CN112375919B - Method for directly recovering gold in thiosulfate system - Google Patents
Method for directly recovering gold in thiosulfate system Download PDFInfo
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- CN112375919B CN112375919B CN202011203271.9A CN202011203271A CN112375919B CN 112375919 B CN112375919 B CN 112375919B CN 202011203271 A CN202011203271 A CN 202011203271A CN 112375919 B CN112375919 B CN 112375919B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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- 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
Abstract
The invention discloses a method for directly recovering gold in a thiosulfate system, belonging to the field of hydrometallurgy and precious metal recovery. The invention aims to recover Au (S) in solution2O3)2 3‑In order to change the composition of the solution, a small amount of thiourea or thiourea derivatives is added into the solution, and the gold in the solution is directly adsorbed by using commercial activated carbon, so that the gold can be efficiently recovered by the activated carbon in a short time, and the multi-stage adsorption of the gold can be realized. The additive is low in dosage, and the dosage of the additive under the condition of similar gold adsorption rate is far lower than that of the additive used in the related patent of the disclosed modified carbon; the invention does not need equipment such as heating and the like, and has low cost; the method has the advantages of short time and low energy consumption investment, and has important significance for promoting the development of the thiosulfate gold extraction process.
Description
Technical Field
The invention relates to a method for directly recovering gold in a thiosulfate system, belonging to the technical field of hydrometallurgy and precious metal recovery.
Background
Gold extraction by a carbon slurry method is a common gold beneficiation process for effectively recovering gold-containing minerals with lower raw ore grade; after the process is developed for more than 100 years, people find that the process is mature and feasible in technology, exceeds other processes in all indexes, and is a main gold recovery method; the active carbon in the carbon slurry method has strong adsorption capacity and can adsorb organic compounds, inorganic metal ions, non-metal ions and the like. However, the thiosulfate method, which is a promising non-cyanide gold extraction technology, cannot effectively adsorb gold in the leachate by activated carbon. To achieve char in thiosulfateThe slurry method, as proposed in patent (CN 104549147A), uses a range of ferrocyanide (Fe (CN))6]4-) The salt solution is stirred and dipped at normal temperature to generate the prussian blue-like compound on the surface of the activated carbon, and the modified carbon prepared by the method has certain effect, but the modification process of depositing the copper ferrocyanide on the surface of the activated carbon is complex, the stability of the generated product is poor, and the industrialization is not facilitated.
In the patent (CN 109574008A), ammonia thiocyanate is used as a modifier to prepare a modified activated carbon material under certain conditions, and the modified activated carbon material can be used for Au (S) in thiosulfate gold leaching solution2O3)2 3-The complex ions generate certain adsorption. In addition, patent (CN 109589953 a) modifies activated carbon by vapor deposition method and then uses it for recovering gold in solution, so as to improve the gold adsorption capacity of activated carbon in thiosulfate solution.
However, in the preparation process of the modified carbon, a large amount of time and energy consumption are required, so that the production cost of the activated carbon is greatly increased, secondary pollution is easily caused, and the preparation method is not suitable for actual production; in addition, in the actual production process, the same carbon is often needed to carry out multi-stage adsorption on the leachate, which has strict requirements on the stability of the gold adsorption performance of the activated carbon, and this is a place to be further improved in the above method. Therefore, there is a need for a more efficient process for the problem of recovery in non-cyanide non-toxic thiosulfate gold leaching systems.
Disclosure of Invention
The present invention addresses the deficiencies of the prior art by adding a small amount of thiourea or a derivative of thiourea to the solution from the standpoint of changing the composition of the solution (the amount of additive is much lower than that used in the published modified carbon-related patents at similar gold adsorption rates) so that gold can be directly adsorbed by the unmodified activated carbon.
In order to achieve the purpose, the invention adopts the following technical scheme: in the presence of Au (S)2O3)2 3-Adding thiourea or thiourea derivatives into the system leaching solution, and adsorbing gold in the solution by using unmodified activated carbon, wherein the method specifically comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
(2) To Au (S)2O3)2 3-The gold leaching solution is added with an additive, the additive is thiourea or a thiourea derivative, the additive amount of the additive is 0.001-1 g/L, and the pH value is adjusted to 6-12.
(3) Adding the activated carbon obtained in the step (1) into the gold leaching solution obtained in the step (2), and adding gold (Au (S)2O3)2 3-) Stirring and adsorbing.
Preferably, the derivative of thiourea provided by the invention comprises propenyl thiourea, phenylthiourea, dicyclohexyl thiourea, 1,2, 3-thiadiazole cyclic thiourea and thiosemicarbazide.
Preferably, the concentration of thiosulfate in the gold leaching solution is 0.01-3 mol/L, and Au (S)2O3)2 3-The concentration is 5 mg/L to 100 mg/L.
Preferably, in step (3) of the present invention, the activated carbon is a commercially available unmodified activated carbon, and the ratio (mL: g) of the volume of the gold leaching solution to the mass of the activated carbon is 100:0.1 to 100: 1.
Preferably, the gold solution in the step (3) is stirred and adsorbed for 0.1-24 h at 15-70 ℃.
The principle of the invention is as follows: as is known from the literature, the leaching solution of thiosulphate contains Au (S)2O3)2 3-The influence of the coordination group charge, the molecular structure space effect and the like causes the distance between the gold atom and the surface of the active carbon to be far, and the adsorption effect is difficult to occur; and the complex ion has a large number of charges and high hydration energy, so that the gold can not be adsorbed almost by directly using the active carbon. The thiourea or the derivative of the thiourea added in the invention can generate cyanamide and other substances under the alkaline condition, thereby changing the solution environment or reacting with Au (S)2O3)2 3-Some chemical reaction occurs to finally convert the gold into gold species which can be adsorbed by the activated carbon, and the hydration energy of the counter ions can be reduced, so that the gold in the form is finally and efficiently adsorbed by the activated carbon.
The beneficial effects of the invention are:
(1) the invention can effectively recover gold by only adding a small amount of additive into the immersion liquid.
(2) The thiourea or the thiourea derivative is relatively stable in property, low in toxicity and easy to control in the adsorption process.
(3) The capacity of gold adsorption on the activated carbon is high, and the method is beneficial to practical production and application.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, but the scope of the present invention is not limited to the contents.
Example 1
In the embodiment, phenylthiourea is used as an additive, and the activated carbon is used for recovering gold in a thiosulfate system, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
(2) Volume 100 mL, Au (S)2O3)2 3-0.001g/L phenylthiourea was added to the gold immersion liquid at a concentration of 5 mg/L to adjust the pH to 6.
(3) And (3) adding 0.1g of activated carbon (the solid-to-liquid ratio is 1: 1000) into the solution obtained in the step (2), and stirring and adsorbing the gold for 0.1 h.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 36%.
Comparative example 1
Under the condition that other conditions and adsorption rates are similar, phenylthiourea is adopted to modify the activated carbon, and the method comprises the following specific steps:
(1) washing with deionized water to remove ash content of activated carbon, filtering, and oven drying.
(2) And putting the activated carbon into a solution containing phenylthiourea, adding the activated carbon into the solution, soaking the activated carbon at normal temperature, filtering the solution and drying the filtered solution to obtain the modified activated carbon.
Adsorption of Au (S) with the modified carbon obtained2O3)2 3-Modified 0.1g of active carbon, the dosage of phenylthiourea is0.01g, and the dosage of the phenylthiourea in the example 1 is only 0.0001 g.
Under the condition that other conditions are similar to the dosage of phenylthiourea, phenylthiourea is adopted to modify the activated carbon, the steps are the same as the specific steps, and then Au (S) is adsorbed2O3)2 3-The adsorption rate was 15%.
Example 2
In the embodiment, thiourea is used as an additive, and activated carbon is used for recovering gold in a thiosulfate system, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
(2) To 100 mL of Au (S)2O3)2 3-Thiourea was added at a concentration of 10mg/L to the gold-leaching solution at a concentration of 0.01g/L to adjust the pH to 7.
(3) And (3) adding 0.5g of activated carbon (the solid-to-liquid ratio is 1: 200) into the solution obtained in the step (2), and stirring and adsorbing the gold for 2 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 52%.
Comparative example 2
Under other conditions and with similar adsorption rate, thiourea is adopted to modify the activated carbon, and then Au (S) is adsorbed2O3)2 3-Modified 0.5g of activated carbon, the amount of thiourea used was 0.75g, and the amount of thiourea used in example 2 was only 0.001 g.
Under other conditions and with the similar dosage of thiourea, thiourea is adopted to modify the activated carbon, and then Au (S) is adsorbed2O3)2 3-The adsorption rate was 30%.
Example 3
In the embodiment, propenyl thiourea is used as an additive, and the activated carbon is used for recovering gold in a thiosulfate system, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
（2）100 mL，Au(S2O3)2 3-Concentration of0.1g/L of thiopropenyl urea was added to the 20mg/L gold immersion liquid to adjust the pH to 8.
(3) And (3) adding 0.5g of activated carbon (the solid-to-liquid ratio is 1: 200) into the solution obtained in the step (2), and stirring and adsorbing the gold for 4 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 56%.
Comparative example 3
Under other conditions and with similar adsorption rate, modifying the activated carbon by adopting thiopropenyl urea, and then adsorbing Au (S)2O3)2 3-Modified 0.5g of activated carbon, the amount of the acrylthiourea used was 1.0g, and the amount of the acrylthiourea used in example 3 was only 0.01 g.
Under other conditions and the similar using amount of the propenyl thiourea, the propenyl thiourea is adopted to modify the activated carbon, and then the Au (S) is adsorbed2O3)2 3-The adsorption rate was 35%.
Example 4
In the embodiment, dicyclohexyl thiourea is used as an additive, and activated carbon is used for recovering gold in a thiosulfate system, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
（2）100 mL，Au(S2O3)2 3-0.5g/L dicyclohexylthiourea was added to the gold-leaching solution at a concentration of 40 mg/L to adjust the pH to 9.
(3) And (3) adding 1.0g of activated carbon (the solid-to-liquid ratio is 1: 100) into the solution obtained in the step (2), and stirring and adsorbing the gold for 8 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 68%.
Comparative example 4
Under other conditions and with similar adsorption rate, the active carbon is modified by dicyclohexyl thiourea and then Au (S) is adsorbed2O3)2 3-Modified 1.0g of activated carbon, 1.0g of dicyclohexylthiourea and example 4But only 0.05 g.
Under other conditions and the similar using amount of dicyclohexyl thiourea, the dicyclohexyl thiourea is adopted to modify the activated carbon and then adsorb Au (S)2O3)2 3-The adsorption rate was 38%.
Example 5
In this embodiment, 1,2, 3-thiadiazole cyclic thiourea is used as an additive, and the activated carbon is used to recover gold in a thiosulfate system, which includes the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
（2）100 mL，Au(S2O3)2 3-1g/L of 1,2, 3-thiadiazole cyclic thiourea is added into the gold leaching solution with the concentration of 50mg/L, and the pH value is adjusted to 11.
(3) And (3) adding 1.0g of activated carbon (the solid-to-liquid ratio is 1: 100) into the solution obtained in the step (2), and stirring and adsorbing the gold for 12 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 75%.
Comparative example 5
Under other conditions and with similar adsorption rate, 1,2, 3-thiadiazole cyclic thiourea is adopted to modify the activated carbon, and then Au (S) is adsorbed2O3)2 3-The modified 1.0g of activated carbon, the dosage of the 1,2, 3-thiadiazole ring thiourea is 2.0g, and the dosage of the 1,2, 3-thiadiazole ring thiourea in example 5 is only 0.1 g.
Under other conditions and the similar using amount of the 1,2, 3-thiadiazole cyclic thiourea, the 1,2, 3-thiadiazole cyclic thiourea is adopted to modify the activated carbon and then adsorb Au (S)2O3)2 3-The adsorption rate was 55%.
Example 6
In the embodiment, thiosemicarbazide is used as an additive, and the gold in a thiosulfate system is recovered by using activated carbon, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
（2）100 mL，Au(S2O3)2 3-1g/L of 1,2, 3-thiadiazole cyclic thiourea is added into the gold leaching solution with the concentration of 80 mg/L, and the pH value is adjusted to 11.
(3) And (3) adding 1.0g of activated carbon (the solid-to-liquid ratio is 1: 100) into the solution obtained in the step (2), and stirring and adsorbing the gold for 12 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 80%.
Comparative example 6
Under other conditions and with similar adsorption rate, the active carbon is modified by the thiosemicarbazide, and then Au (S) is adsorbed2O3)2 3-1.0g of modified carbon, 2.0g of thiosemicarbazide and only 0.1g of thiosemicarbazide in example 6.
Under other conditions and the condition that the dosage of the thiosemicarbazide is similar to that of the thiosemicarbazide, the thiosemicarbazide is adopted to modify the activated carbon, and then Au (S) is adsorbed2O3)2 3-The adsorption rate was 52%.
Example 7
In the embodiment, a mixture (mass ratio is 1:1: 1) of thiourea, propenyl thiourea and phenylthiourea is used as an additive, and the gold in a thiosulfate system is recovered by using activated carbon, and the method comprises the following steps:
(1) washing the activated carbon with deionized water, removing ash, filtering and drying for later use.
（2）100 mL，Au(S2O3)2 3-1g/L of a mixture of thiourea, propenyl thiourea, phenylthiourea, dicyclohexylthiourea, 1,2, 3-thiadiazole cyclic thiourea and thiosemicarbazide is added into the gold leaching solution with the concentration of 100 mg/L, and the pH value is adjusted to 12.
(3) And (3) adding 1.0g of activated carbon (the solid-to-liquid ratio is 1: 100) into the solution obtained in the step (2), and stirring and adsorbing the gold for 24 hours.
The gold concentration was sampled and analyzed, and the adsorption rate was calculated to be 100%.
Comparative example 7
Under other conditions and with similar adsorption rates, sulfur is usedModification of activated carbon by urea, propenyl thiourea and phenylthiourea, and adsorption of Au (S)2O3)2 3-The modified carbon is 1.0g, the dosage of thiourea, acrylthiourea and phenylthiourea is 3.0g, and the dosage of thiourea, acrylthiourea and phenylthiourea in example 7 is only 0.1 g.
Under other conditions and under the condition that the using amount of thiourea, propenyl thiourea and phenylthiourea is similar, thiourea, propenyl thiourea and phenylthiourea are adopted to modify the activated carbon, and then Au (S) is adsorbed2O3)2 3-The adsorption rate was 55%.
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 (4)
1. A method for directly recovering gold in a thiosulfate system is characterized by comprising the following steps:
(1) washing activated carbon with deionized water, removing ash, filtering, and oven drying
(2) To Au (S)2O3)2 3-Adding an additive into the gold leaching solution, wherein the additive is thiourea or a thiourea derivative, the additive amount of the additive is 0.001-1 g/L, and the pH value is adjusted to 6-12;
(3) adding the activated carbon obtained in the step (1) into the gold leaching solution obtained in the step (2) to react with gold (Au (S)2O3)2 3-) Stirring and adsorbing;
the derivative of thiourea is propenyl thiourea, phenylthiourea, dicyclohexyl thiourea, 1,2, 3-thiadiazole thiourea or thiosemicarbazide.
2. The method of direct recovery of gold in a thiosulfate system in accordance with claim 1 characterized in that: the concentration of thiosulfate in the gold leaching solution is 0.01-3 mol/L.
3. The method of direct recovery of gold in a thiosulfate system according to claim 1 characterized in that: the ratio (mL: g) of the volume of the gold leaching solution to the mass of the activated carbon in the step (3) is 100: 0.1-100: 1.
4. The method of direct recovery of gold in a thiosulfate system according to claim 1 characterized in that: and (3) stirring and adsorbing the gold solution in the step (3) for 0.1-24 h at 15-70 ℃.
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