CN103397189B - A kind of method of recover silver and other metal from Oily wastewater - Google Patents
A kind of method of recover silver and other metal from Oily wastewater Download PDFInfo
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- CN103397189B CN103397189B CN201310317378.XA CN201310317378A CN103397189B CN 103397189 B CN103397189 B CN 103397189B CN 201310317378 A CN201310317378 A CN 201310317378A CN 103397189 B CN103397189 B CN 103397189B
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Abstract
The invention discloses a kind of method of recover silver and other metal from Oily wastewater, the method comprises physical method treatment process, nitric acid dissolve operation, Separation and Recovery silver operation, Separation and Recovery tin operation, separating copper operation, reclaims nickel operation.The present invention all adopts wet recycling process process, all metals can also be reclaimed while the shortcoming avoiding traditional recovery process high energy consumption, high pollution, realizes low-cost high-efficiency and reclaims.
Description
Technical field
The present invention relates to metals resources reclaiming field, particularly a kind of method of recover silver and other metal from Oily wastewater.
Background technology
Silver has good electroconductibility and thermal conductivity, is widely used in the fields such as photograph, electric and electronic, plating and health care industry.In silver, add the performance that other alloy element can improve silver, such as, add the hardness that copper can improve silver, reduce fusing point, improve castability, the Application Areas of copper can be further expanded.
Along with increase that is silver-colored and silver alloys consumption, annual generation Oily wastewater is also increasing, and be worth from the regeneration of resource reutilization and silver, from Oily wastewater, recover silver and other metal, have significant economic and social benefit.
Generally pyrometallurgical recovery methods is adopted from recovery at present from Oily wastewater, such as patent (CN1940099A) discloses the treatment process of waste material containing copper, precious metal and/or sludge, and the method is ripe, and processing efficiency is high, but the method energy consumption is large, and environmental pollution is more serious.
Summary of the invention
The invention provides a kind of method of recover silver and other metal from Oily wastewater, achieve silver-colored waste material low cost, the recovery of high benefit.
The present invention discloses a kind of method of recover silver and other metal from Oily wastewater, comprises the following steps:
(1) physical method treatment process: Oily wastewater is pulverized, then sieves, obtaining screen underflow with the screening of 50-70 mesh standard sieve is powdered alloy;
(2) nitric acid leaches operation: step (1) gained powdered alloy is carried out nitric acid leaching, filters, obtains leach liquor;
(3) Separation and Recovery silver operation: the leach liquor obtained to step (2) adds hydrochloric acid and reacts, and react rear filtration and has obtained silver nitride precipitation and filtrate, silver chloride reduces with reductive agent and obtains silver powder after washing, pulp;
(4) Separation and Recovery tin operation: above-mentioned all filtrate is added ammoniacal liquor, filtration after reacting completely, washing obtain tindihydroxide precipitation and filtrate, and tindihydroxide precipitation is added diluted hydrochloric acid dissolution, obtain glass putty after dissolving is complete with zinc dust precipitation;
(5) Separation and Recovery copper process: step (4) gained filtrate is carried out extraction by extraction agent Lix984 and is extracted liquid and raffinate, extraction liquid obtains copper-bath after back extraction, then copper-bath condensing crystal is obtained copper sulfate product;
(6) reclaim nickel operation: step (5) gained raffinate is added sodium hydroxide solution, filter after reacting completely and obtain nickel hydroxide;
In described step (1), pulverized by Oily wastewater, then sieve, obtaining screen underflow with the screening of 50-70 mesh standard sieve is powdered alloy, and described standard sieve is preferably 60 orders.
In described step (2), nitric acid mass concentration is (2.5-1): 1, controls to leach terminal pH value at 0.5-2, and keep certain stirring velocity, temperature of reaction is 50-90 DEG C, and the reaction times is 1-3 hour.
Main chemical reactions is as follows:
3Ag+4HNO
3→3AgNO
3+2H
2O+NO↑
3Sn+8HNO
3→3Sn(NO
3)2+2NO↑+4H
2O
3Cu+8HNO
3→3Cu(NO
3)2+2NO↑+4H
2O
3Ni+8HNO
3→3Ni(NO
3)2+2NO↑+4H
2O
In step (2), the concentration of nitric acid, consumption, temperature of reaction, stirring intensity, in the reaction times, liquid-solid ratio etc. directly can affect silver leaching rate.Test-results shows, when concentration of nitric acid is 1: 1, temperature of reaction is 60 DEG C, and reactor stirring velocity is 110 revs/min, and the reaction times is 3 hours, and liquid-solid ratio is 4: 1, silver leaching yield be 99.7% and more than.
In described step (3), hydrochloric acid add-on is 1.05-1.2 times of theoretical requirement, the slurrying of silver nitride precipitation water is transferred to 9-11 PH, reductive agent is hydrazine hydrate or hydrazine hydrate: ammoniacal liquor: water is (1-2.5): (3-5.5): the ammonia-hydrazine hydrate mixed solution of (8: 15), reduction temperature 30-90 DEG C, recovery time is 1-3 hour, and after reduction, filtration washing obtains silver powder.
Main chemical reactions is as follows:
Ag
++Cl
-→AgCl↓
4AgCl+5N
2H
4+H2O→4Ag↓+4N
2H
5Cl+N
2↑+5H
2O
In step (3), hydrochloric acid add-on, stirring intensity, temperature of reaction, reaction times, the pH value of reduction silver, reductive agent consumption, also the reaction times etc. directly can have influence on the rate of recovery of silver, test-results shows, when 1.05 times that hydrochloric acid add-on is theoretical requirement, stirring velocity is 100 revs/min, temperature of reaction is 60 DEG C, reaction times is 2 hours, the silver nitride precipitation slurrying obtained after filtration washing also adjusts pH value to 10, with hydrazine hydrate or hydrazine hydrate: ammoniacal liquor: water is that the ammonia-hydrazine hydrate mixed solution of 1: 3: 8 is as reductive agent, silver powder part rate of recovery is the highest.
In described step (4), add ammoniacal liquor and make filtrate pH value reach 2.5-3.5, used salt acid concentration is 1-5mol/L, during replacement(metathesis)reaction, keep certain stirring velocity, zinc powder consumption is 1.1-1.3 times of theoretical amount, temperature 30-90 DEG C, time 1-3 hour.
Main chemical reactions is as follows:
2H
++Sn(OH)
2→Sn
2++2H
2O
Sn
2++Zn→Sn↓+Zn
2+
In step (4), zinc powder consumption, stirring intensity, temperature of reaction, the reaction times directly has influence on the rate of recovery of tin, and test-results shows, precipitate with 5.0mol/L dissolving with hydrochloric acid tindihydroxide, go out tin with zinc dust precipitation again, zinc powder consumption is 1.1 times of theoretical amount, and stirring velocity is 80 revs/min, temperature of reaction is 60 DEG C, reaction times is 3 hours, and filtration washing obtains glass putty after drying, and the glass putty rate of recovery is the highest.
In step (5), in lix984 extraction process, organic phase composition, extraction progression, extraction form etc. all directly affect the recovery of copper, test-results shows, organic phase consists of 25%1ix984+75% sulfonated kerosene, adopt 5 stage countercurrents extractions, in solution the percentage extraction of copper reach 99.2% and more than.
In described step (6), add sodium hydroxide solution and make solution pH value reach 10.0-11.0, keep certain stirring intensity, temperature of reaction 30-90 DEG C, reaction times 30-60min.
Main chemical reactions is as follows:
Ni
2++2OH
-→Ni(OH)
2↓
In step (6), stirring intensity temperature of reaction, the reaction times directly has influence on the deposition rate of nickel, and test-results shows, stirring velocity is 120 revs/min, and temperature of reaction is 60 DEG C, and the reaction times is the deposition rate obtaining nickel for 1 hour is 99.5%.
In the present invention, all with wet processing process Oily wastewater, realize high-level efficiency, low cost, low stain reclaims.Wherein the rate of recovery of silver reaches more than 98.2%, and the tin rate of recovery reaches more than 97.5%, and copper recovery reaches more than 98.4%, and nickel recovery reaches more than 98.3%.
Accompanying drawing explanation
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1:
The first step: get 20Kg Oily wastewater and pulverize, with 60 mesh standard sieve screenings after pulverizing, obtains containing alloy for dental amalgam, after testing argentiferous 54.4% in alloy powder, copper 23.1%, tin 11.7%, nickel 10.8%.
Second step: joined in the reactor of liner tetrafluoroethylene of 100 liters containing alloy for dental amalgam by 10Kg, add 40 premium on currency, temperature of reaction is set to 60 DEG C, stirring velocity is 110 revs/min, in still, then constantly adds the nitric acid of 1: 1, carry out nitric acid leaching, reaction times controls at 2 hours, terminal PH controls 2, filters leach liquor, by leach liquor constant volume to 50L, argentiferous 107.71g/L in leach liquor after testing, copper 45.64g/L, tin 23.07g/L, nickel 21.23g/L.
3rd step: leach liquor is joined in the reactor of liner tetrafluoroethylene of 100 liters, temperature of reaction is set to 60 DEG C, and stirring velocity is 100 revs/min, and the add-on of hydrochloric acid is 1.05 times of theoretical amount, reaction times is 2 hours, then filtration washing obtains silver nitride precipitation, prepares silver chloride slurrying with water, and regulates pH value to 10 with ammoniacal liquor, with 40% hydrazine hydrate reduction silver chloride, obtain silver powder, obtain silver ingot after drying founding, the purity of silver is 99.1%.
4th step: filtrate obtained in the previous step is added ammoniacal liquor and regulate PH to 3, filtration washing obtains tindihydroxide precipitation, with the anti-molten tindihydroxide of 5mol/L hydrochloric acid, obtain tin chloride solution, join in tin chloride solution with the zinc powder of theoretical amount 1.1 times, stirring velocity is 80 revs/min, and temperature of reaction is 60 DEG C, reaction times is 3 hours, and the glass putty purity through zinc dust precipitation gained is 99.2%.
5th step: filtrate obtained in the previous step and Lix984 organic phase are extracted, wherein organic phase consists of 25%lix984+75% sulfonated kerosene, adopts 5 stage countercurrent extractions, in solution, the percentage extraction of copper reaches 99.6%, copper sulfate is obtained after the back extraction of 2.0mol/L sulfuric acid, again copper-bath condensing crystal is obtained copper sulfate product, copper sulfate purity is 99.7%.
6th step: filtrate obtained in the previous step is added sodium hydroxide solution and regulate PH to 10, stirring velocity is 120 revs/min, and temperature of reaction is 60 DEG C, and the reaction times is 1 hour, and the deposition rate obtaining nickel hydroxide is 99.5%.
Embodiment 2:
The first step: get 20Kg Oily wastewater and pulverize, with 70 mesh standard sieve screenings after pulverizing, obtains containing alloy for dental amalgam, after testing argentiferous 50.6% in alloy powder, copper 23.5%, tin 11.6%, nickel 11.8%, and other materials.
Second step: 10Kg is joined in the reactor of liner tetrafluoroethylene of 100 liters containing alloy for dental amalgam, add 40 premium on currency, temperature of reaction is set to 80 DEG C, stirring velocity is 110 revs/min, in still, then constantly adds the nitric acid of 2.5: 1, carry out nitric acid leaching, reaction times controls at 1.5 hours, terminal PH controls 1.5, filters leach liquor, by leach liquor constant volume to 50L.
3rd step: will join in the reactor of liner tetrafluoroethylene of 100 liters in leach liquor, temperature of reaction is set to 80 DEG C, stirring velocity is 100 revs/min, hydrochloric acid add-on is 1.2 times of theoretical amount, reaction times is 3 hours, then filtration washing obtains silver nitride precipitation, silver chloride slurrying is prepared with water, and regulate pH value to 10 with ammoniacal liquor, with hydrazine hydrate: ammoniacal liquor: water is the ammonia-hydrazine hydrate mixed solution Reduction of Silver Chloride of 1: 3: 8, obtain silver powder, obtain silver ingot after drying founding, the purity of silver is 99.2%.
4th step: filtrate obtained in the previous step is added ammoniacal liquor and regulate PH to 3.5, filtration washing obtains tindihydroxide precipitation, with the anti-molten tindihydroxide of 3mol/L hydrochloric acid, obtain tin chloride solution, join in tin chloride solution with the zinc powder of theoretical amount 1.2 times, stirring velocity is 80 revs/min, and temperature of reaction is 80 DEG C, reaction times is 2 hours, and the glass putty purity through zinc dust precipitation gained is 99.1%.
5th step: filtrate obtained in the previous step and Lix984 organic phase are extracted, wherein organic phase consists of 25%lix984+75% sulfonated kerosene, adopts 5 stage countercurrent extractions, in solution, the percentage extraction of copper reaches 99.6%, copper sulfate is obtained after the back extraction of 2.0mol/L sulfuric acid, again copper-bath condensing crystal is obtained copper sulfate product, copper sulfate purity is 99.7%.
6th step: filtrate obtained in the previous step is added sodium hydroxide solution and regulate PH to 11.0, stirring velocity is 120 revs/min, and temperature of reaction is 90 DEG C, and the reaction times is 50min, and the deposition rate obtaining nickel hydroxide is 99.6%.
In sum; although the specific embodiment of the present invention is to invention has been detailed description; but persons skilled in the art should be understood that; above-described embodiment is only the description to the preferred embodiments of the present invention; but not limiting the scope of the invention; persons skilled in the art are in the technical scope disclosed by the present invention, and the change that can expect easily, all within protection scope of the present invention.
Claims (9)
1. the method for recover silver and other metal from Oily wastewater, is characterized in that comprising the following steps:
(1) physical method treatment process: Oily wastewater is pulverized, then sieves, obtaining screen underflow with the screening of 50-70 mesh standard sieve is powdered alloy;
(2) nitric acid leaches operation: step (1) gained powdered alloy is carried out nitric acid leaching, filters, obtains leach liquor;
(3) Separation and Recovery silver operation: the leach liquor obtained to step (2) adds hydrochloric acid and reacts, react rear filtration and obtain silver nitride precipitation and filtrate, silver chloride obtains silver powder with reductive agent reduction filtration washing after washing, pulp, wherein hydrochloric acid add-on is 1.05-1.2 times of theoretical requirement, precipitation reaction temperature 30-90 DEG C, the precipitin reaction time is 1-3 hour, the slurrying of silver nitride precipitation water is transferred to 9-11 PH, and reductive agent is hydrazine hydrate: ammoniacal liquor: water is (1-2.5): (3-5.5): the ammonia-hydrazine hydrate mixed solution of (8-15);
(4) Separation and Recovery tin operation: above-mentioned all filtrate is added ammoniacal liquor, filtration after reacting completely, washing obtain tindihydroxide precipitation and filtrate, and tindihydroxide precipitation is added diluted hydrochloric acid dissolution, obtain glass putty after dissolving is complete with zinc dust precipitation;
(5) Separation and Recovery copper process: step (4) gained filtrate is carried out extraction by Lix984 extraction agent and is extracted liquid and raffinate, extraction liquid obtains copper-bath after back extraction, then copper-bath condensing crystal is obtained copper sulfate product;
(6) reclaim nickel operation: step (5) gained raffinate is added sodium hydroxide solution, filter after reacting completely and obtain nickel hydroxide.
2. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, it is characterized in that: in described step (1), described standard sieve is 60 orders.
3. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, it is characterized in that: in described step (2), nitric acid mass concentration is (2.5-1): 1, control to leach terminal pH value at 0.5-2, keep certain stirring velocity, temperature of reaction is 50-90 DEG C, and the reaction times is 1-3 hour.
4. the method for recover silver and other metal from Oily wastewater as claimed in claim 3, it is characterized in that: in step (2), temperature of reaction is 60 DEG C, and stirring velocity is 110 revs/min, and the reaction times is 3 hours.
5. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, it is characterized in that: in step (3), hydrochloric acid add-on is 1.05 times of theoretical requirement, precipitation reaction temperature is 60 DEG C, the precipitin reaction time is 2 hours, the slurrying of silver nitride precipitation water is transferred to 10 PH, with hydrazine hydrate: ammoniacal liquor: water is that the ammonia-hydrazine hydrate mixed solution of 1:3:8 is as reductive agent.
6. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, it is characterized in that: in described step (4), adding ammoniacal liquor makes filtrate pH value reach 2.5-3.5, used salt acid concentration is 1-5mol/L, during replacement(metathesis)reaction, keep certain stirring velocity, zinc powder consumption is 1.1-1.3 times of theoretical amount, temperature 30-90 DEG C, time 1-3 hour.
7. the method for recover silver and other metal from Oily wastewater as claimed in claim 6, it is characterized in that: in step (4), regulate filtrate pH value to 3.0 with ammoniacal liquor, used salt acid concentration is 5mol/L, zinc powder consumption is 1.1 times of theoretical amount, and stirring velocity is 80 revs/min, and temperature of reaction is 60 DEG C, reaction times is 3 hours, and filtration washing obtains glass putty after drying.
8. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, is characterized in that: in step (5), and organic phase consists of 25%lix984+75% sulfonated kerosene, adopts 5 stage countercurrent extractions.
9. the method for recover silver and other metal from Oily wastewater as claimed in claim 1, it is characterized in that: in described step (6), adding sodium hydroxide solution makes solution pH value reach 10.0-11.0, keep certain stirring intensity, temperature of reaction 30-90 DEG C, reaction times 30-60min.
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| CN104651615A (en) * | 2015-01-28 | 2015-05-27 | 昆山全亚冠环保科技有限公司 | Method for recovering silver and palladium from waste |
| CN106119565B (en) * | 2016-06-22 | 2017-09-22 | 湖南大学 | A kind of method of the leaching of manganese from manganese-silver ore and silver production manganese sulfate and silver |
| CN106521176B (en) * | 2016-10-28 | 2019-02-22 | 胡志 | A method of silver is extracted with useless conductive silver glue |
| CN106702166A (en) * | 2017-02-06 | 2017-05-24 | 温州中希电工合金有限公司 | Method for recycling silver in high oil-bearing sludge |
| CN107574313A (en) * | 2017-08-25 | 2018-01-12 | 金川集团股份有限公司 | A kind of method that silver is reclaimed in the electronics support from argentiferous |
| CN108007816A (en) * | 2017-12-18 | 2018-05-08 | 清远先导材料有限公司 | The detection method of active metal simple substance in a kind of hard zinc |
| CN108149018B (en) * | 2017-12-31 | 2019-07-02 | 西北有色金属研究院 | The recovery method of Ag in a kind of Bi system superconducting line strips |
| CN108480647B (en) * | 2018-01-23 | 2022-01-18 | 珠海纳金科技有限公司 | Recycling method of nano-silver particle waste liquid |
| CN109536726A (en) * | 2019-01-14 | 2019-03-29 | 北京科技大学 | A kind of recovery method of argentiferous dead catalyst |
| CN111118289B (en) * | 2019-10-16 | 2021-07-30 | 福达合金材料股份有限公司 | Method for recovering and treating silver tungsten carbide graphite waste |
| CN111455182A (en) * | 2020-04-24 | 2020-07-28 | 金川集团股份有限公司 | Method for separating and extracting silver, palladium and ruthenium from waste catalyst |
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| KR20020057939A (en) * | 2002-06-26 | 2002-07-12 | 박종진 | Precious metals abstraction means from electronic scrap |
| CN101126129A (en) * | 2007-09-07 | 2008-02-20 | 金川集团有限公司 | Method for removing copper from nickel chloride leachate |
| CN102775197B (en) * | 2012-08-13 | 2014-06-11 | 深圳市危险废物处理站有限公司 | Method for preparing fertilizer-grade ammonium nitrate concentrated solution by use of mother liquid after immersion tin of tin-stripping waste liquid of circuit board |
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