CN114672665B - Processing technology for preparing zinc ingot by electrodeposition method - Google Patents
Processing technology for preparing zinc ingot by electrodeposition method 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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- 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
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/18—Extraction of metal compounds from ores or concentrates by wet processes with the aid of microorganisms or enzymes, e.g. bacteria or algae
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- 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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Abstract
The invention discloses a processing technology for preparing zinc ingots by an electro-deposition method; the invention uses the biological heap leaching technology to treat the zinc-containing waste, avoids the mode of high energy consumption and high pollution of the traditional acid leaching method, uses steel mill steel ash as the chemical energy source of ferrous oxide micro helicobacter in the zinc-containing waste, obviously improves the leaching rate of zinc of the zinc-containing waste under the synergistic effect of microorganisms and acid leaching, oxidizes extractant organic matters mixed in the electrodeposit liquid by ozone, destroys the coordination effect and releases Zn 2+ And dropwise adding zinc phosphate solution to further remove Fe in the electro-deposition solution 3+ The purity of the electro-deposition solution is improved, and the quality of zinc ingots is improved.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a processing technology for preparing zinc ingots by an electrodeposition method.
Background
In general, when zinc oxide ore is used to prepare zinc products, direct acid leaching treatment is often adopted, the zinc oxide ore is dissolved in acid solution and then is subjected to the next treatment, but one premise is that the zinc content in the zinc oxide ore is higher than 20% in the direct acid leaching treatment, and only under the condition, the zinc content in the solution prepared by the direct acid leaching can meet the concentration required by an electrodeposition process. Therefore, for zinc oxide ores with zinc content lower than 20%, direct acid leaching treatment can be carried out only after volatilization and enrichment are carried out by high-temperature metallurgical equipment such as a rotary kiln, but the zinc content in the zinc oxide ores exceeds 15% at the moment due to excessively high energy consumption, so that the method has enough economic benefit. Therefore, for low-quality zinc oxide ores with zinc content less than 15% and zinc-containing wastes generated in various production processes, another economical and less-pollution method is needed to realize the reutilization of the zinc-containing wastes
Disclosure of Invention
The invention aims to provide a processing technology for preparing zinc ingots by an electrodeposition method, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the processing technology for preparing the zinc ingot by the electrodeposition method is characterized by comprising the following steps of:
s1, adding 10% -30% of zinc-containing waste into a leaching tank, adding 40% -60% of sulfuric acid solution with the concentration of 16-28g/l, stirring and mixing, inoculating ferrous oxide micro-helicobacter, heating the leaching tank to 28-35 ℃, stirring at the speed of 100-150rpm, and culturing for 9-20 days;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30-40 parts of sulfuric acid solution with the concentration of 250-450g/L, stirring at the speed of 100-150rpm, performing heap leaching for 20-45 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 1% -10% of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 5.5-6.5, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction level is 5-8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1-1.5;
s5, back extraction is carried out by using sulfuric acid solution containing 170-250g/L sulfuric acid, and the mixing time is 10-15min compared with O/A which is 1-1.5:4-8;
s6, introducing ozone into the strip liquor for aeration for 15-30min, wherein the aeration mode is microHole aeration, aeration flow is 5-6L/m 3 After aeration is finished, heating the strip liquor to 60-70 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, cooling the back extraction liquid to room temperature, slowly dripping a sulfuric acid solution containing 0.1-0.5mol/L zinc phosphate into the back extraction liquid until no sediment is generated in the back extraction liquid, and dripping 3-5mL/m into the back extraction liquid 3 Ferric sulfate solution with the concentration of 0.1-3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Further, according to parts by weight, the zinc-containing waste comprises 2-4 parts of low-quality zinc oxide, 4-8 parts of zinc ash and 4-8 parts of steel ash, and the zinc-containing waste is subjected to ultrasonic oscillation treatment with the frequency of 30-45KHz for 1-3 hours.
In general, when zinc oxide ore is used to prepare zinc products, direct acid leaching treatment is often adopted, the zinc oxide ore is dissolved in acid solution and then is subjected to the next treatment, but one premise is that the zinc content in the zinc oxide ore is higher than 20% in the direct acid leaching treatment, and only under the condition, the zinc content in the solution prepared by the direct acid leaching can meet the concentration required by an electrodeposition process. Therefore, for zinc oxide ores with zinc content lower than 20%, direct acid leaching treatment can be carried out only after volatilization and enrichment are carried out by high-temperature metallurgical equipment such as a rotary kiln, but the zinc content in the zinc oxide ores exceeds 15% at the moment due to excessively high energy consumption, so that the method has enough economic benefit. Therefore, for low-quality zinc oxide ores with zinc content less than 15% and zinc-containing wastes generated in various production processes, another economical and less-pollution method is needed to realize the reutilization of the zinc-containing wastes.
The ferrous oxide micro-screw bacteria are gram negative bacteria, the optimal growth temperature is 30 ℃, the structure has flagella, the environment has better mobility, and Fe can be used as an inorganic energy autotrophic bacteria 2+ And (3) oxidation growth:
4Fe 2+ +O 2 +4H + →4Fe 3+ +2H 2 O
Zn+2Fe 3+ →2Fe 2+ +Zn 2+
the zinc-containing waste used in the invention contains steel mill steel ash components, the Zn content in the steel mill steel ash is 20% -60%, and a large amount of Fe is contained, and after being mixed with sulfuric acid, a large amount of Fe can be rapidly generated 2+ The component is used as a chemical energy source of ferrous oxide micro helicobacter, and ultrasonic vibration treatment is carried out on zinc-containing waste by using ultrasonic waves, so that cracks are generated in mineral particles to cause boundary fracture, the minerals are exposed, the bioleaching process is accelerated, and the heap leaching time is shortened.
After the zinc-containing waste is subjected to filter pressing, in order to further extract zinc element in the zinc-containing waste, the filter residue is subjected to further heap leaching by using a high-concentration sulfuric acid solution, the heap leaching time is prolonged, and the filter pressing is used again to extract the zinc element in the filter residue.
Because the zinc-containing waste used in the invention contains more steel dust in steel works, the filtrate after being pressed and filtered by the filter press contains more Fe 2+ With Fe 3+ During extraction, fe 3+ Will be matched with Zn in the filtrate 2+ Competing, leading to extracted Zn 2+ The purity is too low, which ultimately affects the quality of zinc electrowinning.
The invention is to carry out Zn 2+ Before extraction, the pH of the filtrate is adjusted by zinc hydroxide, and the pH of the solution is raised to 5.5-6.5 to lead Fe in the filtrate 2+ With Fe 3+ Fe (OH) formation 2 And Fe (OH) 3 And the concentration of extracted impurity ions during extraction is reduced by precipitation, and the consumption of an extracting agent is reduced.
In the back extraction process, trace extraction liquid organic matters are mixed in the back extraction liquid due to saponification in the extraction process, and in the electrodeposition process, the extraction liquid organic matters are loaded with Zn 2+ Forming a complex compound resulting in partial Zn 2+ Failure to release eventually leads to abnormal precipitation of the end electrodeposited product.
Therefore, the invention further comprises the following back extraction stepsOzone with strong oxidizing property is introduced into the back extraction liquid to decompose organic matters in the decomposed extraction liquid, so that the coordination effect is reduced, and Fe in the solution can be oxidized by ozone 2+ And the generated Fe is enabled to be generated by dripping zinc phosphate 3+ And generating ferric phosphate precipitate, and adding activated carbon for adsorption and sedimentation to further increase the purity of zinc produced by electrodeposition.
Further, the low-quality zinc oxide has a particle size of 30-60 μm.
Further, in the step S1, inoculating a ferrous oxide micro-helicobacter, including the following steps:
a. inoculating ferrous oxide micro-screw bacteria into a culture medium, wherein the culture medium contains (NH 4) 2SO4 0.05-0.15g/L, KCl 0.05-0.15g/L, K HPO4 0.05-0.15g/L, mgSO4.7H2O 0.5-1.5g/L, ca (NO 3) 2.01-0.03 g/L and FeSO4.7H2O 0.1-1g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5-2, placing the culture medium into an incubator, and culturing at the temperature of 28-32 ℃ for 36-48h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, and the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is (3) according to parts by weight: (4-7), adding 0.001-0.005 part of egg white into the culture barrel, after mixing, dropwise adding sulfuric acid solution into the culture barrel until the pH value in the culture barrel is 1.5-2.5, inoculating the ferrous oxide micro-screw bacteria cultured in the step a into the culture barrel, and culturing for 3-5 days;
c. and d, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into the leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank.
Further, in the step S4, the extract is a mixture of p204 extractant and No. 6 industrial light solvent, wherein the mixing ratio of p204 extractant is 20% and the mixing ratio of No. 6 industrial light solvent is 80%.
Further, in the step S4, the extract is a mixture of p204 extractant and No. 6 industrial light solvent, wherein the mixing ratio of p204 extractant is 20% and the mixing ratio of No. 6 industrial light solvent is 80%.
Further, in the step S8, the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the zinc ingot is obtained after electrolysis for 18-36 h.
Further, in the step S8, during the electrodeposition, a rectifying transformer is used, a lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell.
Compared with the prior art, the invention has the following beneficial effects: the invention uses the biological heap leaching technology to treat the zinc-containing waste, avoids the mode of high energy consumption and high pollution of the traditional acid leaching method, uses steel mill steel ash as the chemical energy source of ferrous oxide micro helicobacter in the zinc-containing waste, obviously improves the leaching rate of zinc of the zinc-containing waste under the synergistic effect of microorganisms and acid leaching, oxidizes extractant organic matters mixed in the electrodeposit liquid by ozone, destroys the coordination effect and releases Zn 2+ And dropwise adding zinc phosphate solution to further remove Fe in the electro-deposition solution 3+ The purity of the electro-deposition solution is improved, and the quality of zinc ingots is improved.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a flow chart of a process for preparing zinc ingots by the electrodeposition method of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1, according to parts by weight, 4 parts of low-quality zinc oxide is ball-milled into particles with the particle size of 30-60 mu m, uniformly mixed with 4 parts of zinc ash and 8 parts of steel ash, subjected to ultrasonic vibration treatment for 3 hours at the frequency of 45KHz, transferred into a leaching tank, added with 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirred and mixed, inoculated with ferrous oxide micro-helicobacter, maintained at the temperature of 28-32 ℃ in the leaching tank, stirred at the speed of 100rpm, and cultured for 9 days;
wherein, the inoculation of the ferrous oxide micro-helicobacter comprises the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ) 2 SO 4 0.15g/L、KCl 0.15g/L、K 2 HPO 4 0.15g/L、MgSO 4 .7H 2 O 1.5g/L、Ca(NO 3 ) 2 0.03g/L、FeSO 4 .7H 2 O1 g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5, placing the culture medium in an incubator at 28-32 ℃ for culturing for 36h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is 3:6 in parts by weight, 0.005 part of egg white is additionally added into the culture barrel, after mixing, sulfuric acid solution is dropwise added into the culture barrel until the pH value in the culture barrel is 1, and the ferrous oxide micro-screw bacteria cultured in the step a are inoculated into the culture barrel for 5 days;
c. b, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into a leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1;
wherein the extractant is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s6, introducing ozone into the strip liquor for aeration for 30min, wherein the aeration mode is microporous aeration, and the aeration flow is 6L/m 3 After aeration is finished, heating the strip liquor to 60 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, cooling the back extraction liquid to room temperature, slowly dropwise adding a sulfuric acid solution containing 0.1mol/L zinc phosphate into the back extraction liquid until no sediment is generated in the back extraction liquid, and dropwise adding 5mL/m into the back extraction liquid 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Example 2
This example increases the length of time that zinc-containing waste is treated with ferrous oxide micro-screw bacteria compared to example 1.
S1, according to parts by weight, 4 parts of low-quality zinc oxide is ball-milled into particles with the particle size of 30-60 mu m, uniformly mixed with 4 parts of zinc ash and 8 parts of steel ash, subjected to ultrasonic vibration treatment for 3 hours at the frequency of 45KHz, transferred into a leaching tank, added with 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirred and mixed, inoculated with ferrous oxide micro-helicobacter, maintained at the temperature of 28-32 ℃ in the leaching tank, stirred at the speed of 100rpm, and cultured for 15 days;
wherein, the inoculation of the ferrous oxide micro-helicobacter comprises the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ) 2 SO 4 0.15g/L、KCl 0.15g/L、K 2 HPO 4 0.15g/L、MgSO 4 .7H 2 O 1.5g/L、Ca(NO 3 ) 2 0.03g/L、FeSO 4 .7H 2 O1 g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5, placing the culture medium in an incubator at 28-32 ℃ for culturing for 36h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is 3:6 in parts by weight, 0.005 part of egg white is additionally added into the culture barrel, after mixing, sulfuric acid solution is dropwise added into the culture barrel until the pH value in the culture barrel is 1, and the ferrous oxide micro-screw bacteria cultured in the step a are inoculated into the culture barrel for 5 days;
c. b, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into a leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1; wherein the extractant is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s6, introducing ozone into the strip liquor for aeration for 30min, wherein the aeration mode is microporous aeration, and the aeration flow is 6L/m 3 After aeration is finished, heating the strip liquor to 60 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, cooling the back extraction liquid to room temperature, slowly dropwise adding a sulfuric acid solution containing 0.1mol/L zinc phosphate into the back extraction liquid until no sediment is generated in the back extraction liquid, and dropwise adding 5mL/m into the back extraction liquid 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Example 3
This example increases the length of time that zinc-containing waste is treated with ferrous oxide micro-screw bacteria compared to example 1.
S1, according to parts by weight, 4 parts of low-quality zinc oxide is ball-milled into particles with the particle size of 30-60 mu m, uniformly mixed with 4 parts of zinc ash and 8 parts of steel ash, subjected to ultrasonic vibration treatment for 3 hours at the frequency of 45KHz, transferred into a leaching tank, added with 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirred and mixed, inoculated with ferrous oxide micro-helicobacter, maintained at the temperature of 28-32 ℃ in the leaching tank, stirred at the speed of 100rpm, and cultured for 20 days;
wherein, the inoculation of the ferrous oxide micro-helicobacter comprises the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ) 2 SO 4 0.15g/L、KCl 0.15g/L、K 2 HPO 4 0.15g/L、MgSO 4 .7H 2 O 1.5g/L、Ca(NO 3 ) 2 0.03g/L、FeSO 4 .7H 2 O1 g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5, placing the culture medium in an incubator at 28-32 ℃ for culturing for 36h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is 3:6 in parts by weight, 0.005 part of egg white is additionally added into the culture barrel, after mixing, sulfuric acid solution is dropwise added into the culture barrel until the pH value in the culture barrel is 1, and the ferrous oxide micro-screw bacteria cultured in the step a are inoculated into the culture barrel for 5 days;
c. b, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into a leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1, wherein the extracting agent is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s6, introducing ozone into the strip liquor for aeration for 30min, wherein the aeration mode is microporous aeration, and the aeration flow is 6L/m 3 After aeration is finished, heating the strip liquor to 60 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, reversingCooling the extract liquid to room temperature, slowly dripping sulfuric acid solution containing 0.1mol/L zinc phosphate into the extract liquid until no precipitate is generated in the back extract liquid, and dripping 5mL/m into the extract liquid 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Example 4
This example reduces the duration of ozone treatment of the strip liquor compared to example 1.
S1, according to parts by weight, 4 parts of low-quality zinc oxide is ball-milled into particles with the particle size of 30-60 mu m, uniformly mixed with 4 parts of zinc ash and 8 parts of steel ash, subjected to ultrasonic vibration treatment for 3 hours at the frequency of 45KHz, transferred into a leaching tank, added with 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirred and mixed, inoculated with ferrous oxide micro-helicobacter, maintained at the temperature of 28-32 ℃ in the leaching tank, stirred at the speed of 100rpm, and cultured for 9 days;
wherein, the inoculation of the ferrous oxide micro-helicobacter comprises the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ) 2 SO 4 0.15g/L、KCl0.15g/L、K 2 HPO 4 0.15g/L、MgSO 4 .7H 2 O 1.5g/L、Ca(NO 3 ) 2 0.03g/L、FeSO 4 .7H 2 O1 g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5, placing the culture medium in an incubator at 28-32 ℃ for culturing for 36h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is 3:6 in parts by weight, 0.005 part of egg white is additionally added into the culture barrel, after mixing, sulfuric acid solution is dropwise added into the culture barrel until the pH value in the culture barrel is 1, and the ferrous oxide micro-screw bacteria cultured in the step a are inoculated into the culture barrel for 5 days;
c. b, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into a leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1, wherein the extracting agent is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s6, introducing ozone into the strip liquor for aeration for 15min, wherein the aeration mode is microporous aeration, and the aeration flow is 6L/m 3 After aeration is finished, heating the strip liquor to 60 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, cooling the back extraction liquid to room temperature, slowly dropwise adding a sulfuric acid solution containing 0.1mol/L zinc phosphate into the back extraction liquid until no sediment is generated in the back extraction liquid, and dropwise adding 5mL/m into the back extraction liquid 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Comparative example 1
In comparison with example 1, this comparative example does not use ferrous oxide micro-screw bacteria to treat zinc-containing waste.
S1, according to parts by weight, ball milling 4 parts of low-quality zinc oxide into particles with the particle size of 30-60 mu m, uniformly stirring and mixing the particles with 4 parts of zinc ash and 8 parts of steel ash, using ultrasonic oscillation with the frequency of 45KHz to treat for 3 hours, transferring the particles into a leaching tank, adding 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirring and mixing the particles, maintaining the temperature of the leaching tank at 28-32 ℃, stirring the particles at the speed of 100rpm, and heap leaching for 15 days;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1; wherein the extractant is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s6, introducing ozone into the strip liquor for aeration for 30min, wherein the aeration mode is microporous aeration, and the aeration flow is 6L/m 3 Min, after aeration is finished, mixingHeating the back extraction liquid to 60 ℃, preserving heat for 30min, and removing unreacted ozone in the back extraction liquid;
s7, cooling the back extraction liquid to room temperature, slowly dropwise adding a sulfuric acid solution containing 0.1mol/L zinc phosphate into the back extraction liquid until no sediment is generated in the back extraction liquid, and dropwise adding 5mL/m into the back extraction liquid 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Comparative example 2
In comparison with the examples, no ozone treatment strip liquor was used in this comparative example.
S1, according to parts by weight, 4 parts of low-quality zinc oxide is ball-milled into particles with the particle size of 30-60 mu m, uniformly mixed with 4 parts of zinc ash and 8 parts of steel ash, subjected to ultrasonic vibration treatment for 3 hours at the frequency of 45KHz, transferred into a leaching tank, added with 40 parts of sulfuric acid solution with the sulfuric acid concentration of 28g/L, stirred and mixed, inoculated with ferrous oxide micro-helicobacter, maintained at the temperature of 28-32 ℃ in the leaching tank, stirred at the speed of 100rpm, and cultured for 9 days;
wherein, the inoculation of the ferrous oxide micro-helicobacter comprises the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ) 2 SO 4 0.15g/L、KCl 0.15g/L、K 2 HPO 4 0.15g/L、MgSO 4 .7H 2 O 1.5g/L、Ca(NO 3 ) 2 0.03g/L、FeSO 4 .7H 2 O1 g/L, dropwise adding sulfuric acid solution to adjust the pH of the culture medium to 1.5, placing the culture medium in an incubator at 28-32 ℃ for culturing for 36h;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is 3:6 in parts by weight, 0.005 part of egg white is additionally added into the culture barrel, after mixing, sulfuric acid solution is dropwise added into the culture barrel until the pH value in the culture barrel is 1, and the ferrous oxide micro-screw bacteria cultured in the step a are inoculated into the culture barrel for 5 days;
c. b, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into a leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30 parts of high-concentration sulfuric acid solution with the concentration of 450g/L, stirring at the speed of 150rpm, performing heap leaching for 20 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 6 parts of zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 6.0, filtering the filtrate again to remove iron, and entering the next working procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction stage number is 8, and the ratio of O/A is 4:6, the extraction end point is that the pH is reduced to 1;
wherein the extractant is a mixture of 20% of p204 and 80% of No. 6 industrial light solvent;
s5, back extraction is carried out by using sulfuric acid solution containing 250g/L sulfuric acid, wherein the mixing time is 15min compared with O/A which is 1.5:4;
s7, slowly dripping sulfuric acid solution containing 0.1mol/L zinc phosphate into the back extraction solution until no sediment is generated in the back extraction solution, and dripping 5mL/m into the back extraction solution 3 Iron sulfate solution with concentration of 3 mmol/L;
s8, adding active carbon particles into the back extraction liquid, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
during electrodeposition, a rectification variable-high-voltage cabinet is used, lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell; the current intensity is 8000-12000A, the current density is 250-300A/m3, the cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the product is stripped after 18-36h of electrolysis;
s9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
Zinc ingots of examples 1 to 4 and comparative examples 1 to 2 were tested according to GB/T470-2008, and the results are shown in the following table:
by comparing examples 1-3 with comparative example 1, it is found that the leaching rate of zinc element is remarkably improved and is increased with time by treating zinc-containing waste by ferrous oxide micro-screw bacteria;
by comparison of example 1, example 4 and comparative example 2, it was found that the content of impurity elements in the zinc ingot was reduced after ozone treatment, and the change in the content of impurity iron element was most prominent among them.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The processing technology for preparing the zinc ingot by the electrodeposition method is characterized by comprising the following steps of:
s1, adding 10-30 parts by weight of zinc-containing waste into a leaching tank, adding 40-60 parts by weight of sulfuric acid solution with the concentration of 16-28g/L, stirring and mixing, inoculating ferrous oxide micro-helicobacter, heating the leaching tank to 28-35 ℃, stirring at the speed of 100-150rpm, and culturing for 9-20 days;
wherein, the zinc-containing waste comprises 2-4 parts of low-quality zinc oxide, 4-8 parts of zinc ash and 4-8 parts of steel ash by weight, and the zinc-containing waste is subjected to ultrasonic oscillation treatment with the frequency of 30-45KHz for 1-3h;
s2, transferring the mixture in the leaching tank into a filter press for filter pressing to obtain filtrate 1, transferring the filter residue into another leaching tank, adding 30-40 parts of sulfuric acid solution with the concentration of 250-450g/L, stirring at the speed of 100-150rpm, performing heap leaching for 20-45 days, and then performing filter pressing again to obtain filtrate 2, and transferring the filtrate 2 into the next process;
s3, slowly adding 1% -10% zinc hydroxide into the filtrate obtained in the step S2 for multiple times, adding calcium hydroxide to adjust the pH of the filtrate to 5.5-6.5, filtering the filtrate again to remove iron, and entering the next procedure;
s4, extracting the filtrate by using an extracting agent at room temperature, wherein the extraction level is 5-8, and compared with O/A, the extraction level is 4:6, the extraction end point is that the pH is reduced to 1-1.5;
s5, back extraction is carried out by using sulfuric acid solution containing 170-250g/L sulfuric acid, and the mixing time is 10-15min compared with O/A which is 1-1.5:4-8;
s6, introducing ozone into the strip liquor for aeration for 15-30min, wherein the aeration mode is microporous aeration, and the aeration flow is 5-6L/m 3 After aeration is finished, heating the strip liquor to 60-70 ℃, preserving heat for 30min, and removing unreacted ozone in the strip liquor;
s7, cooling the stripping solution to room temperature, slowly dripping a sulfuric acid solution containing 0.1-0.5mol/L zinc phosphate into the stripping solution until no sediment is generated in the stripping solution, and dripping 3-5mL/m into the stripping solution 3 Ferric sulfate solution with the concentration of 0.1-3 mmol/L;
s8, adding active carbon particles into the strip liquor, uniformly stirring, standing for 12 hours, filtering, and pouring filtrate into an electrodeposition tank for electrodeposition;
and S9, casting the product obtained after electrodeposition to obtain a zinc ingot finished product.
2. The process for preparing zinc ingots by the electrodeposition method as claimed in claim 1, wherein the process comprises the following steps: the particle size of the low-quality zinc oxide is 30-60 mu m.
3. The process for preparing zinc ingots by the electrodeposition method as claimed in claim 1, wherein the process comprises the following steps: in the step S1, inoculating ferrous oxide micro-helicobacter, comprising the following steps:
a. inoculating ferrous oxide micro-screw bacteria into culture medium, and culturing to obtain culture medium containing (NH) 4 ） 2 SO 4 0.05-0.15g/L、KCl 0.05-0.15g/L、K 2 HPO 4 0.05-0.15g/L、MgSO 4 .7H 2 O 0.5-1.5g/L、Ca（NO 3 ） 2 0.01-0.03g/L、FeSO 4 .7H 2 O0.1-1 g/L, adding sulfuric acid solution dropwise to adjust pH of the culture medium to 1.5-2, placing in an incubator at 28-32deg.C, and culturing for 36-48 hr;
b. inoculating the cultured ferrous oxide micro-screw bacteria into a culture barrel for expansion culture, wherein the culture barrel contains zinc-containing waste leaching solution and culture medium culture solution, and the ratio of the zinc-containing waste leaching solution to the culture medium culture solution is (3) according to parts by weight: (4-7), adding 0.001-0.005 part of egg white into the culture barrel, after mixing, dropwise adding sulfuric acid solution into the culture barrel until the pH value in the culture barrel is 1.5-2.5, inoculating the ferrous oxide micro-screw bacteria cultured in the step a into the culture barrel, and culturing for 3-5 days;
c. and d, adding the ferrous oxide micro-helicobacter bacteria cultured in the step b into the leaching tank, wherein the inoculation amount is 1/3 of the amount of sulfuric acid solution added into the leaching tank.
4. The process for preparing zinc ingots by the electrodeposition method as claimed in claim 1, wherein the process comprises the following steps: in the step S4, the extract is a mixture of p204 extractant and No. 6 industrial light solvent, wherein the mixing proportion of the p204 extractant is 20%, and the mixing proportion of the No. 6 industrial light solvent is 80%.
5. The process for preparing zinc ingots by the electrodeposition method as claimed in claim 1, wherein the process comprises the following steps: in the step S8, during the electrodeposition, a rectifying transformer is used, a lead-silver alloy is used as an anode of the electrodeposition cell, and a rolled aluminum plate is used as a cathode of the electrodeposition cell.
6. The process for preparing zinc ingots by the electrodeposition method as claimed in claim 1, wherein the process comprises the following steps: in the step S8, the current intensity during electrodeposition is 8000-12000A, and the current density is 250-300A/m 3 The cell voltage is 0.2-0.4V, the electrolyte temperature is 60-70 ℃, the electrolyte circulation flow is 34-40L/min, and the zinc ingot is obtained after electrolysis for 18-36 h.
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