CN114525413A - Method for separating copper and noble metal from copper alloy containing noble metal - Google Patents
Method for separating copper and noble metal from copper alloy containing noble metal Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0028—Smelting or converting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for separating copper and noble metal from a copper alloy containing noble metal, which comprises the following steps: the method comprises the following steps of pyrometallurgical smelting, atomization powder preparation, selective leaching, purification and electrodeposition; smelting a copper alloy containing noble metals by using a smelting furnace, preparing alloy powder by using an atomization powder-making device in a molten state, adding the alloy powder into a reaction kettle filled with a leaching agent, blowing air for selective leaching, performing solid-liquid separation, performing noble metal separation and purification on leached residues to recover the noble metals, adding copper powder into the solution for desilvering, and performing electrodeposition on the solution after desilvering by using an electrodeposition tank to obtain cathode copper. After the treatment by the method, the copper and the noble metal are separated and the copper is recovered, the noble metal is not lost, and the method provides convenience for the recovery of the noble metal.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy of copper and precious metals, in particular to a method for separating copper and precious metals from a copper alloy containing the precious metals.
Background
A method for separating copper and noble metals from a copper alloy containing noble metals is a current mainstream process which adopts an electrolytic refining method to separate, specifically, the copper alloy containing noble metals is cast into a copper plate and then used as an anode, a copper sheet or a stainless steel plate is used as a cathode, a copper sulfate solution is used as an electrolyte, copper is deposited on the cathode through electrolytic refining to obtain cathode copper with the purity of more than 99.9 percent, the noble metals and the like become anode mud in the electrolytic process, and finally the noble metals are recovered from the anode mud.
However, this separation method is suitable for separating copper and noble metals from a noble metal-containing copper alloy having a copper content of 99% or more and a noble metal (silver and other noble metals) content of less than 0.5%, and when the silver content is too high, an anodic passivation phenomenon easily occurs during electrolysis, making electrolysis difficult. Meanwhile, the separation method is easy to generate anodic polarization in the electrolytic process, generate overvoltage, and dissolve a small amount of noble metal in the anode, so that the total amount of the separated noble metal is lost, and the yield of the separated noble metal is reduced. In addition, the electrolysis period of the separation method is long, generally 15 days, and the anode scrap needs to be re-melted, fused and cast and then electrolyzed, so that the precious metal recovery period is longer, and the capital turnover of enterprises is not facilitated.
Disclosure of Invention
In order to solve the problems of the prior method for separating copper and noble metals from the copper alloy containing noble metals by adopting an electrolytic refining method, the invention provides a novel method for separating copper and noble metals from the copper alloy containing noble metals. The specific technical scheme is as follows:
a method of separating copper and precious metals from a precious metal-containing copper alloy, comprising the steps of:
(1) fire smelting: smelting the alloy material containing the noble metal copper in a smelting furnace at 1200 ℃ to melt the alloy material into a molten state;
(2) atomizing to prepare powder: atomizing and solidifying the noble metal-containing copper alloy material in the molten state in the step (1) by an atomizing powder-making device (a metal atomizer) to obtain noble metal-containing copper powder;
(3) selective leaching: adding the copper powder containing the noble metals in the step (2) into a special reaction kettle (a reaction kettle with a vent pipe at the bottom), adding a leaching agent, starting stirring, simultaneously introducing air (an oxidant) into the reaction kettle through the vent pipe, controlling the oxidation-reduction potential of the reaction kettle to be 300-400mv, reacting for 20-22 hours, filtering to obtain leaching slag and leaching liquid, wherein the leaching slag is used for extracting and recovering the noble metals; when the oxidation-reduction potential of the reaction in the step is controlled at 300-400mv, the copper in the copper powder containing the noble metal can be completely dissolved, the silver is dissolved in a small amount, and the noble metal such as gold, platinum, palladium, rhodium and the like is not dissolved.
(4) Purifying: adding the leachate obtained in the step (3) into another reaction kettle, starting stirring, adding copper powder (an impurity removing agent), reducing silver ions into simple substance silver by the copper powder, filtering to obtain relatively pure copper sulfate solution and silver powder, and recovering the silver powder;
(5) electrodeposition: and (4) conveying the copper sulfate solution obtained in the step (4) to an electrodeposition tank, introducing direct current, obtaining a copper plate at the cathode under the action of the direct current, generating oxygen at the anode and generating electrodeposition waste liquid at the same time.
The specific principle of the method is as follows:
(1) the selective leaching principle is as follows: the alloy material containing noble metal copper is smelted by a pyrogenic process and atomized to form alloy powder in a molten state, and the main technological process of wet selective leaching of copper is to leach copper by using air as an oxidant and sulfuric acid.
The main chemical processes for selective leaching of copper:
2Cu+2H2SO4+O2＝2CuSO4+2H2O
(2) principle of reduction
And (4) adding the copper sulfate leaching solution obtained in the step (3) into another reaction kettle, starting stirring, adding copper powder, reducing silver ions into simple substance silver by the copper powder, and filtering to obtain relatively pure copper sulfate solution and silver powder. The mechanism of reduction is: cu +2Ag+→Cu2++2Ag。
(3) Principle of electrodeposition
After purification in step (4), Cu can be obtained2+The concentration is 35-45g/L, H2SO4At a content of about 150-160g/LCopper sulfate solution, delivering the copper sulfate solution to an electrodeposition tank, introducing direct current, obtaining a copper plate at the cathode under the action of the direct current, generating oxygen at the anode and generating electrodeposition waste liquid, wherein Cu is contained in the copper plate2+The concentration is 30-35g/l, H2SO4The content is 160-180g/L, and the electrodeposition waste liquid is returned to the step (3) for recycling.
The cathode reaction produces copper, namely:
Cu2++2e＝Cu φΘCu2+/Cu＝0.34V
the anode reaction generates oxygen, and the reaction formula is as follows:
H2O-2e＝1/2O2+2H+ φΘO2/H2O＝1.23V
the overall reaction formula for copper electrodeposition is:
Cu2++H2O＝Cu+1/2O2+2H+
the standard electromotive force for the electrodeposition reaction is:
EΘ＝φΘCu2+/Cu-φΘO2/H2O＝-0.89V
further, the precious metal-containing copper alloy material in the step (1) is a copper material containing precious metals such as gold, silver, platinum, palladium, rhodium and the like.
Further, the smelting furnace in the step (1) is a medium-frequency smelting furnace.
Further, the electrodeposition waste liquid generated in the step (5) can be returned to the step (3) for recycling, so that materials are utilized to the maximum extent, the waste liquid output of the method is reduced, and the pollution to the environment is reduced.
Further, the leaching agent used in the step (3) is sulfuric acid and/or the electrodeposition waste liquid generated in the step (5), before the reaction, the concentration (mass percent) of the sulfuric acid in the solution is 10%, the solid-to-liquid ratio of the reaction is 1:20-24, the reaction temperature is normal temperature, and a good selective leaching effect can be ensured under the solid-to-liquid ratio and the concentration of the sulfuric acid. Furthermore, when the concentration of the sulfuric acid in the solution is higher than and close to 10%, in order to ensure that the solid-to-liquid ratio is 1:20-24, the solid-to-liquid ratio and the sulfuric acid concentration of the whole reaction system can be ensured by adding water for adjustment.
Further, the reaction temperature in the step (4) is normal temperature.
Further, the current density in the step (5) is 180-250A/m2, the copper content of the liquid before electrodeposition is 35-45g/L, and the copper content of the liquid after electrodeposition is 30-35 g/L. Has better electrodeposition effect under the conditions.
Compared with the prior art, the invention has the beneficial effects that: on one hand, the method mainly separates the copper and the noble metal in the copper alloy containing the noble metal through selective leaching, and the method has low loss and even no loss on the noble metal under the condition of ensuring that the copper is completely separated from the copper alloy containing the noble metal, thereby improving the yield of the noble metal obtained by separation. On the other hand, the separation method has no strict requirements on the copper content and the silver content in the materials. In addition, the separation period of the method is obviously shortened, and the leaching reaction time is within 24 hours. Generally, after the treatment by the method, copper and noble metal are separated and the copper is recovered, the noble metal is not lost, and convenience is provided for the recovery of the noble metal.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will now be described in more detail with reference to the following examples, but it should be understood that the invention is not limited to the details of the examples set forth herein. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Reagents and starting materials not specifically described in the following examples of the present invention are commercially available. In addition, the copper and precious metal components of the invention are measured according to the following standards: copper GB/T5121.1-2008; gold GB/T4134-2015; silver GB/T4135-2016; platinum GB/T1419-2015; palladium GB/T15072.4-2008; rhodium GB/T8184-2004.
Example 1
98.32kg of precious metal-containing copper alloy raw material is melted into molten alloy at 1200 ℃ by an intermediate frequency furnace fire method, and then is atomized and solidified by an atomizing device to obtain 90.40kg of metal powder, wherein the atomized metal powder is sampled and tested to obtain copper and precious metal components with the following contents: 85.71% of Cu, 0.13% of Au, 0.087% of Pd, 4.7% of Ag, 0.041% of Rh and 0.004% of Pt.
Adding the obtained atomized metal powder into a reaction kettle with a vent pipe, adding 10% dilute sulfuric acid, starting stirring, controlling the reaction temperature to be room temperature, simultaneously introducing air into the reaction kettle, controlling the oxidation-reduction potential of the reaction kettle to be 400mv, controlling the solid-liquid ratio to be 1:20, and reacting for 22 h. The leaching solution is sampled to test the content data of copper and precious metals in the leaching solution to obtain the Cu concentration of 42.3g/l, the Ag concentration of 0.717g/l and the Cu leaching rate of 98.7 percent, copper in metal powder is basically completely dissolved after selective leaching, silver is partially dissolved (30.51 percent), precious metals of gold, palladium and rhodium are not dissolved, filter residue contains precious metal concentrate and filtrate copper sulfate solution, and the precious metal concentrate is extracted and recovered after precious metal separation and refining. Adding the filtrate copper sulfate solution into another reaction kettle, starting stirring, adding copper powder for purification and silver removal, reducing silver ions into simple substance silver by the copper powder, filtering to obtain relatively pure copper sulfate solution and silver powder, recovering the silver by the silver powder, and performing electrodeposition on the copper sulfate solution. The purified copper sulfate solution is sent to an electrowinning cell, direct current is introduced, under the action of the direct current, a copper plate is obtained at a cathode, the copper content at the cathode is 99.52%, oxygen is generated at an anode, an electrowinning waste liquid is generated at the same time, the electrowinning waste liquid returns to the leaching step for recycling, the recovery rate of the precious metals is more than 99% (wherein the recovery rate of silver in the leaching residue is 69.49%, the other part generates 1283.93g of silver powder in the purification step, and the total yield of silver is 99.71%), and the statistical data are shown in Table 1 below.
Table 1 experimental results of example 1
Example 2
62.4kg of precious metal-containing copper alloy raw material is melted into molten alloy at 1200 ℃ by an intermediate frequency furnace fire method, and then atomized and solidified by an atomizing device to obtain 59.84kg of metal powder, wherein the atomized metal powder is sampled and tested to obtain the following copper and precious metal components: cu 87.43%, Au 0.335%, Pd 0.18%, Ag 5.43%, Rh 0.041%, Pt 0.007%.
Adding the obtained atomized metal powder into a reaction kettle with a vent pipe, adding 10% dilute sulfuric acid, starting stirring, controlling the reaction temperature to be room temperature, simultaneously introducing air into the reaction kettle, controlling the oxidation-reduction potential of the reaction kettle to be 400mv, controlling the solid-liquid ratio to be 1:20, and reacting for 20 hours. The leaching solution is sampled to test the content data of copper and precious metals in the leaching solution to obtain the Cu concentration of 43.3g/l, the Ag concentration of 0.88g/l and the Cu leaching rate of 99.05 percent, copper in metal powder is basically completely dissolved after selective leaching, silver is partially dissolved (36.83 percent), precious metals of gold, palladium and rhodium are not dissolved, filter residue contains precious metal concentrate and filtrate copper sulfate solution, and the precious metal concentrate is extracted and recovered after precious metal separation and refining. Adding the filtrate copper sulfate solution into another reaction kettle, starting stirring, adding copper powder for purification and silver removal, reducing silver ions into simple substance silver by the copper powder, filtering to obtain relatively pure copper sulfate solution and silver powder, recovering the silver by the silver powder, and performing electrodeposition on the copper sulfate solution. The purified copper sulfate solution is sent to an electrowinning cell, direct current is introduced, under the action of the direct current, a copper plate is obtained at a cathode, the copper content at the cathode is 99.58%, oxygen is generated at an anode, an electrowinning waste liquid is generated at the same time, the electrowinning waste liquid returns to a leaching step, the electrowinning waste liquid is recycled, the electrowinning waste liquid returns to the leaching step, the recovery rate of precious metals is more than 99% (wherein the recovery rate of silver in leaching residues is 63.17%, the other part generates 1185.12g of silver powder in the purification step, the total yield of silver is 99.64%), and statistical data are shown in Table 2 below.
Table 2 experimental results of example 2
Example 3
104.25kg of precious metal-containing copper alloy raw material is melted into molten alloy at 1200 ℃ by an intermediate frequency furnace fire method, and then is atomized and solidified by an atomizing device to obtain 84.24kg of metal powder, wherein the atomized metal powder is sampled and tested to obtain copper and precious metal components with the following contents: 92.08 percent of Cu, 0.086 percent of Au, 0.01 percent of Pd, 7.072 percent of Ag, 0.025 percent of Rh and 0.004 percent of Pt.
Adding the obtained atomized metal powder into a reaction kettle with a vent pipe, adding 10% dilute sulfuric acid, starting stirring, controlling the reaction temperature to be room temperature, simultaneously introducing air into the reaction kettle, controlling the oxidation-reduction potential of the reaction kettle to be 400mv, controlling the solid-liquid ratio to be 1:24, and reacting for 21 h. The leaching solution is sampled and tested, the copper and precious metal content data of the leaching solution are obtained, the Cu concentration is 37.99g/l, the Ag concentration is 0.62g/l, the Cu leaching rate is 99.02%, after selective leaching, copper in metal powder is basically completely dissolved, silver is partially dissolved (21.04%), precious metals gold, palladium and rhodium are not dissolved, filter residues containing precious metal concentrates and filtrate copper sulfate solution are obtained through filtering, and the precious metal concentrates are subjected to precious metal separation and refining extraction and recovery. Adding the filtrate copper sulfate solution into another reaction kettle, starting stirring, adding copper powder for purification and silver removal, reducing silver ions into simple substance silver by the copper powder, filtering to obtain relatively pure copper sulfate solution and silver powder, recovering the silver by the silver powder, and performing electrodeposition on the copper sulfate solution. The purified copper sulfate solution is sent to an electrowinning cell, direct current is introduced, under the action of the direct current, a copper plate is obtained at a cathode, the copper content at the cathode is 99.52%, oxygen is generated at an anode, an electrowinning waste liquid is generated at the same time, the electrowinning waste liquid returns to a leaching step, the electrowinning waste liquid is recycled, the electrowinning waste liquid returns to the leaching step, the recovery rate of precious metals is more than 99% (wherein the recovery rate of silver in leaching residues is 78.96%, the other part generates 1235.28g of silver powder in the purification step, the total yield of silver is 99.70%), and statistical data are shown in Table 3 below.
Table 3 experimental results of example 3
Comparative example
The same batch of copper material containing noble metal as in example 3 was treated by the current mainstream process (electrolytic refining), wherein the copper and noble metal contents are as follows: 92.08 percent of Cu, 0.086 percent of Au, 0.01 percent of Pd, 7.072 percent of Ag, 0.025 percent of Rh and 0.004 percent of Pt. In the experiment, 6kg of copper material containing noble metal is taken and cast into a copper plate as an anode, the copper plate is taken as a cathode, a copper sulfate solution is taken as an electrolyte, and the separation is carried out by an electrolytic refining method, wherein the specific experimental data are shown in Table 4.
Table 4 experimental results of comparative examples
By adopting the current mainstream process treatment, copper is deposited on the cathode to obtain 98.86 percent of cathode copper, noble metals and the like become anode mud in the electrolytic process, the yield of the noble metals in the anode mud is shown in table 4, and the specific yields are respectively as follows: 99.92% of Au, 85.57% of Ag, 99.25% of Pt, 99.58% of Pd and 81.18% of Rh. The results of example 3, which was treated by the method of the present invention, are shown in Table 3, in which the yield of copper was 99.52%, the yield of noble metal was 99.12% of Au, 99.70% of Ag, 99.27% of Pt, 99.38% of Pd, and 99.51% of Rh. The comparison shows that the total yield of the noble metal is obviously higher than that of the comparative example, and particularly, the yield of the Ag and the Rh is respectively 14.23 percent and 18.33 percent higher than that of the comparative example. Moreover, the unit price of rhodium is expensive, and the method has great economic benefit. Meanwhile, the electrolysis of the comparative example takes up to 135 hours, while the leaching time of the application is within 24 hours, thereby providing convenience for the recovery of the precious metals. In addition, through further analyzing the experimental data of the comparative example, the electrolyte and the cathode copper contain precious metals, and therefore, during the electrolysis process, the precious metals of silver, rhodium and palladium in the anode are lost in the electrolyte and the cathode, the recovery rate of the precious metals in the anode mud is reduced, the precious metals lost in the electrolyte and the cathode are difficult to recover, and even if the precious metals are recovered, the recovery cost is high, which is equivalent to that the waste of the recovered raw materials is caused to some extent by adopting the more mainstream process treatment, and the additional value of the raw materials is reduced.
In general, compared with the method, the method has the advantages that the requirement on copper purity is high in the aspect of recovering some precious metal-containing copper materials, the selective leaching mode is adopted for the precious metal-containing copper materials, and the leachate is purified to recover the silver. In addition, the selective leaching reaction time is generally within 24h, and compared with the time of an electrolytic refining method, the time for separating the precious metals from copper is greatly reduced, so that the precious metal recovery period is shortened.
Claims (8)
1. A method of separating copper and precious metals from a precious metal-containing copper alloy, comprising the steps of:
(1) fire smelting: smelting the alloy material containing the noble metal copper in a smelting furnace at 1200 ℃ to melt the alloy material into a molten state;
(2) atomizing to prepare powder: atomizing and solidifying the noble metal-containing copper alloy material in the molten state in the step (1) by an atomizing powder making device to obtain noble metal-containing copper powder;
(3) selective leaching: adding the copper powder containing the noble metals in the step (2) into a reaction kettle with a vent pipe, adding a leaching agent, starting stirring, introducing air into the reaction kettle through the vent pipe, controlling the oxidation-reduction potential of the reaction kettle to be 300-400mv, reacting for 20-22 hours, filtering to obtain leaching slag and leaching liquid, wherein the leaching slag is used for extracting and recovering the noble metals;
(4) purifying: adding the leachate obtained in the step (3) into another reaction kettle, starting stirring, adding copper powder, reducing silver ions into simple substance silver by the copper powder, filtering to obtain relatively pure copper sulfate solution and silver powder, and recovering the silver powder;
(5) electrodeposition: and (4) conveying the copper sulfate solution obtained in the step (4) to an electrodeposition tank, introducing direct current, obtaining a copper plate at the cathode under the action of the direct current, generating oxygen at the anode and generating electrodeposition waste liquid at the same time.
2. The method of claim 1 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: the noble metal-containing copper alloy material in the step (1) is a copper material at least containing silver and/or rhodium.
3. The method of claim 1 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: the smelting furnace in the step (1) is a medium-frequency smelting furnace.
4. The method of claim 1 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: and (4) returning the electrodeposition waste liquid generated in the step (5) to the step (3) for recycling.
5. The method of claim 1 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: the leaching agent used in the step (3) is sulfuric acid and/or electrodeposition waste liquid generated in the step (5), before reaction, the mass percentage concentration of the sulfuric acid in the solution is 10%, the solid-liquid ratio of the reaction is 1:20-24, and the reaction temperature is normal temperature.
6. The method of claim 5 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: when the concentration of sulfuric acid in the solution is higher than and close to 10%, the solid-to-liquid ratio is 1:20-24, and the adjustment can be realized by adding water.
7. The method of claim 1 for separating copper and noble metals from a noble metal-containing copper alloy, wherein: the reaction temperature in the step (4) is normal temperature.
8. The method of claim 1 for separating copper and precious metals from a precious metal-containing copper alloy, wherein: the current density in the step (5) is 180-2The copper content of the liquid before electrodeposition is 35-45g/L, and the copper content of the liquid after electrodeposition is 30-35 g/L.
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