CN112458307A - Separation method of platinum-silver alloy - Google Patents
Separation method of platinum-silver alloy Download PDFInfo
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- CN112458307A CN112458307A CN202011276581.3A CN202011276581A CN112458307A CN 112458307 A CN112458307 A CN 112458307A CN 202011276581 A CN202011276581 A CN 202011276581A CN 112458307 A CN112458307 A CN 112458307A
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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
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
- 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
- C22B7/006—Wet processes
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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
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Abstract
The invention discloses a method for separating a platinum-silver alloy, which comprises the following steps: crushing the platinum-silver alloy through mechanical equipment; ultrasonic dissolving in aqua regia system; adding ammonia water for dissolution and precipitation; filtering and reducing to obtain low-valence platinum salt; adding hydrazine hydrate to reduce to obtain spongy platinum; the method mainly aims at the platinum-silver alloy, all chemical agents adopted in the whole process are few, firstly, silver in the platinum-silver alloy can be screened and filtered in the separation process, a platinum filter cake is reduced to obtain a solution, and the solution is separated in a sponge platinum state through hydrazine hydrate reaction. And excessive equipment is not needed for matching use, the use cost is relatively low, the content of each metal in the separated mixed solution is also the lowest, no metal emission can be realized, and the environment-friendly production is realized while the precious metal is recovered.
Description
Technical Field
The invention relates to the technical field of precious metal purification and recovery, in particular to a method for separating a platinum-silver alloy.
Background
Noble metals are strategic reserves, mainly comprise 8 metal elements such as gold, silver and platinum group metals, and are often used as valuable jewel cases, currency and the like due to the characteristics of extremely stable physical and chemical properties and the like; in addition, in modern science and technology, precious metals are mainly applied to industrial and scientific research, including aerospace, navigation, chemical engineering, electronics, metallurgy and the like, and due to the rare and wide application performance of precious metal resources, the technology for researching and developing the mining and secondary resource recovery of the precious metals is urgently needed.
The platinum-silver alloy is a binary alloy with platinum as a base and silver added, the smelting and the processing are difficult, the smelting is carried out under the protection of argon gas in a high-frequency furnace, after ingot casting is homogenized, the tensile wire element processed into plates, wires and the like for manufacturing precision instruments is rapidly developed along with the continuous progress of science and technology at present, of course, the speed of updating various devices is also rapidly updated, so that the speed of updating the parts of the platinum-silver alloy products is also increased, and with a large amount of platinum-silver alloy along with the waste products, in order to realize good recycling, the timely recycling of the platinum-silver alloy in the parts becomes the key for recycling resources and reducing the production and use costs, therefore, how to rapidly and efficiently recover the precious metals in the platinum-silver alloy is a problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for separating a platinum-silver alloy, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a separation method of platinum-silver alloy comprises the following steps:
the method comprises the following steps: crushing the platinum-silver alloy material through mechanical equipment to obtain platinum-silver alloy particles for later use;
step two: placing the platinum-silver alloy particles prepared in the step one in a container, adding a certain amount of mixed solution of concentrated hydrochloric acid and concentrated nitric acid into the container, and slightly stirring the mixed solution to obtain a mixed solution;
step three: heating the mixed solution obtained in the step two, and allowing the mixture to react;
step four: placing the mixed solution after the heating reaction in the step three into an ultrasonic instrument for ultrasonic dissolution, and dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for a period of time;
step five: filtering the solution obtained in the fourth step after ultrasonic dissolution and reaction with ammonia water, and then repeating the operation of the fourth step and the operation of the fifth step;
step six: adding the filter cake obtained by filtering in the fifth step into a reducing agent solution for reaction;
step seven: filtering the mixed solution after the reaction in the sixth step to obtain an ammonium platinochloride solution;
step eight: slowly adding hydrazine hydrate into the mixed filtrate obtained in the step seven, and carrying out reduction reaction to obtain spongy platinum;
step nine: placing the spongy platinum obtained in the step eight in a muffle furnace for drying
Preferably, the volume ratio of the concentrated hydrochloric acid to the concentrated nitric acid in the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid in the second step is 2-10: 1.
preferably, the mass ratio of the mixed solution of concentrated hydrochloric acid and concentrated nitric acid to the platinum-silver alloy in the second step is 2-20: 1.
preferably, the heating temperature of the solution in the third step is 70-100 ℃, and the heating reaction time of the mixed solution is 10-60 minutes.
Preferably, the ultrasonic dissolution time in the fourth step is controlled to be 10-60 minutes, and the water bath temperature of the mixed solution during ultrasonic dissolution is 70-90 ℃.
Preferably, the mass ratio of the addition amount of the ammonia water solution to the platinum-silver alloy in the fourth step is 2-50: 1, the reaction time after dropping ammonia water is 20 to 40 minutes.
Preferably, the mass ratio of the reducing agent to the platinum-silver alloy in the step eight is 1: 1-20 ℃, the temperature of the reduction reaction is 70-100 ℃, and the time of the reduction reaction is 0.5-1 hour.
Preferably, the drying temperature in the muffle furnace in the step nine is controlled to be 500-650 ℃, and the drying time is 1-4 hours.
Compared with the prior art, the invention has the beneficial effects that:
the separation method of the platinum-silver alloy mainly aims at the platinum-silver alloy, all chemical agents adopted in the whole process only comprise concentrated hydrochloric acid, concentrated nitric acid, ammonia water, reducing agents and the like, firstly, silver in the platinum-silver alloy can be screened and filtered in the separation process, a platinum filter cake is reduced to obtain a solution, and the solution is obtained by separation in a spongy platinum state through hydrazine hydrate reaction. Meanwhile, excessive equipment is not needed to be used in a matched mode, the use cost is relatively low, the content of each metal in the separated mixed solution is the lowest, metal-free emission can be achieved, and environment-friendly production is achieved while precious metals are recycled.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles.
Example 2: according to the mass ratio of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid to the platinum-silver alloy of 2: preparing a mixed solution according to the proportion of 1, namely preparing 200g of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid, and preparing the mixed solution according to the mixing proportion of the concentrated hydrochloric acid and the concentrated nitric acid in the mixed solution according to the proportion of 2:1, namely preparing 1L of hydrochloric acid and 250ml of nitric acid.
Example 3: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the platinum-silver alloy particles to the mixed solution of concentrated nitric acid and concentrated hydrochloric acid is 2: preparing a mixed solution according to the proportion of 1, namely preparing 200g of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid, and preparing the mixed solution according to the mixed proportion of the concentrated hydrochloric acid and the concentrated nitric acid in the mixed solution according to the proportion of 2:1, mixing and slightly stirring.
Example 4: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the platinum-silver alloy particles to the mixed solution of concentrated nitric acid and concentrated hydrochloric acid is 2: preparing a mixed solution according to the proportion of 1, namely preparing 200g of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid, preparing the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid according to the mixing proportion of 2:1 in the mixed solution, mixing and slightly stirring, heating in a water area, and controlling the continuous heating reaction time to be thirty minutes.
Example 5: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid to the platinum-silver alloy is 2:1, preparing a mixed solution according to a proportion of 1, heating a water area, controlling continuous heating reaction time to be thirty minutes, putting the mixed solution after the heating reaction into an ultrasonic instrument for ultrasonic dissolution, in the embodiment, dropwise adding ammonia water into the mixed solution after ultrasonic dissolution is carried out for 30 minutes, wherein the ultrasonic time is 10 minutes, the water bath temperature during ultrasonic dissolution is 70 ℃, then dropwise adding 1L of ammonia water into the solution, and continuing to react for 30 minutes.
Example 6: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid to the platinum-silver alloy is 2:1, preparing a mixed solution according to a proportion, heating a water area, controlling continuous heating reaction time to be thirty minutes later, placing the mixed solution after the heating reaction into an ultrasonic instrument for ultrasonic dissolution, dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for 30 minutes, filtering the mixed solution after the reaction is carried out for 30 minutes, continuing the steps of ultrasonic dissolution and dropwise adding ammonia water in an environment with the temperature of 70 ℃ after the filtering is finished, then carrying out filtering operation again, and repeating the steps twice.
Example 7: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid to the platinum-silver alloy is 2:1, preparing a mixed solution according to a proportion, heating a water area, controlling continuous heating reaction time to be thirty minutes later, placing the mixed solution after the heating reaction in an ultrasonic instrument for ultrasonic dissolution, dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for 30 minutes, filtering the mixed solution after the reaction is carried out for 30 minutes, continuing the steps of ultrasonic dissolution and dropwise adding ammonia water in an environment with the temperature of 70 ℃ after the filtering is finished, then carrying out filtering operation, obtaining a plurality of filter cakes after the steps are repeated twice, then adding the filter cakes into 200g of hydrazine hydrochloride solution, controlling the concentration of the hydrazine hydrochloride aqueous solution to be 30%, controlling the reaction temperature to be 70 ℃, reacting for 1 hour, and filtering to obtain the ammonium chloroplatinate solution after the reaction is finished.
Example 8: 200g of platinum-silver alloy is crushed by mechanical equipment to obtain platinum-silver alloy particles, and the mass ratio of the mixed solution of concentrated nitric acid and concentrated hydrochloric acid to the platinum-silver alloy is 2:1 proportion preparing a mixed solution, heating a water area, controlling the continuous heating reaction time to thirty minutes later, placing the mixed solution after the heating reaction in an ultrasonic instrument for ultrasonic dissolution, dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for 30 minutes, filtering the mixed solution after the reaction is carried out for 30 minutes, continuing the steps of ultrasonic dissolution and dropwise adding ammonia water under the environment with the temperature of 70 ℃ after the filtering is finished, then carrying out the filtering operation again, obtaining a plurality of filtered substances, namely filter cakes after the steps are repeated twice, then adding the filter cakes into 200g of hydrazine hydrochloride solution, controlling the concentration of the hydrazine hydrochloride solution to be 30 percent, controlling the reaction temperature to be 70 ℃ for 1 hour, filtering after the reaction is finished to obtain an ammonium platinate chloride solution, heating the ammonium platinate chloride solution to 70 ℃, slowly adding the hydrazine hydrate solution for reduction to obtain spongy platinum, placing the sponge platinum in a muffle furnace, heating to 650 ℃, and drying after 2 hours to obtain a sponge platinum product.
The separation method comprises the following steps: the method comprises the following steps: the method comprises the following steps: crushing the platinum-silver alloy material through mechanical equipment to obtain platinum-silver alloy particles for later use; step two: placing the platinum-silver alloy particles prepared in the step one in a container, adding a certain amount of mixed solution of concentrated hydrochloric acid and concentrated nitric acid into the container, and slightly stirring the mixed solution to obtain a mixed solution; step three: heating the mixed solution obtained in the step two, and allowing the mixture to react; step four: placing the mixed solution after the heating reaction in the step three into an ultrasonic instrument for ultrasonic dissolution, and dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for a period of time; step five: filtering the solution obtained in the fourth step after ultrasonic dissolution and reaction with ammonia water, and then repeating the operation of the fourth step and the operation of the fifth step; step six: putting the filter cake obtained by filtering in the fifth step into a reducing agent solution for reaction; step seven: filtering the mixed solution after the reaction in the sixth step to obtain an ammonium platinochloride solution; step eight: slowly adding hydrazine hydrate into the mixed filtrate obtained in the step seven, and carrying out reduction reaction to obtain spongy platinum; step nine: and (5) placing the spongy platinum obtained in the step eight in a muffle furnace for drying.
In summary, the separation method of the platinum-silver alloy mainly aims at the platinum-silver alloy, all chemical agents adopted in the whole process are only concentrated hydrochloric acid, concentrated nitric acid, ammonia water, reducing agents and the like, firstly, silver in the platinum-silver alloy can be screened and filtered in the separation process, a platinum filter cake is reduced to obtain a solution, and the solution is obtained by separation in a sponge platinum state through hydrazine hydrate reaction. Meanwhile, excessive equipment is not needed to be used in a matched mode, the use cost is relatively low, the content of each metal in the separated mixed solution is the lowest, metal-free emission can be achieved, and environment-friendly production is achieved while precious metals are recycled.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A separation method of platinum-silver alloy is characterized by comprising the following steps:
the method comprises the following steps: crushing the platinum-silver alloy material through mechanical equipment to obtain platinum-silver alloy particles for later use;
step two: placing the platinum-silver alloy particles prepared in the step one in a container, adding a certain amount of mixed solution of concentrated hydrochloric acid and concentrated nitric acid into the container, and slightly stirring the mixed solution to obtain a mixed solution;
step three: heating the mixed solution obtained in the step two, and allowing the mixture to react;
step four: placing the mixed solution after the heating reaction in the step three into an ultrasonic instrument for ultrasonic dissolution, and dropwise adding ammonia water into the mixed solution after the ultrasonic dissolution is carried out for a period of time;
step five: filtering the solution obtained in the fourth step after ultrasonic dissolution and reaction with ammonia water, and then repeating the operation of the fourth step and the operation of the fifth step;
step six: adding the filter cake obtained by filtering in the fifth step into a reducing agent solution for reaction;
step seven: filtering the mixed solution after the reaction in the sixth step to obtain an ammonium platinochloride solution;
step eight: slowly adding hydrazine hydrate into the mixed filtrate obtained in the step seven, and carrying out reduction reaction to obtain spongy platinum;
step nine: and (5) placing the spongy platinum obtained in the step eight in a muffle furnace for drying.
2. The method for separating a platinum-silver alloy according to claim 1, wherein: and in the second step, the volume ratio of the concentrated hydrochloric acid to the concentrated nitric acid in the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid is 2-10: 1.
3. the method for separating a platinum-silver alloy according to claim 1, wherein: and in the second step, the mass ratio of the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid to the platinum-silver alloy is 2-20: 1.
4. the method for separating a platinum-silver alloy according to claim 1, wherein: in the third step, the heating temperature of the solution is 70-100 ℃, and the heating reaction time of the mixed solution is 10-60 minutes.
5. The method for separating a platinum-silver alloy according to claim 1, wherein: the ultrasonic dissolving time in the fourth step is controlled to be 10-60 minutes, and the water bath temperature of the mixed solution is 70-90 ℃ during ultrasonic dissolving.
6. The method for separating a platinum-silver alloy according to claim 1, wherein: the mass ratio of the addition amount of the ammonia water solution to the platinum-silver alloy in the fourth step is 2-50: 1, the reaction time after dropping ammonia water is 20 to 40 minutes.
7. The method for separating a platinum-silver alloy according to claim 1, wherein: the mass ratio of the reducing agent to the platinum-silver alloy in the step eight is 1: 1-20 ℃, the temperature of the reduction reaction is 70-100 ℃, and the time of the reduction reaction is 0.5-1 hour.
8. The method for separating a platinum-silver alloy according to claim 1, wherein: and the drying temperature in the muffle furnace in the step nine is controlled to be 500-650 ℃, and the drying time is 1-4 hours.
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| CN1339611A (en) * | 2000-08-25 | 2002-03-13 | 贵研铂业股份有限公司 | Method for recovering silver-platinum from platinum containing silver iodide slag |
| CN101255501A (en) * | 2008-04-08 | 2008-09-03 | 昆明贵研药业有限公司 | Method for reclaiming platinum-silver-iodine form platinum-containing silver iodide slag |
| CN102041393A (en) * | 2010-12-30 | 2011-05-04 | 郴州市金贵银业股份有限公司 | Silver anode mud treatment process |
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| CN106756085A (en) * | 2016-12-22 | 2017-05-31 | 邝贤语 | A kind of smelting process of platinum concentrate |
| CN107604165A (en) * | 2017-09-01 | 2018-01-19 | 鑫广再生资源(上海)有限公司 | A kind of method of platinum group metal extraction and refining in ternary catalyst for automobile tail gas |
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2020
- 2020-11-16 CN CN202011276581.3A patent/CN112458307A/en active Pending
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| CN1339611A (en) * | 2000-08-25 | 2002-03-13 | 贵研铂业股份有限公司 | Method for recovering silver-platinum from platinum containing silver iodide slag |
| CN101255501A (en) * | 2008-04-08 | 2008-09-03 | 昆明贵研药业有限公司 | Method for reclaiming platinum-silver-iodine form platinum-containing silver iodide slag |
| CN102041393A (en) * | 2010-12-30 | 2011-05-04 | 郴州市金贵银业股份有限公司 | Silver anode mud treatment process |
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| CN106756085A (en) * | 2016-12-22 | 2017-05-31 | 邝贤语 | A kind of smelting process of platinum concentrate |
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Non-Patent Citations (1)
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Address after: 214000 Xinba village, Xibei Town, Xishan District, Wuxi City, Jiangsu Province Applicant after: Intel platinum Co.,Ltd. Address before: 214000 Xinba village, Xibei Town, Xishan District, Wuxi City, Jiangsu Province Applicant before: WUXI INTERNATIONAL PLATINUM Co.,Ltd. |
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Application publication date: 20210309 |