Process for extracting high-purity copper from iron
Through a process of extracting high-purity copper from iron, including dissolution, iron powder replacement, filtration and separation, medium-frequency smelting and vacuum distillation, the problem of difficult to achieve ultra-high purity in traditional copper purification processes is solved, the stability and repeatability of high-purity copper are achieved, and the difficulty and cost of purchasing raw materials is reduced.
Patent Information
- Application Number
- CN202510203572.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-24
- Publication Date
- 2025-06-20
Smart Images
Figure CN120174208A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of metal material purification, and particularly relates to a process for extracting high-purity copper from iron. Background Art
[0002] In modern industry, ultra-high-purity copper has a wide range of application requirements in the fields of electronics, electrical, aerospace, etc., and extremely high purity requirements for copper.
[0003] However, traditional copper purification processes are difficult to achieve an ultra-high purity of 99.994824% in terms of purity improvement, and cannot meet the requirements of some high-end application scenarios; moreover, the stability and repeatability of traditional process are poor, resulting in unstable quality of copper products obtained from each operation, affecting the consistency and reliability of products; in addition, in terms of raw material selection, traditional processes usually have strict requirements for specific specifications and types of raw materials, which not only limits the sources of raw materials, increases the difficulty of raw material procurement, but also leads to high procurement costs. Summary of the Invention
[0004] The purpose of the present invention is to provide a process for extracting high-purity copper from iron to solve the technical problems existing in the prior art.
[0005] In order to achieve the above-mentioned invention purpose, the technical solution adopted by the present invention is as follows:
[0006] A process for extracting high-purity copper from iron, comprising the following steps: S1: Raw material preparation, preparing reduced iron powder with uniform purity and particle size; appropriate amounts of concentrated sulfuric acid, copper oxide powder, catalyst, hydrogen peroxide, and native copper powder; S2: Dissolution, adding concentrated sulfuric acid into a reaction vessel, heating it to 10 - 35 °C; adding copper oxide powder according to a preset ratio, using a stirring member to stir the concentrated sulfuric acid and copper oxide powder for 30 - 50 min to complete dissolution and form a solution; S3: Iron powder replacement, heating the solution to 60 - 80 °C, adding reduced iron powder according to a preset ratio to the above solution, and simultaneously adding a catalyst, native copper powder, and hydrogen peroxide in sequence during this process, and stirring, then forming a mixed solution, and allowing the mixed solution to stand at room temperature for 1 - 3 h; S4: Filtration separation, filtering the standing mixed solution through a filtering device, performing solid-liquid separation to obtain copper powder; S5: Medium-frequency melting, putting the copper powder obtained after filtration separation into a medium-frequency melting furnace, with a temperature of 1000 - 1500 °C and a melting time of 1 - 2 h to obtain a high-purity copper ingot; S6: Vacuum distillation, putting the copper ingot obtained after medium-frequency melting into a vacuum distillation furnace, with a temperature of 1600 - 1800 °C and a vacuum degree of 10 ^-3 -10 ^-5 Pa, and a distillation time of 2 - 4 h to obtain an ultra-high-purity copper ingot.
[0007] Further, the catalyst is one or more of oxalic acid, copper sulfate, thiourea, sodium sulfite, sodium thiosulfate, ammonia water or acetic acid.
[0008] Further, the reduced iron powder in S1 is 200-400 mesh iron powder.
[0009] Further, S3: iron powder replacement, specifically including the following steps: S3.1: Heat the solution in S2 to 70 °C, add 400 mesh reduced iron powder in a ratio of 1:10, and continuously stir during the addition of 400 mesh reduced iron powder to obtain a reaction solution; S3.2: Add oxalic acid to the above reaction solution, and the ratio of oxalic acid to the reaction solution is 0.2% - 0.8%; S3.3: After adding oxalic acid, add natural copper powder as crystal nuclei in a weight ratio of 1% - 3% to the reaction solution, and continuously stir at the same time; S3.4: Add hydrogen peroxide with a concentration of 30% - 40% in a weight ratio of 0.5% - 1% to the reaction solution to form a mixed solution; S3.5: Use a stirrer to stir the above mixed solution at a speed of 200 - 400 rpm, and the stirring duration is 1 - 3 h; S3.6: Let the stirred mixed solution stand at room temperature for 1.5 - 2 h.
[0010] Further, S5: intermediate frequency melting, specifically including the following steps: S5.1: Put the copper powder obtained after filtration and separation into the furnace chamber of the intermediate frequency melting furnace, start the equipment, and make the induction coil generate an intermediate frequency electromagnetic field; S5.2: The intermediate frequency electromagnetic field generates an induced current in the copper powder, control the temperature in the furnace chamber at 1200 - 1400 °C for 1.5 h; due to the resistance of the copper material itself, heat will be generated when the current passes through, and the copper material will gradually heat up and melt; S5.3: Add a refining agent to the molten copper that is heating up and melting; S5.4: Pour the completely melted molten copper into a mold, and perform cooling and demolding to obtain a high-purity copper ingot.
[0011] Further, the purity of the high-purity copper ingot in S5 is 96% - 99%; the purity of the ultra-high-purity copper ingot in S6 is 99.994824%.
[0012] Compared with the prior art, the present invention has the following beneficial effects:
[0013] Through the steps of raw material preparation, dissolution, iron powder replacement, filtration and separation, intermediate frequency melting, and vacuum distillation, the present invention makes the entire process highly stable and repeatable, ensuring that copper products with stable quality can be obtained each time; the present invention can obtain ultra-high-purity copper ingots with a purity of up to 99.994824%, and compared with traditional copper purification processes, it can use reduced iron powder of different specifications and a variety of common chemical reagents as raw materials, reducing the difficulty and cost of raw material procurement, resulting in a relatively low overall cost investment and bringing significant economic benefits to enterprises. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 is a flowchart of the present invention; DETAILED DESCRIPTION OF THE INVENTION
[0015] In order to make the content of the present invention more clearly understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. The same reference numerals are used for the same components. It should be noted that the terms "front", "rear", "left", "right", "upper" and "lower" used in the following description refer to the directions in the drawings, and the terms "inner" and "outer" refer to the directions towards or away from the geometric center of a specific component, respectively.
[0016] As Figure 1 shown, in this embodiment, a process for extracting high-purity copper from iron is provided, including the following steps:
[0017] S1: Raw material preparation, preparing reduced iron powder with uniform purity and particle size; appropriate amounts of concentrated sulfuric acid, copper oxide powder, catalyst, hydrogen peroxide, and native copper powder;
[0018] S2: Dissolution, adding concentrated sulfuric acid into a reaction vessel and heating it to 10 - 35 °C; adding copper oxide powder according to a preset ratio, and using a stirring member to stir the concentrated sulfuric acid and copper oxide powder for 30 - 50 min to complete the dissolution to form a solution;
[0019] S3: Iron powder replacement, heating the solution to 60 - 80 °C, adding reduced iron powder in a preset ratio to the above solution, and simultaneously adding the catalyst, native copper powder, and hydrogen peroxide in sequence during this process, and stirring, then forming a mixed solution, and allowing the mixed solution to stand at room temperature for 1 - 3 h;
[0020] S4: Filtration and separation, filtering the mixed solution after standing through a filtration device, and performing solid-liquid separation to obtain copper powder;
[0021] S5: Medium-frequency melting, putting the copper powder obtained after filtration and separation into a medium-frequency melting furnace, with a temperature of 1000 - 1500 °C and a melting time of 1 - 2 h to obtain a high-purity copper ingot;
[0022] S6: Vacuum distillation, putting the copper ingot obtained after medium-frequency melting into a vacuum distillation furnace, with a temperature of 1600 - 1800 °C and a vacuum degree of 10 ^-3 -10 ^-5 Pa and a distillation time of 2 - 4 h to obtain an ultra-high-purity copper ingot.
[0023] The catalyst is one or more of oxalic acid, copper sulfate, thiourea, sodium sulfite, sodium thiosulfate, ammonia water, or acetic acid.
[0024] Example 1:
[0025] In this example, a process for extracting high-purity copper from iron is provided, including the following steps:
[0026] S1: Raw material preparation. Prepare 200-mesh reduced iron powder with uniform purity and particle size; appropriate amounts of concentrated sulfuric acid, copper oxide powder, oxalic acid, hydrogen peroxide, and native copper powder. When preparing, it is necessary to ensure the purity and quality of oxalic acid, hydrogen peroxide, and native copper powder, and prepare a dry reaction container separately;
[0027] S2: Dissolution. Add 500 concentrated sulfuric acid to the reaction container and heat it to 10°C; add 200 g of copper oxide powder, and use a stirrer to stir the concentrated sulfuric acid and copper oxide powder for 30 min to complete the dissolution to form a solution;
[0028] S3: Iron powder replacement. Heat the solution to 60°C, add 200 kg of reduced iron powder to the above solution. During this process, add 50 g of oxalic acid, 100 g of native copper powder, and 50 ml of hydrogen peroxide in sequence, and stir. Then a mixed solution is formed, and the mixed solution is left to stand at room temperature for 1 h;
[0029] Specifically, it includes the following steps:
[0030] S3.1: Heat the solution in S2 to 70°C, add 200-mesh reduced iron powder in a ratio of 1:10, and continuously stir during the addition of 200-mesh reduced iron powder to obtain a reaction solution;
[0031] S3.2: Add oxalic acid to the above reaction solution, and the ratio of oxalic acid to the reaction solution is 0.2% - 0.8%;
[0032] S3.3: After adding oxalic acid, add native copper powder as crystal nuclei in a weight ratio of 1% - 3% to the reaction solution, and continuously stir at the same time;
[0033] S3.4: Add hydrogen peroxide with a concentration of 30% in a weight ratio of 0.5% - 1% to the reaction solution to form a mixed solution;
[0034] S3.5: Use a stirrer to stir the above mixed solution at a speed of 200 rpm, and the stirring duration is 1 h;
[0035] S3.6: Leave the stirred mixed solution to stand at room temperature for 1.5 h
[0036] S4: Filtration and separation. Filter the mixed solution after standing through a filtration device, and after solid-liquid separation, copper powder is obtained;
[0037] S5: Medium-frequency melting. Put the copper powder obtained after filtration and separation into a medium-frequency melting furnace at a temperature of 1000 °C for 1 hour to obtain high-purity copper ingots. The purity of the high-purity copper ingots is 96% - 99%.
[0038] Specifically, it includes the following steps:
[0039] S5.1: Put the copper powder obtained after filtration and separation into the furnace chamber of the medium-frequency melting furnace, start the equipment, and make the induction coil generate a medium-frequency electromagnetic field.
[0040] S5.2: The medium-frequency electromagnetic field generates an induced current in the copper powder, control the temperature in the furnace chamber at 1200 °C for 1.5 hours. Due to the resistance of the copper material itself, heat will be generated when the current passes through, causing the copper material to gradually heat up and melt.
[0041] S5.3: Add a refining agent to the molten copper that has been heated and melted.
[0042] S5.4: Pour the completely melted molten copper into a mold, cool it and demold it to obtain high-purity copper ingots.
[0043] S6: Vacuum distillation. Put the copper ingots obtained after medium-frequency melting into a vacuum distillation furnace at a temperature of 1600 °C, a vacuum degree of 10 ^-3 Pa, and the distillation time is 2 hours to obtain ultra-high-purity copper ingots. The purity of the ultra-high-purity copper ingots is 99.994824%.
[0044] Example 2:
[0045] In this example, a process for extracting high-purity copper from iron is provided, including the following steps:
[0046] S1: Raw material preparation. Prepare 300-mesh reduced iron powder with uniform purity and particle size; appropriate amounts of concentrated sulfuric acid, copper oxide powder, copper sulfate, hydrogen peroxide, and native copper powder. When preparing, it is necessary to ensure the purity and quality of oxalic acid, hydrogen peroxide, and native copper powder, and prepare a dry reaction container separately.
[0047] S2: Dissolution. Add 700 ml of concentrated sulfuric acid to the reaction container and heat it to 20 °C; add 300 g of copper oxide powder, and use a stirring device to stir the concentrated sulfuric acid and copper oxide powder for 40 minutes to complete the dissolution to form a solution.
[0048] S3: Iron powder replacement. Heat the solution to 70 °C, add 300 kg of reduced iron powder to the above solution. During this process, add 75 g of copper sulfate, 125 g of native copper powder, and 75 ml of hydrogen peroxide in sequence and stir, and then form a mixed solution. Let the mixed solution stand at room temperature for 2 hours.
[0049] Specifically, it includes the following steps:
[0050] S3.1: Heat the solution in S2 to 70°C, add reduced iron powder with a mesh size of 300 at a ratio of 1:10, and continuously stir during the addition of the reduced iron powder with a mesh size of 300 to obtain a reaction solution;
[0051] S3.2: Add copper sulfate to the above reaction solution, and the ratio of copper sulfate to the reaction solution is 0.2% - 0.8%;
[0052] S3.3: After adding copper sulfate, add natural copper powder as crystal nuclei at a weight ratio of 1% - 3% to the reaction solution, and continuously stir at the same time;
[0053] S3.4: Add hydrogen peroxide with a concentration of 35% at a weight ratio of 0.5% - 1% to the reaction solution to form a mixed solution;
[0054] S3.5: Use a stirrer to stir the above mixed solution at a speed of 300 rpm, and the stirring duration is 2 h;
[0055] S3.6: Let the stirred mixed solution stand at room temperature for 1.75 h
[0056] S4: Filter and separate. Filter the standing mixed solution through a filtering device. After solid-liquid separation, copper powder is obtained;
[0057] S5: Medium-frequency melting. Put the copper powder obtained after filter separation into a medium-frequency melting furnace, the temperature is 1250°C, and the melting time is 1.5 h to obtain a high-purity copper ingot; the purity of the high-purity copper ingot is 96% - 99%;
[0058] Specifically, it includes the following steps:
[0059] S5.1: Put the copper powder obtained after filter separation into the furnace chamber of the medium-frequency melting furnace, start the equipment, and make the induction coil generate a medium-frequency electromagnetic field;
[0060] S5.2: The medium-frequency electromagnetic field generates an induced current in the copper powder, control the temperature in the furnace chamber at 1300°C for 1.5 h; due to the resistance of the copper material itself, heat will be generated when the current passes through, causing the copper material to gradually heat up and melt;
[0061] S5.3: Add a refining agent to the liquid copper that is heating up and melting;
[0062] S5.4: Pour the completely melted liquid copper into a mold, and perform cooling and demolding to obtain a high-purity copper ingot;
[0063] S6: Vacuum distillation. Put the copper ingot obtained after medium-frequency melting into a vacuum distillation furnace, the temperature is 1700°C, and the vacuum degree is 10 ^-4Pa, with a distillation time of 3 h, an ultra-high purity copper ingot is obtained; the purity of the ultra-high purity copper ingot is 99.994824%.
[0064] Example 3:
[0065] In this example, a process for extracting high-purity copper from iron is provided, including the following steps:
[0066] S1: Raw material preparation, preparing 400-mesh reduced iron powder with uniform purity and particle size; appropriate amounts of concentrated sulfuric acid, copper oxide powder, thiourea, hydrogen peroxide, and native copper powder; when preparing, it is necessary to ensure the purity and quality of oxalic acid, hydrogen peroxide, and native copper powder, and prepare a dry reaction container separately;
[0067] S2: Dissolution, adding 1000 ml of concentrated sulfuric acid to the reaction container, heating it to 35 °C; adding 500 g of copper oxide powder, using a stirrer to stir the concentrated sulfuric acid and copper oxide powder for 50 min to complete dissolution and form a solution;
[0068] S3: Iron powder replacement, heating the solution to 80 °C, adding 500 kg of reduced iron powder to the above solution, and simultaneously adding 100 g of thiourea, 150 g of native copper powder, and 100 ml of hydrogen peroxide in sequence during this process, and stirring, then forming a mixed solution, and allowing the mixed solution to stand at room temperature for 3 h;
[0069] Specifically, it includes the following steps:
[0070] S3.1: Heating the solution in S2 to 70 °C, adding 400-mesh reduced iron powder at a ratio of 1:10, and continuously stirring during the addition of 400-mesh reduced iron powder to obtain a reaction solution;
[0071] S3.2: Adding thiourea to the above reaction solution, and the ratio of thiourea to the reaction solution is 0.2% - 0.8%;
[0072] S3.3: After adding thiourea, adding native copper powder as a crystal nucleus at a weight ratio of 1% - 3% to the reaction solution, and continuously stirring simultaneously;
[0073] S3.4: Adding hydrogen peroxide with a concentration of 40% at a weight ratio of 0.5% - 1% to the reaction solution to form a mixed solution;
[0074] S3.5: Using a stirrer to stir the above mixed solution at a speed of 400 rpm, and the stirring duration is 3 h;
[0075] S3.6: Allowing the stirred mixed solution to stand at room temperature for 2 h;
[0076] S4: Filtration and separation, filtering the standing mixed solution through a filtration device, and after solid-liquid separation, copper powder is obtained;
[0077] S5: Medium-frequency smelting. Put the copper powder obtained after filtration and separation into a medium-frequency smelting furnace at a temperature of 1500 °C for a smelting time of 2 h to obtain high-purity copper ingots. The purity of the high-purity copper ingots is 96% - 99%.
[0078] The said S5: Medium-frequency smelting specifically includes the following steps:
[0079] S5.1: Put the copper powder obtained after filtration and separation into the furnace chamber of the medium-frequency smelting furnace, start the equipment, and make the induction coil generate a medium-frequency electromagnetic field.
[0080] S5.2: The medium-frequency electromagnetic field generates an induced current in the copper powder, control the temperature in the furnace chamber at 1400 °C for 1.5 h. Due to the resistance of the copper material itself, heat will be generated when the current passes through, causing the copper material to gradually heat up and melt.
[0081] S5.3: Add a refining agent to the molten copper that has been heated and melted.
[0082] S5.4: Pour the completely melted molten copper into a mold, cool it and demold it to obtain high-purity copper ingots.
[0083] S6: Vacuum distillation. Put the copper ingots obtained after medium-frequency smelting into a vacuum distillation furnace at a temperature of 1800 °C, a vacuum degree of 10 ^-5 Pa, and a distillation time of 4 h to obtain ultra-high-purity copper ingots. The purity of the ultra-high-purity copper ingots is 99.994824%.
[0084] Table 1 is the test report of the ultra-high-purity copper ingots manufactured by this process:
[0085] Serial number Test item Test result Unit Test method / Instrument 1 Copper Cu 99.994824 ％ ICP-OES
[0086] Table (1)
[0087] The above are only the preferred embodiments of this invention patent and are not used to limit this invention patent. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of this invention patent shall be included within the protection scope of this invention patent.
Claims
1. A process for extracting high-purity copper from iron, characterized in that: The following steps are involved: S1: Raw material preparation, including reduced iron powder with uniform purity and particle size; appropriate amount of concentrated sulfuric acid, copper oxide powder, catalyst, hydrogen peroxide and natural copper powder; S2: Dissolving, adding concentrated sulfuric acid into a reaction vessel and heating it to 10-35°C; adding copper oxide powder according to a preset ratio, and stirring the concentrated sulfuric acid and copper oxide powder for 30-50 minutes using a stirring element to complete the dissolution to form a solution; S3: iron powder replacement, heating the solution to 60-80°C, adding a preset proportion of reduced iron powder to the solution, and simultaneously adding a catalyst, natural copper powder and hydrogen peroxide in sequence during the process, and stirring to form a mixed solution, and then leaving the mixed solution at room temperature for 1-3 hours; S4: filtering and separating, filtering the mixed solution after standing through a filtering device, and obtaining copper powder after solid-liquid separation; S5: Medium frequency smelting, the copper powder obtained after filtration and separation is placed in a medium frequency smelting furnace at a temperature of 1000-1500°C for 1-2 hours to obtain a high-purity copper ingot; S6: Vacuum distillation: put the copper ingot obtained after medium frequency smelting into a vacuum distillation furnace at a temperature of 1600-1800℃ and a vacuum degree of 10 ^-3 -10 ^-5 Pa, the distillation time is 2-4h, and ultra-high purity copper ingots are obtained.
2. The process for extracting high-purity copper from iron according to claim 1, characterized in that: The catalyst is one or more of oxalic acid, copper sulfate, thiourea, sodium sulfite, sodium thiosulfate, ammonia water or acetic acid.
3. The process for extracting high-purity copper from iron according to claim 1, characterized in that: The reduced iron powder in S1 is 200-400 mesh iron powder.
4. The process for extracting high-purity copper from iron according to claim 1, characterized in that: S3: iron powder replacement, specifically includes the following steps: S3.1: The solution in S2 is heated to 70° C., and 400-mesh reduced iron powder is added at a ratio of 1:10, and the mixture is continuously stirred during the addition of the 400-mesh reduced iron powder to obtain a reaction solution; S3.2: Add oxalic acid to the above reaction solution, the ratio of oxalic acid to reaction solution being 0.2% to 0.8%; S3.3: After adding oxalic acid, natural copper powder as a crystal nucleus is added at a weight ratio of 1% to 3% of the reaction solution, while stirring continuously; S3.4: adding 30% to 40% hydrogen peroxide in a weight ratio of 0.5% to 1% to the reaction solution to form a mixed solution; S3.5: Using a stirring rod, stir the mixed solution at a speed of 200-400 rpm for 1-3 hours; S3.6: Let the stirred mixture stand at room temperature for 1.5-2 hours.
5. The process for extracting high-purity copper from iron according to claim 1, characterized in that: The S5: medium frequency smelting specifically comprises the following steps: S5.1: Place the copper powder obtained after filtration and separation into the furnace of the medium frequency smelting furnace, start the equipment, and make the induction coil generate a medium frequency electromagnetic field; S5.2: The medium frequency electromagnetic field generates an induced current in the copper powder, and the temperature in the furnace is controlled at 1200-1400℃ for 1.5 hours. Due to the resistance of the copper material itself, heat is generated when the current passes through, causing the copper material to gradually heat up and melt. S5.3: adding a refining agent to the heated and molten liquid copper; S5.4: The completely melted liquid copper is poured into a mold, cooled and demolded to obtain a high-purity copper ingot.
6. The process for extracting high-purity copper from iron according to claim 5, characterized in that: The purity of the high-purity copper ingot in S5 is 96% to 99%; the purity of the ultra-high-purity copper ingot in S6 is 99.994824%.