CN101016585A - Method of reclaiming silver from silver ion containing solution by polydiaminoanthraquinone as adsorbent - Google Patents
Method of reclaiming silver from silver ion containing solution by polydiaminoanthraquinone as adsorbent Download PDFInfo
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- CN101016585A CN101016585A CNA2007100379145A CN200710037914A CN101016585A CN 101016585 A CN101016585 A CN 101016585A CN A2007100379145 A CNA2007100379145 A CN A2007100379145A CN 200710037914 A CN200710037914 A CN 200710037914A CN 101016585 A CN101016585 A CN 101016585A
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Abstract
The invention discloses a method to reclaim silver from solution with silver ion, which comprises the following steps: adopting static absorption method; using micrometer or nanometer particle of poly diamino corbit as sorbent; adding poly diamino corbit into silver ion solution with initial concentration at 1-100mmol/L; stirring; absorbing 30min-24h; filtering. This invention possesses cheap cost, convenient operation and high adsorption efficiency, which can be used to image fusing waste liquid, plating waste liquid, chemical analysis waste liquid and test waste liquid.
Description
Technical field
The present invention relates to a kind of method that from contain silver ion solution, reclaims silver with polydiaminoanthraquinone as silver ion adsorbant.
Background technology
The recovery method of precious metal ion---silver ions is a lot, and wherein of paramount importance method is an absorption method.Absorption property with synthetic adsorbent is the most superior again among absorption method.The synthetic adsorbent of silver ions absorption mainly contains acticarbon, activated carbon fiber adsorbing substance, chelate fibre and resin and fragrant amido polymer absorbant.In recent years, many investigators are doing a large amount of work aspect the efficient silver ions synthetic adsorbent of exploration.Wherein, Luo Yongyi etc. adopt the ultra-trace silver in the charcoal absorption enrichment natural water, adsorption rate is up to 95.8%, but the adsorption efficiency of the gac of unit mass is very low, adsorptive capacity only be 3～5mg/g (Jiang Ting, Shi Yinrui, Hua Jinyuan. the research of charcoal absorption Trace Silver. forestry chemistry and industry, 1996,16 (2): 49-53.).Once Chinese waited and used chemical conversion treatment and the organic two kinds of activated carbon fibres handling of load simultaneously, it adsorbs silver-colored capacity maximum can reach 800mg/g (CN1208773), but the preparation process of activated carbon fiber itself is with regard to more complicated, the reactivation process of adding the later stage makes its preparation process very loaded down with trivial details, and manufacturing cost is also corresponding to improve a lot.Chelate fibre and resin are the adsorption functional materials that a class can form polygamy position complex compound with heavy metal ion.Once Chinese wait PVF-g-PAN-AO chelate fibre absorption silver, high adsorption capacity be 120.9mg/g (Chinese once, Xu Zhida, Lu Yun. the research II. of chelate fibre contains the absorption property of amidoxim oximido chelate fibre. ion-exchange and absorption, 1993,9 (4): 312.); The maximum adsorption capacity that its silver ions of fundamental mode resin is dredged in employings such as Wu Xiangmei can reach 559mg/g (Wu Xiangmei, Xiong Chunhua, Shu Zengnian. the behavior and the mechanism of thiol resin absorption silver. chemical industry journal, 2003,54 (10): 1466-1469).But chelate fibre and resin are still quite limited for the adsorptive power of silver ions, and preparation method's relative complex.In aromatic amine copolymer, poly-1, the 8-naphthylene diamine has outstanding adsorptive power and adsorption efficiency for silver ions, its loading capacity maximum can reach 1924mg/g (CN1840234), and with the diphenylamine sulfonic acid copolymerization modification after poly-1, the 8-naphthylene diamine has higher loading capacity, can reach 2040mg/g (CN1810354).But, 1,8-naphthylene diamine monomer price is very expensive, carries out large-scale industry and applies the certain difficulty of existence.Therefore, be based on the domestication chemical product, seek inexpensive silver ion adsorbant efficiently, have a great deal of practical meanings.
Polydiaminoanthraquinone belongs to the aromatic amine base polymer, have polyaniline skeleton structure, benzoquinones group and inflexible quinone loop chain joint, so its electrochemical activity, biological electro catalysis and stability is all very strong.All having shown at aspects such as energy storage, electrocatalysis enhanced sensitivities and to be better than the functional of general aromatic amine base polymer, is a kind of new function material that development potentiality is arranged very much.This seminar has adopted easy chemical oxidative polymerization high productivity to synthesize poly-1,5-diamino-anthraquinone (CN1810854), with high-performance poly 1, what the 8-naphthylene diamine was identical is, this also is the polymkeric substance that contains amino and imido grpup in a kind of molecular chain, and, also contain the O atom in its molecular chain, according to the lone-pair electron on these N, the O atom, estimate that it has good adsorptive power to heavy metal ion.The present invention will gather 1, and the 5-diamino-anthraquinone is as the sorbent material of silver ions in the aqueous solution.Up to the present, do not see the report of polydiaminoanthraquinone at home and abroad as yet as silver ion adsorbant.
Summary of the invention
The purpose of this invention is to provide a kind of with low cost, easy to operate, adsorption efficiency is high reclaims the method for silver from contain silver ion solution.
The method that reclaims silver from contain silver ion solution that the present invention proposes is to adopt static adsorptive method, and wherein silver ion adsorbant adopts polydiaminoanthraquinone.
The used polydiaminoanthraquinone of the present invention can be prepared by chemical oxidative polymerization, is micron or nanoparticle.
Static adsorptive method of the present invention, concrete steps are as follows: the micron of polydiaminoanthraquinone or nanoparticle are stirred to add down contain in the silver ion solution, whip attachment 30 minutes-24 hours is filtered; Wherein, the starting point concentration that contains silver ion solution is 1-100mmol/L, and the consumption of polydiaminoanthraquinone is 1-3mg/ml with the ratio that contains silver ion solution.
Concentration of silver ions residual in the filtrate of the present invention adopts the Fo Erhadefa titrimetry, calculates the loading capacity Q (mg/g) of sorbent material then according to following formula.
C in the formula
oBe initial concentration of silver ions (mol/L); C is absorption back residual concentration of silver ions (mol/L).
The silver ion adsorbant that the present invention uses, its adsorptive power is along with the change of size of particles difference and dopant states is different.The polydiaminoanthraquinone nanoparticle is because of having smaller particle size and then have bigger specific surface area, thereby shows higher loading capacity.Wherein, the mix experiment maximum adsorption capacity value of attitude polydiaminoanthraquinone of doping attitude or go can reach 467.1 and 560.5mg/g respectively.The mix loading capacity experimental value of polydiaminoanthraquinone micron particle of doping attitude or go is respectively 327.0mg/g and 467.0mg/g, and behind the visible polymer particle nanometer, loading capacity can increase by 42.8% and 20.0% respectively.On the other hand, polydiaminoanthraquinone is after the past doping treatment, absorption property also can correspondingly improve, this is when being in the doping attitude because of polymkeric substance, part active group on the polydiaminoanthraquinone molecular chain is occupied by the hydrogen proton, simultaneously, during dopant states anionic existence is made active site on the inaccessible polydiaminoanthraquinone molecular chain of silver ions, the two acting in conjunction and make the inerting of polymer chain part.
The silver ion adsorbant that the present invention is used, when concentration of treatment was the silver ion solution of 0.096mol/L, the loading capacity experimental value reached as high as 560.5mg/g, and along with the concentration of silver ions increases, loading capacity further strengthens.Under equal adsorption conditions, the suction silver ability that this sorbent material is inhaled silver-colored performance and electrooxidation activated carbon fiber is suitable, and what be slightly less than open report gathers 1,8-naphthylene diamine silver ion adsorbant.But tool has great advantage on its raw materials cost, and the diamino-anthraquinone monomer is domestic common Chemicals, and raw material is easy to get, and is cheap.Simultaneously, polydiaminoanthraquinone also shows good heavy metal ion adsorbed selectivity, and lead ion is shown very weak adsorptive power, can realize the recovery of silver ions in the blend solion.The constructional feature that adds polydiaminoanthraquinone polymkeric substance self has given this sorbent material very strong acid and alkali-resistance ability and solvent resistance, is fit to be applied to the silver ion solution environment of condition harshness.
Description of drawings
Fig. 1 is the wide-angle X diffracting spectrum before and after the polydiaminoanthraquinone absorption silver.
Embodiment
Embodiment 1
In the dry Erlenmeyer flask of 50mL, the silver ion solution 25mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is 20-80nm) and 0.09615mol/L, Erlenmeyer flask is put into sonic oscillation instrument sonic oscillation to be handled 30-90 minute, take out then, place 30 ℃ of stirred in water bath absorption 24 hours.Filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 467.1mg/g.Adsorbed galactic longitude wide-angle X diffractogram (Fig. 1) spectrum turns out to be simple substance silver.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 560.5mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 2
In the dry Erlenmeyer flask of 50mL, the silver ion solution 30mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter 20-80nm) and 0.083mol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation take out after 1 hour, place 30 ℃ of stirred in water bath absorption 24 hours.Filter paper filtering, with the concentration of Fo Erhadefa titrimetry absorption back silver ions, its loading capacity is 327.0mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 460.7mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 3
In the dry Erlenmeyer flask of 50mL, (number average bead diameter of laser particle size test is the silver ion solution 40mL of 1.3-2.5 μ m and 0.09615mol/L to add doping attitude polydiaminoanthraquinone polymkeric substance 50mg, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation take out after 1 hour, place 30 ℃ of stirred in water bath absorption 15 hours.Filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 243.0mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 322.5mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 4
In the dry Erlenmeyer flask of 50mL, the silver ion solution 25mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is a micron order) and 0.083mol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation take out after 1 hour, place 30 ℃ of stirred in water bath absorption 24 hours.Filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 257.0mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 384.5mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 5
In the dry Erlenmeyer flask of 50mL, the silver ion solution 25mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is a submicron order) and 0.083mol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation take out after 1 hour, place 30 ℃ of stirred in water bath absorption 23 hours.Filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 220.4mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 320.7mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 6
In the dry Erlenmeyer flask of 50mL, the silver ion solution 25mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is a nano level) and 0.083mol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation to be taken out after 1 hour, place 30 ℃ of stirred in water bath absorption 10 hours, filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 184.5mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 219.6mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 7
In the dry Erlenmeyer flask of 50mL, the silver ion solution 50mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is a submicron order) and 0.083mol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation to be taken out after 1 hour, place 30 ℃ of stirred in water bath absorption 23 hours, filter paper filtering, with the concentration of the residual silver ions in Fo Erhadefa titrimetry absorption back, its loading capacity is 212.0mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 249.5mg/g.As seen the state property that goes to mix can be better than the attitude of mixing.
Embodiment 8
In the dry Erlenmeyer flask of 50mL, the lead ion solution 25mL that adds doping attitude polydiaminoanthraquinone polymkeric substance 50mg (particle diameter is a micron order) and 1mmol/L, Erlenmeyer flask is put into the processing of sonic oscillation instrument sonic oscillation to be taken out after 1 hour, place 30 ℃ of stirred in water bath absorption 23 hours, filter paper filtering, with the concentration of the residual lead ion in EDTA complexometry analysis absorption back, its loading capacity is 14.9mg/g.Other condition is identical, uses instead and removes to mix the attitude polymkeric substance accordingly, and loading capacity is 37.0mg/g.Than the loading capacity of silver ions, this sorbent material shows more weak adsorptive power to lead ion, and therefore, it has the potentiality of selective adsorption to silver ions, and the existence of a small amount of lead ion does not influence the recovery to silver ions.
Embodiment 9
1mg puts into beaker with the polydiaminoanthraquinone polymkeric substance, adds 1mL organic solvent or sour water or buck respectively, leaves standstill 2 hours, and intermittently shakes, and observes the polymer dissolution situation, the results are shown in Table 1.Similarity condition uses monomer to carry out solubility experiment down, the results are shown in Table 1.Polydiaminoanthraquinone shows very strong solvent resistance and acid and alkali-resistance ability as can be seen, is applicable under the various soda acid water surroundings recovery to silver ions.
Table 11,5-diamino-anthraquinone monomer and the polymkeric substance solvability in organic solvent and strong acid and strong base
| Sorbent material | The vitriol oil | Formic acid | Methyl-sulphoxide | The N methyl-2-pyrrolidone | Meta-cresol | Tetrahydrofuran (THF) | Chloroform | 1mol/L hydrochloric acid | 1mol/L NaOH | Water |
| Monomer | Dissolving | Dissolving | Dissolving | Dissolving | Dissolving | Dissolving | Dissolving | Insoluble | Insoluble | Insoluble |
| Doped polymer | Dissolving | Be partly dissolved | Be partly dissolved | Be partly dissolved | Be partly dissolved | Minimal amounts of dissolved | Minimal amounts of dissolved | Insoluble | Insoluble | Insoluble |
| Remove doped polymer | Dissolving | Be partly dissolved | Be partly dissolved | Be partly dissolved | Be partly dissolved | Minimal amounts of dissolved | Minimal amounts of dissolved | Insoluble | Insoluble | Insoluble |
Claims (3)
1, a kind of method that reclaims silver from Ag-containing solution is characterized in that adopting static adsorptive method, and wherein, silver ion adsorbant adopts polydiaminoanthraquinone.
2, the method that from Ag-containing solution, reclaims silver according to claim 1, the concrete steps that it is characterized in that described static adsorptive method are as follows: the micron or the nanoparticle stirring of polydiaminoanthraquinone are contained in the silver ion solution following the adding, whip attachment 30 minutes-24 hours is filtered; Wherein, the starting point concentration that contains silver ion solution is 1-100mmol/L, and the consumption of polydiaminoanthraquinone is 1-3mg/ml with the ratio that contains silver ion solution.
3, the method that reclaims silver from Ag-containing solution according to claim 1 is characterized in that described polydiaminoanthraquinone is the doping attitude or the attitude polydiaminoanthraquinone that goes to mix.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012113157A1 (en) * | 2011-02-25 | 2012-08-30 | Tongji University | Poly (sulfoaminoanthraquinone) materials and methods for their preparation and use |
| CN104630478A (en) * | 2013-11-07 | 2015-05-20 | 中国科学院宁波材料技术与工程研究所 | Method utilizing conductive polymer porous separating membrane to recycle metals from electronic wastes |
| CN115232308A (en) * | 2022-08-10 | 2022-10-25 | 燕山大学 | Quinone polymer positive electrode material and preparation method and application thereof |
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| RU2055920C1 (en) * | 1993-07-14 | 1996-03-10 | Иркутский институт органической химии СО РАН | Method to extract silver from solutions |
| US6200364B1 (en) * | 1999-08-13 | 2001-03-13 | Antonio T. Robles | Process for eluting precious metals from activated carbon |
| CA2355491A1 (en) * | 2001-08-21 | 2003-02-21 | Edward Ramsay | Process for the recovery of precious metals from fine carbon |
| JP4204235B2 (en) * | 2002-02-04 | 2009-01-07 | 三菱原子燃料株式会社 | Silver recovery method |
| RU2225454C1 (en) * | 2002-09-19 | 2004-03-10 | Институт химии нефти СО РАН | Method of extraction of gold and silver from low- concentration solutions and device for realization of this method |
| CN100395279C (en) * | 2005-01-26 | 2008-06-18 | 同济大学 | Prepn process of polydiaminoanthraquinone |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012113157A1 (en) * | 2011-02-25 | 2012-08-30 | Tongji University | Poly (sulfoaminoanthraquinone) materials and methods for their preparation and use |
| CN104630478A (en) * | 2013-11-07 | 2015-05-20 | 中国科学院宁波材料技术与工程研究所 | Method utilizing conductive polymer porous separating membrane to recycle metals from electronic wastes |
| CN104630478B (en) * | 2013-11-07 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | Utilize the method that conducting polymer porous diffusion barrier reclaims metal from electron wastes |
| CN115232308A (en) * | 2022-08-10 | 2022-10-25 | 燕山大学 | Quinone polymer positive electrode material and preparation method and application thereof |
| CN115232308B (en) * | 2022-08-10 | 2023-05-23 | 燕山大学 | Quinone polymer positive electrode material, and preparation method and application thereof |
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