CN106244815A - A kind of method separating and recovering silver from photographic film - Google Patents
A kind of method separating and recovering silver from photographic film Download PDFInfo
- Publication number
- CN106244815A CN106244815A CN201610788388.5A CN201610788388A CN106244815A CN 106244815 A CN106244815 A CN 106244815A CN 201610788388 A CN201610788388 A CN 201610788388A CN 106244815 A CN106244815 A CN 106244815A
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- CN
- China
- Prior art keywords
- silver
- compound
- enzyme
- solution
- protease
- 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.)
- Pending
Links
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 36
- 239000004332 silver Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 31
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 102000004190 Enzymes Human genes 0.000 claims abstract description 15
- 108090000790 Enzymes Proteins 0.000 claims abstract description 15
- 108091005804 Peptidases Proteins 0.000 claims abstract description 11
- 239000004365 Protease Substances 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 15
- 229940088598 enzyme Drugs 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 11
- 102000035195 Peptidases Human genes 0.000 claims description 10
- 102000029816 Collagenase Human genes 0.000 claims description 8
- 108060005980 Collagenase Proteins 0.000 claims description 8
- 102000004142 Trypsin Human genes 0.000 claims description 8
- 108090000631 Trypsin Proteins 0.000 claims description 8
- 229960002424 collagenase Drugs 0.000 claims description 8
- 239000012588 trypsin Substances 0.000 claims description 8
- 102000005600 Cathepsins Human genes 0.000 claims description 7
- 108010084457 Cathepsins Proteins 0.000 claims description 7
- 101000924393 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) Vacuolar aminopeptidase 1 Proteins 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000009991 scouring Methods 0.000 claims description 2
- 235000019419 proteases Nutrition 0.000 claims 4
- 108010033040 Histones Proteins 0.000 claims 1
- 235000019833 protease Nutrition 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 239000002585 base Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229920000159 gelatin Polymers 0.000 description 4
- 239000008273 gelatin Substances 0.000 description 4
- 235000019322 gelatine Nutrition 0.000 description 4
- 235000011852 gelatine desserts Nutrition 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000002255 enzymatic effect Effects 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000003500 flue dust Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- SYUXAJSOZXEFPP-UHFFFAOYSA-N glutin Natural products COc1c(O)cc2OC(=CC(=O)c2c1O)c3ccccc3OC4OC(CO)C(O)C(O)C4O SYUXAJSOZXEFPP-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
- 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
- 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
-
- 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
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Abstract
The invention discloses a kind of method separating and recovering silver from photographic film, the method comprises the steps: the configuration of (1) compound aqueous solution of protease；(2) separation of Silver；(3) reuse containing enzyme filtrate.The inventive method has the advantages such as efficient, easy, treating capacity is big, low expense, environmental protection.
Description
Technical field
The present invention relates to noble metal recovery technology field, especially relate to one and utilize compound Protease Treatment film system
The method taking silver.
Background technology
Silver is widely used in sensitive material industry, is increasingly paid attention to as its recycling of precious metal, photoresists
Sheet is mainly used in video display industry, electron trade and medical industry, a large amount of waste films of annual generation, and these waste films contain
Silver, chip base is polyethylene terephthalate, has the highest recycling and is worth.
In waste films, silver exists with elemental silver form, is attached in chip base using gelatin as carrier, tradition separate mode bag
Include following several big class: 1) burning disposal: by burning disposal, ash reclaims silver, simple to operate, equipment requirements is low, process
Amount is big, but the response rate of silver is low, only reaches 75%, secondly can produce a large amount of contaminative flue gas and dust, seriously polluted；It addition,
Burning disposal cannot reclaim base material polyester；2) mechanical cleaning method: the Mechanical Method response rate is high, pollution-free, but process rule
Mould is little, costly；3) chemical dissolution method: the glutin of macromole become the little molecule of water miscible aminoacid by soda acid,
Molecular weight reduces, and water solublity is greatly enhanced, and utilizes the severe corrosive of acid solution and alkali liquor, makes part Ag be transformed into Ag+Ion enters
Solution film, after nitric acid acidleach, forms silver nitrate solution and reaches to separate purpose, and treating capacity is big, but exists and operate complicated, danger
Dangerous big, acid mist pollution serious, produces the shortcomings such as high COD strong acid or highly basic waste liquid.
Summary of the invention
For prior art exist the problems referred to above, the applicant provide a kind of from photographic film separation and recovery silver
Method.The inventive method has the advantages such as efficient, easy, treating capacity is big, low expense, environmental protection.
Technical scheme is as follows:
A kind of method separating and recovering silver from photographic film, described method comprises the steps:
(1) configuration of compound aqueous solution of protease: by compound protease 30～50 DEG C successively ultrasonic disperse be dissolved in
In aqueous solution, it is configured to the aqueous solution of 5～10wt%；
(2) separation of Silver: first the pH of the compound aqueous solution of protease of regulating step (1) gained is 6～9, and is heated to 40
～60 DEG C, then photographic film being immersed in this solution, after ultrasonic vibration 8～10h, take out base, silver comes off molten
In liquid；
(3) reuse containing enzyme filtrate: by being filtrated to get filtering residue silver powder containing the solution of silver, the pH of filtrate is adjusted again
It is 6～9, is re-used for separation of Silver.
Described compound protease is Collagenase, cathepsin, trypsin, the compounding gained of polypeptidase mixing
Compound enzyme；Described Collagenase, cathepsin, trypsin, polypeptidase account for the 15～45% of compound enzyme total amount respectively, always
With 100%.
Described compound enzyme uses pH to be 6～9, and using temperature is 40～60 DEG C, and scouring processes enters under ultrasonic vibration effect
OK.
Described in step (3), filtrate is by utilization repeatable after readjusting pH.
Useful the having the technical effect that of the present invention
The inventive method has treatment conditions gentleness, equipment requirements condition is low, treatment effeciency is high, treating capacity is big, operation is simple
The advantages such as clean convenience, processing cost are low, repeatable operation.
First by enzyme treatment technique, process efficiently, use mild condition, according to the repeatable utilization of enzymatic activity, relatively pass
System technology has low power consuming, without advantages such as tail washings pollutions.
Secondly, by enzyme degumming separation of Silver, silver has neither part nor lot in chemical reaction, and conventional chemical treatment techniques is all to pass through nitric acid
After molten silver, silver is extracted in reduction, and it is high, without acid gas pollution, without advantages such as argentiferous heavy metal wastewater thereby generations that this method has silver raising recovery rate.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is specifically described.
Embodiment 1
Respectively 40mg Collagenase, 30mg cathepsin, 30mg trypsin, 50mg polypeptidase are mixed and be dissolved in
In 100mL water, after NaOH regulation pH to 9, it is warming up to 40 DEG C；Photographic film 25g is immersed in ultrasonic vibration 8h in this enzymatic solution
After, on film, black part drops, and it is muddy that solution sinks black, removes after base also rinses with clear water and records film silver content
Within 0.5mg/g, being filtrated to get black silver pressed powder, silver raising recovery rate reaches 97%；Filtrate repeats profit after readjusting pH
With respond well, within reusing number of times 3 times, effect is almost identical, needs to provide soak time extremely when access times 4 times
10h reaches gelatin hydrolysate separating effect.
Embodiment 2
Respectively 400g Collagenase, 300g cathepsin, 300g trypsin, 500g polypeptidase are mixed and be dissolved in
In 1t water, after being warming up to 60 DEG C after NaOH regulation pH to 7,250 kilograms of waste photographic films are immersed, open ultrasonic vibration
Device after keeping 8h, on film, black part drops, and it is muddy that solution sinks black, removes after base also rinses with clear water and records
Film silver content, within 1mg/g, is filtrated to get black silver pressed powder, and silver raising recovery rate reaches 95%；Filtrate readjusts pH
Rear recycling is respond well, and within reusing number of times 3 times, effect is almost identical, needs to provide leaching when access times 6 times
The bubble time reaches gelatin hydrolysate separating effect to 10h；After adding various enzyme in proportion when access times are more than 6 times, using effect depends on
Old well, reach desired target.
Embodiment 3
Respectively 50mg Collagenase, 40mg cathepsin, 200mg trypsin, 45mg polypeptidase are mixed and molten
In 100mL water, after NaOH regulation pH to 7, it is warming up to 60 DEG C；Photographic film 25g is immersed in ultrasonic vibration in this enzymatic solution
After 8h, on film, black part drops, and it is muddy that solution sinks black, removes after base also rinses with clear water and records film argentiferous
Amount, within 0.5mg/g, is filtrated to get black silver pressed powder, and silver raising recovery rate reaches 97%；Filtrate is repeated after readjusting pH
Utilizing status is good, and within reusing number of times 3 times, effect is almost identical, needs to provide soak time when access times 6 times
Gelatin hydrolysate separating effect is reached to 10h.
Test case:
Fermentoid solution used to embodiment 1 by same ratio 400g Collagenase, 300g cathepsin,
The mixing of 300g trypsin, 500g polypeptidase re-uses after adding compound enzyme regulation pH to 9, can reach embodiment 1 phase and exists together
Reason effect.Relatively process 10t waste films with nitric acid treatment method this method, water consumption, silver-colored average recovery rate, tailwater quantity, power consumption (with
Kw.h counts) contrast.The results are shown in Table 1.
Table 1
| Silver recovery method | Water consumption/t | Silver raising recovery rate/% | Tailwater quantity/t | Power consumption/Kw.h |
| Nitric acid solution reclaiming method | 6 | 86 | 5.6 (high COD spent acid) | 35 |
| Compound enzyme partition method | 2 | 94 | 1.8 (high-COD waste waters) | 5 |
Claims (4)
1. the method separating and recovering silver from photographic film, it is characterised in that described method comprises the steps:
(1) configuration of compound aqueous solution of protease: by compound protease 30～50 DEG C successively ultrasonic disperse be dissolved in water-soluble
In liquid, it is configured to the aqueous solution of 5～10wt%；
(2) separation of Silver: first the pH of the compound aqueous solution of protease of regulating step (1) gained is 6～9, and is heated to 40～60
DEG C, then photographic film being immersed in this solution, after ultrasonic vibration 8～10h, take out base, silver comes off in the solution；
(3) reuse containing enzyme filtrate: by being filtrated to get filtering residue silver powder containing the solution of silver, the pH of filtrate is adjusted to 6 again
～9, it is re-used for separation of Silver.
Method the most according to claim 1, it is characterised in that described compound protease is Collagenase, histone
The compound enzyme of the compounding gained of enzyme, trypsin, polypeptidase mixing；Described Collagenase, cathepsin, trypsin, many
Peptidase accounts for the 15～45% of compound enzyme total amount, summation 100% respectively.
Method the most according to claim 1, it is characterised in that described compound enzyme use pH be 6～9, use temperature be 40～
60 DEG C, scouring processes is carried out under ultrasonic vibration effect.
Method the most according to claim 1, it is characterised in that filtrate described in step (3) is by weighing after readjusting pH
Multiple utilization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610788388.5A CN106244815A (en) | 2016-08-31 | 2016-08-31 | A kind of method separating and recovering silver from photographic film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610788388.5A CN106244815A (en) | 2016-08-31 | 2016-08-31 | A kind of method separating and recovering silver from photographic film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106244815A true CN106244815A (en) | 2016-12-21 |
Family
ID=58079759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610788388.5A Pending CN106244815A (en) | 2016-08-31 | 2016-08-31 | A kind of method separating and recovering silver from photographic film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106244815A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3929466A (en) * | 1974-06-28 | 1975-12-30 | Gaf Corp | Recovery of silver from silver salts |
| US4150977A (en) * | 1977-10-27 | 1979-04-24 | Keltek Processing, Inc. | Process for stripping photographic materials |
| GB2226153B (en) * | 1988-12-07 | 1992-07-22 | Ilford Ltd | Stripping of silver halide emulsions from photographic supports |
| CN1067969A (en) * | 1991-06-22 | 1993-01-13 | 丁锐 | The recovery method of waste sensitive material |
| 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 recovering silver from solid-phase photosensitive material |
| JP5260941B2 (en) * | 2007-11-15 | 2013-08-14 | 独立行政法人海洋研究開発機構 | Novel collagenolytic enzymes and their use |
-
2016
- 2016-08-31 CN CN201610788388.5A patent/CN106244815A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3929466A (en) * | 1974-06-28 | 1975-12-30 | Gaf Corp | Recovery of silver from silver salts |
| US4150977A (en) * | 1977-10-27 | 1979-04-24 | Keltek Processing, Inc. | Process for stripping photographic materials |
| GB2226153B (en) * | 1988-12-07 | 1992-07-22 | Ilford Ltd | Stripping of silver halide emulsions from photographic supports |
| CN1067969A (en) * | 1991-06-22 | 1993-01-13 | 丁锐 | The recovery method of waste sensitive material |
| 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 recovering silver from solid-phase photosensitive material |
| JP5260941B2 (en) * | 2007-11-15 | 2013-08-14 | 独立行政法人海洋研究開発機構 | Novel collagenolytic enzymes and their use |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161221 |
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| RJ01 | Rejection of invention patent application after publication |