CN112111647A - Method for pre-treating gold leaching by using gold ore calcine or roasting cyanidation tailings - Google Patents
Method for pre-treating gold leaching by using gold ore calcine or roasting cyanidation tailings 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
- 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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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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Abstract
The refractory arsenic-containing and sulfur-containing gold ore is generally treated by a two-stage roasting-cyaniding gold leaching process, but secondary package of hematite on gold is generated in the roasting process, the cyaniding leaching rate of gold is only about 85%, and the cyaniding effect of tailings is extremely poor, so that the resource waste is serious, and the economic benefit of enterprises is poor. The invention discloses a method for pretreating gold leaching by using gold ore calcine or roasting cyanidation tailings, which comprises the working procedures of roasting conversion, alkali decomposition, non-toxic gold leaching, silicon-containing alkali liquor carbonation, carbonate solution evaporation crystallization and the like. According to the invention, the gold ore calcine or the roasting cyanidation tailings are treated by the alkali medium, so that the gold coating of hematite and silicon-containing minerals can be effectively opened, gold can be efficiently leached out by using a non-toxic gold leaching agent after treatment, the gold in the tailings can be reduced to below 1g/t, and the silicon component can be prepared into a white carbon black product, so that the resource utilization rate is greatly improved. The method disclosed by the invention has the advantages that no cyaniding tailings are generated, the internal circulation of an alkali medium is realized, no waste water is discharged, and the process is green and clean.
Description
Technical Field
The invention belongs to the field of nonferrous metallurgy, and particularly relates to a method for pretreating gold leaching by using gold ore calcine or roasted cyanidation tailings.
Background
The gold mine resources in China are rich, but the proportion of the refractory gold mine resources is increased year by year, and in the proven geological reserves, the refractory gold mine reserves exceed 3000 tons and account for more than 1/3 of the total proven reserves. The gold concentrate containing arsenic and sulfur is a typical refractory gold-bearing mineral, wherein the gold is subjected to microscopic encapsulation by main mineral phases of pyrite, arsenopyrite and part of quartz, so that the leaching of gold is hindered. For such gold concentrate, the leaching rate of gold is generally lower than 40% if the gold is leached by direct cyanidation by a conventional cyanidation method. Therefore, pretreatment is usually required before the gold leaching process. The main pretreatment method at present is the roasting method. The roasting process can remove most of arsenic and sulfur in gold concentrate, and convert the iron-containing material phase into porous hematite (Fe)2O3). The gold ore calcine obtained after roasting can realize the extraction of gold through a cyaniding leaching process.
However, in the current roasting process, the phenomena of overburning, caking and the like cannot be avoided, so that the iron-containing material phase cannot be completely converted into porous hematite, and one part of the iron-containing material phase is converted into the hematite with a compact structure, and secondary wrapping is generated on gold, so that the subsequent cyaniding and gold leaching effects are seriously influenced. In addition, the roasting process also fails to eliminate the gold coating from quartz and silicate minerals. At present, the content of Au in the roasting cyanidation tailings is 1.5-15 g/t, and the resource waste is serious. Most of gold in the roasting cyanidation tailings is wrapped by hematite, a small part of gold is wrapped by quartz or other silicate minerals, and the tailings are cyanided and leached again, so that the leaching rate of gold is extremely low. How to effectively solve the problem of the package of iron-containing and silicon-containing substances in the gold ore calcine relative to gold and improve the recovery rate of gold in the gold ore calcine or the roasting cyanidation tailings, has important significance for the roasting pretreatment process of the gold ore and the gold smelting industry.
Patent CN103014319A discloses a method for enhancing gold extraction from gold concentrate calcine containing sulfur and arsenic, which aims at the problem of gold encapsulation by iron oxide in gold ore calcine and provides a method for metallization reduction roasting-acid leaching-gold leaching, wherein iron oxide is reduced firstly, and then acid leaching is carried out to open the gold encapsulation by iron oxide. However, this method produces a large amount of iron-containing spent acid solution, which is difficult to handle. The patent CN101942566A discloses a method for recovering gold and silver from tailings of gold concentrate roasting and cyaniding, which comprises the steps of mixing dry tailings with a reducing agent and a desulfurizing agent, reducing for 10-30 h at 900-1200 ℃, cooling in an air-isolated manner, discharging, magnetically separating to obtain metal iron powder containing gold and silver, dissolving the metal iron powder with sulfuric acid to prepare ferrous sulfate, and extracting the gold and silver from acid leaching residues with a cyaniding method. The process has high reduction temperature, long reduction time and great energy consumption. The patent CN104404261A discloses a method for synchronously reducing and recovering gold and iron by chlorination roasting of gold concentrate cyanidation tailings, which is characterized in that the cyanidation tailings are desiliconized and enriched in advance by reverse flotation, dried rough concentrate is mixed with a chlorinating agent, a reducing agent, a dephosphorizing agent, a desulfurizing agent and the like for pelletizing, the dried pellets are subjected to chlorination volatilization, synchronous deep reduction and dephosphorization at 1050-1250 ℃, flue gas is collected for recovering gold, and sponge iron is obtained by magnetic separation. The method adopts a high-temperature chlorination method to volatilize gold, the recovery rate of gold is high, but a high-temperature chlorination volatilization process generates a large amount of highly toxic chlorine and hydrogen chloride gas, and a flue gas dust collection and purification process is complicated.
In summary, the existing treatment method of gold ore calcine or roasting cyanidation tailings has the defects of incapability of realizing clean production, high energy consumption, high treatment cost and the like generally, and the invention provides a novel method for pretreating gold leaching by using gold ore calcine or roasting cyanidation tailings so as to realize high-efficiency clean recovery of gold and comprehensive utilization of associated silicon and iron components.
Disclosure of Invention
The invention aims to provide a method for pre-treating gold leaching from gold ore calcine or roasting cyanidation tailings, which comprises the steps of firstly treating the gold ore calcine or roasting cyanidation tailings by using carbonate to convert hematite and quartz in the gold ore calcine or roasting cyanidation tailings into insoluble iron silicate and soluble silicate, further converting the iron silicate into loose and porous amorphous iron oxide and soluble silicate through an alkaline decomposition reaction, eliminating the package of the hematite and silicon in the gold ore calcine or roasting cyanidation tailings relative to gold through phase transformation, and remarkably improving the leaching rate of gold so as to solve the problems of low gold leaching rate, serious resource waste and poor enterprise economic benefit in the conventional roasting-cyanidation gold extraction process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method comprises the steps of taking gold ore calcine or calcine cyanidation tailings as raw materials, firstly carrying out roasting conversion on the raw materials by using carbonate, converting hematite and siliceous phases in which gold is wrapped into the hematite and the siliceous phases into insoluble iron silicate and soluble silicate, further carrying out conversion reaction on the converted products by using alkali solution, further converting the iron silicate into loose and porous amorphous iron oxide and soluble silicate, eliminating the wrapping of the gold, washing the obtained slag phase after filtering and separation, and carrying out gold leaching on the washed slag phase by using a non-toxic gold leaching agent to obtain gold-containing pregnant solution and a slag phase rich in active iron oxide. The alkali liquor obtained in the alkali solution conversion procedure contains silicate, and carbon dioxide is introduced into the alkali liquor for carbonization, so that a white carbon black byproduct can be prepared. The alkali solution is converted into carbonate solution through the carbonization process, and carbonate crystals can be obtained through the processes of evaporation concentration and cooling crystallization and are returned to the carbonate roasting process for recycling. The method comprises the following specific steps:
(1) uniformly mixing gold ore calcine or calcine cyanidation tailings and carbonate, placing the mixture into a high-temperature furnace for roasting reaction for a certain time, and cooling the mixture after the reaction is finished to obtain a roasted product;
(2) ball-milling the roasted product obtained in the step (1), putting the ball-milled roasted product into a reaction kettle, adding an alkali solution, uniformly mixing, heating to a reaction temperature, reacting at a constant temperature for a certain time, cooling after the reaction is finished, and performing liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the alkaline solution reaction process in the step (2), adding the solid phase obtained by separation into a solution containing a non-toxic gold leaching agent to leach gold, and obtaining gold-containing pregnant solution and leaching residues;
(4) dividing the filtrate obtained in the step (2) into two parts, directly returning one part to the alkali solution reaction process in the step (2), introducing carbon dioxide into the other part for carbonization decomposition reaction, performing liquid-solid separation after the carbonization decomposition reaction is finished to obtain a white carbon black product and a carbonate solution, performing evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother solution, returning the carbonate crystal to the mixing process in the step (1) for recycling, and returning the crystallization mother solution to the evaporation concentration process in the step (4) for recycling;
the carbonate in the step (1) is one of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate;
the non-toxic gold leaching agent in the step (3) is one of sodium thiosulfate, potassium thiosulfate or ammonium thiosulfate.
According to the invention, the mass ratio of the gold ore calcine or the roasted cyanidation tailings to the carbonate in the step (1) is 1: 0.5-1: 3, for example, may be 1: 0.5, 1: 0.75, 1: 1. 1: 1.25, 1: 1.5, 1: 1.75, 1: 2. 1: 2.25, 1: 2.5, 1: 2.75 or 1: 3, and other values than those described above, are not exhaustive for the invention, both for brevity and for brevity.
According to the present invention, the calcination reaction temperature in step (1) is 500 ℃ to 1000 ℃, and may be, for example, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃ or 1000 ℃, and other values than the above-mentioned values, which are not exhaustive for reasons of brevity and simplicity.
According to the present invention, the calcination reaction time in step (1) is 0.5-5 hours, such as 0.5 hour, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours or 5 hours, and other values besides the above-mentioned values, which are not exhaustive and are not for brevity.
According to the invention, the roasted product in the step (2) accounts for not less than 90% of-45 micron particles after ball milling.
According to the present invention, the alkali solution used in the step (2) is a sodium hydroxide solution or a potassium hydroxide solution.
According to the present invention, the concentration of the alkaline solution added in step (2) is 1% to 50% by mass, and may be, for example, 1%, 3%, 5%, 8%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%, and other values than the above-mentioned values, which are not exhaustive for reasons of space and simplicity.
According to the invention, the ratio of the volume of the alkali solution to the mass of the roasted product in step (2) is 1.5: 1-10: 1, for example, may be 1.5: 1. 2: 1. 2.5: 1. 3: 1. 3.5: 1. 4: 1. 4.5: 1. 5: 1. 5.5: 1. 6: 1. 6.5: 1. 7: 1. 7.5: 1. 8: 1. 8.5: 1. 9: 1. 9.5: 1 or 10: 1, and other values than those described above, are not exhaustive for the invention, both for brevity and for brevity.
According to the present invention, the reaction temperature in step (2) is 20 ℃ to 200 ℃, and may be, for example, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃, and other values than the above values, which are not intended to be exhaustive or to be concise, and are not exhaustive.
According to the present invention, the reaction time in step (2) is 1-5 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours or 5 hours, and other values than the above values, which are not limited to space and for brevity, the present invention is not exhaustive.
According to the invention, the ratio of the volume of the solution containing the non-toxic gold leaching agent in the step (3) to the mass of the solid phase added into the solution is 1: 1-5: 1, for example, may be 1: 1. 1.5: 1. 2: 1. 2.5: 1. 3: 1. 3.5: 1. 4: 1. 4.5: 1 or 5: 1, and other values than those described above, are not exhaustive for the invention, both for brevity and for brevity.
According to the present invention, the pH of the solution containing the nontoxic gold leaching agent in step (3) is 9-11, for example, 9, 9.5, 10, 10.5 or 11, and other values than the above values are not exhaustive for reasons of space and simplicity.
According to the invention, the solution containing the nontoxic gold leaching agent in the step (3) also contains copper sulfate and ammonium sulfate.
According to the invention, the concentration of the non-toxic gold leaching agent in the solution containing the non-toxic gold leaching agent in the step (3) is 0.05-1 mol/L, for example, 0.05mol/L, 0.1mol/L, 0.15mol/L, 0.2mol/L, 0.25mol/L, 0.3mol/L, 0.35mol/L, 0.4mol/L, 0.45mol/L, 0.5mol/L, 0.55mol/L, 0.6mol/L, 0.65mol/L, 0.7mol/L, 0.75mol/L, 0.8mol/L, 0.85mol/L, 0.9mol/L, 0.95mol/L or 1mol/L, and other values than the above-mentioned values are not limited to space and simple list, and the invention is not exhaustive.
According to the invention, the concentration of copper sulfate in the solution containing the nontoxic gold leaching agent in the step (3) is 0.01-0.5 mol/L, for example, 0.01mol/L, 0.02mol/L, 0.04mol/L, 0.06mol/L, 0.08mol/L, 0.1mol/L, 0.15mol/L, 0.2mol/L, 0.25mol/L, 0.3mol/L, 0.35mol/L, 0.4mol/L, 0.45mol/L or 0.5mol/L, and other values than the above-mentioned values, which are not exhaustive for the sake of simplicity and space, the invention is not limited to the whole.
According to the invention, the concentration of ammonium sulfate in the solution containing the nontoxic gold leaching agent in the step (3) is 0.05-1 mol/L, for example, 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or 1mol/L, and other values besides the above-mentioned values, which are not limited to space and for brevity, the invention is not exhaustive.
According to the present invention, the gold leaching time in step (3) is 1-12 hours, such as 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours or 12 hours, and other values besides the above values, which are limited by space and for brevity, the present invention is not exhaustive.
According to the invention, the ratio of the volume of the alkali solution directly returned to the alkali solution reaction step in the step (2) in the step (4) to the volume of the alkali solution introduced with carbon dioxide for the carbonization decomposition reaction is 1: 0.2-1: 5, for example, may be 1: 0.2, 1: 0.3, 1: 0.4, 1: 0.5, 1: 0.6, 1: 0.7, 1: 0.8, 1: 0.9, 1: 1. 1: 1.5, 1: 2. 1: 2.5, 1: 3. 1: 3.5, 1: 4. 1: 4.5 or 1: 5, and other values than those described above, are not exhaustive for the invention, being limited to space and for the sake of brevity.
The invention adopts the alkaline method to carry out conversion treatment on the gold ore calcine or the roasting cyanidation tailings, can effectively break the package of hematite and siliceous matter relative to gold, and the conversion product adopts a non-toxic gold leaching agent to leach the gold, so that the leaching rate of the gold is greatly improved compared with the traditional cyanidation method, the gold content in the tailings can be reduced to below 1g/t, and meanwhile, the silicon component in the tailings can be prepared into a white carbon black product, thereby greatly improving the resource utilization rate and being very beneficial to improving the economic benefit of gold smelting enterprises. Meanwhile, the method can realize the high-efficiency extraction of the gold by adopting a non-toxic gold leaching agent, does not generate highly toxic cyaniding tailings, and can be used as a raw material for preparing iron-based products, wherein the main component of a slag phase is active ferric oxide. The alkali medium used in the method can realize internal circulation, no waste water and gas is discharged, and the process is green and clean.
Drawings
FIG. 1 is a process flow diagram of a method for pre-treating gold leaching by gold ore calcine or calcine cyanidation tailings.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.
Example 1:
the method treats the two-stage roasting calcine of certain refractory arsenic-containing and sulfur-containing gold ore in Hunan, wherein the gold content is 71.4g/t, the ferric oxide content is 49.8 wt%, and the silicon dioxide content is 28.9 wt%. The main metal mineral is hematite containing a small amount of magnetite, and the main gangue mineral is quartz containing a small amount of mica. The gold ore calcine is treated by a conventional cyanidation method, the leaching rate of gold is only 83.5%, and the gold content in cyanidation tailings is 11.8 g/t.
The treatment is carried out according to the process flow shown in figure 1, and the specific steps are as follows:
(1) taking 200g of gold ore calcine, and mixing the gold ore calcine and sodium carbonate according to the mass ratio of 1: 0.5, adding sodium carbonate, uniformly mixing, placing into a high-temperature furnace, roasting at 1000 ℃ for 0.5 hour, and cooling after the reaction is finished to obtain a roasted product;
(2) ball-milling the obtained roasting product until the proportion of-45 micron particles is more than or equal to 90%, putting the roasted product into a reaction kettle, and mixing the roasted product with the organic solvent according to the volume/mass ratio of 3: 1, adding a sodium hydroxide solution with the mass concentration of 10%, stirring and reacting for 3 hours at 150 ℃, cooling after the reaction is finished, and performing liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the step (2) of alkaline solution reaction, adding the solid phase obtained by separation into a solution containing 0.5mol/L sodium thiosulfate, 0.2mol/L copper sulfate and 0.1mol/L ammonium sulfate to leach out gold, wherein the volume/mass ratio of the solution to the solid phase is 3: 1, the pH value of the solution is 10, the gold leaching time is 4 hours, the gold leaching rate is 99.3 percent, and the gold content in the leaching residue is reduced to 0.5 g/t. And obtaining gold-containing pregnant solution and leaching residues after leaching. The gold-containing pregnant solution is used for recovering gold, and most of iron-containing substances in leaching residues are active ferric oxide which can be used as raw materials for preparing iron-based products;
(4) dividing the filtrate obtained in the step (2) into two parts, wherein one part is directly returned to the step (2) of alkali solution reaction, and the other part is introduced with carbon dioxide for carbonization decomposition reaction, and the volume ratio of the two parts is 1: 1, carrying out liquid-solid separation after the carbonization-decomposition reaction to obtain a white carbon black primary product and a carbonate solution, carrying out evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother liquor, returning the carbonate crystal to the mixing process of the step (1) for recycling, and returning the crystallization mother liquor to the evaporation concentration process of the step (4) for recycling.
Example 2:
the cyanidation tailings obtained by the two-stage roasting-cyanidation gold leaching process of certain intractable arsenic-containing and sulfur-containing gold ore in Henan are treated, wherein the gold content is 10.5g/t, the ferric oxide content is 48.3 wt%, and the silicon dioxide content is 29.2 wt%. The main metal mineral is hematite containing a small amount of magnetite, and the main gangue mineral is quartz containing a small amount of mica. The cyanidation tailings are leached again by a conventional cyanidation method, and gold is hardly leached.
The treatment is carried out according to the process flow shown in figure 1, and the specific steps are as follows:
(1) taking 200g of cyanidation tailings, and mixing the cyanidation tailings with potassium carbonate according to a mass ratio of 1: 1, adding potassium carbonate, uniformly mixing, placing into a high-temperature furnace, roasting at 500 ℃ for 1.5 hours, and cooling after the reaction is finished to obtain a roasted product;
(2) ball-milling the obtained roasting product until the proportion of-45 micron particles is more than or equal to 90%, putting the roasted product into a reaction kettle, and mixing the roasted product and the reaction kettle according to the volume/mass ratio of 2: 1, adding a potassium hydroxide solution with the mass concentration of 20%, stirring and reacting for 1h at 80 ℃, cooling after the reaction is finished, and carrying out liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the step (2) of alkaline solution reaction, adding the solid phase obtained by separation into a solution containing 1mol/L potassium thiosulfate, 0.05mol/L copper sulfate and 1mol/L ammonium sulfate to leach out gold, wherein the volume/mass ratio of the solution to the solid phase is 5: 1, the pH value of the solution is 9, the gold leaching time is 1 hour, the gold leaching rate is 94.3 percent, and the gold content in the leaching residue is reduced to 0.6 g/t. And obtaining gold-containing pregnant solution and leaching residues after leaching. The gold-containing pregnant solution is used for recovering gold, and most of iron-containing substances in leaching residues are active ferric oxide which can be used as raw materials for preparing iron-based products;
(4) dividing the filtrate obtained in the step (2) into two parts, wherein one part is directly returned to the step (2) of alkali solution reaction, and the other part is introduced with carbon dioxide for carbonization decomposition reaction, and the volume ratio of the two parts is 1: and 3, carrying out liquid-solid separation after the carbonization-decomposition reaction is finished to obtain a white carbon black primary product and a carbonate solution, carrying out evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother liquor, returning the carbonate crystal to the mixing process of the step (1) for recycling, and returning the crystallization mother liquor to the evaporation concentration process of the step (4) for recycling.
Example 3:
the method is used for treating the two-stage roasting calcine of certain refractory arsenic-containing and sulfur-containing gold ore in Shaanxi, wherein the gold content is 59.9g/t, the iron oxide content is 50.4 wt%, and the silicon dioxide content is 27.3 wt%. The main metal mineral is hematite containing a small amount of magnetite, and the main gangue mineral is quartz containing a small amount of mica. The gold ore calcine is treated by a conventional cyanidation method, the leaching rate of gold is only 81.9%, and the gold content in cyanidation tailings is 10.8 g/t.
The treatment is carried out according to the process flow shown in figure 1, and the specific steps are as follows:
(1) taking 200g of gold ore calcine, and mixing the gold ore calcine and sodium bicarbonate according to the mass ratio of 1: 3, adding sodium bicarbonate, uniformly mixing, placing into a high-temperature furnace, roasting at 650 ℃ for 3.5 hours, and cooling after the reaction is finished to obtain a roasted product;
(2) ball-milling the obtained roasting product until the proportion of-45 micron particles is more than or equal to 90%, putting the roasted product into a reaction kettle, and mixing the roasted product with the raw materials according to the volume/mass ratio of 5: 1, adding a sodium hydroxide solution with the mass concentration of 1%, stirring and reacting for 2 hours at 200 ℃, cooling after the reaction is finished, and carrying out liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the step (2) of alkaline solution reaction, adding the solid phase obtained by separation into a solution containing 0.05mol/L sodium thiosulfate, 0.01mol/L copper sulfate and 0.5mol/L ammonium sulfate to leach out gold, wherein the volume/mass ratio of the solution to the solid phase is 1: 1, the pH value of the solution is 9.5, the gold leaching time is 12 hours, the gold leaching rate is 98.7 percent, and the gold content in the leaching residue is reduced to 0.8 g/t. And obtaining gold-containing pregnant solution and leaching residues after leaching. The gold-containing pregnant solution is used for recovering gold, and most of iron-containing substances in leaching residues are active ferric oxide which can be used as raw materials for preparing iron-based products;
(4) dividing the filtrate obtained in the step (2) into two parts, wherein one part is directly returned to the step (2) of alkali solution reaction, and the other part is introduced with carbon dioxide for carbonization decomposition reaction, and the volume ratio of the two parts is 1: and 0.2, carrying out liquid-solid separation after the carbonization-decomposition reaction to obtain a white carbon black primary product and a carbonate solution, carrying out evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother liquor, returning the carbonate crystal to the mixing process in the step (1) for recycling, and returning the crystallization mother liquor to the evaporation concentration process in the step (4) for recycling.
Example 4:
the cyanidation tailings obtained by the two-stage roasting-cyanidation gold leaching process of certain refractory arsenic-containing and sulfur-containing gold ore in Shandong are treated, wherein the gold content is 6.7g/t, the ferric oxide content is 46.5 wt%, and the silicon dioxide content is 27.3 wt%. The main metal mineral is hematite containing a small amount of magnetite, and the main gangue mineral is quartz containing a small amount of mica. The cyanidation tailings are leached again by a conventional cyanidation method, and gold is hardly leached.
The treatment is carried out according to the process flow shown in figure 1, and the specific steps are as follows:
(1) taking 200g of cyanidation tailings, and mixing the cyanidation tailings with potassium bicarbonate according to a mass ratio of 1: 2 adding potassium bicarbonate, uniformly mixing, placing into a high-temperature furnace, roasting at 800 ℃ for 5 hours, and cooling after the reaction is finished to obtain a roasted product;
(2) ball-milling the obtained roasting product until the proportion of-45 micron particles is more than or equal to 90%, putting the roasted product into a reaction kettle, and mixing the roasted product with the raw materials according to the volume/mass ratio of 10: 1, adding a potassium hydroxide solution with the mass concentration of 50%, stirring and reacting for 5 hours at 20 ℃, and after the reaction is finished, carrying out liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the step (2) of alkaline solution reaction, adding the solid phase obtained by separation into a solution containing 0.2mol/L ammonium thiosulfate, 0.5mol/L copper sulfate and 0.05mol/L ammonium sulfate to leach out gold, wherein the volume/mass ratio of the solution to the solid phase is 2: 1, the pH value of the solution is 11, the gold leaching time is 8 hours, the gold leaching rate is 89.6 percent, and the gold content in the leaching residue is reduced to 0.7 g/t. And obtaining gold-containing pregnant solution and leaching residues after leaching. The gold-containing pregnant solution is used for recovering gold, and most of iron-containing substances in leaching residues are active ferric oxide which can be used as raw materials for preparing iron-based products;
(4) dividing the filtrate obtained in the step (2) into two parts, wherein one part is directly returned to the step (2) of alkali solution reaction, and the other part is introduced with carbon dioxide for carbonization decomposition reaction, and the volume ratio of the two parts is 1: and 5, carrying out liquid-solid separation after the carbonization-decomposition reaction to obtain a white carbon black primary product and a carbonate solution, carrying out evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother liquor, returning the carbonate crystal to the mixing process of the step (1) for recycling, and returning the crystallization mother liquor to the evaporation concentration process of the step (4) for recycling.
Claims (5)
1. A method for pre-treating gold leaching by using gold ore calcine or roasting cyanidation tailings is characterized by comprising the following steps:
(1) uniformly mixing gold ore calcine or calcine cyanidation tailings and carbonate, placing the mixture into a high-temperature furnace for roasting reaction for a certain time, and cooling the mixture after the reaction is finished to obtain a roasted product;
(2) ball-milling the roasted product obtained in the step (1), putting the ball-milled roasted product into a reaction kettle, adding an alkali solution, uniformly mixing, heating to a reaction temperature, reacting at a constant temperature for a certain time, cooling after the reaction is finished, and performing liquid-solid separation to obtain a solid phase and a filtrate;
(3) washing the solid phase obtained in the step (2) with water, carrying out liquid-solid separation, returning the liquid phase obtained by separation to the alkaline solution reaction process in the step (2), adding the solid phase obtained by separation into a solution containing a non-toxic gold leaching agent to leach gold, and obtaining gold-containing pregnant solution and leaching residues;
(4) dividing the filtrate obtained in the step (2) into two parts, directly returning one part to the alkali solution reaction process in the step (2), introducing carbon dioxide into the other part for carbonization decomposition reaction, performing liquid-solid separation after the carbonization decomposition reaction is finished to obtain a white carbon black product and a carbonate solution, performing evaporation concentration, cooling crystallization and liquid-solid separation on the carbonate solution to obtain a carbonate crystal and a crystallization mother solution, returning the carbonate crystal to the mixing process in the step (1) for recycling, and returning the crystallization mother solution to the evaporation concentration process in the step (4) for recycling;
the carbonate in the step (1) is one of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate;
the non-toxic gold leaching agent in the step (3) is one of sodium thiosulfate, potassium thiosulfate or ammonium thiosulfate.
2. The method according to claim 1, wherein the mass ratio of the gold ore calcine or the roasted cyanidation tailings to the carbonate in the step (1) is 1: 0.5-1: 3, the roasting reaction temperature is 500-1000 ℃, and the roasting reaction time is 0.5-5 hours.
3. The method according to claim 1, wherein in the step (2), the proportion of-45 μm particles of the roasted product after ball milling is not less than 90%, the alkali solution is sodium hydroxide solution or potassium hydroxide solution, the mass concentration of the alkali solution is 1-50%, and the proportion of the volume of the alkali solution to the mass of the roasted product is 2: 1-10: 1, the reaction temperature is 20-200 ℃, and the reaction time is 1-5 hours.
4. The method according to claim 1, wherein the ratio of the volume of the solution containing the nontoxic gold leaching agent in the step (3) to the mass of the solid phase added thereto is 1: 1-5: 1, the pH value of the solution is 9-11, the solution also contains copper sulfate and ammonium sulfate, the concentration of the non-toxic gold leaching agent is 0.05-1 mol/L, the concentration of the copper sulfate is 0.01-0.5 mol/L, the concentration of the ammonium sulfate is 0.05-1 mol/L, and the gold leaching time is 1-12 hours.
5. The method according to claim 1, wherein the ratio of the volume of the alkali solution directly returned to the alkali solution reaction step (2) in the step (4) to the volume of the alkali solution subjected to the carbonization decomposition reaction by introducing carbon dioxide is 1: 0.2-1: 5.
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