CN114934188A - Increase Cu (II) -NH 3 -S 2 O 32- Method for recovering gold (I) in system - Google Patents

Increase Cu (II) -NH 3 -S 2 O 32- Method for recovering gold (I) in system Download PDF

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CN114934188A
CN114934188A CN202210543966.4A CN202210543966A CN114934188A CN 114934188 A CN114934188 A CN 114934188A CN 202210543966 A CN202210543966 A CN 202210543966A CN 114934188 A CN114934188 A CN 114934188A
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gold
solution
silica gel
modified silica
adsorption
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字富庭
李娟�
胡显智
李鑫容
陈树梁
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Environmental & Geological Engineering (AREA)
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Abstract

The invention discloses a method for improving Cu (II) -NH content 3 ‑S 2 O 3 2‑ A method for recovering the recovery rate of gold (I) in a system, belonging to the fields of hydrometallurgy and precious metal recovery; the invention takes polyamine (ammonia) substances and citric acid as additives, overcomes the competitive adsorption of coexisting ionic copper (II) in the solution by changing the composition and the property of the adsorption solution, thereby greatly improving the Cu (II) -NH of the sulfydryl modified silica gel 3 ‑S 2 O 3 2‑ The adsorption capacity of the gold (I) in the system, thereby solving the problem of difficult recovery of the gold (I) in the solution; the method has the characteristics of simple process flow, short time consumption, low energy consumption, small additive dosage, wide pH application range, high gold recovery rate and the like.

Description

Improve Cu (II) -NH 3 -S 2 O 32- Method for recovering gold (I) in system
Technical Field
The invention relates to a method for increasing Cu (II) -NH content 3 -S 2 O 3 2- A method for recovering gold (I) in a system belongs to the field of hydrometallurgy and precious metal recovery.
Background
In the wet extraction technique of gold, the traditional cyanidation method is gradually replaced by non-cyanidation method due to the strong toxicity of gold leaching reagent. Among them, the thiosulfate method is considered to be a non-cyanide gold extraction method with the most popularization prospect due to the characteristics of no toxicity, environmental protection and low corrosivity, and is simultaneously suitable for treating copper-containing gold ores and carbonaceous gold ores which are difficult to treat by a cyanidation method. The thiosulfate has very slow dissolving speed to gold, but can greatly improve the dissolving rate of gold under the catalytic oxidation action of cuprammonium complex ions, thereby meeting the requirements of industrial production. Meanwhile, the existence of ammonia can also inhibit the dissolution of impurity elements such as iron, calcium, magnesium and the like by keeping the leaching solution in an alkaline environment, and eliminate the influence of impurity ions on the leaching solution. Although the problem of slow gold leaching rate is primarily solved at present, the problem of effective recovery of gold from the leaching solution still limits the further popularization of the thiosulfate method. Therefore, a great deal of research has been devoted to how to recover gold from thiosulfate gold leaching solutions.
Currently, methods for recovering gold from thiosulfate solutions include displacement methods, solvent extraction methods, electrodeposition methods, adsorption methods, and the like. The adsorption method is an effective mode for recovering metal ions in a solution, and is a method for enriching substances in a pore structure of a porous adsorbent and separating the adsorbent from the adsorbate by using a corresponding reagent. Common adsorbents include porous materials such as resin, activated carbon and silica gel. In the patent (CN 113278815A), an ionizing radiation grafting method or a chemical grafting method is adopted to modify a high-molecular base material to obtain resin containing nitrogen and sulfur on the surface, so that the effective recovery of gold in gold leaching barren solution is realized, but the method has a complex modification process, and the resin is expensive and is not beneficial to industrial application; the patent (CN 109589953A) uses thiourea to modify the active carbon to prepare the adsorbent with the surface rich in nitrogen, sulfur, oxygen and other atoms, so that the surface property of the material is changed to the Au (S) in the thiosulfate solution 2 O 3 ) 2 3- The complex ions generate effective adsorption, but the method has large using amount of the modifier and harsh reaction conditions; in the patent (CN 108754173A), silica gel is used as a substrate, a mercaptosilane coupling agent is used as a modifier, and mercapto group with strong binding force to gold (I) in thiosulfate solution is introduced to the surface of the silica gel, so that the purpose of adding gold (I) into the thiosulfate solution is achievedEffectively enriching the gold (I). However, the material is used for Cu (II) -NH 3 -S 2 O 3 2- When gold is recovered from the system, the effect of recovering gold from the solution by the sulfydryl modified silica gel is not ideal due to competitive adsorption of copper (II); at present, Cu (II) -NH is a rare effective component 3 -S 2 O 3 2- The key to breaking through this bottleneck is the effective recovery method explored by the report of gold recovery in the system.
Disclosure of Invention
The invention discloses a method for improving Cu (II) -NH content 3 -S 2 O 3 2- The method for recovering the recovery rate of the gold (I) in the system adopts the method that a proper additive is added into a leaching solution to change the property of the solution, reduce the content of copper-ammonia complex ions, weaken the competitive adsorption of the copper-ammonia complex ions and the gold, and effectively solve the problem of recovering Cu (II) -NH from the sulfydryl modified silica gel 3 -S 2 O 3 2- The effect of gold (I) in the system is not ideal, and the improvement of the Cu (II) -NH of the sulfydryl modified silica gel 3 -S 2 O 3 2- The method for recovering and enriching the gold (I) in the system specifically comprises the following steps:
(1) to Cu (II) -NH 3 -S 2 O 3 2- Adding an additive into the system, and adjusting the pH of the solution to 8-12; the additive is one or a mixture of more of ethylenediamine, triethylenediamine, triethylenetetramine, tetraethylenepentamine, ethylenediamine tetraacetic acid and citric acid.
(2) And (2) adding the sulfydryl modified silica gel into the solution obtained in the step (1), and stirring and adsorbing the gold in the system.
Cu (II) -NH according to the invention 3 -S 2 O 3 2- The system refers to Au (S) containing copper and ammonia 2 O 3 ) 2 3- The general copper (II) concentration is 0.5-50 mmol/L, and the molar ratio of copper to ammonia is 1:100, the concentration of thiosulfate (sodium) is 0.01-1 mol/L, and the concentration of gold (I) is 5-100 mg/L.
Preferably, the addition amount of the additive in the step (1) is 0.1-10 g/L.
Preferably, the solid-to-liquid ratio of the mercapto-modified silica gel to the gold-containing solution in step (2) of the invention is 1:1000 to 1: 200.
Preferably, the preparation process of the mercapto-modified silica gel of the present invention is prepared by referring to the method of patent (CN 108754173A) claim.
The principle of the invention is as follows:
recovery of Cu (II) -NH from mercapto-modified silica gel 3 -S 2 O 3 2- The competitive adsorption of copper (II) exists when gold (I) exists in the system, so that the recovery rate of gold by the adsorbent is low. The addition of amine (ammonia) substances and citric acid as polybase ligands can form stable chelate with most metal cations in solution, and the stability of the chelate formed by the amine (ammonia) substances and the citric acid is higher than that of Cu (NH) 3 ) 4 2+ The influence of copper (II) on gold (I) adsorption can be obviously reduced by changing the existence form of copper (II) in the solution, so that the adsorption capacity of the sulfydryl modified silica gel on gold (I) is enhanced.
The invention has the beneficial effects that:
(1) the invention effectively overcomes the influence of copper (II) on the adsorption process by adding polyamine (ammonia) substances and citric acid, and greatly improves the Cu (II) -NH of the mercapto-modified silica gel 3 -S 2 O 3 2- Adsorption capacity of gold (I) in the system.
(2) The invention has simple process flow and simple and easy operation method; the used additive has small dosage and strong stability; the reaction condition is mild, and gold can be effectively recovered only by adding a small amount of additive into the gold leaching solution, thereby being beneficial to large-scale application.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
This example used triethylene diamine as an additive and the mercapto-modified silica gel to recover Cu (II) -NH 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- Concentration 5 mg/L, Cu (NH) 3 ) 4 2+ 0.1 g/L triethylene diamine was added to the solution having a concentration of 0.5 mmol/L, and the pH of the solution was adjusted to 8.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the materials in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) And (2) adding 0.1 g of the mercapto-modified silica gel obtained in the step (2) into the solution obtained in the step (1) (the solid-to-liquid ratio is 1:1000 in the case), stirring and adsorbing the gold, wherein the adsorption rate is 35.7% and the loading amount is 1.785 kg/t after adsorbing for 2 h, and the adsorption rate is 14.58% and the loading amount is 0.729 kg/t under the same conditions without adding an additive.
Example 2
In this example, Cu (II) -NH was recovered from a mercapto-modified silica gel using ethylenediamine as additive 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- Cu (NH) at a concentration of 50 mg/L 3 ) 4 2+ 1 g/L of ethylenediamine was added to the 5 mmol/L solution to adjust the pH of the solution to 9.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the material in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) And (2) adding 0.2 g of the mercapto-modified silica gel obtained in the step (2) into the solution obtained in the step (1) (the solid-to-liquid ratio is 1: 500 in the case), stirring and adsorbing the gold, wherein the adsorption rate is 76.3% and the loading amount is 19.1 kg/t after adsorption for 4 hours, and the adsorption rate is 11.3% and the loading amount is 2.825 kg/t under the same conditions without adding an additive.
Example 3
This example uses EDTA as an additive and mercapto-modified silica gel to recover Cu (II) -NH 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- The concentration is 25 mg/L, Cu (NH) 3 ) 4 2+ 2.5 g/L of ethylenediamine tetraacetic acid was added to the 20 mmol/L solution to adjust the pH of the solution to 12.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the materials in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) 0.25 g of the mercapto-modified silica gel obtained in the step (2) (in this case, the solid-to-liquid ratio is 1: 400) was added to the solution obtained in the step (1), gold was adsorbed by stirring, and the adsorption rate was 62.8% and the loading was 6.28 kg/t, as measured after 40 min, and the adsorption rate was 8.56% and the loading was 0.856 kg/t in the case where no additive was added under the same conditions.
Example 4
This example used tetraethylenepentamine as an additive and Cu (II) -NH was recovered using a mercapto-modified silica gel 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) in 100 mL volume, Au (S) 2 O 3 ) 2 3- Cu (NH) at a concentration of 75 mg/L 3 ) 4 2+ To the 40 mmol/L solution was added 5 g/L tetraethylenepentamine to adjust the pH of the solution to 11.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the materials in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) 0.5 g of the mercapto-modified silica gel obtained in the step (2) (in this case, the solid-to-liquid ratio is 1: 200) was added to the solution obtained in the step (1), gold was adsorbed by stirring, and after 12 hours, the adsorption rate was 48.7% and the loading was 7.31 kg/t, while under the same conditions, the adsorption rate without an additive was 5.48% and the loading was 0.822 kg/t.
Example 5
The example uses citric acid as additive and sulfhydryl-modified silica gel to recover Cu (II) -NH 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- Cu (NH) at a concentration of 75 mg/L 3 ) 4 2+ To the 10 mmol/L solution was added 7.5 g/L citric acid to adjust the pH of the solution to 10.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the materials in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) 0.5 g of the mercapto-modified silica gel obtained in the step (2) (in this case, the solid-to-liquid ratio is 1: 200) was added to the solution obtained in the step (1), gold was adsorbed by stirring, and the adsorption rate was 52.4% and the loading was 7.86 kg/t when measured after 24 hours, and the adsorption rate was 18.2% and the loading was 2.73 kg/t when no additive was added under the same conditions.
Example 6
In the example, a mixture of ethylenediamine and triethylenetetramine (mass ratio 2: 1) was used as an additive, and mercapto-modified silica gel was used to recover Cu (II) -NH 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- Concentration of 100 mg/L, Cu: (NH 3 ) 4 2+ Adding a mixture of 10 g/L of ethylenediamine and triethylene tetramine into a gold leaching solution with the concentration of 50 mmol/L, and adjusting the pH value of the solution to 10.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene serving as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane serving as a modifier into a 150 ml round-bottom flask, placing the flask at 70 ℃, magnetically stirring the flask at a constant temperature for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the material in a vacuum oven at 60 ℃ for drying for later use.
(3) 0.2 g of the mercapto-modified silica gel obtained in the step (2) (in this case, the solid-to-liquid ratio is 1: 500) was added to the solution obtained in the step (1), gold was adsorbed by stirring, the adsorption rate was 37.8% and the loading was 18.9 kg/t, when no additive was added under the same conditions, the adsorption rate was 6.52% and the loading was 3.26 kg/t, as measured after 8 hours of adsorption.
Example 7
In the example, a mixture of triethylene diamine and ethylene diamine tetraacetic acid (mass ratio of 1: 1) is used as an additive, and sulfydryl modified silica gel is used for recovering Cu (II) -NH 3 -S 2 O 3 2- The gold (I) in the system specifically comprises the following steps:
(1) volume 100 mL, Au (S) 2 O 3 ) 2 3- Cu (NH) at a concentration of 50 mg/L 3 ) 4 2+ Adding a mixture of ethylenediamine and triethylene tetramine with the mass of 5 g/L into the gold leaching solution with the concentration of 25 mmol/L, and adjusting the pH value of the solution to 9.
(2) Preparing materials: taking 4 g of activated silica gel, adding 30 ml of toluene as a solvent and 5 ml of 3-mercaptopropyl-trimethoxysilane as a modifier into a 150 ml round-bottom flask, placing the flask at a constant temperature of 70 ℃, magnetically stirring the flask for reaction for 4 hours, alternately cleaning residual organic reagents on the surface by using ethanol-water solution, and then placing the materials in a vacuum oven at a temperature of 60 ℃ for drying for later use.
(3) 0.2 g of the mercapto-modified silica gel obtained in the step (2) (in this case, the solid-to-liquid ratio is 1: 500) was added to the solution obtained in the step (1), gold was adsorbed by stirring, and the adsorption rate was 46.1% and the loading was 11.52 kg/t, when no additive was added under the same conditions, the adsorption rate was 7.26% and the loading was 1.815 kg/t, as measured after 1 hour of adsorption.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, 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 (5)

1. Improve Cu (II) -NH 3 -S 2 O 3 2- The method for recovering the gold (I) in the system is characterized by specifically reporting the following steps:
(1) to Cu (II) -NH 3 -S 2 O 3 2- Adding an additive into the system, and adjusting the pH value of the solution to 8-12; the additive is one or a mixture of more of ethylenediamine, triethylenediamine, triethylenetetramine, tetraethylenepentamine, ethylenediamine tetraacetic acid and citric acid;
(2) and (2) adding the sulfydryl modified silica gel into the solution obtained in the step (1), and stirring and adsorbing the gold in the system.
2. The method of claim 1 for increasing Cu (II) -NH 3 -S 2 O 3 2- A method for recovering gold (I) from a system, characterized by: the Cu (II) -NH 3 -S 2 O 3 2- The system refers to Au (S) containing copper and ammonia 2 O 3 ) 2 3- And (3) solution.
3. The method of claim 1 for increasing Cu (II) -NH 3 -S 2 O 3 2- A method for recovering gold (I) from a system, characterized by: the addition amount of the additive in the step (1) is 0.1-10 g/L.
4. The method of claim 1 for increasing Cu (II) -NH 3 -S 2 O 3 2- A method for recovering gold (I) in a system, characterized by: solid-liquid of sulfydryl modified silica gel and gold-containing solution in step (2)The ratio is 1:1000 to 1: 200.
5. The method of claim 1 for increasing Cu (II) -NH 3 -S 2 O 3 2- A method for recovering gold (I) in a system, characterized by: the preparation process of the sulfhydryl modified silica gel is prepared by the method described in the patent (CN 108754173A).
CN202210543966.4A 2022-05-19 2022-05-19 Increase Cu (II) -NH 3 -S 2 O 32- Method for recovering gold (I) in system Pending CN114934188A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0609769A2 (en) * 1993-02-05 1994-08-10 Du Pont De Nemours (Deutschland) Gmbh Method and apparatus for recycling wash water in photographic processing
AU8965198A (en) * 1998-09-04 1999-03-29 Oretek Limited Process for recovery of gold and/or silver
CN101775490A (en) * 2010-02-10 2010-07-14 昆明理工大学 Gold extracting method by thiosulfate using polyamine compoud as additive
CN103276206A (en) * 2013-06-09 2013-09-04 中南大学 Method for leaching gold in alkaline thiourea system efficiently and stably
CN108754173A (en) * 2018-05-04 2018-11-06 昆明理工大学 A method of recycling gold from thiosulfate solution
CN109680163A (en) * 2019-01-14 2019-04-26 东北大学 A method of using triethanolamine as the Leaching of Gold Using Thiosulfate of additive
CN111889068A (en) * 2020-06-19 2020-11-06 昆明理工大学 For adsorbing and recovering Au (S)2O3)2]3-Modification method of ion-complexed active carbon
CN112961991A (en) * 2021-02-05 2021-06-15 江西理工大学 Copper-catalyzed glycine-thiosulfate composite gold leaching process

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0609769A2 (en) * 1993-02-05 1994-08-10 Du Pont De Nemours (Deutschland) Gmbh Method and apparatus for recycling wash water in photographic processing
AU8965198A (en) * 1998-09-04 1999-03-29 Oretek Limited Process for recovery of gold and/or silver
CN101775490A (en) * 2010-02-10 2010-07-14 昆明理工大学 Gold extracting method by thiosulfate using polyamine compoud as additive
CN103276206A (en) * 2013-06-09 2013-09-04 中南大学 Method for leaching gold in alkaline thiourea system efficiently and stably
CN108754173A (en) * 2018-05-04 2018-11-06 昆明理工大学 A method of recycling gold from thiosulfate solution
CN109680163A (en) * 2019-01-14 2019-04-26 东北大学 A method of using triethanolamine as the Leaching of Gold Using Thiosulfate of additive
CN111889068A (en) * 2020-06-19 2020-11-06 昆明理工大学 For adsorbing and recovering Au (S)2O3)2]3-Modification method of ion-complexed active carbon
CN112961991A (en) * 2021-02-05 2021-06-15 江西理工大学 Copper-catalyzed glycine-thiosulfate composite gold leaching process

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