CN112479334A - Purification treatment method of silver electrolyte - Google Patents
Purification treatment method of silver electrolyte Download PDFInfo
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- CN112479334A CN112479334A CN202011162188.1A CN202011162188A CN112479334A CN 112479334 A CN112479334 A CN 112479334A CN 202011162188 A CN202011162188 A CN 202011162188A CN 112479334 A CN112479334 A CN 112479334A
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- silver
- electrolyte
- silver oxide
- purified
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 74
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 57
- 239000004332 silver Substances 0.000 title claims abstract description 57
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000746 purification Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 22
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 116
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 58
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000006228 supernatant Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010908 decantation Methods 0.000 claims description 4
- 239000003814 drug Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims 1
- 239000008151 electrolyte solution Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 10
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- UKHWJBVVWVYFEY-UHFFFAOYSA-M silver;hydroxide Chemical compound [OH-].[Ag+] UKHWJBVVWVYFEY-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012629 purifying agent Substances 0.000 description 2
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 2
- 229910001958 silver carbonate Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
-
- 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
-
- 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
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
Abstract
The invention provides a purification treatment method of silver electrolyte, which comprises the following steps: taking pure silver electrolyte, adding an alkaline agent into the pure silver electrolyte, and heating and stirring to generate silver oxide; adding the silver oxide into the silver electrolyte to be purified, heating and stirring, and controlling the pH value of a reaction system to be between 5.5 and 6.8; and standing the electrolyte to be purified, which is added with the silver oxide for reaction, and performing precipitation separation to obtain the purified silver electrolyte. According to the purification method of the silver electrolyte, the silver oxide is prepared firstly, and is subjected to chemical reaction with the electrolyte to be purified, and the temperature and the pH value of a reaction system are strictly controlled, so that impurity elements in a solution can be removed in a hydrolysis precipitation mode to the maximum extent, the separation of the impurity elements and silver is realized, and the purification of the silver electrolyte is realized.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal environmental protection, and relates to a purification treatment method of silver electrolyte.
Background
At present, the production of metallic silver is mainly completed by an electrolytic process. In order to achieve a better electrolysis effect, copper ions are usually added into the electrolyte to enhance the conductivity, but as the electrolysis is continuously carried out, the concentration of silver ions in the electrolyte is continuously reduced, and the concentration of heavy metal ions such as copper, lead and the like is also continuously increased, so that the impurity content of electrolytic silver is increased, the purity of products is reduced, and even waste products are generated. Direct reconfiguration of new electrolyte is neither economical nor efficient in the use of spent electrolyte, and so it is often necessary to purify the spent silver electrolyte to enable it to continue electrolytic production.
At present, the purified electrolyte is mainly purified by a precipitation method, and the pH value of the electrolyte is adjusted to reach a proper range, so that impurity elements can be separated from a system by hydrolyzing to form a form of precipitate insoluble substances. The pH regulator mainly used at present mainly comprises sodium hydroxide, silver carbonate, silver oxide and the like. The pH of the electrolyte can be greatly increased after the addition of sodium hydroxide, but sodium ions are difficult to be discharged from the system with the passage of time, thereby affecting the electrolysis effect. The silver carbonate purifies electrolyte and mainly produces the carbon dioxide bubble, and the bubble is easily attached to because the container bottom also makes the solution after the purification have certain carbonate simultaneously, is unfavorable for the getting rid of foreign element. The more effective purifying agent is silver oxide as pH regulator. After the silver oxide is added, other metal ions and gases are not generated, and the reaction product is only water, so that the silver oxide is green and pollution-free. Therefore, the silver oxide is an ideal silver electrolyte purifying agent. How to reasonably select the adding time of the silver oxide and the purification reaction conditions becomes the key of whether the purified liquid is qualified or not.
The existing silver oxide purification method does not consider the problem of adjusting the pH value of the solution after temperature rise. The reaction rate is increased by raising the temperature, but the pH value of the solution is lowered by raising the temperature, which inevitably affects the removal of impurity metal ions, so that the purification effect is not ideal.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the purification treatment method of the silver electrolyte can effectively precipitate impurity metal ions to obtain the purified silver electrolyte.
In order to solve the technical problems, the invention adopts the technical scheme that:
the invention provides a purification treatment method of silver electrolyte, which comprises the following steps:
taking pure silver electrolyte, adding an alkaline medicament into the pure silver electrolyte, and heating and stirring to generate silver oxide;
adding the silver oxide into the silver electrolyte to be purified, heating and stirring, and controlling the pH value of a reaction system to be between 5.5 and 6.8;
and standing the electrolyte to be purified, which is added with the silver oxide for reaction, and performing precipitation separation to obtain the purified silver electrolyte.
Further, the step of taking pure silver electrolyte, adding an alkaline agent into the pure silver electrolyte, and heating and stirring the mixture to generate silver oxide comprises the following steps:
dropping alkaline agent into the pure silver electrolyte, and controlling the pH value of the mixed solution to be between 8 and 10;
and heating the mixed solution to 50-70 ℃, and mechanically stirring to generate silver oxide precipitate.
Further, the alkaline agent comprises at least one of a sodium hydroxide solution and a potassium hydroxide solution.
Further, the mechanical stirring intensity is 150-.
Further, the stirring to generate silver oxide precipitate further comprises:
and washing the silver oxide precipitate, and separating to obtain the silver oxide.
Further, the silver oxide precipitate was washed with pure water, and the silver oxide precipitate was separated from the supernatant by decantation.
Further, the number of washing times is 4 to 6.
Further, the adding of the silver oxide into the silver electrolyte to be purified for heating and stirring comprises:
heating the electrolyte to be purified, which is added with the silver oxide, to 70-90 ℃; mechanical stirring was carried out at 300-.
Further, the standing treatment time of the electrolyte to be purified, which is added with the silver oxide for reaction, is 2 hours, and supernatant liquid and lower-layer sediment are filtered and separated, wherein the supernatant liquid is the purified silver electrolyte.
The invention has the beneficial effects that: according to the purification method of the silver electrolyte, silver oxide is prepared firstly, then the silver oxide and the electrolyte to be purified are subjected to chemical reaction, and the temperature and the pH value of a reaction system are strictly controlled, so that impurity elements in the solution can be removed in a hydrolysis precipitation mode to the maximum extent, the separation of the impurity elements and silver is realized, and the purification of the silver electrolyte is realized.
Drawings
The detailed structure of the invention is described in detail below with reference to the accompanying drawings
FIG. 1 is a flow chart of the purification treatment of the silver electrolyte according to the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
Referring to fig. 1, the present invention provides a purification treatment method of silver electrolyte, including:
taking pure silver electrolyte, adding an alkaline medicament into the pure silver electrolyte, and heating and stirring to generate silver oxide;
adding the silver oxide into the silver electrolyte to be purified, heating and stirring, and controlling the pH value of a reaction system to be between 5.5 and 6.8;
and standing the electrolyte to be purified, which is added with the silver oxide for reaction, and performing precipitation separation to obtain the purified silver electrolyte.
The invention adopts relatively pure electrolyte as a silver source, adds alkaline agent into the pure electrolyte to adjust proper pH value, generates a large amount of silver hydroxide, and then the silver hydroxide is unstable and decomposed into silver oxide precipitate.
Specifically, an alkaline medicament is dripped into the pure silver electrolyte, and the pH value of the mixed solution is controlled to be between 8 and 10; heating the mixed solution to 50-70 ℃, and mechanically stirring at the rotating speed of 150-300rpm to generate a large amount of silver hydroxide; the stirring time is 1h, and then the silver hydroxide is decomposed to generate silver oxide precipitate.
Further, the stirring to generate silver oxide precipitate further comprises:
and washing the silver oxide precipitate, and separating to obtain the silver oxide. And washing the silver oxide precipitate for 4-6 times by adopting pure water, and separating the silver oxide precipitate and the supernatant by using a decantation method to obtain the required silver oxide.
Then, mixing the obtained silver oxide with the electrolyte to be purified, and adjusting a proper pH value, the temperature of a system, the stirring intensity and the like so as to facilitate the purification process;
the temperature of the reaction system is 70-90 ℃;
the stirring intensity of the reaction system is 300-500rpm, and the stirring time is 4 h.
And finally, standing the electrolyte to be purified, which is added with the silver oxide for reaction, for 2 hours, and filtering and separating a supernatant and a lower-layer precipitate, wherein the supernatant is the purified silver electrolyte.
Examples
Referring to fig. 1, the alkaline chemical in the embodiment uses a sodium hydroxide solution.
S10, putting 1L of pure silver electrolyte into a 3L glass beaker; dripping sodium hydroxide solution into electrolyte, controlling the pH value of the solution to be 9, heating to 55 ℃, mechanically stirring at 200rpm for 1h, and stopping heating and stirring;
s20, washing the generated silver oxide precipitate by using 2L of pure water each time, separating the supernatant from the precipitate by using a decantation method, and stopping the washing process after washing for 4-6 times; obtaining silver oxide;
s30, putting 2L of silver electrolyte to be purified in a 5L beaker; continuously adding the obtained silver oxide into the electrolyte to be purified, heating the reaction system at the temperature of 80 ℃, mechanically stirring at 400rpm, controlling the pH value of the system to be 6 after the temperature rises, and continuously adding the silver oxide to maintain the pH value if the pH value drops midway. After 4h, stopping heating and stirring;
s40, standing for 2h, filtering and separating supernatant and lower-layer precipitate, wherein the supernatant is purified silver electrolyte, and the precipitate is further processed.
In the method for purifying silver electrolyte according to the present invention, the alkaline agent in the embodiment may be other alkaline solution such as potassium hydroxide. The mechanical stirring and heating process in step S30 in example 1 can be replaced by introducing hot steam, and the other steps are the same as in example.
In summary, the purification method of silver electrolyte provided by the invention first prepares silver oxide, then makes the silver oxide and the electrolyte to be purified perform chemical reaction, and strictly controls the temperature and the pH value of the reaction system, so that the impurity elements in the solution can be removed in a hydrolysis precipitation manner to the maximum extent, and the separation of the impurity elements and silver is realized, thereby realizing the purification of the silver electrolyte.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A purification treatment method for a silver electrolytic solution, characterized by comprising:
taking pure silver electrolyte, adding an alkaline medicament into the pure silver electrolyte, and heating and stirring to generate silver oxide;
adding the silver oxide into the silver electrolyte to be purified, heating and stirring, and controlling the pH value of a reaction system to be between 5.5 and 6.8;
and standing the electrolyte to be purified, which is added with the silver oxide for reaction, and performing precipitation separation to obtain the purified silver electrolyte.
2. The purification treatment method according to claim 1, wherein the step of taking the pure silver electrolyte and adding an alkaline agent to the pure silver electrolyte to generate the silver oxide by heating and stirring comprises:
dropping alkaline agent into the pure silver electrolyte, and controlling the pH value of the mixed solution to be between 8 and 10;
and heating the mixed solution to 50-70 ℃, and mechanically stirring to generate silver oxide precipitate.
3. The purification process of claim 2, wherein the alkaline agent comprises at least one of a sodium hydroxide solution and a potassium hydroxide solution.
4. The purification treatment method according to claim 3, wherein; the mechanical stirring intensity is 150-300rpm, and the stirring time is 1 h.
5. The purification process of claim 4, wherein the mechanical agitation to produce a silver oxide precipitate further comprises:
and washing the silver oxide precipitate, and separating to obtain the silver oxide.
6. The purification process of claim 5, wherein the silver oxide precipitate is washed with pure water and the silver oxide precipitate is separated from the supernatant by decantation.
7. The purification process of claim 6, wherein the number of washing is 4 to 6.
8. The purification treatment method according to claim 1, wherein the adding of the silver oxide to the silver electrolyte to be purified by heating and stirring comprises:
heating the electrolyte to be purified, which is added with the silver oxide, to 70-90 ℃; mechanical stirring was carried out at 300-.
9. The purification treatment method according to claim 8, wherein the treatment time of the electrolyte to be purified to which the silver oxide is added is 2 hours, and the supernatant, i.e., the purified silver electrolyte, is separated from the lower precipitate by filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011162188.1A CN112479334A (en) | 2020-10-27 | 2020-10-27 | Purification treatment method of silver electrolyte |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011162188.1A CN112479334A (en) | 2020-10-27 | 2020-10-27 | Purification treatment method of silver electrolyte |
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| CN112479334A true CN112479334A (en) | 2021-03-12 |
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| CN202011162188.1A Pending CN112479334A (en) | 2020-10-27 | 2020-10-27 | Purification treatment method of silver electrolyte |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114540880A (en) * | 2022-01-27 | 2022-05-27 | 大冶有色金属有限责任公司 | Method for removing copper in silver electrolyte |
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|---|---|---|---|---|
| CN1339619A (en) * | 2000-08-23 | 2002-03-13 | 内蒙古乾坤金银精炼股份有限公司 | Method for removing bismuth and antiomny from silver electrolyte |
| CN1884623B (en) * | 2006-05-21 | 2010-05-12 | 郴州市金贵银业股份有限公司 | Purifying method for silver electrolytic solution |
| 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 |
| CN109023421A (en) * | 2018-08-15 | 2018-12-18 | 云南铜业股份有限公司西南铜业分公司 | A kind of purifying treatment method of silver electrolyte |
-
2020
- 2020-10-27 CN CN202011162188.1A patent/CN112479334A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| CN1339619A (en) * | 2000-08-23 | 2002-03-13 | 内蒙古乾坤金银精炼股份有限公司 | Method for removing bismuth and antiomny from silver electrolyte |
| CN1884623B (en) * | 2006-05-21 | 2010-05-12 | 郴州市金贵银业股份有限公司 | Purifying method for silver electrolytic solution |
| 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 |
| CN109023421A (en) * | 2018-08-15 | 2018-12-18 | 云南铜业股份有限公司西南铜业分公司 | A kind of purifying treatment method of silver electrolyte |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114540880A (en) * | 2022-01-27 | 2022-05-27 | 大冶有色金属有限责任公司 | Method for removing copper in silver electrolyte |
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