CN115286143A - Method for recovering silver from silver-containing waste liquid - Google Patents
Method for recovering silver from silver-containing waste liquid Download PDFInfo
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- CN115286143A CN115286143A CN202210991088.2A CN202210991088A CN115286143A CN 115286143 A CN115286143 A CN 115286143A CN 202210991088 A CN202210991088 A CN 202210991088A CN 115286143 A CN115286143 A CN 115286143A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C22B11/042—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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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
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Abstract
The application discloses a method for recovering silver from silver-containing waste liquid, which comprises the following steps: step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water, firstly generating brown precipitate in the solution, dissolving the precipitate along with dropwise adding of the ammonia water, changing the solution into a colorless and transparent solution again, and continuously stirring; step two, silver oxide synthesis reaction: keeping stirring, adding a sodium hydroxide solution into the precipitation kettle, standing, starting stirring again, and heating the solution to control the pH value; step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters; step four, washing: and unloading the filter cake into a washing tank, and repeatedly washing the filter cake with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm. The method has the advantages of short process flow and simple operation, and can treat the silver-containing wastewater in a large scale.
Description
Technical Field
The invention relates to the field of hydrometallurgy recovery, in particular to a method for recovering silver from silver-containing waste liquid.
Background
In the production process of silver nitrate, a plurality of heating processes are involved, particularly in an evaporation concentration section, a large amount of silver-containing distillate is generated, the silver content of the distillate is 500-800mg/L, although a part of clean silver-containing distillate can be used for replacing pure water as feeding water, the production amount of the silver-containing distillate is far larger than the feeding consumption amount, and in the industrial production of the silver nitrate, the cleaning of equipment can also generate a plurality of silver-containing washing water, wherein silver mainly exists in the form of silver ions. Silver is a precious metal and it is important to recover silver from silver-containing solutions. The method for recovering silver from silver-containing waste liquid mainly comprises a precipitation method, an electrolysis method, a reduction substitution method, an ion exchange method and an adsorption method, wherein the method for recovering silver from the silver-containing waste liquid by the precipitation method is to add proper anions into a silver-containing solution to enrich the silver in the waste liquid in a precipitation form, obtain silver precipitates after filtration, washing and drying, then mix the precipitates with a certain amount of sodium carbonate and roast the precipitates at about 1100 ℃ to obtain simple substance silver. The precipitation method comprises a silver sulfide precipitation method and a silver chloride precipitation method. However, both the silver sulfide precipitation method and the silver chloride precipitation method have the defects of complex operation methods, more chemicals used in the processes, long period and the like.
Disclosure of Invention
In view of the problems in the prior art, it is an object of the present disclosure to provide a method for recovering silver from a silver-containing waste liquid.
In order to achieve the above object, the present disclosure provides a method for recovering silver from a silver-containing waste liquid, comprising the steps of: step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water, wherein brown precipitate appears in the solution at first, the precipitate is dissolved along with the dropwise adding of the ammonia water, the solution is changed into a colorless transparent solution again, and continuously stirring for 10-30 min; step two, silver oxide synthesis reaction: keeping stirring, adding sodium hydroxide solution into the precipitation kettle, standing, starting stirring again, heating the solution to 60-80 ℃, and controlling the pH value to be 11.5-12.5; step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters; step four, washing: and unloading the filter cake into a washing tank, and repeatedly washing the filter cake with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm.
In some embodiments, in step one, the ammonia is added dropwise at a rate of: 1L/h-5L/h.
In some embodiments, in step one, the concentration of ammonia added is 5 to 10mol/L.
In some embodiments, in step two, the rate of addition of the sodium hydroxide solution is: 1-5L/h.
In some embodiments, in step two, the concentration of the sodium hydroxide solution added is 3 to 5mol/L.
In some embodiments, in step two, the mass ratio of Ag to NaOH is 1.15: 1.
In some embodiments, in step two, the stirring is again turned on for 10-20min.
The beneficial effects of this disclosure are as follows:
the method disclosed by the invention has the advantages that the recovery rate of noble metals is improved, the yield of a production line is improved, and meanwhile, the concentration of silver ions in the waste liquid reaches the relevant pollution discharge standard.
Detailed Description
The method for recovering silver from a silver-containing waste liquid according to the present disclosure is explained in detail below.
The application discloses a method for recovering silver from silver-containing waste liquid, which comprises the following steps: step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water, wherein brown precipitate appears in the solution at first, the precipitate is dissolved along with the dropwise adding of the ammonia water, the solution is changed into a colorless transparent solution again, and continuously stirring for 10-30 min; step two, silver oxide synthesis reaction: keeping stirring, adding sodium hydroxide solution into the precipitation kettle, standing, starting stirring again, heating the solution to 60-80 ℃, and controlling the pH value to be 11.5-12.5; step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters; step four, washing: and (4) unloading the filter cake into a washing tank, and repeatedly washing with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm.
This application is through silver ion joining in marriage ammonia in the given waste water, then the dropwise add speed of control stirring speed and sodium hydroxide solution, and the size that can effectively increase the precipitate is easily filtered, and makes the silver precipitation in the waste liquid more thorough, improves the rate of recovery of silver, can ensure that the silver ion content in the synthetic waste liquid is less than 0.5ppm to the silver of form recovery of silver oxide, its purity is high.
In the first step, ammonia water is dripped into the silver-containing wastewater, brown precipitate appears in the solution at first, the precipitate is dissolved along with the dripping of the ammonia water, and the solution is changed into colorless and transparent solution again.
In some embodiments, in step one, the rate of dropwise addition of aqueous ammonia is: 1L/h-5L/h. The recovery efficiency is influenced by too slow dripping and too long time, and the conversion of silver ions is influenced if the dripping is insufficient, so that the recovery rate is influenced; the dropping is too fast, the ammonia water is easy to be excessive, the release of silver ions can be inhibited, and the yield of the silver oxide can be influenced.
In some embodiments, in step one, the concentration of ammonia added is 5 to 10mol/L. The silver oxide generated by too low concentration is too small in size and difficult to recover completely, and the amount of waste water is greatly increased; if the concentration is too high, local NH is generated 3 The excessive silver ions are easy to be excessive and are excessively complexed, so that the release of the silver ions is influenced.
In some embodiments, in step two, the rate of addition of the sodium hydroxide solution is: 1-5L/h. The recovery efficiency is influenced if the dripping speed is too slow and the time is too long, and the conversion of silver ions is influenced if the dripping speed is insufficient, so that the recovery rate is influenced; the dropping is too fast, the sodium hydroxide is easy to be excessive, and the pH value is too high, so that other impurities in the solution are precipitated together, and the purity of the silver oxide is influenced.
In some embodiments, in step two, the sodium hydroxide solution is added at a concentration of 3 to 5mol/L. The silver oxide generated by too low concentration is too small in size and difficult to recover completely, and meanwhile, the amount of wastewater is greatly increased; if the concentration is too high, the local OH - The excessive silver oxide is easy to cause the local impurity ions to be precipitated together with the silver oxide, and the purity of the silver oxide is influenced.
In some embodiments, in step two, the mass ratio of Ag to NaOH is 1.15: 1. The proportion can lead the sodium hydroxide and the silver ammonia ions in the wastewater to generate silver oxide.
In some embodiments, in step two, the agitation is again turned on for 10-20min.
[ test ]
Example 1
Step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water with the concentration of 8mol/L, firstly generating brown precipitate in the solution, dissolving the precipitate along with dropwise addition of the ammonia water, changing the solution into a colorless transparent solution again, and continuously stirring for 10min;
step two, silver oxide synthesis reaction: keeping stirring, adding a sodium hydroxide solution into the precipitation kettle, wherein the concentration of the sodium hydroxide solution is 4mol/L, starting to generate silver oxide in the wastewater, continuously dropwise adding the sodium hydroxide solution until the pH value of the solution is 11.87, standing for 1h, starting stirring again, and heating the solution to 80 ℃;
step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters;
step four, washing: and unloading the filter cake into a washing tank, and repeatedly washing with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm to obtain the silver oxide, wherein the silver concentration of the silver oxide synthetic waste liquid is 0.43mg/l, and the recovery rate of the silver is 99.91%.
Example 2
Step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water with the concentration of 10mol/L, firstly generating brown precipitate in the solution, dissolving the precipitate along with dropwise adding the ammonia water, changing the solution into a colorless transparent solution again, and continuously stirring for 10min;
step two, silver oxide synthesis reaction: keeping stirring, adding a sodium hydroxide solution into the precipitation kettle, wherein the concentration of the sodium hydroxide solution is 5mol/L, starting to generate silver oxide in the wastewater, continuously dropwise adding the sodium hydroxide solution until the pH of the solution is 11.91, standing for 1h, starting stirring again, and heating the solution to 80 ℃;
step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters;
step four, washing: and unloading the filter cake into a washing tank, and repeatedly washing with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm to obtain the silver oxide, wherein the silver concentration of the silver oxide synthetic waste liquid is 0.38mg/l, and the recovery rate of the silver is 99.94%.
Example 3
Step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, wherein the silver content of the wastewater is 672.25mg/1, starting stirring, then dropwise adding ammonia water with the concentration of 7mol/L, firstly generating brown precipitate in the solution, dissolving the precipitate along with dropwise adding of the ammonia water, changing the solution into a colorless transparent solution again, and continuing stirring for 10min;
step two, silver oxide synthesis reaction: keeping stirring, adding a sodium hydroxide solution into the precipitation kettle, wherein the concentration of the sodium hydroxide solution is 3mol/L, starting to generate silver oxide in the wastewater, continuously dropwise adding the sodium hydroxide solution until the pH of the solution is 11.83, standing for 1h, starting stirring again, and heating the solution to 80 ℃;
step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters;
step four, washing: and (3) unloading the filter cake into a washing tank, and repeatedly washing with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm to obtain the silver oxide, wherein the silver concentration of the silver oxide synthetic waste liquid is 0.40mg/l, and the recovery rate of the silver is 99.94%.
As can be seen from the above examples, the recovery method of the present application recovers silver in the form of silver oxide with high purity and high recovery rate.
The above-disclosed features are not intended to limit the scope of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (7)
1. A method for recovering silver from a silver-containing waste liquid, comprising the following steps:
step one, preparing ammonia from silver-containing wastewater: adding the silver-containing wastewater into a precipitation kettle to a high liquid level, starting stirring, then dropwise adding ammonia water, wherein brown precipitate appears in the solution at first, the precipitate is dissolved along with the dropwise adding of the ammonia water, the solution is changed into a colorless transparent solution again, and continuously stirring for 10-30 min;
step two, silver oxide synthesis reaction: keeping stirring, adding sodium hydroxide solution into the precipitation kettle, standing, starting stirring again, heating the solution to 60-80 ℃, and controlling the pH value to be 11.5-12.5;
step three, filter pressing: filter-pressing the slurry in the precipitation kettle, pressing the filtrate to a washing tank, circulating the pressed filtrate between the washing tank and a filter press until the filtrate is clear, and then sequentially discharging the filtrate to a sewage workshop through two-stage precision filters;
step four, washing: and unloading the filter cake into a washing tank, and repeatedly washing the filter cake with pure water until the conductivity of the supernatant of the washing liquid is less than 50us/cm.
2. The method according to claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in the first step, the ammonia water is added dropwise at the rate: 1L/h-5L/h.
3. The method according to claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in the first step, the concentration of the added ammonia water is 5-10 mol/L.
4. The method of claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in step two, the rate of addition of the sodium hydroxide solution was: 1-5L/h.
5. The method according to claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in the second step, the concentration of the added sodium hydroxide solution is 3-5 mol/L.
6. The method according to claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in the second step, the mass ratio of Ag to NaOH is 1.15: 1.
7. The method of claim 1, wherein the silver is recovered from the silver-containing waste liquid,
in the second step, the stirring time is started again for 10-20min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210991088.2A CN115286143A (en) | 2022-08-17 | 2022-08-17 | Method for recovering silver from silver-containing waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210991088.2A CN115286143A (en) | 2022-08-17 | 2022-08-17 | Method for recovering silver from silver-containing waste liquid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090021005A (en) * | 2007-08-24 | 2009-02-27 | 서강대학교산학협력단 | Preparation of silver colloid from impure silver salt |
| KR20090021004A (en) * | 2007-08-24 | 2009-02-27 | 서강대학교산학협력단 | Preparation of silver powder by using the insoluble silver salts |
| CN103420409A (en) * | 2013-06-19 | 2013-12-04 | 太仓沪试试剂有限公司 | Method for synthesizing high-purity silver sulfate |
| CN104263948A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for recovering sliver from silver-bearing waste liquor |
| CN107058757A (en) * | 2017-03-24 | 2017-08-18 | 金川集团股份有限公司 | A kind of production method of the separation of Silver from silver-containing liquid waste |
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- 2022-08-17 CN CN202210991088.2A patent/CN115286143A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090021005A (en) * | 2007-08-24 | 2009-02-27 | 서강대학교산학협력단 | Preparation of silver colloid from impure silver salt |
| KR20090021004A (en) * | 2007-08-24 | 2009-02-27 | 서강대학교산학협력단 | Preparation of silver powder by using the insoluble silver salts |
| CN103420409A (en) * | 2013-06-19 | 2013-12-04 | 太仓沪试试剂有限公司 | Method for synthesizing high-purity silver sulfate |
| CN104263948A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for recovering sliver from silver-bearing waste liquor |
| CN107058757A (en) * | 2017-03-24 | 2017-08-18 | 金川集团股份有限公司 | A kind of production method of the separation of Silver from silver-containing liquid waste |
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