CN100434547C - Method of reclaiming silver from silver containing solution by poly o-phenylenediamine as adsorbent - Google Patents
Method of reclaiming silver from silver containing solution by poly o-phenylenediamine as adsorbent Download PDFInfo
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- CN100434547C CN100434547C CNB200710037915XA CN200710037915A CN100434547C CN 100434547 C CN100434547 C CN 100434547C CN B200710037915X A CNB200710037915X A CN B200710037915XA CN 200710037915 A CN200710037915 A CN 200710037915A CN 100434547 C CN100434547 C CN 100434547C
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Abstract
The invention discloses a method to reclaim silver from solution with silver, which comprises the following steps: adopting static absorption method; using poly o-phenylenediamine as silver ion sorbent; adding silver ion solution with initial density at 1.2-100mmol/L; stirring; absorbing at 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 with the method that from Ag-containing solution, reclaims silver of poly-o-phenylenediamine as silver ion adsorbant.
Background technology
The traditional method that reclaims silver from silver-containing liquid waste mainly contains the precipitator method, electrolytic process, reduction method of substitution and ion exchange method.The power consumption of these traditional method ubiquities is big, secondary pollution is arranged, to shortcomings such as the Trace Silver effect are little.Absorption method can overcome the shortcoming of above-mentioned four kinds of methods to a certain extent, thereby has bigger development potentiality.The adsorption effect of absorption method depends primarily on the performance of employed sorbent material.As sorbent material the most frequently used in the absorption method, gac is mainly used in the trace in the silver-containing liquid waste or the recovery of ultra-trace silver.Adopt ultra-trace silver in the charcoal absorption enrichment natural water, adsorption rate is up to 95.8%, and the mass concentration that minimum detects has only 0.025 μ g/L (Luo Yongyi, Zhang Kerong, Zhang Yao, etc. the absorption behavior of silver on gac and the research [J] of mechanism. environmental chemistry, 1995,14 (1): 75-79).Select for use shell class water purification to contain the film industry waste water of Trace Silver (171 μ g/L) with activated carbon treatment with gac and ature of coal water purification, can make the mass concentration of the silver in the waste water reduce to national hygiene standard for drinking water less than 50 μ g/L, adsorptive capacity can reach 3～5mg/g (Jiang Ting, Shi Yinyue, Hua Jinai. the research of charcoal absorption Trace Silver [J]. chemistry of forest product and industry, 1996,16 (2): 49-53).Though it is gac can remedy the deficiency of traditional method to a certain extent, powerless to the silver-colored waste liquid of high density owing to be subjected to the restriction of himself adsorptive power.Except that gac, activated carbon fiber, resin, poly-(1, the 8-naphthylene diamine) also can be used as silver ion adsorbant owing to contain a large amount of functional groups, especially gather (1, the 8-naphthylene diamine) has maximum silver ions loading capacity 1920mg/g (Li X G, HuangM R, Li S X.Facile synthesis of poly (1,8-diaminonaphthalene) microparticles with a very highsilver-ion adsorbality by a chemical oxidative polymerization[J] .Acta Materialia, 2004,52:5363-5374.), but these three kinds of materials are all had higher use cost as silver ion adsorbant, thereby limited its widespread use.
Summary of the invention
Purpose of the present invention just provide a kind of with low cost, easy to operate, adsorption efficiency is high reclaims the method for silver from Ag-containing solution.
The method that reclaims silver from Ag-containing solution that the present invention proposes adopts static adsorptive method, and wherein, silver ion adsorbant adopts poly-o-phenylenediamine.Poly-o-phenylenediamine can be synthetic with chemical oxidative polymerization, contain on it can with the NH-of silver ions generation complexing action or redoxomorphism, NH
2-group, the poly-o-phenylenediamine structural formula is as follows:
Static adsorptive method of the present invention, concrete steps are as follows:
The poly-o-phenylenediamine adding is contained in the silver ion solution, whip attachment 30 minutes-24 hours, wherein, containing the silver ion solution starting point concentration is 1.24-100mmol/L, poly-o-phenylenediamine is 1-3mg/mL with the proportioning that contains silver ion solution.
Residual concentration of silver ions adopts the Fo Erhadefa titration or with plasma body absorption spectroscopy mensuration, then according to the loading capacity of (1) formula calculating sorbent material, calculates the adsorption rate of silver ions according to (2) formula in the filtrate.
Q: the loading capacity of silver ions (mg/g); Q: the absorption percentage of silver ions; C
o: initial silver ions degree (mol/L);
C: absorption back residual concentration of silver ions (mol/L); V: contain silver ion solution volume (mL); M: the molecular weight (g/mol) of silver;
W: the weight (g) that adds polymkeric substance.
Loading capacity is with the variation of adsorption time when adsorbing certain density silver ions according to poly-o-phenylenediamine, can draw out loading capacity curve over time, can obtain adsorption equilibrium time and maximum adsorption capacity under a certain concentration of silver ions by this curve, and can utilize accurate second-order kinetics equation to carry out the kinetics of adsorption simulation, thereby draw initial adsorption rate constant h.
Because the absorption property of sorbent material is subjected to the influence of adsorption time, initial concentration of silver ions, sorbent material consumption, among the present invention, initial concentration of silver ions scope is 1.24～100mmol/L, the consumption of poly-o-phenylenediamine is 1-3mg/mL with the ratio that contains silver ion solution, and adsorption time is 30 minutes～24 hours.
Among the present invention, the described silver ion solution that contains can be silver nitrate solution, also can contain silver ion solution for other.
Beneficial effect of the present invention: relatively disclosed silver ion adsorbant gathers (1,8 naphthylene diamine), and the cost of material of poly-o-phenylenediamine is cheap, and therefore, its raw materials cost is well below poly-(1,8 naphthylene diamine).And it is easy to operate, add its silver ions adsorptive power efficiently faster, silver recovery at wasted fixing solution, electroplating effluent, chemical analysis waste liquid, test waste liquid is handled, and the process field again of the silver-containing waste water of crossing through conventional process such as chemical precipitation method, electrolytic process, ion exchange method, metallic reducing method, microbial methods has application promise in clinical practice.
Description of drawings
Fig. 1 is that synthetic doping attitude poly-o-phenylenediamine is adsorbed in the wide-angle x-ray diffracting spectrum of 100mmol/L silver ions after 24 hours under 1/1 condition for oxygen digital ratio.
Fig. 2 is absorption of synthetic doping attitude poly-o-phenylenediamine and the XPS figure of 100mmol/L silver ions after 24 hours under 1/1 condition for oxygen digital ratio.
Fig. 3 is synthetic go to mix absorption of attitude poly-o-phenylenediamine and the XPS figure of 100mmol/L silver ions after 24 hours under 1/1 condition for oxygen digital ratio.
Embodiment
Embodiment 1
Get synthetic doping attitude poly-o-phenylenediamine 50mg under oxygen digital ratio 1/1 condition, 30 ℃ of following inputs in the silver ion solution that the 25mL starting point concentration is 100mmol/L are stirred reaction 24h; After the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly-o-phenylenediamine silver ions being got loading capacity is 533mg/g, and adsorption rate is 9.9%.The wide-angle x-ray diffracting spectrum of the poly-o-phenylenediamine behind the absorption silver is seen Fig. 1, and Fig. 2 is seen in the analysis of XPS surface-element.As seen Xi Fu silver is mainly the simple substance attitude, and ionic state is also arranged, and the two weight ratio is 74/26.Under the same adsorption operations condition, use oxygen digital ratio instead and be respectively synthetic doping attitude poly-o-phenylenediamine under 2/1,3/1 condition, the gained loading capacity is respectively 447mg/g, 375mg/g, and adsorption rate is respectively 8.3%, 6.9%.
Embodiment 2
Get under oxygen digital ratio 1/1 condition synthetic attitude poly-o-phenylenediamine 50mg that goes to mix, 30 ℃ are dropped into the 25mL starting point concentrations down is in the silver ion solution of 100mmol/L mmol/L, stirring reaction 24h; After the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly-o-phenylenediamine silver ions being got loading capacity is 444mg/g, and adsorption rate is 8.2%.The XPS analysis of the poly-o-phenylenediamine behind the absorption silver is seen Fig. 3.As seen Xi Fu silver is simple substance attitude and ionic state coexistence, and the two weight ratio is 44/56.Under the same adsorption operations condition, use oxygen digital ratio instead and be respectively under 2/1,3/1 condition synthetic attitude poly m-phenylene diamine that goes to mix, the gained loading capacity is respectively 408mg/g, 371mg/g, and adsorption rate is respectively 7.6%, 6.9%.
Embodiment 3
Get synthetic doping attitude poly-o-phenylenediamine 50mg under oxygen digital ratio 1/1 condition, 30 ℃ are dropped into the 25mL starting point concentration down is in the silver ion solution of 43.1mmol/L, stirring reaction 0.5 hour, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can getting poly-o-phenylenediamine, silver ions is got loading capacity is 316mg/g, adsorption rate is 13.6%, XPS analysis shows that adsorbed silver is simple substance attitude and ionic state coexistence, and the two weight ratio is 51/49.Under the similarity condition, changing adsorption time was respectively 1 hour, 3 hours, 6 hours, 12 hours, 24 hours, the gained loading capacity is respectively 324mg/g, 332mg/g, 342mg/g, 370mg/g, 415mg/g, adsorption rate is respectively 13.9%, 14.3%, 14.7%, 15.9%, 17.8%, wherein the XPS analysis of the doping attitude poly-o-phenylenediamine of absorption silver after 24 hours shows, the adsorbed simple substance attitude that is mainly also has ionic state, and the two weight ratio is 61/39.
The equilibrium adsorption time is 24 hours in the time of can obtaining the silver ions of this adsorption treatment starting point concentration 43.1mmol//L thus, carries out the kinetics of adsorption simulation with accurate second-order kinetics equation, and the mimic relation conefficient is 0.9999, and standard deviation is 1.149 * 10
-4The initial adsorption rate constant h that simulation obtains is 5107mg/ (g.h).
Embodiment 4
Get synthetic doping attitude poly-o-phenylenediamine 50mg under oxygen digital ratio 1/1 condition, 30 ℃ are dropped into the 25mL starting point concentration down is in the silver ion solution of 1.24mmol/L, stirring reaction 10 hours, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can getting poly m-phenylene diamine, silver ions is got loading capacity is 65.7mg/g, adsorption rate is 99.1%, under the similarity condition, change initial concentration of silver ions and be respectively 2.50mmol/L, 5.00mmol/L, 10.8mmol/L, 21.6mmol/L, 43.1mmol/L, 100mmol/L, the gained loading capacity is respectively 109mg/g, 169mg/g, 276mg/g, 342mg/g, 415mg/g, 533mg/g, adsorption rate is respectively 81.2%, 63.1%, 47.5%, 29.4%, 17.8%, 9.9%.
Claims (3)
1, a kind of method that reclaims silver from Ag-containing solution is characterized in that adopting static adsorptive method, and silver ion adsorbant uses poly-o-phenylenediamine.
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 poly-o-phenylenediamine adding is contained in the silver ion solution, whip attachment 30 minutes-24 hours, wherein, containing the initial concentration of silver ions of silver ion solution is 1.24-100mmol/L, and poly-o-phenylenediamine is 1-3mg/mL with the proportioning that contains silver ion solution.
3, the method that reclaims silver from Ag-containing solution according to claim 1 is characterized in that described poly-o-phenylenediamine is the doping attitude or the attitude poly-o-phenylenediamine that goes to mix.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20030039605A1 (en) * | 2001-08-21 | 2003-02-27 | Edward Ramsay | Process for the recovery of precious metals from fine carbon |
| JP2003226923A (en) * | 2002-02-04 | 2003-08-15 | Mitsubishi Nuclear Fuel Co Ltd | Method of recovering silver |
| 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 |
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- 2007-03-08 CN CNB200710037915XA patent/CN100434547C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20030039605A1 (en) * | 2001-08-21 | 2003-02-27 | Edward Ramsay | Process for the recovery of precious metals from fine carbon |
| JP2003226923A (en) * | 2002-02-04 | 2003-08-15 | Mitsubishi Nuclear Fuel Co Ltd | Method of recovering silver |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 三聚氰胺对银离子的吸附性能. 黄美荣，李振宇，谢芸，李新贵.工业水处理，第26卷第1期. 2006 * |
| 含银废液来源及其回收方法. 黄美荣，李振宇，李新贵.工业用水与废水，第36卷第1期. 2005 * |
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Granted publication date: 20081119 Termination date: 20110308 |