Method for producing sponge platinum from ammoniation slag in short process

By using ammonia slurry washing, hydrazine hydrate reduction and homemade resin treatment in the ammonia slag, the problems of long process flow, large consumption and unstable quality in the prior art are solved, and efficient and high purity platinum recycling and continuous production are achieved.

CN119899944APending Publication Date: 2025-04-29安徽铜冠产业技术研究院有限责任公司
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Patent Information

Application Number
CN202510055629.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-14
Publication Date
2025-04-29

AI Technical Summary

Technical Problem

When the prior art recovers platinum products from ammonia slag, the process flow is long, the chemical reagents are consumed, the product quality is unstable, and the requirements of industrial continuous production are not met.

Method used

The Ag and Pd in ​​the ammonia slag are removed by slurry washing at 20-25% concentration, and then the efficient recovery of platinum is achieved through steps such as hydrazine hydrate reduction, HCl+NaClO3 mixed dissolving agent dissolution, homemade resin treatment and hydrochloric acid washing.

Benefits of technology

The platinum recovery rate is achieved above 95%, the purity of sponge platinum products is ≥99.95%, the process operation is simple, and the waste liquid can be looped, meeting the requirements of industrial continuous production.

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Abstract

The invention discloses a method for producing sponge platinum from ammoniation residues in a short process. The method comprises the following steps: S1, slurrying and washing by adopting ammonia water; s2, a proper amount of water is added to pulpify the leaching residues in the step S1, hydrazine hydrate is added for reduction, and crude platinum and reducing residues can be obtained; s3, dissolving the crude platinum in the step S2 by adopting a mixed dissolving agent of HCl and NaClO3 to obtain a platinum-rich solution and dissolving slag; s4, the platinum-rich liquid in the step S3 is treated with self-made resin, the platinum-rich liquid is introduced into a resin column, and platinum-loaded resin and exchange tail liquid can be obtained; s5, repeatedly washing the platinum-loaded resin obtained in the step S4 for 2-3 times by using hydrochloric acid; s6, desorbing Pt from the platinum-loaded resin in the step S5 by using a hydrochloric acid solution; and S7, hydrazine hydrate is added into the platinum desorption solution obtained in the step S6 to reduce Pd, water bath heating and stirring are conducted, and filtering, washing and vacuum drying are conducted. The method is used for recovering platinum in ammoniation residues, the recovery rate can reach 95% or above, the purity of a sponge platinum product is larger than or equal to 99.95%, operation is easy, and produced waste liquid can be recycled.
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Description

Technical Field

[0001] The invention relates to the field of rare and precious metal recovery and production, and in particular to a method for producing sponge platinum from ammoniation slag in a short process. Background Art

[0002] Ammoniated slag is an intermediate product in the copper anode mud treatment process. It is rich in rare and precious metal elements such as platinum and is the main raw material for producing platinum products.

[0003] Due to its special physical and chemical properties, precious metal platinum is widely used in chemical catalysis, artificial medical devices, integrated circuits, etc., and plays a very important role in the national economy. At present, the recovery of platinum products from ammoniated slag is mainly chemical. The chemical method mainly separates the precious metal platinum from impurities in the form of precipitation. This method has the disadvantages of long process, high consumption of chemical reagents, and large backlog of precious metals.

[0004] For example, the invention patent with publication number CN114717418A provides a method for preparing high-purity sponge platinum using low-concentration platinum waste liquid as raw material, including: selectively separating platinum from other impurities through the steps of Fe powder replacement of platinum waste liquid, sodium halide dissolution, iron separation and gold precipitation, platinum dissolution and gold separation, and hydrazine hydrate dissolution and reduction in sequence, thereby effectively improving the recovery rate of platinum and shortening the circulation period of waste liquid entering the anode mud treatment large circulation system. The purity of high-purity sponge platinum extracted by this process method is greater than 99.995%.

[0005] For example, the invention patent with publication number CN110387469A provides a process for separating and purifying sponge platinum from ammonium chloroplatinate-containing materials, comprising: adding water to crude ammonium chloroplatinate to make a slurry, adding hydrochloric acid, raising the temperature to 90-95°C, adding sodium chlorate until the solid is completely dissolved, raising the temperature to 95-100°C to drive out the chlorine, cooling and filtering; heating the filtrate to 40-65°C, adding ammonium chloride to precipitate platinum, cooling and filtering; repeating the refining once, adding NaOH to the secondary platinum solution for hydrolysis; adjusting the acidity of the hydrolysis filtrate, adding dimethylglyoxime to remove palladium; adding ammonium chloride to the filtrate, filtering to obtain pure ammonium chloroplatinate, reducing it with hydrazine hydrate to obtain high-purity platinum powder, and boiling it with nitric acid to obtain sponge platinum powder. The process of the present invention can stably produce sponge platinum that meets SM-99.99, and has a simple process flow, strong raw material adaptability, and a high platinum recovery rate. It also avoids the use of ammonium chloroplatinate calcination, aqua regia dissolution and other operations, and overcomes a series of problems such as excessive palladium in sponge platinum caused by incomplete removal of nitrate. Therefore, the present application provides a method for producing sponge platinum from ammoniated slag in a short process to meet the needs. Summary of the invention

[0006] The purpose of the present application is to provide a method for producing sponge platinum from ammoniated slag in a short process, so as to solve the problems that the existing technology for producing sponge platinum products has a long process flow, a large consumption of chemical reagents, unstable product quality, and cannot meet the requirements of industrial continuous production. Therefore, a method for producing sponge platinum in a short process is provided, which has the advantages of low cost, easy operation, high purity, and continuous production.

[0007] To achieve the above objectives, the present application provides the following technical solution: A method for producing sponge platinum from ammoniated slag in a short process:

[0008] S1: using 20-25% ammonia water (using ammonia water in this concentration range can improve reaction efficiency, reduce the volume of ammonia water, and reduce the pressure of subsequent treatment of the complex solution) to remove Ag and Pd in ​​the ammoniated slag in the form of silver ammonia complex and dichlorotetraamine palladium solution, and filtering to obtain a decontaminated liquid and leached slag, wherein the content of Ag in the ammoniated slag is 20-25%, and the content of Pd is 15-20%;

[0009] S2: Add appropriate amount of water to slurry the leached residue in S1, add hydrazine hydrate in small batches for reduction, and filter to obtain crude platinum and reduced residue after the reaction is completed;

[0010] S3: using a theoretical 1.2-1.3 times reaction equivalent HCl+NaClO3 mixed solvent at 70-90°C (within this temperature range, the dissolution reaction of crude platinum can be guaranteed to proceed effectively at a certain rate) to dissolve the crude platinum in S2, and after filtering, a platinum-rich solution and a dissolving slag can be obtained, wherein the content of Pt in the platinum-rich solution is 25-30 g / L;

[0011] S4: using a homemade resin to treat the platinum-rich solution in step S3, and passing the platinum-rich solution into the resin column to obtain a platinum-loaded resin and an exchange tail liquid;

[0012] The preparation method of the self-made resin is as follows:

[0013] S41: Take 27 parts of 2,6-dichloro-4-nitrile-5-sulfonic acid chloro-pyridine and 10 parts of aluminum powder, add them to 250 parts of dimethyl sulfoxide, stir evenly, slowly drop 2-3 mol / L (2-3 mol / L sulfuric acid has a lower concentration and is used to quench the reaction. This process will release a lot of heat and a small amount of hydrogen. Therefore, for safety reasons, sulfuric acid with a lower concentration should be used and added slowly, and the reaction should be carried out at a low temperature) 50 parts of sulfuric acid, stir while dropping and react for 1-2 hours, and then cool the reaction solution to room temperature;

[0014] S42: The reaction liquid after cooling in S1 is introduced into water, solid will precipitate, filter and dry, add 20 parts of deionized water and 50 parts of ethanol to the filter cake, heat and reflux, stir for 0.5 to 1 hour and then slowly cool, filter the reaction liquid again, and dry the filter cake to obtain 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor;

[0015] S43: placing 20 parts of the macroporous cross-linked polystyrene matrix in a reactor, adding an aprotic solvent, and stirring to swell;

[0016] S44: adding 27 parts of 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor into a reactor, stirring and heating, and performing a functionalization reaction to obtain a self-made resin having a selective mercapto group as a functional group;

[0017] S5: The platinum-loaded resin described in S4 is repeatedly washed 2 to 3 times with hydrochloric acid to remove most of the soluble metal impurities, thereby obtaining a pure platinum-loaded resin and a washing solution;

[0018] S6: desorbing Pt from the platinum-loaded resin in S5 with a hydrochloric acid solution to obtain a Pt desorption solution;

[0019] S7: Add 1.1 to 1.2 times the theoretical reaction equivalent of hydrazine hydrate to the platinum desorption solution in S6 to reduce Pd, heat in a water bath at 40 to 50°C (generally controlled within this temperature range because hydrazine hydrate may affect its reducibility at temperatures above 50°C, and a certain reduction effect can be guaranteed within this temperature range) with stirring for 1 to 2 hours, filter, wash, and vacuum dry to obtain a sponge platinum product.

[0020] As a preferred implementation in this embodiment, the hydrazine hydrate concentration is 40-80%. The use of hydrazine hydrate in this concentration range can improve the reduction efficiency, while minimizing the volume of hydrazine hydrate and reducing the subsequent treatment pressure of the reducing solution; each additional amount is 1 / 500-1 / 200 of the total reaction system volume. A single additional amount that is too low will affect the process production cycle, and a too high amount will cause the reaction system to boil over, which is prone to production accidents. It is best within this range.

[0021] As a preferred implementation in this embodiment, in S41, after stirring evenly, the mixture is placed at 0° C. and then sulfuric acid is slowly added dropwise.

[0022] Aluminum powder is highly active, and low-temperature reaction can reduce the reaction rate and prevent the reaction from being dangerous due to violent heat release. Therefore, sulfuric acid is slowly added at 0°C.

[0023] As a preferred implementation in this embodiment, in S4, the platinum-rich solution is introduced into the resin column at a flow rate of 1.5 to 2 BV / H.

[0024] If the flow rate is controlled too fast, the platinum-rich liquid may not be fully in contact with the homemade resin before being carried out, resulting in incomplete platinum adsorption; although a too low flow rate can increase the contact time, it will extend the treatment cycle and reduce production efficiency. When the flow rate is 1.5-2BV / H, it can not only ensure complete platinum adsorption, but also avoid extending the treatment cycle and improve production efficiency.

[0025] As a preferred implementation in this example, in S5, the platinum-loaded resin is repeatedly washed 2 to 3 times with 0.1 to 0.2 mol / L hydrochloric acid at a flow rate of 2.5 to 3 BV / H.

[0026] Hydrochloric acid in a low concentration range can effectively elute soluble base metal impurities, but has no elution effect on platinum, thereby achieving the purpose of separating platinum from other impurities. In addition, since the content of base metal impurities adsorbed by the platinum-loaded resin is not too high and the elution difficulty is low, appropriately increasing the washing speed is beneficial to shortening the production cycle.

[0027] As a preferred implementation in this embodiment, in S6, 2-3 mol / L hydrochloric acid solution is used to desorb Pt at a flow rate of 1.5-2 BV / H.

[0028] In this concentration range, hydrochloric acid can effectively elute the platinum in the resin and enter the solution. Since the platinum content adsorbed by the platinum-loaded resin is relatively high, the desorption rate can be appropriately reduced to ensure the elution effect.

[0029] In summary, the technical effects and advantages of the present invention are as follows:

[0030] 1. The method of the present invention is used to recover platinum from ammoniated slag, with a recovery rate of more than 95%, and the purity of the sponge platinum product is ≥ 99.95%. The method is simple to operate and the waste liquid produced can be recycled;

[0031] 2. The present invention obtains a functionalized platinum ion adsorption resin by grafting a self-made thiol-containing precursor and a cross-linked polystyrene, wherein the macroporous cross-linked polystyrene is used as a polymer backbone, which can provide a high surface area for ligand anchoring and has higher physical and chemical stability, and can be used for selective adsorption of platinum in an acidic medium. The 2,6-dichloro-4-nitrile-5-mercapto-pyridine can provide a platinum ion chelating group, and its thiol group can react with PtCl4 in the acidic medium. 2- and PtCl6 2- Coordination, strong affinity and high selectivity. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without paying any creative work.

[0033] Figure 1 The present invention is a schematic diagram of a short process for producing a sponge platinum product with a purity of 99.95% using ammoniated slag as a raw material. DETAILED DESCRIPTION

[0034] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0035] Example 1

[0036] S1. Use 20% ammonia slurry washing method to remove Ag and Pd in ​​the ammoniation slag in the form of silver ammonia complex and dichlorotetraamine palladium solution, and filter to obtain impurity-removed liquid and leached slag; the content of Ag in the ammoniation slag is 20%, and the content of Pd is 15%. S2. Add appropriate amount of water to slurry the leached slag in S1, add hydrazine hydrate in small batches for reduction, and filter to obtain crude platinum and reduced slag after the reaction is completed; the concentration of hydrazine hydrate is 40%, and the amount added each time is 1 / 500 of the total reaction system volume. S3. Use 1.2 times the theoretical reaction equivalent of HCl+NaClO3 mixed solvent to dissolve the crude platinum in S2 at 70°C, and filter to obtain platinum-rich liquid and dissolved slag; the content of Pt in the platinum-rich liquid is 25g / L. S4. Use homemade resin to treat the platinum-rich liquid in S3, and pass the platinum-rich liquid into the resin column at a flow rate of 1.5BV / H to obtain platinum-loaded resin and exchange tail liquid. S5. Wash the platinum-loaded resin in S4 repeatedly 2 to 3 times with 0.1 mol / L hydrochloric acid at a flow rate of 2.5 BV / H to remove most of the soluble metal impurities, and obtain pure platinum-loaded resin and washing liquid. S6. Desorb Pt from the platinum-loaded resin in S5 with 2 mol / L hydrochloric acid solution at a flow rate of 1.5 BV / H to obtain a Pt desorption liquid. S7. Add 1.1 times the theoretical reaction equivalent of hydrazine hydrate to the platinum desorption liquid in S6 to reduce Pd, heat in a water bath at 40 to 50°C with stirring for 1 hour, filter, wash, and vacuum dry to obtain a sponge platinum product.

[0037] Further, the preparation method of the self-made resin described in S4 is as follows:

[0038] S41: Take 27 parts of 2,6-dichloro-4-nitrile-5-sulfonic acid chloro-pyridine and 10 parts of aluminum powder, add them to 250 parts of dimethyl sulfoxide, stir evenly, place at 0°C, slowly drop 50 parts of 2M sulfuric acid, stir and react for 1 to 2 hours, then cool the reaction solution to room temperature;

[0039] S42: The reaction liquid after cooling in S1 is introduced into water, solid will precipitate, filter and dry, add 20 parts of deionized water and 50 parts of ethanol to the filter cake, heat and reflux, stir for 0.5h and then slowly cool, filter the reaction liquid again, and dry the filter cake to obtain 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor;

[0040] S43: placing 20 parts of the macroporous cross-linked polystyrene matrix in a reactor, adding an aprotic solvent, and stirring to swell;

[0041] S44: 27 parts of 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor are added to a reactor, stirred and heated to perform a functionalization reaction, and a self-made resin having a functional group containing a selective thiol group is obtained.

[0042] Example 2

[0043] S1, using 22% concentration of ammonia water slurry washing method to remove Ag and Pd in ​​the ammoniation slag in the form of silver ammonia complex and dichlorotetraamine palladium solution, filtering to obtain impurity-removed liquid and leached slag; the content of Ag in the ammoniation slag is 22%, and the content of Pd is 18%; S2, adding appropriate amount of water to slurry the leached slag in S1, adding hydrazine hydrate in small batches for reduction, filtering after the reaction is completed to obtain crude platinum and reduced slag; the concentration of hydrazine hydrate is 60%, and the amount added each time is 3 / 1000 of the total reaction system volume; S3, using 1.2 times the theoretical reaction equivalent of HCl+NaClO3 mixed solvent to dissolve the crude platinum in S2 at 70°C, filtering to obtain platinum-rich liquid and dissolved slag; the content of Pt in the platinum-rich liquid is 25g / L. S4, using homemade resin to treat the platinum-rich liquid in S3, passing the platinum-rich liquid into the resin column at a flow rate of 2BV / H to obtain platinum-loaded resin and exchange tail liquid. S5. Wash the platinum-loaded resin described in S4 repeatedly 2 to 3 times with 0.1 mol / L hydrochloric acid at a flow rate of 2.8 BV / H to wash away most of the soluble metal impurities, and obtain pure platinum-loaded resin and washing liquid. S6. Desorb Pt from the platinum-loaded resin in S5 with 2.5 mol / L hydrochloric acid solution at a flow rate of 1.8 BV / H to obtain a Pt desorption liquid. S7. Add 1.15 times the theoretical reaction equivalent of hydrazine hydrate to the platinum desorption liquid described in S6 to reduce Pd, heat in a water bath at 45°C with stirring for 1 hour, filter, wash, and vacuum dry to obtain a sponge platinum product.

[0044] Further, the preparation method of the self-made resin described in S4 is as follows:

[0045] S41: Take 27 parts of 2,6-dichloro-4-nitrile-5-sulfonic acid chloro-pyridine and 10 parts of aluminum powder, add them to 250 parts of dimethyl sulfoxide, stir evenly, place at 0°C, slowly drop 50 parts of 2.5M sulfuric acid, stir and react for 1.5 hours, then cool the reaction solution to room temperature;

[0046] S42: The reaction liquid after cooling in S1 is introduced into water, solid will precipitate, filter and dry, add 20 parts of deionized water and 50 parts of ethanol to the filter cake, heat and reflux, stir for 1 hour and then slowly cool, filter the reaction liquid again, and dry the filter cake to obtain 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor;

[0047] S43: placing 20 parts of the macroporous cross-linked polystyrene matrix in a reactor, adding an aprotic solvent, and stirring to swell;

[0048] S44: adding 27 parts of 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor into a reactor, stirring and heating, and performing a functionalization reaction to obtain a self-made resin having a selective mercapto group as a functional group;

[0049] Example 3

[0050] S1. Use 25% ammonia slurry washing method to remove Ag and Pd in ​​the ammoniation slag in the form of silver ammonia complex and dichlorotetraamine palladium solution, and filter to obtain impurity-removed liquid and leached slag; the content of Ag in the ammoniation slag is 25%, and the content of Pd is 19%. S2. Add appropriate amount of water to slurry the leached slag in S1, add hydrazine hydrate in small batches for reduction, and filter to obtain crude platinum and reduced slag after the reaction is completed; the concentration of hydrazine hydrate is 80%, and the amount added each time is 1 / 200 of the total reaction system volume. S3. Use 1.3 times the theoretical reaction equivalent of HCl+NaClO3 mixed solvent to dissolve the crude platinum in S2 at 90℃, and filter to obtain platinum-rich liquid and dissolved slag; the content of Pt in the platinum-rich liquid is 30g / L. S4. Use homemade resin to treat the platinum-rich liquid in S3, and pass the platinum-rich liquid into the resin column at a flow rate of 2BV / H to obtain platinum-loaded resin and exchange tail liquid. S5. Wash the platinum-loaded resin described in S4 repeatedly 2 to 3 times with 0.2 mol / L hydrochloric acid at a flow rate of 3 BV / H to wash away most of the soluble metal impurities, and obtain pure platinum-loaded resin and washing liquid. S6. Desorb Pt from the platinum-loaded resin in S5 with 3 mol / L hydrochloric acid solution at a flow rate of 2 BV / H to obtain a Pt desorption liquid. S7. Add 1.2 times the theoretical reaction equivalent of hydrazine hydrate to the platinum desorption liquid described in S6 to reduce Pd, heat in a water bath at 50°C with stirring for 2 h, filter, wash, and vacuum dry to obtain a sponge platinum product.

[0051] Further, the preparation method of the self-made resin described in S4 is as follows:

[0052] S41: Take 27 parts of 2,6-dichloro-4-nitrile-5-sulfonic acid chloro-pyridine and 10 parts of aluminum powder, add them to 250 parts of dimethyl sulfoxide, stir evenly, place at 0°C, slowly drop 50 parts of 3M sulfuric acid, stir and react for 2 hours, then cool the reaction solution to room temperature;

[0053] S42: The reaction liquid after cooling in S1 is introduced into water, solid will precipitate, filter and dry, add 20 parts of deionized water and 50 parts of ethanol to the filter cake, heat and reflux, stir for 1 hour and then slowly cool, filter the reaction liquid again, and dry the filter cake to obtain 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor;

[0054] S43: placing 20 parts of the macroporous cross-linked polystyrene matrix in a reactor, adding an aprotic solvent, and stirring to swell;

[0055] S44: 27 parts of 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor are added to a reactor, stirred and heated to perform a functionalization reaction, and a self-made resin having a functional group containing a selective thiol group is obtained.

[0056] Finally, the test results of the sponge platinum products in Examples 1 to 3 are given, and the chemical composition is shown in the following table (unit: ppm).

[0057]

[0058]

[0059] Through the above tests, it can be seen that the purity of sponge platinum is relatively high and can reach the standard of SM-Pt 99.95. The impurities in it are well removed. More importantly, the above process is not only short in process, but also can achieve efficient recovery of platinum.

[0060] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for producing sponge platinum from ammoniation slag in a short process, characterized in that: S1: removing Ag and Pd from the ammoniation slag in the form of silver-ammine complex and dichlorotetraamine palladium solution by slurry washing with 20-25% ammonia water, filtering to obtain a decontaminated liquid and leached slag, wherein the content of Ag in the ammoniation slag is 20-25%, and the content of Pd is 15-20%; S2: Add appropriate amount of water to slurry the leached residue in S1, add hydrazine hydrate in small batches for reduction, and filter to obtain crude platinum and reduced residue after the reaction is completed; S3: using a theoretical 1.2-1.3 times reaction equivalent HCl+NaClO3 mixed solvent to dissolve the crude platinum in S2 at 70-90°C, and filtering to obtain a platinum-rich solution and a dissolving residue, wherein the content of Pt in the platinum-rich solution is 25-30 g / L; S4: using a homemade resin to treat the platinum-rich solution in step S3, and passing the platinum-rich solution into the resin column to obtain a platinum-loaded resin and an exchange tail liquid; The preparation method of the homemade resin is as follows: S41: Take 27 parts of 2,6-dichloro-4-nitrile-5-sulfonic acid chloro-pyridine and 10 parts of aluminum powder, add them to 250 parts of dimethyl sulfoxide, stir evenly, slowly drop 50 parts of 2-3 mol / L sulfuric acid, stir and react for 1-2 hours, then cool the reaction solution to room temperature; S42: The reaction liquid after cooling in S1 is introduced into water, solid will precipitate, filter and dry, add 20 parts of deionized water and 50 parts of ethanol to the filter cake, heat and reflux, stir for 0.5 to 1 hour and then slowly cool, filter the reaction liquid again, and dry the filter cake to obtain 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor; S43: placing 20 parts of the macroporous cross-linked polystyrene matrix in a reactor, adding an aprotic solvent, and stirring to swell; S44: adding 27 parts of 2,6-dichloro-4-nitrile-5-mercapto-pyridine precursor into a reactor, stirring and heating, and performing a functionalization reaction to obtain a self-made resin having a selective mercapto group as a functional group; S5: The platinum-loaded resin described in S4 is repeatedly washed 2 to 3 times with hydrochloric acid to remove most of the soluble metal impurities, thereby obtaining a pure platinum-loaded resin and a washing solution; S6: desorbing Pt from the platinum-loaded resin in S5 with a hydrochloric acid solution to obtain a Pt desorption solution; S7: Add 1.1 to 1.2 times the theoretical reaction equivalent of hydrazine hydrate to the platinum desorption solution in S6 to reduce Pd, heat in a water bath at 40 to 50° C. with stirring for 1 to 2 h, filter, wash, and vacuum dry to obtain a sponge platinum product.

2. The method for producing sponge platinum from ammoniated slag in a short process according to claim 1, characterized in that: The concentration of the hydrazine hydrate is 40-80%, and the amount added each time is 1 / 500-1 / 200 of the volume of the total reaction system.

3. The method for producing sponge platinum from ammoniated slag in a short process according to claim 1, characterized in that: In the S41, after stirring evenly, the mixture is placed at 0°C and then sulfuric acid is slowly added dropwise.

4. The method for producing sponge platinum from ammoniated slag in a short process according to claim 1, characterized in that: In S4, the platinum-rich solution is introduced into the resin column at a flow rate of 1.5 to 2 BV / H.

5. The method for producing sponge platinum from ammoniated slag in a short process according to claim 4, characterized in that: In the step S5, the platinum-loaded resin is repeatedly washed with 0.1-0.2 mol / L hydrochloric acid at a flow rate of 2.5-3 BV / H.

6. The method for producing sponge platinum from ammoniated slag in a short process according to claim 5, characterized in that: In the S6, Pt is desorbed using a 2-3 mol / L hydrochloric acid solution at a flow rate of 1.5-2 BV / H.

Citation Information

Patent Citations

  • Process for separating and purifying spongy platinum from ammonium chloroplatinate

    CN110387469A

  • Method for extracting high-purity sponge platinum from platinum waste liquid

    CN114717418A