CN110964905A - Method for purifying crude ammonium chloroplatinate - Google Patents
Method for purifying crude ammonium chloroplatinate Download PDFInfo
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- CN110964905A CN110964905A CN201811140336.2A CN201811140336A CN110964905A CN 110964905 A CN110964905 A CN 110964905A CN 201811140336 A CN201811140336 A CN 201811140336A CN 110964905 A CN110964905 A CN 110964905A
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- Prior art keywords
- ammonium chloroplatinate
- mixed solution
- crude ammonium
- heating
- chloroplatinate
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- 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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- 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
Abstract
The invention discloses a method for purifying crude ammonium chloroplatinate, which is implemented according to the following steps: step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and stirring to obtain a mixed solution; step 2, boiling the mixed solution and keeping the mixed solution for a fixed time, adding ammonium chloride, and filtering the mixed solution after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate and filtrate; step 3, adjusting the pH value of the filtrate to 8-9, heating, adding hydrazine hydrate for reduction, and recovering gold, palladium and tellurium; the invention adopts an aqueous solution chlorination method to remove impurity elements such as gold, palladium, tellurium and the like in the crude ammonium chloroplatinate, and the process is simple and easy to implement.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a method for purifying crude ammonium chloroplatinate.
Background
And dissolving the mixture of ammonium chloroplatinate and ammonium chloroplatinate by sodium sulfite to separate palladium to obtain crude ammonium chloroplatinate, wherein the crude ammonium chloroplatinate also contains impurity elements such as gold, palladium, tellurium and the like. If the crude ammonium chloroplatinate is directly fed into the platinum refining process, the impurity elements are not removed, and the load of the platinum refining process is increased. Therefore, it is necessary to adopt a new process for removing impurity elements from the crude ammonium chloroplatinate.
Disclosure of Invention
The invention aims to provide a method for purifying crude ammonium chloroplatinate, which can reduce the dissolving time and the energy consumption.
The technical scheme adopted by the invention is that the purification method of the crude ammonium chloroplatinate is implemented according to the following steps:
step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
step 2, boiling the mixed solution obtained in the step 1 and keeping the mixed solution for a fixed time, then adding ammonium chloride, and filtering after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate and filtrate;
and 3, adjusting the pH value of the filtrate obtained in the step 2 to 8-9, heating, adding hydrazine hydrate for reduction, and recovering gold, palladium and tellurium.
The present invention is also characterized in that,
the specific method for slurrying crude ammonium chloroplatinate in the step 1 comprises the following steps: mixing pure water according to the proportion of 5-10: 1 volume ratio was added to crude ammonium chloroplatinate for slurrying.
The heating temperature in the step 1 is 80-90 ℃, the adding amount of hydrochloric acid is 10-20% of the volume of the slurried solution, the adding amount of sodium chlorate is 5-10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 h.
The fixed time in the step 2 is 2-4 h.
In the step 2, the adding amount of the ammonium chloride is 50-100% of the mass of the crude ammonium chloroplatinate.
Heating to 60-90 ℃ in the step 3.
The method has the beneficial effects that the method adopts an aqueous solution chlorination method to remove impurity elements such as gold, palladium, tellurium and the like in the crude ammonium chloroplatinate, and the process is simple and easy to implement.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for purifying crude ammonium chloroplatinate, which is implemented according to the following steps:
step 1, according to the ratio of 5-10: 1, pulping the crude ammonium chloroplatinate by using pure water, heating to 80-90 ℃, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
wherein, the adding amount of the hydrochloric acid is 10-20% of the volume of the slurried solution, the adding amount of the sodium chlorate is 5-10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 h;
step 2, boiling the mixed solution obtained in the step 1 and keeping the boiled mixed solution for 2-4 hours, then adding ammonium chloride, and filtering after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate and filtrate; wherein the adding amount of the ammonium chloride is 50-100% of the mass of the crude ammonium chloroplatinate;
and 3, adjusting the pH value of the filtrate obtained in the step 2 to 8-9, heating to 60-90 ℃, adding hydrazine hydrate for reduction, and recovering gold, palladium and tellurium.
Compared with the existing preparation method, the invention mainly has the following technical advantages: the invention adopts an aqueous solution chlorination method to remove impurity elements such as gold, palladium, tellurium and the like in the crude ammonium chloroplatinate, and the process is simple and easy to implement.
Example 1
Embodiment 1 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
adding 10L of water into 1kg of crude ammonium chloroplatinate for slurrying, heating to 85 ℃, adding 1.2L of industrial hydrochloric acid and 70g of sodium chlorate, keeping the temperature and stirring for 1h, boiling the solution for 2h for chlorine removal, adding 800g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, entering a platinum refining process, adding caustic soda flakes into the filtrate to adjust the pH value to 8, heating to 80 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and bright and no slag exists in a small test, and recovering gold, palladium and tellurium.
Example 2
Embodiment 2 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
1kg of crude ammonium chloroplatinate was slurried by adding 8L of water, the temperature was raised to 88 ℃ and 1.5L of industrial hydrochloric acid and 60g of sodium chlorate were added, and the mixture was stirred for 1.5 hours while maintaining the temperature. The solution was boiled for 3h to drive off chlorine. Adding 900g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, and performing a platinum refining process. Adding caustic soda flakes into the filtrate to adjust the pH value to 8, heating to 70 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and no residue exists in a small test, and recovering gold, palladium and tellurium.
Example 3
Embodiment 3 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
adding 7L of water into 1kg of crude ammonium chloroplatinate for slurrying, heating to 82 ℃, adding 1.8L of industrial hydrochloric acid and 80g of sodium chlorate, keeping the temperature, stirring for 2 hours, and boiling the solution for 4 hours for chlorine removal. Adding 1000g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, performing a platinum refining process, adding caustic soda flakes into the filtrate to adjust the pH value to 8, heating to 65 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and the small test has no slag, and recovering gold, palladium and tellurium.
Example 4
Embodiment 4 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
adding 8L of water into 1kg of crude ammonium chloroplatinate to perform slurrying, heating to 83 ℃, adding 1.2L of industrial hydrochloric acid and 72g of sodium chlorate, keeping the temperature and stirring for 1h, boiling the solution for 2.5h to remove chlorine, adding 800g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, entering a platinum refining process, adding caustic soda flakes into the filtrate to adjust the pH value to 8.5, heating to 80 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and no slag exists in a small test, and recovering gold, palladium and tellurium.
Example 5
Embodiment 5 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
1kg of crude ammonium chloroplatinate was slurried with 9L of water, heated to 88 ℃ and added with 1.5L of industrial hydrochloric acid and 60g of sodium chlorate, the temperature was maintained and the mixture was stirred for 1.5 h. The solution was boiled for 4h to drive off chlorine. Adding 900g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, and performing a platinum refining process. Adding caustic soda flakes into the filtrate to adjust the pH value to 8.9, heating to 77 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and no residue exists in a small test, and recovering gold, palladium and tellurium.
Example 6
Embodiment 6 of the present invention provides a method for purifying crude ammonium chloroplatinate, which is specifically implemented according to the following steps:
1kg of crude ammonium chloroplatinate was slurried by adding 8.5L of water, heated to 90 ℃ and added with 1.8L of industrial hydrochloric acid and 79g of sodium chlorate, the temperature was maintained and the mixture was stirred for 2 hours. The solution was boiled for 3.5h to drive off chlorine. And adding 1000g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, and performing a platinum refining process. Adding caustic soda flakes into the filtrate to adjust the pH value to 9, heating to 65 ℃, adding a proper amount of hydrazine hydrate until the solution is clear and no residue exists in a small test, and recovering gold, palladium and tellurium.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (6)
1. A method for purifying crude ammonium chloroplatinate is characterized by comprising the following steps:
step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
step 2, boiling the mixed solution obtained in the step 1 and keeping the mixed solution for a fixed time, then adding ammonium chloride, and filtering after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate and filtrate;
and 3, adjusting the pH value of the filtrate obtained in the step 2 to 8-9, heating, adding hydrazine hydrate for reduction, and recovering gold, palladium and tellurium.
2. The method as claimed in claim 1, wherein the step 1 of slurrying the crude ammonium chloroplatinate comprises: mixing pure water according to the proportion of 5-10: 1 volume ratio was added to crude ammonium chloroplatinate for slurrying.
3. The method for purifying crude ammonium chloroplatinate as claimed in any one of claims 1 or 2, characterized in that the heating temperature in step 1 is 80-90 ℃, the addition amount of hydrochloric acid is 10-20% of the volume of the solution after slurrying, the addition amount of sodium chlorate is 5-10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 h.
4. The method as claimed in claim 3, wherein the fixed time in step 2 is 2-4 h.
5. The method as claimed in claim 4, wherein the amount of ammonium chloride added in step 2 is 50-100% by mass of the crude ammonium chloroplatinate.
6. The method as claimed in claim 5, wherein the heating in step 3 is carried out to 60-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811140336.2A CN110964905A (en) | 2018-09-28 | 2018-09-28 | Method for purifying crude ammonium chloroplatinate |
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| CN201811140336.2A CN110964905A (en) | 2018-09-28 | 2018-09-28 | Method for purifying crude ammonium chloroplatinate |
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| CN110964905A true CN110964905A (en) | 2020-04-07 |
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| CN201811140336.2A Pending CN110964905A (en) | 2018-09-28 | 2018-09-28 | Method for purifying crude ammonium chloroplatinate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114604911A (en) * | 2022-03-08 | 2022-06-10 | 金川集团股份有限公司 | Method for removing potassium and sodium from ammonium chloroplatinate product |
| CN114717418A (en) * | 2022-02-24 | 2022-07-08 | 阳谷祥光铜业有限公司 | Method for extracting high-purity spongy platinum from platinum waste liquid |
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| GB863517A (en) * | 1958-12-24 | 1961-03-22 | Mond Nickel Co Ltd | Improvements relating to the separation of platinum from other metals |
| JP2003027154A (en) * | 2001-07-18 | 2003-01-29 | Nikko Materials Co Ltd | Method of recovering high-purity platinum and palladium |
| CN102277497A (en) * | 2011-08-05 | 2011-12-14 | 武汉格林美资源循环有限公司 | Method of reclaiming gold, palladium, platinum and silver from waste circuit board |
| CN103014353A (en) * | 2013-01-11 | 2013-04-03 | 成都光明光电股份有限公司 | Method for recovering noble metal platinum |
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| CN106319241A (en) * | 2016-08-29 | 2017-01-11 | 金川集团股份有限公司 | Method for purifying platinum through reduction |
| CN108315564A (en) * | 2017-12-28 | 2018-07-24 | 核工业北京化工冶金研究院 | The method that a kind of molten carrier recycles platinum from aluminium-based catalyst |
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2018
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Patent Citations (7)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114717418A (en) * | 2022-02-24 | 2022-07-08 | 阳谷祥光铜业有限公司 | Method for extracting high-purity spongy platinum from platinum waste liquid |
| CN114717418B (en) * | 2022-02-24 | 2024-02-23 | 阳谷祥光铜业有限公司 | Method for extracting high-purity sponge platinum from platinum waste liquid |
| CN114604911A (en) * | 2022-03-08 | 2022-06-10 | 金川集团股份有限公司 | Method for removing potassium and sodium from ammonium chloroplatinate product |
| CN114604911B (en) * | 2022-03-08 | 2023-09-22 | 金川集团股份有限公司 | Method for removing potassium and sodium from ammonium chloroplatinate product |
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