CN101016587A - Method of reclaiming silver from silver containing solution by poly m-phenylenediamine as adsorbent - Google Patents
Method of reclaiming silver from silver containing solution by poly m-phenylenediamine as adsorbent Download PDFInfo
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- CN101016587A CN101016587A CNA2007100379164A CN200710037916A CN101016587A CN 101016587 A CN101016587 A CN 101016587A CN A2007100379164 A CNA2007100379164 A CN A2007100379164A CN 200710037916 A CN200710037916 A CN 200710037916A CN 101016587 A CN101016587 A CN 101016587A
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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 m-phenylenediamine as sorbent; adding poly m-phenylenediamine into silver ion solution with initial concentration at 0.5-102mmol/L; stirring; absorbing 10min-144h; 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 poly m-phenylene diamine reclaims silver from Ag-containing solution as silver ion adsorbant method.
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, but these traditional method ubiquities power consumptions 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 Jinyuan. 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 contain silver ion 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 m-phenylene diamine.Poly m-phenylene diamine can adopt chemical oxidative polymerization synthetic, contain on it can with the NH-of silver ions generation complexing action or redoxomorphism, NH
2-group.
Static adsorptive method of the present invention, concrete steps are as follows:
The poly m-phenylene diamine adding is contained in the silver ion solution, and whip attachment 10 minutes-144 hours is filtered then; Wherein, the starting point concentration that contains silver ion solution is 0.5-102mmol/L, and the consumption of poly m-phenylene diamine 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 m-phenylene diamine, 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 0.5～102mmol/L, the consumption of poly m-phenylene diamine is 1-3mg/mL with the ratio that contains silver ion solution, and adsorption time is 10 minutes～144 hours.Sorbent material can be the doping attitude or the attitude of going to mix.
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: the poly m-phenylene diamine price is lower, analytically pure poly m-phenylene diamine only is 0.3 a yuan/gram, the consumption of oxygenant ammonium persulphate is taken into account, the cost of absorption one gram silver only is 1.56 yuan, well below poly-(1,8 naphthylene diamines) be used as the cost of silver ion adsorbant, and be lower than the price of silver on the market.And as a kind of industrial raw material, poly m-phenylene diamine is scale operation at home also, if adopt the raw material of other poly m-phenylene diamine of technical pure level as the preparation silver ion adsorbant, the cost of then every absorption one gram silver is expected to be reduced to below 0.3 yuan, suitable with gac as the cost of silver ion adsorbant, and it is easy to operate, thereby have broad application prospects, specifically can contain the silver recovery processing of silver ions waste liquid with wasted fixing solution, electroplating effluent, chemical analysis waste liquid, test waste liquid etc.
Description of drawings
Fig. 1 is absorption of synthetic doping attitude poly m-phenylene diamine and the wide-angle x-ray diffracting spectrum of 102mmol/L silver ions after 24 hours under 1/1 condition for oxygen digital ratio.
Fig. 2 is synthetic go to mix attitude poly m-phenylene diamine absorption and the wide-angle x-ray diffracting spectrum of 102mmol/L silver ions after 24 hours under 1/1 condition for oxygen digital ratio.
Fig. 3 is the XPS collection of illustrative plates behind the synthetic doping attitude poly m-phenylene diamine suction silver under 0.5/1 condition for oxygen digital ratio.
Fig. 4 is that the synthetic attitude poly m-phenylene diamine that goes to mix is inhaled XPS collection of illustrative plates behind the silver under 3/1 condition for oxygen digital ratio.
Embodiment
Embodiment 1
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 1/1 condition, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 102mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 386mg/g, and adsorption rate is 6.8%.The wide-angle x-ray diffracting spectrum of the poly m-phenylene diamine behind the suction silver is seen Fig. 1, and the silver of visible absorption is mainly the simple substance attitude.Under the same adsorption operations condition, use oxygen digital ratio instead and be respectively synthetic doping attitude poly m-phenylene diamine under 0.5/1,2/1,3/1 condition, the gained loading capacity is respectively 494mg/g, 275mg/g, and 235mg/g, adsorption rate is respectively 8.9%, 5%, and 4.3%.
Embodiment 2
Get under oxygen digital ratio 1/1 condition synthetic attitude poly m-phenylene diamine 50mg that goes to mix, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 102mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 358mg/g, adsorption rate is 6%, and the wide-angle x-ray diffracting spectrum of the poly m-phenylene diamine behind the suction silver is seen Fig. 2, and the silver of visible absorption is mainly the simple substance attitude.Under the same adsorption operations condition, use oxygen digital ratio instead and be respectively under 0.5/1,2/1,3/1 condition synthetic attitude poly m-phenylene diamine that goes to mix, the gained loading capacity is respectively 411mg/g, 306mg/g, and 260mg/g, adsorption rate is respectively 7.4%, 5.5%, and 4.7%.
Embodiment 3
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 0.5/1 condition, stirring reaction is 24 hours in the silver ion solution of 30 ℃ of following input 25mL starting point concentration 42.92mmol/L, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 317mg/g, adsorption rate is 13.7%, and the XPS of the poly m-phenylene diamine behind the suction silver sees Fig. 3.As seen Xi Fu silver is mainly the simple substance attitude, and ionic state is also arranged, and the two weight ratio is 76/24.Under the similarity condition, the change adsorption time is 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 12 hours, 48 hours, 72 hours, 144 hours respectively, the gained loading capacity is respectively 125mg/g, 135mg/g, 156mg/g, 189mg/g, 227mg/g, 255mg/g, 394mg/g, 489mg/g, 625mg/g, and adsorption rate is respectively 5.45%, 5.89%, 6.78%, 8.24%, 9.84%, 12.2%, 20.8%, 25.8%, 33%.
The equilibrium adsorption time is 144 hours in the time of can obtaining the silver ions of this adsorption treatment starting point concentration 42.92mmol//L thus, carries out the kinetics of adsorption simulation with accurate second-order kinetics equation, and the mimic relation conefficient is 0.9981, and standard deviation is 4.8688 * 10
-4。The initial adsorption rate constant h that simulation obtains is 1018 mg/ (g.h).
Embodiment 4
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 1/1 condition, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 232mg/g, and adsorption rate is 10%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 48 hours, 72 hours, the gained loading capacity is respectively 120mg/g, 130mg/g, 135mg/g, 146mg/g, 155mg/g, 250mg/g, 256mg/g, and adsorption rate is respectively 5.22%, 5.66%, 5.88%, 6.35%, 6.75%, 10.6%, 11.2%.
Embodiment 5
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 2/1 condition, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 165mg/g, and adsorption rate is 6.9%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 48 hours, the gained loading capacity be respectively 125mg/g, 135mg/g, 137mg/g, 140mg/g, 143mg/g, 170mg/g,, adsorption rate is respectively 5.3%, 5.66%, 5.74%, 5.87%, 6%, 7.1%.
Embodiment 6
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 3/1 condition, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 160mg/g, and adsorption rate is 6.9%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 48 hours, the gained loading capacity is respectively 133mg/g, 143mg/g, 148mg/g, 150mg/g, 152mg/g, 163mg/g, and adsorption rate is respectively 5.7%, 6.13%, 6.34%, 6.43%, 6.52%, 7%.
Embodiment 7
Get under oxygen digital ratio 0.5/1 condition synthetic attitude poly m-phenylene diamine 50mg that goes to mix, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 215mg/g, and adsorption rate is 11.4%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 48 hours, 72 hours, 144 hours, the gained loading capacity is respectively 133mg/g, 143mg/g, 147mg/g, 182mg/g, 198mg/g, 242mg/g, 283mg/g, 326mg/g, and adsorption rate is respectively 5.77%, 6.2%, 6.4%, 7.9%, 8.6%, 12.8%, 15%, 17.3%.
Embodiment 8
Get under oxygen digital ratio 1/1 condition synthetic attitude poly m-phenylene diamine 50mg that goes to mix, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 216mg/g, and adsorption rate is 9.3%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 3 hours, 6 hours, 48 hours, 72 hours, the gained loading capacity is respectively 150mg/g, 161mg/g, 172mg/g, 179mg/g, 228mg/g, 240mg/g, and adsorption rate is respectively 4.13%, 7%, 7.48%, 7.78%, 10%, 10.5%.
Embodiment 9
Get under oxygen digital ratio 2/1 condition synthetic attitude poly m-phenylene diamine 50mg that goes to mix, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 190mg/g, and adsorption rate is 8.15%.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 48 hours, the gained loading capacity is respectively 145mg/g, 150mg/g, 157mg/g, 161mg/g, 165mg/g, 197mg/g, and adsorption rate is respectively 6.57%, 6.7%, 6.74%, 6.91%, 7.08%, 8.46%.
Get under oxygen digital ratio 3/1 condition synthetic attitude poly m-phenylene diamine 50mg that goes to mix, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, after the filtration, analyze remaining silver ion content in the filtrate with Fo Erhadefa, can this poly m-phenylene diamine silver ions being got loading capacity is 188mg/g, adsorption rate is 8.4%, and the XPS of the poly m-phenylene diamine behind the suction silver sees Fig. 4.As seen Xi Fu silver is mainly the simple substance attitude, and ionic state is also arranged, and the two weight ratio is 80/20.Under the similarity condition, change adsorption time and be respectively 10 minutes, half an hour, 1 hour, 3 hours, 6 hours, 12 hours, 48 hours, the gained loading capacity is respectively 150mg/g, 155mg/g, 160mg/g, 165mg/g, 170mg/g, 178mg/g, 192mg/g, and adsorption rate is respectively 6.77%, 7%, 7.3%, 7.4%, 7.6%, 7.8%, 8.8%.
Embodiment 11
Get synthetic doping attitude poly m-phenylene diamine 50mg under oxygen digital ratio 0.5/1 condition, stirring reaction 24h in the silver ion solution of input 25mL starting point concentration 42.92mmol/L under 30 ℃, 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 317mg/g, adsorption rate is 13.7%, under the similarity condition, change initial concentration of silver ions and be respectively 0.5mmol/L, 2.5mmol/L, 5mmol/L, 10.77mmol/L, 21.55mmol/L, 102mmol/L, the gained loading capacity is respectively 26.9mg/g, 62.4mg/g, 113mg/g, 197mg/g, 250mg/g, 494mg/g, adsorption rate is respectively 99.57%, 46.4%, 42.1%, 33.9%, 21.5%, 8.9%.
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 m-phenylene diamine.
2, the method that reclaims silver from Ag-containing solution according to claim 1 is characterized in that the concrete steps of described static adsorptive method are as follows: poly m-phenylene diamine is added contain in the silver ion solution whip attachment 10 minutes-144 hours, filtration then; Wherein, the starting point concentration that contains silver ion solution is 0.5-102mmol/L, and the consumption of poly m-phenylene diamine 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 m-phenylene diamine is the doping attitude or the attitude poly m-phenylene diamine that goes to mix.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432084A (en) * | 2011-11-09 | 2012-05-02 | 中南大学 | Application method of polymetaphenylene diamine adsorbent to treatment of sexivalent-Cr-containing acidic wastewater |
| CN102923825A (en) * | 2012-11-12 | 2013-02-13 | 常州大学 | Application of poly m-phenylenediamine |
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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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432084A (en) * | 2011-11-09 | 2012-05-02 | 中南大学 | Application method of polymetaphenylene diamine adsorbent to treatment of sexivalent-Cr-containing acidic wastewater |
| CN102923825A (en) * | 2012-11-12 | 2013-02-13 | 常州大学 | Application of poly m-phenylenediamine |
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