CN109663663B - Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization - Google Patents

Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization Download PDF

Info

Publication number
CN109663663B
CN109663663B CN201910057647.0A CN201910057647A CN109663663B CN 109663663 B CN109663663 B CN 109663663B CN 201910057647 A CN201910057647 A CN 201910057647A CN 109663663 B CN109663663 B CN 109663663B
Authority
CN
China
Prior art keywords
mineral
oxidized
minerals
heavy metal
sulfide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910057647.0A
Other languages
Chinese (zh)
Other versions
CN109663663A (en
Inventor
刘殿文
李佳磊
章晓林
李健民
刘瑞增
刘思言
蔡锦鹏
贾晓东
申培伦
赵文娟
苏超
曹阳
李江丽
杨升旺
裴斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kunming University of Science and Technology
Original Assignee
Kunming University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kunming University of Science and Technology filed Critical Kunming University of Science and Technology
Priority to CN201910057647.0A priority Critical patent/CN109663663B/en
Publication of CN109663663A publication Critical patent/CN109663663A/en
Application granted granted Critical
Publication of CN109663663B publication Critical patent/CN109663663B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets

Landscapes

  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for extracting a vulcanized product after vulcanization of a pure mineral of a heavy metal oxidized mineral, which comprises the steps of firstly determining the vulcanization condition of the pure mineral of the heavy metal oxidized mineral, vulcanizing under the determined vulcanization condition to obtain vulcanized ore pulp, standing the ore pulp, removing supernatant, then adding an antioxidant selective dissolving agent into a precipitate, dissolving the heavy metal oxidized mineral in the precipitate by using the selective dissolving agent, and enabling sulfide generated after vulcanization of the oxidized mineral to be incapable of being dissolved and still exist in a solid form to obtain a solid-liquid mixture; carrying out centrifugal cleaning on the obtained solid-liquid mixture for more than one time, and drying the final bottom slurry to obtain a sulfide product after the pure mineral of the heavy metal oxidized mineral is vulcanized; the invention can quickly, economically and simply extract the sulfide products of various oxidized minerals, test and analyze the extracted sulfide products, further solve the scientific problem in the field of oxidized ore sulfide flotation, optimize the sulfide flotation process and efficiently develop the oxidized minerals in an environment-friendly way.

Description

Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization
Technical Field
The invention relates to a method for extracting substances, in particular to a method for extracting a sulfide product of a heavy metal oxidized mineral after pure mineral vulcanization, and belongs to the technical field of flotation.
Background
Ores such as copper oxide, lead, zinc, cobalt and the like are important mineral resources, and the efficient utilization of the ores has important significance for guaranteeing the safety of resources and meeting the requirements of nonferrous metals. Flotation is the most economic and effective means for recovering the enriched minerals at present. Compared with corresponding sulfide minerals, the oxide minerals have large surface wettability, are relatively difficult to directly float, and need fatty acid or fatty amine medicaments with long carbon chains, but the medicaments have poor selectivity and large dosage. In industrial practice, a sulfidation flotation method is generally adopted to recover oxidized minerals, sulfidation is a key link of the process, and the effect of sulfidation directly influences flotation indexes.
The most common sulfidation method used in industrial practice is the addition of sodium sulfide solution to the pulp, also known as surface sulfidation, by the mechanism: the method is characterized in that sulfur ions in ore pulp and mineral particles are subjected to multiphase chemical reaction, metal sulfide (MeS) is generated and covered on the surface layer of oxidized minerals to form an oxidized ore/sulfide multiphase composite structure, as shown in figure 1, sulfide has strong surface hydrophobicity and stronger adsorption capacity on a collecting agent, and sulfide can activate flotation of the oxidized minerals.
In the concentration range of the flotation reagent, the amount of the sulfide product generated after vulcanization is very small, and due to the structural characteristics shown in figure 1, the travel of X rays, infrared light and the like in the sulfide product is short, and the signal generated after action is weak; the effective signals of the sulfide are difficult to collect by using analytical test means such as ordinary powder diffraction, infrared spectroscopy and the like, so that the phase, the physical and chemical properties and the like of the sulfide product cannot be effectively characterized in the past, and the research on the sulfide flotation of the oxidized minerals is slow for many years.
The sulfuration is a key link for flotation and recovery of minerals such as copper oxide, lead, zinc and the like, and the quality of the sulfuration directly affects the flotation indexes, so that effective information is obtained by extracting surface sulfuration products of heavy metal oxidized minerals such as copper, lead, zinc and the like and characterizing the physical and chemical properties of the heavy metal oxidized minerals through a modern analysis and test means, and the method has important guiding significance for industrial practice of the sulfuration and flotation of the oxidized minerals.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a method for extracting the sulfide product of the heavy metal oxidized mineral after pure mineral vulcanization, and the method analyzes and detects various physical and chemical properties of the extracted sulfide product, such as phase, elements, valence state and the like to obtain effective information, thereby having important guiding significance for the industrial practice of the sulfide flotation of the heavy metal oxidized mineral.
In order to achieve the effect of the technical scheme, the technical scheme of the invention is as follows: a method for extracting a sulfide product of a pure mineral of a heavy metal oxidized mineral after vulcanization comprises the following specific steps:
(1) firstly, carrying out a vulcanization flotation condition test on pure minerals of heavy metal oxidized minerals to determine the vulcanization conditions of the pure minerals of the heavy metal oxidized minerals, wherein the heavy metal oxidized minerals are copper oxidized minerals, lead oxidized minerals or zinc oxidized minerals, the copper oxidized minerals are malachite, pinosylite or chalcopyrite, the lead oxidized minerals are white lead minerals or lead alum, and the zinc oxidized minerals are calamine or calamine;
the conditions in the sulfuration flotation condition test comprise the conditions of ore pulp pH value, vulcanizing agent type and dosage, vulcanizing agent adding mode, vulcanizing time, vulcanizing temperature, additive type (ammonium salt and ethylenediamine) and the like.
(2) Carrying out vulcanization flotation on pure minerals of heavy metal oxidized minerals under the optimal vulcanization condition to obtain vulcanized ore pulp, standing the ore pulp for 1-3 min to obtain supernatant and precipitate, removing the supernatant, adding a selective dissolving agent and an antioxidant into the precipitate, dissolving the heavy metal oxidized minerals in the precipitate by using the selective dissolving agent, wherein sulfides generated by oxide vulcanization cannot be dissolved and still exist in a solid form to obtain a solid-liquid mixture;
(3) and (3) performing centrifugal cleaning on the solid-liquid mixture obtained in the step (2) for more than one time, and drying the bottom slurry subjected to centrifugal cleaning at low temperature to obtain a sulfide product obtained after the pure mineral of the heavy metal oxidized mineral is vulcanized.
The antioxidant in the step (2) is one or a mixture of more of ascorbic acid, hydroxylamine sulfate and sodium sulfite, and the antioxidant prevents oxidation of vulcanization products.
When the copper oxide mineral is malachite or chalcopyrite, the corresponding selective dissolvent is single dilute sulfuric acid or a mixture of ammonia water and ammonium carbonate, and when the copper oxide mineral is peacock stone, the corresponding selective dissolvent is dilute sulfuric acid and NH4HF2The mixture of (1), when lead oxide mineral is plumbite, corresponding selective dissolving agent is the mixture of acetic acid and sodium acetate, when lead oxide mineral is plumbite, corresponding selective dissolving agent is sodium chloride, when zinc oxide mineral is calamine, corresponding selective dissolving agent is the mixture of acetic acid and sodium acetate or the mixture of aqueous ammonia and ammonium carbonate, zinc oxide mineral be hemimorphite, corresponding selective dissolving agent is aqueous ammonia, ammonium carbonate and NH4HF2A mixture of (a).
The drying temperature in the step (3) is 30-60 ℃.
Repeating the steps (1) to (3) for more than one time, mixing the vulcanization products extracted for more than one time, and carrying out analysis test.
The invention has the beneficial effects that:
the invention can quickly, economically and simply extract the surface sulfide products of various oxidized ore pure minerals after vulcanization, and can carry out various test analyses on the extracted sulfide products to obtain the crystalline phase, the grain size, the crystallinity and other various physicochemical information of the sulfide products, thereby further solving the existing scientific problems in the field of oxidized ore sulfide flotation, optimizing the sulfide flotation process of copper oxide lead zinc ores and efficiently developing the oxidized minerals in an environment-friendly way.
Drawings
FIG. 1 is a schematic diagram of oxide ore sulfidation;
FIG. 2 is a schematic process flow diagram of the present invention;
FIG. 3 is an XRD pattern of a sulfidic product of the white lead ore of example 1 of the present invention;
FIG. 4 is a graph showing the relationship between the usage amount of sodium sulfide in malachite and the flotation recovery rate in example 2 of the present invention;
figure 5 is an XRD pattern of a cured product of malachite of example 2 of the invention.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1: the white lead ore is the lead oxide mineral with the most industrial recovery value, the yellow sulfur method is used for recovering the lead oxide ore industrially at present, and the vulcanization is an important link of the process. The reaction formula of the sodium sulfide-sulfidic galena can be represented by the formula (1):
PbCO3/PbCO3 +Na2S →PbCO3/PbS +Na2CO3 (1)
scholars at home and abroad do a great deal of research work in the field of sulfidation flotation of white lead ore, but still some unsolved problems exist: as mentioned above, due to the limitation of XRD instrument sensitivity, no diffraction signal of PbS (lead sulfide) can be detected in the range of the amount of sodium sulfide used for flotation; in order to determine the phase of the vulcanizate, researchers have typically added extremely large amounts of vulcanizing agents. But the sulfide flotation behavior of the oxidized ore is closely related to the amount of sodium sulfide, and the recovery rate of the oxidized ore increases along with the increase of the amount of sodium sulfide within a certain sodium sulfide amount range; when the amount of sodium sulfide exceeds the optimum amount, the recovery rate decreases as the amount of sodium sulfide increases. Therefore, the sulfide product phase at the optimal sodium sulfide dosage is determined, the physicochemical properties of the sulfide product phase are explored, and the method has positive significance for the flotation practice of the lead oxide ore. This example describes a method for extracting a pure mineral sulfide product of galena, and the phase of the sulfide product is characterized;
as shown in fig. 2, the extraction steps of the pure mineral surface sulfidation product of the galena are as follows:
(1) firstly, carrying out a sulfidation flotation condition test on the pure minerals of the white lead ore to determine the optimal sulfidation conditions of the pure minerals of the white lead ore;
research on flotation behavior of the pure lead ore:
the influence of the amount of sodium sulfide on the flotation behavior of the white lead ore is researched by using a single bubble tube with the volume of 50mL, the amount of the pure ore of the white lead ore is 0.5000g each time, the temperature of ore pulp is room temperature, the pH value is kept within the range of 10.20 +/-0.10, the collecting agent is butyl xanthate, and the amount of the butyl xanthate is 30 mg/L.
(2) Selecting a mixed solution of acetic acid and sodium acetate as a selective dissolving agent according to the property of the white lead ore, using ascorbic acid as an antioxidant to prevent oxidation of a vulcanized product, preparing 500mL of a mixed solution of acetic acid, sodium acetate and ascorbic acid as an antioxidant selective dissolving agent, wherein the mass concentration of acetic acid in the mixed solution is 12%, the concentration of sodium acetate is 120g/L, the concentration of ascorbic acid is 40g/L, and the mixed solution is called 0.5g of the white lead ore, vulcanizing the white lead ore under the condition that the amount of sodium sulfide is 75mg/L according to the flotation process, standing ore pulp for 1min after vulcanization to obtain a supernatant and a precipitate, then removing the supernatant, adding 30mL of the antioxidant selective dissolving agent into a beaker, reacting for 3h, dissolving the white lead ore in the precipitate by the selective dissolving agent, and enabling sulfide generated after the white lead ore vulcanization to be incapable of being dissolved and still exist in a solid form, obtaining a solid-liquid mixture;
(3) transferring the solid-liquid mixture in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; drying the bottom slurry after 8 times of cleaning at 30 ℃ to obtain a sulfide product purified product;
repeating the steps (1) - (3) for 5 times under the same conditions, uniformly mixing the 5 purified products, and using the obtained extract for various analysis tests, wherein the XRD (X-ray diffraction) spectrum of the purified product is consistent with the standard diffraction spectrum of lead sulfide (galena phase), and the result shows that the purified vulcanized product has high purity and only contains a very small amount of impurities.
Example 2: malachite is the most industrially significant copper oxide mineral, and the copper oxide mineral resources are generally recovered by sulfuration flotation in industry, and the sulfuration flotation of copper oxide ores can be traced to the early 20 th century; in 1970, Castro et al demonstrated by XRD that the sulfidation product of black copper ore was CuS (covellite), after which they proposed the sulfidation reaction equation for malachite (equation 2), after which Zhou et al proposed equation (3) to explain the copper sulfide colloid generation phenomenon in the sulfidation flotation of malachite; thereafter, it was generally accepted that the malachite vulcanizate product was CuS (covellite). Liu palatine et al identified the sulfidation product as Cu by XRD under conditions of very excessive sodium sulfide7S4(Roxbyite). This example describes the extraction of a pure mineral sulphide of malachite, and identifies the phase of the sulphide:
CuCO3Cu(OH)2+HS- +OH- =Cu(OH)2CuS +CO3 2-+H2O (2)
CuCO3Cu(OH)2+HS- =CuS+Cu2++2OH-+HCO3- (3)
the extraction steps of the pure mineral surface sulfuration products of malachite are as follows:
(1) research on sulfuration flotation behavior of malachite:
the influence of the amount of sodium sulfide on the flotation behavior of the malachite is researched by using a single bubble tube with the volume of 50mL, 0.5g of the malachite pure mineral is used in each experiment, butyl xanthate is used as a collecting agent, and the amount of the butyl xanthate is 10-4mol/L, pH is kept within the range of 9.00 +/-0.10, and the vulcanization time is 3 min; the results are shown in the figure4, as can be seen from FIG. 4, the amount of sodium sulfide used was 5X 10-4The highest recovery rate is obtained when the mol/L is higher than the standard.
(2) According to the property of the malachite, selecting a sulfuric acid solution as a selective dissolvent, using ascorbic acid as an antioxidant to prevent the oxidation of a vulcanization product, preparing 500mL of antioxidant selective dissolvent, wherein the sulfuric acid concentration is 0.5 percent, the ascorbic acid concentration is 40g/L, which is called 0.5g of malachite, and according to the flotation flow, the using amount of sodium sulfide is 5 multiplied by 10-4Vulcanizing the mixture under the condition of mol/L, standing oxidized ore pulp for 2min after vulcanization, and then removing supernatant; adding 20mL of antioxidant selective dissolving agent into a beaker, reacting for 1h, completely dissolving the malachite in the precipitate by using the selective dissolving agent, and allowing the sulfide product to exist in a solid state;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; drying the bottom slurry after being washed by the washing solution 6 at 40 ℃ to obtain a purified product of the vulcanized product;
repeating the steps (1) - (3) for 8 times under the same condition, and mixing the 8 purified products uniformly. The purified product was analyzed by sexual XRD to determine the phase of the sulfide product, and the result is shown in FIG. 5, from which it is known that the malachite sulfide product is mainly Cu7S4(Roxbyite), and a small amount of Cu31S16(Djuleite)。
The embodiment can quickly, economically and simply extract the sulfide products on the surfaces of the oxidized minerals, and can carry out various analysis tests on the sulfide products to obtain the physical and chemical information of the sulfide products.
Example 3: the extraction steps of the lead vanadium pure mineral surface sulfide product are as follows:
(1) research on lead-vanadium sulfide flotation behavior:
the influence of the amount of sodium sulfide on the flotation behavior of the lead alum is researched by using a single bubble tube with the volume of 50mL, 0.5g of pure lead alum mineral is used in each experiment, the butyl xanthate is used as a collecting agent, the amount is 50mg/L, the pH value is kept within the range of 9.00 +/-0.10, and the vulcanization time is 3 min; the result of the flotation test shows that the lead alum has the highest recovery rate when the dosage of the sodium sulfide is 100 mg/L.
(2) According to the properties of lead and vanadium, a sodium chloride solution is selected as a selective dissolving agent, sodium sulfite is used as an antioxidant to prevent oxidation of a sulfide product, and 500mL of antioxidant selective dissolving agent is prepared, wherein the concentration of sodium chloride is 250g/L, and the concentration of ascorbic acid is 40 g/L. Weighing 0.5g of lead and vanadium, vulcanizing the lead and vanadium under the condition that the using amount of sodium sulfide is 100mg/L according to the flotation process, standing oxidized ore pulp for 3min after vulcanization, and then removing supernatant; adding 30mL of antioxidant selective dissolving agent into a beaker, reacting for 3h, completely dissolving lead and vanadium in the precipitate by using the selective dissolving agent, and enabling the sulfide product to exist in a solid state;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; and 6, drying the bottom slurry at 50 ℃ after cleaning to obtain a sulfide product purified product.
Example 4: the extraction of the pure mineral surface sulphidic product of peacock stone is as follows:
(1) study of sulfuration flotation behavior of peacock stone:
the influence of the amount of sodium sulfide on the floatation behavior of the peacock stone under the action of the ethylenediamine phosphate is researched by using a single bubble tube with the volume of 50mL, 0.5g of the pure peacock stone mineral is used in each experiment, and the amount of the ethylenediamine phosphate is 0.5 multiplied by 10-3mol/L, the dosage of isoamyl xanthate is 5 multiplied by 10-3At mol/L, the effect of sodium sulfide dosage on the floatation of the peacock stone was studied. When the amount of sodium sulfide is 1.5X 10-3The recovery of the peacock stone reaches the maximum value at mol/L.
(2) Selecting dilute sulphuric acid + NH according to the properties of the peacock stone4HF2For selective dissolvent, using mixed solution of hydroxylamine sulfate and sodium sulfite as antioxidant to prevent oxidation of sulfuration product, 500mL antioxidant selective dissolvent is prepared, wherein dilute sulfuric acid concentration is 5%, NH4HF2The concentration is 5%, the concentration of hydroxylamine sulfate and sodium sulfite is 30g/L (the ratio of the hydroxylamine sulfate to the sodium sulfite is 1:1), and the concentration is 1.5 multiplied by 10-3Vulcanizing the oxidized ore pulp under the condition of mol/L mol/L, standing the oxidized ore pulp for 3min after vulcanization, and then removing supernatant; adding 30mL of antioxidant selective dissolving agent into a beaker, reacting for 5h, completely dissolving the deposit with the selective dissolving agent, and obtaining a vulcanized productIn solid form;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; and (4) drying the bottom slurry after being washed by the liquor 6 at the temperature of 60 ℃ to obtain a purified product of the vulcanized product.
Example 5: the extraction steps of the pure mineral surface sulfide product of the chalcopyrite are as follows:
the influence of the amount of sodium sulfide on the flotation behavior of the chalcopyrite is researched by using a single bubble tube with the volume of 50mL, 0.5g of pure chalcopyrite is used in each experiment, butyl xanthate is used as a collecting agent, the amount of the butyl xanthate is 2 multiplied by 10 mol/L, the pH value is kept within the range of 9.00 +/-0.10, and the vulcanization time is 5 min; the flotation experiment shows that the dosage of the sodium sulfide is 7.5 multiplied by 10-4The highest recovery rate is obtained when mol/L is used.
(2) According to the property of the chalcopyrite, a mixture of ammonia water and ammonium carbonate is selected as a selective dissolving agent, a sodium sulfite antioxidant is used for preventing oxidation of a sulfide product, and 500mL of an antioxidant selective dissolving agent is prepared, wherein the total ammonium concentration is 50%, and the ammonium-ammonia ratio is 1:1, the concentration of sodium sulfate is 40g/L, which is called 0.5g of chalcocite, according to the flotation process, the dosage of sodium sulfide is 7.5 multiplied by 10-4Vulcanizing the mixture under the condition of mol/L, standing oxidized ore pulp for 3min after vulcanization, and then removing supernatant; adding 30mL of antioxidant selective dissolving agent into a beaker, reacting for 90min, dissolving the chalcopyrite in the precipitate by using the selective dissolving agent, and enabling the sulfide product to exist in a solid state;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; and 6, drying the bottom slurry at 60 ℃ after cleaning to obtain a sulfide product purified product.
Example 6: the extraction steps of the pure mineral surface vulcanization products of the calamine are as follows:
the influence of the amount of sodium sulfide on the flotation of the calamine is researched by using a 40mL tank hanging machine, 2g of calamine is used in each experiment, dodecylamine is used as a collecting agent, and the amount of the dodecylamine is 1 multiplied by 10-3mol/L, and the vulcanization time is 5 min; as shown by flotation experiments, the highest recovery rate is achieved when the dosage of the sodium sulfide is 400 mg/L.
(2) According to the properties of the calamine, a mixture of ammonia water and ammonium carbonate is selected as a selective dissolving agent, ascorbic acid is used as an antioxidant to prevent oxidation of vulcanized products, and 500mL of antioxidant selective dissolving agent is prepared, wherein the total ammonium concentration is 50%, and the ammonium-ammonia ratio is 1:1, weighing 2g of calamine with the ascorbic acid concentration of 40g/L, vulcanizing the calamine according to the flotation process under the condition that the using amount of sodium sulfide is 400mg/L, standing oxidized ore pulp for 3min after vulcanization, and then removing supernatant; adding 30mL of antioxidant selective dissolving agent into a beaker, reacting for 90min, dissolving the calamine in the precipitate by the dissolving agent, and allowing the sulfide product to exist in a solid state;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; and (4) drying the bottom slurry after being washed by the liquor 6 at the temperature of 60 ℃ to obtain a purified product of the vulcanized product.
Example 7: the extraction steps of the pure mineral surface sulfide product of the hemimorphite are as follows:
(1) the influence of the amount of sodium sulfide on the flotation of the hemimorphite is researched by using a 40 mL-volume trough hanging machine, 2g of sodium sulfide is used in each experiment, dodecylamine is used as a collecting agent, the amount of sodium sulfide is 40mg/L, the vulcanization time is 5min, and the experiment shows that the amount of sodium sulfide is 8 multiplied by 10- 4mol/L has the highest recovery.
(2) Selecting ammonia water, ammonium carbonate and NH according to the properties of the hemimorphite4HF2The mixture of (a) is a selective dissolvent, hydroxylamine sulfate is used as an antioxidant to prevent oxidation of vulcanization products, 500mL of antioxidant selective dissolvent is prepared, wherein the total ammonium concentration is 50%, and the ammonium-ammonia ratio is 1:1, NH4HF2The concentration is 5 percent, the hydroxylamine sulfate concentration is 30g/L, 2g of hemimorphite is called, according to the flotation process, the sodium sulfide dosage is 8 multiplied by 10-4Sulfurizing under mg/L condition, standing oxidized ore pulp for 3min after sulfurization, and removing supernatant; adding 30mL of antioxidant selective dissolving agent into a beaker, reacting for 180min, dissolving hemimorphite in the precipitate by using the dissolving agent, and enabling the sulfide product to exist in a solid state;
(3) transferring the slurry in the beaker into a 50mL centrifuge tube, and repeatedly centrifuging and cleaning; and (4) drying the bottom slurry after being washed by the liquor 6 at the temperature of 60 ℃ to obtain a purified product of the vulcanized product.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.

Claims (3)

1. A method for extracting a sulfide product of a pure mineral of a heavy metal oxidized mineral after vulcanization is characterized by comprising the following specific steps:
(1) firstly, carrying out a vulcanization flotation condition test on pure minerals of heavy metal oxidized minerals to determine the vulcanization conditions of the pure minerals of the heavy metal oxidized minerals, wherein the heavy metal oxidized minerals are copper oxidized minerals, lead oxidized minerals or zinc oxidized minerals, the copper oxidized minerals are malachite, pinosylite or chalcopyrite, the lead oxidized minerals are white lead minerals or lead alum, and the zinc oxidized minerals are calamine or calamine;
(2) vulcanizing pure minerals of heavy metal oxidized minerals under the determined vulcanization condition to obtain vulcanized ore pulp, standing the ore pulp for 1-3 min to obtain supernatant and precipitate, removing the supernatant, adding an antioxidant selective dissolving agent into the precipitate, wherein the antioxidant selective dissolving agent is a mixed substance of an antioxidant and the selective dissolving agent, the antioxidant is one or a mixture of more of ascorbic acid, hydroxylamine sulfate and sodium sulfite, when the copper oxidized minerals are malachite or chalcopyrite, the corresponding selective dissolving agent is single dilute sulfuric acid or a mixture of ammonia water and ammonium carbonate, and when the copper oxidized minerals are peacock stones, the corresponding selective dissolving agents are dilute sulfuric acid and NH4HF2The mixture of (1), when lead oxide mineral is plumbite, corresponding selective dissolving agent is the mixture of acetic acid and sodium acetate, when lead oxide mineral is plumbite, corresponding selective dissolving agent is sodium chloride, when zinc oxide mineral is calamine, corresponding selective dissolving agent is the mixture of acetic acid and sodium acetate or the mixture of aqueous ammonia and ammonium carbonate, zinc oxide mineral be hemimorphite, corresponding selective dissolving agent is aqueous ammonia, ammonium carbonate and NH4HF2In the precipitate with a selective dissolving agentThe heavy metal oxidized mineral is dissolved, and sulfide generated by vulcanizing the oxidized mineral is not dissolved and still exists in a solid form to obtain a solid-liquid mixture;
(3) and (3) centrifugally cleaning the solid-liquid mixture obtained in the step (2) for more than one time, and drying the bottom slurry after centrifugal cleaning to obtain a vulcanized product after the pure mineral of the heavy metal oxidized mineral is vulcanized.
2. The method for extracting a sulfide product after pure mineral vulcanization of a heavy metal oxidized mineral according to claim 1, characterized in that: the drying temperature in the step (3) is 30-60 ℃.
3. The method for extracting a sulfide product after pure mineral vulcanization of a heavy metal oxidized mineral according to claim 1, characterized in that: repeating the steps (1) to (3) for more than one time, mixing the vulcanization products extracted for more than one time, and carrying out analysis test.
CN201910057647.0A 2019-01-22 2019-01-22 Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization Active CN109663663B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910057647.0A CN109663663B (en) 2019-01-22 2019-01-22 Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910057647.0A CN109663663B (en) 2019-01-22 2019-01-22 Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization

Publications (2)

Publication Number Publication Date
CN109663663A CN109663663A (en) 2019-04-23
CN109663663B true CN109663663B (en) 2020-11-27

Family

ID=66149656

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910057647.0A Active CN109663663B (en) 2019-01-22 2019-01-22 Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization

Country Status (1)

Country Link
CN (1) CN109663663B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112191370B (en) * 2020-08-27 2022-07-12 中国恩菲工程技术有限公司 Flotation method for copper minerals
CN112239286B (en) * 2020-08-27 2022-07-12 中国恩菲工程技术有限公司 Copper ion modified water treatment method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101497061A (en) * 2009-03-13 2009-08-05 昆明理工大学 Active flotation method for refractory sulfide mineral in oxidized-sulfide mixed ore
JP5025537B2 (en) * 2008-03-21 2012-09-12 太平洋セメント株式会社 Method for treating fine powder containing calcium component and lead component
CN103301929A (en) * 2013-03-29 2013-09-18 云南金鼎锌业有限公司 Selective zinc oxide leaching and weak acidic zinc sulfide flotation smelting and selection combining process
JP5374041B2 (en) * 2005-03-22 2013-12-25 アングロ オペレーションズ リミティッド Leaching method in the presence of hydrochloric acid to recover valuable metals from ora
CN105435952A (en) * 2015-11-09 2016-03-30 湖南有色金属研究院 Method for recovering high-pelitic and high-iron copper oxide ore hard to treat
WO2018002448A1 (en) * 2016-06-30 2018-01-04 Haarla Oy Method for improving separation of mineral particles by high intensity conditioning

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5374041B2 (en) * 2005-03-22 2013-12-25 アングロ オペレーションズ リミティッド Leaching method in the presence of hydrochloric acid to recover valuable metals from ora
JP5025537B2 (en) * 2008-03-21 2012-09-12 太平洋セメント株式会社 Method for treating fine powder containing calcium component and lead component
CN101497061A (en) * 2009-03-13 2009-08-05 昆明理工大学 Active flotation method for refractory sulfide mineral in oxidized-sulfide mixed ore
CN103301929A (en) * 2013-03-29 2013-09-18 云南金鼎锌业有限公司 Selective zinc oxide leaching and weak acidic zinc sulfide flotation smelting and selection combining process
CN105435952A (en) * 2015-11-09 2016-03-30 湖南有色金属研究院 Method for recovering high-pelitic and high-iron copper oxide ore hard to treat
WO2018002448A1 (en) * 2016-06-30 2018-01-04 Haarla Oy Method for improving separation of mineral particles by high intensity conditioning

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
典型氧化铜铅锌矿物浮选的表面硫化研究进展;宋凯伟等;《化工进展》;20180905;第37卷(第9期);第3618-3628页 *
化学物相分析;北京矿业研究院编;《化学物相分析》;北京:冶金工业出版社;19790228;第105-137页 *
氧化铜矿物抗抑制作用的表面形貌研究;刘殿文等;《金属矿山》;20090315(第3期);第59-60页 *
硫化矿氧化率测定问题的研究Ⅱ. 硫化铅矿中氧化铅的分离测定;黄宝贵等;《冶金分析》;19940630;第14卷(第3期);第21-24页 *

Also Published As

Publication number Publication date
CN109663663A (en) 2019-04-23

Similar Documents

Publication Publication Date Title
US5484579A (en) Hydrometallurical recovery of copper and zinc from complex sulfide ores
CN103014355B (en) Multi-metal comprehensive recycling process for copper smelting ash
CN102191391B (en) Method for extracting germanium from high-impurity low-grade complex zinc oxide powder
CN109663663B (en) Method for extracting sulfide product of heavy metal oxidized mineral after pure mineral vulcanization
CN103924102B (en) Method for removing antimony from refractory gold ore and preparing cubic crystal sodium pyroantimonate
CN111495581A (en) Beneficiation method for recycling lead-zinc ore beneficiation treatment wastewater
CN104775032A (en) Method for separating selenium and mercury from acid mud produced in acid preparation through roasting of gold concentrate
CN104010962B (en) Method for separating arsenic and heavy metals in acidic washing solution
Yazici et al. Precipitation of zinc from cyanide leach solutions using Trimercapto-s-triazine (TMT)
CA1059769A (en) Extraction of metal values from leached slurries
CN109306408A (en) A kind of ilmenite flue dust arsenic removal and the method for recycling valuable metal
FI65805C (en) FOERFARANDE FOER AOTERVINNING AV BLY SILVER OCH GULD UR JAERNHALTIGT AVFALL FRAON EN ELEKTROLYTISK ZINKPROCESS
CN104762473A (en) Method for leaching low-grade zinc oxide ore
AU2017279746A1 (en) Beneficiation of Lead Sulphide Bearing Material
Canpolat et al. Recovery of copper from complex copper oxide ore by flotation and leaching methods
CN101816979B (en) Flotation activating agent of marmatite and blende and preparation method thereof
US3357823A (en) Recovery of gold, silver, copper and zinc by alkaline cyaniding with electrodialysis
CN116422457A (en) Method for recycling fine-grained cassiterite
US11220725B2 (en) Method of copper concentrate sulfation and leaching
WO2012034255A1 (en) Method for extracting gold coated by gangue
CN111647750B (en) Resource utilization method of tailings
RU2366736C2 (en) Method of processing copper-zinc products containing noble metals
CN113042190A (en) Flotation pretreatment method for pyrite in cyanide-containing and sulfur-containing tailings
Klyushnikov Study of Copper and Zinc Extraction from Underspoil Water
JPH031069B2 (en)

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant