CN115232964B - Method for extracting gold from alkaline solution of gold thiosulfate complex based on natural eutectic solvent - Google Patents
Method for extracting gold from alkaline solution of gold thiosulfate complex based on natural eutectic solvent Download PDFInfo
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Abstract
The application discloses a method for extracting gold from a thiosulfate complex alkaline solution based on a natural eutectic solvent. The method comprises the steps of adding a certain content of natural eutectic solvent, potassium phosphate and gold thiosulfate solution to construct a natural eutectic solvent double-aqueous-phase system, reacting at room temperature and normal pressure, and standing for separation. After extraction, gold is efficiently enriched in the natural eutectic solvent phase. The invention adopts the natural eutectic solvent as the extractant, has natural sources of raw materials, low cost and 100 percent of atom utilization rate, and overcomes the defects of high volatility, high toxicity and the like of the traditional solvent which pollute the environment. Meanwhile, the constructed natural eutectic solvent double-water-phase system has the advantages of low energy consumption, low cost, high extraction and separation efficiency, simple required equipment and easy operation, and is suitable for industrial mass production.
Description
Technical Field
The application relates to the technical field of gold extraction, in particular to a method for extracting gold from an alkaline solution of a gold thiosulfate complex based on a natural eutectic solvent.
Background
Cyanidation is the predominant process currently used to extract gold from ores. As cyanide is a highly toxic chemical, a large amount of cyanide-containing tailings and cyanide-containing wastewater are generated in the gold extraction process, and environmental pollution is very easy to cause.
With the increasing attention of people on the environmental pollution problem, the cyanide yellow leaching process is gradually limited, and the cyanide-free environment-friendly gold leaching process is gradually paid attention to. Because thiosulfate has the advantages of no toxicity, low cost, good ore adaptability, high efficiency, quick leaching kinetics and the like, the gold leaching process from the ore by using thiosulfate is the most promising non-cyanide environment-friendly gold leaching process at present.
At present, the method for recovering gold from thiosulfate leaching solution mainly comprises the following steps: metal substitution, resin exchange and activated carbon adsorption. Patent CN114672660a uses a three-electrode system to apply voltage to copper-containing aminothiosulfate gold leaching solution, then adds a proper amount of zinc powder into the systemAnd reducing the gold by the copper powder and the aluminum powder, and filtering, pickling and purifying the reduced solution to obtain pure gold. The method has the defects of large consumption of exchange metal, complex subsequent refining process and serious environmental pollution. Patent CN107400778A reports the adsorption of gold from gold thiosulfate solutions with strongly basic anion exchange resins, followed by Na 2 SO 3 And Na (Na) 2 SO 4 The mixed solution of (2) is used as a desorbing agent to desorb the supported gold thiosulfate complex ions. The resin exchange method has the problems of poor selectivity, easy breakage of resin, difficult elution and the like. Patent CN111004922a reports the use of thiols as an additive, followed by the adsorption of gold using commercial activated carbon. Due to the complex Au (S) 2 O 3 ) 2 3- The negative charge of the catalyst is high, the affinity of the catalyst to the activated carbon is poor, and the recovery efficiency of gold is greatly reduced.
Solvent extraction has high selectivity to metal ions and is a suitable method for recovering gold thiosulfate. Patent CN113802012a reports that gold in thiosulfate leachate is extracted by a solvent extraction method using diphenyl phosphine and a derivative thereof as an extractant and toluene as a diluent, wherein the gold extraction rate can reach 99% at the highest. However, in the solvent extraction process, toluene which is a carcinogenic solvent is used as a diluent, and diphenyl phosphine and derivatives thereof are GHS 07-class harmful substances; phase separation extraction is performed by virtue of the hydrophobicity of the extractant and the diluent. The solvent extraction process often uses a large amount of toxic, volatile and difficult-to-degrade organic solvents, which easily causes environmental problems.
The natural deep eutectic solvent is a natural deep eutectic solvent obtained by taking natural compounds as hydrogen bond acceptors and hydrogen bond donors and through hydrogen bond combination, and has excellent biodegradability, environmental compatibility and stability. The eutectic solvent is mainly used in extraction of bioactive materials. For example Yu Feng, the existing various natural eutectic solvent systems are screened, betaine, L-lactic acid and water are used as the eutectic solvent systems for ultrasonic extraction, and the yield of chlorogenic acid in eucommia ulmoides leaves is 31.46mg/g. (Yu Feng, wang Zhihong, zhang Guangyao, du Zhiyun, peng Mijun. Natural eutectic solvent extraction of eucommia ulmoides leaf chlorogenic acid and its antioxidant Activity [ J ]. Forest chemical and Industrial, 2022,42 (01): 101-109.)
The natural eutectic solvent is used as an extraction solvent after at least one organic matter is combined with other organic matters or inorganic matters, and the solvent is especially suitable for extracting certain organic matters from various natural solution systems containing a large amount of complex organic matters according to the similar principle of compatibility. Natural eutectic solvents are very hydrophilic, readily soluble in water, and not readily soluble in organic diluents, and therefore are difficult to apply to extraction of metal ions in aqueous solutions by conventional solvent extraction processes.
However, the following problems exist in the direct use of natural eutectic solvents for the extraction of gold from gold thiosulfate solutions:
(1) Au (I) in thiosulfate solutions is often present as a stable complex Au (S) 2 O 3 ) 2 3- Exists in the form of Au (S 2 O 3 ) 2 3- Is of high negative charge, has poor affinity with most natural eutectic solvents, and has low gold extraction efficiency. The existing natural eutectic solvents are various, but the combination of the eutectic solvents cannot be determined, so that the existing natural eutectic solvents have higher extraction rate on gold;
(2) Complex impurities such as copper, cobalt, nickel and the like often exist in thiosulfate leaching solutions. At the same time, elemental sulfur, polythioates, and other sulfides are often present in the solution. The complexity of thiosulfate gold leaching chemical systems increases the difficulty of high-efficiency, high-selectivity extraction of gold sulfite complexes with eutectic solvents.
(3) Furthermore, the natural eutectic solvent has strong hydrophilicity, is easily dissolved in water and is not easily dissolved in an organic diluent, so that the natural eutectic solvent is difficult to apply to the extraction of the gold thiosulfate complex in the aqueous solution by the traditional solvent extraction process. Thus, there is currently no report on gold recovery from thiosulfate leaching systems using natural eutectic solvents.
Disclosure of Invention
The application provides an extraction method of gold in a gold thiosulfate complex alkaline solution based on a natural eutectic solvent, which is used for solving the technical problems of poor selectivity, low extraction separation efficiency, environment harm of the solvent, low purity of gold after separation and complex purification treatment operation in the recovery of gold from a thiosulfate leaching system in the prior art.
The application provides a method for extracting gold in a gold thiosulfate complex alkaline solution based on a natural eutectic solvent, which comprises the following steps:
step S1: after mixing the component A and the component B, stirring for 1-2 hours at 80-90 ℃, and cooling to obtain a transparent uniform natural eutectic solvent;
step S2: adding potassium phosphate solution into the obtained natural eutectic solvent, and then adding the natural eutectic solvent into alkaline solution of the thiogold sulfite complex with gold concentration of 1-200 mg/L;
step S3: oscillating for 10-30 min at 25 ℃, mixing the solution system uniformly, standing until phase separation is completed, and taking the lower phase as Jin Fuji phase;
the combination of the component A and the component B is any one of choline chloride/xylitol, choline chloride/lactic acid or betaine hydrochloride/lactic acid;
the molar ratio of the component A to the component B is as follows: 1:1.
The natural eutectic solvent prepared by the combination and mixing can be used for extracting the alkaline solution containing the gold thiosulfate complex according to the operation, so that the gold element contained in the alkaline solution can be effectively extracted, the extraction rate can reach 100%, and the extraction efficiency is higher.
More preferably, the gold concentration in the alkaline solution containing the gold thiosulfate complex is 10, 50, 25mg/L. The extraction rate can reach 100%, and the extraction efficiency is high.
The extraction solvents are organic matters, and the A component and the B component in the organic matters are in hydrogen bond connection to generate a natural eutectic solvent, and the application provides Fourier infrared figures 1, 3 and 5. During the extraction process, the gold thiosulfate to be extracted is matched with anion Au (S 2 O 3 ) 2 3- Substitution of chloride ions Cl in natural eutectic solvent molecules by electrostatic action - Nitrogen positive ion N in A component + Generating stable ion pairs, the same asAnd a new stable hydrogen bond connection is formed with the component B, so that the high-efficiency extraction of gold element in the gold thiosulfate complex solution is realized. The molecular structure of the obtained betaine hydrochloride-lactic acid natural eutectic solvent is shown in figure 2; the molecular structure of the obtained choline chloride-lactic acid natural eutectic solvent is shown in figure 4; the molecular structure of the obtained choline chloride-xylitol natural eutectic solvent is shown in figure 6
The aqueous two-phase system provided by the application is an aqueous two-phase system formed by a polymer and a salt. Unlike traditional extraction system, the double water phase system has no great amount of volatile and toxic organic solvent, water as the main component, low cost, high biocompatibility and environment friendship, and is one new kind of solvent extraction process to replace traditional solvent extraction technology.
The aqueous two-phase system of the natural eutectic solvent newly developed by the application can be used for extracting and separating metal ions, can combine the dual advantages of a green extractant (natural eutectic solvent) and the aqueous two-phase system, does not need to use an organic solvent, and realizes the real green environment-friendly characteristic.
Preferably, component a is betaine hydrochloride and component B is lactic acid; betaine hydrochloride and lactic acid are added according to a molar ratio of 1:1. After the combined eutectic solvent is used for extracting the alkaline solution containing the gold thiosulfate complex, the extraction rate of gold elements in the upper phase can reach 100%.
Preferably, component a is choline chloride and component B is xylitol; choline chloride and xylitol are added in a molar ratio of 1:1. When the eutectic solvent obtained by the combination is used for extraction, the extraction rate of gold element in the upper phase can reach 100 percent.
Preferably, component a is choline chloride and component B is lactic acid; choline chloride and lactic acid are added in a molar ratio of 1:1. When the eutectic solvent obtained by the combination is used for extraction, better selectivity can be obtained, and when the alkaline solution containing the gold thiosulfate complex contains copper, nickel and cobalt, the extraction rate of gold element in the upper phase after extraction is 97%; the extraction rates of copper, nickel and cobalt in the lower phase were 0.0%, 0.0% and 8.8%, respectively.
Preferably, the concentration of the potassium phosphate solution is 30.0 to 40.0wt%. The potassium sulfate solution with the concentration can effectively realize the separation of the solution into an upper water phase and a lower water phase.
Preferably, step S3: and (5) oscillating for 20min, and standing for 10min after oscillating.
The beneficial effects that this application can produce include:
1) The method for extracting gold in the gold thiosulfate complex alkaline solution based on the natural eutectic solvent selects N + The betaine hydrochloride or choline chloride of the component A of the group and the natural acid or alcohol of the component B with carboxyl or hydroxyl are synthesized into a stable hydrophilic natural eutectic solvent. The double-aqueous-phase system is constructed by the natural eutectic solvent and the inorganic salt solution to extract gold in the gold thiosulfate complex solution, so that the technical problem that the eutectic solvent is difficult to use for gold extraction in the gold thiosulfate aqueous solution is overcome. Meanwhile, when the gold thiosulfate complex is added into the natural eutectic solvent-two-aqueous phase system, the anion Au (S 2 O 3 ) 2 3- Substitution of the chloride anion in the natural eutectic solvent molecule precursor component A with the N-cation in component A + Generating stable ion pairs through electrostatic attraction, generating new hydrogen bonds with carboxyl or hydroxyl in the component B, and stabilizing the extracted ion pairs by the new hydrogen bonds, thereby realizing effective extraction of the gold sulfite thiosulfate complex. Therefore, the natural eutectic solvent provided by the application solves the problem of the prior art of Au (S 2 O 3 ) 2 3- High charge, weak affinity with most extractants and difficult extraction. The constructed natural eutectic solvent double-water-phase system has the advantages of being green, efficient, low in energy consumption, low in cost, high in separation efficiency, simple and mild in process condition, easy to industrialize and the like; the advantages of the eutectic solvent, such as small vapor pressure, difficult volatilization and good biocompatibility, are also achieved; meanwhile, the defects that the ionic liquid is high in cost, high in toxicity and not easy to realize industrial production are overcome.
2) The gold extraction method in the gold thiosulfate complex alkaline solution based on the natural eutectic solvent has the advantages that the used natural eutectic solvent is good in chemical stability, nontoxic, high in gold extraction efficiency, biodegradable and environment-friendly, and the defects of high toxicity and high volatility of an organic solvent and easiness in causing environmental pollution are overcome. The natural eutectic solvent has natural raw material source, low cost, 100% of atom utilization rate and environmental friendliness. The natural eutectic solvent double-aqueous phase system is simple and convenient to operate, short in extraction time and high in extraction efficiency, and gold in thiosulfate leaching liquid can be completely extracted within 20 minutes.
3) According to the extraction method of gold in the gold thiosulfate complex alkaline solution based on the natural eutectic solvent, the constructed natural eutectic solvent double-aqueous-phase system is green, efficient and low in cost, and the extraction rate of gold thiosulfate enriched in the natural eutectic solvent relative to 1-50 mg/L can reach 100.0%. The energy consumption in the extraction process is low, the extraction can be completed at the normal temperature of 25 ℃, and the separation can be completed automatically without the assistance of external force. The extraction condition is mild, the required equipment is simple, the operation is easy to operate by hands, and the industrial production is convenient.
Drawings
FIG. 1 is a Fourier infrared spectrum of betaine hydrochloride, lactic acid and synthetic betaine hydrochloride-lactic acid natural eutectic solvents provided herein; in the infrared spectrum of pure lactic acid in FIG. 1, 3445.90cm -1 The broad peak of (C) corresponds to the telescopic vibration absorption peak of-OH, when the natural eutectic solvent is generated, the telescopic vibration absorption band of-OH is dispersed and widened, and the frequency is red shifted to 3338.26cm -1 The method comprises the steps of carrying out a first treatment on the surface of the This result indicates that-OH in the carboxyl group of lactic acid forms intermolecular hydrogen bonds with chloride ions in betaine hydrochloride, which is a typical feature of natural eutectic solvent synthesis; meanwhile, in the pure lactic acid infrared spectrum, the stretching vibration peak of C=O is positioned at 1728.61cm -1 After the natural eutectic solvent is generated, the stretching vibration peak of C=O shifts blue to 1740.54cm -1 The method comprises the steps of carrying out a first treatment on the surface of the This is because, after intermolecular hydrogen bonds are formed, the electron cloud between c=o originally close to the oxygen atom is moved to the carbon atom to some extent, thereby affecting the stretching vibration of c=oThe method comprises the steps of carrying out a first treatment on the surface of the The result of Fourier infrared spectrum proves that the betaine hydrochloride and the lactic acid generate a natural eutectic solvent by virtue of hydrogen bonding;
FIG. 2 is a molecular structure diagram of the betaine hydrochloride-lactic acid natural eutectic solvent provided in the present application;
FIG. 3 is a Fourier infrared spectrum of the natural eutectic solvents of choline chloride, lactic acid and synthetic choline chloride-lactic acid provided herein; 3445.90cm in the spectrum of pure lactic acid -1 The broad peak of (C) corresponds to the telescopic vibration absorption peak of-OH, when the natural eutectic solvent is generated, the telescopic absorption band of-OH is dispersed and widened, and the frequency is red shifted to 3362.58cm -1 This suggests that-OH in the lactic acid carboxyl group forms intermolecular hydrogen bonds with chloride ions in choline chloride, which is a typical feature of natural eutectic solvent synthesis; the C=O stretching vibration peak in the pure lactic acid spectrum is 1728.61cm -1 After the natural eutectic solvent was generated, the stretching vibration peak of c=o blue shifted to 1732.50cm -1 The method comprises the steps of carrying out a first treatment on the surface of the This is because the generation of intermolecular hydrogen bonds causes electron clouds between c=o originally close to the oxygen atoms to move to carbon atoms to some extent, thereby affecting the stretching vibration of c=o; the result of Fourier infrared spectrum proves that the choline chloride and the lactic acid generate a natural eutectic solvent by virtue of hydrogen bonding;
FIG. 4 is a molecular structure diagram of the choline chloride-lactic acid natural eutectic solvent provided herein;
FIG. 5 is a Fourier infrared spectrum of the natural eutectic solvents of choline chloride, xylitol and synthetic choline chloride-xylitol provided herein; in the pure xylitol spectrum of FIG. 5, 3394.26cm -1 The broad peak of (2) corresponds to the telescopic vibration absorption peak of-OH, after the natural eutectic solvent is generated, the telescopic vibration absorption band of the corresponding-OH is dispersed and widened, and the frequency is red shifted to 3372.82cm -1 This suggests that-OH in the xylitol hydroxyl group forms intermolecular hydrogen bonds with chloride ions in choline chloride, which is a typical feature of natural eutectic solvent synthesis relying on hydrogen bonding;
fig. 6 is a molecular structure diagram of the choline chloride-xylitol natural eutectic solvent provided in the present application.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments.
Technical means which are not described in detail in the application and are not used for solving the technical problems of the application are all arranged according to common general knowledge in the field, and various common general knowledge arrangement modes can be realized.
Examples
And (3) measuring the gold content in the inorganic salt enrichment lower phase by adopting a flame atomic absorber, and calculating the gold content in the eutectic solvent enrichment upper phase according to the principle of mass conservation. The extraction efficiency (E%) of gold thiosulfate is calculated from the following formula:
wherein C is Auo And V Auo Representing the concentration and volume of gold in the original gold thiosulfate solution, cs and Vs represent the concentration of gold thiosulfate in the inorganic salt-enriched lower phase and the volume of the inorganic salt-enriched lower phase, respectively.
Example 1:
(1) Eutectic solvent synthesis: firstly, 15.36g of betaine and 9.00g of lactic acid (the molar ratio is 1:1) are weighed, then are mixed and stirred for 2 hours at the temperature of 80 ℃ to obtain a uniform transparent eutectic solvent, and then are subjected to Fourier infrared spectrum characterization, as shown in figure 1, and the molecular structural formula of the obtained betaine hydrochloride-lactic acid natural eutectic solvent is shown in figure 2. The result shows that after the natural eutectic solvent is formed, the-OH telescopic vibration absorption band in lactic acid carboxyl becomes dispersed and widened, and the frequency is 3445.90cm of that of pure lactic acid -1 Red shifted to 3338.26cm -1 . Proves that the-OH in the lactic acid carboxyl group and the chloride ion in the betaine hydrochloride form intermolecular hydrogen bonds, and proves that the betaine hydrochloride-lactic acid natural eutectic solvent is successfully synthesized.
(2) 1.25g of a natural eutectic solvent was added with a solution containing 1.75g of potassium phosphate (potassium phosphate concentration: 30.0 wt%) and then with 1.0mL of gold thiosulfate solution having a gold concentration of 25.0mg/L, and finally the total weight of the aqueous two-phase system was made up to 5g with deionized water having a pH of 9.0, to obtain a natural eutectic solvent/potassium phosphate aqueous two-phase system. Three parallel experiments were performed for each set of experiments;
(3) And (3) placing the solution system obtained in the step (2) on a constant-temperature oscillator at 25 ℃ for oscillating for 20min, ensuring uniform mixing of the whole system, standing for 10min, selecting a lower phase which is easier to measure the gold content after phase separation is completed, measuring, and calculating the gold content in the upper phase which is actually enriched in gold according to mass conservation. Measuring the volume of a lower phase (inorganic salt enrichment phase), and then measuring the concentration of gold element in the obtained inorganic salt enrichment phase by using a flame atomic spectrophotometer;
(4) The extraction rate of gold in the natural eutectic solvent phase of the method provided in this example was calculated to be 100.0% according to formula (1).
(5) Gold enriched in the natural eutectic solvent is reduced by hydrazine hydrate to obtain pure gold.
Example 2:
(1) Eutectic solvent synthesis: 13.96g of choline chloride and 9.00g of lactic acid were first weighed, then mixed and stirred at 80 ℃ for 2 hours to obtain a uniform transparent eutectic solvent, and then fourier infrared spectrum characterization was performed, as shown in fig. 3, and the molecular structure diagram of the obtained choline chloride-lactic acid natural eutectic solvent is shown in fig. 4. The results show that after the natural eutectic solvent is generated, the telescopic vibration absorption band of-OH is dispersed and widened, and the frequency is 3445.90cm of that of pure lactic acid -1 Red shifted to 3362.58cm -1 . Proved that the-OH in the lactic acid carboxyl group and the chloride ion in the choline chloride form intermolecular hydrogen bonds, and the choline chloride-lactic acid natural eutectic solvent is successfully synthesized.
(2) Adding a solution containing 1.625g of potassium phosphate (the concentration of the potassium phosphate is 40.0 wt%) into 1.25g of a natural eutectic solvent to obtain a solvent test solution, adding 1.0mL of a mixed solution (the mixed solution is obtained by mixing gold thiosulfate solution (gold concentration of 800 mg/L), copper ammonia solution (copper concentration of 800 mg/L), nickel ammonia solution (nickel concentration of 800 mg/L) and cobalt ammonia ion solution (cobalt concentration of 800 mg/L) according to a volume ratio of 1:1:1:1) into the solvent test solution, adding 200mg/L of gold, 200mg/L of copper, 200mg/L of nickel and 200mg/L of cobalt into the mixed solution, and finally supplementing the total weight of the aqueous two-phase system to 5g by deionized water with a pH value of 9.0 to obtain the natural eutectic solvent/potassium phosphate aqueous two-phase system. Three replicates were run for each set of experiments.
(3) Placing the natural eutectic solvent double water phase into a constant temperature oscillator with the temperature of 25 ℃ to oscillate for 20min, ensuring that the whole system is uniformly mixed, and then standing for 10min. After the phase separation is completed, the volume of the lower phase (inorganic salt-enriched phase) is measured, and then the concentrations of gold, copper, nickel and cobalt in the inorganic salt-enriched phase are measured by a flame atomic spectrophotometer.
(4) The extraction rates of gold, copper, nickel and cobalt were calculated according to equation (1). The results show that the extraction rates of gold, copper, nickel and cobalt are 97.0%, 0.0% and 8.8%, respectively, and the constructed aqueous two-phase system has good selectivity on thiosulfuric acid hardware in the presence of other metals.
Example 3:
(1) Eutectic solvent synthesis: 13.96g of choline chloride and 15.22g of xylitol are first weighed, then mixed and stirred at 80 ℃ for 2 hours to obtain a uniform transparent eutectic solvent, and then fourier infrared spectrum characterization is carried out, as shown in fig. 5, and the molecular structure of the obtained choline chloride-xylitol natural eutectic solvent is shown in fig. 6. The results show that after formation of the natural eutectic solvent, the absorption band of-OH is dispersed and broadened, with a frequency of 3394.26cm from pure xylitol -1 Red shifted to 3372.82cm -1 . Proves that the-OH at the xylitol terminal forms intermolecular hydrogen bond with chloride ions in choline chloride, and proves that the natural eutectic solvent choline chloride-xylitol is successfully synthesized.
(2) To 1.25g of the natural eutectic solvent, a solution containing 2.00g of potassium phosphate (potassium phosphate concentration: 35.0 wt%) was added, then 1.0mL of gold thiosulfate solution having a gold concentration of 50.0mg/L was added, and finally deionized water having a pH of 9.0 was added to make up the total weight of the aqueous two-phase system to 5.0g, thereby obtaining a natural eutectic solvent/potassium phosphate aqueous two-phase system. Three replicates were run for each set of experiments.
(3) After the preparation of the natural eutectic solvent double-water phase system is completed, the natural eutectic solvent double-water phase system is placed on a constant temperature oscillator with the temperature of 25 ℃ to oscillate for 20min, so that the whole system is ensured to be uniformly mixed, and then the natural eutectic solvent double-water phase system is placed for 10min. After the phase separation was completed, the volume of the lower phase (inorganic salt-enriched phase) was measured, and then the concentration of gold in the inorganic salt-enriched phase was measured with a flame atomic spectrophotometer.
(4) The extraction rate of gold in the natural eutectic solvent phase of the method provided in this example was calculated to be 100.0% according to formula (1).
(5) Gold enriched in the natural eutectic solvent is reduced by hydrazine hydrate to obtain pure gold.
Example 4:
(1) Eutectic solvent synthesis: 13.96g of choline chloride and 9.00g of lactic acid were first weighed, then mixed and stirred at 80℃for 2 hours to obtain a uniform transparent eutectic solvent, and then subjected to Fourier infrared spectrum characterization as shown in FIG. 3. The results show that after the natural eutectic solvent is generated, the telescopic vibration absorption band of-OH is dispersed and widened, and the frequency is 3445.90cm of that of pure lactic acid -1 Red shifted to 3362.58cm -1 . Proved that the-OH in the lactic acid carboxyl group and the chloride ion in the choline chloride form intermolecular hydrogen bonds, and the choline chloride-lactic acid natural eutectic solvent is successfully synthesized.
(2) 1.25g of natural eutectic solvent is added with 1.50g of potassium phosphate solution, then 1.0mL of gold thiosulfate solution with the gold concentration of 1.0mg/L is added, and finally deionized water with the pH value of 9.0 is added to supplement the total weight of the aqueous two-phase system to 5.0g, so that the natural eutectic solvent/potassium phosphate aqueous two-phase system is obtained. Three replicates were run for each set of experiments.
(3) After the preparation of the natural eutectic solvent double-water phase system is finished, the natural eutectic solvent double-water phase system is placed on a constant temperature oscillator with the temperature of 25 ℃ to oscillate for 30min, so that the whole system is ensured to be uniformly mixed, and then the natural eutectic solvent double-water phase system is placed for 10min. After the phase separation was completed, the volume of the lower phase (inorganic salt-enriched phase) was measured, and then the concentration of gold in the inorganic salt-enriched phase was measured with a flame atomic spectrophotometer.
(4) The extraction rate of gold in the natural eutectic solvent phase of the method provided in this example was calculated to be 100.0% according to formula (1).
(5) Concentrating gold in natural eutectic solvent, and reducing with hydrazine hydrate to obtain pure gold
Example 5:
(1) Eutectic solvent synthesis: 13.96g of choline chloride and 15.22g of xylitol were first weighed, then mixed and stirred at 80℃for 2 hours to obtain a uniform transparent eutectic solvent, and then subjected to Fourier infrared spectrum characterization, as shown in FIG. 5. The results show that after formation of the natural eutectic solvent, the absorption band of-OH is dispersed and broadened, with a frequency of 3394.26cm from pure xylitol -1 Red shifted to 3372.82cm -1 . Proves that the-OH at the xylitol terminal forms intermolecular hydrogen bond with chloride ions in choline chloride, and proves that the natural eutectic solvent choline chloride-xylitol is successfully synthesized.
(2) To 1.25g of the natural eutectic solvent, a solution containing 2.00g of potassium phosphate (the concentration of potassium phosphate is 32.0 wt%) was added, then 1.0mL of gold thiosulfate solution having a gold concentration of 10.0mg/L was added, and finally deionized water having a pH value of 9.0 was added to make up the total weight of the aqueous two-phase system to 5.0g, thereby obtaining a natural eutectic solvent/potassium phosphate aqueous two-phase system. Three replicates were run for each set of experiments.
(3) After the preparation of the natural eutectic solvent double-water phase system is finished, the natural eutectic solvent double-water phase system is placed on a constant temperature oscillator with the temperature of 25 ℃ to oscillate for 10min, so that the whole system is ensured to be uniformly mixed, and then the natural eutectic solvent double-water phase system is placed for 10min. After the phase separation was completed, the volume of the lower phase (inorganic salt-enriched phase) was measured, and then the concentration of gold in the inorganic salt-enriched phase was measured with a flame atomic spectrophotometer.
(4) The extraction rate of gold in the natural eutectic solvent phase of the method provided in this example was calculated to be 100.0% according to formula (1).
(5) Gold enriched in the natural eutectic solvent is reduced by hydrazine hydrate to obtain pure gold.
According to the embodiments 1 to 5, the choline chloride/xylitol, the choline chloride/lactic acid and the betaine/lactic acid provided by the application can not only show a better extraction rate for gold in the gold thiosulfate solution, but also have higher selectivity, and can not be interfered and influenced by other metal elements.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (3)
1. The method for extracting gold in the alkaline solution of the gold thiosulfate complex based on the natural eutectic solvent is characterized by comprising the following steps of:
step S1: mixing the component A and the component B, stirring for 1-2 hours at 80-90 ℃, and cooling to obtain a transparent uniform natural eutectic solvent;
step S2: adding a potassium phosphate solution into the obtained natural eutectic solvent, and then adding an alkaline solution of a gold thiosulfate complex with the gold concentration of 1-200 mg/L;
step S3: oscillating for 10-30 min at 25 ℃, mixing the solution system uniformly, standing until phase separation is completed, and taking an upper phase as Jin Fuji phase; the molar ratio of the component A to the component B is 1:1;
the combination of the component A and the component B is as follows: the component A is choline chloride and the component B is xylitol; alternatively, component a is choline chloride and component B is lactic acid; alternatively, component a is betaine hydrochloride and component B is lactic acid.
2. The method for extracting gold from a gold thiosulfate complex alkaline solution based on a natural eutectic solvent according to claim 1, wherein the concentration of the potassium phosphate solution is 30.0-40.0 wt%.
3. The method for extracting gold from an alkaline solution of a gold thiosulfate complex based on a natural eutectic solvent as claimed in claim 1, wherein the shaking is performed for 20min in step S3, and the mixture is left to stand for 10min after the shaking.
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| WO2018092042A2 (en) * | 2016-11-15 | 2018-05-24 | Landlab S.R.L. | Solvent and method for extracting active compound from plants and use of such a solvent |
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| US6197214B1 (en) * | 1996-06-26 | 2001-03-06 | Henkel Corporation | Ammonium thiosulfate complex of gold or silver and an amine |
| US6660059B2 (en) * | 2000-05-19 | 2003-12-09 | Placer Dome Technical Services Limited | Method for thiosulfate leaching of precious metal-containing materials |
| US6632264B2 (en) * | 2001-04-17 | 2003-10-14 | The University Of British Columbia | Gold recovery from thiosulfate leaching |
| JP2003221628A (en) * | 2002-01-31 | 2003-08-08 | Japan Science & Technology Corp | Method for extracting gold |
| NL2004835C2 (en) * | 2010-06-07 | 2011-12-08 | Univ Leiden | Process for extracting materials from biological material. |
| US9194023B2 (en) * | 2012-10-23 | 2015-11-24 | Barrick Gold Corporation | Recovery of gold from roaster calcine leach tailings |
| CN111004922A (en) * | 2019-12-12 | 2020-04-14 | 昆明理工大学 | Method for recovering gold in thiosulfate system |
| CN113802012A (en) * | 2021-09-08 | 2021-12-17 | 昆明理工大学 | Method for separating gold from thiosulfate gold leaching solution |
| CN114712893A (en) * | 2022-03-26 | 2022-07-08 | 昆明理工大学 | Method for recovering gold in thiosulfate solution |
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| US5284633A (en) * | 1992-11-12 | 1994-02-08 | Sherex Chemical Co., Inc. | Solvent extraction of precious metals with hydroxyquinoline and stripping with acidified thiourea |
| WO2018092042A2 (en) * | 2016-11-15 | 2018-05-24 | Landlab S.R.L. | Solvent and method for extracting active compound from plants and use of such a solvent |
| CN111087299A (en) * | 2019-12-13 | 2020-05-01 | 华南理工大学 | Method for extracting vanillic acid by using eutectic solvent/n-propanol aqueous two-phase system |
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