WO2008013479A2 - Method for refining precious metals - Google Patents
Method for refining precious metals Download PDFInfo
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- WO2008013479A2 WO2008013479A2 PCT/RU2007/000401 RU2007000401W WO2008013479A2 WO 2008013479 A2 WO2008013479 A2 WO 2008013479A2 RU 2007000401 W RU2007000401 W RU 2007000401W WO 2008013479 A2 WO2008013479 A2 WO 2008013479A2
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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
- C22B11/02—Obtaining noble metals by dry processes
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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
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/023—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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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
Definitions
- the present invention relates to low-waste metallurgy of precious metals, in particular, to a method for refining metals and it can be used to increase the degree of extraction of precious metals from alloys and their purity.
- a known method of vacuum refining a metal including lowering the pressure of the gas mixture above the melt surface to obtain partial gas pressures above the melt below the partial gas pressures in the melt, treating the melt with pressure pulsations (A. Kablukovsky et al. "Overview”. Moscow, Chermetinformation 1985 p. 14-16).
- a vacuum is created above the melt surface, which pulsates in the high frequency range.
- the disadvantage of this method is the inability to provide the required degree of metal refining, since the processing depth is small, which generally does not allow to obtain metal of the required quality.
- the closest method is the method of refining precious metals, including the melting of the starting material, saturation of the melt with a gas composition with the formation of impurity compounds in the form of saturation products and their removal (RU, 2086685, IPC C22B 1 1/02, publ. 08/10/1997)
- the melt is obtained by granulation and grinding of waste, the saturation of the melt is carried out by treatment with an oxidizing agent such as ozonized oxygen, Cl 2 , H 2 O, HNO 3 , HClO 4 , CH 3 COOH in a medium of H 2 SO 4 and / or HCl at an elevated temperature (up to the boiling point).
- an oxidizing agent such as ozonized oxygen, Cl 2 , H 2 O, HNO 3 , HClO 4 , CH 3 COOH in a medium of H 2 SO 4 and / or HCl at an elevated temperature (up to the boiling point).
- the adsorption of saturation products is carried out by adding to the liquid phase an organic reducing agent from the group of CHOH, HCOOH, glucose and other saccharides. Precipitated precious metals are removed by reduction by known methods.
- the disadvantage of this method is that, together with the noble metals, part of the impurities also passes into the solution, while the degree of extraction of the noble metals decreases. Disclosure of the essence of the invention.
- the problem solved by the invention is the creation of a method of refining a material containing noble metals to their most complete extraction with ultra-high purity.
- the technical result in the present invention is achieved by creating a method for refining precious metals, including melting the starting material, saturating the melt with a gas composition with the formation of impurity compounds in the form of saturation products and their removal, characterized in that the saturation is carried out by a gaseous composition consisting of at least two gas components forming compounds with impurities at constant ultrahigh pressure, the removal of impurities is carried out by adsorption of saturation products melt filtration in vacuo through a pad of sorbent material with a high specific surface area, the heating temperature is above the melt temperature.
- the proposed method has a number of additional advantages compared to known refining methods: the maximum ratio of the amount of extracted metal to the weight of the sorbent material;
- a sorbent material with a high specific surface area of 500-1000 m 2 / gp makes it possible to extract impurities in the form of compounds with gaseous saturation compositions.
- the invention is also characterized in that the temperature of the filter is higher than the melt temperature by 100-200 C °.
- gaseous composition for example, oxygen and / or hydrocarbons and / or oxygen and / or nitrogen, or other components depends on the composition of the impurities to be removed as a result of the formation of compounds that slag on the sorbing surface.
- the repetition of the operations and their sequence are determined depending on the chemical composition of the impurities (see examples. Execution.)
- the modes of refining operations are determined empirically and the excess of their values beyond the specified ones will not allow to solve the task, i.e. implement a method of refining a material containing noble metals with the most complete extraction of them and with ultra-high purity. If, for example, the sorbent material has a smaller specific surface than 500 - 1000 m 2 / gp, and its temperature is lower than the melt temperature, then refining will not be complete.
- Sorbent material with a specific surface of more than 1000 m 2 / gp does not currently exist.
- Example 1 The source material was taken gold concentrate containing gold Au-81%, iron Fe-7%, copper Cu-3%, silicon
- the gas composition used for the refining method consists of oxygen Ch -5%, acetyl C2H2 - 7%, nitrogen N2 - the rest.
- the starting material is heated to a temperature of 1500 C °, saturated with a gas composition under a pressure of 20OMTIa for 15 minutes, and subjected to sorption and filtration through a material with a specific surface of 1500 m 2 / gp at a temperature of 1650 C 0 in a vacuum of 5 * 10 mm Hg.
- Example 2 An analysis of the chemical composition of the sludge showed that the gold content increased to 99.5% in one refining operation, the repeated processing of the melt only due to the filtration reaction increases the gold concentration to 99.97%.
- Example 2 A palladium concentrate containing palladium Pd - 43 was taken as the starting material. %, copper Cu- 13%, silver Ag - 27%, sulfur S- 13%, arsenic As -3%, tellurium Tl- 1%
- the gas composition used in the refining process consists of oxygen Ch -7%, acetyl C2H2 - 15%, nitrogen N 2 - 78%
- the starting material is heated to a temperature of 1700 C °, saturated with a gas composition under a pressure of 150MTTa for 30 minutes, and subjected to sorption-filtration through a material with a specific surface of 1700 m 2 / gp at a temperature of 1750 C ° in a vacuum of 10 "2 mm Hg.
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- Chemical & Material Sciences (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Способ рафинирования благородных металлов. The method of refining precious metals.
Область техники.The field of technology.
Предлагаемое изобретение относится к малоотходной металлургии благородных металлов, в частности, к способу рафинирования металлов и оно может быть использовано для увеличения степени извлечения благородных металлов из сплавов и их чистоты.The present invention relates to low-waste metallurgy of precious metals, in particular, to a method for refining metals and it can be used to increase the degree of extraction of precious metals from alloys and their purity.
Предшествующий уровень техники.The prior art.
Известен способ вакуумного рафинирования металла, включающий понижение давления смеси газов над поверхностью расплава до получения парциальных давлений газов над расплавом ниже парциальных давлений газов в расплаве, обработку расплава пульсациями давления (Каблуковский А. Ф. и др. "Обзорная информация". Москва, Черметинформация 1985, с. 14-16). В известном способе над поверхностью расплава создают разрежение, которое пульсирует в диапазоне высоких частот.A known method of vacuum refining a metal, including lowering the pressure of the gas mixture above the melt surface to obtain partial gas pressures above the melt below the partial gas pressures in the melt, treating the melt with pressure pulsations (A. Kablukovsky et al. "Overview". Moscow, Chermetinformation 1985 p. 14-16). In the known method, a vacuum is created above the melt surface, which pulsates in the high frequency range.
Недостатком способа является невозможность обеспечить требуемую степень рафинирования металла, поскольку мала глубина обработки, что в целом не позволяет получать металл требуемого качества.The disadvantage of this method is the inability to provide the required degree of metal refining, since the processing depth is small, which generally does not allow to obtain metal of the required quality.
Наиболее близким способом является способ рафинирования благородных металлов, включающий расплавление исходного материала, насыщение расплава газовой композицией с образованием соединений примесей в виде продуктов насыщения и их удаление (RU ,2086685 , МПК C22B 1 1/02, опубл. 10.08.1997)The closest method is the method of refining precious metals, including the melting of the starting material, saturation of the melt with a gas composition with the formation of impurity compounds in the form of saturation products and their removal (RU, 2086685, IPC C22B 1 1/02, publ. 08/10/1997)
Известным способом могут извлекать платину, родий, палладий и золото из отходов. В нем расплав получают путем гранулирования и измельчения отходов, насыщение расплава проводят путем обработки окислителем типа озонированного кислорода, Cl2, H2O, HNO3, HClO4, CH3COOH в среде H2SO4 и/или HCl при повышенной температуре (вплоть до температуры кипения) .In a known manner, platinum, rhodium, palladium and gold can be recovered from waste. In it, the melt is obtained by granulation and grinding of waste, the saturation of the melt is carried out by treatment with an oxidizing agent such as ozonized oxygen, Cl 2 , H 2 O, HNO 3 , HClO 4 , CH 3 COOH in a medium of H 2 SO 4 and / or HCl at an elevated temperature (up to the boiling point).
Адсорбцию продуктов насыщения проводят путем добавления в жидкую фазу органического восстановителя из группы CHOH, HCOOH, глюкозы и других сахаридов. Осаждающиеся драгоценные металлы удаляют восстановлением известными способами.The adsorption of saturation products is carried out by adding to the liquid phase an organic reducing agent from the group of CHOH, HCOOH, glucose and other saccharides. Precipitated precious metals are removed by reduction by known methods.
Недостатком известного способа является то, что вместе с благородными металлами в раствор переходит и часть примесей, при этом уменьшается степень извлечения благородных металлов. Раскрытие сущности предлагаемого изобретения.The disadvantage of this method is that, together with the noble metals, part of the impurities also passes into the solution, while the degree of extraction of the noble metals decreases. Disclosure of the essence of the invention.
Задачей, решаемой предлагаемым изобретением, является создание способа рафинирования материала, содержащего благородные металлы к наиболее полному извлечению их с сверхвысокой чистотой. Технический результат в предлагаемом изобретение достигают созданием способа рафинирования благородных металлов, включающего расплавление исходного материала, насыщение расплава газовой композицией с образованием соединений примесей в виде продуктов насыщения и их удаление, отличающийся тем, что насыщение проводят газообразной композицией, состоящей, по крайней мере, из двух газовых компонентов, образующих соединения с примесями, при постоянном сверхвысоком давлении, удаление примесей проводят адсорбцией продуктов насыщения путем фильтрации расплава в вакууме через фильтр из сорбирующего материала с высокой удельной поверхностью, температура нагрева которого выше температуры расплава.The problem solved by the invention is the creation of a method of refining a material containing noble metals to their most complete extraction with ultra-high purity. The technical result in the present invention is achieved by creating a method for refining precious metals, including melting the starting material, saturating the melt with a gas composition with the formation of impurity compounds in the form of saturation products and their removal, characterized in that the saturation is carried out by a gaseous composition consisting of at least two gas components forming compounds with impurities at constant ultrahigh pressure, the removal of impurities is carried out by adsorption of saturation products melt filtration in vacuo through a pad of sorbent material with a high specific surface area, the heating temperature is above the melt temperature.
Предлагаемый способ имеет ряд дополнительных преимуществ по сравнению с известными способами рафинирования: максимальное отношение количества извлеченного металла к весу сорбирующего материала;The proposed method has a number of additional advantages compared to known refining methods: the maximum ratio of the amount of extracted metal to the weight of the sorbent material;
- низкую энергоемкость процесса рафинирования на единицу веса извлеченных примесей; - возможность комплексно-дифференционного извлечения разных, в том числе редкоземельных элементов из основного примесного сплава;- low energy intensity of the refining process per unit weight of the extracted impurities; - the possibility of complex differential extraction of various, including rare-earth elements from the main impurity alloy;
- высокую экологичность, особенно, при рафинирование извлекаемого урана и плутония из отработанного ядерного топлива. Использование в качестве материала фильтра сорбирующий материал с высокой удельной поверхностью 500 - 1000 м2/гp позволяет извлекать примеси в виде соединений с газообразными композициями насыщения.- high environmental friendliness, especially when refining extracted uranium and plutonium from spent nuclear fuel. The use of a sorbent material with a high specific surface area of 500-1000 m 2 / gp as a filter material makes it possible to extract impurities in the form of compounds with gaseous saturation compositions.
Изобретение также характеризуется тем, что температура нагрева фильтра, выше температуры расплава на 100-200 C°.The invention is also characterized in that the temperature of the filter is higher than the melt temperature by 100-200 C °.
Это обеспечивает создание более высокой чувствительности сорбирующего материала, и как следствие, увеличение глубины извлечения.This ensures the creation of a higher sensitivity of the sorbent material, and as a result, an increase in the depth of extraction.
Насыщение расплава под давлением 10- 50OMITa в течение 15- 45 мин позволяет максимально связать растворенные в расплаве примеси в устойчивое соединение типа карбиды, нитриды и т.д.Saturation of the melt under a pressure of 10–50OMITa for 15–45 min allows maximum bonding of impurities dissolved in the melt into a stable compound such as carbides, nitrides, etc.
Использование температуры расплава в момент его насыщение газообразной композицией выше температуры плавления исходного материала на 100-300 C° позволяет повысить растворимость газообразных компонентов в расплаве.Using the temperature of the melt at the time it is saturated with the gaseous composition above the melting temperature of the starting material by 100-300 C ° allows you to increase the solubility of the gaseous components in the melt.
Проведение адсорбции продуктов насыщения в вакууме 10"2- 10"3 мм рт.ст позволяет более полное очищение металла от примесей.Carrying out the adsorption of saturation products in a vacuum of 10 "2 - 10 " 3 mm Hg allows a more complete purification of the metal from impurities.
Использование в качестве газообразной композиции, например, кислорода и /или углеводородов, и/или кислорода, и/или азота, или других компонентов, зависит от состава примесей, подлежащих удалению в результате образования соединений, которые отшлаковывают на сорбирующей поверхности.Use as a gaseous composition, for example, oxygen and / or hydrocarbons and / or oxygen and / or nitrogen, or other components depends on the composition of the impurities to be removed as a result of the formation of compounds that slag on the sorbing surface.
В предлагаемом способе рафинирования металла для получения более чистого металла и создания условий избирательного извлечения примесей возможно повтор операций, из которых состоит предлагаемый способ.In the proposed method of refining metal to obtain a cleaner metal and create conditions for the selective extraction of impurities, it is possible to repeat the operations that make up the proposed method.
Повторение операций и их последовательность определяют в зависимости от химсостава примесей (см.примеры выполнение.) Режимы проведения операций рафинирования определены опытным путем и выход их значений за пределы указанных не позволит решить поставленную задачу ,т.e. осуществить способ рафинирования материала, содержащего благородные металлы с наиболее полным извлечением их и с сверхвысокой чистотой. В случае если ,нaпpимep, сорбирующий материал будет иметь меньшую удельную поверхность, чем 500 - 1000 м2/гp, а его температуру ниже температуры расплава, то рафинирование не будет полным .The repetition of the operations and their sequence are determined depending on the chemical composition of the impurities (see examples. Execution.) The modes of refining operations are determined empirically and the excess of their values beyond the specified ones will not allow to solve the task, i.e. implement a method of refining a material containing noble metals with the most complete extraction of them and with ultra-high purity. If, for example, the sorbent material has a smaller specific surface than 500 - 1000 m 2 / gp, and its temperature is lower than the melt temperature, then refining will not be complete.
Сорбирующий материал с удельной поверхностью больше 1000 м2/гp в настоящее не существует .Sorbent material with a specific surface of more than 1000 m 2 / gp does not currently exist.
В случае, если процесс насыщения расплава будет проходить при режимах ниже указанных в описание, т.е. ниже давления 10- 500MПa и ниже температур насыщения расплава, то эти режимы не могут обеспечить связывание всех элементов примесей в устойчивое соединение.If the process of saturation of the melt will take place under the conditions below specified in the description, i.e. If the pressure is below 10–500 MPa and below the saturation temperature of the melt, these modes cannot ensure the binding of all impurity elements to a stable compound.
Если процесс насыщения расплава будет проходить при режимах выше указанных в описание, то в несколько раз возрастает стоимость процесса и оборудования. В случае в процессе рафинирования не полного извлечения примесей за счет образования устойчивого соединения и их сорбции, оставшиеся элементы примесей реагируют с материалом фильтра и остаются на его поверхности. В качестве материала реакционного фильтра используют сорбирующий материал, разработанный и запатентованный заявителемIf the process of saturation of the melt will take place under the conditions above specified in the description, the cost of the process and equipment increases several times. In the case when the process of refining does not completely remove impurities due to the formation of a stable compound and their sorption, the remaining elements of the impurities react with the filter material and remain on its surface. As the material of the reaction filter using sorbent material developed and patented by the applicant
Лучшие примеры осуществления предлагаемого способа рафинирования благородных металлов. Пример 1. Исходным материалом взят золотой шлих, содержащий золото Au-81%, железо Fe- 7%, медь Cu- 3% , кремнийThe best examples of the proposed method of refining precious metals. Example 1. The source material was taken gold concentrate containing gold Au-81%, iron Fe-7%, copper Cu-3%, silicon
Si -5%, сера S- 1%, углерод С- 1%Si -5%, sulfur S- 1%, carbon С- 1%
Газовая композиция, которую использовали для проведения способа рафинирования, состоит из кислорода Ch -5%, ацетил C2H2 - 7%, азот N2 - остальное.The gas composition used for the refining method consists of oxygen Ch -5%, acetyl C2H2 - 7%, nitrogen N2 - the rest.
Исходный материал нагревают до температуры 1500 C°, насыщают газовой композицией под давлением 20OMTIa в течение 15 минут, и подвергают сорбции и фильтрации через материал с удельной поверхностью 1500 м2/гp при температуре 1650 C0 в вакууме 5*10 мм рт.ст.The starting material is heated to a temperature of 1500 C °, saturated with a gas composition under a pressure of 20OMTIa for 15 minutes, and subjected to sorption and filtration through a material with a specific surface of 1500 m 2 / gp at a temperature of 1650 C 0 in a vacuum of 5 * 10 mm Hg.
Анализ химического состава шлама показал, что содержание золота возросло до 99,5% за одну операцию рафинирования, повторная обработка расплава только за счет реакции фильтрации повышает концентрацию золота до 99,97% Пример 2. Исходным материалом взят палладиевый концентрат, содержащий палладий Pd - 43%, медь Cu- 13% , серебро Ag - 27%, сера S- 13%, мышьяк As -3%, теллур Tl- 1% Газовая композиция, которую использовали при проведении способа рафинирования, состоит из кислорода Ch -7%, ацетил C2H2 - 15%, азот N2 - 78%An analysis of the chemical composition of the sludge showed that the gold content increased to 99.5% in one refining operation, the repeated processing of the melt only due to the filtration reaction increases the gold concentration to 99.97%. Example 2. A palladium concentrate containing palladium Pd - 43 was taken as the starting material. %, copper Cu- 13%, silver Ag - 27%, sulfur S- 13%, arsenic As -3%, tellurium Tl- 1% The gas composition used in the refining process consists of oxygen Ch -7%, acetyl C2H2 - 15%, nitrogen N 2 - 78%
Исходный материал нагревают до температуры 1700 C°, насыщают газовой композицией под давлением 150MTTa в течение 30 минут, и подвергают сорбции - фильтрации через материал с удельной поверхностью 1700 м2/гp при температуре 1750 C° в вакууме 10"2 мм рт.ст.The starting material is heated to a temperature of 1700 C °, saturated with a gas composition under a pressure of 150MTTa for 30 minutes, and subjected to sorption-filtration through a material with a specific surface of 1700 m 2 / gp at a temperature of 1750 C ° in a vacuum of 10 "2 mm Hg.
Химического анализ палладиевого сплава показал, что после акта рафинирования его состав стал равен палладий Pd - 97%, серебро Ag - 1 ,5%, медь Cu- 0,5% , теллур Tl- 1 %A chemical analysis of the palladium alloy showed that after the act of refining its composition became equal to palladium Pd - 97%, silver Ag - 1, 5%, copper Cu - 0.5%, tellurium Tl - 1%
Повторное рафинирование в две стадии привело к увеличению концентрации палладия Pd - 98,9%, серебро Ag - 1,01%, медь Cu- 0,001% , Tl-0,005% Промышленная применимость.Repeated refining in two stages led to an increase in the concentration of palladium Pd - 98.9%, silver Ag - 1.01%, copper Cu-0.001%, Tl-0.005% Industrial applicability.
Вышеприведенные результаты проведенного способа рафинирования благородных металлов доказывают возможность наиболее полное извлечение металлов с сверхвысокой чистотой, (рафинирование золотого шлиха в палладиевом концентрате позволяет получать золота в слитке в интервале от 99% до 99,9995 в зависимости от многократности стадии рафинирования The above results of the refining method of precious metals prove the possibility of the most complete extraction of metals with ultra-high purity, (refining of gold concentrate in palladium concentrate allows you to get gold in the ingot in the range from 99% to 99.9995 depending on the multiple stages of refining
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2006127399A RU2318886C1 (en) | 2006-07-28 | 2006-07-28 | Noble metal refining method |
| RU2006127399 | 2006-07-28 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| WO2008013479A2 true WO2008013479A2 (en) | 2008-01-31 |
| WO2008013479A3 WO2008013479A3 (en) | 2008-03-13 |
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ID=38981911
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/RU2007/000401 Ceased WO2008013479A2 (en) | 2006-07-28 | 2007-07-20 | Method for refining precious metals |
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| Country | Link |
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| RU (1) | RU2318886C1 (en) |
| WO (1) | WO2008013479A2 (en) |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA981911A (en) * | 1973-03-12 | 1976-01-20 | Derek G. Kerfoot | Refining silver-bearing residues |
| EP0077128B1 (en) * | 1981-09-16 | 1989-04-19 | Matthey Rustenburg Refiners (Proprietary) Limited | Recovery of platinum group metals from scrap and residues |
| RU2033447C1 (en) * | 1991-03-14 | 1995-04-20 | Научно-производственный комплекс "Суперметалл" | Method of refining of noble metals and their alloys |
| RU2048554C1 (en) * | 1992-05-13 | 1995-11-20 | Крылов Владимир Владимирович | Method for gold refining |
| RU2086685C1 (en) * | 1995-12-14 | 1997-08-10 | Акционерное общество открытого типа "Екатеринбургский завод по обработке цветных металлов" | Method for pyrometallurgical refining gold- and silver-containing wastes |
| TR200401861T4 (en) * | 2000-01-28 | 2004-09-21 | Umicore | Wet process for refining silver ingots including gold separation |
| JP4455985B2 (en) * | 2004-12-28 | 2010-04-21 | 日鉱金属株式会社 | Method for removing impurities in platinum |
-
2006
- 2006-07-28 RU RU2006127399A patent/RU2318886C1/en not_active IP Right Cessation
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2007
- 2007-07-20 WO PCT/RU2007/000401 patent/WO2008013479A2/en not_active Ceased
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| WO2008013479A3 (en) | 2008-03-13 |
| RU2318886C1 (en) | 2008-03-10 |
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