CN107964590A - A kind of technique of solvent extraction efficiently concentrating recycling noble silver - Google Patents
A kind of technique of solvent extraction efficiently concentrating recycling noble silver Download PDFInfo
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- CN107964590A CN107964590A CN201711226222.5A CN201711226222A CN107964590A CN 107964590 A CN107964590 A CN 107964590A CN 201711226222 A CN201711226222 A CN 201711226222A CN 107964590 A CN107964590 A CN 107964590A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/34—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing sulfur, e.g. sulfonium
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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
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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
The present invention relates to a kind of technique of solvent extraction efficiently concentrating recycling noble silver, with 1, 3 diethyl imidazolium thioketones are extractant, extractant is dissolved in 1 ethyl of hydrophobic ionic liquid, 3 methylimidazole bis-trifluoromethylsulfoandimide salt as the step of ion liquid abstraction phase including (1), (2) the pending liquid of silver nitrate is dissolved in deionized water and adding nitric acid makes the concentration of nitrate anion in pending liquid be 0.1 1M, the step of preparing silver ion solution, (3) by ion liquid abstraction phase 1, 3 diethyl imidazolium thioketones/1 ethyl, 3 methylimidazole bis-trifluoromethylsulfoandimide salt is thoroughly mixed with silver ion solution, the step of extract and separate.The present invention is using 1,3 diethyl imidazolium thioketones as extractant, and whole technical process is without using volatile organic solvent；Extractive reaction kinetic rate is fast, with short production cycle, can reach the purpose of efficient extraction silver, to the extraction yield of silver close to 100%.
Description
Technical field
The invention belongs to noble metal extraction and recovery technical field, is recycled more particularly to a kind of solvent extraction efficiently concentrating
The technique of noble silver.
Background technology
Aerospace, communication system, electronics row are widely used in since noble metal has unique physicochemical properties
The fields such as industry, Chemical Manufacture, Medical Devices, its demand rise year by year.Silver not only has as one kind in Precious Metals Resources
The distinctive advantageous property of noble metal race, and there is larger advantage in price, make its application more extensive, usage amount is more
Greatly.
Solvent extraction is one of effective ways of enriching and recovering silver in the prior art.Due to the spy of silver ion extraction conditions
Different property, silver-colored solvent extraction apply in general to nitric acid medium.Patent document CN98104435 is extracted and the method for recycling silver discloses
A kind of organic extractant solution of the organic phosphorus compound with the molecular sulfur of ionic species containing S2- and the method for recycling silver；Patent text
Offer CN104744395A and disclose a kind of side of sulphur-containing extractants 2- ethylhexyls sulfenyl -4- methylthiazols extract and separate silver
Method.Above method uses poisonous, inflammable, volatile organic solvent more, it is difficult to tackles the increasingly harsh peace of current Chemical Manufacture
Loopful guaranteed request.
Ionic liquid is because its heat endurance is good, difficult volatilization, the characteristic such as liquid journey is wide, ionic conductivity is high, selective dissolution exist
Excellent performance is shown in terms of metal extraction, it is considered to be the new generation of green solvent of extraction and separation technology, widely should have
Use prospect.But compared with the diluents such as traditional alkane, halogenated hydrocarbons, hydrophobic ionic liquid is since stickiness is larger, and there are boundary
The deficiencies of face mass transfer is slowly, the extraction equilibrium time is long, extraction efficiency is relatively low.
The content of the invention
It is an object of the invention to overcome the shortcomings of conventional solvent extraction process, suitable ion liquid abstraction body is established
System, there is provided it is a kind of without using volatile solvent, the simple to operation and technique of being capable of rapidly and efficiently enriching and recovering noble silver.
Term explanation：
1,3- diethyl imidazolium thioketones：Molecular formula is C7H12N2S, relative molecular mass 156.3, structural formula are：
1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt, structural formula are：
The pending liquid of silver nitrate：By solid matter such as ore, electron wastes etc. containing silver, it is dissolved in nitric acid and obtains
Silver nitrate aqueous solution, since pending liquid silver nitrate concentration is than relatively low, of the invention be characterized by extracts from silver nitrate solution
Enrichment silver.
Technical scheme is as follows：
A kind of technique of solvent extraction efficiently concentrating recycling noble silver, is extraction with 1,3- diethyl imidazoliums thioketones
Extractant is dissolved in hydrophobic ionic liquid 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt and makees by agent, including (1)
For ion liquid abstraction phase the step of, (2) by the dissolving of silver nitrate pending liquid in deionized water and add nitric acid make it is pending
The concentration of nitrate anion is 0.1-1M in liquid, the step of preparing silver ion solution, and (3) make the ion liquid abstraction phase of certain volume
The silver ion solution of 1,3- diethyl imidazolium thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt and certain volume
It is thoroughly mixed, the step of extract and separate.
Preferable according to the present invention, the concentration of extractant is 0.01-0.03M in step (1) extraction phase, further preferred
Concentration is 0.01M；
Preferable according to the present invention, concentration of silver ions is 0.005-0.015M in silver ion solution prepared by step (2), nitre
The concentration of acid group is 0.1M, it is further preferred that concentration of silver ions is 0.01M；
Preferable according to the present invention, the volume ratio of step (3) intermediate ion liquid extraction phase and water phase is 1:1-1:3, vibration
Time is 1-10min；Further preferred volume ratio is 1:1, duration of oscillation 1min.
Extractant 1 used in the present invention, 3- diethyl imidazoliums thioketones can be prepared according to the prior art, by elemental sulfur with
Ionic liquid 1,3- diethyl imidazolium acetic acid reactant salt one-step synthesis methods extractant 1,3- diethyl imidazolium thioketones, method are as follows：
By 1,3- diethyl imidazolium acetate ([C2C2Im] [OAc]) 11.00g, it is stirred, reacts with 1.87g elemental sulfurs
Temperature is controlled at 50 DEG C with water-bath；After stirring reaction 24h, 30mL acetonitriles are added into flask, continue to stir 10min；By true
Sky, which filters, removes unreacted elemental sulfur, and rotary evaporation in vacuo removes acetonitrile solvent；The product obtained is dissolved in 50mL dichloromethane,
Respectively washed three times with deionized water and 5% sodium bicarbonate aqueous solution, remove unreacted 1,3- diethyl imidazoliums acetate and anti-
The acetic acid generated during answering；Last rotary evaporation in vacuo removes dichloromethane, up to 1,3- diethyl imidazolium thioketones.
According to the present invention it is further preferred that a kind of solvent extraction efficiently concentrating recycles the technique of noble silver, including
Step：
(1) with 1,3- diethyl imidazoliums thioketones for extractant, it is dissolved in hydrophobic ionic liquid 1- ethyl -3- methyl
It is used as ion liquid abstraction phase in imidazoles bis-trifluoromethylsulfoandimide salt, the concentration of extractant is 0.01-0.03M in extraction phase；
(2) (2) at ambient temperature, by the dissolving of silver nitrate pending liquid in deionized water and add nitric acid make it is pending
The concentration of nitrate anion is 0.1-1M in liquid；It is configured to the silver ion solution that concentration of silver ions is 0.005-0.015M；
(3) the ion liquid abstraction phase 1 for taking certain volume step (1) to prepare, 3- diethyl imidazoliums thioketones/1- ethyls -3-
Silver ion solution prepared by the step of methylimidazole bis-trifluoromethylsulfoandimide salt and certain volume (2) adds centrifuge tube at the same time
In, certain time is extracted under oscillating condition, is thoroughly mixed two-phase；Centrifuge tube is put into supercentrifuge after the completion of extraction
In, 2000rpm centrifugation 2min, are kept completely separate two-phase；Wherein, the volume ratio of ion liquid abstraction phase and water phase is 1:1-1:3,
Duration of oscillation is 1-10min.
The present invention takes upper strata aqueous solution to be diluted in the method for 1,3- diethyl imidazoliums thioketones extraction silver after step (3)
A certain concentration, with the concentration of flame atomic absorption spectrometry silver ion, calculates silver-colored in ionic liquid phase according to mass balance
Concentration, and calculate extraction yield.
Below by specific experiment example, the invention will be further described, illustrate the present invention substantive distinguishing features and into
Step, it is not limited to this.
Experimental example：Extraction experiments
1. influence of the extraction time to silver-colored extraction yield
At ambient temperature, Ag in feed liquid+Concentration be 0.01molL-1, concentration of nitric acid 0.1molL-1 is organic
Xiang Yushui phases compare O/A=1:1, mechanical oscillation incorporation time, that is, extraction time is 0.5-10min, selects ionic liquid 1- second
Diluent of the base -3- methylimidazole bis-trifluoromethylsulfoandimide salt as extraction system, extractant 1 in ionic liquid phase, 3- bis-
The concentration of ethyl imidazol(e) thioketones is 0.02molL-1.Experimental result is as shown in table 1.
Influence of 1 extraction time of table to silver-colored extraction yield
| Extraction time min | 0.5 | 1 | 5 | 10 |
| Extraction yield | 98.06 | 99.95 | 99.97 | a |
a：Silver ion is not detected in water phase.
Experiment shows：Extractive reaction kinetic rate is fast, and when extraction time is 1min, the extraction yield of silver ion is up to
99.95, %, extraction is i.e. up to balance.
2. influence of the extractant concentration to silver-colored extraction yield
At ambient temperature, Ag in feed liquid+Concentration be 0.01molL-1, concentration of nitric acid 0.1molL-1 is organic
Xiang Yushui phases compare O/A=1:1, mechanical oscillation incorporation time, that is, extraction time is 1min, selects ionic liquid 1- ethyls -3-
Diluent of the methylimidazole bis-trifluoromethylsulfoandimide salt as extraction system, extractant 1 in ionic liquid phase, 3- diethyl miaows
The concentration of azoles thioketones is 0-0.03molL-1.Experimental result is as shown in table 2.
2 extractant 1 of table, 3- diethyl imidazolium thioketones (C2C2ImT influence of the concentration) to silver-colored extraction yield
a：Silver ion is not detected in water phase.
Experiment shows：Ability of the ionic liquid without extraction silver in itself, the extraction yield of silver ion is with ionic liquid phase
The concentration of middle extractant increases and increases.
3. compared to the influence to silver-colored extraction yield
At ambient temperature, Ag in feed liquid+Concentration be 0.01molL-1, concentration of nitric acid 0.1molL-1, ion
Liquid extraction phase O/A=1 compared with water phase:1-1:3, mechanical oscillation incorporation time, that is, extraction time is 1min, selects ion
Diluent of the liquid 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt as extraction system, extracts in ionic liquid phase
Agent 1, the concentration of 3- diethyl imidazolium thioketones is 0.02molL-1.Experimental result is as shown in table 3.
Table 3 is compared to the influence to silver-colored extraction yield
| Compared to (O/A) | 1:1 | 1:2 | 1:3 |
| Extraction yield | 99.95 | 98.06 | 65.07 |
Experiment shows：The extraction yield of silver ion is as ionic liquid phase and water phase volume ratio increase and decline.
Beneficial effects of the present invention：
(1) present invention using 1,3- diethyl imidazoliums thioketones be used as extractant, the extractant can by elemental sulfur and from
Sub- liquid 1,3- diethyl imidazolium acetic acid reactant salt one-step synthesis methods, building-up process are simple to operation and molten without using volatility
Agent.
(2) ionic liquid 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt of the present invention has similar to extractant
Structure, can not only improve solubility of the extractant in ionic liquid phase, 1,3- diethyl imidazolium thioketones can also be improved
Solubility of the extracted species formed with silver in ionic liquid phase, so as to achieve the purpose that efficient extraction silver, the present invention is implemented
It is equal to the extraction yield of silver that example calculates 1,3- diethyl imidazoliums thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt
Close to 100%.
(3) whole extraction process is environmentally protective without using volatile organic solvent；
(4) extractive reaction kinetic rate is fast, and several minutes are to reach balance, with short production cycle.
Embodiment
For a better understanding of the present invention, below by specific embodiment, the invention will be further described, but listed
For embodiment be not intended to limit the scope of protection of the invention.
Embodiment 1：Extractant 1, the preparation of 3- diethyl imidazolium thioketones
1,3- diethyl imidazoliums acetate ([C2C2im] [OAc]) 11.00g (59.40mmol) is weighed, with 1.87g simple substance
Sulphur (7.29mmol, equivalent to 58.30mmol sulphur atoms) mechanical agitation in round mouth flask mixes, and reaction temperature is controlled with water-bath
At 50 DEG C.For 1,3- diethyl imidazolium acetate within a few minutes after adding sulphur powder, color is changed into sepia from faint yellow.Stirring
After reaction 24 as a child, 30mL acetonitriles are added into flask, continue to stir 10min.By the way that unreacted list is removed by suction filtration under vacuum
Matter sulphur, rotary evaporation in vacuo remove acetonitrile solvent.Obtained product is dissolved in 50mL dichloromethane, with deionized water and 5%
Sodium bicarbonate aqueous solution respectively wash three times, remove the second generated in unreacted 1,3- diethyl imidazoliums acetate and reaction process
Acid.Last rotary evaporation in vacuo removes dichloromethane, and product is Light brown solid.1H-NMR(300MHz,DMSO)：δ=7.378
(s,1H),4.051(t,4H),1.247(trip,6H)。
Embodiment 2：The extraction process of silver
(1) 1,3- diethyl imidazoliums thioketones prepared by embodiment 1 is dissolved in hydrophobic ionic liquid 1- second for extractant
Extraction phase is used as in base -3- methylimidazole bis-trifluoromethylsulfoandimide salt, the wherein concentration of extractant is 0.01M；
(2) at ambient temperature, dissolving in deionized water and add nitric acid the pending liquid of silver nitrate makes pending liquid
The concentration of middle nitrate anion is 0.1M, is configured to the silver ion solution that concentration of silver ions is 0.005M；
(3) the ion liquid abstraction phase 1 for taking 3mL steps (1) to prepare, 3- diethyl imidazoliums thioketones/1- ethyl -3- methyl miaows
Azoles bis-trifluoromethylsulfoandimide salt and the silver ion solution that prepared by (2) the step of 3mL are added in centrifuge tube at the same time, centrifuge tube machinery
Put it into after the completion of vibration extraction in 1 minute in supercentrifuge, 2000rpm centrifugation 2min, are kept completely separate two-phase.
With concentration silver-colored in Water by Flame Atomic Absorption Spectrometer phase after split-phase, silver-colored concentration is by minusing in ionic liquid phase
Obtain.Calculate extraction yield of 1, the 3- diethyl imidazoliums thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt to silver
Nearly 100%.
Embodiment 3：The extraction process of silver
(1) 1,3- diethyl imidazoliums thioketones prepared by embodiment 1 is dissolved in hydrophobic ionic liquid 1- second for extractant
Extraction phase is used as in base -3- methylimidazole bis-trifluoromethylsulfoandimide salt, the wherein concentration of extractant is 0.01M；
(2) at ambient temperature, at ambient temperature, the pending liquid of silver nitrate is dissolved in deionized water and adds nitre
Acid makes the concentration of nitrate anion in pending liquid be 0.1M, is configured to the silver ion solution that concentration of silver ions is 0.015M；
(3) the ion liquid abstraction phase 1 for taking 3mL steps (1) to prepare, 3- diethyl imidazoliums thioketones/1- ethyl -3- methyl miaows
Azoles bis-trifluoromethylsulfoandimide salt and the silver ion solution that prepared by (2) the step of 3mL are added in centrifuge tube at the same time, centrifuge tube machinery
Put it into after the completion of vibration extraction in 1 minute in supercentrifuge, 2000rpm centrifugation 2min, are kept completely separate two-phase.Centrifuge tube
Put it into after the completion of mechanical oscillation extraction in 1 minute in supercentrifuge, 2000rpm centrifugation 2min, are kept completely separate two-phase.
With concentration silver-colored in Water by Flame Atomic Absorption Spectrometer phase after split-phase, silver-colored concentration is by minusing in ionic liquid phase
Obtain.Calculate extraction yield of 1, the 3- diethyl imidazoliums thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt to silver
For 99.69%.
Embodiment 4：The extraction process of silver
(1) 1,3- diethyl imidazoliums thioketones prepared by embodiment 1 is dissolved in hydrophobic ionic liquid 1- second for extractant
Extraction phase is used as in base -3- methylimidazole bis-trifluoromethylsulfoandimide salt, the wherein concentration of extractant is 0.015M；
(2) at ambient temperature, at ambient temperature, the pending liquid of silver nitrate is dissolved in deionized water and adds nitre
Acid makes the concentration of nitrate anion in pending liquid be 1M, is configured to the silver ion solution that concentration of silver ions is 0.01M；
(3) the ion liquid abstraction phase 1 for taking 3mL steps (1) to prepare, 3- diethyl imidazoliums thioketones/1- ethyl -3- methyl miaows
Azoles bis-trifluoromethylsulfoandimide salt and the silver ion solution that prepared by (2) the step of 3mL are added in centrifuge tube at the same time, centrifuge tube machinery
Put it into after the completion of vibration extraction in 1 minute in supercentrifuge, 2000rpm centrifugation 2min, are kept completely separate two-phase.Centrifuge tube
Put it into after the completion of mechanical oscillation extraction in 1 minute in supercentrifuge, 2000rpm centrifugation 2min, are kept completely separate two-phase.
With concentration silver-colored in Water by Flame Atomic Absorption Spectrometer phase after split-phase, silver-colored concentration is by minusing in ionic liquid phase
Obtain.Calculate extraction yield of 1, the 3- diethyl imidazoliums thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt to silver
For 99.85%.
Claims (8)
1. a kind of technique of solvent extraction efficiently concentrating recycling noble silver, it is characterised in that with 1,3- diethyl imidazolium sulphur
Ketone is extractant, including (1) that extractant is dissolved in the double trifluoro methylsulfonyls of hydrophobic ionic liquid 1- ethyl-3-methylimidazoles is sub-
The pending liquid of silver nitrate is dissolved in deionized water and adds nitric acid by the step of ion liquid abstraction phase is used as in amine salt, (2)
The step of making the concentration of nitrate anion in pending liquid be 0.1-1M, prepare silver ion solution, and (3) make the ionic liquid of certain volume
The silver of body extraction phase 1,3- diethyl imidazoliums thioketones/1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt and certain volume
The step of solion is thoroughly mixed, extract and separate.
2. technique as claimed in claim 1, it is characterised in that the concentration of extractant is 0.01- in step (1) extraction phase
0.03M。
3. technique as claimed in claim 2, it is characterised in that the concentration of extractant is 0.01M in step (1) extraction phase.
4. technique as claimed in claim 1, it is characterised in that concentration of silver ions is in silver ion solution prepared by step (2)
0.005-0.015M, the concentration of nitrate anion is 0.1M.
5. technique as claimed in claim 4, it is characterised in that concentration of silver ions is in silver ion solution prepared by step (2)
0.01M。
6. technique as claimed in claim 1, it is characterised in that the volume ratio of step (3) intermediate ion liquid extraction phase and water phase
For 1:1-1:3, duration of oscillation 1-10min.
7. technique as claimed in claim 6, it is characterised in that the volume ratio of step (3) intermediate ion liquid extraction phase and water phase
For 1:1, duration of oscillation 1min.
8. technique as claimed in claim 1, it is characterised in that including step：
(1) with 1,3- diethyl imidazoliums thioketones for extractant, hydrophobic ionic liquid 1- ethyl-3-methylimidazoles are dissolved in
It is used as ion liquid abstraction phase in bis-trifluoromethylsulfoandimide salt, the concentration of extractant is 0.01-0.03M in extraction phase；
(2) dissolving of silver nitrate pending liquid at ambient temperature, in deionized water and is added nitric acid and made in pending liquid by (2)
The concentration of nitrate anion is 0.1-1M；It is configured to the silver ion solution that concentration of silver ions is 0.005-0.015M；
(3) the ion liquid abstraction phase 1 for taking certain volume step (1) to prepare, 3- diethyl imidazoliums thioketones/1- ethyl -3- methyl
Silver ion solution prepared by the step of imidazoles bis-trifluoromethylsulfoandimide salt and certain volume (2) is added in centrifuge tube at the same time,
Certain time is extracted under oscillating condition, is thoroughly mixed two-phase；Centrifuge tube is put into supercentrifuge after the completion of extraction,
2000rpm centrifuges 2min, is kept completely separate two-phase；Wherein, the volume ratio of ion liquid abstraction phase and water phase is 1:1-1:3, shake
It is 1-10min to swing the time.
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| CN110484745A (en) * | 2019-08-27 | 2019-11-22 | 浙江工业大学 | A kind of method of noble metal in noble metal leaching agent and recycling dead catalyst |
| CN114002174A (en) * | 2021-09-26 | 2022-02-01 | 陕西新时代生物转化检测有限公司 | Ultraviolet absorption spectrometry method for accurately measuring content of silver ions |
| CN115354496A (en) * | 2022-07-18 | 2022-11-18 | 南通大学 | Super-hydrophobic antibacterial cotton fabric and preparation method thereof |
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