CN111748690B - Method for purifying and deironing hydrometallurgy leaching solution based on hydrothermal lattice transformation - Google Patents
Method for purifying and deironing hydrometallurgy leaching solution based on hydrothermal lattice transformation Download PDFInfo
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- CN111748690B CN111748690B CN202010751934.4A CN202010751934A CN111748690B CN 111748690 B CN111748690 B CN 111748690B CN 202010751934 A CN202010751934 A CN 202010751934A CN 111748690 B CN111748690 B CN 111748690B
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for purifying and deironing a hydrometallurgy leaching solution based on hydrothermal lattice transformation, and belongs to the field of hydrometallurgy purification and impurity removal. The method comprises the steps of completely oxidizing ferrous ions in the hydrometallurgy leaching solution into ferric ions, hydrolyzing the ferric ions through neutralization and precipitation to form ferric hydroxide precipitates, and converting the ferric hydroxide precipitates into hematite crystals through hydrothermal reaction. The method has the characteristics of good iron removal effect, direct utilization of iron removal slag, simple operation, low operation cost and the like, ensures the deep purification of iron ions in the leaching solution, and can also obtain the hematite with high iron content to be recycled as an iron making raw material.
Description
Technical Field
The invention relates to a method for purifying and deironing a hydrometallurgy leaching solution, in particular to a method for purifying and deironing a hydrometallurgy leaching solution based on hydrothermal lattice transformation, and belongs to the technical field of purification and impurity removal of hydrometallurgy and resource recycling.
Background
In hydrometallurgical processing of non-ferrous metals such as copper, zinc, nickel, manganese, etc., the concentrates contain small amounts of iron-containing ores. In the wet smelting process, the iron elements are inevitably introduced into the leaching solution, and the concentration of iron ions is often more than 1 g/L. Because the activity of iron ions is high, the iron ions are removed from the solution before subsequent zinc powder replacement, extraction impurity removal, vulcanization impurity removal, electrodeposition and other processes, for example, the concentration of the iron ions in the solution is required to be lower than 10mg/L in zinc electrodeposition, and the iron content of the solution is required to be lower than 50mg/L when the nickel solution is used for extracting and purifying cobalt.
Iron removal by precipitation is the most important and widely applied method in the existing hydrometallurgy process. Ferric iron ions are oxidized into ferric iron at different temperatures, and alkaline reagents such as calcium oxide, calcium hydroxide, calcium carbonate, sodium hydroxide, sodium carbonate and the like are added to adjust the pH of the solution, so that the ferric iron ions are hydrolyzed to form different solid phases, namely, double hydroxide salt (containing jarosite), hematite, goethite and ferric hydroxide, as shown in figure 1, and the iron phase precipitation is the most important methods for removing iron from the solution in the current industrial application.
1) Iron removal by jarosite process
The introduction of the technology of removing iron by the jarosite method in the zinc industry can lead the recovery rate of zinc in the whole process to reach 96 to 98 percent. Mainly because the technology can recover zinc iron spinel (Fe) besides zinc in zinc oxide (ZnO)2O3ZnO). Therefore, the double salts of jarosite have been extensively studied.
Jarosite is a double salt precipitate based on ferric sulphate, the formation of which can be represented by formula (1):
3Fe2(SO4)3+M2SO4+12H2O→2MFe3(SO4)2(OH)6↓+6H2SO4 (1)
wherein M represents Na+、NH4 +、H3O+、Li+、K+、Pb2+And (3) plasma. There has been extensive interest in the jarosite precipitation reactions, and particularly in zinc hydrometallurgy, a great deal of research work has been reported on the reaction parameters of jarosite precipitation. The test results show that the jarosite precipitation process is closely related to temperature, pH and reaction time. In fact, the reaction temperature is raised from 70 ℃ to 110 ℃ which significantly increases the reaction rate for the formation of the precipitate. To avoid costly autoclave equipment, the temperature was typically 97 ℃ and the iron ion precipitation was confirmed to be complete within a few hours. The ideal conditions for the formation of jarosite according to different developers are a temperature of 95 ℃ to 100 ℃ and a pH of 1.5 to 1.8, requiring vigorous stirring and the addition of jarosite seeds. The disadvantage of the jarosite process for removing iron is that it may co-precipitate with valuable metal ions in solution, such as copper, zinc, cobalt, nickel, manganese, indium, gallium, germanium, aluminum, etc. Dutrizac found that the doping modes of divalent metal and trivalent metal in jarosite precipitation are different, the pH value of the solution is increased, and coprecipitation is carried outThe proportion is increased, and the concentration of doping ions is increased along with the increase of the concentration of iron ions in the solution, so that a large amount of zinc, precious metals and the like are lost, and a large amount of heavy metal solid waste is generated to seriously pollute the environment. It is strictly required by law that the polluting slag is stored in a completely impervious tailings dam and that the nearby waters are strictly controlled from contamination. Although some researchers research the conversion of jarosite slag into marketable hematite in order to treat a large amount of polluting jarosite slag accumulated for a long time, no industrial application case exists due to the large difficulty in impurity removal or high treatment cost.
2) Removal of iron by goethite process
The process for removing iron by goethite method is developed and applied by Baran factory of Laoshan corporation of Belgium. The ferric ions in the solution are converted into goethite precipitate to be removed, and the real-time concentration of the ferric ions in the solution is required to be lower than 1 g/L. The consumed iron ions can be kept consistent with the added iron ions by reducing all iron ions to ferrous ions and then slowly oxidizing to ferric ions (VM method) or by spraying to control the addition of the leachate in the reaction kettle (EZ method). The reaction for removing iron by goethite method is shown as the following formula (2):
Fe2(SO4)3+4H2O→2FeOOH↓+3H2SO4 (2)
the reaction can be carried out only under the conditions of 80-90 ℃ and pH 2-4, and an alkaline material is required to be added in the reaction process to neutralize the generated acid. The goethite precipitate has a low level of impurity ions, and most of the impurity ions can be removed by acid washing, but cannot be completely removed.
Compared with the jarosite process, the goethite process has much less slag generated by iron removal. However, in actual production operation, the goethite method for removing iron generates ferric hydroxide precipitate, which causes the difficulty of sedimentation and filtration operation of the iron-removing slag, and the iron-removing slag has high water content and serious loss of valuable metals, for example, the iron-removing slag generated by a zinc solution goethite process contains about 6 percent of zinc. The disposal and the recycling of the goethite iron-removing slag are also reported in more researches, mainly comprising a wet method and a fire method, but the iron content of the iron-precipitating slag produced industrially is only about 30 percent, and the iron-precipitating slag contains elements such as zinc, arsenic, germanium, indium and the like, so that the requirement of iron-making raw materials is difficult to meet.
3) Iron removal by hematite method
A significant objective of removing iron from solution using the hematite process is for the resulting hematite precipitate to be used in the production of cement, as a raw material for iron manufacture, or as a pigment. This means that the problem of iron slag accumulation in the hydrometallurgical industry is solved.
The reaction of the hydrolysis of ferric sulfate in solution to produce hematite precipitate is shown in the following formula (3):
2FeSO4+1/2O2+2H2O→Fe2O3↓+2H2SO4 (3)
the process requires a partial pressure of oxygen (P)O2) Above 5bar, at temperatures above 185 ℃. According to literature data, iron ions are removed by conversion to hematite precipitate at 200 ℃, and the reaction produces acid. When the concentration of sulfuric acid is increased to 65g/L, FeOOHSO is preferentially precipitated4And (4) precipitating. Fe is obtained from the initial iron ion concentration2O3And FeOOHSO4Mixed precipitates with different proportions. The required concentration of sulfuric acid to produce hematite precipitate at 185 ℃ would need to be less than 56 g/L. In the process, a high-temperature high-pressure reaction kettle with the functions of air inflation and medicine addition is required to heat all the leaching solution to 200 ℃ and maintain the temperature for 1-2 hours, the investment and operation cost is high, and the cost is difficult to bear by a wet-process smelting plant.
Disclosure of Invention
The invention aims to solve the problems that in the existing hydrometallurgical purification and iron removal process of copper, zinc, nickel, manganese and the like, a great amount of hazardous waste iron removal slag generated by iron removal by a jarosite method and a goethite method is piled up in a tailing dam for a long time, iron removal equipment by a hematite method is used, the operation cost is high and the like.
In order to achieve the technical purpose, the invention provides a method for purifying and deironing a hydrometallurgy leaching solution based on hydrothermal lattice transformation, which comprises the following steps:
1) when the hydrometallurgical leaching solution contains ferrous ions or contains ferrous ions and ferric ions at the same time, adding a chemical oxidant into the hydrometallurgical leaching solution to convert the ferrous ions into ferric ions, and converting the ferric ions into ferric hydroxide and/or goethite-like precipitates through neutralization precipitation;
alternatively, the first and second electrodes may be,
when the hydrometallurgical leaching solution contains ferric ions, the hydrometallurgical leaching solution is subjected to neutralization precipitation to convert the ferric ions into ferric hydroxide and/or goethite-like precipitates;
2) transferring the obtained ferric hydroxide and/or goethite-like sediment into a high-pressure reaction kettle for hydrothermal reaction to generate hematite particles.
The key point of the technical scheme of the invention is that the ferric hydroxide or goethite-like ore precipitate generated by neutralizing, precipitating, purifying and deironing is subjected to hydrothermal reaction, so that the ferric hydroxide or goethite-like ore precipitate lattice is transformed into hematite (Fe)2O3) The product has high iron-containing grade, good filterability and low impurity ion content and can be directly used as a steel smelting raw material or an iron oxide red pigment.
As a preferred scheme, the neutralization and precipitation process is as follows: controlling the temperature of the hydrometallurgy leaching solution to be 0-100 ℃ and adjusting the pH value to be more than 3, so that ferric ions are hydrolyzed and converted into ferric hydroxide and/or goethite-like precipitates. By controlling the pH and temperature conditions of the hydrometallurgical leachate, the ferric ions can be guaranteed to be hydrolyzed completely, and ferric hydroxide precipitate or goethite-like precipitate can be formed efficiently.
As a further preferable scheme, the temperature is adjusted to be 70-100 ℃ in the neutralization and precipitation process. A large number of experiments show that in the temperature range of 0-100 ℃, the higher the crystallinity and the better the sedimentation performance of ferric hydroxide sediment or goethite-like sediment generated by the neutralization precipitation along with the rise of the temperature, and the lower the water content of the concentrated underflow, the smaller the precipitation amount of the hydrothermal reaction is, so the neutralization precipitation is preferably carried out in the temperature range of 70-100 ℃.
As a further preferable scheme, the pH value is adjusted to be 4-5 in the neutralization and precipitation process.
As a preferred scheme, the ferric hydroxide and/or goethite-like ore precipitate obtained by neutralizing and precipitating is subjected to solid-liquid separation by using a thickener, dense underflow is transferred into a high-pressure reaction kettle for hydrothermal reaction, and when the concentration of iron ions in filtrate meets the requirement of a purification iron removal index, the filtrate is merged with dense overflow and enters a subsequent purification working section; and when the concentration of iron ions in the filtrate does not meet the index requirement of iron removal by purification, returning to the wet-process metallurgy leachate.
Preferably, the hydrothermal reaction is carried out at a temperature of 140 to 220 ℃ for 0.5 hour or more. Under the optimal reaction conditions, the lattice transformation of the ferric hydroxide and/or goethite-like ore precipitates can be realized, so that the ferric hydroxide and/or goethite-like ore precipitates with high water content, low grade, difficult sedimentation and filtration operation and large valuable metal carrying capacity are completely transformed into hematite with high purity, good sedimentation and filtration performance and high grade. Particularly, the higher the temperature of the hydrothermal reaction is, the higher the iron content in the obtained hematite precipitate is (60-65%), the better the crystal form is, therefore, the preferred hydrothermal reaction temperature is 140-220 ℃, and the preferred hydrothermal reaction time is 2-3 hours.
As a preferable scheme, the dense underflow is pumped into a high-pressure reaction kettle for hydrothermal reaction, the reaction temperature is controlled to be 140-220 ℃, the reaction is carried out for more than 0.5 hour, iron hydroxide or goethite-like particles are converted into hematite particles, and hematite solid particles and filtrate are obtained after solid-liquid separation.
As a preferred scheme, the filtrate is converged with the dense overflow according to the iron ion concentration of the filtrate, and enters a subsequent purification section if the iron ion concentration of the filtrate meets the index requirement of purification and iron removal; if the concentration of the iron ions in the filtrate can not meet the index requirement of iron removal by purification, the filtrate is returned to the iron-containing solution.
As a preferred scheme, the hematite solid particles can be used as iron and steel smelting raw materials, iron red pigments and the like for recycling according to the iron content and other impurity contents.
As a preferable scheme, a chemical oxidant is added in the neutralization and precipitation process to convert ferrous ions into ferric ions, the chemical oxidant is oxygen, hydrogen peroxide and other common oxidants in the industries, and the dosage of the oxidant is controlled to oxidize all ferrous ions into ferric ions.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the method for purifying and removing iron based on hydrothermal lattice transformation directly forms hematite precipitate in aqueous solution, the amount of the generated iron-removing slag is only 20-40% of that of the iron-removing slag generated by purifying and removing iron by the traditional jarosite method, goethite method and neutralization precipitation method, and the filtering performance of the iron-removing slag is obviously improved.
The content of the hematite precipitated iron produced by the method for purifying and removing iron based on hydrothermal lattice transformation is higher than 60 percent, and the hematite precipitated iron can be used as a steel smelting raw material or iron oxide red pigment for absorption without being stockpiled in a slag dam.
The method for purifying and removing iron based on hydrothermal lattice transformation disclosed by the invention has the advantages that the content of impurity elements in hematite precipitate is low, the content of nickel is less than 1%, the content of zinc is less than 2%, the content of copper is less than 4%, and the amount of iron removal slag is low, so that the loss rate of valuable metal elements in a purification and iron removal working section is obviously reduced.
Compared with the traditional hematite method for purifying and removing iron, the hydrothermal lattice transformation-based method for purifying and removing iron only needs to treat the dense underflow which accounts for about 15% of the total volume of the solution by the hydrothermal reaction, does not need to pump oxygen and alkaline reagents at high pressure, reduces the equipment investment cost and obviously reduces the operation energy consumption.
Drawings
FIG. 1 is a schematic illustration of the conditions under which the different iron phases in a ferric sulphate solution precipitate;
FIG. 2 is a result of a hydrometallurgical purification and iron removal technology based on hydrothermal lattice regulation;
wherein the content of the first and second substances,
FIG. 2a is a process flow diagram;
FIG. 2b shows that the iron-removed slag obtained by neutralization precipitation method iron removal has better settling property by heating;
fig. 2c and 2d show hydrothermal lattice transformation of the dense underflow to convert the amorphous ferric hydroxide precipitate to the crystalline hematite precipitate.
Detailed Description
The following examples are intended to further illustrate the present invention and are not intended to limit the scope of the invention as claimed.
Example 1
The green low-consumption purification and iron removal method based on hydrothermal lattice transformation is applied to a laboratory zinc solution purification and iron removal simulation solution, the solution is prepared by dissolving zinc sulfate heptahydrate and ferric sulfate in deionized water, wherein the concentration of zinc ions is 100g/L, and the concentration of iron ions is 2 g/L. The experimental technical route is shown in figure 2a, firstly, iron ions are purified and deironized by a neutralization precipitation method at 80 ℃, 1mol/L sodium hydroxide solution is added to adjust the end point pH of the solution to be 4.0, and the purification depth of the iron ions in the solution can reach the production requirement (Fe)3+<10mg/L), the ferric hydroxide precipitate generated at 80 ℃ has better sedimentation performance (figure 2b), 500ml of suspension solution is settled for 4 hours, then the volume of the sedimentation layer is compressed to 75ml, the supernatant is used as dense overflow to directly carry out the subsequent purification working section, the sedimentation layer is used as dense underflow to carry out hydrothermal reaction (100-200 ℃) in a high-pressure reaction kettle, and the ferric hydroxide precipitate is heated and transformed into hematite (Fe)2O3) Precipitation, the higher the temperature of hydrothermal reaction, the higher the iron content in hematite precipitate obtained (60% -65%), the better the crystalline form (fig. 2c-2 d).
Example 2
The method is applied to a zinc hydrometallurgy, oxidation and iron removal process of a Yunnan Chihong Zige smelting division company, the concentration of ferrous ions in a liquid before iron removal is 2.54g/L, 50L of solution is taken for iron removal test, the temperature of the solution is controlled at 80-85 ℃, oxygen is introduced to oxidize ferrous ions into ferric ions, an alkali solution is added to adjust the end point pH of the solution to be 4.0-4.5, a suspension is kept stand for sedimentation after iron removal, a supernatant is extracted after 4 hours to analyze the concentration of the ferric ions in the solution, and a sedimentation layer is transferred to a Yunnan Chien Hongzagge smelting division company to analyze the concentration of the ferric ions in the solutionCarrying out hydrothermal reaction in a high-pressure reaction kettle, controlling the temperature to be 200 ℃, cooling and discharging after reacting for 3 hours, analyzing the concentration of iron ions in the filtrate after filtering, and testing the contents of elements such as iron, zinc, germanium, arsenic and the like in the filter residue after drying the filter residue at 60 ℃. And the iron removal process of the existing goethite method of the enterprise is used for testing as comparison, and the result arrangement is favorable for the table 1. The results show that: the iron removal process can meet the requirement of solution purification and iron removal, simultaneously, the iron content in the generated iron removal slag reaches more than 62 percent, the slag amount is reduced by more than 50 times compared with the original process, and the zinc loss is obviously reduced to 10g/m3The following. The superiority of the iron removal process can be shown by comparing with the original iron removal process on site.
TABLE 1 test results of zinc hydrometallurgy and iron oxide removal by Yunnan Zhang Hongzhong Ge Huizze smelting division
Example 3
The green low-consumption purification and iron removal method based on hydrothermal lattice transformation is applied to purification and iron removal of electrolytic anolyte in a Jinchuan nickel smelting plant, the concentration of iron ions in the electrolytic anolyte is 0.16-0.57 g/L, and an astrakanite method is adopted for iron removal on site. Taking 50L of solution to carry out the iron removal process test of the invention, controlling the temperature of the solution at 80-85 ℃, adding an alkali solution to adjust the end point pH of the solution to be 4.5-5.0, standing and settling the suspension after purifying and removing iron, extracting supernatant after 3 hours to analyze the concentration of iron ions in the solution, transferring the settled layer into a high-pressure reaction kettle to carry out hydrothermal reaction, controlling the temperature to be 200 ℃, cooling and discharging after 2 hours of reaction, analyzing the concentration of iron ions in filtrate after filtering, and testing the content of elements such as iron, zinc, germanium, arsenic and the like in the filter residue after drying the filter residue at 60 ℃. And the iron removal process of the existing jarosite method of the enterprise is used for testing as comparison, and the result arrangement is favorable for the table 2. The results show that: iron removal according to the inventionThe process can meet the requirement of solution purification and iron removal, and simultaneously, the iron content in the iron-removed slag reaches more than 63 percent, the iron-removed slag can be used as iron ore or iron oxide red pigment for resource utilization, and the nickel loss is remarkably reduced to 0.5g/m3The following. The superiority of the iron removal process can be shown by comparing with the original iron removal process on site.
TABLE 2 purification and deironing test results of electrolytic anolyte in NiCuAlCu smeltery
Claims (2)
1. A method for purifying and deironing a hydrometallurgy leaching solution based on hydrothermal lattice transformation is characterized by comprising the following steps: the method comprises the following steps:
1) when the hydrometallurgical leaching solution contains ferrous ions or contains ferrous ions and ferric ions at the same time, adding a chemical oxidant into the hydrometallurgical leaching solution to convert the ferrous ions into ferric ions, and converting the ferric ions into ferric hydroxide and/or goethite-like precipitates through neutralization precipitation;
alternatively, the first and second electrodes may be,
when the hydrometallurgical leaching solution contains ferric ions, the hydrometallurgical leaching solution is subjected to neutralization precipitation to convert the ferric ions into ferric hydroxide and/or goethite-like precipitates;
adjusting the temperature to be 70-100 ℃ in the neutralization and precipitation process;
adjusting the pH value to 4-5 in the neutralization and precipitation process;
2) transferring the obtained ferric hydroxide and/or goethite-like sediment into a high-pressure reaction kettle, and carrying out hydrothermal reaction to generate hematite particles; the temperature of the hydrothermal reaction is 140-220 ℃, and the time is more than 0.5 hour.
2. The method for purifying and deironing hydrometallurgical leachate based on hydrothermal lattice transformation as claimed in claim 1, wherein the method comprises the following steps: carrying out solid-liquid separation on the ferric hydroxide and/or goethite-like ore precipitate obtained by neutralizing and precipitating by adopting a thickener, transferring the concentrated underflow into a high-pressure reaction kettle for hydrothermal reaction, and converging the concentrated underflow with concentrated overflow when the concentration of iron ions in the filtrate meets the requirement of a purification iron removal index, and entering a subsequent purification working section; and when the concentration of iron ions in the filtrate does not meet the index requirement of iron removal by purification, returning to the wet-process metallurgy leachate.
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| CN115652104B (en) * | 2022-11-01 | 2023-09-12 | 中南大学 | Lead-free jarosite crystal, jarosite slag, preparation method and application |
| CN116692941A (en) * | 2023-07-06 | 2023-09-05 | 中南大学 | Method for preparing high-quality sodium pyroantimonate through gradient purification and oxidation |
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| CN106435183B (en) * | 2016-10-13 | 2018-08-07 | 中南大学 | A kind of wet-process metallurgy leachate neutralization removes solid oxidizer and its application of iron |
| CN106868304A (en) * | 2016-12-27 | 2017-06-20 | 河南豫光锌业有限公司 | A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum |
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| JPH03150222A (en) * | 1989-11-02 | 1991-06-26 | Tsukishima Kikai Co Ltd | Method for removing si from dissolved solution of zinc-containing substance containing si |
| CN1675133A (en) * | 2002-08-16 | 2005-09-28 | 阿尔伯麦尔荷兰有限公司 | Preparation of iron compounds by hydrothermal conversion |
| CN102168181A (en) * | 2011-03-17 | 2011-08-31 | 云南永昌铅锌股份有限公司 | Horizontal type pressure leaching kettle and zinc sulfide concentrate leaching method using same |
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