatic method for deposition; the temperature of the electrodeposition is 323-373K;
the hydrogen bond donor is at least one of choline chloride or betaine hydrochloride;
the hydrogen bond acceptor is an amide compound.
One embodiment is: the hydrogen bond donor in the step (1) is choline chloride.
One embodiment is: the hydrogen bond acceptor in the step (1) is formamide, acrylamide, acetamide or urea.
One embodiment is: the particle size of the recovered blast furnace gas mud in the step (1) is less than 74 mu m.
One embodiment is: and (3) controlling the temperature 323-343K in the step (2).
One embodiment is: and (3) the deposition time of the electrodeposition in the step (2) is 1-24 h.
One embodiment is: and (3) the deposition time of the electrodeposition in the step (2) is 1-12 h.
One embodiment is: the three electrode systems in the step (3) are as follows: the cathode is a red copper sheet; the auxiliary electrode is a platinum column; the reference electrode was Ag/AgCl.
One embodiment is: polishing the surface of the red copper sheet in the step (3) to be bright, and washing with deionized water and absolute ethyl alcohol.
One embodiment is: and (3) carrying out cyclic voltammetry on the deposition potential deposited by the potentiostatic method, namely the blast furnace gas mud, and determining the deposition potential deposited by the potentiostatic method in the step (3) between the initial reduction potential and the peak potential of the zinc (II) by analyzing the reduction peak of the zinc (II).
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
The blast furnace gas mud adopted by the embodiment of the invention is taken from a certain iron plant in Sichuan, and the main metal elements are iron, calcium, zinc and titanium. The experimental sample is ground by a mortar and sieved to be-74 mu m, and the ore sample is dried at the constant temperature of 80 ℃ for 12h and dried to constant weight for experiment. The leaching experiment is carried out by controlling the experiment conditions such as liquid-solid ratio, leaching temperature, leaching time, stirring speed and the like, supernatant is taken after the experiment is finished, the zinc content in the leaching solution is respectively determined by EDTA titration, and the leaching rate is determined by calculation. Cyclic voltammetry tests and electrodeposition experiments were performed on an electrochemical workstation.
Example 1
The embodiment 1 of the invention provides a method for leaching blast furnace gas mud and recovering zinc through electrodeposition, which comprises the following steps:
(1) firstly, mixing choline chloride and urea according to a molar ratio of 1: 2, placing the mixture in a beaker, uniformly mixing the mixture, and heating and stirring the mixture at the temperature of 80 ℃ for 12 hours to form a eutectic solvent as a leaching agent;
(2) then adding 5g of blast furnace gas mud into 50mL of eutectic solvent, stirring at 300 rpm and 343K for 20h, titrating by EDTA and calculating the leaching rate of zinc to be 71%;
(3) then, the leached ore pulp is subjected to cyclic voltammetry test, a cyclic voltammetry curve of the eutectic solvent leached blast furnace gas mud in the embodiment is shown in figure 1 in detail, zinc (II) is reduced when the zinc (II) is reduced to-1.45V as shown in figure 1, and the deposition potential is-1.45V;
(4) and finally, carrying out three-electrode constant potential deposition, wherein the deposition potential is-1.45V, the temperature is 343K, and the time is 4h, so that a coating containing 98% of zinc and with uniform grain size of about 1 mu m is obtained.
The three electrode systems are: the cathode is a red copper sheet; the auxiliary electrode is a platinum column; the reference electrode was Ag/AgCl. Polishing the surface of the red copper sheet to be bright, and washing with deionized water and absolute ethyl alcohol.
The cyclic voltammogram, the SEM image of the electrodeposited zinc coating, and the EDS spectrum of the blast furnace gas mud leached by the eutectic solvent in this example are shown in fig. 1, fig. 2, and fig. 3.
The reduction is started when the voltage is-1.45V as shown in figure 1, and the zinc coating prepared by the zinc recovered from the gas mud according to the invention is well combined with the matrix, the grain size is more uniform, the crystallization is good, and the purity of the zinc is higher as shown in figure 2 and figure 3. The process is further optimized, and the zinc can be directly plated on the iron sheet for practical production.
Example 2
The embodiment 2 of the invention provides a method for leaching blast furnace gas mud and recovering zinc through electrodeposition, which comprises the following steps:
(1) firstly, mixing choline chloride and urea according to a molar ratio of 1: 2, placing the mixture in a beaker, uniformly mixing the mixture, and heating and stirring the mixture at the temperature of 70 ℃ for 18 hours to form a eutectic solvent as a leaching agent;
(2) then 2.5g of blast furnace gas mud is added into 50mL of eutectic solvent, the stirring speed is 400 r/min, the temperature is 353K, the leaching time is 30h, EDTA titration is carried out, and the leaching rate of zinc is calculated to be 73%;
(3) and performing cyclic voltammetry on the leached ore pulp, and determining the deposition potential by analyzing the reduction peak of zinc (II).
(4) And finally, carrying out three-electrode constant potential deposition, wherein the deposition potential is-1.5V, the temperature is 343K, and the time is 4h, so as to obtain a coating containing 98.2% of zinc.
Example 3
The embodiment 3 of the invention provides a method for leaching blast furnace gas mud and recovering zinc through electrodeposition, which comprises the following steps:
(1) firstly, mixing choline chloride and urea according to a molar ratio of 1: 2, placing the mixture in a beaker, uniformly mixing the mixture, and heating and stirring the mixture at the temperature of 60 ℃ for 20 hours to form a eutectic solvent as a leaching agent;
(2) then adding 5g of blast furnace gas mud into 50mL of eutectic solvent, stirring at 400 rpm, at 333K for 30h, titrating with EDTA and calculating the leaching rate of zinc to be 71.5%;
(3) and performing cyclic voltammetry on the leached ore pulp, and determining the deposition potential by analyzing the reduction peak of zinc (II).
(4) And finally, carrying out three-electrode constant potential deposition, wherein the deposition potential is-1.48V, the temperature is 343K, and the time is 12h, so as to obtain a coating containing 98.5% of zinc.
Example 4
The embodiment 4 of the invention provides a method for leaching blast furnace gas mud and recovering zinc through electrodeposition, which comprises the following steps:
(1) firstly, mixing betaine hydrochloride and urea according to a molar ratio of 1: 3, placing the mixture in a beaker, uniformly mixing the mixture, and heating and stirring the mixture at the temperature of 75 ℃ for 24 hours to form a eutectic solvent as a leaching agent;
(2) then adding 5.0g of blast furnace gas mud into 50mL of eutectic solvent, stirring at 300 r/min and at 353K for 24h, titrating by EDTA and calculating the leaching rate of zinc to be 74%;
(3) and performing cyclic voltammetry on the leached ore pulp, and determining the deposition potential by analyzing the reduction peak of zinc (II).
(4) And finally, carrying out three-electrode constant potential deposition, wherein the deposition potential is-1.44V, the temperature is 343K, and the time is 4h, so that a coating containing 97.8% of zinc is obtained.
Claims (10)
1. The method for recovering zinc from blast furnace gas mud is characterized by comprising the following steps:
(1) and (3) enabling the hydrogen bond donor and the hydrogen bond acceptor to be in a molar ratio of 1-2: 1-4, uniformly mixing, and stirring at 60-80 ℃ for 12-24 hours to obtain a leaching agent;
(2) according to the liquid-solid ratio of 10-20: mixing 1mL/g of gas mud with the leaching agent, and leaching for 10-40 h under the conditions of stirring speed of 200-500 rpm and temperature of 323-373K to obtain ore pulp;
(3) directly carrying out electrodeposition on the ore pulp obtained in the step (2) to obtain zinc; the electrodeposition adopts a three-electrode system and a potentiostatic method for deposition; the temperature of the electrodeposition is 323-373K;
the hydrogen bond donor is at least one of choline chloride or betaine hydrochloride;
the hydrogen bond acceptor is an amide compound.
2. The method for recovering zinc from blast furnace sludge as claimed in claim 1, wherein the hydrogen bond donor in step (1) is choline chloride.
3. The method for recovering zinc from blast furnace gas mud according to claim 1 or 2, wherein the hydrogen bond acceptor in step (1) is at least one of formamide, acrylamide, acetamide or urea.
4. The method for recovering zinc from blast furnace gas sludge as claimed in claim 1 or 2, wherein the particle size of the recovered blast furnace gas sludge of step (1) is 74 μm or less.
5. The method for recovering zinc from blast furnace gas mud according to any one of claims 1 to 4, wherein the temperature in the step (2) is 323 to 343K.
6. The method for recovering zinc from blast furnace gas mud according to any one of claims 1 to 5, wherein the deposition time of the electrodeposition in the step (2) is 1 to 24 hours.
7. The method for recovering zinc from blast furnace gas mud according to claim 6, wherein the deposition time of the electrodeposition in the step (2) is 1-12 h.
8. The method for recovering zinc from blast furnace gas mud according to any one of claims 1 to 7, wherein the three-electrode system in the step (3) is as follows: the cathode is a red copper sheet; the auxiliary electrode is a platinum column; the reference electrode was Ag/AgCl.
9. The method for recovering zinc from blast furnace gas mud of claim 8, wherein the surface of the red copper sheet in the step (3) is polished to be bright and is washed by deionized water and absolute ethyl alcohol.
10. The method for recovering zinc from blast furnace gas mud according to any one of claims 1 to 9, wherein the deposition potential deposited by the potentiostatic method in step (3) is between the initial reduction potential and the peak potential of zinc (II) by performing cyclic voltammetry on the eutectic solvent-blast furnace gas mud.
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| CN202010349231.9A CN112063849A (en) | 2020-04-28 | 2020-04-28 | Method for recovering zinc from blast furnace gas mud |
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| CN202010349231.9A CN112063849A (en) | 2020-04-28 | 2020-04-28 | Method for recovering zinc from blast furnace gas mud |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113215412A (en) * | 2021-05-10 | 2021-08-06 | 上海第二工业大学 | Method for selectively leaching and recovering silver on surface of waste silver-plated piece or silver-containing solid waste |
| CN114317984A (en) * | 2022-01-04 | 2022-04-12 | 华北理工大学 | Method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasonic synergy |
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| US20040089613A1 (en) * | 2002-08-14 | 2004-05-13 | Consortium Fur Elecktrochemische Industrie Gmbh & Co. Kg | Removal of zinc salts from nonaqueous synthesis solutions comprising zinc alkoxides or zinc amides |
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2020
- 2020-04-28 CN CN202010349231.9A patent/CN112063849A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040089613A1 (en) * | 2002-08-14 | 2004-05-13 | Consortium Fur Elecktrochemische Industrie Gmbh & Co. Kg | Removal of zinc salts from nonaqueous synthesis solutions comprising zinc alkoxides or zinc amides |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113215412A (en) * | 2021-05-10 | 2021-08-06 | 上海第二工业大学 | Method for selectively leaching and recovering silver on surface of waste silver-plated piece or silver-containing solid waste |
| CN113215412B (en) * | 2021-05-10 | 2022-07-29 | 上海第二工业大学 | Method for selectively leaching and recovering silver on surface of waste silver-plated part or silver-containing solid waste |
| CN114317984A (en) * | 2022-01-04 | 2022-04-12 | 华北理工大学 | Method for selectively soaking zinc by utilizing cyclone classification-ionic liquid-ultrasonic synergy |
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Application publication date: 20201211 |