CN115369255B - Silver recovery process of electronic element - Google Patents
Silver recovery process of electronic element Download PDFInfo
- Publication number
- CN115369255B CN115369255B CN202210800827.5A CN202210800827A CN115369255B CN 115369255 B CN115369255 B CN 115369255B CN 202210800827 A CN202210800827 A CN 202210800827A CN 115369255 B CN115369255 B CN 115369255B
- Authority
- CN
- China
- Prior art keywords
- silver
- filtrate
- leaching
- recovery process
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application relates to the technical field of precious metal recovery, in particular to a silver recovery process of an electronic element. The silver recovery process includes recovering silver from a chlorinated extract, comprising: s1, stirring and cleaning the chloridized extract, and filtering the cleaned material to obtain primary cleaning slag; s2, adding pure water into the primary cleaning slag, and filtering the cleaned material to obtain secondary cleaning slag; s3, adding pure water into the secondary cleaning slag, heating the mixture to 30-35 ℃, adjusting the pH value of the mixture to 8-9, carrying out a complexing reaction on sodium sulfite and silver in the mixture, and filtering the mixture to obtain complex filtrate which is a leaching solution enriched with silver; s4, putting the leaching solution into an electrodeposition tank for electrodeposition treatment, wherein the obtained solid is silver powder, and the silver recovery process of the electronic element improves the recovery efficiency of silver and has the advantages of environmental protection, good quality and high purity of the recovered silver powder.
Description
Technical Field
The application relates to the technical field of metal recovery of electronic elements, in particular to a silver recovery process of electronic elements.
Background
With the rapid development of world electronic information, electronic products are more and more widely related, more and more used, and more rapidly updated, so that more and more waste electronic products are available in the market. The waste circuit boards and chips contain precious metals such as gold, silver, palladium and the like, and the recycling of the waste circuit boards and the chips is a market requirement and an environmental requirement. Silver is an indispensable component of various electronic devices, and its commercial price is not high, so that it is an important way to reduce the production cost in the process of recovering silver from waste circuit boards at one time.
At present, the processing method for processing the waste circuit board and the chip in the waste gas mobile phone mainly comprises the steps of separation, crushing, enrichment, purification and the like.
Chinese patent CN108950217a discloses a method for recovering gold and silver from waste printed circuit board, which is to leach silver and gold respectively by nitric acid and aqua regia after crushing the waste printed circuit board and smelting at high temperature. However, the molten material contains gold and silver elements, and also contains copper and a large amount of base metals such as iron, nickel, tin, and the like, and only nitric acid and aqua regia are used for leaching the gold and silver elements, and only dissolution is performed according to the activity of the metals, so that the dissolution effect of gold and silver is not ideal.
Chinese patent CN102952947B discloses a method for comprehensively recovering rare noble metals from waste circuit boards, which comprises low-temperature roasting, ammonia leaching, nitric acid leaching, hydrochloric acid and sodium hypochlorite comprehensive leaching and SO 2 The gold powder replacement and other processes realize production. However, gold and silver in the waste circuit board cannot be separated from nonmetal in the crushing process, and a part containing metal after electrostatic separation contains a large amount of nonmetal at the same time, so that a large amount of dioxin can be generated by baking at 200-300 ℃; and the dangerous chemicals used comprise ammonia water, hydrochloric acid, sulfuric acid, nitric acid, sulfur dioxide, zinc powder and the like, and the storage and the use of the dangerous chemicals have great comprehensive dangerous hidden dangers, so that the production cost is too high, and the dangerous chemicals are not suitable for industrial production.
Disclosure of Invention
The application aims to avoid the defects in the prior art and provide the silver recovery process of the electronic element, which can rapidly and efficiently leach the leaching solution enriched with silver, effectively improve the recovery rate of silver, has the advantage of environmental protection in the recovery process, and has the advantages of good quality and high purity of the recovered silver powder.
In order to achieve the above purpose, the present application provides the following technical solutions:
there is provided a silver recovery process for an electronic component, comprising the steps of: pretreating electronic components to obtain chloridized extract containing silver ions,
recovering silver from the chlorinated extract, comprising:
s1, adding a proper amount of pure water and a proper amount of hydrogen peroxide into the chlorinated extract, heating to 30-35 ℃, fully stirring to clean the chlorinated extract, and filtering after cleaning to obtain primary cleaning slag;
s2, adding pure water into the primary cleaning slag, fully stirring again to clean the primary cleaning slag, and filtering after cleaning to obtain secondary cleaning slag;
s3, adding pure water into the secondary cleaning slag, continuously stirring to obtain a mixed material, heating the mixed material to 30-35 ℃, adjusting the pH value of the mixed material to 8-9, adding sodium sulfite into the mixed material to cause the sodium sulfite to generate a complex reaction with the mixed material, and filtering the reacted mixed material to obtain complex filtrate, wherein the complex filtrate is a leaching solution rich in silver ions;
and S4, adding the leaching solution obtained in the step S3 into an electrodeposition tank, performing electrodeposition reduction treatment, filtering the leaching solution after the reduction treatment, and obtaining solid silver powder after filtering.
In some embodiments, the pretreatment comprises the steps of: crushing the electronic element to prepare electronic element powder;
adding the electronic component powder into a mixed solution containing a proper amount of sulfuric acid solution and a proper amount of hydrogen peroxide, fully reacting the electronic component powder with the mixed solution, adding a proper amount of sodium chloride after the reaction, and fully stirring to obtain a first solid-liquid material;
filtering the first solid-liquid material to obtain a first filtrate and a first solid material;
dissolving gold in the first solid material in a chlorination leaching manner to obtain a second solid-liquid material;
and filtering the second solid-liquid material to obtain a second filtrate and a second solid material, wherein the second solid material is chloridized extract.
In some embodiments, the step of comminuting the electronic component comprises: and (3) carrying out heat treatment on the electronic element at 150-170 ℃ to separate a chip containing noble metal, mechanically crushing the chip into fragments smaller than or equal to 5mm, and grinding the fragments into electronic element powder with the particle size smaller than 100 meshes.
In some embodiments, the first filtrate is fed into a copper cyclone electrodepositing apparatus to recover electrodeposited copper tubes.
In some embodiments, a saturated sodium sulfite solution is added to the second filtrate until the second filtrate reaches a potential of 180mV to 210mV, and the second filtrate is fully reacted with the sodium sulfite solution to obtain the reduced gold powder.
In some embodiments, in the step S1, the concentration of the hydrogen peroxide is 1% -5%, the hydrogen peroxide is continuously added into the pure water at a speed of 5 ml/min-20 ml/min, and the solid-liquid ratio of the chloridized extract to the pure water and the hydrogen peroxide is kept at 1:3-5;
in some embodiments, in S2, the solid-to-liquid ratio of the primary cleaning slag to the pure water is 1:3-5.
In some embodiments, in S3, the complex filtrate is cyclically leached, the step of cyclically leaching comprising:
fully mixing the complex filtrate with cleaning slag of the next batch to obtain a circulating material, wherein the cleaning slag is secondary cleaning slag after being sequentially processed by S1 and S2;
controlling the temperature of the circulating material to be 30-35 ℃, adding sodium sulfite, adjusting the pH value of the circulating material to be 8-9, and then filtering to obtain a circulating leaching filtrate;
repeating the step of circulating leaching of the circulating leaching filtrate until silver ions in the circulating leaching filtrate are saturated, and finally obtaining the circulating leaching filtrate which is the leaching solution enriched with silver.
In some embodiments, in S3, the sodium sulfite has a purity of greater than 95% and is added in an amount of 190g to 200g per liter of the mixture;
in the cyclic leaching step, the addition amount of the sodium sulfite is 3-5% of the addition amount of the sodium sulfite in the previous batch.
In some embodiments, in S4, the leaching solution is vacuum filtered before being fed into the electrowinning cell.
In some embodiments, the electrowinning cell has a current density of 200-300mA/m 2 The voltage is 3-5V, and the electrodeposition mode is continuous electrodeposition.
The silver recovery process of the electronic element has the beneficial effects that:
(1) The application relates to a silver recovery process of an electronic element, which comprises the steps of firstly preprocessing the electronic element to obtain a chloridized extract enriched with silver, and then leaching the silver of the chloridized extract by sodium sulfite to obtain Ag (SO) 3 ) 2 3- Complexes of Ag (SO) 3 ) 2 3- The complex is subjected to electrodeposition to recover silver, the whole silver recovery process is a full wet method, and the silver recovery process through electrodeposition does not involve chemical substances, so that the method has the advantages of environmental protection and production cost reduction, and is suitable for industrial production.
(2) In the silver recovery process of the electronic component, in the step of recovering silver of the chlorinated extract, chlorine removal treatment is carried out on the chlorinated extract, so that the chlorine content of the chlorinated extract is reduced, the influence of chloride ions on silver leached by sodium sulfite is reduced by reducing the chlorine content of the chlorinated extract, the silver leaching rate in the chlorinated extract is improved, and the recovery rate is effectively improved; according to the method, chlorine is reduced by hydrogen peroxide through primary cleaning, the chlorine is volatilized through a heating mode, and redundant hydrogen peroxide is removed through secondary cleaning, so that the chlorine can be efficiently removed, and the influence of the hydrogen peroxide on chlorinated extract can be avoided.
Drawings
Fig. 1 is a schematic flow chart of a silver recovery process of an electronic component of an embodiment.
Fig. 2 is a schematic diagram showing the operation of the electrodeposition of silver according to the embodiment.
Detailed Description
Preferred embodiments of the present application will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present application are shown in the drawings, it should be understood that the present application may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the application to those skilled in the art.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first," "second," "third," etc. may be used herein to describe various information, these information should not be limited by these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the application. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Example 1
Silver is an indispensable component of various electronic devices, and its commercial price is not high, so that it is an important way to reduce the production cost in the process of recovering silver from waste circuit boards at one time.
In the prior art, the waste circuit board is crushed, smelted at high temperature and then leached with nitric acid and aqua regia to obtain silver and gold respectively. However, the molten material contains gold and silver elements, and also contains copper and a large amount of base metals such as iron, nickel, tin, and the like, and only nitric acid and aqua regia are used for leaching the gold and silver elements, and only dissolution is performed according to the activity of the metals, so that the dissolution effect of gold and silver is not ideal.
The prior art also firstly comprises low-temperature roasting, ammonia leaching, nitric acid leaching, hydrochloric acid and sodium hypochlorite comprehensive leaching and SO 2 The gold powder replacement and other processes realize production. However, gold and silver in the waste circuit board cannot be separated from nonmetal in the crushing process, and a part containing metal after electrostatic separation contains a large amount of nonmetal at the same time, so that a large amount of dioxin can be generated by baking at 200-300 ℃; and the dangerous chemicals used comprise ammonia water, hydrochloric acid, sulfuric acid, nitric acid, sulfur dioxide, zinc powder and the like, and the storage and the use of the dangerous chemicals have great comprehensive dangerous hidden dangers, so that the production cost is too high, and the dangerous chemicals are not suitable for industrial production.
In view of the above problems, this embodiment discloses a silver recovery process for electronic components, as shown in fig. 1, comprising the steps of:
crushing the electronic element to obtain electronic element powder;
the electronic component powder is added into a mixed solution containing a proper amount of sulfuric acid solution and a proper amount of hydrogen peroxide, and the concentration of the sulfuric acid solution is 1.5ml/L, the hydrogen peroxide is continuously added into the sulfuric acid solution in an amount of 20ml/min, the solid-to-liquid ratio of the mixed solution is 1:10, and in practical application, the dosage of the sulfuric acid solution and the proper amount of hydrogen peroxide can be adjusted according to practical conditions, so long as the electronic component powder is dissolved, and the method is not limited. And (3) fully reacting the electronic component powder with the mixed solution, adding a proper amount of sodium chloride after the reaction, and fully stirring to obtain a first solid-liquid material. For example, 100 kg of sodium chloride is added to each cube of the mixed solution, and in practical application, the dosage of the sodium chloride can be adjusted according to practical situations, so long as silver ions in the mixed solution are precipitated, and the method is not limited.
And adding sulfuric acid and hydrogen peroxide into the electronic component powder, leaching copper, iron, nickel, tin and other metals in the electronic component by the sulfuric acid and the hydrogen peroxide in the reaction process, adding sodium chloride, and precipitating silver in the leaching solution by the sodium chloride to separate the silver from the copper, the iron, the nickel and the tin in the electronic component, thereby obtaining a first solid-liquid material.
Filtering the first solid-liquid material to obtain a first filtrate and a first solid material;
dissolving gold in the first solid material in a chlorination leaching manner to obtain a second solid-liquid material, wherein the chlorination leaching manner is to use hydrochloric acid as a leaching agent, for example, so that gold-soluble metal chloride form in the first solid material is transferred into solution to realize gold and silver separation and further enrich silver;
filtering the second solid-liquid material to obtain a second filtrate and a second solid material, wherein the second solid material is a chloridized extract;
recovering silver from the chlorinated extract, comprising:
s1, adding a proper amount of pure water and a proper amount of hydrogen peroxide into the chlorinated extract, heating to 30-35 ℃, preferably 32 ℃, fully stirring to clean the chlorinated extract, wherein the stirring time is 0.5H, the stirring speed is 60-80 r/min, the stirring parameters are only required to fully mix the materials, the stirring parameters can be adjusted according to actual conditions, and the primary cleaning slag is obtained after cleaning;
s2, adding pure water into the primary cleaning slag, fully stirring again to clean the primary cleaning slag, wherein the stirring time is 0.5H, the stirring speed is 60r/min-80r/min, the materials are fully mixed, and the stirring parameters can be adjusted according to the actual situation. Filtering the cleaned material to obtain secondary cleaning slag;
s3, adding pure water into the secondary cleaning slag, continuously stirring, and heating the mixture to 30-35 ℃, preferably 32 ℃, adjusting the pH of the mixture to 8-9, adding sodium sulfite into the mixture to carry out complexation reaction on the sodium sulfite and silver in the mixture, and filtering the reacted mixture to obtain complex filtrate, wherein the complex filtrate is leaching liquid enriched with silver ions;
and S4, adding the leaching solution obtained in the step S3 into an electrodeposition tank, performing electrodeposition reduction treatment, filtering the leaching solution after the reduction treatment, and obtaining solid silver powder after filtering.
The silver recovery process of the electronic element comprises the steps of firstly, treating the electronic element by sulfuric acid and hydrogen peroxide to leach metals such as copper, iron, nickel, tin and the like in the electronic element, so as to obtain a solid material enriched with gold and silver, namely a first solid material; further leaching gold from the first solid material by chloridizing leaching to obtain chloridized extract enriched with silver, and leaching silver of the chloridized extract by sodium sulfite to obtain Ag (SO) 3 ) 2 3- Complexes of Ag (SO) 3 ) 2 3- The complex is subjected to electrodeposition to recover silver, the whole silver recovery process is a full wet method, and the silver recovery process through electrodeposition does not involve chemical substances, so that the method has the advantages of environmental protection and production cost reduction, and is suitable for industrial production. In the step of recovering silver from the chloride extract, chlorine removal treatment is carried out on the chloride extract, so that the chlorine content of the chloride extract is reduced, the influence of chloride ions on silver leaching from sodium sulfite is reduced by reducing the chlorine content in the chloride extract, the silver leaching rate in the chloride extract is improved, and the recovery rate is effectively improved; according to the method, chlorine is reduced by hydrogen peroxide through primary cleaning, the chlorine is volatilized through a heating mode, and redundant hydrogen peroxide is removed through secondary cleaning, so that the chlorine can be efficiently removed, and the influence of the hydrogen peroxide on chlorinated extract can be avoided.
In this embodiment, in the step S1, the concentration of the hydrogen peroxide is 1% -5%, preferably 3%, the hydrogen peroxide is continuously added into the pure water at a speed of 5 ml/min-20 ml/min, preferably at a speed of 10ml/min, and the solid-liquid ratio of the chlorinated extract to the pure water to the hydrogen peroxide is kept at 1:3-5, preferably at 1:4. The solid-liquid ratio can be adjusted according to the actual situation, and is not limited as long as the chlorine substance in the chlorinated extract can be cleaned.
In the step S2, the solid-liquid ratio of the primary cleaning slag to the pure water is 1:3-5, preferably 1:4. The solid-liquid ratio can be adjusted according to the actual situation, and is not limited as long as the chlorine substance in the chlorinated extract can be cleaned.
In this embodiment, in the S3, the purity of the sodium sulfite is greater than 95%, the amount of the sodium sulfite added per liter of the mixture is 190 g-200 g, preferably 195g, and the addition amount of the sodium sulfite can ensure a good reduction effect, and of course, the addition amount of the sodium sulfite can be adjusted according to actual conditions, and the method is not limited herein.
In this example, a plate and frame filter press was used to filter in a press filtration manner. The plate-frame filter press can accelerate and ensure the filtering effect, and is beneficial to improving the production efficiency.
In this embodiment, in S4, the leaching solution is first placed in a vacuum filter of polypropylene fiber with a filter cloth model 840A for suction filtration, and then the suction-filtered leaching solution is put into the electrowinning tank, so that the leaching solution can be preliminarily filtered to contain solid impurities.
The cathode plate and the anode plate are arranged in the electrode tank, so that the leaching solution enriched with silver can be reduced, and the problem that formaldehyde, formic acid, hydrazine hydrate and other harmful chemicals are needed in the silver reduction process of silver sulfite complex ions is solved.
Example 2
It is to be understood that the following provides an example of a silver recovery process for electronic components, and in practical applications, the step of pulverizing the electronic components includes: and (3) carrying out heat treatment on the electronic element at 150-170 ℃ to separate a chip containing noble metal, mechanically crushing the chip into fragments smaller than or equal to 5mm, and grinding the fragments into electronic element powder with the particle size smaller than 100 meshes.
And part of nonmetallic substances are removed in a heat treatment mode, so that the rapid recovery of metals is facilitated. The collected chips are crushed again, so that metals can be recovered from crushed materials conveniently.
Other operation manners are the same as those of embodiment 1, and will not be described here again.
Example 3
It will be appreciated that the following provides an example of a silver recovery process for electronic components, in which the first filtrate is fed into a copper cyclone electrowinning apparatus to recover the electrodeposited copper tubes.
The electrolytic copper cyclone equipment commonly used in the market of the copper cyclone electro-deposition equipment utilizes an electrolysis technology to recycle copper, thereby avoiding the generation and discharge of a large amount of copper sludge and playing an environmental protection role.
Other operation manners are the same as those of embodiment 1, and will not be described here again.
Example 4
It is to be understood that the following description of one embodiment of the silver recovery process for electronic components is provided, and in practical application, a saturated sodium sulfite solution is added to the second filtrate until the second filtrate has a potential of 180mV to 210mV, preferably 200mV, and the second filtrate is sufficiently reacted with the sodium sulfite solution to obtain reduced gold powder.
The second filtrate has leached gold, and the sodium sulfite solution can reduce gold in the second filtrate to obtain coarse gold powder.
Other operation manners are the same as those of embodiment 1, and will not be described here again.
Example 5
It is to be understood that, in the following description of an embodiment of a silver recovery process for electronic components is provided, in practical application, since the silver ion content in the leachate for the first silver enrichment is not saturated yet, in order to save the usage and improve the environmental protection, in S3, the step of circularly leaching the complex filtrate includes:
and fully mixing the complex filtrate with the cleaning slag of the next batch to ensure that the solid-liquid ratio of the complex filtrate to the cleaning slag is 1:3, wherein the solid-liquid ratio can be adjusted according to actual conditions, and a circulating material is obtained. The added cleaning slag is secondary cleaning slag after being sequentially processed by S1 and S2, namely, the newly added cleaning slag is chloridized extract with the chlorine content reduced firstly.
The temperature of the circulating material is controlled to be 30-35 ℃, preferably 32 ℃, sodium sulfite is added in a supplementary way, the adding amount of the sodium sulfite is 3-5% of the adding amount of the sodium sulfite at the last time, then the pH value of the circulating material is adjusted to be 8-9, and then the circulating leaching filtrate is obtained by filtering.
The cyclic leaching step utilizes the characteristic that the leaching solution is unsaturated for repeated use, reduces the material used in the leaching process, and can improve the silver enrichment rate of the leaching solution.
And repeating the step of circulating leaching by the circulating leaching filtrate until silver ions in the circulating leaching filtrate are saturated, wherein the finally obtained circulating leaching filtrate is a leaching solution rich in silver.
According to actual production, 4 batches of cleaning residues are circularly leached by using the leaching liquid, the silver content in the 4 batches of cleaning residues is respectively reduced from 7011.14g/t to 3143.60g/t, 7449.89g/t to 3787.04g/t, 6209.24g/t to 3225.79, 5974.40g/t to 36395.81g/t, leaching rates are 55.16%, 49.17%, 48.05% and 43.16%, and leaching rates of 4 batches of silver ions are respectively 55.16%, 49.17%, 48.05% and 43.16%.
Therefore, the leaching solution is used for circulating leaching, the leaching rate in the circulating leaching process is not influenced, the utilization rate of the leaching solution is effectively improved, and the method is suitable for large-scale production and application.
Other operation manners are the same as those of embodiment 1, and will not be described here again.
Example 6
It will be appreciated that one example of a silver recovery process for electronic components is provided below, and in practical use, the electrodeposition cell has a current density of 200mA/m as shown in FIG. 2 2 -300mA/m 2 The voltage is 3V-5V, and the electrodeposition mode is continuous electrodeposition.
The parameters of the electrodeposition tank can be adjusted according to actual needs, so long as silver in the electrodeposition reducing leaching solution can be realized.
After the electrodeposition is completed, as shown in fig. 2, the lower end opening of the electrodeposition tank is opened, the liquid after the electrodeposition flows to the vacuum filter cloth on the electrodeposition plate through the lower end opening of the electrodeposition tank, the silver powder deposited by the electrodeposition stays on the filter cloth, is removed from the filter cloth by a shovel, a brush and the like manually, and the electrodeposition tank is required to be sufficiently cleaned to prevent short circuit.
Other operation manners are the same as those of embodiment 1, and will not be described here again.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present application unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that like reference numerals and letters refer to like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
In the description of the present application, it should be understood that the azimuth or positional relationships indicated by the azimuth terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present application and simplify the description, and these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present application; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
In addition, the terms "first", "second", etc. are used to define the components, and are only for convenience of distinguishing the corresponding components, and the terms have no special meaning unless otherwise stated, and therefore should not be construed as limiting the scope of the present application.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (11)
1. A silver recovery process for electronic components, comprising the steps of: pretreating electronic components to obtain chloridized extract containing silver ions,
recovering silver from the chlorinated extract, comprising:
s1, adding a proper amount of pure water and a proper amount of hydrogen peroxide into the chlorinated extract, heating to 30-35 ℃, fully stirring to clean the chlorinated extract, and filtering after cleaning to obtain primary cleaning slag;
s2, adding pure water into the primary cleaning slag, fully stirring again to clean the primary cleaning slag, and filtering after cleaning to obtain secondary cleaning slag;
s3, adding pure water into the secondary cleaning slag, continuously stirring to obtain a mixed material, heating the mixed material to 30-35 ℃, adjusting the pH value of the mixed material to 8-9, adding sodium sulfite into the mixed material to cause the sodium sulfite to generate a complex reaction with the mixed material, and filtering the reacted mixed material to obtain complex filtrate, wherein the complex filtrate is a leaching solution rich in silver ions;
and S4, adding the leaching solution obtained in the step S3 into an electrodeposition tank, performing electrodeposition reduction treatment, filtering the leaching solution after the reduction treatment, and obtaining solid silver powder after filtering.
2. The silver recovery process of electronic components according to claim 1, wherein the pretreatment comprises the steps of:
crushing the electronic element to prepare electronic element powder;
adding the electronic component powder into a mixed solution containing a proper amount of sulfuric acid solution and a proper amount of hydrogen peroxide, fully reacting the electronic component powder with the mixed solution, adding a proper amount of sodium chloride after the reaction, and fully stirring to obtain a first solid-liquid material;
filtering the first solid-liquid material to obtain a first filtrate and a first solid material;
dissolving gold in the first solid material in a chlorination leaching manner to obtain a second solid-liquid material;
and filtering the second solid-liquid material to obtain a second filtrate and a second solid material, wherein the second solid material is chloridized extract.
3. The silver recovery process of electronic components according to claim 2, wherein the step of pulverizing the electronic components comprises: and (3) carrying out heat treatment on the electronic element at 150-170 ℃ to separate a chip containing noble metal, mechanically crushing the chip into fragments smaller than or equal to 5mm, and grinding the fragments into electronic element powder with the particle size smaller than 100 meshes.
4. The silver recovery process of an electronic component according to claim 2, wherein the first filtrate is fed into a copper cyclone electrodeposition apparatus to recover an electrodeposited copper tube.
5. The silver recovery process of an electronic component according to claim 2, wherein a saturated sodium sulfite solution is added to the second filtrate until the second filtrate reaches a potential of 180mV to 210mV, and the second filtrate is sufficiently reacted with the sodium sulfite solution to obtain reduced gold powder.
6. The silver recovery process of an electronic component according to claim 1, wherein in S1, the concentration of the hydrogen peroxide is 1% -5%, the hydrogen peroxide is continuously added into the pure water at a speed of 5 ml/min-20 ml/min, and the solid-liquid ratio of the chlorinated extract to the pure water and the hydrogen peroxide is kept at 1:3-5.
7. The silver recovery process of electronic components according to claim 1, wherein in S2, the solid-to-liquid ratio of the primary cleaning slag to the pure water is 1:3 to 5.
8. The silver recovery process of electronic components according to claim 1, wherein in S3, the complex filtrate is circularly leached, and the step of circularly leaching includes:
fully mixing the complex filtrate with cleaning slag of the next batch to obtain a circulating material, wherein the cleaning slag is secondary cleaning slag after being sequentially processed by S1 and S2;
controlling the temperature of the circulating material to be 30-35 ℃, adding sodium sulfite, adjusting the pH value of the circulating material to be 8-9, and then filtering to obtain a circulating leaching filtrate;
repeating the step of circulating leaching of the circulating leaching filtrate until silver ions in the circulating leaching filtrate are saturated, and finally obtaining the circulating leaching filtrate which is the leaching solution enriched with silver.
9. The silver recovery process of electronic components according to claim 8, wherein in S3, the purity of the sodium sulfite is more than 95%, and the amount of the sodium sulfite added per liter of the mixture is 190g to 200g;
in the cyclic leaching step, the addition amount of the sodium sulfite is 3-5% of the addition amount of the sodium sulfite in the previous batch.
10. The silver recovery process of electronic components according to claim 1, wherein in S4, the leaching solution is vacuum filtered before being fed into the electrodeposition tank.
11. The silver recovery process of electronic component according to claim 1, wherein the current density of the electrodeposition bath is 200-300mA/m 2 The voltage is 3-5V, and the electrodeposition mode is continuous electrodeposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210800827.5A CN115369255B (en) | 2022-07-08 | 2022-07-08 | Silver recovery process of electronic element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210800827.5A CN115369255B (en) | 2022-07-08 | 2022-07-08 | Silver recovery process of electronic element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115369255A CN115369255A (en) | 2022-11-22 |
| CN115369255B true CN115369255B (en) | 2023-10-20 |
Family
ID=84062387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210800827.5A Active CN115369255B (en) | 2022-07-08 | 2022-07-08 | Silver recovery process of electronic element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115369255B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703708A (en) * | 2012-06-19 | 2012-10-03 | 姚彦君 | Method for extracting gold and silver from electronic wastes |
| KR20140045199A (en) * | 2012-10-08 | 2014-04-16 | 한국지질자원연구원 | Method for recovering precious metals from printed circuit boards scrap of end-of-life mobile phones |
| JP2015232170A (en) * | 2014-05-12 | 2015-12-24 | Jx日鉱日石金属株式会社 | Method for refining silver |
| CN106048233A (en) * | 2016-07-30 | 2016-10-26 | 江西铜业股份有限公司 | Leaching method of silver |
| CA2950811A1 (en) * | 2015-12-15 | 2017-06-15 | Institut National De La Recherche Scientifique (Inrs) | Method for recycling valuable metals from spent batteries |
| CN108950211A (en) * | 2018-06-13 | 2018-12-07 | 珠海格力电器股份有限公司 | A method of recycling silver and copper from waste and old chip |
| WO2020113325A1 (en) * | 2018-12-03 | 2020-06-11 | Dundee Sustainable Technologies Inc. | A method and a system for gold recovery from halogen extraction treatment |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10202668B2 (en) * | 2015-08-27 | 2019-02-12 | All Green Recycling, Inc. | Metal recovery processes |
-
2022
- 2022-07-08 CN CN202210800827.5A patent/CN115369255B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703708A (en) * | 2012-06-19 | 2012-10-03 | 姚彦君 | Method for extracting gold and silver from electronic wastes |
| KR20140045199A (en) * | 2012-10-08 | 2014-04-16 | 한국지질자원연구원 | Method for recovering precious metals from printed circuit boards scrap of end-of-life mobile phones |
| JP2015232170A (en) * | 2014-05-12 | 2015-12-24 | Jx日鉱日石金属株式会社 | Method for refining silver |
| CA2950811A1 (en) * | 2015-12-15 | 2017-06-15 | Institut National De La Recherche Scientifique (Inrs) | Method for recycling valuable metals from spent batteries |
| CN106048233A (en) * | 2016-07-30 | 2016-10-26 | 江西铜业股份有限公司 | Leaching method of silver |
| CN108950211A (en) * | 2018-06-13 | 2018-12-07 | 珠海格力电器股份有限公司 | A method of recycling silver and copper from waste and old chip |
| WO2020113325A1 (en) * | 2018-12-03 | 2020-06-11 | Dundee Sustainable Technologies Inc. | A method and a system for gold recovery from halogen extraction treatment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115369255A (en) | 2022-11-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ashiq et al. | Hydrometallurgical recovery of metals from e-waste | |
| CN101575715B (en) | Method for extracting valuable metals from electronic waste | |
| US8585798B2 (en) | Method for recovering metal from ore | |
| US5882502A (en) | Electrochemical system and method | |
| CN102994771B (en) | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid | |
| JP2001316736A (en) | Method for recovering silver | |
| CN111041207A (en) | Electrochemical gold leaching agent and method for recovering gold from waste gold-plated circuit board | |
| CN103572322A (en) | Method for recycling gold and copper from copper-containing oxidization gold ores | |
| US20150082943A1 (en) | Process for preparing a ferric nitrate reagent from copper raffinate solution and use of such reagent in the leaching and/or curing of copper substances | |
| CN208532949U (en) | A kind of rotation of anode is compeled to hit electrolysis unit | |
| CN107177865A (en) | Process for separating lead and bismuth from high-bismuth lead alloy | |
| Liang et al. | Electrolyte circulation: Metal recovery from waste printed circuit boards of mobile phones by alkaline slurry electrolysis | |
| JP2003247089A (en) | Method of recovering indium | |
| CN101864519A (en) | Method for selectively leaching and separating tin, lead and copper from waste circuit board | |
| CN108517410A (en) | A kind of method of metallic copper in hydrometallurgical recovery printed wiring board (PCB) | |
| CN110438337A (en) | A method of based on drum-type anode rotary electrolysis device recovery train sheetmetal | |
| CN115369255B (en) | Silver recovery process of electronic element | |
| CN108950218A (en) | A method of recycling gold, silver and copper from waste printed circuit board | |
| Bo et al. | Selective separation of copper and cadmium from zinc solutions by low current density electrolysis | |
| KR101844771B1 (en) | A method recovered of high purity copper and valuable metal from the crude copper | |
| KR101431532B1 (en) | Method for separating valuable metals from pb-free waste solder | |
| CN108070722A (en) | A kind of method that valuable metal is recycled in copper ashes of sinking from silver electrolysis mother liquor | |
| CN112410557A (en) | Environment-friendly acid-cyanide-free gold refining technology for waste circuit boards and circuit boards | |
| CN112921356B (en) | Method for recovering copper from waste printed circuit board | |
| CN113481371A (en) | Method for efficiently recovering antimony, bismuth, copper and silver from silver separating slag of lead anode slime |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |