RU2356959C1 - Extraction method of palladium, silver and copper of waste electrolytes - Google Patents
Extraction method of palladium, silver and copper of waste electrolytes Download PDFInfo
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- RU2356959C1 RU2356959C1 RU2007149103A RU2007149103A RU2356959C1 RU 2356959 C1 RU2356959 C1 RU 2356959C1 RU 2007149103 A RU2007149103 A RU 2007149103A RU 2007149103 A RU2007149103 A RU 2007149103A RU 2356959 C1 RU2356959 C1 RU 2356959C1
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- Prior art keywords
- silver
- palladium
- copper
- electrolyte
- solution
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000004332 silver Substances 0.000 title claims abstract description 27
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 26
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000003792 electrolyte Substances 0.000 title claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 17
- 239000010949 copper Substances 0.000 title claims abstract description 17
- 238000000605 extraction Methods 0.000 title claims abstract description 4
- 239000002699 waste material Substances 0.000 title abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010802 sludge Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims description 8
- 230000006378 damage Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 229910001316 Ag alloy Inorganic materials 0.000 claims description 2
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 2
- 238000004040 coloring Methods 0.000 abstract 1
- 238000002955 isolation Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- KTCBLMXNWYGCRT-UHFFFAOYSA-N 1-[2-(1h-indol-3-yl)ethyl]-3-methylthiourea Chemical compound C1=CC=C2C(CCNC(=S)NC)=CNC2=C1 KTCBLMXNWYGCRT-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Область техникиTechnical field
Изобретение относится к химической промышленности, а именно к технологии утилизации палладия, серебра и меди из отработанных электролитов.The invention relates to the chemical industry, and in particular to a technology for the disposal of palladium, silver and copper from spent electrolytes.
Уровень техникиState of the art
В целях повышения качества изделий из драгоценных металлов, содержащих палладий, серебро и медь, применяют электрополировку в электролите состава: тиомочевина, серная кислота, вода (1 л электролита содержит 90 г тиомочевины, 20 г In order to improve the quality of precious metal products containing palladium, silver and copper, electro-polishing is used in an electrolyte of the composition: thiourea, sulfuric acid, water (1 liter of electrolyte contains 90 g of thiourea, 20 g
H2SO4 концентрированной, воду). Отработанный электролит состоит из раствора и осадка (шлама) и содержит до 10% палладия, серебра и меди. Для утилизации данного электролита на практике используют метод цементации, заключающийся в добавлении к электролиту цинкового порошка, обеспечивающего восстановление благородных ионов металлов из их комплексов с тиомочевиной до металлов в свободном состоянии. При этом последние выделяются на цинковой основе (Справочник пробирера / Сост.: канд. техн. наук Е.А.Маренков. Под ред. инж. Д.Г.Гребенкина. - М.: Госфиниздат, 1953. - 230 с.):H 2 SO 4 concentrated, water). The spent electrolyte consists of a solution and a precipitate (sludge) and contains up to 10% palladium, silver and copper. To utilize this electrolyte, the cementation method is used in practice, which consists in adding zinc powder to the electrolyte, which ensures the restoration of noble metal ions from their complexes with thiourea to metals in a free state. At the same time, the latter are isolated on a zinc basis (Handbook of the probiere / Comp .: Candidate of Technical Sciences E.A. Marenkov. Edited by engineer D.G. Grebenkin. - M.: Gosfinizdat, 1953. - 230 p.):
2T2MeHSO4+Zn=2Ме+Zn(HSO4)2+4Т,2T 2 MeHSO 4 + Zn = 2Me + Zn (HSO 4 ) 2 + 4T,
где Т - тиомочевина (NH2)2CS.where T is thiourea (NH 2 ) 2 CS.
Данный способ взят за прототип.This method is taken as a prototype.
Недостатками способа прототипа является недостаточно эффективная утилизация палладия и серебра из электролита.The disadvantages of the prototype method is the insufficiently efficient disposal of palladium and silver from the electrolyte.
Раскрытие изобретенияDisclosure of invention
Задачей изобретения является разработка способа извлечения палладия, серебра и меди из отработанных электролитов для электрополировки изделий, который обеспечил бы технический результат - возможность количественного выделения из электролита (раствор и осадок) палладия и серебра в виде свободных металлов, которые в дальнейшем могут использоваться в промышленных целях.The objective of the invention is to develop a method for the extraction of palladium, silver and copper from spent electrolytes for electropolishing products, which would provide a technical result - the possibility of quantitative separation from the electrolyte (solution and precipitate) of palladium and silver in the form of free metals, which can be used in future .
Этот технический результат достигается благодаря настоящему изобретению, предлагающему способ извлечения палладия, серебра и меди из отработанных электролитов, содержащих тиомочевину, серную кислоту, воду и шлам, включающий разрушение комплекса палладия, серебра и меди, отличающийся тем, что для разрушения комплексов палладия, серебра и меди в отработанный электролит добавляют 33,0-67,5%-ный пероксид водорода при перемешивании с переводом палладия и серебра в осадок, а меди в раствор, после появления зеленой окраски раствора, его охлаждают, фильтруют, осадок нагревают с получением сплава из палладия и серебра.This technical result is achieved thanks to the present invention, which provides a method for the recovery of palladium, silver and copper from spent electrolytes containing thiourea, sulfuric acid, water and sludge, including the destruction of a complex of palladium, silver and copper, characterized in that for the destruction of complexes of palladium, silver and 33.0-67.5% hydrogen peroxide is added to the spent electrolyte with stirring with the transfer of palladium and silver to the precipitate, and the copper in the solution, after the green color of the solution appears, it is cooled, filtered, the precipitate is heated to obtain an alloy of palladium and silver.
В предлагаемом способе вместо цинкового порошка вводят 33,0-67,5%-ный пероксид водорода, который разрушает комплексы палладия, серебра и меди с тиомочевиной. При этом выделяются в свободном состоянии палладий и серебро, медь переходит в раствор, а тиомочевина разлагается с выделением серы, диоксида углерода и сульфата аммония.In the proposed method, instead of zinc powder, 33.0-67.5% hydrogen peroxide is introduced, which destroys the complexes of palladium, silver and copper with thiourea. In this case, palladium and silver are released in a free state, copper passes into solution, and thiourea decomposes with the release of sulfur, carbon dioxide and ammonium sulfate.
Окончание реакции фиксируется по появлению зеленой окраски раствора.The end of the reaction is fixed by the appearance of a green color of the solution.
Осуществление изобретенияThe implementation of the invention
Нижеследующий пример подтверждает осуществимость изобретения.The following example confirms the feasibility of the invention.
Пример.Example.
Сплав с содержанием палладия 47,5%, серебра 22,0%, меди 30,5% подвергается электрополировке в электролите состава 1 л: 90 г тиомочевины, 20 г H2SO4 96-98% и 890-900 мл воды. К отработанному электролиту (раствор и осадок) при перемешивании постепенно небольшими порциями приливают 300 мл 67,5%-ного или 600 мл 33%-ного пероксида водорода. В результате реакции разрушения комплексов палладия, серебра и меди с тиомочевиной наблюдается сильное разогревание с выделением углекислого газа.The alloy with the content of palladium 47.5%, silver 22.0%, copper 30.5% is electropolished in an electrolyte of 1 l composition: 90 g of thiourea, 20 g of H 2 SO 4 96-98% and 890-900 ml of water. To the spent electrolyte (solution and precipitate), 300 ml of 67.5% or 600 ml of 33% hydrogen peroxide are gradually added in small portions with stirring. As a result of the decomposition reaction of the complexes of palladium, silver and copper with thiourea, strong heating is observed with the release of carbon dioxide.
T2PdHSO4+Н2O2=Pd+2Т+H2SO4+H2OT 2 PdHSO 4 + H 2 O 2 = Pd + 2T + H 2 SO 4 + H 2 O
T2AgHSO4+H2O2=Ag+2Т+H2SO4+H2OT 2 AgHSO 4 + H 2 O 2 = Ag + 2T + H 2 SO 4 + H 2 O
2Т+2H2O2+2H2SO4=2S+2CO2+2(NH4)2SO4 2T + 2H 2 O 2 + 2H 2 SO 4 = 2S + 2CO 2 +2 (NH 4 ) 2 SO 4
2T2CuHSO4+H2O2=2CuSO4+4T+2H2O2T 2 CuHSO 4 + H 2 O 2 = 2 CuSO 4 + 4T + 2H 2 O
Появление зеленой окраски раствора свидетельствует об окончании реакции. После охлаждения палладий, серебро и сера отфильтровываются через фильтр с синей лентой. Осадок помещают в муфель и нагревают до температуры 800°С, сера выгорает, а палладий и серебро образуют сплав (2,85 г), который используют в дальнейшем для промышленных целей.The appearance of a green color of the solution indicates the end of the reaction. After cooling, palladium, silver and sulfur are filtered through a blue ribbon filter. The precipitate is placed in a muffle and heated to a temperature of 800 ° C, sulfur burns out, and palladium and silver form an alloy (2.85 g), which is then used for industrial purposes.
Предлагаемый способ может найти широкое применение для утилизации отходов драгоценных металлов при изготовлении изделий, украшений, содержащих палладий и серебро.The proposed method can find wide application for the disposal of waste precious metals in the manufacture of products, jewelry containing palladium and silver.
Хотя настоящее изобретение описано посредством примера его выполнения, объем данного изобретения не ограничивается этими примерами, но определяется лишь формулой изобретения с учетом возможных эквивалентов.Although the present invention has been described by way of example, the scope of the present invention is not limited to these examples, but is defined only by the claims taking into account possible equivalents.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2007149103A RU2356959C1 (en) | 2007-12-28 | 2007-12-28 | Extraction method of palladium, silver and copper of waste electrolytes |
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| Application Number | Priority Date | Filing Date | Title |
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| RU2007149103A RU2356959C1 (en) | 2007-12-28 | 2007-12-28 | Extraction method of palladium, silver and copper of waste electrolytes |
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| Publication Number | Publication Date |
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| RU2356959C1 true RU2356959C1 (en) | 2009-05-27 |
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| RU2007149103A RU2356959C1 (en) | 2007-12-28 | 2007-12-28 | Extraction method of palladium, silver and copper of waste electrolytes |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1534485A (en) * | 1976-10-19 | 1978-12-06 | Mines Fond Zinc Vieille | Process for recovering silver and possibly gold from a solid starting material containing such metals |
| SU770274A1 (en) * | 1974-06-25 | 1988-03-07 | Иркутский государственный научно-исследовательский институт редких и цветных металлов "Иргиредмет" | Method of extracting gold and silver from thiocarbamide solutions by electrolysis |
| US5449396A (en) * | 1993-02-16 | 1995-09-12 | Laskorin; Boris N. | Method for recovering gold and silver from ore starting materials |
| JP2005298850A (en) * | 2004-04-07 | 2005-10-27 | Sumitomo Metal Mining Co Ltd | Method for recovering gold from copper concentrate leach residue |
-
2007
- 2007-12-28 RU RU2007149103A patent/RU2356959C1/en not_active IP Right Cessation
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU770274A1 (en) * | 1974-06-25 | 1988-03-07 | Иркутский государственный научно-исследовательский институт редких и цветных металлов "Иргиредмет" | Method of extracting gold and silver from thiocarbamide solutions by electrolysis |
| GB1534485A (en) * | 1976-10-19 | 1978-12-06 | Mines Fond Zinc Vieille | Process for recovering silver and possibly gold from a solid starting material containing such metals |
| US5449396A (en) * | 1993-02-16 | 1995-09-12 | Laskorin; Boris N. | Method for recovering gold and silver from ore starting materials |
| JP2005298850A (en) * | 2004-04-07 | 2005-10-27 | Sumitomo Metal Mining Co Ltd | Method for recovering gold from copper concentrate leach residue |
Non-Patent Citations (1)
| Title |
|---|
| МАРЕНКОВ Е.А. Справочник пробирера, под ред. Д.Г.ГРЕБЕНКИНА. - М.: Госфиниздат, 1953, с.230. * |
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