CN214612692U - System for recovering valuable elements from acid leaching solution of roasting slag of gold-containing sulfur concentrate - Google Patents
System for recovering valuable elements from acid leaching solution of roasting slag of gold-containing sulfur concentrate Download PDFInfo
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Abstract
The invention relates to a system for recovering valuable elements from a pickling solution of gold-containing sulfur concentrate roasting slag, which belongs to the field of chemical ore dressing or wet metallurgy.A sulfate radical recovery stirring barrel is connected with a gypsum thickener; a concentrated liquid outlet of the gypsum thickener is connected with a No. 1 filter press, and a liquid outlet of the No. 1 filter press is connected with an iron and arsenic pre-enrichment stirring barrel; a concentrated solution outlet of the iron-arsenic rough concentrate thickener is connected with a No. 2 filter press, and a liquid outlet of the No. 2 filter press is connected with a copper extraction stirring barrel; the concentrated solution outlet of the copper concentrate thickener is connected with a 3# filter press, and the liquid outlet of the 3# filter press is waste acid solution. The utility model provides a retrieve valuable element system in follow auriferous sulphur concentrate roasting slag pickle liquor can handle arsenic-containing waste water, to valuable element recycle wherein.
Description
Technical Field
The invention relates to a system for recovering valuable elements from acid leaching solution of gold-containing sulfur concentrate roasting slag, belongs to the field of chemical ore dressing or wet metallurgy, and relates to the technical field of acid leaching or washing waste liquid treatment of the gold-containing sulfur concentrate roasting slag in gold smelting.
Background
At present, for the treatment of fine-grain dip-dyeing type gold-containing sulfur concentrate, more domestic enterprises adopt a method of roasting-pickling or washing pretreatment-re-leaching gold, but when the method is used for extracting gold, in order to remove harmful elements influencing gold leaching and improve the quality of slag (iron concentrate), slag burning pretreatment (namely pickling or washing) is required, so that the problem of treatment of acid waste liquid is also involved. With different roasting raw materials, processes and acid washing circulation times, the acid leaching waste liquid has larger element types and content differences, and generally contains valuable elements such as copper, zinc, iron, arsenic and the like, wherein relatively speaking, the iron content is higher, the arsenic content is low, but the acid leaching waste liquid is directly discharged without being treated, and serious environmental pollution is generated. At present, the methods for treating arsenic-containing wastewater comprise the following steps: lime-iron salt method, sulfurization method, ion exchange method, adsorption method, membrane separation technique, etc. The lime-iron salt method is characterized in that lime, ferrous sulfate and air are added to form a ferric arsenate and ferric hydroxide colloid mixture, the adsorption force of the ferric arsenate and ferric hydroxide colloid mixture is strong, and the ferric arsenate and the ferric hydroxide colloid mixture form coprecipitation together; in order to improve the arsenic removal effect, the pH value is generally controlled to be 9-10.5, and at the moment, other sulfate radicals, copper, zinc, iron and other ions also form precipitates, so that the produced sediment is large in amount, the post-treatment cost is high, and valuable elements are difficult to recover; the sulfuration method is characterized in that metal ions and arsenic are converted into insoluble sulfide precipitate by utilizing a vulcanizing agent, and then solid-liquid separation or flotation recovery is carried out to remove arsenic and heavy metal ions; the ion exchange method is effective in treating the arsenate and arsenite-containing sewage under the condition of proper pH by using weak-base anion resin, but the method has high equipment investment, the used resin needs to be regenerated frequently, and the treatment cost is high; the adsorption method is characterized in that insoluble solid materials with high specific surface area are used as adsorbents, and arsenic pollutants in water are fixed on the surfaces of the adsorbents through mechanisms such as physical adsorption, chemical adsorption or ion exchange, so that the aim of removing arsenic is fulfilled, but the regeneration, recovery and reuse of the adsorbents are difficult; the membrane separation technology is a method for separating, grading, purifying or enriching the components in a multi-component fluid by using a high-molecular or inorganic semipermeable membrane As a separation medium and using external energy As a driving force and utilizing the difference of mass transfer selectivity of each component in the membrane. In conclusion, most of the methods are only limited to harmless treatment on the arsenic-containing wastewater, the valuable elements are not considered to be recycled, secondary pollution is easily caused to some of the arsenic-containing wastewater, the amount of waste residues and waste liquid is large, the treatment cost is high, and recycling is difficult to realize. In order to overcome the defects of the prior art and effectively solve the problems, a system for recovering valuable elements from the pickle liquor of the roasting residue of the auriferous sulfur concentrate is needed.
Disclosure of Invention
In order to solve the technical problem, the utility model provides a retrieve valuable element system in follow auriferous sulphur concentrate roasting slag pickle liquor can handle arsenic-containing waste water, to valuable element recycle wherein.
The specific technical scheme is as follows: a system for recovering valuable elements from a pickling solution of gold-containing sulfur concentrate roasting slag comprises a sulfate radical recovery stirring barrel, wherein an overflow port of the sulfate radical recovery stirring barrel is connected with a gypsum thickener through a delivery pump, an overflow port of the gypsum thickener is connected with an iron and arsenic pre-enrichment stirring barrel through the delivery pump, an overflow port of the iron and arsenic pre-enrichment stirring barrel is connected with an iron and arsenic rough concentrate thickener through the delivery pump, an overflow port of the iron and arsenic rough concentrate thickener is connected with a copper extraction stirring barrel through the delivery pump, an overflow port of the copper extraction stirring barrel is connected with a copper concentrate thickener through the delivery pump, and an overflow port of the copper concentrate thickener is a waste acid solution;
the concentrated liquid outlet of the gypsum thickener is connected with a No. 1 filter press, the liquid outlet of the No. 1 filter press is connected with the iron and arsenic pre-enrichment stirring barrel through a delivery pump, and the solid of the No. 1 filter press is gypsum;
a concentrated solution outlet of the iron-arsenic rough concentrate thickener is connected with a No. 2 filter press, and a liquid outlet of the No. 2 filter press is connected with a copper extraction stirring barrel through a delivery pump;
a concentrated solution outlet of the copper concentrate thickener is connected with a 3# filter press, a liquid outlet of the 3# filter press is a waste acid solution, and a solid outlet of the 3# filter press is copper-zinc concentrate;
conveying solids of the No. 2 filter press to an arsenic leaching tank, wherein an arsenic leaching overflow port is connected with an iron concentrate thickener through a conveying pump, an iron concentrate thickener overflow port is connected with an acidification arsenic extraction stirring barrel through a conveying pump, the acidification arsenic extraction stirring barrel overflow port is connected with the arsenic concentrate thickener through a conveying pump, and the arsenic concentrate thickener overflow port is waste acid liquor;
the concentrated liquid outlet of the iron ore concentrate thickener is connected with a No. 4 filter press, the liquid outlet of the No. 4 filter press is connected with the acidification arsenic extraction stirring barrel through a delivery pump, and the solid outlet of the No. 4 filter press is iron ore concentrate;
the concentrated solution outlet of the arsenic concentrate thickener is connected with a No. 5 filter press, the solid outlet of the No. 5 filter press is arsenic concentrate, and the liquid outlet of the No. 5 filter press is waste acid liquid;
the sulfate radical recovery stirring barrel, the iron and arsenic pre-enrichment stirring barrel, the copper extraction stirring barrel, the arsenic leaching tank and the acidification arsenic extraction stirring barrel are provided with a stirrer and a charging opening.
Adding acidic water (containing gold and sulfur concentrate roasting slag pickle liquor) containing copper, zinc, iron and arsenic and calcium carbonate into a sulfate radical recovery stirring barrel; adding an oxidant (manganese dioxide or oxygen) and a sodium hydroxide solution into the iron and arsenic pre-enrichment stirring barrel; adding thioacetamide solution into a copper extraction stirring barrel; adding a sodium hydroxide solution and water into the arsenic leaching tank; adding sulfuric acid and thioacetamide solution into an acidification arsenic extraction stirring barrel.
The technical scheme comprises the following steps:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding calcium carbonate or lime to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic solution obtained in the step (2) to a stirring barrel B, adding one of manganese dioxide and oxygen, and stirring for 20 minutes, wherein the amount of the manganese dioxide is calculated according to the theory of manganese dioxide reacting with ferrous iron and arsenic; then adding sodium hydroxide while stirring to enable the slurry to have a pH = 2.7-3.7 after the slurry is reacted for 2 hours, concentrating and filtering to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
because the primary acid leaching solution contains a large amount of iron ions, when the acidity is adjusted to be pH = 2.7-3.7, a large amount of ferric hydroxide colloid is generated, arsenic acid is adsorbed on the surface of the primary acid leaching solution by a large surface area in the precipitation process or ferric arsenate is generated to form coprecipitation, so that the arsenic content in the solution is greatly reduced, and the enrichment and recovery of the arsenic and iron are realized.
(4) Valuable gold such as copper and zincBelongs to the field of recovery. And (3) conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding one or a mixture of thioacetamide and sodium sulfide with the amount of 1.1 times of the theoretical amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
due to the solubility product KSP（Fe(OH)3）=10*10-40Solubility product KSP（FeAsO4）=5.7*10-21,The solubility product of ferric hydroxide is far less than
The solubility product of ferric arsenate, so that the ferric arsenate is quickly converted into ferric hydroxide, and the arsenate enters the solution; at the same time, OH-The complexing ability to ferric hydroxide is far superior to AsO4 3-The complexing ability of the arsenic acid is that the arsenic acid radical is not easy to be absorbed by ferric hydroxide and desorbed into the solution under the strong stirring, and the higher leaching rate is kept.
(6) And (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding one or a mixture of thioacetamide and sodium sulfide, wherein the usage amount of the thioacetamide or the sodium sulfide is 1.1 times of the theoretical calculation amount, stirring and reacting for 20-30 minutes, and then concentrating and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
The method aims at extracting valuable elements such as copper, zinc, iron, arsenic and the like from the main copper, zinc, iron, arsenic and sulfate ion-containing waste acid liquor generated in the general gold-containing sulfur concentrate refining process, and avoids the defects that the elements are easy to mix and influence the quality and the recovery rate of each product in the recovery treatment process by reasonably designing the recovery sequence of each valuable element in the gold-containing sulfur concentrate pickle liquor. Aiming at the components to be recovered in different steps, respective optimal treatment methods are adopted, in the whole treatment process, the pH value of the solution is gradually increased, the main steps are completed under an acidic condition, the pH value of the treatment is not greatly adjusted, the production cost and the production control difficulty are reduced, the quality and the recovery rate of each recovered element are ensured, the comprehensive recovery of each valuable component is realized, and the resource value maximization is realized while the comprehensive utilization of resources is realized.
Aiming at the gold-containing sulfur concentrate roasting slag pickling solution, creatively, sulfate ions with the largest content are firstly recovered under an acidic condition, the influence on the quality of other products is avoided, then, a large amount of primary iron ions in the pickling solution are utilized, ferric arsenate and colloidal ferric hydroxide with extremely strong arsenic ion adsorption capacity are generated (at the moment, ferric ions generate ferric hydroxide precipitation, copper and zinc ions cannot generate precipitation), arsenic and iron form coprecipitation in a short time to obtain pre-enrichment recovery, and the pre-enrichment product is used for dissolving arsenic in time under a high-alkali condition through sodium hydroxide to separate ferric hydroxide from arsenic, so that the quality and the recovery rate of iron and arsenic products are ensured; when the pH = 2.7-3.7, copper and zinc ions cannot combine with hydroxide ions to generate precipitates, so that the quality and recovery rate of copper and zinc products recovered from a solution after pre-enrichment are ensured, the quality and recovery rate of arsenic products recovered from a solution after iron and arsenic separation are higher, the comprehensive recovery of valuable elements in a gold-containing sulfur concentrate roasting slag pickling solution is realized, and the resource value is maximized while the comprehensive utilization of resources is realized; and ensures that the acidity is not reduced too much when the treated waste liquid is returned for recycling, and more sulfuric acid is needed to adjust the acidity.
Compared with the prior method, has the advantages and positive effects
(1) The used medicament has less types, low consumption, wide sources and low production cost;
(2) the process flow is simple, the treatment equipment is simple, the operation and the control are easy, and the automatic control is easy to realize;
(3) the production index is stable, the recovery rate is high, the concentrate grade is high, and the harmful doping among concentrates is low;
(4) harmless treatment and valuable component recovery are completed at one time, no waste residue or waste liquid is generated in the treatment process, and the potential safety hazard of secondary pollution generated in the waste residue stacking process is avoided;
(5) the method has strong adaptability and is suitable for recovering valuable components or treating similar waste liquid from the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate containing more metal species.
Drawings
FIG. 1 is a process flow for recovering valuable elements from acid leaching solution of roasting slag of gold-containing sulfur concentrate;
FIG. 2 is a schematic diagram of a system for recovering valuable elements from a pickling solution of a roasting slag of a gold-containing sulfur concentrate;
1: sulfate radical recovery agitator (agitator A), 2: slurry pump, 3: gypsum thickener, 4: filter press # 1, 5: iron and arsenic preconcentration stirring barrel (stirring barrel B), 6: iron and arsenic rough concentrate thickener, 7: 2# filter press, 8: copper extraction stirring barrel (stirring barrel C), 9: copper concentrate thickener, 10: 3# pressure filter, 11: arsenic leaching tank (stirring barrel D), 12: iron concentrate thickener, 13: acidification arsenic extraction stirring barrel (stirring barrel E), 14: arsenic concentrate thickener, 15: filter press # 5, 16: 4# Filter Press.
Detailed Description
As shown in fig. 2, the system for recovering valuable elements from the pickle liquor of the roasting residue of the auriferous sulfur concentrate comprises a sulfate radical recovery stirring barrel 1, wherein an overflow port of the sulfate radical recovery stirring barrel 1 is connected with a gypsum thickener 3 through a delivery pump, an overflow port of the gypsum thickener 3 is connected with an iron and arsenic pre-enrichment stirring barrel 5 through the delivery pump, an overflow port of the iron and arsenic pre-enrichment stirring barrel 5 is connected with an iron and arsenic rough concentrate thickener 6 through the delivery pump, an overflow port of the iron and arsenic rough concentrate thickener 6 is connected with a copper extraction stirring barrel 8 through the delivery pump, an overflow port of the copper extraction stirring barrel 8 is connected with a copper concentrate thickener 9 through the delivery pump, and an overflow port of the copper concentrate thickener 9 is waste acid liquor;
a concentrated liquid outlet of the gypsum thickener 3 is connected with a No. 1 filter press 4, a liquid outlet of the No. 1 filter press 4 is connected with an iron and arsenic pre-enrichment stirring barrel 5 through a delivery pump, and the solid of the No. 1 filter press 4 is gypsum;
a concentrated solution outlet of the iron-arsenic rough concentrate thickener 6 is connected with a No. 2 filter press 7, and a liquid outlet of the No. 2 filter press 7 is connected with a copper extraction stirring barrel 8 through a delivery pump;
a concentrated solution outlet of the copper concentrate thickener 9 is connected with a 3# filter press 10, a liquid outlet of the 3# filter press 10 is a waste acid solution, and a solid outlet of the 3# filter press 10 is copper-zinc concentrate;
the 2# filter press 7 conveys solids into an arsenic leaching tank 11, an overflow port of the arsenic leaching tank 11 is connected with an iron concentrate thickener 12 through a conveying pump, an overflow port of the iron concentrate thickener 12 is connected with an acidification arsenic extraction stirring barrel 13 through a conveying pump, an overflow port of the acidification arsenic extraction stirring barrel 13 is connected with an arsenic concentrate thickener 14 through a conveying pump, and an overflow port of the arsenic concentrate thickener 14 is waste acid liquor;
a concentrated liquid outlet of the iron ore concentrate thickener 12 is connected with a 4# filter press 16, a liquid outlet of the 4# filter press 16 is connected with an acidification arsenic extraction stirring barrel 13 through a delivery pump, and a solid outlet of the 4# filter press 16 is iron ore concentrate;
the concentrated solution outlet of the arsenic concentrate thickener 14 is connected with a 5# filter press 15, the solid outlet of the 5# filter press 15 is arsenic concentrate, and the liquid outlet of the 5# filter press 15 is waste acid liquid;
the sulfate radical recovery stirring barrel 1, the iron and arsenic pre-enrichment stirring barrel 5, the copper extraction stirring barrel 8, the arsenic leaching tank 11 and the acidification arsenic extraction stirring barrel 13 are provided with a stirrer and a charging hole. The liquid outlet pipes of the thickener and the filter press are provided with gate valves.
The technical scheme comprises the following steps:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding calcium carbonate or lime to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic solution obtained in the step (2) to a stirring barrel B, adding one of manganese dioxide and oxygen, and stirring for 20 minutes, wherein the amount of the manganese dioxide is calculated according to the theory of manganese dioxide reacting with ferrous iron and arsenic; then adding sodium hydroxide while stirring to enable the slurry to have a pH = 2.7-3.7 after the slurry is reacted for 2 hours, concentrating and filtering to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
because the primary acid leaching solution contains a large amount of iron ions, when the acidity is adjusted to be pH = 2.7-3.7, a large amount of ferric hydroxide colloid is generated, arsenic acid is adsorbed on the surface of the primary acid leaching solution by a large surface area in the precipitation process or ferric arsenate is generated to form coprecipitation, so that the arsenic content in the solution is greatly reduced, and the enrichment and recovery of the arsenic and iron are realized.
(4) And recovering valuable metals such as copper, zinc and the like. And (3) conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding one or a mixture of thioacetamide and sodium sulfide with the amount of 1.1 times of the theoretical amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
due to the solubility product KSP（Fe(OH)3）=10*10-40Solubility product KSP（FeAsO4）=5.7*10-21,The solubility product of ferric hydroxide is far less than
The solubility product of ferric arsenate, so that the ferric arsenate is quickly converted into ferric hydroxide, and the arsenate enters the solution; at the same time, OH-The complexing ability to ferric hydroxide is far superior to AsO4 3-The complexing ability of the arsenic acid is that the arsenic acid radical is not easy to be absorbed by ferric hydroxide and desorbed into the solution under the strong stirring, and the higher leaching rate is kept.
(6) And (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding one or a mixture of thioacetamide and sodium sulfide, wherein the usage amount of the thioacetamide or the sodium sulfide is 1.1 times of the theoretical calculation amount, stirring and reacting for 20-30 minutes, and then concentrating and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
The first embodiment is as follows:
the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate has the pH =0.6, and the analysis result of main elements is as follows: contains Cu 3130mg/L, Zn 160mg/L, Fe 19210mg/L, As 2325mg/L and a certain amount of Ca, Mg, etc.
The method is adopted to implement the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate, and the technical steps comprise:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding calcium carbonate to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic solution obtained in the step (2) to a stirring barrel B, adding manganese dioxide, and stirring for 20 minutes, wherein the amount of manganese dioxide is calculated according to the theory of manganese dioxide reacting with ferrous iron and arsenic; then, adding sodium hydroxide while stirring to make the slurry react to the end of pH =2.7, concentrating and filtering after 2 hours to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
(4) and recovering valuable metals such as copper, zinc and the like. And (4) conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding sodium sulfide with the amount being 1.1 times of the theoretical calculation amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
(6) and (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding sodium sulfide with the dosage being 1.1 times of the theoretical calculation amount, stirring for reacting for 20-30 minutes, and then concentrating and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
By adopting the treatment method, the obtained test results are as follows: grade of zinc-copper containing concentrate: copper 52.83%, zinc 3.25%, recovery: 95.31% of copper; the iron grade of the iron ore concentrate is 47.67 percent, and the recovery rate is 95.44 percent; the arsenic grade of the arsenic concentrate is 38.12 percent, and the recovery rate is 86.62 percent.
Example two:
the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate has the pH =1, and the analysis result of main elements is as follows: contains 4520mg/L copper, 135mg/L zinc, 19480mg/L iron, 2035mg/L arsenic and calcium and magnesium.
The method is adopted to implement the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate, and the technical steps comprise:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding lime to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic solution obtained in the step (2) to a stirring barrel B, adding manganese dioxide, and stirring for 20 minutes, wherein the amount of manganese dioxide is calculated according to the theory of manganese dioxide reacting with ferrous iron and arsenic; then, adding sodium hydroxide while stirring to make the slurry react to the end of pH =3.7, concentrating and filtering after 2 hours to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
(4) and recovering valuable metals such as copper, zinc and the like. And (3) conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding thioacetamide with the amount of 1.1 times of the theoretical calculation amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
(6) and (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding thioacetamide with the dosage being 1.1 times of the theoretical calculation amount, stirring for reacting for 20-30 minutes, concentrating, and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
By adopting the treatment method, the obtained test results are as follows: the copper grade of the copper concentrate is 53.66 percent, the zinc content is 2.76 percent, and the copper recovery rate is 96.23 percent; the iron grade of the iron ore concentrate is 48.51 percent, and the recovery rate is 96.12 percent; arsenic concentrate has 37.78% arsenic grade and 84.18% recovery rate.
Example three:
the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate has the pH =2, and the analysis result of main elements is as follows: contains copper 3683mg/L, zinc 384mg/L, iron 18792mg/L, arsenic 2163mg/L and certain amount of calcium, magnesium, etc.
The method is adopted to implement the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate, and the technical steps comprise:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding calcium carbonate to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic liquid obtained in the step (2) to a stirring barrel B, filling oxygen, and stirring for 20 minutes; then, adding sodium hydroxide while stirring to make the slurry react to the end of pH =3, concentrating and filtering after 2 hours to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
(4) and recovering valuable metals such as copper, zinc and the like. Conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding a mixture of thioacetamide and sodium sulfide with the amount of 1.1 times of the theoretical calculated amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (C)Product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
(6) and (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding a mixture of thioacetamide and sodium sulfide, wherein the usage amount of the mixture is 1.1 times of the theoretical calculation amount, stirring for reacting for 20-30 minutes, and then concentrating and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
By adopting the treatment method, the obtained test results are as follows: the copper grade of the copper concentrate is 52.13 percent, the zinc content is 7.11 percent, and the copper recovery rate is 95.88 percent; the iron grade of the iron ore concentrate is 47.87 percent, and the recovery rate is 94.86 percent; the arsenic grade of the arsenic concentrate is 38.05 percent, and the recovery rate is 85.44 percent.
Example four:
the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate has the pH =1.5, and the analysis result of main elements is as follows: 165mg/L of copper, 3216mg/L of zinc, 19613mg/L of iron, 2237mg/L of arsenic and certain amount of calcium, magnesium and other elements.
The method is adopted to implement the acid leaching solution of the roasting slag of the gold-containing sulfur concentrate, and the technical steps comprise:
(1) and (4) measuring the contents of copper, zinc, iron, arsenic and sulfate radicals and the acidity (pH) of the acidic waste liquid. Taking a certain amount of acidic waste liquid to be treated, and analyzing the contents and acidity of ions such as copper, zinc, ferrous iron, total iron, arsenic, total arsenic, sulfate radical and the like;
(2) and (5) recovering sulfate radicals. And (3) conveying the acidic waste liquid to be treated to a stirring barrel A, and adding lime to prepare gypsum. In the process, the calcium carbonate or lime is added according to the theoretical calculation amount of the chemical reaction, and then the calcium carbonate or lime is concentrated and filtered to obtain a gypsum product and an acid solution;
(3) pre-enriching iron and arsenic. Conveying the acidic solution obtained in the step (2) to a stirring barrel B, adding manganese dioxide, and stirring for 20 minutes, wherein the amount of manganese dioxide is calculated according to the theory of manganese dioxide reacting with ferrous iron and arsenic; then, adding sodium hydroxide while stirring to make the slurry react to the end of pH =3.5, concentrating and filtering after 2 hours to obtain arsenic-containing iron concentrate and copper-containing zinc filtrate;
(4) and recovering valuable metals such as copper, zinc and the like. And (3) conveying the copper-zinc-containing filtrate obtained in the step (3) into a stirring barrel C, slowly adding thioacetamide with the amount of 1.1 times of the theoretical calculation amount, reacting for 30 minutes, concentrating and filtering to obtain copper-zinc concentrate (product) and acid-containing waste liquid. The theoretical dosage of thioacetamide or sodium sulfide is as follows: cu2++ S2-= CuS ↓andzn2++ S2-= ZnS ↓ was calculated (the same applies below);
(5) iron and arsenic separation (i.e., arsenate leaching). And (3) conveying the arsenic-containing iron ore concentrate obtained in the step (3) into a stirring barrel D, adjusting the concentration of ore pulp to be 50%, adding a sodium hydroxide solution, stirring strongly until the pH of the slurry is =13.5, leaching for 30-60 min, filtering, and washing to obtain iron ore concentrate (product) and arsenate radical-containing alkali liquor. In the process, the stirring speed is 500 r/min;
(6) and (5) recovering arsenic. And (3) conveying the arsenate-containing alkali liquor obtained in the step (5) to a reactor E, adding sulfuric acid, adjusting the pH of the solution to be =1, slowly adding thioacetamide with the dosage being 1.1 times of the theoretical calculation amount, stirring for reacting for 20-30 minutes, concentrating, and filtering to obtain arsenic concentrate (product) and acid-containing waste liquor. And (4) returning the acid-containing waste liquid and the acid-containing waste liquid obtained in the step (4) to a roasting slag leaching system for recycling.
By adopting the treatment method, the obtained test results are as follows: the zinc grade of the zinc concentrate is 52.35 percent, the copper content is 2.56 percent, and the zinc recovery rate is 94.05 percent; the iron grade of the iron ore concentrate is 58.04, and the recovery rate is 94.33%; arsenic concentrate has 37.52 percent of arsenic grade and 86.17 percent of recovery rate.
In conclusion, the method for treating the acid leaching solution of the gold-containing sulfur concentrate roasting slag achieves the better aims of achieving harmless treatment and one-time completion of valuable component recovery, generating no waste slag and waste liquid (the waste liquid is returned to a new roasting slag leaching system for use) in the treatment process and avoiding the later potential safety hazard generated by stockpiling the waste slag.
Claims (1)
1. A system for recovering valuable elements from a pickling solution of gold-containing sulfur concentrate roasting slag is characterized by comprising a sulfate radical recovery stirring barrel, wherein an overflow port of the sulfate radical recovery stirring barrel is connected with a gypsum thickener through a delivery pump, an overflow port of the gypsum thickener is connected with an iron and arsenic pre-enrichment stirring barrel through the delivery pump, an overflow port of the iron and arsenic pre-enrichment stirring barrel is connected with an iron and arsenic rough concentrate thickener through the delivery pump, an overflow port of the iron and arsenic rough concentrate thickener is connected with a copper extraction stirring barrel through the delivery pump, an overflow port of the copper extraction stirring barrel is connected with a copper concentrate thickener through the delivery pump, and an overflow port of the copper concentrate thickener is a waste acid solution;
the concentrated liquid outlet of the gypsum thickener is connected with a No. 1 filter press, the liquid outlet of the No. 1 filter press is connected with the iron and arsenic pre-enrichment stirring barrel through a delivery pump, and the solid of the No. 1 filter press is gypsum;
a concentrated solution outlet of the iron-arsenic rough concentrate thickener is connected with a No. 2 filter press, and a liquid outlet of the No. 2 filter press is connected with a copper extraction stirring barrel through a delivery pump;
a concentrated solution outlet of the copper concentrate thickener is connected with a 3# filter press, a liquid outlet of the 3# filter press is a waste acid solution, and a solid outlet of the 3# filter press is copper-zinc concentrate;
conveying solids of the No. 2 filter press to an arsenic leaching tank, wherein an arsenic leaching overflow port is connected with an iron concentrate thickener through a conveying pump, an iron concentrate thickener overflow port is connected with an acidification arsenic extraction stirring barrel through a conveying pump, the acidification arsenic extraction stirring barrel overflow port is connected with the arsenic concentrate thickener through a conveying pump, and the arsenic concentrate thickener overflow port is waste acid liquor;
the concentrated liquid outlet of the iron ore concentrate thickener is connected with a No. 4 filter press, the liquid outlet of the No. 4 filter press is connected with the acidification arsenic extraction stirring barrel through a delivery pump, and the solid outlet of the No. 4 filter press is iron ore concentrate;
the concentrated solution outlet of the arsenic concentrate thickener is connected with a No. 5 filter press, the solid outlet of the No. 5 filter press is arsenic concentrate, and the liquid outlet of the No. 5 filter press is waste acid liquid;
the sulfate radical recovery stirring barrel, the iron and arsenic pre-enrichment stirring barrel, the copper extraction stirring barrel, the arsenic leaching tank and the acidification arsenic extraction stirring barrel are provided with a stirrer and a charging opening.
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