CN106125498A - A kind of waste photographic film reclaims the method for silver and chip base - Google Patents
A kind of waste photographic film reclaims the method for silver and chip base Download PDFInfo
- Publication number
- CN106125498A CN106125498A CN201610747462.9A CN201610747462A CN106125498A CN 106125498 A CN106125498 A CN 106125498A CN 201610747462 A CN201610747462 A CN 201610747462A CN 106125498 A CN106125498 A CN 106125498A
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- solution
- chip base
- silver
- thin film
- described step
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C11/00—Auxiliary processes in photography
- G03C11/24—Removing emulsion from waste photographic material; Recovery of photosensitive or other substances
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Abstract
A kind of waste photographic film reclaims the method for silver and chip base, comprises the following steps: waste photographic film is added in sheet aqueous slkali by (1), is passed through ozone, isolates chip base, thin film and solution 1. after heated and stirred;Chip base and thin film are washed through hot water respectively, and 2. the solution obtained prepared with solution 3. return piece aqueous slkali;(2) chip base after washing adds additive dichloromethane and ethanol, again makes the chip base of sensitive material;(3) obtaining solution 4. after 1. solution add sulfur acid for adjusting pH, by solution 4. after flocculant settles, isolated Argent grain and solution are 5.;(4) highly purified silver is obtained after Argent grain being added auxiliary agent high melt;Solution 5. add sheet alkali and Posterior circle repeatedly after, can qualified discharge after biochemical treatment.Present invention achieves chip base and thin film, the separation of silver, meet the regeneration cycle of chip base, the recovery of silver and wastewater biodegradability, be that a kind of technique is simple, pollution-free, it is simple to the processing method of popularization.
Description
Technical field
The present invention relates to waste photographic film processing technology field, particularly relate to a kind of recovery silver and sheet from waste photographic film
The processing method of base.
Background technology
The sensitive material manufacturing enterprise of China can produce substantial amounts of film every year, becomes after industrial application through medical
Waste films, containing silver on these waste films, chip base is polyethylene terephthalate, all has the highest recycling valency
Value.Silver is noble metal, is non-renewable resources, expensive, is widely used in the industries such as electronics, chemical industry and sensitive material, chip base
Can again raw material as various sensitive material chip base or other goods use after recovered.In terms of environmental pollution, due to silver
Ion pair humans and animals has the strongest toxicity, also must be considered that the removing of silver as environmental protection treatment and is reclaimed.
At present, the method reclaiming silver from waste photographic film mainly has burning method, chemical method and bioanalysis.Burning method is to silver
The response rate the highest, and the flue gas produced pollutes the environment, the chip base of heavy damage simultaneously;Bioanalysis mainly uses protease,
Though this method environmental pollution is little, but process conditions are harsh, and operating difficulties needs special equipment, it is difficult to industrialization, currently mainly uses
Or chemical method, is most widely used that nitric acid dissolution method, but this method process has NO_x formation, the waste water of generation is because of salt
High condition is divided to constrain biochemical treatment.
Summary of the invention
The problems referred to above existed for prior art, the applicant provides a kind of waste photographic film and reclaims silver and chip base
Method.Present invention achieves chip base and thin film, the separation of silver, meeting the regeneration cycle of chip base, the recovery of silver and waste water can give birth to
The property changed, is that a kind of technique is simple, pollution-free, it is simple to the processing method of popularization.
Technical scheme is as follows:
A kind of waste photographic film reclaims the method for silver and chip base, comprises the following steps:
(1) waste photographic film is added in sheet aqueous slkali, then pass to ozone, after heated stirring, isolate chip base, thin
Film and solution are 1.;Chip base and thin film are washed through hot water respectively, and 2. the solution obtained prepared with solution 3. return piece aqueous slkali;
(2) chip base after the washing that step (1) obtains adds additive dichloromethane and ethanol, again makes photosensitive material
The chip base of material;
(3) 4. the solution obtained to step (1) obtain solution after 1. adding sulfur acid for adjusting pH, is 4. sunk through flocculant by solution
After fall, isolated Argent grain and solution are 5.;
(4) highly purified silver is obtained after the Argent grain obtained in step (3) being added auxiliary agent high melt;5. solution added
Sheet alkali and Posterior circle repeatedly after, can qualified discharge after biochemical treatment.
In described step (1), sheet alkali concn is 0.1~0.5wt%, is passed through ozone flow 0.9m under agitating heating3/ h,
Time 3~5h, heating-up temperature is 70~90 DEG C.In described step (1), the solid-to-liquid ratio of chip base and thin film and hot water is 1:2~3,
Hot water temperature is 60~80 DEG C.
In described step (2), the mass ratio of chip base, dichloromethane and ethanol is 1:0.1~0.3:0.01~0.05.
In described step (3), adding sulfur acid for adjusting pH is 6~8, and the concentration of flocculant is 0.5wt%, and addition is solution
4. the 0.5~2% of volume, the sedimentation time 12~24h.
In described step (4), described high temperature auxiliary agent is sodium carbonate with Borax according to mass ratio is 2.5~3:1 to mix
The mixed flux obtained, the consumption of described mixed flux is before melting the 4~6wt% of Argent grain, smelting temperature be 1000~
1200 DEG C, smelting time is 2~3h.
In described step (4), 5. solution circulate 2~3 times, adds the 0.1 of solution 5. quality~the sheet alkali of 0.3% every time.
Useful the having the technical effect that of the present invention
1, present invention achieves silver and the recovery of chip base in waste photographic film, solve the isolation technics of thin film and chip base;
2, the present invention does not destroy chip base, it is achieved that the recyclable resources of chip base;
3, present invention achieves the recycling of water, be substantially reduced the generation of waste water, waste water can carry out biochemical treatment simultaneously,
Qualified discharge;
4, present invention process is simple to operate, low cost, non-secondary pollution.
Accompanying drawing explanation
Fig. 1 is the technological process signal of the processing method reclaiming silver and chip base from waste photographic film provided by the present invention
Figure.
Detailed description of the invention
Below in conjunction with the accompanying drawings 1 and embodiment, the present invention is specifically described.
Embodiment 1
Take the waste photographic film 200kg that certain factory produces, join in 0.1wt% sheet aqueous slkali, open steam, stir at 70 DEG C
Mix down, ozone flow 0.9m3/ h is passed through 3h, and the thin film sloughed is isolated on upper strata, and then 1. blowing filters out chip base and solution;Thin
Film and chip base add 60 DEG C of hot washes according to solid-to-liquid ratio 1:2, and 2. and 3. aqueous solution collects the preparation for sheet aqueous slkali;Cleaning
Chip base enters other workshop, is 1:0.1:0.01 according to the mass ratio of chip base, dichloromethane and ethanol, is re-prepared as photosensitive material
The chip base (light sensitivitys >=12, contrast factor >=3) of material;1. solution be adjusted to pH=6 by sulphuric acid, adds solution 1. volume
0.5%, after concentration is 0.5wt% flocculation flocculating sedimentation 12h, filter pressing separation desilver granule and solution are 5.;By Argent grain before melting
4wt% amount add sodium carbonate: the mixed flux of Borax mass ratio 2.5:1, at 1000 DEG C of melting 2h, purity 98% can be obtained
Silver, silver raising recovery rate 85%;Solution is added after 0.1% alkali circulates 2 silver-colored laggard biochemical treatments of recovery the most again and is entered at sewage
Reason factory.
Embodiment 2
Take the waste photographic film 300kg that certain factory produces, join in 0.3wt% sheet aqueous slkali, open steam, stir at 80 DEG C
Mix down, ozone flow 0.9m3/ h is passed through 4h, and the thin film sloughed is isolated on upper strata, and then 1. blowing filters out chip base and solution;Thin
Film and chip base add 70 DEG C of hot washes according to solid-to-liquid ratio 1:2, and 2. and 3. aqueous solution collects the preparation for sheet aqueous slkali;Cleaning
Chip base enters other workshop, is 1:0.2:0.03 according to the mass ratio of chip base, dichloromethane and ethanol, is re-prepared as photosensitive material
The chip base (light sensitivitys >=12, contrast factor >=3) of material;1. solution be adjusted to pH=7 by sulphuric acid, adds solution 1. volume
0.15%, after concentration is 0.5wt% flocculation flocculating sedimentation 18h, filter pressing separation desilver granule and solution are 5.;By Argent grain before melting
5wt% amount add sodium carbonate: the mixed flux of Borax mass ratio 3:1, at 1100 DEG C of melting 2h, purity 99% can be obtained
Silver, silver raising recovery rate 88%;Solution is added after 0.2% alkali circulates 3 silver-colored laggard biochemical treatments of recovery the most again and is entered sewage disposal
Factory.
Embodiment 3
Take the waste photographic film 500kg that certain factory produces, join in 0.5wt% sheet aqueous slkali, open steam, stir at 90 DEG C
Mix down, ozone flow 0.9m3/ h is passed through 5h, and the thin film sloughed is isolated on upper strata, and then 1. blowing filters out chip base and solution;Thin
Film and chip base add 80 DEG C of hot washes according to solid-to-liquid ratio 1:3, and 2. and 3. aqueous solution collects the preparation for sheet aqueous slkali;Cleaning
Chip base enters other workshop, is 1:0.3:0.05 according to the mass ratio of chip base, dichloromethane and ethanol, is re-prepared as photosensitive material
The chip base (light sensitivitys >=12, contrast factor >=3) of material;1. solution be adjusted to pH=8 by sulphuric acid, adds solution 1. volume
0.2%, after concentration is 0.5wt% flocculation flocculating sedimentation 24h, filter pressing separation desilver granule and solution are 5.;By Argent grain before melting
6wt% amount add sodium carbonate: the mixed flux of Borax mass ratio 3.5:1, at 1200 DEG C of melting 3h, purity can be obtained
The silver of 98.8%, silver raising recovery rate 90%;Solution is added after 0.3% alkali circulates 2 silver-colored laggard biochemical treatments of recovery the most again and is entered
Sewage treatment plant.
The above, be illustrative rather than determinate, be therefore not limited thereto in protection scope of the present invention,
Any those familiar with the art in the technical scope that the present invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.
Claims (7)
1. the method that a waste photographic film reclaims silver and chip base, it is characterised in that comprise the following steps:
(1) waste photographic film is added in sheet aqueous slkali, then passes to ozone, after heated stirring, isolate chip base, thin film and
Solution is 1.;Chip base and thin film are washed through hot water respectively, and 2. the solution obtained prepared with solution 3. return piece aqueous slkali;
(2) chip base after the washing that step (1) obtains adds additive dichloromethane and ethanol, again makes sensitive material
Chip base;
(3) 4. the solution obtained to step (1) obtain solution after 1. adding sulfur acid for adjusting pH, is 4. settled through flocculant by solution
After, isolated Argent grain and solution are 5.;
(4) highly purified silver is obtained after the Argent grain obtained in step (3) being added auxiliary agent high melt;5. solution add sheet alkali
With Posterior circle repeatedly after, can qualified discharge after biochemical treatment.
Method the most according to claim 1, it is characterised in that: in described step (1), sheet alkali concn be 0.1~
0.5wt%, is passed through ozone flow 0.9m under agitating heating3/ h, the time 3~5h, heating-up temperature is 70~90 DEG C.
Method the most according to claim 1, it is characterised in that: in described step (1), chip base and thin film and the solid-liquid of hot water
Ratio is 1:2~3, and hot water temperature is 60~80 DEG C.
Method the most according to claim 1, it is characterised in that: in described step (2), chip base, dichloromethane and ethanol
Mass ratio is 1:0.1~0.3:0.01~0.05.
Method the most according to claim 1, it is characterised in that: in described step (3), adding sulfur acid for adjusting pH is 6~8,
The concentration of flocculant is 0.5wt%, and addition is the 0.5~2% of solution 4. volume, the sedimentation time 12~24h.
Method the most according to claim 1, it is characterised in that: in described step (4), described high temperature auxiliary agent be sodium carbonate with
Borax is the 2.5~3:1 mixed fluxs carrying out being mixed to get according to mass ratio, and the consumption of described mixed flux is silver before melting
The 4~6wt% of grain, smelting temperature is 1000~1200 DEG C, and smelting time is 2~3h.
Method the most according to claim 1, it is characterised in that: in described step (4), 5. solution circulate 2~3 times, every time
Add the 0.1 of solution 5. quality~the sheet alkali of 0.3%.
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CN201610747462.9A CN106125498A (en) | 2016-08-27 | 2016-08-27 | A kind of waste photographic film reclaims the method for silver and chip base |
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CN201610747462.9A CN106125498A (en) | 2016-08-27 | 2016-08-27 | A kind of waste photographic film reclaims the method for silver and chip base |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107338141A (en) * | 2017-07-25 | 2017-11-10 | 丁浩淇 | A kind of photosensitive waste films degumming agent and its reuse method of application and degumming agent |
CN109366800A (en) * | 2017-08-02 | 2019-02-22 | 鹏鼎控股(深圳)股份有限公司 | The recoverying and utilizing method of egative film |
CN112111653A (en) * | 2020-09-29 | 2020-12-22 | 东莞市银辉环保科技有限公司 | Comprehensive utilization and silver recovery processing method for waste film |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1151033A (en) * | 1995-11-20 | 1997-06-04 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovery silver from solid sensitive material |
CN1282002A (en) * | 2000-08-28 | 2001-01-31 | 江阴霞客色纺有限公司 | Film release treatment process for photosensitive material |
CN103074497A (en) * | 2013-01-24 | 2013-05-01 | 惠州Tcl环境科技有限公司 | Method for recovering silver from waste film |
-
2016
- 2016-08-27 CN CN201610747462.9A patent/CN106125498A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1151033A (en) * | 1995-11-20 | 1997-06-04 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovery silver from solid sensitive material |
CN1282002A (en) * | 2000-08-28 | 2001-01-31 | 江阴霞客色纺有限公司 | Film release treatment process for photosensitive material |
CN103074497A (en) * | 2013-01-24 | 2013-05-01 | 惠州Tcl环境科技有限公司 | Method for recovering silver from waste film |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107338141A (en) * | 2017-07-25 | 2017-11-10 | 丁浩淇 | A kind of photosensitive waste films degumming agent and its reuse method of application and degumming agent |
CN107338141B (en) * | 2017-07-25 | 2020-05-12 | 丁浩淇 | Photosensitive waste film degumming agent, application thereof and recycling method of degumming agent |
CN107338141B8 (en) * | 2017-07-25 | 2020-06-09 | 丁浩淇 | Photosensitive waste film degumming agent, application thereof and recycling method of degumming agent |
CN109366800A (en) * | 2017-08-02 | 2019-02-22 | 鹏鼎控股(深圳)股份有限公司 | The recoverying and utilizing method of egative film |
CN112111653A (en) * | 2020-09-29 | 2020-12-22 | 东莞市银辉环保科技有限公司 | Comprehensive utilization and silver recovery processing method for waste film |
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