CN107974564A - A kind of method that super fine silver powder is prepared using waste photographic film - Google Patents
A kind of method that super fine silver powder is prepared using waste photographic film Download PDFInfo
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- CN107974564A CN107974564A CN201711175892.9A CN201711175892A CN107974564A CN 107974564 A CN107974564 A CN 107974564A CN 201711175892 A CN201711175892 A CN 201711175892A CN 107974564 A CN107974564 A CN 107974564A
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- silver
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to Rare Metals Materials and field of engineering technology, and in particular to a kind of method that super fine silver powder is prepared using waste photographic film.A kind of method that super fine silver powder is prepared using waste photographic film：Comprise the following steps：Thick silver salt silver is first prepared with waste films, then thick silver salt is put into graphite crucible, adds suitable sodium carbonate and boric acid, in 1100 DEG C of meltings, the sodium chloride of suspension is discarded, the high-purity silver that content is more than 99.5% is dried to obtain after cooling.Recycle high-purity silver that super fine silver powder is prepared.The present invention, which can be leached using nitric acid dissolution method as raw material using waste films and content is prepared, is higher than 99.5% high-purity silver, again using ascorbic acid as reducing agent, use macromolecular (PVP) surfactant (TEA) compound system that the controllable spherical super fine silver powder of epigranular, regular shape, good dispersion, granularity can be prepared for dispersant.
Description
Technical field
The present invention relates to Rare Metals Materials and field of engineering technology, and in particular to one kind is prepared super using waste photographic film
The method of thin silver powder.
Background technology
Super fine silver powder is a kind of emerging functional material, have granularity is small, specific surface area is big, fusing point is low, sintering character is good,
Active big, the advantages that catalytic activity is good, while it is good to also retains the good conductivity of metallic silver, anti-microbial property, electroforming silver color of light
The features such as bright, be widely used as catalyst material, antistatic material, low temperature superconducting material, electric slurry, biology sensor material with
And functional material of antibacterial, deodorization and absorption some ultra violet rays etc..The preparation method of super fine silver powder can be divided into Physical and chemistry
Reduction method, chemical reduction method has the particle diameter and shape that powder manufacturing apparatus was simple and convenient to operate, was easy to control powder compared with Physical
Shape, production cost are low, are easily achieved the advantages that industrialization, thus prepare the report of super fine silver powder very using chemical reduction process
It is more, its principle be all using reducing agent by chemical reduction reaction silver from the solution of its salt or complex with the shape of powder
Formula is deposited.Since superfine powder has, particle diameter is small, specific surface area is big, surface residual electric charge is more, surface tension is big, unit ratio
The high property of table energy so that single ultrafine particle thermodynamically often plays pendulum, spontaneous mutual between ultrafine particle
Attraction, cohesion, agglomerate easily occur to prepare in particle and last handling process, therefore chemical reduction reaction need to be under the protection of dispersant
Carry out.But using macromolecular-face activating agent compound system for dispersant to prepare super fine silver powder, there is not been reported.
The content of the invention
A kind of the present invention is directed to propose method that super fine silver powder is prepared using waste photographic film.
Technical program of the present invention lies in：
A kind of method that super fine silver powder is prepared using waste photographic film：Comprise the following steps：
Step 1：The preparation of raw material：
Material：Waste films；
Reagent：Nitric acid, sodium chloride, sodium hydroxide, aluminium chloride, sodium carbonate, borax, ammonium hydroxide, ascorbic acid, polyvinyl pyrrolidone
(PVP), cetyl trimethylammonium bromide (CTAB), cationic polyacrylamide (PAM), lauryl sodium sulfate (SDS)；Three
Monoethanolamine (TEA)；
Instrument：Thermostatic water-circulator bath, acidometer, van-type resistance furnace, magnetic stirring apparatus, supercentrifuge, vacuum drying chamber, X are penetrated
Line diffractometer, scanning electron microscope；
Step 2：Waste films prepare silver：
（1）By the certain density HN0 of 100 mL3Solution is added in 250 mL three-necked flasks, opens stirring, and input 6g is shredded into
The waste films of fritter substrate, water bath with thermostatic control are heated to certain temperature, stirring leaching silver, and reaction terminates to leach again after taking out substrate,
Silver paste raw material is obtained to leaching liquid filtering, washing；
（2）Due to the gelatin containing waste films dissolving in silver paste material liquid, NaCl solution is added, it is 3.4 to adjust pH value with NaOH
~4.0, A1Cl is added, flocculant, makes particulate silver salt be condensed into AgCl sediments and stand 10h, and sediment filtering washing is dry
It is dry to obtain thick silver salt；
（3）Thick silver salt is put into graphite crucible, adds suitable sodium carbonate and boric acid, in 1100 DEG C of meltings, discards suspension
Sodium chloride, is dried to obtain the high-purity silver that content is more than 99.5% after cooling；
Step 3：It is prepared by super fine silver powder：
（1）Weigh high-purity recycling silver to be dissolved in nitric acid, add deionized water to be made into the silver nitrate solution of 0.5mol/L；
（2）Take silver nitrate solution to add deionized water, ammonium hydroxide to be prepared into real silver ammino solution, add macromolecular polyvinyl pyrrolidone
(PVP)；Take ascorbic acid and deionized water wiring solution-forming and add surfactant；
（3）The silver ammino solution of prepared addition macromolecular polyvinyl pyrrolidone is added drop-wise under the conditions of magnetic agitation and is furnished with
In the ascorbic acid solution of surfactant, reduction reaction terminates to stand 2 h, centrifuges, sediment deionized water and nothing
After water-ethanol washing, super fine silver powder is obtained after being placed in vacuum drying chamber drying.
Preferably, it is described recycled from waste films silver leaching condition be：Concentration of nitric acid is 1.6 molL-1, leaching
Temperature is 50 DEG C, leaching time 10min, and leaching number is 3 times.
Or preferably, 0.02 molL of silver nitrate concentration-1, m (PVP)/m (AgN03)>4.5, m (TEA)/m
(AgN03)=1, pH value 8.
The technical effects of the invention are that：
The present invention, which can be leached using nitric acid dissolution method as raw material using waste films and content is prepared, is higher than 99.5% high-purity silver,
Again using ascorbic acid as reducing agent, macromolecular (PVP)-surfactant (TEA) compound system is used to be prepared into for dispersant
The spherical super fine silver powder controllable to epigranular, regular shape, good dispersion, granularity.
Embodiment
A kind of method that super fine silver powder is prepared using waste photographic film：Comprise the following steps：
Step 1：The preparation of raw material：
Material：Waste films；
Reagent：Nitric acid, sodium chloride, sodium hydroxide, aluminium chloride, sodium carbonate, borax, ammonium hydroxide, ascorbic acid, polyvinyl pyrrolidone
(PVP), cetyl trimethylammonium bromide (CTAB), cationic polyacrylamide (PAM), lauryl sodium sulfate (SDS)；Three
Monoethanolamine (TEA)；
Instrument：Thermostatic water-circulator bath, acidometer, van-type resistance furnace, magnetic stirring apparatus, supercentrifuge, vacuum drying chamber, X are penetrated
Line diffractometer, scanning electron microscope；
Step 2：Waste films prepare silver：
（1）By the certain density HN0 of 100 mL3Solution is added in 250 mL three-necked flasks, opens stirring, and input 6g is shredded into
The waste films of fritter substrate, water bath with thermostatic control are heated to certain temperature, stirring leaching silver, and reaction terminates to leach again after taking out substrate,
Silver paste raw material is obtained to leaching liquid filtering, washing；
（2）Due to the gelatin containing waste films dissolving in silver paste material liquid, NaCl solution is added, it is 3.4 to adjust pH value with NaOH
~4.0, A1Cl is added, flocculant, makes particulate silver salt be condensed into AgCl sediments and stand 10h, and sediment filtering washing is dry
It is dry to obtain thick silver salt；
（3）Thick silver salt is put into graphite crucible, adds suitable sodium carbonate and boric acid, in 1100 DEG C of meltings, discards suspension
Sodium chloride, is dried to obtain the high-purity silver that content is more than 99.5% after cooling；
Step 3：It is prepared by super fine silver powder：
（1）Weigh high-purity recycling silver to be dissolved in nitric acid, add deionized water to be made into the silver nitrate solution of 0.5mol/L；
（2）Take silver nitrate solution to add deionized water, ammonium hydroxide to be prepared into real silver ammino solution, add macromolecular polyvinyl pyrrolidone
(PVP)；Take ascorbic acid and deionized water wiring solution-forming and add surfactant；
（3）The silver ammino solution of prepared addition macromolecular polyvinyl pyrrolidone is added drop-wise under the conditions of magnetic agitation and is furnished with
In the ascorbic acid solution of surfactant, reduction reaction terminates to stand 2 h, centrifuges, sediment deionized water and nothing
After water-ethanol washing, super fine silver powder is obtained after being placed in vacuum drying chamber drying.
Wherein, silver-colored leaching condition is recycled from waste films is：Concentration of nitric acid is 1.6 molL-1, leaching temperature 50
DEG C, leaching time 10min, leaching number is 3 times.0.02 molL of silver nitrate concentration-1, m (PVP)/m (AgN03)>4.5, m
(TEA)/m (AgN03)=1, pH value 8.
Claims (3)
- A kind of 1. method that super fine silver powder is prepared using waste photographic film, it is characterised in that：Comprise the following steps：Step 1：The preparation of raw material：Material：Waste films；Reagent：Nitric acid, sodium chloride, sodium hydroxide, aluminium chloride, sodium carbonate, borax, ammonium hydroxide, ascorbic acid, polyvinyl pyrrolidone (PVP), cetyl trimethylammonium bromide (CTAB), cationic polyacrylamide (PAM), lauryl sodium sulfate (SDS)；Three Monoethanolamine (TEA)；Instrument：Thermostatic water-circulator bath, acidometer, van-type resistance furnace, magnetic stirring apparatus, supercentrifuge, vacuum drying chamber, X are penetrated Line diffractometer, scanning electron microscope；Step 2：Waste films prepare silver：（1）By the certain density HN0 of 100 mL3Solution is added in 250 mL three-necked flasks, opens stirring, and input 6g is shredded into The waste films of fritter substrate, water bath with thermostatic control are heated to certain temperature, stirring leaching silver, and reaction terminates to leach again after taking out substrate, Silver paste raw material is obtained to leaching liquid filtering, washing；（2）Due to the gelatin containing waste films dissolving in silver paste material liquid, NaCl solution is added, it is 3.4 to adjust pH value with NaOH ~4.0, A1Cl is added, flocculant, makes particulate silver salt be condensed into AgCl sediments and stand 10h, and sediment filtering washing is dry It is dry to obtain thick silver salt；（3）Thick silver salt is put into graphite crucible, adds suitable sodium carbonate and boric acid, in 1100 DEG C of meltings, discards suspension Sodium chloride, is dried to obtain the high-purity silver that content is more than 99.5% after cooling；Step 3：It is prepared by super fine silver powder：（1）Weigh high-purity recycling silver to be dissolved in nitric acid, add deionized water to be made into the silver nitrate solution of 0.5mol/L；（2）Take silver nitrate solution to add deionized water, ammonium hydroxide to be prepared into real silver ammino solution, add macromolecular polyvinyl pyrrolidone (PVP)；Take ascorbic acid and deionized water wiring solution-forming and add surfactant；（3）The silver ammino solution of prepared addition macromolecular polyvinyl pyrrolidone is added drop-wise under the conditions of magnetic agitation and is furnished with In the ascorbic acid solution of surfactant, reduction reaction terminates to stand 2 h, centrifuges, sediment deionized water and nothing After water-ethanol washing, super fine silver powder is obtained after being placed in vacuum drying chamber drying.
- 2. such as a kind of method that super fine silver powder is prepared using waste photographic film of claim 1, it is characterised in that：The slave scrap rubber Silver-colored leaching condition is recycled in piece is：Concentration of nitric acid is 1.6 molL-1, leaching temperature is 50 DEG C, leaching time 10min, It is 3 times to leach number.
- 3. such as a kind of method that super fine silver powder is prepared using waste photographic film of claim 1, it is characterised in that：The silver nitrate 0.02 molL of concentration-1, m (PVP)/m (AgN03)>4.5, m (TEA)/m (AgN03)=1, pH value 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711175892.9A CN107974564A (en) | 2017-11-22 | 2017-11-22 | A kind of method that super fine silver powder is prepared using waste photographic film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711175892.9A CN107974564A (en) | 2017-11-22 | 2017-11-22 | A kind of method that super fine silver powder is prepared using waste photographic film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107974564A true CN107974564A (en) | 2018-05-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711175892.9A Withdrawn CN107974564A (en) | 2017-11-22 | 2017-11-22 | A kind of method that super fine silver powder is prepared using waste photographic film |
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| CN (1) | CN107974564A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110466090A (en) * | 2019-09-10 | 2019-11-19 | 珠海市安能环保科技有限公司 | A method of recycling silver and PET film from HW16 waste photographic film |
-
2017
- 2017-11-22 CN CN201711175892.9A patent/CN107974564A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110466090A (en) * | 2019-09-10 | 2019-11-19 | 珠海市安能环保科技有限公司 | A method of recycling silver and PET film from HW16 waste photographic film |
| CN110466090B (en) * | 2019-09-10 | 2021-03-30 | 珠海市安能环保科技有限公司 | Method for recovering silver and PET (polyethylene terephthalate) film from HW16 waste photosensitive film |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180501 |
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| WW01 | Invention patent application withdrawn after publication |