A treatment method and system for comprehensive recovery of high-purity gold and silver platinum palladium
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-04-21
- Publication Date
- 2026-08-11
AI Technical Summary
针对上述现有技术中存在的回收的贵金属纯度较差的问题,本发明提供了一种高纯金及银铂钯的综合回收的处理方法及系统
本发明提供了一种高纯金及银铂钯的综合回收的处理方法及系统,首先通过使用硝酸预浸银阳极泥,使得银阳极泥中的银、钯、铜尽可能的浸出在预浸液中,后续过程不再产生大量分金渣;而预浸液中采用先后加入碱性试剂和钾盐进行精准的控制pH,将钯沉淀产出,减少钯的损失;而钯的化合物沉淀可以进一步处理得到钯粉;通过调节沉钯后液中的pH,可以进一步沉银,不再产生氯化银沉淀,产生更稳定的黑色沉淀,而黑色沉淀通过加入酸可以使得银溶解,变成硝酸银溶液,做为补充新电解液使用;分金液中采用先后加入碱性试剂和钾盐进行精准的控制pH,将铂沉淀产出,使得溶液更加纯净,可以使后续还原过程中更加快捷,缩短工艺流程,降低流程占用;分金液除杂可以使得其他杂质微乎其微,后续还原得到高纯金。
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Figure CN122542818A_ABST
Abstract
Description
Summary of the Invention Technical Field
[0001] This invention relates to the field of precious metal recycling technology, specifically to a comprehensive recycling method and system for high-purity gold, silver, platinum, and palladium. Background Technology
[0002] In the electrolytic purification process of silver, the resulting silver anode mud is a key recycled raw material. Rich in rare metals such as gold, silver, palladium, and platinum, it not only possesses significant market value but also plays a crucial strategic role in resource security. Currently, with the government continuously strengthening its support for the resource recycling industry, a number of supporting incentive policies have been introduced and implemented, providing strong support and new opportunities for the overall development of the precious metal recycling industry.
[0003] Currently, there are various methods for treating silver anode slime. A common method involves hydrochloric acid pre-leaching, chlorination-gold separation, gold powder reduction, and platinum-palladium replacement. However, this process cannot completely dissolve platinum and palladium during pre-leaching, causing them to enter the pre-leaching residue. During gold separation, platinum and palladium are chlorinated, resulting in high concentrations of platinum and palladium in the separation solution, which in turn affects the grade of the reduced gold. Simultaneously, this process generates gold separation residue, primarily composed of silver chloride precipitate. Due to the high viscosity of silver chloride, the precipitate contains gold separation solution, making effective washing of the solution impossible. Therefore, the gold separation residue is typically subjected to multiple chlorination treatments and ultimately processed using a reflow method. The generation of gold separation residue reduces gold recovery and increases silver flow, hindering effective silver recovery. Since palladium in silver anode slime is primarily contained in the separation solution, the amount and rate of reducing agent addition during gold separation reduction must be strictly controlled; otherwise, palladium levels in the gold powder will exceed acceptable limits. Palladium metal is typically processed at the end of the silver anode slime process, resulting in a lengthy process and a very low palladium recovery rate. Furthermore, the reducing agent used for palladium metal replacement is usually iron powder, which leads to the displacement of metals less reactive than iron, resulting in a high impurity content in the palladium concentrate. Multiple treatments are required to purify the palladium concentrate. CN 121137357 A discloses a method for recovering gold, silver, palladium, and platinum from silver anode slime. This method uses a potassium-magnesium mixture (potassium sulfate and magnesium chloride) to precipitate palladium and platinum in the solution and uses hydroxylamine hydrochloride as a separating reagent for palladium and platinum. While this method can improve the recovery rate of gold, platinum, and palladium to some extent, the purity of the recovered precious metals is poor.
[0004] It is evident that existing technologies for recovering gold, silver, palladium, and platinum from silver anode mud generally suffer from problems such as poor purity of the recovered precious metals, and a better method and system are urgently needed to solve these technical challenges. Summary of the Invention To address the problem of poor purity of recovered precious metals in the existing technologies, this invention provides a comprehensive recovery method and system for high-purity gold, silver, platinum, and palladium.
[0006] To achieve the above objectives, the technical solution of the present invention is as follows: A comprehensive recycling method for high-purity gold, silver, platinum, and palladium, characterized by comprising the following steps: gold refining, palladium refining, and platinum refining; The gold refining process includes the following steps: S1 pre-impregnation; S2 Palladium precipitation: First, add an alkaline reagent to the pre-leaching solution obtained in S1 to adjust the pH to 1.4-1.6, then add potassium salt to adjust the pH to 2.2-2.4, and react at 66-73℃ for 60-80 minutes to obtain palladium concentrate and palladium precipitation solution; S3 Silver precipitation: Add potassium salt to the palladium precipitation solution to adjust the pH to 4.0-4.2, react at room temperature for 30-40 minutes to obtain silver precipitation residue; S4 Copper Removal: An acidic reagent is added to the silver precipitate residue to obtain a silver electrolyte; S5 cents; S6 Platinum Precipitation: First, add an alkaline reagent to the gold separation solution obtained in S5 to adjust the pH to 2.7-2.9, then add potassium salt to adjust the pH to 3.4-3.6, and react at 60-70℃ for 40-60 min to obtain platinum concentrate and platinum precipitation solution; S7 Acid Reversion: An acidic reagent is added to the platinum-precipitated solution, and a high-gold solution is obtained after the reaction. S8 Reduction: Formic acid is added to the high-purity gold solution for reduction, followed by washing to obtain high-purity gold powder.
[0007] Further, in S1, the silver anode mud is pre-impregnated with pure water and nitric acid with a concentration of 65-68%, and the mass ratio of silver anode mud, pure water and nitric acid is (2.1-5.6):(5.4-16.8):(1.2-3.6); in S2 and S6, the alkaline reagent is sodium hydroxide with a concentration of 40-50%, and the potassium salt is potassium carbonate with a concentration of 15-25%; in S3, the potassium salt is potassium carbonate with a concentration of 15-25%; in S4, the acidic reagent is nitric acid with a concentration of 65-68%; in S5, the gold separation step is as follows: after washing the pre-impregnated residue obtained in S1, hydrochloric acid with a concentration of 33-39% and sodium chlorate oxidant with a concentration of 40-60% are added for gold separation; in S7, the acidic reagent is hydrochloric acid with a concentration of 33-39%, and in S8, the formic acid concentration is 15-25%.
[0008] Further, in the gold refining process, in S1, the reaction temperature is 75-85℃, the stirring speed is 140-180 rpm, and the reaction time is 3-5 h; in S2, the stirring speed is 115-135 rpm; in S3, the stirring speed is 105-125 rpm; in S4, the reaction temperature is 40-45℃, the stirring speed is 90-100 rpm, and the reaction time is 25-30 min; in S5, the reaction temperature is 85-95℃, the stirring speed is 120-140 rpm, and the reaction time is 80-120 min; in S6, the stirring speed is 117-137 rpm; in S7, the reaction temperature is room temperature, the stirring speed is 30-60 rpm, and the reaction time is 10-20 min; in S8, the reaction temperature is 55-75℃, the stirring speed is 110-130 rpm, and the reaction time is 70-90 min.
[0009] Further, the palladium refining specifically includes the following steps: S21 Pre-leaching: Hydrochloric acid is added to the palladium concentrate obtained in S2 of gold refining, and a palladium-containing solution is obtained after the reaction; S22 Palladium enrichment: A precipitating agent and an oxidizing agent are added to the palladium-containing solution, and a palladium-rich slag is obtained after the reaction; the precipitating agent is a mixed reagent of sodium chloride and potassium sulfate in a mass ratio of 1:1.4-1.6, and the amount added is 1.2-1.8 times the palladium content in the solution; the oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.5-0.7 times the palladium content in the solution; S23 Palladium dissolution: The palladium-rich slag is dissolved in ammonia water. The reaction yields a palladium-containing solution; S24 High Palladium: A precipitating agent and an oxidizing agent are added to the palladium-containing solution, and a high palladium ore is obtained after the reaction; the precipitating agent is a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.4-1.6, and the amount added is 1.2-1.8 times the palladium content in the solution; the oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.5-0.7 times the palladium content in the solution; S25 Secondary Palladium Dissolution: The high palladium ore is dissolved in ammonia water, and a high palladium solution is obtained after the reaction; S26 Reduction: Formic acid is added to the high palladium solution for reduction, and then washed until neutral to obtain sponge palladium.
[0010] In one specific implementation, during the palladium refining process, in S21, the concentration of hydrochloric acid is 33-39%; in S23 and S25, the concentration of ammonia is 20-30%; and in S26, the concentration of formic acid is 15-25%.
[0011] Further, in the palladium refining process, in S21, the reaction temperature is 58-75℃, the stirring speed is 85-105 rpm, and the reaction time is 23-43 min; in S22, the reaction temperature is 59-79℃, the stirring speed is 102-132 rpm, and the reaction time is 60-90 min; in S23, the reaction temperature is 84-94℃, the stirring speed is 101-121 rpm, and the reaction time is 33-53 min; in S24, the reaction temperature is 69-89℃, the stirring speed is 105-125 rpm, and the reaction time is 30-60 min; in S25, the reaction temperature is 64-84℃, the stirring speed is 81-101 rpm, and the reaction time is 13-33 min; and in S26, the reaction temperature is at room temperature, the stirring speed is 55-75 rpm, and the reaction time is 22-42 min.
[0012] Further, the platinum refining specifically includes the following steps: S61 Pre-leaching: Hydrochloric acid is added to the platinum concentrate obtained in S6 of gold refining, and a platinum-containing solution is obtained after the reaction; S62 Platinum enrichment: A precipitating agent and an oxidizing agent are added to the platinum-containing solution, and a platinum-rich slag is obtained after the reaction; the precipitating agent is a mixed reagent of sodium chloride and potassium sulfate in a mass ratio of 1:1.4-1.6, and the amount added is 1.1-1.5 times the platinum content in the solution; the oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.9-1 times the platinum content in the solution; S63 Impurity removal and separation: Hydrazine sulfate is added to the platinum-rich slag for separation, and a platinum-containing slag is obtained after the reaction; S6 4. Platinum Dissolution: The platinum-containing slag is dissolved in hydrazine sulfate, and the reaction yields a platinum-separated solution; S65. High Platinum: A precipitating agent and an oxidizing agent are added to the platinum-separated solution, and the reaction yields a high-platinum slag; the precipitating agent is a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.4-1.6, and the amount added is 1.2-1.8 times the platinum content in the solution; the oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.9-1 times the platinum content in the solution; S66. Secondary Platinum Dissolution: The high-platinum slag is dissolved in hydrazine sulfate, and the reaction yields a high-platinum solution; S67. Reduction: Formic acid is added to the high-platinum solution for reduction, and after washing, sponge platinum is obtained.
[0013] In one specific implementation, in the platinum refining process, the concentration of hydrochloric acid in S61 is 33-39%, the concentration of hydrazine sulfate in S63, S64, and S66 is 30-40%, and the concentration of formic acid in S67 is 15-25%.
[0014] Furthermore, in the platinum refining process, in S61, the reaction temperature is 30-50℃, the stirring speed is 77-97 rpm, and the reaction time is 56-86 min; in S62, the reaction temperature is 55-75℃, the stirring speed is 108-128 rpm, and the reaction time is 34-54 min. In S63, the reaction temperature is 58-84℃, the stirring speed is 113-133 rpm, and the reaction time is 8-18 min; in S64, the reaction temperature is 92-98℃, the stirring speed is 112-132 rpm, and the reaction time is 26-46 min; in S65, the reaction temperature is 68-88℃, the stirring speed is 89-109 rpm, and the reaction time is 13-33 min; in S66, the reaction temperature is 92-98℃, the stirring speed is 112-132 rpm, and the reaction time is 26-46 min; in S67, the reaction temperature is room temperature, the stirring speed is 63-83 rpm, and the reaction time is 23-43 min.
[0015] This invention also includes the following technical solutions: A comprehensive recycling system for high-purity gold, silver, platinum, and palladium, wherein the comprehensive recycling system is used in the aforementioned comprehensive recycling method; the comprehensive recycling system includes a gold refining system, a palladium refining system, and a platinum refining system; The gold refining system includes: a pre-impregnation kettle connected to a pre-impregnation filter tank; the outlet of the pre-impregnation filter tank connected to a palladium precipitation kettle; the slag outlet of the pre-impregnation filter tank connected to a gold separation kettle; the gold separation kettle connected to a gold separation filter tank; the outlet of the gold separation filter tank connected to a platinum precipitation kettle; the platinum precipitation kettle connected to a platinum precipitation filter press; the outlet of the platinum precipitation filter press connected to a gold reduction kettle; the palladium precipitation kettle connected to a palladium precipitation filter press; the outlet of the palladium precipitation filter press connected to a silver precipitation kettle; the silver precipitation kettle connected to a silver precipitation filter press; the outlet of the silver precipitation filter press connected to a wastewater tank; the slag outlet of the silver precipitation filter press connected to a copper kettle; and the copper kettle connected to a copper removal filter press via a pipeline.
[0016] The palladium refining system includes: a palladium melting kettle connected to a palladium melting filter press; the outlet of the palladium melting filter press connected to a palladium-rich kettle; the palladium-rich kettle connected to a palladium-rich filter press; the slag outlet of the palladium-rich filter press connected to a palladium separating kettle; the palladium separating kettle connected to a palladium separating filter press; the outlet of the palladium separating filter press connected to a high-palladium kettle; the high-palladium kettle connected to a high-palladium filter press; the slag outlet of the high-palladium filter press connected to a high-palladium water kettle; the high-palladium water kettle connected to a high-palladium water filter press; the outlet of the high-palladium water filter press connected to a palladium reduction kettle; and the palladium reduction kettle connected to a palladium reduction filter press.
[0017] The platinum refining system includes: a platinum dissolving kettle connected to a platinum dissolving filter press; the outlet of the platinum dissolving filter press connected to a platinum enrichment kettle; the platinum enrichment kettle connected to a platinum enrichment filter press; the slag outlet of the platinum enrichment filter press connected to a purification kettle; the purification kettle connected to a purification filter press; the slag outlet of the purification filter press connected to a platinum separation kettle; the platinum separation kettle connected to a platinum separation filter press; the outlet of the platinum separation filter press connected to a high platinum kettle; the high platinum kettle connected to a high platinum ore filter press; the slag outlet of the high platinum ore filter press connected to a high platinum water kettle; the high platinum water kettle connected to a high platinum water filter press; the outlet of the high platinum water filter press connected to a platinum reduction kettle; and the platinum reduction kettle connected to a platinum reduction filter press.
[0018] Furthermore, in the gold-separating vessel, a compressed air pipe is added and coiled along the vessel wall, with holes of 1-2 cm in diameter opened every 20-40 cm below the pipe; a first electronic hydrometer is installed in the middle of the gold-separating vessel, and a second electronic hydrometer is installed at the bottom of the gold-separating vessel. The two electronic hydrometers are interlocked with the compressed air regulating valve. The interlock is as follows: if the difference between the two electronic hydrometers is less than 0.05, the compressed air regulating valve maintains this opening; if the difference between the two electronic hydrometers is greater than 0.05, the compressed air regulating valve increases its opening by 3-7% every 1-3 minutes.
[0019] Furthermore, the gold reduction vessel is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the first high-level tank. The interlock is as follows: if the potential inside the vessel is less than -0.67V, the outlet valve of the first high-level tank is closed.
[0020] Furthermore, the palladium precipitation vessel is equipped with an electronic pH meter, which is interlocked with the outlet valves of the second and third high-level tanks. The interlocking mechanism is as follows: when pH ≤ 1.5, the outlet valve of the second high-level tank is open and the outlet valve of the third high-level tank is closed; when pH > 1.5 and ≤ 2.3, the outlet valve of the second high-level tank is closed and the outlet valve of the third high-level tank is open; when pH > 2.3, both the outlet valves of the second and third high-level tanks are closed. The platinum precipitation reactor is equipped with an electronic pH meter, which is interlocked with the outlet valves of the second and third high-level tanks. The interlocking mechanism is as follows: when pH < 2.8, the outlet valve of the second high-level tank is open and the outlet valve of the third high-level tank is closed; when pH > 2.8 and ≤ 3.5, the outlet valve of the second high-level tank is closed and the outlet valve of the third high-level tank is open; when pH > 3.5, both the outlet valves of the second and third high-level tanks are closed.
[0021] Furthermore, the palladium reduction reactor is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank. The interlocking mechanism is as follows: if the potential inside the reactor is less than -1.32V, the outlet valve is closed; and the single-point direct feeding method is changed to a four-point feeding method parallel to the stirring. The platinum reduction reactor is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank. The interlocking mechanism is as follows: if the potential inside the reactor is less than -1.17V, the outlet valve is closed; and the single-point direct feeding method is changed to a four-point feeding method parallel to the stirring.
[0022] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention provides a comprehensive recovery method and system for high-purity gold, silver, platinum, and palladium. First, silver anode mud is pre-leached with nitric acid to maximize the leaching of silver, palladium, and copper into the pre-leaching solution, preventing the generation of large amounts of gold-separating slag in subsequent processes. The pH of the pre-leaching solution is precisely controlled by sequentially adding alkaline reagents and potassium salts to precipitate palladium, minimizing palladium loss. The palladium compound precipitate can be further processed to obtain palladium powder. By adjusting the pH of the solution after palladium precipitation, silver can be further precipitated, preventing the formation of silver chloride precipitate and producing a more stable black precipitate. This black precipitate can be dissolved by adding acid to form silver nitrate solution, which can be used as a replenishing electrolyte. In the gold separation solution, the pH is precisely controlled by sequentially adding alkaline reagents and potassium salts to precipitate platinum, resulting in a purer solution. This allows for faster subsequent reduction processes, shortening the process flow and reducing process time. The gold separation solution removes impurities to negligible levels, leading to the subsequent reduction of high-purity gold.
[0023] The method provided by this invention for processing platinum and palladium can significantly improve the purity of gold, silver, platinum, and palladium, thereby increasing enterprise profits. This method is a fully wet process, which is more environmentally friendly and provides a better operating environment for operators compared to traditional pyrometallurgical and extraction processes. The waste gas generated by this method can be purified and neutralized by an acid mist purification tower, making it even more environmentally friendly and producing less wastewater. Furthermore, the wastewater contains fewer precious and heavy metals, and replacement is faster and more convenient. In addition, this method uses modern interlocking equipment, achieving more precise reduction, reducing labor intensity and personnel costs, increasing enterprise profits, and expanding the enterprise's market competitiveness.
[0024] The method provided by this invention ensures that the recovery rate of gold, silver, platinum, and palladium is above 99.0%, while significantly improving the purity of gold, silver, platinum, and palladium. The purity of gold reaches 99.999%, and the purity of silver, platinum, and palladium reaches above 99.96%. Attached Figure Description
[0025] The embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein: Figure 1 A process flow diagram of the present invention is shown.
[0026] Figure 2 A diagram of the gold refining system of the present invention is shown.
[0027] Figure 3 A diagram of the palladium refining system of the present invention is shown.
[0028] Figure 4 A diagram of the platinum refining system of the present invention is shown.
[0029] Attached diagram labels: 1-Pre-impregnation kettle, 2-Pre-impregnation filter tank, 3-Gold separation kettle, 4-Gold separation filter tank, 5-Pipeline connection pump, 6-Platinum precipitation kettle, 7-Pipeline connection pump, 8-Platinum precipitation filter press, 9-First high-level tank, 10-Gold reduction kettle, 11-Gold powder filter tank, 12-Pipeline connection pump, 13-Pipeline connection pump, 14-Palladium precipitation kettle, 15-Pipeline connection pump, 16-Palladium precipitation filter press, 17-Silver precipitation kettle 18-Pipeline connection pump, 19-Silver immersion filter press, 20-Copper reactor, 21-Pipeline connection pump, 22-Copper removal filter press, 23-Wastewater tank, 24-Second high-level tank, 25-Third high-level tank, 26-Palladium dissolution reactor, 27-Pipeline connection pump, 28-Palladium dissolution filter press, 29-Palladium-rich reactor, 31-Palladium-rich filter press, 32-Palladium separation reactor, 33-Pipeline connection pump, 34-Palladium separation filter press, 35- High palladium reactor, 36 - pipeline connection pump, 37 - high palladium filter press, 38 - fourth high-level tank, 39 - palladium reduction reactor, 40 - pipeline connection pump, 41 - palladium reduction filter press, 42 - platinum dissolution reactor, 43 - pipeline connection pump, 44 - platinum dissolution filter press, 45 - platinum enrichment reactor, 46 - pipeline connection pump, 47 - platinum enrichment filter press, 48 - pipeline connection pump, 49 - impurity removal filter press, 50 - platinum separation reactor, 51 - pipeline connection 52-Platinum Reduction Filter Press, 53-High Platinum Kettle, 54-Pipeline Connecting Pump, 55-High Platinum Ore Filter Press, 56-High Platinum Water Kettle, 57-Pipeline Connecting Pump, 58-High Platinum Water Filter Press, 59-Platinum Reduction Kettle, 60-Pipeline Connecting Pump, 61-Platinum Reduction Filter Press, 62-High Palladium Water Kettle, 63-Pipeline Connecting Pump, 64-High Palladium Water Filter Press, 65-Impurity Removal Kettle, 66-Compressed Air Regulating Valve. Detailed Implementation
[0030] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0031] Example 1 This embodiment provides a comprehensive recovery and processing method for high-purity gold, silver, platinum, and palladium, including the following steps: gold refining, palladium refining, and platinum refining; the process flow diagram is shown below. Figure 1As shown; the specific process is as follows.
[0032] I. Gold Refining S1 Pre-impregnation: Add 100g of silver anode mud to a 1500ml three-necked flask, add 300ml of pure water, add 50ml of 67% nitric acid, start stirring at 180rpm, heat to 85℃, stir for 3h. After the reaction is complete, separate the solid and liquid to obtain pre-impregnation residue and pre-impregnation liquid. Further process the pre-impregnation liquid and wash the pre-impregnation residue twice with 70℃ hot water. Separate the solid and liquid to obtain pre-impregnation residue. The mass ratio of silver anode mud, pure water and nitric acid is 4:12:2. S2 Palladium Precipitation: The volume of the pre-impregnation solution was measured to be 216 ml using a graduated cylinder. It was then added to a 500 ml three-necked flask. Stirring was started, and the temperature was raised to 73°C. Sodium hydroxide and potassium carbonate were added. The pH was first adjusted to 1.6 using 45% sodium hydroxide, and then adjusted to 2.2 using 20% potassium carbonate. The stirring speed was 115 rpm, and the mixture was stirred for 60 min. After the reaction was completed, the solid and liquid were separated to obtain palladium concentrate and palladium precipitation liquid. The palladium concentrate was sent to the palladium refining system for further processing. S3 Silver Precipitation: The volume of the palladium-precipitated liquid after measurement with a graduated cylinder is 202ml. It is added to a 500ml three-necked flask, stirred, and 20% potassium carbonate is added. The pH is adjusted to 4.2, the stirring speed is 125rpm, and the mixture is stirred at room temperature for 30min. After the reaction is complete, the solid and liquid are separated to obtain silver precipitated residue and silver precipitated liquid. The silver precipitated liquid is sent to the wastewater tank. S4 Copper Removal: Weigh the silver precipitate residue and measure its moisture content. Place 32.3g of the silver precipitate residue into a 250ml three-necked flask, add 120ml of water, start stirring, heat to 45℃, and stir at 90rpm for 25min. Add 66% nitric acid and observe the reaction. The reaction is complete when the solution turns blue. Separate the solid and liquid to obtain copper-containing residue and silver electrolyte. The silver electrolyte is used as a supplementary electrolyte for evaporation. S5 gold separation: The pre-impregnated residue obtained from S1 is washed twice with pure water at 70℃. 56.7g of the pre-impregnated residue is placed in a 500ml three-necked flask, 186ml of water is added, and 20ml of 36% hydrochloric acid is added. Stirring is started, the temperature is raised to 95℃, the rotation speed is 120rpm, and 50% sodium chlorate is slowly added. Stirring is carried out for 80min. After the reaction is completed, the solid and liquid are separated to obtain gold separation residue and gold separation solution. The gold separation residue is dried, weighed, and the moisture content is measured. After testing, it is sent to the pyrometallurgical process. S6 Platinum Precipitation: The volume of the gold-separating solution obtained from S5 was measured to be 183 ml using a graduated cylinder. It was then placed in a 500 ml three-necked flask, stirred, and heated to 70°C. First, 45% sodium hydroxide was added to adjust the pH to 2.7, and then 20% potassium carbonate was added to adjust the pH to 3.6. The stirring speed was 117 rpm for 40 min. After the reaction was completed, the solid and liquid were separated to obtain platinum concentrate and platinum precipitation liquid. The platinum concentrate was then sent to the platinum refining process. S7 Acid Reversion: The volume of the liquid after platinum precipitation is measured to be 165ml using a graduated cylinder. It is then placed in a 500ml three-necked flask. Stirring is started, and the acid concentration is calculated. Hydrochloric acid with a concentration of 36% is added to a concentration of 120g / L. The stirring speed is 30rpm, and the mixture is stirred for 20min. After the reaction is complete, solid and liquid are separated to obtain waste acid residue and high gold solution. The waste acid residue is dried, weighed, and the moisture content is measured. After being sent to the pyrometallurgical process, the sample is sent to the pyrometallurgical process. S8 Reduction: The volume of the high-purity gold solution was measured to be 178 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started, and the temperature was raised to 75°C at 110 rpm. Formic acid with a concentration of 20% was added. The reaction was complete when the solution was colorless and transparent. The mixture was stirred for 70 min, and the solid and liquid were separated to obtain qualified gold powder and the high-purity gold reduced solution. The high-purity gold reduced solution was sent to the wastewater tank. The qualified gold powder was washed with 70°C pure water until neutral, and the solid and liquid were separated to obtain high-purity gold.
[0033] II. Palladium Refining S21 Pre-leaching: Take 100g of palladium concentrate obtained from gold refining S2 and add it to a 1500ml three-necked flask. Add 300ml of pure water and 25ml of 36% hydrochloric acid. Turn on the stirrer at 85rpm and heat it to 75℃. Stir for 23min until the reaction is complete. Separate the solid and liquid to obtain palladium-dissolving slag and palladium-containing solution. Dry the palladium-dissolving slag, weigh it, and determine its moisture content. Send the sample to the pyrometallurgical process. S22 Palladium-Rich Solution: The volume of the palladium-containing solution was measured to be 331 ml using a graduated cylinder. This solution was then added to a 500 ml three-necked flask. The mixture was stirred at 102 rpm and heated to 79°C. A precipitating agent (a mixture of sodium chloride and potassium sulfate in a 1:1.5 mass ratio, added in an amount 1.8 times the palladium content in the solution) was added. An oxidizing agent (50% sodium chlorate, added in an amount 0.6 times the palladium content in the solution) was slowly added. The mixture was stirred for 60 minutes. After the reaction was complete, the solid and liquid were separated to obtain palladium-rich residue and palladium-rich post-residue. The palladium-rich post-residue was sent to the wastewater tank. S23 Palladium Dissolution: Weigh the palladium-rich residue and determine its moisture content. Place 112.6g of the palladium-rich residue into a 500ml three-necked flask, add 448ml of 25% ammonia water, start stirring at 101rpm, heat to 94℃, stir for 33min, and after the reaction is complete, separate the solid and liquid to obtain a palladium-containing solution and a primary palladium-dissolution residue. Dry the primary palladium-dissolution residue, weigh it, determine its moisture content, and send it to the pyrometallurgical process. S24 High Palladium: The volume of the palladium-separated solution was measured to be 396 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 105 rpm, and the temperature was raised to 89°C. Precipitating reagent (a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.5, with the amount added being 1.8 times the palladium content in the solution) was added. Oxidizing agent (50% sodium chlorate, with the amount added being 0.6 times the palladium content in the solution) was slowly added. The mixture was stirred for 30 min. After the reaction was completed, the solid and liquid were separated to obtain high palladium ore and palladium-separated solution. The palladium-separated solution was sent to the wastewater tank. S25 Secondary Palladium Dissolution: Weigh the high-palladium ore and determine its moisture content. Place 108.7g of high-palladium ore into a 500ml three-necked flask, add 420ml of 25% ammonia water, start stirring at 81rpm, heat to 84℃, stir for 13min, and after the reaction is complete, separate the solid and liquid to obtain high-palladium solution and secondary palladium dissolution residue. Dry the secondary palladium dissolution residue, weigh it, determine its moisture content, and send it to the pyrometallurgical process. S26 Reduction: The volume of the high-palladium solution was measured to be 379 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 75 rpm. 20% formic acid was added and the solution was observed to turn pale yellow. After stirring for 22 min, the reaction was completed. Solid-liquid separation was performed to obtain the high-palladium reduced solution and palladium powder. The high-palladium reduced solution was sent to the wastewater tank. The palladium powder was washed with 70℃ pure water until neutral. Solid-liquid separation was performed to obtain qualified palladium powder.
[0034] III. Platinum Refining S61 pre-leaching: Take 100g of platinum concentrate obtained from gold refining S6 and add it to a 1500ml three-necked flask. Add 420ml of pure water and 33ml of 36% hydrochloric acid. Start stirring at 77rpm and heat to 50℃. Stir for 56min. After the reaction is complete, separate the solid and liquid to obtain platinum slag and platinum-containing solution. Dry the platinum slag, weigh it and determine its moisture content. Send the sample to the pyrometallurgical process. S62 Platinum-Rich Solution: The volume of the platinum-containing solution measured with a graduated cylinder is 354 ml. It is added to a 500 ml three-necked flask, stirred at 108 rpm, and heated to 75°C. A precipitating agent (a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.5, with the amount added being 1.5 times the platinum content in the solution) is added. An oxidizing agent (a 50% sodium chlorate solution, with the amount added being 0.95 times the platinum content in the solution) is slowly added. The mixture is stirred for 34 min. After the reaction is complete, the solid and liquid are separated to obtain platinum-rich residue and platinum-rich post-residue. The platinum-rich post-residue is sent to the wastewater tank. S63 Impurity Removal and Separation: Weigh the platinum-rich slag, measure its moisture content, put 117.5g of platinum-rich slag into a 500ml three-necked flask, add 350ml of pure water, start stirring at 113rpm, heat to 84℃, add 35% hydrazine sulfate, the amount of hydrazine sulfate added is 1.45 times the palladium content in the solution, stir for 8min, after the reaction is complete, separate the solid and liquid to obtain platinum-containing slag and palladium-separated solution, and then go through the palladium refining process to enrich the palladium. S64 Platinum Dissolution: Weigh the platinum-containing slag and determine its moisture content. Place 107.6g of platinum-containing slag into a 500ml three-necked flask, add 330ml of pure water, start stirring at 112rpm, heat to 98℃, add 35% hydrazine sulfate (the amount of hydrazine sulfate added is 1.8 times the platinum content in the solution), stir for 26min, after the reaction is complete, separate the solid and liquid to obtain primary platinum-dissolving slag and platinum-separated solution. Dry the primary platinum-dissolving slag, weigh it, and determine its moisture content. After sending the sample, proceed to the pyrometallurgical process. S65 High Platinum: The volume of the platinum-separated liquid measured with a graduated cylinder is 308 ml. It is placed in a 500 ml three-necked flask, stirred at 89 rpm, and heated to 88°C. A precipitating reagent (a mixture of sodium chloride and potassium sulfate in a 1:1.5 mass ratio, added in an amount 1.5 times the platinum content in the solution) is added. An oxidizing agent (50% sodium chlorate, added in an amount 0.95 times the platinum content in the solution) is slowly added. The mixture is stirred for 13 min. After the reaction is complete, the solid and liquid are separated to obtain high platinum residue and platinum-separated liquid. The platinum-separated liquid is sent to the wastewater tank. S66 Secondary Platinum Dissolution: Weigh the high-platinum residue and determine its moisture content. Place 99.3g of the high-platinum residue into a 500ml three-necked flask, add 300ml of pure water, start stirring at 112rpm, heat to 98℃, add 35% hydrazine sulfate (the amount of hydrazine sulfate added is 1.8 times the platinum content in the solution), stir for 26min, after the reaction is complete, separate the solid and liquid to obtain secondary platinum dissolution residue and high-platinum solution. Dry the secondary platinum dissolution residue, weigh it, and determine its moisture content. After sending the sample, proceed to the pyrometallurgical process. S67 Reduction: The volume of the high-platinum solution was measured to be 283 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 83 rpm. 20% formic acid was added and the solution was observed to turn pale yellow. After stirring for 23 min, the reaction was completed. Solid-liquid separation was performed to obtain the high-platinum reduced solution and platinum powder. The high-platinum reduced solution was sent to the wastewater tank. The platinum powder was washed with 70℃ pure water until neutral. Solid-liquid separation was performed to obtain qualified platinum powder.
[0035] In this embodiment, the recovery rate of gold is 99.3%, the recovery rate of silver is 99.7%, the recovery rate of platinum is 99.1%, and the recovery rate of palladium is 99.0%; the purity of gold is 99.999%, the purity of silver is 99.992%, the purity of platinum is 99.992%, and the purity of palladium is 99.993%.
[0036] Example 2 This embodiment provides a comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium, comprising the following steps: I. Gold Refining S1 Pre-impregnation: Pre-impregnation: Add 100g of silver anode mud to a 1500ml three-necked flask, add 300ml of pure water, add 50ml of 67% nitric acid, start stirring at 140rpm, heat to 75℃, stir for 5h, after the reaction is complete, separate the solid and liquid to obtain pre-impregnation residue and pre-impregnation liquid, further process the pre-impregnation liquid, wash the pre-impregnation residue twice with 70℃ hot water, and separate the solid and liquid to obtain pre-impregnation residue; the mass ratio of silver anode mud, pure water and nitric acid is 4:12:2; S2 Palladium Precipitation: The volume of the pre-impregnation solution was measured to be 224 ml using a graduated cylinder. It was then added to a 500 ml three-necked flask. Stirring was started, and the temperature was raised to 66°C. Sodium hydroxide and potassium carbonate were added. The pH was first adjusted to 1.4 using 45% sodium hydroxide, and then adjusted to 2.4 using 20% potassium carbonate. The stirring speed was 135 rpm, and the mixture was stirred for 80 min. After the reaction was completed, the solid and liquid were separated to obtain palladium concentrate and palladium precipitation liquid. The palladium concentrate was sent to the palladium refining system for further processing. S3 Silver Precipitation: The volume of the palladium-precipitated liquid after measurement with a graduated cylinder is 213ml. It is added to a 500ml three-necked flask, stirred, and 20% potassium carbonate is added. The pH is adjusted to 4.0, the stirring speed is 105rpm, and the mixture is stirred at room temperature for 40min. After the reaction is complete, the solid and liquid are separated to obtain silver precipitate residue and silver precipitate liquid. The silver precipitate liquid is sent to the wastewater tank. S4 Copper Removal: Weigh the silver precipitate residue and measure its moisture content. Place 31.8g of the silver precipitate residue into a 250ml three-necked flask, add 120ml of water, start stirring, heat to 40℃, and stir at 100rpm for 30min. Add 66% nitric acid and observe the reaction. The reaction is complete when the solution turns blue. Separate the solid and liquid to obtain copper-containing residue and silver electrolyte. The silver electrolyte is used as a supplementary electrolyte for evaporation. S5 gold separation: The pre-impregnated residue obtained from S1 is washed twice with pure water at 70℃. 54.9g of the pre-impregnated residue is placed in a 500ml three-necked flask, 178ml of water is added, and 18ml of 36% hydrochloric acid is added. Stirring is started, the temperature is raised to 85℃, the rotation speed is 140rpm, and 50% sodium chlorate is slowly added. Stirring is carried out for 120min. After the reaction is completed, solid and liquid are separated to obtain gold separation residue and gold separation solution. The gold separation residue is dried, weighed, and the moisture content is measured. After testing, it is sent to the pyrometallurgical process. S6 Platinum Precipitation: The volume of the gold-precipitating solution was measured to be 174 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started, and the temperature was raised to 60°C. First, 45% sodium hydroxide was added to adjust the pH to 2.9, and then 20% potassium carbonate was added to adjust the pH to 3.4. The stirring speed was 137 rpm, and the mixture was stirred for 60 min. After the reaction was completed, the solid and liquid were separated to obtain platinum concentrate and platinum precipitation liquid. The platinum concentrate was then sent to the platinum refining process. S7 Acid Reversion: The volume of the gold-reducing solution was measured to be 161 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started, and the acid concentration was calculated. Hydrochloric acid with a concentration of 36% was added to 120 g / L. The stirring speed was 60 rpm, and the mixture was stirred for 10 min. After the reaction was completed, the solid and liquid were separated to obtain waste acid residue and high gold solution. The waste acid residue was dried, weighed, and the moisture content was measured. After being sent to the pyrometallurgical process, the sample was sent to the pyrometallurgical process. S8 Reduction: The volume of the high-purity gold solution was measured to be 176 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started, and the temperature was raised to 55°C at 130 rpm. Formic acid with a concentration of 20% was added. The reaction was complete when the solution was colorless and transparent. The mixture was stirred for 90 min, and the solid and liquid were separated to obtain qualified gold powder and the high-purity gold reduced solution. The high-purity gold reduced solution was sent to the wastewater tank. The qualified gold powder was washed with 70°C pure water until neutral, and the solid and liquid were separated to obtain high-purity gold.
[0037] II. Palladium Refining S21 Pre-leaching: Take 100g of palladium concentrate obtained from gold refining S2 and add it to a 1500ml three-necked flask. Add 300ml of pure water and 25ml of 36% hydrochloric acid. Turn on the stirrer at 105rpm and heat it to 58℃. Stir for 43min until the reaction is complete. Separate the solid and liquid to obtain palladium-dissolving slag and palladium-containing solution. Dry the palladium-dissolving slag, weigh it, and determine its moisture content. Send the sample to the pyrometallurgical process. S22 Palladium-Rich Solution: The volume of the palladium-containing solution was measured to be 326 ml using a graduated cylinder. This solution was then added to a 500 ml three-necked flask. Stirring was started at 132 rpm, and the temperature was raised to 59°C. A precipitating agent (a mixture of sodium chloride and potassium sulfate in a 1:1.5 mass ratio, added in an amount 1.8 times the palladium content in the solution) was added. An oxidizing agent (50% sodium chlorate, added in an amount 0.6 times the palladium content in the solution) was slowly added. The mixture was stirred for 90 minutes. After the reaction was complete, the solid and liquid were separated to obtain palladium-rich residue and palladium-rich post-residue. The palladium-rich post-residue was sent to the wastewater tank. S23 Palladium Dissolution: Weigh the palladium-rich residue and determine its moisture content. Place 108.8g of the palladium-rich residue into a 500ml three-necked flask, add 432ml of 25% ammonia water, start stirring at 121rpm, heat to 84℃, stir for 53min, and after the reaction is complete, separate the solid and liquid to obtain a palladium-containing solution and a primary palladium-dissolution residue. Dry the primary palladium-dissolution residue, weigh it, determine its moisture content, and send the sample to the pyrometallurgical process. S24 High Palladium: The volume of the palladium-separated solution was measured to be 379 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 125 rpm, and the temperature was raised to 69°C. Precipitating reagent (a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.5, with the amount added being 1.8 times the palladium content in the solution) was added. Oxidizing agent (50% sodium chlorate, with the amount added being 0.6 times the palladium content in the solution) was slowly added. The mixture was stirred for 60 min. After the reaction was completed, the solid and liquid were separated to obtain high palladium ore and palladium-separated solution. The palladium-separated solution was sent to the wastewater tank. S25 Secondary Palladium Dissolution: Weigh the high-palladium ore and determine its moisture content. Place 109.6g of high-palladium ore into a 500ml three-necked flask, add 440ml of 25% ammonia water, start stirring at 101rpm, heat to 64℃, stir for 33min, and after the reaction is complete, separate the solid and liquid to obtain high-palladium solution and secondary palladium dissolution residue. Dry the secondary palladium dissolution residue, weigh it, determine its moisture content, and send it to the pyrometallurgical process. S26 Reduction: The volume of the high-palladium solution was measured to be 386 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 55 rpm. 20% formic acid was added and the solution was observed to turn pale yellow. After stirring for 42 min, the reaction was completed. Solid-liquid separation was performed to obtain the high-palladium reduced solution and palladium powder. The high-palladium reduced solution was sent to the wastewater tank. The palladium powder was washed with 70℃ pure water until neutral. Solid-liquid separation was performed to obtain qualified palladium powder.
[0038] III. Platinum Refining S61 pre-leaching: Take 100g of platinum concentrate obtained from gold refining S6 and add it to a 1500ml three-necked flask. Add 420ml of pure water and 33ml of 36% hydrochloric acid. Start stirring at 97rpm and heat to 30℃. Stir for 86min until the reaction is complete. Separate the solid and liquid to obtain platinum slag and platinum-containing solution. Dry the platinum slag, weigh it, and determine its moisture content. Send the sample to the pyrometallurgical process. S62 Platinum-Rich Solution: The volume of the platinum-containing solution was measured to be 366 ml using a graduated cylinder. This solution was then added to a 500 ml three-necked flask. Stirring was started at 128 rpm, and the temperature was raised to 55°C. A precipitating agent (a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:1.5, with the amount added being 1.5 times the platinum content in the solution) was added. An oxidizing agent (a 50% sodium chlorate solution, with the amount added being 0.95 times the platinum content in the solution) was slowly added. The mixture was stirred for 54 min until the reaction was complete. Solid-liquid separation was performed to obtain platinum-rich residue and platinum-rich post-residue. The platinum-rich post-residue was sent to the wastewater tank. S63 Impurity Removal and Separation: Weigh the platinum-rich slag, measure its moisture content, put 109.1g of platinum-rich slag into a 500ml three-necked flask, add 330ml of pure water, start stirring at 133rpm, heat to 58℃, add 35% hydrazine sulfate, the amount of hydrazine sulfate added is 1.45 times the palladium content in the solution, stir for 18min, after the reaction is complete, separate the solid and liquid to obtain platinum-containing slag and platinum-separated solution, and send the palladium-separated solution to the palladium refining process and the palladium enrichment process; S64 Platinum Dissolution: Weigh the platinum-containing slag and determine its moisture content. Place 102.4g of platinum-containing slag into a 500ml three-necked flask, add 310ml of pure water, start stirring at 132rpm, heat to 92℃, add 35% hydrazine sulfate (the amount of hydrazine sulfate added is 1.8 times the platinum content in the solution), stir for 46min, after the reaction is complete, separate the solid and liquid to obtain primary platinum-dissolving slag and platinum-separated solution. Dry the primary platinum-dissolving slag, weigh it, and determine its moisture content. After sending the sample, proceed to the pyrometallurgical process. S65 High Platinum: The volume of the platinum-separated liquid measured with a graduated cylinder is 297 ml. It is placed in a 500 ml three-necked flask, stirred at 109 rpm, and heated to 68°C. A precipitating reagent (a mixture of sodium chloride and potassium sulfate in a 1:1.5 mass ratio, added in an amount 1.5 times the platinum content in the solution) is added. An oxidizing agent (50% sodium chlorate, added in an amount 0.95 times the platinum content in the solution) is slowly added. The mixture is stirred for 33 min. After the reaction is complete, the solid and liquid are separated to obtain high platinum residue and platinum-separated liquid. The platinum-separated liquid is sent to the wastewater tank. S66 Secondary Platinum Dissolution: Weigh the high-platinum slag and determine its moisture content. Place 97.5g of the high-platinum slag into a 500ml three-necked flask, add 290ml of pure water, start stirring at 132rpm, heat to 92℃, add 35% hydrazine sulfate (the amount of hydrazine sulfate added is 1.8 times the platinum content in the solution), stir for 46min, after the reaction is complete, separate the solid and liquid to obtain secondary platinum dissolution slag and high-platinum solution. Dry the secondary platinum dissolution slag, weigh it, and determine its moisture content. After sending the sample, proceed to the pyrometallurgical process. S67 Reduction: The volume of the high-platinum solution was measured to be 274 ml using a graduated cylinder and placed in a 500 ml three-necked flask. Stirring was started at 63 rpm. 20% formic acid was added and the solution was observed to turn pale yellow. After stirring for 43 min, the reaction was completed. Solid-liquid separation was performed to obtain the high-platinum reduced solution and platinum powder. The high-platinum reduced solution was sent to the wastewater tank. The platinum powder was washed with 70℃ pure water until neutral. Solid-liquid separation was performed to obtain qualified platinum powder.
[0039] In this embodiment, the recovery rate of gold is 99.2%, the recovery rate of silver is 99.6%, the recovery rate of platinum is 99.2%, and the recovery rate of palladium is 99.0%; the purity of gold is 99.999%, the purity of silver is 99.991%, the purity of platinum is 99.993%, and the purity of palladium is 99.992%.
[0040] Example 3 This embodiment provides a comprehensive recycling method for high-purity gold, silver, platinum, and palladium.
[0041] The difference between this embodiment and Example 1 is that in palladium refining, in steps S22 (palladium enrichment) and S24 (high palladium), a mixed reagent of sodium chloride and potassium sulfate in a 1:1 mass ratio is used as the precipitating agent. In platinum refining, in steps S62 (platinum enrichment) and S64 (high platinum), a mixed reagent of sodium chloride and potassium sulfate in a 1:1 mass ratio is used as the precipitating agent. All other parameters are the same as in Example 1.
[0042] In this embodiment, the recovery rate of platinum was 99.0% and the recovery rate of palladium was 99.1%; the purity of platinum was 99.982% and the purity of palladium was 99.978%.
[0043] Example 4 This embodiment provides a comprehensive recycling method for high-purity gold, silver, platinum, and palladium.
[0044] The difference between this embodiment and Example 1 is that in the platinum refining process, 25% ammonia water is used instead of hydrazine sulfate as the dissolving agent in the S62 platinum-rich and S64 high-platinum steps. All other parameters are the same as in Example 1.
[0045] In this embodiment, the platinum recovery rate was 99.0%, and the platinum purity was 99.965%.
[0046] Example 5 This embodiment provides a comprehensive recycling system for high-purity gold, silver, platinum, and palladium, including a gold refining system (as shown in the device diagram). Figure 2 (As shown), palladium refining system (device diagram as shown) Figure 3 As shown), platinum refining system (device diagram as shown) Figure 4 (as shown) The gold refining system includes: a pre-impregnation tank 1 connected to a pre-impregnation filter tank 2; the outlet of the pre-impregnation filter tank 2 is connected to a palladium precipitation tank 14 via a pipeline connected to a pump 13; the slag outlet of the pre-impregnation filter tank 2 is connected to a gold separation tank 3; the gold separation tank 3 is connected to a gold separation filter tank 4; the outlet of the gold separation filter tank 4 is connected to a platinum-palladium precipitation tank 6 via a pipeline connected to a pump 5; reagents flow by gravity into the platinum precipitation tank 6 through a second high-level tank 24 and a third high-level tank 25; the platinum precipitation tank 6 is connected to a platinum precipitation filter press 8 via a pipeline connected to a pump 7; the outlet of the platinum precipitation filter press 8 is connected to a gold reduction tank 10; reagents are added to the gold reduction tank 10 through a first high-level tank 9; the gold reduction tank... 10 connects to the gold powder filter tank 11. The outlet of the gold powder filter tank 11 is connected to the wastewater tank 23 via a pipeline to the pump 12. The reagent flows into the palladium precipitation kettle 14 by gravity through the second high-level tank 24 and the third high-level tank 25. The palladium precipitation kettle 14 is connected to the palladium precipitation filter press 16 via a pipeline to the pump 15. The outlet of the palladium precipitation filter press 16 is connected to the silver precipitation kettle 17. The silver precipitation kettle 17 is connected to the silver precipitation filter press 19 via a pipeline to the pump 18. The outlet of the silver precipitation filter press 19 is connected to the wastewater tank 23. The slag outlet of the silver precipitation filter press 19 is connected to the copper kettle 20. The copper kettle 20 is connected to the copper removal filter press 22 via a pipeline to the pump 21.
[0047] The palladium refining system includes: a palladium melting kettle 26 connected to a palladium melting filter press 28 via a pipeline and a pump 27; the outlet of the palladium melting filter press 28 is connected to a palladium enrichment kettle 29; the palladium enrichment kettle 29 is connected to a palladium enrichment filter press 31; the outlet of the palladium enrichment filter press 31 is connected to a wastewater tank 23; the slag outlet of the palladium enrichment filter press 31 is connected to a palladium separation kettle 32; the palladium separation kettle 32 is connected to a palladium separation filter press 34 via a pipeline and a pump 33; the outlet of the palladium separation filter press 34 is connected to a high palladium kettle 35; and the high palladium kettle 35 is connected to a pump 36 via a pipeline. A high-palladium filter press 37 is connected to a wastewater tank 23 at its outlet and to a high-palladium water reactor 62 at its slag outlet. The high-palladium water reactor 62 is connected to a high-palladium water filter press 64 via a pipeline connected to a pump 63. The outlet of the high-palladium water filter press 64 is connected to a palladium reduction reactor 39. Reagents are added to the palladium reduction reactor 39 by gravity through a fourth high-level tank 38. The palladium reduction reactor 39 is connected to a palladium reduction filter press 41 via a pipeline connected to a pump 40. The outlet of the palladium reduction filter press 41 is connected to the wastewater tank 23.
[0048] The platinum refining system includes: a platinum dissolving kettle 42 connected to a platinum dissolving filter press 44 via a pipeline and a pump 43; the outlet of the platinum dissolving filter press 44 is connected to a platinum enrichment kettle 45; the platinum enrichment kettle 45 is connected to a platinum enrichment filter press 47 via a pipeline and a pump 46; the outlet of the platinum enrichment filter press 47 is connected to a wastewater tank 23; the slag outlet of the platinum enrichment filter press 47 is connected to a purification kettle 65; the purification kettle 65 is connected to a purification filter press 49 via a pipeline and a pump 48; the slag outlet of the purification filter press 49 is connected to a platinum separation kettle 50; and the platinum separation kettle 50 is connected to a platinum separation filter press 52 via a pipeline and a pump 51. The outlet of the platinum reduction filter press 52 is connected to the high platinum reactor 53. The high platinum reactor 53 is connected to the high platinum ore filter press 55 via a pipeline to the pump 54. The outlet of the high platinum ore filter press 55 is connected to the wastewater tank 23. The slag outlet of the high platinum ore filter press 55 is connected to the high platinum water reactor 56. The high platinum water reactor 56 is connected to the high platinum water filter press 58 via a pipeline to the pump 57. The outlet of the high platinum water filter press 58 is connected to the platinum reduction reactor 59. The platinum reduction reactor 59 is connected to the platinum reduction filter press 61 via a pipeline to the pump 60. The outlet of the platinum reduction filter press 61 is connected to the wastewater tank 23.
[0049] Among them, the pre-impregnation kettle 1, gold separation kettle 3, platinum-palladium immersion kettle 3, and gold reduction kettle 10 are made of composite titanium jacketed reactors; the pre-impregnation filter tank 2, gold separation filter tank 4, and gold powder filter tank 11 are made of titanium; the first high-level tank 9, the second high-level tank 24, the third high-level tank 25, and the fourth high-level tank 38 are made of steel-lined PO; the palladium immersion kettle 14, the silver immersion kettle 17, and the copper removal kettle 20 are made of enamel; the wastewater tank 23 is made of PPH; and the palladium dissolving kettle 26, the palladium-rich kettle 29, the palladium separation kettle 32, the high palladium kettle 35, the high palladium water kettle 62, the palladium reduction kettle 39, the platinum dissolving kettle 42, the platinum-rich kettle 45, the impurity removal kettle 48, the platinum separation kettle 50, the high platinum kettle 53, the high platinum water kettle 56, and the platinum reduction kettle 59 are all made of enamel.
[0050] In this embodiment, due to the large amount and density of slag in the gold separating kettle 3, the particle size is large, and the contact area is small, so a compressed air pipe is added to the gold separating kettle 3 and coiled along the kettle wall. Holes with a diameter of 1.5 cm are opened every 30 cm below the pipe. A first electronic hydrometer is installed in the middle of the gold separating kettle 3, and a second electronic hydrometer is installed at the bottom of the gold separating kettle 3. The density at the bottom and the middle is monitored in real time to determine whether it is uniform. The two electronic hydrometers are interlocked with the compressed air regulating valve 66. The interlock is as follows: if the difference between the two electronic hydrometers is less than 0.05, the compressed air regulating valve 66 maintains this opening. If the difference between the two electronic hydrometers is greater than 0.05, the compressed air regulating valve 66 increases the opening by 5% every 2 minutes, so that the material in the kettle is more uniform.
[0051] In this embodiment, the reduction vessel 10 is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the first high-level tank 9. The interlock is as follows: if the potential inside the vessel is less than -0.67V, the outlet valve of the first high-level tank 9 will be closed. This measure can reduce manual labor and make the reduction more thorough.
[0052] In this embodiment, the palladium precipitation vessel 14 is equipped with an electronic pH meter. The electronic pH meter is interlocked with the outlet valves of the second high-level tank 24 and the third high-level tank 25. The interlocking mechanism is as follows: when pH ≤ 1.5, the outlet valve of the second high-level tank is open and the outlet valve of the third high-level tank is closed; when pH > 1.5 and ≤ 2.3, the outlet valve of the second high-level tank is closed and the outlet valve of the third high-level tank is open; when pH > 2.3, both the outlet valves of the second and third high-level tanks are closed.
[0053] In this embodiment, the platinum precipitation vessel is equipped with an electronic pH meter. The electronic pH meter is interlocked with the outlet valves of the second high-level tank 24 and the third high-level tank 25. The interlocking mechanism is as follows: when pH < 2.8, the outlet valve of the second high-level tank 24 is open and the outlet valve of the third high-level tank 25 is closed; when pH > 2.8 and ≤ 3.5, the outlet valve of the second high-level tank 24 is closed and the outlet valve of the third high-level tank 25 is open; when pH > 3.5, both the outlet valves of the second high-level tank 24 and the outlet valve of the third high-level tank 25 are closed.
[0054] In this embodiment, the palladium reduction vessel 39 is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank 38. The interlocking mechanism is as follows: if the potential inside the vessel is less than -1.32V, the outlet valve is closed; and the single-point direct addition method is changed to a four-point feeding method parallel to the stirring, so that the reduction is more thorough.
[0055] In this embodiment, the platinum reduction vessel 59 is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank 38. The interlocking mechanism is as follows: if the potential inside the vessel is less than -1.17V, the outlet valve is closed; and the single-point direct addition method is changed to a four-point feeding method parallel to the stirring, so that the reduction is more thorough.
[0056] Comparative Example 1 This comparative example provides a comprehensive recovery and processing method for high-purity gold, silver, platinum, and palladium.
[0057] The difference between this comparative example and Example 1 is that in the gold refining process, the palladium precipitation step S2 is as follows: potassium sulfate and magnesium chloride are added to the pre-impregnation solution obtained in S1, with a molar ratio of potassium sulfate to magnesium chloride of 1.4:1. The amount of potassium sulfate and magnesium chloride added is 2.4 times the palladium content in the solution. The temperature is raised to 60°C, the stirring speed is 130 rpm, and then sodium chlorate with a concentration of 53% is added. The reaction is carried out for 90 minutes, and solid-liquid separation is performed. After the reaction is completed, palladium concentrate and palladium precipitation liquid are obtained from the solid-liquid separation. The palladium concentrate is sent to the palladium refining system for further processing.
[0058] In this comparative example, the recovery rate of silver was 98.5%, and the recovery rate of palladium was 98.4%; the purity of silver was 99.93%, and the purity of platinum was 99.92%.
[0059] Comparative Example 2 This comparative example provides a comprehensive recovery and processing method for high-purity gold, silver, platinum, and palladium.
[0060] The difference between this comparative example and Example 1 is that in the gold refining process, the palladium precipitation step S2 is as follows: the pre-impregnation solution obtained in S1 is heated to 73°C, sodium hydroxide and potassium carbonate are added, the pH is first adjusted to 1.8 using 45% sodium hydroxide, and then the pH is adjusted to 3 using 20% potassium carbonate. The stirring speed is 115 rpm, and the mixture is stirred for 60 minutes. After the reaction is completed, the solid and liquid are separated to obtain palladium concentrate and palladium precipitation liquid. The palladium concentrate is then sent to the palladium refining system for further processing.
[0061] In this comparative example, the recovery rate of silver was 98.2% and the recovery rate of palladium was 98.8%; the purity of silver was 99.94% and the purity of platinum was 99.91%.
[0062] Comparative Example 3 This comparative example provides a comprehensive recovery and processing method for high-purity gold, silver, platinum, and palladium.
[0063] The difference between this comparative example and Example 1 is that in the gold refining process, the S3 silver precipitation step is as follows: 20% potassium carbonate is added to the palladium precipitation solution to adjust the pH to 4.8. The mixture is stirred for 30 minutes at room temperature and 125 rpm to obtain silver precipitation residue. In this comparative example, the silver recovery rate was 99.7%, and the silver purity was 99.95%.
[0064] Comparative Example 4 This comparative example provides a comprehensive recovery and processing method for high-purity gold, silver, platinum, and palladium.
[0065] The difference between this comparative example and Example 1 is that in the gold refining process, the S6 platinum precipitation step is as follows: the gold separation solution obtained in S5 is heated to 70°C, 45% sodium hydroxide is added to adjust the pH to 2, then 20% potassium carbonate is added to adjust the pH to 4, the stirring speed is 117 rpm, and the stirring is carried out for 40 minutes. After the reaction is completed, the solid and liquid are separated to obtain platinum concentrate and platinum precipitation liquid. The platinum concentrate is then sent to the platinum refining process.
[0066] In this comparative example, the recovery rate of gold was 98.8% and the recovery rate of platinum was 98.0%; the purity of gold was 99.92% and the purity of platinum was 99.93%.
[0067] In summary, this invention provides a method and system for recovering gold, silver, palladium, and platinum from silver anode mud. First, the silver anode mud is pre-leached with nitric acid, allowing silver, palladium, and copper to be leached out as much as possible into the pre-leaching solution, preventing the generation of large amounts of gold-separating slag in subsequent processes. The pH of the pre-leaching solution is precisely controlled by sequentially adding alkaline reagents and potassium salts, precipitating palladium and reducing palladium loss. The palladium compound precipitate can be further processed to obtain palladium powder. By adjusting the pH of the solution after palladium precipitation, silver can be further precipitated, preventing the formation of silver chloride precipitate and producing a more stable black precipitate. The black precipitate can be dissolved by adding acid, turning it into a silver nitrate solution, which can be used as a replenishing electrolyte. In the gold-separating solution, the pH is precisely controlled by sequentially adding alkaline reagents and potassium salts, precipitating platinum and making the solution purer. This allows for faster subsequent reduction processes, shortening the process flow and reducing process time. The gold-separating solution removes impurities to negligible levels, resulting in high-purity gold in subsequent reduction.
[0068] The method provided by this invention significantly improves the purity of gold, silver, platinum, and palladium while ensuring a recovery rate of over 99.0%. Gold purity reaches 99.999%, and the purity of silver, platinum, and palladium reaches over 99.96%. Furthermore, in the palladium enrichment and high-palladium steps of palladium refining, this invention uses a mixed reagent of sodium chloride and potassium sulfate at a mass ratio of 1:1.4-1.6 as a precipitating agent; in the platinum enrichment and high-platinum steps of platinum refining, it uses a mixed reagent of sodium chloride and potassium sulfate at a mass ratio of 1:1.4-1.6 as a precipitating agent, and uses hydrazine sulfate as a platinum dissolving agent, which further improves the recovery rate and purity of platinum and palladium.
[0069] The foregoing descriptions have outlined some exemplary embodiments of the present invention. It is understood that these embodiments are merely illustrative and do not constitute a limitation on the scope of protection of the present invention. Features in these embodiments can be rearranged in suitable ways, and the resulting solutions remain within the scope of protection claimed by the present invention. All other embodiments obtained by those skilled in the art based on the foregoing embodiments without inventive effort, i.e., all modifications, equivalent substitutions, and improvements made within the spirit and principles of this application, fall within the scope of protection claimed by the present invention.
Claims
1. A method for comprehensive recovery of high-purity gold and silver platinum-palladium, characterized by, Includes the following steps: Gold refining, palladium refining, platinum refining; the gold refining includes the following steps: S1 pre-impregnation; S2 Palladium precipitation: First, add an alkaline reagent to the pre-leaching solution obtained in S1 to adjust the pH to 4-6, then add potassium salt to adjust the pH to 2-4, and react at 66-73℃ for 60-80 minutes to obtain palladium concentrate and palladium precipitation solution; S3 Silver precipitation: Add potassium salt to the palladium precipitation solution to adjust the pH to 0-2, react at room temperature for 30-40 minutes to obtain silver precipitation residue; S4 Copper Removal: An acidic reagent is added to the silver precipitate residue to obtain a silver electrolyte; S5 cents; S6 Platinum Precipitation: First, add an alkaline reagent to the gold separation solution obtained in S5 to adjust the pH to 7-9, then add potassium salt to adjust the pH to 4-6, and react at 60-70℃ for 40-60 min to obtain platinum concentrate and platinum precipitation solution. S7 Acid Reversion: An acidic reagent is added to the platinum-precipitated solution, and a high-gold solution is obtained after the reaction. S8 Reduction: Formic acid is added to the high-purity gold solution for reduction, followed by washing to obtain high-purity gold powder.
2. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 1, characterized in that, In S1, the silver anode mud is pre-impregnated with pure water and nitric acid with a concentration of 65-68%, and the mass ratio of silver anode mud, pure water and nitric acid is (1-5.6):(5.4-16.8):(2-6); In S2 and S6, the alkaline reagent is sodium hydroxide with a concentration of 40-50%, and the potassium salt is potassium carbonate with a concentration of 15-25%; In S3, the potassium salt is potassium carbonate with a concentration of 15-25%; In S4, the acidic reagent is nitric acid with a concentration of 65-68%; In S5, the gold separation step is as follows: after washing the pre-impregnated residue obtained in S1, hydrochloric acid with a concentration of 33-39% and sodium chlorate oxidant with a concentration of 40-60% are added for gold separation; In S7, the acidic reagent is hydrochloric acid with a concentration of 33-39%, and in S8, formic acid has a concentration of 15-25%.
3. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 1, characterized in that, In S1, the reaction temperature is 75-85℃, the stirring speed is 140-180 rpm, and the reaction time is 3-5 h; in S2, the stirring speed is 115-135 rpm; in S3, the stirring speed is 105-125 rpm; in S4, the reaction temperature is 40-45℃, the stirring speed is 90-100 rpm, and the reaction time is 25-30 min; in S5, the reaction temperature is 85-95℃, the stirring speed is 120-140 rpm, and the reaction time is 80-120 min; in S6, the stirring speed is 117-137 rpm; in S7, the reaction temperature is room temperature, the stirring speed is 30-60 rpm, and the reaction time is 10-20 min; in S8, the reaction temperature is 55-75℃, the stirring speed is 110-130 rpm, and the reaction time is 70-90 min.
4. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 1, characterized in that, The palladium refining process specifically includes the following steps: S21 Pre-leaching: Hydrochloric acid is added to the palladium concentrate obtained in S2 during gold refining, and a palladium-containing solution is obtained after the reaction. S22 Palladium-rich: A precipitating agent and an oxidizing agent are added to the palladium-containing solution, and a palladium-rich slag is obtained after the reaction; the precipitating agent is a mixed reagent of sodium chloride and potassium sulfate in a mass ratio of 1:4-6, and the amount added is 2-8 times the palladium content in the solution; the oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.5-0.7 times the palladium content in the solution. S23 Palladium Dissolution: The palladium-rich slag is dissolved in ammonia water, and after the reaction, a palladium-separated solution is obtained. S24 High Palladium: A precipitating agent and an oxidizing agent are added to the palladium-separating solution, and a high palladium ore is obtained after the reaction. The precipitating agent is a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:4-6, and the amount added is 2-8 times the palladium content in the solution. The oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.5-0.7 times the palladium content in the solution. S25 Secondary Palladium Dissolution: The high-palladium ore is dissolved in ammonia water, and a high-palladium solution is obtained after the reaction. S26 Reduction: Formic acid is added to the high palladium solution for reduction, and then the solution is washed until neutral to obtain sponge palladium.
5. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 4, characterized in that, In S21, the reaction temperature is 58-75℃, the stirring speed is 85-105 rpm, and the reaction time is 23-43 min; in S22, the reaction temperature is 59-79℃, the stirring speed is 102-132 rpm, and the reaction time is 60-90 min; in S23, the reaction temperature is 84-94℃, the stirring speed is 101-121 rpm, and the reaction time is 33-53 min; in S24, the reaction temperature is 69-89℃, the stirring speed is 105-125 rpm, and the reaction time is 30-60 min; in S25, the reaction temperature is 64-84℃, the stirring speed is 81-101 rpm, and the reaction time is 13-33 min; in S26, the reaction temperature is room temperature, the stirring speed is 55-75 rpm, and the reaction time is 22-42 min.
6. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 1, characterized in that, The platinum refining process specifically includes the following steps: S61 Pre-leaching: Hydrochloric acid is added to the platinum concentrate obtained in S6 of gold refining, and a platinum-containing solution is obtained after the reaction. S62 Platinum-Rich: A precipitating agent and an oxidizing agent are added to the platinum-containing solution, and a platinum-rich residue is obtained after the reaction. The precipitating agent is a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:4-6, and the amount added is 1-5 times the platinum content in the solution. The oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.9-1 times the platinum content in the solution. S63 Impurity Removal and Separation: Hydrazine sulfuric acid is added to the platinum-rich slag for separation, and platinum-containing slag is obtained after the reaction; S64 Platinum Dissolution: The platinum-containing slag is dissolved in hydrazine sulfuric acid, and after the reaction, a platinum-separated solution is obtained. S65 High Platinum: A precipitating agent and an oxidizing agent are added to the platinum-separating solution, and a high platinum residue is obtained after the reaction. The precipitating agent is a mixture of sodium chloride and potassium sulfate in a mass ratio of 1:4-6, and the amount added is 2-8 times the platinum content in the solution. The oxidizing agent is sodium chlorate with a concentration of 45-55%, and the amount added is 0.9-1 times the platinum content in the solution. S66 Secondary Platinum Dissolution: Add hydrazine sulfuric acid to the high-platinum slag for dissolution, and after the reaction, a high-platinum solution is obtained; S67 Reduction: Formic acid is added to the high platinum solution for reduction, followed by washing to obtain sponge platinum.
7. The comprehensive recovery and treatment method for high-purity gold, silver, platinum, and palladium according to claim 6, characterized in that, In S61, the reaction temperature is 30-50℃, the stirring speed is 77-97 rpm, and the reaction time is 56-86 min; in S62, the reaction temperature is 55-75℃, the stirring speed is 108-128 rpm, and the reaction time is 34-54 min; in S63, the reaction temperature is 58-84℃, the stirring speed is 113-133 rpm, and the reaction time is 8-18 min; in S64, the reaction temperature is 92-98℃, and the stirring speed is... In S65, the reaction temperature is 68-88℃, the stirring speed is 89-109 rpm, and the reaction time is 13-33 min; in S66, the reaction temperature is 92-98℃, the stirring speed is 112-132 rpm, and the reaction time is 26-46 min; in S67, the reaction temperature is room temperature, the stirring speed is 63-83 rpm, and the reaction time is 23-43 min.
8. A comprehensive recycling and processing system for high-purity gold, silver, platinum, and palladium, characterized in that, The integrated recycling system is used in the integrated recycling method according to any one of claims 1-7; the integrated recycling system includes a gold refining system, a palladium refining system, and a platinum refining system; The gold refining system includes: a pre-impregnation tank (1) connected to a pre-impregnation filter tank (2), the outlet of the pre-impregnation filter tank (2) connected to a palladium precipitation tank (14), and the slag outlet of the pre-impregnation filter tank (2) connected to a gold separation tank (3); the gold separation tank (3) connected to a gold separation filter tank (4), the outlet of the gold separation filter tank (4) connected to a platinum precipitation tank (6), the platinum precipitation tank (6) connected to a platinum precipitation filter press (8), and the outlet of the platinum precipitation filter press (8) connected to a gold reduction tank (10); The palladium precipitation vessel (14) is connected to the palladium precipitation filter press (16), the outlet of the palladium precipitation filter press (16) is connected to the silver precipitation vessel (17), the silver precipitation vessel (17) is connected to the silver precipitation filter press (19), the outlet of the silver precipitation filter press (19) is connected to the wastewater tank (23), the slag outlet of the silver precipitation filter press (19) is connected to the copper vessel (20), and the copper vessel (20) is connected to the copper removal filter press (22).
9. The comprehensive recovery and processing system for high-purity gold, silver, platinum, and palladium according to claim 8, characterized in that, The palladium refining system includes: a palladium melting kettle (26) connected to a palladium melting filter press (28); the outlet of the palladium melting filter press (28) connected to a palladium enrichment kettle (29); the palladium enrichment kettle (29) connected to a palladium enrichment filter press (31); the outlet of the palladium enrichment filter press (31) connected to a wastewater tank (23); the slag outlet of the palladium enrichment filter press (31) connected to a palladium separation kettle (32); and the palladium separation kettle (32) connected to a palladium separation filter press (34). The outlet of the palladium filter press (34) is connected to the high palladium reactor (35), the high palladium reactor (35) is connected to the high palladium filter press (37), the slag outlet of the high palladium filter press (37) is connected to the high palladium water reactor (62), the high palladium water reactor (62) is connected to the high palladium water filter press (64), the outlet of the high palladium water filter press (64) is connected to the palladium reduction reactor (39), and the palladium reduction reactor (39) is connected to the palladium reduction filter press (41).
10. The comprehensive recovery and processing system for high-purity gold, silver, platinum, and palladium according to claim 8, characterized in that, The platinum refining system includes: a platinum dissolving kettle (42) connected to a platinum dissolving filter press (44); the outlet of the platinum dissolving filter press (44) connected to a platinum enrichment kettle (45); the platinum enrichment kettle (45) connected to a platinum enrichment filter press (47); the outlet of the platinum enrichment filter press (47) connected to a wastewater tank (23); the slag outlet of the platinum enrichment filter press (47) connected to a purification kettle (65); the purification kettle (65) connected to a purification filter press (49); and the slag outlet of the purification filter press (49) connected to a platinum separation kettle (50). The platinum separation kettle (50) is connected to the platinum separation filter press (52). The outlet of the platinum separation filter press (52) is connected to the high platinum kettle (53). The high platinum kettle (53) is connected to the high platinum ore filter press (55). The slag outlet of the high platinum ore filter press (55) is connected to the high platinum water kettle (56). The high platinum water kettle (56) is connected to the high platinum water filter press (58). The outlet of the high platinum water filter press (58) is connected to the platinum reduction kettle (59). The platinum reduction kettle (59) is connected to the platinum reduction filter press (61).
11. The comprehensive recovery and processing system for high-purity gold, silver, platinum, and palladium according to claim 8, characterized in that, In the gold-separating vessel (3), a compressed air pipe is added and coiled along the vessel wall, and holes with a diameter of 1-2 cm are opened every 20-40 cm below the pipe; a first electronic hydrometer is provided in the middle of the gold-separating vessel (3), and a second electronic hydrometer is provided at the bottom of the gold-separating vessel (3). The two electronic hydrometers are interlocked with the compressed air regulating valve (66). The interlock is as follows: if the difference between the two electronic hydrometers is less than 0.05, the compressed air regulating valve (66) maintains this opening; if the difference between the two electronic hydrometers is greater than 0.05, the compressed air regulating valve (66) increases the opening by 3-7% every 1-3 minutes.
12. The comprehensive recovery and processing system for high-purity gold, silver, platinum, and palladium according to claim 8, characterized in that, The gold reduction vessel (10) is equipped with an electronic potentiometer. The electronic potentiometer is interlocked with the outlet valve of the first high-level tank (9). The interlock is as follows: if the potential inside the vessel is less than -0.67V, the outlet valve of the first high-level tank (9) will be closed.
13. The comprehensive recovery and processing system for high-purity gold, silver, platinum, and palladium according to claim 8, characterized in that, The palladium precipitation vessel (14) is equipped with an electronic pH meter. The electronic pH meter is interlocked with the outlet valves of the second high-level tank (24) and the third high-level tank (25). The interlocking mechanism is as follows: when pH ≤ 5, the outlet valve of the second high-level tank (24) is opened and the outlet valve of the third high-level tank (25) is closed; when pH > 5 and ≤ 3, the outlet valve of the second high-level tank (24) is closed and the outlet valve of the third high-level tank (25) is opened; when pH > 3, the outlet valves of the second high-level tank (24) and the outlet valve of the third high-level tank (25) are closed. The platinum precipitation vessel (6) is equipped with an electronic pH meter. The electronic pH meter is interlocked with the outlet valves of the second high-level tank (24) and the third high-level tank (25). The interlocking mechanism is as follows: when pH < 8, the outlet valve of the second high-level tank (24) is opened and the outlet valve of the third high-level tank (25) is closed; when pH > 8 and ≤ 5, the outlet valve of the second high-level tank (24) is closed and the outlet valve of the third high-level tank (25) is opened; when pH > 5, the outlet valves of the second high-level tank (24) and the third high-level tank (25) are closed.
14. The integrated recovery and processing system for high-purity gold, silver, platinum, and palladium according to any one of claims 9-10, characterized in that, The palladium reduction reactor (39) is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank (38). The interlocking mechanism is as follows: if the potential inside the reactor is less than -32V, the outlet valve is closed; and the single-point direct addition method is changed to a four-point feeding method parallel to the stirring. The platinum reduction vessel (59) is equipped with an electronic potentiometer, which is interlocked with the outlet valve of the fourth high-level tank (38). The interlocking mechanism is as follows: if the potential inside the vessel is less than -17V, the outlet valve is closed; and the single-point direct addition method is changed to a four-point feeding method parallel to the stirring.
Citation Information
Patent Citations
Method and system for recovering gold, silver, palladium and platinum from silver anode slime
CN121137357A