CN113122735B - Alkali-process zinc powder combined smelting method - Google Patents
Alkali-process zinc powder combined smelting method Download PDFInfo
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- CN113122735B CN113122735B CN202110364546.5A CN202110364546A CN113122735B CN 113122735 B CN113122735 B CN 113122735B CN 202110364546 A CN202110364546 A CN 202110364546A CN 113122735 B CN113122735 B CN 113122735B
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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
- C22B19/20—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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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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 discloses an alkaline zinc powder combined smelting method, which comprises the following steps: the method comprises the following steps of zinc precipitation, filtering, alkaline leaching, electrolysis, washing, size mixing and purification, wherein the stock solution before zinc precipitation in the zinc precipitation is the new electrolysis solution in the zinc hydrometallurgy process. The invention provides an alkaline zinc powder combined smelting method, which adopts an alkaline zinc powder preparation and wet purification combined smelting mode and simultaneously utilizes a zinc powder wet adding technology, thereby solving the problems of high equipment price, high cost and high energy consumption in the existing alkaline zinc powder drying process and the problem of severe operation environment in the zinc powder transporting process; meanwhile, the problems that the alkaline leaching raw material of the alkaline zinc powder is unstable in grade, high in impurity content and needs to be added with a purification process to remove impurities are solved. The combined smelting method provided by the invention has the characteristics of low use cost, good effect and excellent operation environment, and meets the requirements of low carbon, green and environmental protection.
Description
Technical Field
The invention relates to the field of zinc smelting, in particular to an alkaline zinc powder combined smelting method.
Background
In the production process of the alkaline zinc powder, the electrolyzed alkaline zinc powder has high activity, after vacuum filtration and washing, the wet alkaline zinc powder is placed in a drying cabin of a double-cone rotary dryer for drying, after the drying cabin is closed, a vacuum pump is started for pumping vacuum, after a certain vacuum degree is reached, a heating device is started, the drying is carried out for 1-2h at the temperature lower than 60-80 ℃, and the produced alkaline zinc powder is crushed, screened, weighed and packaged for sale. In the traditional zinc hydrometallurgy process, metal zinc powder and electric furnace zinc powder are used for removing impurities such as copper, cadmium, cobalt, antimony and the like in a purification process, and the alkaline zinc powder has the characteristics of large specific surface area and high activity and can completely replace the metal zinc powder and the electric furnace zinc powder. However, the alkaline zinc powder drying process has the problems of high equipment price, high cost, high energy consumption and severe working environment in the zinc powder transporting process.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an alkali-method zinc powder combined smelting method, and aims to solve the problems of high equipment price, high cost and high energy consumption in the existing alkali-method zinc powder drying process and the problem of severe working environment in the zinc powder transporting process.
The technical scheme of the invention is as follows:
an alkaline zinc powder combined smelting method comprises the following steps:
and (3) zinc precipitation: taking the new electrolytic solution in the zinc hydrometallurgy process as a zinc deposition stock solution, and adding an alkaline material into the zinc deposition stock solution to perform zinc deposition reaction to obtain a zinc deposition solution containing zinc deposition residues;
a filtering process: filtering the zinc precipitation solution containing the zinc precipitation slag to obtain zinc precipitation slag;
an alkaline leaching process: dissolving the zinc precipitation slag in an alkali solution to carry out an alkali leaching reaction to obtain an alkali leaching solution;
an electrolysis process: electrolyzing the alkaline leaching solution to obtain an alkaline zinc powder solution;
a washing procedure: filtering and washing the alkaline zinc powder solution to obtain alkaline zinc powder;
a size mixing procedure: mixing the alkaline zinc powder with water for size mixing to obtain zinc powder size;
a purification process: and purifying the supernatant in the wet zinc smelting process by using the zinc powder slurry to obtain the new electrolytic solution in the wet zinc smelting process.
Optionally, in the zinc precipitating process, the PH value of the zinc precipitating solution at the reaction end point of the zinc precipitating reaction is 5.5 to 7, and the reaction time is 15 to 45min.
Optionally, in the zinc precipitation process, the alkaline material is selected from one or more of calcium oxide, sodium hydroxide and potassium hydroxide.
Optionally, in the filtering process, the filtering equipment used for filtering is selected from one or more of a vertical plate and frame filter, a ceramic filter, a box-type membrane filter and a centrifugal filter.
Optionally, in the alkaline leaching step, the ratio of liquid to solid is 6-10:1, dissolving the zinc precipitation slag in an alkali solution with the initial concentration of 4-6mol/L for alkali leaching reaction, wherein the liquid-solid ratio is as follows in mL: and g, calculating.
Optionally, the reaction temperature of the alkaline leaching reaction is 50-90 ℃, and the reaction time is 1-2h.
Optionally, in the electrolysis process, the electrolysis temperature is 20-45 ℃ and the time is less than 5h.
Optionally, in the washing procedure, the alkaline zinc powder solution is filtered and washed for 3-5 times by a filter, so that the pH of the washing water in the last washing is less than or equal to 8.
Optionally, in the size mixing process, the mass content of zinc powder in the zinc powder size is 10% to 20%.
Optionally, in the purification step, after the zinc powder slurry is added to the supernatant, sulfuric acid is added to adjust the PH of the supernatant to be less than or equal to 5.3.
Has the beneficial effects that: the invention provides an alkaline zinc powder combined smelting method, which adopts an alkaline zinc powder preparation and wet purification combined smelting mode and simultaneously utilizes a zinc powder wet processing technology to solve the problems of high equipment price, high cost and high energy consumption in the existing alkaline zinc powder drying process and the problem of severe operation environment in the zinc powder transporting process.
Drawings
FIG. 1 is a process flow chart of an alkaline zinc powder combined smelting method.
Detailed Description
The invention provides an alkali-process zinc powder combined smelting method, which is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The embodiment of the invention provides an alkali-process zinc powder combined smelting method, which comprises the following steps:
and (3) zinc precipitation: taking the new electrolytic solution in the zinc hydrometallurgy process as a zinc deposition stock solution, and adding an alkaline material into the zinc deposition stock solution to perform zinc deposition reaction to obtain a zinc deposition solution containing zinc deposition residues;
a filtering process: filtering the zinc precipitation solution containing the zinc precipitation slag to obtain zinc precipitation slag;
an alkaline leaching process: dissolving the zinc precipitation slag in an alkali solution to carry out an alkali leaching reaction to obtain an alkali leaching solution;
an electrolysis process: electrolyzing the alkaline leaching solution to obtain an alkaline zinc powder solution;
a washing procedure: filtering and washing the alkaline zinc powder solution to obtain alkaline zinc powder;
and (3) size mixing procedure: mixing the alkaline zinc powder with water for size mixing to obtain zinc powder size;
a purification process: and purifying the supernatant in the wet zinc smelting process by using the zinc powder slurry to obtain the new electrolytic solution in the wet zinc smelting process.
In the embodiment, a zinc powder wet adding technology is simultaneously utilized by adopting a combined smelting mode of alkaline zinc powder preparation and wet purification, the preparation characteristics of alkaline zinc powder and the advantages of the zinc powder wet adding technology are combined, the problems of high equipment price, high cost and high energy consumption in the existing alkaline zinc powder drying process are solved, and the problems that the source of the alkaline zinc powder raw material is unstable and the purification process needs to be added are solved. The alkaline leaching is adopted to precipitate the zinc slag, the alkaline leaching solution has high quality, the alkaline electrolysis can be started without purification, the zinc powder wet-adding technology is adopted, the optimization of the alkaline drying process is realized, the alkaline leaching solution is directly used in the production practice process, the operation environment is further optimized, the problem of zinc powder flying is solved, the treatment process is environment-friendly, and the environment-friendly effect is realized.
In this embodiment, the zinc precipitation stock solution, that is, the new electrolytic solution in the zinc hydrometallurgy process, is obtained through the purification process, and the zinc precipitation reaction can be performed only when the requirement that the temperature is 40 to 50 ℃ and the pH =4.0 to 5.0 is satisfied.
In the embodiment of the invention, in the zinc precipitation process, the alkaline material is used for regulating and controlling the pH value of the zinc-containing solution, when the pH value of the zinc-containing solution reaches 7, zinc ions in the solution can undergo a zinc precipitation reaction to obtain a precipitate, and the precipitate is a zinc hydroxide precipitate and a basic zinc sulfate precipitate. Therefore, the zinc precipitation slag is zinc hydroxide precipitation and basic zinc sulfate precipitation.
In one embodiment, the PH of the zinc precipitating solution at the end of the zinc precipitating reaction is 5.5 to 7, and the reaction time is 15 to 45min.
The end point of the zinc deposition reaction is controlled by the PH value, the sensitivity is higher, namely when the PH value of the solution of the zinc deposition reaction reaches 5.5-7, the zinc deposition reaction is finished.
In the zinc deposition step, in one embodiment, the alkaline material is selected from one or more of calcium oxide, sodium hydroxide and potassium hydroxide, but not limited thereto.
In the filtering process, in an embodiment, the filtering device used for filtering is one or more selected from a vertical plate and frame filter, a ceramic filter, a box type membrane filter, and a centrifugal filter, but is not limited thereto.
In the embodiment of the present invention, in the alkaline leaching step, the zinc precipitation slag (zinc hydroxide precipitation and basic zinc sulfate precipitation) is dissolved in an alkaline solution to obtain an alkaline leaching solution containing zinc ions.
In the alkaline leaching process, in one embodiment, the ratio of liquid to solid is 6-10:1, dissolving the zinc precipitation slag in an alkali solution with the initial concentration of 4-6mol/L for alkali leaching reaction, wherein the liquid-solid ratio is as follows in mL: and g, calculating.
Specifically, for example, 1000g of zinc precipitation slag is dissolved in 6000mL of alkali solution with the concentration of 4-6mol/L, and the liquid-solid ratio is 6:1.
in one embodiment, the alkali solution is a sodium hydroxide solution or a potassium hydroxide solution.
And when the alkali solution is a sodium hydroxide solution, dissolving zinc precipitation slag in the sodium hydroxide solution to generate sodium tetrahydroxy zincate, and dissolving the sodium tetrahydroxy zincate in the solution to obtain an alkaline leaching solution containing zinc ions. And when the alkali solution is a potassium hydroxide solution, dissolving zinc precipitation slag in the alkali solution to generate potassium tetrahydroxy zincate, and dissolving the potassium tetrahydroxy zincate in the alkali solution to obtain an alkali leaching solution containing zinc ions.
In one embodiment, the alkaline leaching reaction is carried out at a temperature of 50-90 ℃ for 1-2h.
The alkaline leaching process of alkaline zinc powder strictly controls the liquid-solid ratio and the reaction temperature, and ensures the leaching rate of the zinc-containing raw material.
In the embodiment of the present invention, in the electrolysis step, an alkaline leaching solution containing zinc ions is electrolyzed to obtain an alkaline zinc powder solution.
In one embodiment, the electrolysis process is carried out at a temperature of 20-45 ℃ for less than 5h.
In the washing procedure, in one embodiment, the alkaline zinc powder solution is filtered and washed for 3-5 times by a filter, so that the pH of the washing water in the last washing is less than or equal to 8, and the alkaline zinc powder is obtained. The obtained alkaline zinc powder has small particles, large specific surface area and high activity, and can replace metal zinc powder and electric furnace zinc powder for purification.
In one embodiment, the filter is a centrifugal filter.
In one embodiment, in the kneading step, the water used in kneading the alkaline zinc powder and water is industrial water.
In one embodiment, the zinc powder slurry has a zinc powder content of 10% to 20% by weight, which is convenient to add using a metering pump and reduces problems of clogging of piping and agglomeration of the zinc powder during the size mixing process.
In one embodiment of the purification process, after the zinc powder slurry is added to the supernatant, sulfuric acid is added to adjust the PH of the supernatant to be less than or equal to 5.3. After the zinc powder slurry is added into the supernatant, the pH fluctuation of the purification process can be caused, and the pH of the supernatant needs to be adjusted to be less than or equal to 5.3 by using sulfuric acid.
In the purification process, impurities such as copper, cadmium, cobalt, antimony and the like in the solution are removed by utilizing alkaline zinc powder replacement, the impurities such as copper, cadmium, cobalt, antimony and the like are precipitated in a precipitation mode, and zinc exists in the solution in the form of zinc ions. If the PH is too high, zinc ions can precipitate, so that waste of zinc powder is caused, and the cost for recovering and separating impurities is increased, so that the PH of the supernatant needs to be adjusted to be less than or equal to 5.3 by using sulfuric acid.
The alkali zinc powder combined smelting process of the invention is specifically described with reference to fig. 1. And (4) allowing the supernatant from the zinc hydrometallurgy process to enter a purification process to obtain purified slag and new electrolytic solution. And comprehensively treating the purification slag, and using part of the new electrolytic solution for acidic electrolysis to obtain the zinc sheets. And the other part of the zinc solution enters a zinc precipitation process for zinc precipitation reaction to obtain a zinc precipitation solution, wherein the zinc precipitation solution contains zinc precipitation slag. And (4) the zinc precipitation solution enters a filtering process, and is filtered to obtain a solution after zinc precipitation and zinc precipitation slag. And the liquid after zinc precipitation returns to the middle leaching process in the zinc hydrometallurgy process again, the zinc precipitation slag enters the alkaline leaching process, and alkaline leaching reaction is carried out to obtain alkaline leaching solution, wherein the alkaline leaching solution contains zinc ions. And the alkaline leaching solution enters an electrolysis process to carry out electrolysis reaction, so as to obtain the alkaline zinc powder solution. And (3) the alkaline zinc powder solution enters a washing process, and is filtered and washed to obtain washing water and alkaline zinc powder. And recycling the washing water, and allowing the alkaline zinc powder to enter a size mixing process for size mixing to obtain zinc powder size. And returning the zinc powder slurry to the purification process, and carrying out purification reaction to remove impurities in the supernatant in the zinc hydrometallurgy process to obtain new electrolytic solution in the zinc hydrometallurgy process.
The invention is further illustrated by the following specific examples.
Example 1
A certain smelter adopts a hydrometallurgy method and a three-stage reverse antimony purification method to realize deep purification.
The analysis of the new electrolyte is shown in the following table, wherein the unit of Zn is g/L,
| Zn | Fe | Sb | Cd | Co | Ge | pH | |
| liquid 1 | 139.62 | 6.28 | 0.003 | 0.03 | 0.10 | 0.006 | 4.95 |
Adding a proper amount of caustic soda flakes into 3L of new electrolytic solution to obtain a zinc precipitation solution with the pH =7, filtering to obtain zinc precipitation residues, putting the zinc precipitation residues into a NaOH solution with the initial concentration of 6mol/L according to the liquid-solid ratio of 8. The purification results are shown below in mg/L, where Zn is in g/L.
| Zn | Fe | Sb | Cd | Co | Ge | pH | |
| 10％ | 138.72 | 4.75 | 0.003 | 0.03 | 0.10 | 0.006 | 4.97 |
| 15％ | 138.55 | 4.15 | 0.003 | 0.03 | 0.10 | 0.006 | 4.95 |
| 20％ | 139.23 | 4.89 | 0.003 | 0.03 | 0.10 | 0.006 | 5.08 |
The results of analysis of the dried alkaline zinc powder samples are given in units% in the following table.
| Zn All-purpose | Zn Is provided with | Cd | Fe | S | Pb | As | Ca | Mg | Cu | In(g/t) |
| 98.99 | 96.51 | 0.0036 | 0.01 | 0.07 | 0.055 | — | 0.044 | 0.017 | 0.0098 | 6 |
Zn All-purpose : represents the sum of the effective zinc powder and the oxidized zinc powder.
Zn Is provided with : representing the available zinc powder.
The implementation 1 proves that after the alkaline zinc powder obtained by the process is used for purifying the supernatant, the impurity content in the supernatant is lower, so that a better purification effect is obtained, and the impurity content in the alkaline zinc powder obtained by the process is lower.
In conclusion, the invention provides an alkali zinc powder combined smelting method, which adopts a combined smelting mode of alkali zinc powder preparation and wet purification and simultaneously utilizes a zinc powder wet addition technology, solves the problems of high equipment price, high cost and high energy consumption in the existing alkali zinc powder drying process and the problem of severe operation environment in the zinc powder transportation process, and solves the problem of low-cost application of alkali zinc powder in a wet system; meanwhile, the problems that the alkaline leaching raw material of the alkaline zinc powder is unstable in grade, high in impurity content and needs to be added with a purification process to remove impurities are solved. The alkali-process zinc powder combined smelting method provided by the invention has the characteristics of low use cost, good effect and excellent operation environment, and meets the requirements of low carbon, green and environmental protection.
It will be understood that the invention is not limited to the examples described above, but that modifications and variations will occur to those skilled in the art in light of the above teachings, and that all such modifications and variations are considered to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. An alkali-method zinc powder combined smelting method is characterized by comprising the following steps:
and (3) zinc precipitation: taking the new electrolytic solution in the zinc hydrometallurgy process as a zinc deposition stock solution, and adding an alkaline material into the zinc deposition stock solution to perform zinc deposition reaction to obtain a zinc deposition solution containing zinc deposition residues;
a filtering process: filtering the zinc precipitation solution containing the zinc precipitation slag to obtain zinc precipitation slag;
an alkaline leaching process: dissolving the zinc precipitation slag in an alkali solution for alkali leaching reaction to obtain an alkali leaching solution;
an electrolysis process: electrolyzing the alkaline leaching solution to obtain an alkaline zinc powder solution;
a washing procedure: filtering and washing the alkaline zinc powder solution to obtain alkaline zinc powder;
a size mixing procedure: mixing the alkaline zinc powder with water for size mixing to obtain zinc powder size;
a purification process: purifying the supernatant in the wet zinc smelting process by using the zinc powder slurry to obtain new electrolytic solution in the wet zinc smelting process; in the zinc precipitation procedure, the pH value of the zinc precipitation solution at the reaction end point of the zinc precipitation reaction is 5.5-7, and the reaction time is 15-45min; in the size mixing procedure, the mass content of zinc powder in the zinc powder size is 10-20%; in the purification procedure, after the zinc powder slurry is added into the supernatant, sulfuric acid is added to adjust the pH of the supernatant to be less than or equal to 5.3.
2. The combined smelting method of alkaline zinc powder as defined in claim 1, wherein in the zinc precipitation step, the alkaline material is selected from one or more of calcium oxide, sodium hydroxide and potassium hydroxide.
3. The alkali zinc powder combined smelting method according to claim 1, wherein in the filtering step, the filtering equipment used for filtering is selected from one or more of a vertical plate and frame filter, a ceramic filter, a box-type diaphragm filter and a centrifugal filter.
4. The alkali-process zinc powder combined smelting method of claim 1, wherein in the alkali leaching process, the ratio of liquid to solid is 6-10:1, dissolving the zinc precipitation slag in an alkali solution with the initial concentration of 4-6mol/L for alkali leaching reaction, wherein the liquid-solid ratio is as follows in mL: and g is measured.
5. The alkali zinc powder combined smelting method according to claim 4, wherein the reaction temperature of the alkali leaching reaction is 50-90 ℃, and the reaction time is 1-2h.
6. The combined smelting method of alkaline zinc powder as defined in claim 1, wherein in the electrolysis step, the electrolysis temperature is 20-45 ℃ and the time is less than 5h.
7. The combined smelting method of alkaline zinc powder as claimed in claim 1, wherein in the washing step, the alkaline zinc powder solution is filtered and washed for 3-5 times by a filter, so that the pH of the washing water in the last washing is less than or equal to 8.
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