CN109097593A - A method of it is recycled using persulfate-ammono-system silver-colored in waste old ceramics capacitor - Google Patents
A method of it is recycled using persulfate-ammono-system silver-colored in waste old ceramics capacitor Download PDFInfo
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- CN109097593A CN109097593A CN201811218716.3A CN201811218716A CN109097593A CN 109097593 A CN109097593 A CN 109097593A CN 201811218716 A CN201811218716 A CN 201811218716A CN 109097593 A CN109097593 A CN 109097593A
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- silver
- persulfate
- concentration
- colored
- waste old
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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
- 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
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- 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
Abstract
Method silver-colored in persulfate-ammono-system recycling waste old ceramics capacitor is utilized the invention discloses a kind of.The method of the present invention is the following steps are included: the first step, silver leaching: first by waste old ceramics capacitor ball milling or be chopped into average grain diameter be less than 0.2mm partial size particle, above-mentioned particle is added to hybrid reaction in persulfate-ammonia-aqueous slkali again, is then filtered, argentiferous filtrate is obtained；Second step, silver-colored reduction are extracted: being reduced directly with reducing agents such as hydrazine hydrates and extracted silver；Silver-colored purification: the concentrated base immersion of obtained crude product silver heat is removed dezincify, aluminium, tin and lead, then is impregnated with acidified ferric chloride solution and remove manganese, iron, copper and mickel, silver most can be obtained through drying afterwards by third step.Method of the invention can carry out high efficiente callback, simple possible, energy conservation and environmental protection to the noble silver in waste and old capacitor.
Description
Technical field
The present application relates to a kind of using method silver-colored in persulfate-ammono-system recycling waste old ceramics capacitor, belongs to
In environmental protection and technical field of resource recovery.
Background technique
General ceramic capacitor is a kind of using ceramic material as the capacitor of medium, and the two sides of ceramic matrix sprays silver layer,
It is subsequent to pass through low-temperature treatment, it is burnt into silver film and is made as pole plate.Its with small size, low ESR, it is low at
Originally, high reliability and high ripple current ability etc. a little, become extremely widespread in electric equipment products.
With the rapid development of electronic apparatus industry, electron wastes are largely generated, the processing of the component on wiring board
Become especially urgent and important.Containing precious metal palladium, gold, silver etc. in waste old ceramics capacitor, wherein the content of silver is about every thousand
Grams 1.4 grams.
Processing ceramic capacitor mainly recycles the silver in ceramic capacitor at present, however recycles and be related to nitric acid, hydrochloric acid mostly
Equal strong acid, treatment process can generate toxic harmful exhaust gas, cause environmental pollution, not meet energy-saving and environment-friendly requirement.
Summary of the invention
In view of the above technical problems, persulfate-ammonia is utilized the purpose of the present invention is to provide a kind of Novel pollution-free
System recycles method silver-colored in waste old ceramics capacitor.The method of the present invention simple possible, environmentally protective, energy high efficiente callback capacitor
In silver.
Technical solution of the present invention is specifically described as follows.
The present invention provide it is a kind of utilize method silver-colored in persulfate-ammono-system recycling waste old ceramics capacitor, it is specific to walk
It is rapid as follows:
(1) by way of ball milling or chopping, so that waste old ceramics capacitor is broken into the particle that average grain diameter is less than 0.125mm
Object；
(2) above-mentioned particulate matter is put into and is filled in the persulfate-ammonia-aqueous slkali reactor prepared, in 20-35 DEG C of temperature
Under degree, be stirred to react 45 ~ 60min, after reaction, filter residue and argentiferous mother liquor be obtained by filtration, at this time in argentiferous mother liquor include silver,
Copper, nickel, zinc, manganese, aluminium, lead, tin and iron ion；Wherein: the persulfate-ammonia-aqueous slkali is by persulfate, ammonium hydroxide, highly basic
It is formulated with water；The concentration of persulfate between 0.02 ~ 0.4mol/L, the concentration of ammonium hydroxide between 0.05 ~ 1.5mol/L,
The concentration of highly basic is between 0.05 ~ 0.5mol/L；
(3) argentiferous mother liquor is restored with reducing agent, until silver-colored all reduction, obtains crude product silver；
(4) obtained crude product silver is first impregnated with the concentrated base of heat to remove dezincify, aluminium, tin and lead, then with acidified iron chloride
Until solution is dipped to no longer dissolution, extra copper, nickel, manganese and iron are removed, is refiltered, filter residue is washed with dilute hydrochloric acid, is finally done
It is dry, fine silver is obtained, realizes recycling silver-colored in waste old ceramics capacitor.
In the present invention, in step (2), persulfate is any in potassium peroxydisulfate, sodium peroxydisulfate or ammonium persulfate.
In the present invention, in step (2), highly basic is any in potassium hydroxide or sodium hydroxide.
In the present invention, in step (2), particulate matter and persulfate-ammonia-aqueous slkali solid-liquid mass ratio are in 1:120 ~ 1:
Between 50g/ml, the concentration of persulfate is between 0.14 ~ 0.4mol/L, and the concentration of ammonium hydroxide is between 1.0 ~ 1.5mol/L, by force
The concentration of alkali is between 0.2 ~ 0.5mol/L.
In the present invention, in step (3), the molar ratio of anion is between 10:1 ~ 50:1 in reducing agent and argentiferous mother liquor, also
Former agent is hydrazine hydrate, and the reduction reaction time is between 30min ~ 50min.
In the present invention, in step (4), hot concentrated base is temperature between 35 ~ 80 DEG C, hydrogen of the concentration not less than 2.5mol/L
Sodium oxide molybdena or potassium hydroxide solution；Acid is hydrochloric acid, and the hydrionic concentration in acidified ferric chloride solution is greater than
The concentration of 0.01mol/L, i.e. pH < 2, iron chloride are not less than 0.01mol/L.
Compared to the prior art, the beneficial effects of the present invention are:
The present invention can carry out high efficiente callback to the silver in recycling waste old ceramics capacitor, realize the resource of waste old ceramics capacitor
Change, increases the recycling of resource, avoid waste；Step simple possible, it is low in cost；Process does not generate venomous injurant
Matter, it is environmentally protective, widely it can promote and apply.
Detailed description of the invention
Fig. 1 is the process flow chart of method silver-colored in recycling waste old ceramics capacitor of the invention.
Specific embodiment
The present patent application technical solution is specifically described below in conjunction with drawings and examples, in order to Gong Zhonggeng
The good understanding contents of the present invention, rather than the limitation to the technology contents, with the method for the invention or approximate principle,
To the transformation that the present patent application the method carries out, replaced in all steps including the same or similar reactant of character of use
Respective reaction object, it is available without creative labor that the change to reaction condition is all those skilled in the art, therefore all
Within the present patent application technical solution claimed.
In embodiment, silver-colored leaching rate indicates the silver content in argentiferous filtrate in quality/particle of silver ion；The precipitating of silver
Rate indicates the gross mass of the silver ion in the silver ion quality/argentiferous filtrate being reduced；The purity expression of silver finally obtains silver
Through resolution, measurement, calculating silver quality/finally obtain silver quality；The rate of recovery of silver indicates leaching rate × silver of silver
Rate of deposition × silver purity.
Embodiment 1
As shown in Figure 1, recycling the silver in waste old ceramics capacitor with the following method, its step are as follows:
1. break process: by way of ball mill dry ball milling, being less than so that waste old ceramics capacitor is broken into average grain diameter
The particle of 0.1mm；
2. above-mentioned particle 1g addition is filled in 100ml potassium peroxydisulfate-ammonia-sodium hydroxide mixed liquor reactor；Mixed liquor
In, potassium peroxydisulfate concentration is 0.14mol/L, ammonia concn 1.2mol/L, naoh concentration 0.5mol/L；At 25 DEG C
Under the conditions of, it is stirred to react 50min, the ammonia of generation is absorbed with NaOH, can be utilized again；Be obtained by filtration after reaction filter residue and
Argentiferous filtrate, wherein the leaching rate of silver is 90.8%；
3. by leachate hydrazine hydrate reduction: 50wt% hydrazine hydrate 0.5ml being added into above-mentioned leachate, is 30 DEG C in temperature, turns
Under conditions of speed is 700rpm, it is stirred to react 30min, after reaction, filtering obtains crude product silver；Silver rate of deposition be
99.8%, the rate of deposition of copper is 71.6%, also there is other precipitated metals；
4. obtained impure silver is gone out dezincify, aluminium, tin with the hot soaking with sodium hydroxide that temperature is 50 DEG C, concentration is 2.5mol/L
And lead, filtering remove until the ferric chloride solution for the 0.01mol/L that the hydrochloric acid that filter residue is 1.5 with pH is acidified is dipped to no longer dissolution
Extra copper, nickel, manganese and iron are removed, filter residue is washed with 1wt% dilute hydrochloric acid, then through drying, obtains silver, and obtained galactic longitude resolution is surveyed
ICP, calculated purity, purity 99.3%.Realize the recycling of silver, the silver-colored rate of recovery is 89.96%.
Embodiment 2
The silver in waste old ceramics capacitor is recycled with the following method, and its step are as follows:
1. break process: in such a way that ball mill crushes, being less than so that waste old ceramics capacitor is crushed to average grain diameter
The particle of 0.125mm；
2. being filled in potassium peroxydisulfate-ammonia-sodium hydroxide mixed liquor reactor that 100ml is prepared in above-mentioned particle 1g addition；
In mixed liquor, potassium peroxydisulfate concentration is 0.08mol/L, ammonia concn 1.2mol/L, naoh concentration 0.5mol/L；?
Under conditions of 25 DEG C, it is stirred to react 50min, the ammonia of generation is absorbed with NaOH, can be utilized again；It is obtained by filtration after reaction
Filter residue and argentiferous filtrate, in which: silver-colored leaching rate is 71.8%；
3. by leachate hydrazine hydrate reduction: 50wt% hydrazine hydrate 0.5ml is added into above-mentioned leachate, is 30 DEG C in temperature,
Under conditions of revolving speed is 700rpm, it is stirred to react 30min, after reaction, filtering obtains crude product silver；The rate of deposition of silver
99.8%, the rate of deposition of copper is 58.6% and other precipitated metals；
4. with temperature be 50 DEG C by obtained crude product silver, the hot soaking with sodium hydroxide that concentration is 3mol/L go out dezincify, aluminium, tin and
Lead, filtering remove more until the ferric chloride solution for the 0.02mol/L that the hydrochloric acid that filter residue is 1 with pH is acidified is dipped to no longer dissolution
Remaining copper, nickel, manganese and iron, filter residue are washed with 1wt% dilute hydrochloric acid, then through drying, obtain silver, and ICP, meter are surveyed in obtained galactic longitude resolution
Calculate purity, purity 99.3%.Realize the recycling of silver, the rate of recovery 71.2% of final silver.
Embodiment 3
As shown in Figure 1, recycling the silver in waste old ceramics capacitor with the following method, its step are as follows:
1. break process: by way of chopping, so that waste old ceramics capacitor is crushed to the average grain diameter less than 0.125mm；
2. above-mentioned particle 1g addition is filled in sodium peroxydisulfate-ammonia-sodium hydroxide mixed liquor reactor that 100ml is prepared；It is mixed
It closes in liquid, sodium peroxydisulfate concentration is 0.26mol/L, ammonia concn 1.2mol/L, naoh concentration 0.5mol/L；25
Under conditions of DEG C, it is stirred to react 50min, the ammonia of generation is absorbed with NaOH, can be utilized again；Filter is obtained by filtration after reaction
Slag and argentiferous filtrate, silver-colored leaching rate are 73.5%；
3. by leachate hydrazine hydrate reduction: hydrazine hydrate 0.5ml being added into above-mentioned leachate, is 30 DEG C in temperature, revolving speed is
Under conditions of 700rpm, it is stirred to react 30min, after reaction, filtering obtains crude product silver.Rate of deposition 99.8%, the copper of silver
Rate of deposition is 60.4% and other precipitated metals；
4. with temperature be 50 DEG C by obtained crude product silver, the hot soaking with sodium hydroxide that concentration is 4mol/L go out dezincify, aluminium, tin and
Lead, filtering remove more until the ferric chloride solution for the 0.02mol/L that the hydrochloric acid that filter residue is 1 with pH is acidified is dipped to no longer dissolution
Remaining copper, nickel, manganese and iron, filter residue are washed with 1wt% dilute hydrochloric acid, then through drying, obtain silver, and ICP, meter are surveyed in obtained galactic longitude resolution
Calculate purity, purity 99.3%.The rate of recovery 72.8% of final silver.
Embodiment 4
As shown in Figure 1, recycling the silver in waste old ceramics capacitor with the following method, its step are as follows:
1. break process: by way of chopping, so that waste old ceramics capacitor is crushed to the particle that average grain diameter is 0.1mm；
2. being filled in ammonium persulfate-ammonia-sodium hydroxide mixed liquor reactor that 100ml is prepared in above-mentioned particle 1g addition；
In mixed liquor: ammonium persulfate concentrations 0.26mol/L, ammonia concn 1.2mol/L, naoh concentration 0.5mol/L；?
Under conditions of 25 DEG C, it is stirred to react 50min, the ammonia of generation is absorbed with NaOH, can be utilized again；After reaction, it filters
To filter residue and argentiferous filtrate, silver-colored leaching rate is 72.1%；
3. by leachate hydrazine hydrate reduction: hydrazine hydrate 0.5ml being added into above-mentioned leachate, temperature is 30 DEG C, and revolving speed is
Under conditions of 700rpm, it is stirred to react 30min, after reaction, filtering obtains crude product silver.Rate of deposition 99.8%, the copper of silver
Rate of deposition is 59.6% and other precipitated metals；
4. by obtained impure silver with the hot soaking with sodium hydroxide that temperature is 80 DEG C, concentration is 2.5mol/L go out dezincify, aluminium,
Tin and lead, filtering remove until the ferric chloride solution for the 0.1mol/L that the hydrochloric acid that filter residue is 1 with pH is acidified is dipped to no longer dissolution
Extra copper, nickel, manganese and iron are removed, filter residue is washed with 1wt% dilute hydrochloric acid, then through drying, obtains silver, and obtained galactic longitude resolution is surveyed
ICP, calculated purity, purity 99.3%.Realize the recycling of silver, the rate of recovery 71.5% of final silver.
Claims (6)
1. a kind of utilize method silver-colored in persulfate-ammono-system recycling waste old ceramics capacitor, which is characterized in that specific steps
It is as follows:
(1) by way of ball milling or chopping, so that waste old ceramics capacitor is broken into the particle that average grain diameter is less than 0.125mm
Object；
(2) above-mentioned particulate matter is put into and is filled in the persulfate-ammonia-aqueous slkali reactor prepared, in 20-35 DEG C of temperature
Under degree, be stirred to react 45 ~ 60min, after reaction, filter residue and argentiferous mother liquor be obtained by filtration, at this time in argentiferous mother liquor include silver,
Copper, nickel, zinc, manganese, aluminium, lead, tin and iron ion；Wherein: the persulfate-ammonia-aqueous slkali is by persulfate, ammonium hydroxide, highly basic
It is formulated with water；The concentration of persulfate between 0.02 ~ 0.4mol/L, the concentration of ammonium hydroxide between 0.05 ~ 1.5mol/L,
The concentration of highly basic is between 0.05 ~ 0.5mol/L；
(3) argentiferous mother liquor is restored with reducing agent, until silver-colored all reduction, obtains crude product silver；
(4) obtained crude product silver is first impregnated with the concentrated base of heat to remove dezincify, aluminium, tin and lead, then with acidified iron chloride
Until solution is dipped to no longer dissolution, extra copper, nickel, manganese and iron are removed, is refiltered, filter residue is washed with dilute hydrochloric acid, is finally done
It is dry, fine silver is obtained, realizes recycling silver-colored in waste old ceramics capacitor.
2. according to the method described in claim 1, it is characterized by: persulfate is selected from potassium peroxydisulfate, over cure in step (2)
It is any in sour sodium or ammonium persulfate.
3. according to the method described in claim 1, it is characterized by: highly basic is selected from potassium hydroxide or sodium hydroxide in step (2)
In it is any.
4. according to the method described in claim 1, it is characterized by: in step (2), particulate matter and persulfate-ammonia-aqueous slkali
Solid-liquid mass ratio between 1:120 ~ 1:50g/ml, the concentration of persulfate is between 0.14 ~ 0.4mol/L, the concentration of ammonium hydroxide
Between 1.0 ~ 1.5mol/L, the concentration of highly basic is between 0.2 ~ 0.5mol/L.
5. according to the method described in claim 1, it is characterized by: in step (3), anion in reducing agent and argentiferous mother liquor
Molar ratio is between 10:1 ~ 50:1, and reducing agent is hydrazine hydrate, and the reduction reaction time is between 30min ~ 50min.
6. according to the method described in claim 1, it is characterized by: in step (4), hot concentrated base be temperature 35 ~ 80 DEG C it
Between, concentration be not less than 2.5mol/L sodium hydroxide or potassium hydroxide solution；Acid is hydrochloric acid, in acidified ferric chloride solution
Hydrionic concentration be greater than 0.01mol/L, i.e. the concentration of pH < 2, iron chloride is not less than 0.01mol/L.
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|---|---|---|---|
| CN201811218716.3A CN109097593A (en) | 2018-10-19 | 2018-10-19 | A method of it is recycled using persulfate-ammono-system silver-colored in waste old ceramics capacitor |
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| CN201811218716.3A CN109097593A (en) | 2018-10-19 | 2018-10-19 | A method of it is recycled using persulfate-ammono-system silver-colored in waste old ceramics capacitor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129569A (en) * | 2019-05-27 | 2019-08-16 | 上海第二工业大学 | A kind of method of a variety of valuable metals in hydrometallurgic recovery waste old ceramics capacitor |
| CN115015466A (en) * | 2022-06-10 | 2022-09-06 | 温州伟达贵金属粉体材料有限公司 | Silver content detection method for silver waste containing chloride ions |
| CN117021420A (en) * | 2023-10-08 | 2023-11-10 | 国能龙源环保有限公司 | Method for recycling bassa wood from waste wind power blades |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009113842A1 (en) * | 2008-03-14 | 2009-09-17 | Universidad Autónoma Metropolitana | Process for leaching and recovering silver and gold with ammoniacal thiosulphate solutions of copper |
| CN101575715A (en) * | 2009-06-22 | 2009-11-11 | 中南大学 | Method for extracting valuable metals from electronic waste |
| CN102936657A (en) * | 2011-08-15 | 2013-02-20 | 江西格林美资源循环有限公司 | Method for metal recovery by ceramic capacitor |
-
2018
- 2018-10-19 CN CN201811218716.3A patent/CN109097593A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009113842A1 (en) * | 2008-03-14 | 2009-09-17 | Universidad Autónoma Metropolitana | Process for leaching and recovering silver and gold with ammoniacal thiosulphate solutions of copper |
| CN101575715A (en) * | 2009-06-22 | 2009-11-11 | 中南大学 | Method for extracting valuable metals from electronic waste |
| CN102936657A (en) * | 2011-08-15 | 2013-02-20 | 江西格林美资源循环有限公司 | Method for metal recovery by ceramic capacitor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129569A (en) * | 2019-05-27 | 2019-08-16 | 上海第二工业大学 | A kind of method of a variety of valuable metals in hydrometallurgic recovery waste old ceramics capacitor |
| CN115015466A (en) * | 2022-06-10 | 2022-09-06 | 温州伟达贵金属粉体材料有限公司 | Silver content detection method for silver waste containing chloride ions |
| CN117021420A (en) * | 2023-10-08 | 2023-11-10 | 国能龙源环保有限公司 | Method for recycling bassa wood from waste wind power blades |
| CN117021420B (en) * | 2023-10-08 | 2024-02-02 | 国能龙源环保有限公司 | Method for recycling bassa wood from waste wind power blades |
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