Method for asynchronous enrichment and continuous determination of platinum and gold in ore

Through the combination of high-temperature strong alkali oxidation and melting and special chelating collectors, the problem of low accuracy in detecting platinum and gold elements in minerals is solved, and efficient asynchronous separation and precise determination of platinum and gold is achieved, which is suitable for rapid detection.

CN119845689BActive Publication Date: 2025-07-22CHANGCHUN GOLD RES INST
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Patent Information

Application Number
CN202510330875.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-20
Publication Date
2025-07-22
Estimated Expiration
2045-03-20

AI Technical Summary

Technical Problem

The existing fire test method is not accurate when detecting the content of platinum and gold in minerals, and it is cumbersome and time-consuming, making it difficult to separate precious metal elements of similar properties.

Method used

The target minerals were mixed with the enrichment agent by high-temperature and strong alkali oxidation and melting method to achieve the transformation of the existence form of platinum and be asynchronously separated from gold. The platinum element was efficiently captured in a strong alkaline environment using a special chelating capture diluent, and the platinum and gold content was determined by ICP-OES and fire test method respectively.

Benefits of technology

It realizes efficient asynchronous separation and precise determination of platinum and gold in minerals, shortens detection time, improves detection accuracy, and meets the needs of rapid detection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application provides a method for asynchronous enrichment and continuous determination of platinum and gold in ores, belonging to the field of detection of the contents of platinum and gold elements in minerals. Among them, minerals containing platinum and gold are melted with enrichment agents to change the valence state of platinum and ensure that the valence state of gold does not change; subsequently, through soaking and filtration, platinum is separated from gold in the form of a solution; then, a special chelating collector diluent is used to efficiently collect platinum elements from the solution obtained by soaking, filtering and separating the molten minerals; this chelating collector uses aliphatic cyclic diols as raw materials, and makes the chemical activities of two hydroxyl groups different by using the unique spatial structure of the molecule, and realizes the derivatization of the asymmetric molecular skeleton through chemical reactions; then an amino group is introduced, and by regulating the types of amino groups and substituents, the chemical activity of the chelating site N is improved; the specific chemical structure combines with the chemical activity of the chelating site to achieve efficient collection of platinum elements, so that the accuracy of the determination of platinum elements can be improved subsequently.
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Description

Technical Field

[0001] The present invention relates to the technical field of detecting the contents of platinum and gold elements in minerals, and particularly relates to a method for asynchronous enrichment and continuous determination of platinum and gold in ores. Background Art

[0002] At present, although the fire assay method is a widely used precious metal detection method, it also has some limitations. For example: First, the operation process is relatively cumbersome and highly dependent on the experience of the operator, requiring professional technical personnel to carry out; Second, it takes a long time. Since it needs to go through multiple smelting and processing steps, the entire detection process may take from several hours to several days, which does not meet the requirements of rapid detection; Third, after several precious metal elements with similar properties are enriched by lead, it is difficult to separate them by the traditional cupellation method. Subsequently, silver in the gold-silver alloy particles can be removed by boiling with nitric acid, but the remaining particle samples contain both platinum and gold at the same time. The method of using the gravimetric method to determine the metal content in minerals fails, so the data measured by conventional methods is not accurate enough.

[0003] In view of this, it is necessary to design a method for asynchronous enrichment and continuous determination of platinum and gold in ores to solve the above problems. Summary of the Invention

[0004] In view of the technical problems existing in the background art, the present application provides a method for asynchronous enrichment and continuous determination of platinum and gold in ores, aiming to solve the technical problem of low detection accuracy of the contents of platinum and gold elements in target minerals by existing detection methods.

[0005] The embodiment of the present application provides a method for asynchronous enrichment and continuous determination of platinum and gold in ores, including the following steps:

[0006] S1. Asynchronously separate the target mineral containing platinum and gold, specifically as follows;

[0007] Mix the target mineral with an enrichment agent and place it at high temperature for melting to obtain a molten mineral; then place the molten mineral in water, soak and filter it in sequence, and separate the solid and the solution;

[0008] The enrichment agent includes a strong base agent and an oxidizing agent;

[0009] S2. Sequentially carry out flotation and content testing on the separated platinum, specifically as follows;

[0010] Mix the solution separated in step S1 with a chelating flotation diluent, and collect the organic phase solution; then add a reverse flotation agent to the organic phase solution, mix it evenly, and collect the inorganic aqueous phase solution; and test the platinum content of the inorganic aqueous phase solution;

[0011] S3. Test the content of the separated gold.

[0012] In this embodiment, a mineral containing platinum and gold elements is mixed with an enrichment agent and then subjected to high-temperature strong alkali oxidation melting to achieve a change in the form of the platinum element in the mineral, while ensuring that the valence state of gold in the mineral does not change; subsequently, the molten mineral can be soaked and filtered to separate the platinum from the mineral in the form of a solution, while the gold remains in the mineral in a solid form, thereby achieving asynchronous separation of platinum and gold in the mineral.

[0013] In some embodiments, in step S2, the chelating collector diluent is prepared by mixing a chelating collector and sulfonated kerosene in a volume ratio of 1:5-10.

[0014] In some embodiments, the chelating collector has the following structural formula:

[0015] .

[0016] In this embodiment, by using a special chelating collector diluent on the solution separated from the melted mineral after soaking and filtering, platinum can be efficiently captured in a strong alkaline environment; wherein, the chelating collector uses aliphatic cyclic diols as raw materials, utilizes the unique spatial structure of the molecule to make the chemical activity of the two hydroxyl groups different, and realizes the derivatization of the asymmetric molecular skeleton through chemical reaction (through nucleophilic substitution reaction, the highly active hydroxyl group is converted into a chloro group, while the less active hydroxyl group does not undergo nucleophilic substitution reaction, ensuring that one side of the original molecular skeleton is derivatized); then, an amine group of a specific structure is introduced, and the original binary hydroxyl group in the amine compound can realize the improvement of the chemical activity of the chelating site N; in this way, under strong alkaline conditions, the specific chemical structure combined with the chemical activity of the chelating site can realize the efficient capture of platinum.

[0017] In some embodiments, in step S1, the melting temperature is 500-700°C.

[0018] In some embodiments, in step S1, the mass ratio of the strong base agent to the oxidant in the enrichment agent is 10~100:1; the strong base agent includes one or more of sodium hydroxide and potassium hydroxide; the oxidant includes one or more of sodium perchlorate, potassium perchlorate, sodium perbromate, and potassium perbromate.

[0019] In some embodiments, in step S1, the mass ratio of the target mineral to the enrichment agent is 1:1-5;

[0020] The ratio of the molten mineral to water is 1-50 g:1 L.

[0021] In some embodiments, in step S2, the volume ratio of the solution to the chelating collector diluent is 1000:1-10.

[0022] In some embodiments, in step S2, the reverse collector includes one or more of a saturated solution of ammonium chloride and ammonia water; the volume ratio of the reverse collector to the chelating collector diluent is 2 to 5:1.

[0023] In some embodiments, in step S2, the method for testing the platinum content of the inorganic aqueous solution includes ICP-OES.

[0024] In some embodiments, in step S3, the method for testing the content of the separated gold includes the fire assay method.

[0025] Beneficial effects:

[0026] In the present invention, by mixing the mineral containing platinum and gold elements with enrichment agents and then subjecting them to high-temperature strong-base oxidative melting, the transformation of the existence form of platinum elements in the mineral is realized, while ensuring that the valence state of gold in the mineral does not change; subsequently, the molten mineral can be soaked and filtered, so that platinum is separated from the mineral in the form of a solution, while gold still remains in the mineral in a solid state. In this way, platinum and gold in the mineral are separated asynchronously first; then, by using a special chelating collector diluent for the solution separated after soaking and filtering the molten mineral, platinum elements can be efficiently collected in a strongly alkaline environment; among them, this chelating collector uses aliphatic cyclic diols as raw materials, and the chemical activities of two hydroxyl groups are different due to the unique spatial structure of the molecule, and the derivatization of the asymmetric molecular skeleton is realized through a series of chemical reactions; subsequently, amino groups are introduced, and by regulating the types of amino groups and substituents, the chemical activity of the chelating site N is improved; thus, under strongly alkaline conditions, the specific chemical structure combined with the chemical activity of the chelating site can achieve the efficient collection of platinum elements, and thus the subsequent accurate determination of platinum elements is completed.

[0027] The above description is only an overview of the technical solution of the present application. In order to be able to understand the technical means of the present application more clearly, it can be implemented according to the content of the specification. And in order to make the above and other purposes, features and advantages of the present application more obvious and understandable, the following specific embodiments of the present application are specifically given. Description of the drawings

[0028] In order to more clearly illustrate the technical solution of the present application, the drawings used in the present application will be briefly introduced below. Obviously, the following described drawings are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0029] Figure 1 It is the synthesis process of the chelating collector in the present application;

[0030] Figure 2 1H NMR spectrum of the chelating collector in this application. Detailed implementation mode

[0031] The embodiments of the technical solutions of this application will be described in detail below with reference to the accompanying drawings. The following embodiments are only used to illustrate the technical solutions of this application more clearly, so they are only examples and cannot be used to limit the protection scope of this application.

[0032] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which this application belongs; the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" and any variations thereof in the specification and claims of this application and the above accompanying drawing descriptions are intended to cover non-exclusive inclusion.

[0033] In the description of the embodiments of this application, technical terms such as "first" and "second" are only used to distinguish different objects and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity, specific order or primary-secondary relationship of the indicated technical features. In the description of the embodiments of this application, "a plurality of" means more than two unless otherwise specifically defined.

[0034] Referring to "embodiments" herein means that specific features, structures or characteristics described in connection with the embodiments can be included in at least one embodiment of this application. The phrase appears in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment mutually exclusive with other embodiments. Those skilled in the art will explicitly and implicitly understand that the embodiments described herein can be combined with other embodiments.

[0035] In the description of the embodiments of this application, the term "and / or" is only a description of the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist simultaneously, and B exists alone. In addition, the character " / " in this article generally represents an "or" relationship between the associated objects before and after.

[0036] In the prior art, the fire assay method is mostly used for the determination method of the content of platinum and gold in minerals, but the measurement accuracy of the content of precious metal elements with similar properties by the fire assay method is not high enough. Therefore, how to provide a determination method that can accurately distinguish the content of precious metal elements with similar properties in minerals is particularly important.

[0037] To solve the above technical problems, the present application provides a method for asynchronous enrichment and continuous determination of platinum and gold in ores. Specifically, minerals containing platinum and gold elements are mixed with enrichment reagents and then subjected to high-temperature strong-base oxidative melting to achieve the transformation of the existing form of platinum elements in the minerals, while ensuring that the valence state of gold in the minerals does not change. Subsequently, a special chelating collector diluent is used for the solution separated after soaking and filtering the melted minerals to efficiently collect platinum elements in a strongly alkaline environment. In this way, after the efficient separation of platinum and gold in the minerals, the respective elements are measured separately, thereby ensuring the accurate determination of the precious metal content in the minerals.

[0038] The embodiments of the present application provide a method for asynchronous enrichment and continuous determination of platinum and gold in ores, including the following steps:

[0039] S1. Asynchronously separate the target minerals containing platinum and gold, specifically as follows;

[0040] Mix the target minerals with the enrichment reagents and place them at high temperature for melting. After reacting for 4 - 6 hours, molten minerals are obtained (to transform the existing form of platinum elements in the target minerals); then place the molten minerals in water, soak and filter them in sequence, and separate the solid and the solution;

[0041] The enrichment reagents include strong-base reagents and oxidants;

[0042] The temperature for melting is 500 - 700 °C;

[0043] The mass ratio of the target minerals to the enrichment reagents is 1:1 - 5;

[0044] The ratio of the molten minerals to water is 1 - 50 g:1 L;

[0045] The mass ratio of the strong-base reagent to the oxidant in the enrichment reagents is 10 - 100:1; the strong-base reagent includes one or more of sodium hydroxide and potassium hydroxide; the oxidant includes one or more of sodium perchlorate, potassium perchlorate, sodium perbromate, and potassium perbromate;

[0046] S2. Perform collection and content testing on the separated platinum, specifically as follows;

[0047] Mix the solution separated in step S1 with the chelating collector diluent according to a volume ratio of 1000:1 - 10, stir for 30 minutes, and collect the organic-phase solution; then add a reverse collector to the organic-phase solution, mix, and stir for another 30 minutes, and collect the inorganic aqueous-phase solution; and perform platinum content testing on the inorganic aqueous-phase solution;

[0048] The reverse collector includes one or more of a saturated solution of ammonium chloride and ammonia water (the concentration of ammonia water is 30%); the volume ratio of the reverse collector to the chelating collector diluent is 2-5:1;

[0049] The method for testing the platinum content of the inorganic aqueous solution includes ICP-OES;

[0050] The calculation formula for the platinum content is: W Pt = C × V / m ×100%;

[0051] Among them, W Pt ——The content of platinum in the target mineral (%);

[0052] C ——The mass concentration of platinum element in the inorganic aqueous solution;

[0053] V ——The volume of the inorganic aqueous solution;

[0054] m ——The mass of the target mineral.

[0055] S3. Test the content of the separated gold,

[0056] The method for testing the content of the separated gold includes the fire assay method, and the specific determination steps refer to "GB / T7739".

[0057] In this way, by mixing the mineral containing platinum and gold elements with the enrichment agent and then undergoing high-temperature strong alkali oxidation melting, the transformation of the existence form of platinum elements in the mineral is realized, and at the same time, it is ensured that the valence of gold in the mineral does not change; subsequently, the molten mineral can be soaked and filtered to separate platinum from the mineral in the form of a solution, while gold still remains in the mineral in a solid state, thus realizing the asynchronous separation of platinum and gold in the mineral;

[0058] Among them, taking potassium hydroxide and potassium perchlorate as examples:

[0059] Pt+KOH+KClO3→K2PtO4+KCl+H2O;

[0060] During the reaction process, platinum (Pt) is melted with potassium hydroxide and potassium chlorate to generate soluble potassium platinite (K2PtO4), while the gold element still exists in the form of elemental gold, thus realizing the separation of elements with similar properties.

[0061] Furthermore, in some embodiments, in step S2, the chelating collector diluent is prepared by mixing a chelating collector and sulfonated kerosene in a volume ratio of 1:5-10.

[0062] Further, in some embodiments, the chelating collector has the following structural formula:

[0063] ;

[0064] The synthesis process of the chelating collector is as follows Figure 1 As shown, the specific preparation method comprises the following steps:

[0065] A1. Synthesize isosorbide into compound B; (For the specific synthesis route and parameters of the preparation method, please refer to the reference "Hydroformylation of Olefinic Derivatives of Isosorbide and Isomannide. J. Org. Chem. 2016, 81, 7510−7517.")

[0066] A2. Add N-di-2-hydroxyethylamine and the compound B prepared in the above steps to a sufficient amount of anhydrous ethanol at a molar ratio of 1.5-3:1; then add an appropriate amount of sodium hydroxide (wherein, anhydrous ethanol: sodium hydroxide = 1L: 6-8g); then react at 50-100°C for 48-72h; after the reaction is completed, remove the solvent by rotary distillation under reduced pressure, and collect a light yellow oil; then add deionized water, ultrasonically dissolve, filter, and remove inorganic substances (alkali, salt); finally, add 200ml-1L of cyclohexane and 200ml-1L of deionized water and extract, collect the organic phase, dry it with anhydrous magnesium sulfate, filter, and collect the liquid phase, and then perform rotary distillation under reduced pressure on the collected liquid phase to remove the solvent, and finally obtain an oily product C, i.e., a chelating collector, with a yield of 57-62%.

[0067] In this way, by using a special chelating collector diluent on the solution separated from the molten mineral after soaking and filtration, the platinum element can be efficiently captured in a strongly alkaline environment; wherein, this chelating collector uses aliphatic cyclic diols as raw materials, utilizes the unique spatial structure of the molecule to make the two hydroxyl groups have different chemical activities, and realizes the derivatization of the asymmetric molecular skeleton through a series of chemical reactions; then, the amine group is introduced, and the chemical activity of the chelating site N is increased by regulating the types of amine groups and substituents; thus, under strongly alkaline conditions, the specific chemical structure combined with the chemical activity of the chelating site can realize the efficient capture of the platinum element, thus completing the subsequent precise determination of the platinum element.

[0068] Further, in some embodiments, in step S2, the reverse collector includes one or more of a saturated solution of ammonium chloride and ammonia water; the volume ratio of the reverse collector to the chelating collector diluent is 2-5:1.

[0069] Some specific embodiments are listed below. It should be noted that the embodiments described below are exemplary and are only used to explain the present application and should not be construed as a limitation of the present application. For those techniques or conditions not specified in the embodiments, they shall be carried out according to the techniques or conditions described in the literature in the art or according to the product instructions. For reagents or instruments not indicated with the manufacturer, they are all conventional products that can be obtained through commercial purchase.

[0070] Example 1

[0071] The embodiment of the present application provides a method for asynchronous enrichment and continuous determination of platinum and gold in ores, including the following steps:

[0072] S1. Asynchronous separation of the target minerals containing platinum and gold is carried out as follows;

[0073] According to a mass ratio of 1:5, a standard ore sample (10 g) (the content of gold in the standard ore sample is 11.51 g / t, and the content of platinum is 26.7 g / t) and an enrichment reagent (50 g) (the enrichment reagent is composed of potassium hydroxide and potassium perchlorate with a mass ratio of 49 g:1 g) are mixed evenly and then placed at a high temperature of 600 °C for melting. After reacting for 4 h, a molten mineral is obtained; then the crushed molten mineral is placed in water (the ratio of the molten mineral to water is 10 g:1 L), and is soaked (for 30 min) and filtered in sequence to separate the solid and the solution;

[0074] S2. The collected platinum is sequentially subjected to collection and content testing as follows;

[0075] 5 mL of a chelating collector diluent is added to the solution obtained in step S1, and after mixing, it is stirred for 30 min to collect the organic phase solution; then 20 mL of a reverse collector (saturated solution of ammonium chloride) is added to the organic phase solution, and after mixing, it is stirred for another 30 min to collect the inorganic aqueous phase solution; and the platinum content of the inorganic aqueous phase solution is tested;

[0076] The chelating collector diluent is formed by mixing a chelating collector and sulfonated kerosene according to a volume ratio of 1:5; the structural formula of the chelating collector is as follows:

[0077] ;

[0078] Among them, the synthesis route of the chelating collector in the present application is as Figure 1 shown, and the specific preparation method includes the following steps:

[0079] A1. Synthesize isosorbide into compound B; (For the synthetic route and specific parameters of the specific preparation method, please refer to the reference "Hydroformylation of Olefinic Derivatives of Isosorbide and Isomannide. J. Org. Chem. 2016, 81, 7510−7517.");

[0080] A2. According to the molar ratio of 3:1, add N-di-2-hydroxyethylamine and the compound B prepared in the above step into 2 L of anhydrous ethanol; then add 32 g of sodium hydroxide with a concentration of 0.4 mol / L; then react at 80 °C for 72 h; after the reaction, use rotary evaporation under reduced pressure to remove the solvent, and collect the pale yellow oil; then add deionized water, dissolve it by ultrasonic treatment, filter to remove inorganic substances (alkali, salt); finally, add 1 L of cyclohexane and 1 L of deionized water for extraction, collect the organic phase, dry it with anhydrous magnesium sulfate, filter to collect the liquid phase, and then perform rotary evaporation under reduced pressure on the collected liquid phase to remove the solvent, and finally obtain the oily product C, that is, the chelating collector, and its yield is 57 - 62%;

[0081] The data of the nuclear magnetic resonance hydrogen spectrum ( 1 H-NMR) of the chelating collector are as follows: chemical shift 2.00 - 2.99, 4H; 3.00 - 3.99, 7H; 4.00 - 4.50, 6H; the nuclear magnetic resonance hydrogen spectrum is as shown in Figure 2 Figure.

[0082] The method for testing the platinum content in the inorganic aqueous solution is ICP-OES;

[0083] The calculation formula for the platinum content is: W Pt = C × V / m ×100%;

[0084] Among them, W Pt ——The content of platinum in the target mineral (%);

[0085] C ——The mass concentration of platinum element in the inorganic aqueous solution;

[0086] V ——The volume of the inorganic aqueous solution;

[0087] m ——The mass of the target mineral;

[0088] S3. Test the content of the separated gold,

[0089] The method for testing the content of the separated gold is the fire assay method, and the specific process refers to "GB / T 7739".

[0090] Among them, .

[0091] Examples 2 to 3

[0092] Examples 2 to 3 respectively provide a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the target minerals selected in step S1 are different. The target mineral selected in Example 2 is a standard ore sample with a standard gold content of 120.89 g / t and a platinum content of 17.6 g / t; the target mineral selected in Example 3 is a standard ore sample with a standard gold content of 5.00 g / t and a platinum content of 897.1 g / t. The remaining steps are the same as those in Example 1 and will not be repeated here.

[0093] The specific determination results of Examples 1 to 3 are shown in Table 1.

[0094] Table 1 Standard values and experimental determination values of element contents in the target minerals of Examples 1 to 3

[0095]

[0096] As can be seen from Table 1, an efficient method for asynchronous enrichment and continuous determination of platinum and gold provided by this application has high accuracy in standard mineral samples with different content ratios, and the error range is less than 3%, meeting the requirements of existing tests and their standards.

[0097] Examples 4 to 5

[0098] Examples 4 to 5 respectively provide a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the enrichment agents in step S1 are different. The ratio of the strong base agent to the oxidant in the enrichment agent of Example 4 is 10:1; the ratio of the strong base agent to the oxidant in the enrichment agent of Example 5 is 90:1. The remaining steps are the same as those in Example 1 and will not be repeated here.

[0099] Examples 6 to 7

[0100] Examples 6 to 7 respectively provide a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the content of the reverse collector in step S2 is different. The volume ratio of the reverse collector to the chelating collector diluent in Example 6 is 2:1; the volume ratio of the reverse collector to the chelating collector diluent in Example 7 is 5:1. The remaining steps are the same as those in Example 1 and will not be repeated here.

[0101] Comparative Example 1

[0102] Comparative Example 1 provides a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the enrichment agents in step S1 are different. In the enrichment agents of Comparative Example 1, the ratio of the strong base agent to the oxidizing agent is 8:1. The other steps are the same as those in Example 1 and will not be elaborated here.

[0103] Comparative Examples 2 - 3

[0104] Comparative Examples 2 - 3 respectively provide a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the content of the reverse collector in step S2 is different. In Comparative Example 2, the volume ratio of the reverse collector to the chelating collector diluent is 1:1; in Comparative Example 3, the volume ratio of the reverse collector to the chelating collector diluent is 7:1. The other steps are the same as those in Example 1 and will not be elaborated here.

[0105] The specific measurement results of Examples 4 - 6 and Comparative Examples 1 - 2 are shown in Table 2.

[0106] Table 2 Standard values and experimental measurement values of element contents in the target minerals of Examples 4 - 6 and Comparative Examples 1 - 2

[0107]

[0108] The reason for the large error in Comparative Example 3 is that after there is too much reverse collector, it cannot all dissolve.

[0109] Comparative Examples 4 - 5

[0110] Comparative Examples 4 - 5 respectively provide a method for asynchronous enrichment and continuous determination of platinum and gold in ore. The difference from Example 1 is that the types of chelating collector diluents in step S2 are different. The specific structural formulas of the chelating collectors in the reverse collectors of Comparative Example 4 and Comparative Example 5 are shown in Table 3. The other steps are the same as those in Example 1 and will not be elaborated here. The final platinum capture ability and the measurement results of each element in the minerals of Comparative Examples 4 - 5 are shown in Table 3.

[0111] Table 3 Platinum capture ability and measurement results of each element in the minerals of Example 1 and Comparative Examples 4 - 5

[0112]

[0113] As can be seen from Table 3, the chelating collector prepared in Example 1 has excellent chelating effect on platinum, while the chelating collectors involved in Comparative Examples 4-5 cannot carry out effective chelating reaction with platinum. The main reason is attributed to the difference in the molecular spatial structure of the chelating collector: the chelating collector in Example 1 has a cyclic structure with spatial specificity - a spatial V-shaped structure; while the chelating collectors in Comparative Examples 4-5 have a binary cyclic structure in the same plane, making it difficult to achieve the synergistic chelation of the N atom and the oxygen atom of the para-hydroxy group in the heterocycle to the target metal ion, and thus a stable chelate cannot be formed; this difference in spatial structure leads to the difference in the chelating effect on platinum element.

[0114] As can be seen from Tables 2-3, an efficient method for asynchronous enrichment and continuous determination of platinum and gold provided by the present application can achieve accurate determination of platinum and gold in minerals only under the synergistic action of various reagents.

[0115] In addition, an experiment was conducted separately to analyze the collecting ability of the prepared chelating collector for platinum under alkaline conditions:

[0116] 10 mL of chelating collector diluent was added to 1 L of alkaline solution of K2PtO4 (where the concentration of K2PtO4 was 10 mg / L), and the volume ratio of the chelating collector to sulfonated kerosene in the chelating collector diluent was 1:9. After stirring for 30 min, the organic phase solution was collected; then 20 mL of saturated ammonium chloride solution was added to the collected organic phase solution, stirred for 30 min, and the inorganic aqueous phase solution was collected for ICP-OES detection of platinum concentration. The collecting ability of the chelating collector diluent was judged according to the following formula.

[0117] The pH of the alkaline solution in the alkaline solution of K2PtO4 varied in the range of 8-14, and the specific experimental value range is shown in Table 4.

[0118] Platinum content (%) = C 1× V 1 / ( C 0× V 0)×100%

[0119] Wherein, C 1 - the concentration of platinum element in the inorganic aqueous phase solution detected by ICP-OES;

[0120] V 1 - the volume of the reverse collector (saturated ammonium chloride solution);

[0121] C 0 - the concentration of K2PtO4 used in the experiment;

[0122] V 0 - the volume of the alkaline solution of K2PtO4 used in the experiment.

[0123] The results of the influence of the chelating collector diluent's ability to capture platinum on the pH in the alkaline solution of K2PtO4 are shown in Table 4 below.

[0124] Table 4 The collecting ability of the chelating collector diluent for platinum in different pH environments in the alkaline solution of K2PtO4

[0125]

[0126] As can be seen from Table 4, the collecting ability of the prepared chelating collector diluent for platinum under alkaline conditions is significantly affected by pH. The extraction effect reaches over 99% within a specific pH range (11 - 14). However, as the alkalinity of the environment weakens, K2PtO4 hydrolyzes and precipitates are formed, thus affecting the collecting effect of the chelating collector diluent in the solution. In addition, in subsequent experiments, after the asynchronous separation process of natural minerals containing platinum and gold elements, the pH of the solution is greater than 11. This phenomenon ensures the optimal application conditions of the chelating collector and provides a prerequisite guarantee for the determination of the platinum content in the ore sample.

[0127] In summary, the method for asynchronous enrichment and continuous determination of platinum and gold in ores provided by the present invention involves, for minerals containing platinum and gold elements, after mixing with enrichment agents, undergoing high-temperature strong alkali oxidative melting to achieve the transformation of the existing form of platinum elements in the minerals, while ensuring that the valence state of gold in the minerals does not change; subsequently, the molten minerals can be soaked and filtered, so that platinum is separated from the minerals in the form of a solution, while gold remains in the minerals in a solid state, thus first separating platinum and gold in the minerals asynchronously; then, by using a special chelating collector diluent for the solution separated after soaking and filtering the molten minerals, in a strongly alkaline environment, platinum elements can be efficiently collected; among them, this chelating collector uses aliphatic cyclic diols as raw materials, utilizes the unique spatial structure of the molecule to make the chemical activities of the two hydroxyl groups different, and realizes the derivatization of the asymmetric molecular skeleton through a series of chemical reactions; subsequently, amine groups are introduced, and by regulating the types of amine groups and substituents, the chemical activity of the chelating site N is increased; thus, under strongly alkaline conditions, the specific chemical structure combined with the chemical activity of the chelating site can achieve the efficient collection of platinum elements, and thus the subsequent accurate determination of platinum elements is completed.

[0128] It should be noted that this application is not limited to the above embodiments. The above embodiments are only examples, and embodiments with the same constituent elements and the same function and effect as the technical idea within the scope of the technical solution of this application are all included in the technical scope of this application. In addition, within the scope of not departing from the main idea of this application, various modifications that can be thought of by those skilled in the art to the embodiments, and other ways constructed by combining some constituent elements of the embodiments are also included in the scope of this application.

Claims

1. A method for asynchronous enrichment and continuous determination of platinum and gold in ores, characterized in that, It includes the following steps: S1. Asynchronous separation of the target minerals containing platinum and gold is carried out as follows: The target minerals are mixed evenly with the enrichment reagent and then melted at high temperature to obtain molten minerals; then the molten minerals are placed in water, soaked and filtered in sequence to separate solids and solutions; The enrichment reagent includes a strong base reagent and an oxidant; S2. The collected platinum is subjected to flotation and content testing in sequence as follows: The solution separated in step S1 is mixed evenly with the chelating collector diluent, and the organic phase solution is collected; then a reverse collector is added to the organic phase solution, and after mixing evenly, the inorganic aqueous phase solution is collected; and the platinum content of the inorganic aqueous phase solution is tested; S3. The content of the separated gold is tested; The chelating collector diluent is composed of a chelating collector and sulfonated kerosene mixed in a volume ratio of 1:5 - 10; The structural formula of the chelating collector is as follows: 。 2. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, characterized in that, In step S1, the melting temperature is 500 - 700 °C.

3. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, characterized in that, In step S1, the mass ratio of the strong base reagent to the oxidant in the enrichment reagent is 10 - 100:1; the strong base reagent is one or more of sodium hydroxide and potassium hydroxide; the oxidant is one or more of sodium perchlorate, potassium perchlorate, sodium perbromate, and potassium perbromate.

4. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 2, characterized in that, In step S1, the mass ratio of the target minerals to the enrichment reagent is 1:1 - 5; The ratio of the molten minerals to water is 1 - 50 g:1 L.

5. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, characterized in that, In step S2, the volume ratio of the solution to the chelating collector diluent is 1000:1 - 10.

6. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, wherein In step S2, the reverse collector is one or more of a saturated solution of ammonium chloride and ammonia water; the volume ratio of the reverse collector to the chelating collector diluent is 2 - 5:

1.

7. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, wherein, In step S2, the method for testing the platinum content of the inorganic aqueous phase solution is ICP - OES.

8. The method for asynchronous enrichment and continuous determination of platinum and gold in ore according to claim 1, characterized in that, In step S3, the method for testing the content of the separated gold is the fire assay method.

Citation Information

Patent Citations

  • Method for determining platinum group elements in metallurgical material

    CN108169216A