CN112458289B - Method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste - Google Patents

Method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste Download PDF

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CN112458289B
CN112458289B CN202011204369.6A CN202011204369A CN112458289B CN 112458289 B CN112458289 B CN 112458289B CN 202011204369 A CN202011204369 A CN 202011204369A CN 112458289 B CN112458289 B CN 112458289B
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silver
cleaning
solid
copper
solid treatment
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CN112458289A (en
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代林涛
周克武
钟民
林应涛
宋振阳
夏宗斌
张明江
王达武
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Wenzhou Weida Precious Metal Powder Material Co ltd
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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
    • C22B11/042—Recovery of noble metals from waste materials
    • 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
    • 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
    • C22B15/0073—Leaching or slurrying with acids or salts thereof containing nitrogen
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043—Sulfurated acids or salts thereof
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/0438—Nitric acids or salts thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
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Abstract

The invention discloses a method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste, which comprises the following steps: s1, placing the silver-nickel alloy copper-based rivet waste into a reactor with an ultrasonic oscillation function, adding a proper amount of preheated reactant, filtering and cleaning after the reaction is finished, and marking the obtained solid as a first solid treatment substance; s2, adding the first solid treatment substance into a reducing solution, and after the reaction is finished, filtering and cleaning to obtain a second solid treatment substance; s3, adding the second solid treatment substance into the filtrate collected in the step S1, performing ultrasonic oscillation, filtering and cleaning to obtain a third solid treatment substance, and combining and mixing the cleaning solution filtered in the step S1 with the filtrate and the cleaning solution filtered in the step to obtain a mixed solution; s4, the mixed solution is a solution containing silver ions, the silver is recovered by reduction, and a third solid treatment object is dried, wherein the third solid treatment object is a mixture of copper and nickel, so that the recovery and separation of the silver are realized. The method has the advantages of simple technical route, low treatment cost, good silver separation effect and high silver recovery rate which is more than 99.5 percent.

Description

Method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste
Technical Field
The invention belongs to the field of precious metal hydrometallurgy, and particularly relates to a method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste.
Background
Along with the development of the society, various electrical appliances come into operation, a key component, namely a contact, exists in most electrical appliances, the contact is an intersection point for mutual separation and contact when the electronic electrical appliances are opened and closed, the key component plays an important role, and the performance of the key component directly influences the reliable operation of the switching electrical appliances. Various types of silver alloys are widely used in the contact industry due to excellent performance, but the contacts have a certain rejection rate in the production process, nearly thousand tons of silver alloy contact wastes are generated in China every year, and the silver-nickel-based copper-clad rivets with high nickel content have complex components and easy passivation of nickel, so that no proper method is available for recycling.
In the prior art, documents of 'process for recovering silver from copper-based silver-plated waste and copper-based silver-containing electrical contact waste', royal weiliang, and the like, China resource regeneration, stage 1998/05, describe a method for dissolving copper-based silver-plated waste and copper-based silver-containing electrical contact waste by mixing nitric acid and sulfuric acid, the method has good separation effect on copper-based silver-containing electrical contact waste of copper-based silver-plated waste, but because nickel is easily passivated in the mixed acid and part of silver is wrapped after passivation, the method has poor separation effect on high-nickel-content silver alloy copper-based rivet waste.
The document, "direct preparation of silver-copper bimetallic powder by using waste silver-copper alloy contacts", royal jelly and the like, gold, volume 10/31 of 2010 introduces a method for recovering silver-copper bimetallic powder by dissolving with nitric acid and reducing with a reducing agent, the method does not separate silver and copper and directly recovers mixed metal powder for contact manufacturing and the like, the method shortens the process flow to a certain extent, but the method has large nitric acid consumption and large treatment pressure of nitric oxide and is not beneficial to environmental protection treatment, and in addition, whether the silver-copper bimetallic powder directly recovered by the method can be used for contact processing needs further industrial verification.
In the document of silver-copper composite waste separation technology, congratulatory lagoon and the like, nonferrous metallurgy, 1999 02, various silver-copper waste separation technologies are introduced, including an electrolytic method, a nitric acid dissolution method, a pyrometallurgical method and the like, and various methods have advantages and disadvantages, but no suitable method is provided for the silver-nickel alloy copper-based rivet waste with high nickel content.
Therefore, a new method for recovering the high-nickel-content silver-nickel alloy copper-based rivet waste needs to be explored.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provide a method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste. The method has the advantages of simple technical route, low treatment cost, good silver separation effect and high silver recovery rate which is more than 99.5 percent.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
s1, placing the silver-nickel alloy copper-based rivet waste into a reactor with an ultrasonic oscillation function, adding a proper amount of preheated reactant, wherein the reactant is a mixed solution of sulfuric acid, nitric acid and hydrogen peroxide, starting ultrasonic oscillation, filtering and cleaning after the reaction is finished, respectively collecting filtrate and washing liquor, and marking the obtained solid as a first solid treatment substance;
s2, adding the first solid treatment substance into a reducing solution, and after the reaction is finished, filtering and cleaning to obtain a second solid treatment substance;
s3, adding the second solid treatment substance into the filtrate collected in the step S1, performing ultrasonic oscillation for a certain time, filtering and cleaning to obtain a third solid treatment substance, and combining and mixing the cleaning solution filtered in the step S1 with the filtrate and the cleaning solution filtered in the step to obtain a mixed solution;
and S4, using the mixed solution to recover silver, and drying a third solid treatment substance, wherein the third solid treatment substance is a mixture of copper and nickel, so that the recovery and separation of the silver are realized.
The silver-nickel alloy copper-based rivet waste material further comprises the following components: comprises 15-25 wt% of silver, 3.75-10 wt% of nickel and the balance of copper.
The preheating temperature of the reactant is further set to be 80-140 ℃.
The reaction agent further comprises the following components: the concentration of the nitric acid is 8-12 wt%, the concentration of the hydrogen peroxide is 1wt%, and the balance is concentrated sulfuric acid.
Further, the ultrasonic oscillation frequency in the steps S1 and S3 is set to be 20-40 kHz.
The innovative mechanism of the method is that the method is based on a method for selectively dissolving silver by nitric-sulfuric mixed acid, and 20-40 kHz low-frequency ultrasonic vibration is added to destroy the adsorption of a passivation film and a metal matrix, so that the passivation film is prevented from hindering the reaction. A small amount of hydrogen peroxide is added to accelerate the reaction speed. And simultaneously, one-step reduction operation and secondary dissolution are carried out, so that the recovery rate of silver is ensured.
The invention has the beneficial effects that: in the prior art, no appropriate hydrometallurgical method is available for recycling the waste, and if a nitric acid dissolving method is adopted, a large amount of nitrogen oxides can be generated, so that great environmental protection pressure is brought. Meanwhile, the selective copper dissolving method is not suitable because of low silver content. The nitric acid and sulfuric acid mixed acid selective silver dissolving method is adopted, and the recovery rate of silver is low due to the existence of nickel. On the basis of a nitric acid and sulfuric acid mixed acid selective silver dissolving method, the invention adds low-frequency ultrasonic oscillation to destroy the adsorption of a passivation film of nickel and a metal matrix and prevent the passivation film from hindering the reaction. A small amount of hydrogen peroxide is added to accelerate the reaction speed. And simultaneously, one-step reduction operation and secondary dissolution are carried out, so that the recovery rate of silver is ensured.
The method has the advantages of simple process route, low treatment cost, good silver separation effect and high silver recovery rate which is more than 99.5 percent. The invention effectively solves the problem of difficult recovery of the waste, and has remarkable economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1
(1) Putting 1000g of rivet waste (containing 18.6% of silver and 4.7% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 2000g of prepared hot reactant, wherein the concentration of nitric acid is 8%, the concentration of hydrogen peroxide is 1%, the temperature is 90 ℃, starting the ultrasonic oscillation, the frequency is 28kHz, reacting for 30min, filtering and cleaning, and respectively collecting filtrate and cleaning solution, wherein the obtained solid is 1. (2) 5% hydrazine hydrate 1L is added into the solid 1, and after reaction for 30min, filtration and cleaning are carried out. The filtrate was worked up and the resulting solid was solid 2. (3) Adding the solid 2 into the filtrate collected by the first filtration, controlling the temperature at 90 ℃ and the frequency at 28KHz, performing ultrasonic oscillation for 30min, filtering and cleaning, and combining the washing solution filtered in one step with the filtrate and the washing solution filtered in the third step to obtain a solid 3. (4) The liquid collected in the third step was passed through a silver recovery system to obtain 184.9g of silver powder, with a silver recovery rate of 99.4%. The dried solid 3 weighed 796.8g, and contained 92.4% copper, 4.6% nickel and 0.09% silver.
Example 2
(1) Putting 2000g of rivet waste (containing 22.8% of silver and 9.2% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 4000g of prepared hot reactant, wherein the concentration of nitric acid is 10%, the concentration of hydrogen peroxide is 1%, the temperature is 110 ℃, starting the ultrasonic oscillation, the frequency is 28kHz, reacting for 30min, filtering and cleaning, and respectively collecting filtrate and cleaning solution, wherein the obtained solid is 1. (2) 5% hydrazine hydrate 1L is added into the solid 1, and after reaction for 30min, filtration and cleaning are carried out. The filtrate was worked up and the resulting solid was solid 2. (3) Adding the solid 2 into the filtrate collected by the first filtration, controlling the temperature at 120 ℃ and the frequency at 28kHz, filtering and cleaning after ultrasonic oscillation for 30min, and combining the cleaning solution filtered in the first step with the filtrate and the cleaning solution filtered in the third step to obtain a solid 3. (4) 428.7g of silver powder is prepared from the liquid collected in the third step through a silver recovery system, and the silver recovery rate is 99.7%. The dried solid 3 weighed 1501.8g, contained 87.9% copper, 8.3% nickel and 0.15% silver.
Example 3
1) Putting 1000g of rivet waste (containing 18.6% of silver and 4.7% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 2000g of prepared hot reactant, wherein the concentration of nitric acid is 8%, the concentration of hydrogen peroxide is 1%, the temperature is 90 ℃, starting the ultrasonic oscillation, the frequency is 20kHz, reacting for 30min, filtering and cleaning, and respectively collecting filtrate and cleaning solution, wherein the obtained solid is 1. (2) 5% hydrazine hydrate 1L is added into the solid 1, and after reaction for 30min, filtration and cleaning are carried out. The filtrate was worked up and the resulting solid was solid 2. (3) Adding the solid 2 into the filtrate collected by the first filtration, controlling the temperature at 90 ℃ and the frequency at 20KHz, performing ultrasonic oscillation for 30min, filtering and cleaning, and combining the washing solution filtered in one step with the filtrate and the washing solution filtered in the third step to obtain a solid 3. (4) And (3) passing the liquid collected in the third step through a silver recovery system to obtain 183.5g of silver powder, wherein the silver recovery rate is 98.6%. The dried solid 3 weighed 806.5g, and contained 94.1% copper, 5.2% nickel and 0.18% silver.
Example 4
1) Putting 1000g of rivet waste (containing 18.6% of silver and 4.7% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 2000g of prepared hot reactant, wherein the concentration of nitric acid is 8%, the concentration of hydrogen peroxide is 1%, the temperature is 90 ℃, starting the ultrasonic oscillation, the frequency is 40kHz, reacting for 30min, filtering and cleaning, and respectively collecting filtrate and cleaning solution, wherein the obtained solid is 1. (2) 5% hydrazine hydrate 1L is added into the solid 1, and after reaction for 30min, filtration and cleaning are carried out. The filtrate was worked up and the resulting solid was solid 2. (3) Adding the solid 2 into the filtrate collected by the first filtration, controlling the temperature at 90 ℃ and the frequency at 40KHz, performing ultrasonic oscillation for 30min, filtering and cleaning, and combining the washing solution filtered in one step with the filtrate and the washing solution filtered in the third step to obtain a solid 3. (4) And (5) passing the liquid collected in the third step through a silver recovery system to obtain 185.5g of silver powder, wherein the silver recovery rate is 99.7%. The dried solid 3 weighed 780.2g, and contained 96.1% copper, 3.2% nickel and 0.05% silver.
Comparative example 1
(1) Putting 1000g of rivet waste (containing 22.8% of silver and 5.7% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 2000g of prepared hot reactant, wherein the concentration of nitric acid is 9%, the concentration of hydrogen peroxide is 1%, the temperature is 90 ℃, starting the ultrasonic oscillation, the frequency is 80kHz, reacting for 60min, filtering and cleaning, and respectively collecting filtrate and cleaning solution, wherein the obtained solid is 1. (2) 5% hydrazine hydrate 1L is added into the solid 1, and after reaction for 30min, filtration and cleaning are carried out. The filtrate was worked up and the resulting solid was solid 2. (3) Adding the solid 2 into the filtrate collected by the first filtration, controlling the temperature at 90 ℃ and the frequency at 80kHz, performing ultrasonic oscillation for 30min, then performing filtration and cleaning, and combining the filtrate filtered in the first step with the filtrate and the washing liquid filtered in the third step to obtain a solid 3. (4) The liquid collected in the third step was passed through a silver recovery system to obtain 122.1g of silver powder, with a silver recovery rate of 53.6%. The dried solid 3 weighed 860.8g, and contained 81.4% copper, 6.1% nickel and 12.2% silver.
Comparative example 2
(1) Putting 1000g of rivet waste (containing 19.3% of silver and 4.8% of nickel) into a stainless steel reactor with ultrasonic oscillation, adding 2000g of prepared hot reactant, wherein the concentration of nitric acid is 9%, the concentration of hydrogen peroxide is 1%, the temperature is 90 ℃, starting the ultrasonic oscillation, the frequency is 28kHz, reacting for 30min, filtering and cleaning, collecting filtrate and cleaning solution, and obtaining a solid 1. (2) The liquid collected in the first step was passed through a silver recovery system to obtain 157.9g of silver powder, with a silver recovery rate of 81.8%. The dried solid 1 weighed 845.8g, and contained 88.6% copper, 4.3% nickel and 4% silver.
Through comparative analysis of the embodiment 1 and the comparative examples 1 to 4, the ultrasonic oscillation frequency is very important, the ultrasonic oscillation frequency is too high, the cavitation effect is small, the destructive effect on the adsorption effect between the passivation film and the metal matrix is limited, and the recovery rate of silver is influenced. The silver recovery rate is low because the adsorption action of all the passivation films and the metal matrix cannot be guaranteed to be destroyed even if ultrasonic oscillation is added, and at the moment, reduction must be carried out firstly to recover the metal activity, and then the silver is dissolved once again to guarantee the separation recovery rate of the silver.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.

Claims (3)

1. A method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste is characterized by comprising the following steps:
s1, placing the silver-nickel alloy copper-based rivet waste into a reactor with an ultrasonic oscillation function, adding a proper amount of preheated reactant, wherein the reactant is a mixed solution of sulfuric acid, nitric acid and hydrogen peroxide, starting ultrasonic oscillation, filtering and cleaning after the reaction is finished, and respectively collecting filtrate and washing liquor, wherein the obtained solid is marked as a first solid treatment substance;
s2, adding the first solid treatment substance into a reducing solution, and after the reaction is finished, filtering and cleaning to obtain a second solid treatment substance;
s3, adding the second solid treatment substance into the filtrate collected in the step S1, performing ultrasonic oscillation treatment, filtering and cleaning to obtain a third solid treatment substance, and combining and mixing the cleaning solution filtered in the step S1 with the filtrate and the cleaning solution filtered in the step to obtain a mixed solution;
s4, the mixed solution is a solution containing silver ions, the silver is recovered by reduction, and a third solid treatment object is dried, wherein the third solid treatment object is a mixture of copper and nickel, so that the recovery and separation of the silver are realized;
the silver-nickel alloy copper-based rivet waste comprises the following components: comprises 15-25 wt% of silver, 3.75-10 wt% of nickel and the balance of copper;
the components of the reactant are as follows: the concentration of the nitric acid is 8-12 wt%, the concentration of the hydrogen peroxide is 1wt%, and the balance is concentrated sulfuric acid.
2. The method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet scrap according to claim 1, characterized in that: the preheating temperature of the reactant is 80-140 ℃.
3. The method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet scrap according to claim 1, characterized in that: the ultrasonic oscillation frequency in the steps S1 and S3 is 20-40 kHz.
CN202011204369.6A 2020-11-02 2020-11-02 Method for selectively separating and recovering silver from silver-nickel alloy copper-based rivet waste Active CN112458289B (en)

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