CN111394577A - Method for leaching coated hematite in secondary calcine by using oxalic acid - Google Patents
Method for leaching coated hematite in secondary calcine by using oxalic acid Download PDFInfo
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- CN111394577A CN111394577A CN202010364750.2A CN202010364750A CN111394577A CN 111394577 A CN111394577 A CN 111394577A CN 202010364750 A CN202010364750 A CN 202010364750A CN 111394577 A CN111394577 A CN 111394577A
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/08—Obtaining noble metals by cyaniding
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
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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 coating hematite in secondary calcine by using oxalic acid leaching, which comprises the following steps of firstly, adding oxalic acid into a leaching tank; adding the second-stage calcine and water into a leaching tank with oxalic acid, stirring and leaching, and performing liquid-solid separation after the leaching process is finished to obtain a leaching solution and leaching residues; performing illumination treatment on the leaching solution to obtain a light yellow precipitate and an illuminated solution; cyaniding and leaching the leaching residue, and performing liquid-solid separation after the leaching process is finished to obtain gold-containing pregnant solution; in the invention, oxalic acid is added to utilize C2O4 2‑For Fe3+Strong complexation enables hematite in the secondary calcine to be leached in the form of an iron oxalate complex, the iron leaching speed is high, the iron leaching rate is high, the energy consumption in the leaching process is low, and the industrialization is easy to realize; by applying light to the leach solutionTreating to obtain ferrous oxalate and recycling part of oxalic acid to realize the recycling of iron, the recycling of part of leaching agent oxalic acid and the recycling of system water; cyaniding the iron-removed slag to extract gold, thereby effectively improving the leaching rate of gold.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of metallurgical secondary resources, in particular to a method for leaching coated hematite in secondary calcine by using oxalic acid.
Background
Along with the large-scale exploitation of gold ore resources, the easily-treated gold ore resources are gradually exhausted, and the research on gold extraction processes of refractory gold ores, particularly arsenic-containing gold ores, is increasingly and widely concerned by people; the arsenious gold ore reserves in China are rich and account for over 1/3 of the gold reserves in China, and the arsenious gold ore reserves become an important raw material for gold ore production. Because the gold in the arsenious gold ore is closely symbiotic with arsenopyrite, and the gold exists in the form of fine grains in the ore and belongs to the refractory gold ore, the gold ore is generally subjected to pre-oxidation treatment. The best pretreatment method in the industry at present is a two-stage roasting method, namely, one-stage anoxic magnetization roasting for dearsenification, and two-stage oxidation roasting for desulfurization to obtain two-stage roasted sand, and the two-stage roasted sand is cyanided for gold leaching, so that the gold cyaniding leaching rate is greatly improved compared with the conventional cyaniding leaching rate. However, the arsenic-containing gold concentrate inevitably forms part of hematite to secondarily coat gold in the two-stage roasting process, so that the cyaniding leaching rate of gold in the two-stage roasted product is only about 80-85%, the gold content in cyaniding tailings is too high, generally is 7-15 g/t, the effective recovery of the gold cannot be realized, the resource waste is serious, and the economic benefit of enterprises is poor or even loss.
In the prior art, a sulfuric acid high-temperature curing-water leaching method, a sulfuric acid high-temperature leaching reduction method, a sub-molten salt method, a calcine water quenching method and a fine grinding method are often adopted to destroy hematite coated with gold in second-stage calcine; the defects of the sulfuric acid high-temperature curing-water leaching method, the sulfuric acid high-temperature leaching-immersion iron sheet reduction method and the sulfuric acid leaching copper powder reduction method are that the sulfuric acid concentration is large, the acid consumption is large, the equipment corrosion is serious, the purification process of preparing the iron chemical product by using the leaching solution is complex, and the wastewater treatment cost is high; the sub-molten salt method requires high-temperature and high-pressure equipment, has high production cost, large investment and high requirement on the safety performance of the equipment; the leaching rate of gold in the second-stage calcine is not greatly improved by the water quenching method, the operation process is complex, and the water consumption is large; the fine grinding method can improve the leaching rate of gold to a certain extent, but the effect is not good enough, and the fine grinding cost is high. At present, none of these methods is industrially applied.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a method for leaching gold hematite wrapped in secondary calcine by using oxalic acid, which aims to solve the technical problems of high acid consumption, high treatment temperature, complex operation process and high cost in the prior art of destroying the hematite structure in the secondary calcine.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a method for coating hematite in secondary calcine by using oxalic acid leaching, which comprises the following steps:
step 1, adding oxalic acid into a leaching tank;
step 2, adding the second-stage calcine and water into a leaching tank with oxalic acid, stirring and leaching, and performing liquid-solid separation after the leaching process is finished to obtain a leaching solution and leaching residues;
step 3, performing illumination treatment on the leaching solution in the step 2 to obtain a light yellow precipitate and an illuminated solution;
and 4, cyaniding and leaching the leaching residue obtained in the step 2, and performing liquid-solid separation after the leaching process is finished to obtain gold-containing pregnant solution and iron-removal cyaniding tailings.
Furthermore, the molar mass of the added oxalic acid is 3.5 to 4.5 times of the molar mass of the total iron in the second-stage calcine to be treated.
Further, in step 2, the liquid-solid ratio of the secondary calcine to water is (12-15) m L/1 g.
Further, in the step 2, the stirring leaching time is 3-5h, the leaching temperature is 70-95 ℃, and the stirring speed is 400-.
Further, in the step 3, the leachate is subjected to illumination treatment by using sunlight or ultraviolet light, and the illumination treatment time is 3-10 hours.
Further, in the step 3, in the cyaniding gold leaching process, leaching residues are added into a sodium cyanide solution, stirred for leaching, filtered and separated to obtain gold-containing pregnant solution and iron-removal cyaniding tailings; wherein the concentration of the sodium cyanide solution is 8-10kg/tMineThe pH value is 10-11.5.
Further, zinc powder replacement or activated carbon adsorption is adopted to replace the gold-containing pregnant solution to respectively obtain gold mud or gold-loaded activated carbon; the iron-removing cyaniding tailings are piled up or used as a slagging solvent in the copper pyrometallurgy process.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for leaching coated hematite in secondary calcine by oxalic acid, which utilizes C2O4 2-For Fe3+Strong complexation, so that the hematite in the second-stage calcine is leached in the form of an iron oxalate complex; the speed of leaching the hematite coated with gold in the secondary calcine by the oxalic acid is higher, the iron leaching rate is high, and the iron leaching process is simple; the main component of the leachate is ferric oxalate complex with light absorption, and the iron in the ferric oxalate complex is treated by light so as to be FeC2O4·2H2The precipitate is separated in the form of O, part of oxalic acid is remained in the solution after the illumination, and the solution can return to the process of leaching hematite in the second-stage calcine, so that the recovery of iron in the leaching solution and the recycling of part of oxalic acid are realized; and the gold leaching rate of the second-stage roasted product after iron removal is effectively improved by adopting a cyaniding method to leach gold.
Furthermore, when the molar mass of the oxalic acid serving as the leaching agent is 3.5 to 4.5 times of the molar mass of the total iron in the second-stage calcine, the Fe (C) can be ensured to be used as the hematite2O4)2 -And Fe (C)2O4)3 3-The hematite is leached in a form, the leaching effect of the hematite is better, and the iron leaching speed is higher.
Furthermore, when the pH value of the oxalic acid is lower, hematite in the second-stage calcine is leached, part of the oxalic acid exists in the form of oxalic acid molecules and does not participate in complexing leaching the hematite in the second-stage calcine, and the part of the oxalic acid only plays a role in adjusting the pH value of a system; at lower leach pH values, hematite is dominated by Fe (C)2O4)+And Fe (C)2O4)2 -Leaching in two ion forms, wherein the hematite is Fe (C) along with the increase of the pH value of a leaching system2O4)+The form leaching is gradually reduced, and Fe (C)2O4)2 -And Fe (C)2O4)3 3-The leaching is gradually increased, and the pH value is continuously increased to form Fe (C)2O4)2 -Less leaching in form, but as Fe (C)2O4)3 3-Therefore, the liquid-solid ratio of the secondary calcine and water is controlled to be (12-15) m L/1 g, which is beneficial to improving the pH value of a leaching system and leading the hematite to be mainly Fe (C)2O4)2 -And Fe (C)2O4)3 3-The two forms of leaching can improve the leaching rate of the iron in the second-stage calcine.
Furthermore, the hematite in the second-stage calcine is leached by oxalic acid, iron exists in the leachate as an iron oxalate complex with light absorption, the leachate is subjected to sunlight or ultraviolet light illumination treatment, the leachate treatment process is simple, and iron recovery, part of oxalic acid recycling and system water recycling can be realized.
The invention has simple process flow and lower energy consumption and production cost; is not only suitable for the iron removal of the two-stage calcine but also suitable for the iron removal of the calcine cyanidation tailings.
Drawings
FIG. 1 is a microscopic morphology of the precipitate obtained after the leachate is subjected to the static sunlight irradiation treatment in example 1;
FIG. 2 is a microscopic morphology of the precipitate obtained from the leaching solution treated by ultraviolet light irradiation at different stirring rates in example 2.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more apparent, the following geometric drawings and embodiments are further described in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a method for coating hematite in secondary calcine by using oxalic acid leaching, which comprises the following steps:
step 1, adding oxalic acid into a leaching tank, wherein the molar mass of the added oxalic acid is 3.5-4.5 times of the molar mass of total iron in the two-stage calcine to be treated;
step 2, adding the second-stage calcine and water into a leaching tank with oxalic acid according to the liquid-solid ratio of (12-15) m L/1 g, and leaching for 3-5h under stirring at the temperature of 70-95 ℃ and the stirring speed of 400-500 r/min;
step 3, soaking in the step 2 by adopting sunlight or ultraviolet lightPerforming light treatment on the effluent, performing liquid-solid separation after the light treatment for 3-10h, and separating to obtain light yellow solid precipitate and light-treated liquid, wherein the light yellow solid precipitate is FeC2O4·2H2O, returning the solution after illumination to the process of leaching hematite in the second-stage calcine, so as to realize the recycling of part of oxalic acid;
step 4, adopting sodium cyanide solution to carry out cyaniding gold leaching on the leaching residue in the step 2, wherein the using amount of the sodium cyanide is 8-10kg/tMineThe pH value is 10-11.5, the stirring leaching time is 48h, and liquid-solid separation is carried out after the leaching process is finished to obtain gold-containing pregnant solution and iron-removing cyaniding tailings; zinc powder replacement or activated carbon adsorption is adopted for the gold-containing pregnant solution to respectively obtain gold mud or gold-loaded activated carbon; the iron-removing cyaniding tailings can be stockpiled or used as a solvent for copper smelting or can be sold to a cement factory for use as a batching material for producing cement according to the gold grade in the iron-removing cyaniding tailings.
The invention provides a method for leaching coated hematite in secondary calcine by oxalic acid, which utilizes C2O4 2-For Fe3+Strong complexation enables the hematite in the secondary calcine to be leached in the form of an iron oxalate complex, and the hematite coated with gold in the oxalic acid leached secondary calcine has the characteristics of high iron leaching speed, high iron leaching rate and simple leaching process; the leaching solution is treated by light to lead the iron in the leaching solution to be FeC2O4·2H2The precipitate is separated in the form of O, part of oxalic acid is remained in the solution after the illumination, and the solution can return to the process of leaching hematite in the second-stage calcine, so that the recovery of iron in the leaching solution and the recycling of part of oxalic acid are realized; because most of iron is removed, gold wrapped by hematite in the secondary calcine is exposed, and gold is extracted by adopting a cyanidation method, so that the leaching rate of gold can be effectively improved.
Example 1
Embodiment 1 provides a method for leaching coated hematite in secondary calcine by oxalic acid, which comprises the following steps:
step 1, adding oxalic acid into a leaching tank, wherein the molar mass of the added oxalic acid is 3.5 times of the molar mass of total iron in the two-stage calcine to be treated;
step 2, adding the second-stage calcine and water into a leaching tank with oxalic acid according to the liquid-solid ratio of 12m L/1 g, stirring and leaching for 5 hours at 70 ℃, wherein the stirring speed is 500r/min, and performing liquid-solid separation after the leaching process is finished to obtain a leaching solution and leaching slag, wherein the gold content in the second-stage calcine is 57.50g/t, and the hematite content is 25.12%;
and 3, performing sunlight static illumination treatment on the leachate obtained in the step 2 for 10 hours, performing solid-liquid separation after the illumination process is finished to obtain a light yellow solid precipitate and an illuminated liquid, and returning the illuminated liquid to the process of leaching hematite in the two sections of calcines by oxalic acid.
Step 4, cyaniding the leaching residues in the step 2 for gold leaching, wherein the gold leaching conditions are as follows: the dosage of sodium cyanide is 10kg/tMineThe pH value is 11.2, the stirring leaching time is 48h, and liquid-solid separation is carried out after the leaching process is finished to obtain gold-containing pregnant solution and iron-removing cyaniding tailings; zinc powder replacement or activated carbon adsorption is adopted for the gold-containing pregnant solution to respectively obtain gold mud or gold-loaded activated carbon; analyzing the gold content in the slag, and storing the iron-removing cyaniding tailings in a disposal mode according to the gold grade in the iron-removing cyaniding tailings, or using the iron-removing cyaniding tailings as a solvent for copper smelting or selling the iron-removing cyaniding tailings to a cement factory for use as an ingredient for producing cement.
In example 1, according to the method for leaching the coated gold hematite in the secondary calcine by using oxalic acid, after the secondary calcine is leached by using oxalic acid for iron leaching, the leaching rate of iron reaches 75.61%, and the cyaniding leaching rate of the iron removing slag is improved by 9.25% compared with the cyaniding leaching rate of gold in the two stages of calcine before iron removal; and (3) performing light treatment on the leaching solution in the step (3), wherein the oxidation rate of oxalic acid in the leaching solution is 42.62%, and the precipitation rate of iron is 100%.
In the process of treating the leachate by using sunlight static illumination in the embodiment 1, the color of the leachate is gradually changed into brownish red from emerald green and then into light red until the leachate is colorless finally; as can be seen from the attached FIG. 1, the precipitate generated in the illumination process is light yellow regular columnar FeC2O4·2H2O。
Example 2
Embodiment 2 provides a method for leaching coated hematite in secondary calcine by oxalic acid, which comprises the following steps:
step 1, adding oxalic acid into a leaching tank, wherein the molar mass of the added oxalic acid is 4.5 times of the molar mass of total iron in the two-stage calcine to be treated;
step 2, adding the second-stage calcine and water into a leaching tank added with oxalic acid according to a liquid-solid ratio of 15m L/1 g, stirring and leaching for 3 hours at 95 ℃, wherein the stirring speed is 450r/min, and after the leaching process is finished, performing liquid-solid separation to obtain a leaching solution and leaching slag, wherein the weight of the second-stage calcine is 50g, the volume of the water is 750m L, the content of gold in the second-stage calcine is 47.49g/t, and the content of hematite reaches 30.17%;
step 3, averagely dividing the leaching solution in the step 3 into 6 parts, wherein 1 part of the leaching solution is subjected to ultraviolet static illumination treatment for 6.5 hours; the other 5 parts are respectively subjected to ultraviolet light illumination treatment under magnetic stirring at different rotating speeds, and the ultraviolet light illumination time is 3 hours; and (3) carrying out liquid-solid separation after the ultraviolet light illumination process is finished to obtain a light yellow solid precipitate and an illuminated liquid, and returning the illuminated liquid to the process of leaching hematite in the two sections of calcines by oxalic acid. Wherein, in the ultraviolet irradiation process, the photocurrent is 14A, and the light source area is 191cm2；
Step 4, cyaniding the leaching residues in the step 2 for gold leaching, wherein the gold leaching conditions are as follows: the amount of sodium cyanide is 8kg/tMineThe pH value is 10.6, the stirring leaching time is 48 hours, and liquid-solid separation is carried out after the leaching process is finished to obtain gold-containing pregnant solution and iron-removing cyaniding tailings; zinc powder replacement or activated carbon adsorption is adopted for the gold-containing pregnant solution to respectively obtain gold mud or gold-loaded activated carbon; analyzing the gold content in the slag, and storing the iron-removing cyaniding tailings in a disposal mode according to the gold grade in the iron-removing cyaniding tailings, or using the iron-removing cyaniding tailings as a solvent for copper smelting or selling the iron-removing cyaniding tailings to a cement factory for use as an ingredient for producing cement.
In example 2, the method for leaching the gold hematite wrapped in the secondary calcine by using oxalic acid according to the embodiment is used for leaching the hematite in the secondary calcine, the iron removal rate of the secondary calcine reaches 77.80%, iron removal residues are cyanided to leach gold, and the gold leaching rate is improved by 9.74% compared with that before iron removal; and (3) treating the leachate obtained in the step (3) by adopting ultraviolet light, wherein the oxalic acid oxidation rate in the leachate is 8.71-12.86%, and the iron precipitation rate is 100%.
In the embodiment 2, during the process of treating the leachate by sunlight static illumination, the color of the leachate gradually changes from emerald green to brownish red and then to light red until the leachate is colorless, and the light yellow solid precipitate generated in the illumination process is FeC2O4·2H2O。
In example 2, the leachate is subjected to dynamic ultraviolet light irradiation treatment, and the light yellow solid precipitate FeC can be seen from the attached figure 22O4·2H2The regular columnar crystal structure of O is destroyed, and the larger the stirring speed, the larger the destruction degree of the crystal structure of the precipitate and the smaller the particle size.
Example 3
Embodiment 3 provides a method for leaching coated hematite in secondary calcine by oxalic acid, which comprises the following steps:
step 1, adding oxalic acid into a leaching tank, wherein the molar mass of the added oxalic acid is 4.02 times of the molar mass of total iron in the two-stage calcine to be treated;
step 2, adding the second-stage calcine and water into a leaching tank with oxalic acid according to a liquid-solid ratio of 14m L/1 g, stirring and leaching for 4 hours at 80 ℃, wherein the stirring speed is 450r/min, and performing liquid-solid separation after the leaching process is finished to obtain a leaching solution and leaching residues, wherein the gold content in the second-stage calcine is 50.33g/t, and the hematite content reaches 27.65%;
and 3, performing sunlight static illumination treatment on the leachate obtained in the step 2 for 9 hours, performing solid-liquid separation on the illuminated liquid to obtain a light yellow solid precipitate and an illuminated liquid, and returning the illuminated liquid to the process of leaching the hematite in the two sections of calcines by oxalic acid.
Step 4, cyaniding and leaching gold from the leaching residue in the step 2, wherein the leaching conditions are as follows: the amount of sodium cyanide used was 9.3kg/tMineThe pH value is 11.5, the stirring leaching time is 48 hours, and liquid-solid separation is carried out after the leaching process is finished to obtain gold-containing pregnant solution and iron-removing cyaniding tailings; zinc powder replacement or activated carbon adsorption is adopted for the gold-containing pregnant solution to respectively obtain gold mud or gold-loaded activated carbon; analyzing the gold content in the slag, and removing iron and cyaniding tailThe slag can be stockpiled or used as a solvent for copper smelting or sold to a cement plant for being used as a batching material for producing cement according to the grade of gold in the slag.
In example 3, by using the method for leaching the coated hematite in the secondary calcine by using oxalic acid described in this example, the iron removal rate of the secondary calcine reaches 75.02%; the cyaniding leaching rate of the leaching residue is improved by 10.07 percent compared with the cyaniding leaching rate of gold in the second-stage calcine; and (3) performing sunlight static illumination treatment on the leachate obtained in the step (3), wherein the oxalic acid oxidation rate is 40.07%, and the iron precipitation rate is 100%.
The above description is only illustrative of the preferred embodiments of the present invention, and any structural changes, improvements, modifications, etc. made without departing from the principle of the present invention are deemed to be within the scope of the present invention.
Claims (7)
1. A method for leaching coated hematite in secondary calcine by using oxalic acid is characterized by comprising the following steps:
step 1, adding oxalic acid into a leaching tank;
step 2, adding the second-stage calcine and water into a leaching tank with oxalic acid, stirring and leaching, and performing liquid-solid separation after the leaching process is finished to obtain a leaching solution and leaching residues;
step 3, performing illumination treatment on the leaching solution in the step 2 to obtain a light yellow precipitate and an illuminated solution;
and 4, cyaniding and leaching the leaching residue obtained in the step 2, and performing liquid-solid separation after the leaching process is finished to obtain gold-containing pregnant solution and iron-removal cyaniding tailings.
2. The method for leaching the coated aurite in the secondary calcine by using oxalic acid as claimed in claim 1, wherein the molar mass of the added oxalic acid is 3.5-4.5 times of the molar mass of the total iron in the secondary calcine to be treated.
3. The method for leaching the coated hematite from the secondary calcine by using oxalic acid as claimed in claim 1, wherein the liquid-solid ratio of the secondary calcine to water in step 2 is (12-15) m L/1 g.
4. The method for leaching the gold hematite coated in the secondary calcine by using the oxalic acid as claimed in claim 1, wherein the agitation leaching time in the step 2 is 3-5h, the leaching temperature is 70-95 ℃, and the agitation speed is 400-500 r/min.
5. The method for leaching coated hematite in secondary calcine by using oxalic acid according to claim 1, wherein in step 3, the leachate is subjected to light treatment by using sunlight or ultraviolet light, and the light treatment time is 3-10 h.
6. The method for leaching the gold-coated hematite in the secondary calcine by using oxalic acid according to claim 1, wherein in the step 3, in the cyaniding gold leaching process, leaching residues are added into a sodium cyanide solution, stirred for leaching, filtered and separated to obtain a gold-containing pregnant solution and iron-removal cyaniding tailings; wherein the concentration of the sodium cyanide solution is 8-10kg/tMineThe pH value is 10-11.5.
7. The method for leaching coated gold hematite in secondary calcine by using oxalic acid as claimed in claim 1, wherein the gold-containing pregnant solution is replaced by zinc powder or adsorbed by activated carbon to obtain gold mud or gold-loaded activated carbon, respectively; the iron-removing cyaniding tailings are piled up or used as a slagging solvent in the copper pyrometallurgy process.
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