CN113604678A - Method for recovering zinc in tin smelting smoke dust through ammonia leaching-extraction process - Google Patents
Method for recovering zinc in tin smelting smoke dust through ammonia leaching-extraction process Download PDFInfo
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- CN113604678A CN113604678A CN202110942622.6A CN202110942622A CN113604678A CN 113604678 A CN113604678 A CN 113604678A CN 202110942622 A CN202110942622 A CN 202110942622A CN 113604678 A CN113604678 A CN 113604678A
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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
- C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
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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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- 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
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
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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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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 method for recovering zinc in tin smelting smoke dust by an ammonia leaching-extraction process, which adopts ammonia-ammonium mixed solution as leaching solution, and performs liquid-solid separation after leaching for a certain time under the condition of a certain temperature according to a certain liquid-solid ratio; washing the obtained slag to be used as a raw material for smelting tin, adding zinc powder into the leaching solution to replace and remove cadmium, extracting the leaching solution again, returning to leaching, and performing back extraction on the extracted organic phase by using dilute sulfuric acid solution to be continuously used as an extraction phase for recycling; and finally, electrolyzing the zinc sulfate solution after the back extraction and enrichment to recover cathode zinc, and electrodepositing the electrolyte to recover zinc, wherein the zinc can be used as a back extraction solution. The invention provides a method for recovering zinc from tin smelting smoke through an ammonia leaching-extraction process, which realizes the recovery of valuable metal zinc while removing harmful element zinc in the tin smelting smoke, and realizes the purpose of recovering zinc from the tin smelting smoke.
Description
Technical Field
The invention relates to the technical field of recovering valuable metals in tin smelting smoke dust by using a wet process, in particular to a method for recovering zinc in tin smelting smoke dust by using an ammonia leaching-extraction process.
Background
With the gradual consumption of tin resources of large-scale tin mines, the relatively large amount of tin ore raw materials with fixed types are gradually reduced, in recent years, the types of tin-containing materials in large-scale tin smelting plants are more and more complex, and particularly, after the proportion of various types of tin secondary raw materials in the tin smelting plants is gradually increased, one or more metal impurities which are not common in the traditional tin smelting field are circularly enriched in a tin smelting process. In order to reduce the influence of the impurity metals on the yield, quality and production efficiency of products in each production section of a tin smelting plant, and based on the principle of comprehensively recovering valuable metals and improving smelting benefits, a process for circularly enriching the impurity metals in the tin smelting process by removing and recovering is urgently needed to be additionally arranged in the tin smelting plant.
In the tin smelting process, tin smoke dust recovered from the flue gas in the smelting process is generally used as a returned product for granulation or humidification to be directly returned to a smelting furnace for smelting due to high tin content (Sn is more than or equal to 30 percent), so that the phenomenon of cyclic enrichment of low-melting-point metal impurities is easily caused in the process. After crude tin smelting production in a certain large tin smelting plant for a period of time, the phenomenon of gradual enrichment of zinc appears in smelting smoke dust, the zinc content of the smoke dust is generally 8-15 wt.%, the phenomena that a flue of a smelting furnace is easy to form nodules and block and the smoke dust in a smoke dust bin is easy to form agglomerates and is difficult to clean are caused, and smelting energy consumption is increased, so that smelting production efficiency is influenced. In addition, the smelting plant generates smoke dust rich in zinc and also generates enrichment of cadmium and chlorine, and the cadmium content is generally 1.5-5 wt%, and the chlorine content is generally 6-12 wt%. The influence of cadmium on tin smelting is similar to that of zinc, and chlorine can corrode smelting equipment, reduce the direct yield of tin smelting and damage the normal operation of a low-concentration sulfur dioxide acid making system in a tail gas treatment part in a smelting process. After phase analysis of tin smelting dust containing harmful impurities of zinc, cadmium and chlorine, zinc exists mostly as oxide, a small amount of zinc exists as chloride, cadmium exists mostly as chloride, and tin is basically oxide. Because most of cadmium in the smoke exists in a chloride state, the smoke is treated by a wet process to recover zinc, and the aim of simultaneously removing cadmium and chlorine can be fulfilled.
In the smelting industry, zinc enriched in smoke dust is generally recovered by adopting a wet leaching method, and a sulfuric acid leaching method is more common, for example, a sulfuric acid leaching-purifying-electrodeposition method is adopted in a lead smelting plant to recover the zinc. However, this method is not suitable for treating low-zinc flue dust (containing about 10% of Zn), and in the case of high content of elements harmful to zinc recovery, such as Fe, As, Cl, etc. Because the low-zinc smoke is treated by a sulfuric acid leaching mode, the concentration of zinc ions in the leaching solution is low, enrichment is difficult, and a large amount of harmful impurity elements such as iron, arsenic, chlorine and the like are introduced into the leaching solution, so that the zinc recovery from the purified solution is very difficult. The zinc content and impurity characteristics of the zinc-containing tin smoke dust produced by tin smelting belong to the situation that the common sulfuric acid is not suitable for direct leaching and recovery, so a new process route for recovering zinc from the tin smelting smoke dust with low zinc content and high impurity content needs to be found.
The invention provides a method for recovering zinc in tin smelting smoke dust through an ammonia leaching-extraction process. The problem that impurity zinc in the smelting smoke dust is circularly enriched in the smelting smoke dust to have adverse effect on the smelting process of tin is solved, and the problem that zinc is more effectively recovered is urgently needed to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides a method for recovering zinc from tin smelting smoke through an ammonia leaching-extraction process based on the harm of zinc enrichment in tin smelting smoke to a tin smelting production process, so that while harmful elements zinc in tin smelting smoke is removed, valuable metal zinc is recovered, and the purpose of recovering zinc from tin smelting smoke is achieved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for recovering zinc in tin smelting smoke dust through an ammonia leaching-extraction process comprises the following specific steps:
s1, preparing a mixed solution of ammonia water and ammonium chloride as a leachate of zinc-tin-containing smelting smoke dust, wherein the concentration of the ammonia water is 2-6mol/L, the concentration of the ammonium chloride is 2-6mol/L, and the mixed solution is stirred and leached for 1.5-3h at the temperature of 30-50 ℃ according to the liquid-solid ratio of 4-6: 1;
s2, performing liquid-solid separation on the leached slurry in a plate-and-frame filter pressing mode, washing filter residues to obtain dezincification tin smoke dust serving as a tin smelting raw material to return to a tin smelting working section, wherein the liquid-solid ratio of the filter residues in washing is 3:1, the washing liquid is repeatedly used for 5-10 times, and the obtained repeatedly used washing liquid is used as a supplement liquid for the leaching liquid of the zinc-containing tin smelting smoke dust;
s3, adding zinc powder to the filtrate after solid-liquid separation according to the cadmium concentration for removing cadmium by replacement, wherein the zinc powder: the molar ratio of cadmium is 1.05-1.1: 1, mixing P204 and kerosene in a volume ratio of 3:7 to obtain an organic phase as an extracting agent, setting the volume ratio of the organic phase to a filtrate obtained after cadmium removal to be 1:1, setting the temperature to be 30-45 ℃ in the extraction process, setting the time to be 0.5-1h, then carrying out three-stage countercurrent extraction and back extraction, using 120-doped 220g/L dilute sulfuric acid solution as a back extraction solution, setting the volume ratio of the organic phase to the back extraction solution to be 1-2:1, setting the temperature to be 30-45 ℃ and the time to be 0.5-1h, continuously and circularly back extracting the zinc-loaded organic phase by the back extraction solution for 3-5 times, and sending the zinc sulfate solution after back extraction and enrichment to an electrolysis section for electrodeposition to recover cathode zinc.
Preferably, the ammonium salt added to the leachate is one of ammonium chloride, ammonium sulfate, ammonium bicarbonate and ammonium carbonate.
By adopting the preferable scheme, the invention has the beneficial effects that:
1. by adopting the ammonia-ammonium mixed solution as the leaching solution, the combination mode can continuously add ammonia water into the solution under the condition that the ammonium salt is basically saturated, thereby further improving the total ammonia amount (NH) in the solution3+NH4 +) Make the reaction more favorable to the formation of zinc ammonia complex [ Zn (NH)3)n]2+The direction of the zinc leaching tank is changed to accelerate the zinc leaching speed and improve the zinc leaching rate. Tests show that under the condition of a certain liquid-solid ratio, when the total ammonia amount (molar weight) in the solution is 5-10 times of the total zinc amount (molar weight) in the smoke dust participating in the reaction, the leaching rate of zinc in the tin smelting smoke dust can be maintained within the range of 80% -90%. The leaching solution can selectively leach zinc and a small amount of cadmium, and tin and other impurities such as lead, iron, arsenic and the like are basically not leached, and tests show that the contents of tin and arsenic in the leaching solution are less than 0.1g/L, and the contents of lead and iron are both less than 0.01g/L, so that tin can be basically and completely recovered in leaching residues, and a relatively pure zinc leaching solution is obtained.
2. The zinc powder is added into the ammonia leaching solution for replacement and impurity removal, and compared with the process of purification and impurity removal after back extraction, the impurity removal process can be simplified, because the back extraction solution is dilute sulfuric acid, and neutralization treatment is required in advance if replacement and impurity removal are carried out in the dilute sulfuric acid solution.
3. The invention removes most cadmium and chlorine harmful to the tin smelting process while removing zinc in the tin smelting smoke dust, so that the smoke dust is returned to the smelting process after being treated and is easier to treat.
4. The leachate can be returned to be continuously used as leachate after being extracted, the leaching residue washing liquor can also be used as leachate replenishing liquor after being washed for many times, the electrolyte can be used as back extraction liquor after being electrodeposited with zinc, and the extraction organic phase is recycled.
5. The extraction method can effectively enrich zinc in the zinc-containing leachate with low concentration, so that the zinc obtained by leaching can be recovered more easily in a metal zinc product mode with higher value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram showing a detailed process of example 1 of the present invention;
FIG. 2 is a drawing showing the connection of an apparatus according to embodiment 1 of the present invention;
in the figure: 1-leaching tank, 2-corrosion-resistant pump for pumping leaching slurry, 3-plate-and-frame filter press for leaching slurry solid separation, 4-slag washing tank, 5-corrosion-resistant pump for pumping slag washing slurry, 6-plate-and-frame filter press for washing slurry solid separation, 7-replacement tank, 8-plate-and-frame filter press for separating replacement slag, 9-plate-and-frame filter press for pumping replaced slag-liquid mixture, 10-extraction and back-extraction tank, and 11-electrolytic tank for recovering zinc by electrodeposition.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the embodiment 1 of the invention discloses a method for recovering zinc in tin smelting smoke dust by an ammonia leaching-extraction process, which adopts the following technical scheme:
the treatment 300t composition was high zinc tin soot with Sn 41.80 wt.%, Zn 8.97 wt.%, As 2.08 wt.%, Cd 3.30 wt.%, Cl 10.21 wt.%.
First, NH is prepared3·H2O and NH4And leaching the leachate with the Cl concentration of 5mol/L for 2 hours under the conditions of liquid-solid ratio of 6:1, leaching temperature of 35 ℃ and stirring. Pumping the leached slag into a plate-and-frame filter press for liquid-solid separation after leaching is finished, washing the leached slag according to the liquid-solid ratio of 3:1, pumping the washed leached slag into the plate-and-frame filter press for liquid-solid separation, finally obtaining the impurity-removed tin smoke dust returned to the tin smelting section, and repeatedly washing the washing liquid for 8 times to serve as a leachate replenishing liquid; the obtained leachate contains 10.2g/L of Zn and 2.8g/L of Cd, the leaching rate of Zn reaches 81%, zinc powder with the cadmium content of 1.1 times is added into the leachate for displacement and cadmium removal, an organic phase with the volume ratio of P204 to kerosene of 3:7 is used as an extracting agent, and zinc is extracted by adopting a three-stage countercurrent extraction mode under the conditions that the volume ratio of the organic phase to a solution phase is 1:1.2, the temperature is 40 ℃ and the time is 0.6 h; the back extraction uses a dilute sulphuric acid solution with the concentration of 150g/L as a back extraction solution, the volume ratio of an organic phase to a solution phase of the back extraction is 1:1, the reaction time is 0.5h, the temperature is 30 ℃, the back extraction solution continuously and circularly back extracts the zinc-loaded organic phase for 5 times, and finally zinc sulfate solution containing 52g/L Zn is obtained; and then the zinc sulfate solution is sent to an electrolytic zinc working section for treatment, zinc is finally recovered in a cathode zinc product mode, 20t of product zinc is produced, and the residual electrolytic zinc waste liquid is used for treating the zinc-tin-containing smoke back extraction liquid of the next batch.
Example 2:
the embodiment 2 of the invention discloses a method for recovering zinc in tin smelting smoke dust by an ammonia leaching-extraction process, which adopts the following technical scheme:
the treatment 500t composition was high zinc tin soot with Sn 40.69 wt.%, Zn 9.36 wt.%, As 1.27 wt.%, Cd 3.50 wt.%, Cl 9.37 wt.%.
First, NH is contained3·H2O4 mol/L, containing NH4And leaching the leachate with the Cl concentration of 6mol/L for 2 hours under the conditions of liquid-solid ratio of 6:1, leaching temperature of 45 ℃ and stirring. Pumping the leached residue into a plate-and-frame filter press for liquid-solid separation after leaching is finished, washing the leached residue according to the liquid-solid ratio of 3:1, pumping the leached residue into the plate-and-frame filter press for liquid-solid separation after washing, and finally obtaining the impurity-removed tinReturning the smoke dust to a tin smelting working section, and repeatedly washing the washing liquid for 6 times to serve as a leachate replenishing liquid; the obtained leachate contains 11.5g/L of Zn and 3.6g/L of Cd, the leaching rate of Zn reaches 83%, zinc powder with the cadmium content of 1.1 times is added into the leachate for displacement and cadmium removal, an organic phase with the volume ratio of P204 to kerosene of 3:7 is used as an extracting agent, and zinc is extracted by adopting a three-stage countercurrent extraction mode under the conditions that the volume ratio of the organic phase to the solution phase is 1:1, the temperature is 40 ℃ and the time is 1 h; the back extraction uses a dilute sulfuric acid solution with the concentration of 120g/L as a back extraction solution, the volume ratio of an organic phase to a solution phase of the back extraction is 1.5:1, the reaction time is 1h, the temperature is 40 ℃, the back extraction solution continuously and circularly back extracts the zinc-loaded organic phase for 4 times, and finally zinc sulfate solution containing 58g/L Zn is obtained; and then the zinc sulfate solution is sent to an electrolytic zinc working section for treatment, zinc is finally recovered in a cathode zinc product mode, 40t of product zinc is produced, and the residual electrolytic zinc waste liquid is used for treating the zinc-tin-containing smoke back extraction liquid of the next batch.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (2)
1. A method for recovering zinc in tin smelting smoke dust through an ammonia leaching-extraction process is characterized by comprising the following specific steps:
s1, preparing a mixed solution of ammonia water and ammonium chloride as a leachate of zinc-tin-containing smelting smoke dust, wherein the concentration of the ammonia water is 2-6mol/L, the concentration of the ammonium chloride is 2-6mol/L, and the mixed solution is stirred and leached for 1.5-3h at the temperature of 30-50 ℃ according to the liquid-solid ratio of 4-6: 1;
s2, performing liquid-solid separation on the leached slurry in a plate-and-frame filter pressing mode, washing filter residues to obtain dezincification tin smoke dust serving as a tin smelting raw material to return to a tin smelting working section, wherein the liquid-solid ratio of the filter residues in washing is 3:1, the washing liquid is repeatedly used for 5-10 times, and the obtained repeatedly used washing liquid is used as a supplement liquid for the leaching liquid of the zinc-containing tin smelting smoke dust;
s3, adding zinc powder to the filtrate after solid-liquid separation according to the cadmium concentration for removing cadmium by replacement, wherein the zinc powder: the molar ratio of cadmium is 1.05-1.1: 1, mixing P204 and kerosene in a volume ratio of 3:7 to obtain an organic phase as an extracting agent, setting the volume ratio of the organic phase to a filtrate obtained after cadmium removal to be 1:1, setting the temperature to be 30-45 ℃ in the extraction process, setting the time to be 0.5-1h, then carrying out three-stage countercurrent extraction and back extraction, using 120-doped 220g/L dilute sulfuric acid solution as a back extraction solution, setting the volume ratio of the organic phase to the back extraction solution to be 1-2:1, setting the temperature to be 30-45 ℃ and the time to be 0.5-1h, continuously and circularly back extracting the zinc-loaded organic phase by the back extraction solution for 3-5 times, and sending the zinc sulfate solution after back extraction and enrichment to an electrolysis section for electrodeposition to recover cathode zinc.
2. The method for recovering zinc from tin smelting fumes through ammonia leaching-extraction process according to claim 1, wherein the added ammonium salt in the leaching solution is one of ammonium chloride, ammonium sulfate, ammonium bicarbonate and ammonium carbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112663090A (en) * | 2020-12-10 | 2021-04-16 | 广东臻鼎环境科技有限公司 | Method for recovering copper from copper-containing tin mud |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112663090A (en) * | 2020-12-10 | 2021-04-16 | 广东臻鼎环境科技有限公司 | Method for recovering copper from copper-containing tin mud |
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