CN112126790A - Chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy - Google Patents
Chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy Download PDFInfo
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- CN112126790A CN112126790A CN202010987825.2A CN202010987825A CN112126790A CN 112126790 A CN112126790 A CN 112126790A CN 202010987825 A CN202010987825 A CN 202010987825A CN 112126790 A CN112126790 A CN 112126790A
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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
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
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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
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
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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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- 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
- Y02P10/25—Process efficiency
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Abstract
The invention relates to a chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy, belonging to the technical field of metal materials. The aim of removing base metals is achieved by melting platinum, platinum rhodium or platinum rhodium palladium metals and then introducing chlorine above the metal liquid level. The method can efficiently remove base metal elements such as copper, iron, nickel, tin and the like in precious metals such as platinum, platinum rhodium or platinum rhodium palladium alloy, and the total impurity content of the prepared metal ingot is less than 0.05%. The invention improves the purification efficiency of noble metals of platinum, platinum rhodium and platinum rhodium palladium, greatly simplifies the purification process and can ensure that the material meets the manufacturing requirements of general products.
Description
Technical Field
The invention relates to a chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy, in particular to a method for quickly removing base metals in precious metals of platinum, platinum rhodium or platinum rhodium palladium alloy, belonging to the technical field of metal materials.
Background
Platinum, platinum rhodium and platinum rhodium palladium alloys are common noble metal alloys and can be respectively used in the fields of optical glass, glass fiber, catalytic mesh and the like, and when the waste noble metals are produced, the recovery problem exists.
Generally, the traditional precious metal recovery adopts chemical purification, namely, precious metal is dissolved by aqua regia and then separated and purified. The method has the defects of long recovery period and large precious metal loss. In modern industry, precious metals are purified mainly by removing base metals, mainly iron, copper, nickel, tin and other elements, in the precious metals, the content of each component of the precious metals can be determined by a modern test method, when the total amount of impurities meets the requirement of a common product, separation and purification are not necessary, and the precious metals can be supplemented according to the amount of the missing precious metal components during batching, so that the industrial requirement can be met.
Disclosure of Invention
The invention aims to provide a chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy aiming at various defects of chemical purification, and skillfully provides a chlorination purification process, wherein chloride is formed by chlorine and base metal at high temperature, and then the base metal is removed by utilizing the characteristic of low saturated vapor pressure of the chloride.
The technical scheme of the invention is a chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy, which is characterized by comprising the following steps:
(1) preparing chlorine gas: preparing chlorine gas by potassium permanganate and concentrated hydrochloric acid by adopting a Kipp's generator;
(2) preheating: preheating the metal to be purified by using a high-frequency induction furnace, wherein the preheating power is 8-16 kw, and the time is 5-15 min;
(3) ingot melting: adjusting the power to 20-30 kw until all the metals preheated in the step (2) are melted;
(4) and (3) heat preservation: adjusting the power to 16-20 kw, and preserving the temperature of the molten liquid;
(5) chlorination and impurity removal: introducing the chlorine prepared in the step (1) into the molten liquid level obtained in the step (4), and determining chlorination impurity removal time according to the total amount of impurities;
(6) casting: and (5) casting the molten metal obtained in the step (5) into a water-cooled copper mold to obtain an alloy ingot.
Furthermore, in the step (1), the concentrated hydrochloric acid is excessive relative to the potassium permanganate, and the dropping speed of the concentrated hydrochloric acid is kept between 1 and 2 d/s.
Further, in the step (2), the atmosphere of the high-frequency induction melting is an atmospheric atmosphere.
Further, the chlorination impurity removal time in the step (5) is related to the impurity types and the total amount of impurities, and the impurities are all converted by iron;
when the total amount of impurities is less than 0.01%, the chlorination time is 1-1.5 h;
when the total amount of impurities is 0.01-0.05%, the chlorination time is 1.5-3 h;
when the total amount of impurities is 0.05-0.1%, the chlorination time is 3-6 h;
when the total amount of impurities is more than 0.1 percent, chlorination and impurity removal are carried out for many times.
Further, the distance between the chlorine outlet and the molten liquid level in the step (5) is 8-20 mm.
Further, the casting power in the step (6) is 16-20 kw.
The invention has the beneficial effects that: the waste material of noble metal is platinum, platinum rhodium or platinum rhodium palladium, besides silver, the contents of other noble metals such as gold, iridium, ruthenium and osmium are required to meet the requirement of less than 0.01 percent.
The invention can effectively remove iron, copper, nickel, tin and other base metals, and other base metals which can be effectively chlorinated can be removed according to the process of the invention. The invention finally enables the total content of impurities in the noble metal to be less than 0.05 percent, and meets the requirement that the main content of the noble metal is more than 99.95 percent.
Detailed Description
The technical solutions in the embodiments of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
Example 1
(1) Preparing chlorine gas: prepared by potassium permanganate and concentrated hydrochloric acid by adopting a Kipp's generator.
(2) Preheating: preheating the platinum waste to be purified by using a high-frequency induction furnace, wherein the measured iron content in the platinum waste is 0.015%, the measured copper content is 0.005%, the measured nickel content in the platinum waste is 0.006%, the preheating power is 8kw, and the time is 5 min;
(3) ingot melting: adjusting the power to 20kw until the metal is completely melted;
(4) and (3) heat preservation: the power was adjusted to 16kw and the melt was kept warm.
(5) Chlorination and impurity removal: and introducing chlorine into the liquid level of the melt, wherein the chlorine introducing rate controls the dropping speed of the concentrated hydrochloric acid in the Kipp apparatus to be 1 drop per second and the time to be 2 hours.
(6) Casting: and (4) casting the molten metal into a water-cooled copper mold to obtain an alloy cast ingot.
(7) And (3) testing: finally, the contents of iron, copper and nickel are respectively measured to be 0.003%, 0.0005% and 0.001% respectively, and the judgment is carried out according to the requirements of GB/T1419-2015, so that the requirements of 99.95% are met.
The energy efficiency comparison of the purification method of the embodiment 1 of the invention and the traditional chemical purification is carried out, the consumed materials are shown in table 1, and the energy efficiency comparison result is shown in table 2.
TABLE 1
As shown in table 1, in example 1, excessive elements such as iron, copper, and nickel were removed by chemical materials, and thus the consumed materials were small. The traditional method needs to dissolve all metals and then carry out reduction purification, thereby consuming a large amount of chemical materials.
TABLE 2
Efficiency of | Energy consumption | Device | |
Example 1 | 2 hours | 30 kilowatt-hour | High-frequency induction furnace and Kipp generator |
Chemical purification method | 3 days | 200 kilowatt-hour | Various glassware and heating pad |
The invention has the advantages of high efficiency, low energy consumption, high automation degree of equipment and the like. In actual production, one worker can watch four devices at the same time, and the traditional method needs three workers to work for three days to complete the same work task. Taking eight hours of work per day as an example, the method can improve 144 times of labor efficiency compared with the traditional method, so the method has excellent practical significance and popularization value.
Example 2
(1) Preparing chlorine gas: prepared by potassium permanganate and concentrated hydrochloric acid by adopting a Kipp's generator.
(2) Preheating: preheating platinum-rhodium waste to be purified by using a high-frequency induction electric furnace, wherein the measured iron content in the platinum-rhodium waste is 0.02%, the measured copper content is 0.008%, the measured nickel content is 0.003%, the measured tin content is 0.01%, the preheating power is 16kw, and the preheating time is 15 min;
(3) ingot melting: adjusting the power to 30kw until the metal is completely melted;
(4) and (3) heat preservation: the power was adjusted to 20kw and the melt was kept warm.
(5) Chlorination and impurity removal: chlorine gas is introduced into the liquid level of the melt, and the chlorine gas introduction rate controls the dropping speed of concentrated hydrochloric acid in the Kipp apparatus to be 2 drops per second and the time to be 2 hours.
(6) Casting: and (4) casting the molten metal into a water-cooled copper mold to obtain an alloy cast ingot.
(7) And (3) testing: finally, the contents of iron, copper, nickel and tin are respectively measured to be 0.002%, 0.0005%, 0.0015% and 0.003% respectively, and the contents of platinum and rhodium in the main content meet the requirement of 99.95% by judging other elements except rhodium according to the requirement of GB/T1419-2015.
Example 3
(1) Preparing chlorine gas: prepared by potassium permanganate and concentrated hydrochloric acid by adopting a Kipp's generator.
(2) Preheating: preheating platinum-rhodium-palladium waste to be purified by using a high-frequency induction furnace, wherein the measured iron content in the platinum-rhodium-palladium waste is 0.025%, the measured copper content is 0.006%, the measured nickel content is 0.002%, the measured tin content is 0.008%, the preheating power is 18kw, and the preheating time is 12 min;
(3) ingot melting: adjusting the power to 28kw until the metal is completely melted;
(4) and (3) heat preservation: the power was adjusted to 18kw and the melt was kept warm.
(5) Chlorination and impurity removal: chlorine gas is introduced into the liquid level of the melt, and the chlorine gas introduction rate controls the dropping speed of concentrated hydrochloric acid in the Kipp apparatus to be 2 drops per second and the time to be 3 hours.
(6) Casting: and (4) casting the molten metal into a water-cooled copper mold to obtain an alloy cast ingot.
(7) And (3) testing: finally, the iron content is 0.002%, the copper content is 0.0005%, the nickel content is 0.0005%, and the tin content is 0.001%, and the total content of the main platinum and the rhodium palladium meets the requirement of 99.95% by judging other elements except the rhodium and the palladium according to the requirement of GB/T1419-.
Claims (6)
1. A chlorination purification method of platinum, platinum rhodium or platinum rhodium palladium alloy is characterized by comprising the following steps:
(1) preparing chlorine gas: preparing chlorine gas by potassium permanganate and concentrated hydrochloric acid by adopting a Kipp's generator;
(2) preheating: preheating the metal to be purified by using a high-frequency induction furnace, wherein the preheating power is 8-16 kw, and the time is 5-15 min;
(3) ingot melting: adjusting the power to 20-30 kw until all the metals preheated in the step (2) are melted;
(4) and (3) heat preservation: adjusting the power to 16-20 kw, and preserving the temperature of the molten liquid;
(5) chlorination and impurity removal: introducing the chlorine prepared in the step (1) into the molten liquid level obtained in the step (4), and determining chlorination impurity removal time according to the total amount of impurities;
(6) casting: and (5) casting the molten metal obtained in the step (5) into a water-cooled copper mold to obtain an alloy ingot.
2. The method for purifying platinum, platinum rhodium or platinum rhodium palladium alloy by chlorination as claimed in claim 1, wherein: in the step (1), the concentrated hydrochloric acid is excessive relative to potassium permanganate, and the dropping speed of the concentrated hydrochloric acid is kept at 1-2 d/s.
3. The method for purifying platinum, platinum rhodium or platinum rhodium palladium alloy by chlorination as claimed in claim 1, wherein: in the step (2), the atmosphere of the high-frequency induction melting is atmospheric atmosphere.
4. The method for purifying platinum, platinum rhodium or platinum rhodium palladium alloy by chlorination as claimed in claim 1, wherein: the chlorination impurity removal time in the step (5) is related to the impurity types and the total amount of impurities, and the impurities are all converted by iron;
when the total amount of impurities is less than 0.01%, the chlorination time is 1-1.5 h;
when the total amount of impurities is 0.01-0.05%, the chlorination time is 1.5-3 h;
when the total amount of impurities is 0.05-0.1%, the chlorination time is 3-6 h;
when the total amount of impurities is more than 0.1 percent, chlorination and impurity removal are carried out for many times.
5. The method for purifying platinum, platinum rhodium or platinum rhodium palladium alloy by chlorination as claimed in claim 1, wherein: in the step (5), the distance between the chlorine outlet and the molten liquid level is 8-20 mm.
6. The method for purifying platinum, platinum rhodium or platinum rhodium palladium alloy by chlorination as claimed in claim 1, wherein: in the step (6), the casting power is 16-20 kw.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114737063A (en) * | 2022-03-22 | 2022-07-12 | 咸阳欧冶科技有限公司 | Platinum alloy purification process |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101713030A (en) * | 2008-09-29 | 2010-05-26 | 日矿金属株式会社 | Method of separating rhodium from platinum and/or palladium |
CN101974698A (en) * | 2010-09-17 | 2011-02-16 | 重庆国际复合材料有限公司 | Method for chloridizing, refining and purifying old bushing platinum-rhodium alloy for glass fiber |
CN104342558A (en) * | 2014-05-12 | 2015-02-11 | 上海派特贵金属环保科技有限公司 | A method for recycling palladium from a spent precious metal catalyst |
CN110172570A (en) * | 2018-12-27 | 2019-08-27 | 昆明理工大学 | A kind of processing method of precious metals containing lead |
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- 2020-09-18 CN CN202010987825.2A patent/CN112126790A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101713030A (en) * | 2008-09-29 | 2010-05-26 | 日矿金属株式会社 | Method of separating rhodium from platinum and/or palladium |
CN101974698A (en) * | 2010-09-17 | 2011-02-16 | 重庆国际复合材料有限公司 | Method for chloridizing, refining and purifying old bushing platinum-rhodium alloy for glass fiber |
CN104342558A (en) * | 2014-05-12 | 2015-02-11 | 上海派特贵金属环保科技有限公司 | A method for recycling palladium from a spent precious metal catalyst |
CN110172570A (en) * | 2018-12-27 | 2019-08-27 | 昆明理工大学 | A kind of processing method of precious metals containing lead |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114737063A (en) * | 2022-03-22 | 2022-07-12 | 咸阳欧冶科技有限公司 | Platinum alloy purification process |
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Address after: Xishan District Beizhen Jiangsu province 214192 new Tin Village in Wuxi City Applicant after: Intel platinum Co.,Ltd. Address before: Xishan District Beizhen Jiangsu province 214192 new Tin Village in Wuxi City Applicant before: WUXI INTERNATIONAL PLATINUM Co.,Ltd. |
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Application publication date: 20201225 |