CN114717428A - Method for extracting platinum from TBP extraction liquid - Google Patents
Method for extracting platinum from TBP extraction liquid Download PDFInfo
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- CN114717428A CN114717428A CN202210437482.1A CN202210437482A CN114717428A CN 114717428 A CN114717428 A CN 114717428A CN 202210437482 A CN202210437482 A CN 202210437482A CN 114717428 A CN114717428 A CN 114717428A
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- platinum
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 63
- 238000000605 extraction Methods 0.000 title claims abstract description 45
- 239000007788 liquid Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 229910000629 Rh alloy Inorganic materials 0.000 claims abstract description 15
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000284 extract Substances 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 13
- 239000012071 phase Substances 0.000 claims description 12
- 239000012074 organic phase Substances 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- -1 ammonium chloride platinum Chemical compound 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000005191 phase separation Methods 0.000 abstract description 4
- 239000010970 precious metal Substances 0.000 abstract description 4
- 229910002651 NO3 Inorganic materials 0.000 abstract description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 3
- 238000009854 hydrometallurgy Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 239000010948 rhodium Substances 0.000 description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 6
- 235000002639 sodium chloride Nutrition 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910052703 rhodium Inorganic materials 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910000923 precious metal alloy Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
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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
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting platinum from TBP extraction liquid, which adopts NaCl and NaHCO3、Na2CO3The mixed stripping agent is used for stripping, the stripping efficiency of platinum in the platinum-rhodium alloy extraction liquid is high, the phase separation is fast, the operation is convenient, the obtained stripping liquid can be linked with the platinum refining process without nitrate removal treatment, the stripping rate is more than 99% when the method is used for stripping platinum, compared with the stripping process in the prior art, the stripping efficiency is obviously improved, the problem of platinum waste in the extraction liquid is solved, the direct yield of platinum in the platinum-rhodium alloy is improved, and the treatment process is shortened. The invention can be applied to the processing technology for extracting platinum from platinum-containing extract liquor in the precious metal hydrometallurgy process.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, and particularly relates to a method for extracting platinum from TBP extraction liquid.
Background
Nowadays, the recycling of precious metal secondary resources becomes an industry hot, and researches and applications for extracting and recycling precious metals from automobile exhaust spent catalysts, petrochemical spent catalysts, fine chemical spent catalysts and precious metal alloy waste materials are increasing. The platinum-rhodium-containing alloy material is an important recovered raw material, and currently, tributyl phosphate is used for extraction and separation of platinum and rhodium in the treatment of platinum-rhodium alloy, but nitric acid or water back extraction is often used in the traditional tributyl phosphate extraction. The stripping solution produced by the nitric acid stripping is usually subjected to nitrate removal treatment, and the platinum can be refined after the nitro in the stripping solution is removed, and the nitric acid is a strong acid and has high use risk. And the water back extraction has the defects of slow phase separation, low back extraction rate and the like. Therefore, it is urgently needed to develop a stripping agent with high stripping efficiency and simple and easy operation to replace the traditional nitric acid or water stripping.
Disclosure of Invention
The invention aims to solve the defects in the back extraction of platinum in the existing platinum-rhodium back extraction solution, and provides a method for extracting platinum from TBP (tert-butyl-p) extraction liquid.
In order to achieve the purpose, the invention adopts the following technical scheme:
(1) mixing a platinum-rhodium alloy solution and tributyl phosphate according to the ratio of O: A =1:1, and then extracting in a glass extraction barrel, wherein the stirring time is 20-30 min during single-stage extraction, and obtaining a platinum-carrying organic phase after extraction;
(2) NaCl and NaHCO3、Na2CO3Mixing the raw materials according to the mass ratio of 1: 0.5-1 to prepare a 30% solution used as a stripping agent;
(3) mixing the platinum-loaded organic phase and the stripping agent prepared in the step (2) according to the ratio of O: A =1:1, mixing in a glass extraction barrel, stirring for 5-10 min, standing, phase-splitting and separating an oil phase and a water phase to obtain platinum stripping liquid;
(4) adjusting the pH of the platinum back extraction solution obtained in the step (3) to be 8-11, filtering, and returning acid to be 0.5-1;
(5) and (4) carrying out ammonium chloride platinum precipitation on the solution obtained in the step (4) to obtain ammonium chloroplatinate, and then calcining and reducing to obtain a platinum product.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts NaCl and NaHCO3、Na2CO3The back extraction is carried out on the mixture, the back extraction efficiency of the platinum in the platinum rhodium alloy extract liquid is high, the phase separation is fast, the operation is convenient, and the obtained back extraction liquid can be linked with the platinum refining process without nitrate removing treatment. When the method is used for back extraction of platinum, the back extraction rate is more than 99%, compared with the back extraction process in the prior art, the back extraction efficiency is obviously improved, the problem of waste of platinum in the extraction liquid is solved, the direct yield of platinum in the platinum-rhodium alloy is improved, and the treatment process is shortened. The invention can be applied to the processing technology for extracting platinum from platinum-containing extract liquor in the precious metal hydrometallurgy process.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are included as part of the present invention and are intended to provide further details and to demonstrate the effectiveness of the invention.
Example 1
The concentration of Pt and Rh in the platinum-rhodium alloy extraction liquid is 25g/L, the concentration of Rh is 0.07g/L, 100ml of the platinum-rhodium alloy extraction liquid is placed in a beaker, 100ml of tributyl phosphate is added, stirring is carried out for 25min, and the mixture is poured into a separating funnel after stirring, stands and carries out phase splitting to obtain a platinum-loaded organic phase; NaCl and NaHCO3、Na2CO3Mixing the raw materials according to the mass ratio of 1:0.5:0.5 to prepare a 30% solution used as a back extractant; mixing the platinum-loaded organic phase and the prepared stripping agent according to the ratio of O: A =1:1, mixing in a glass extraction barrel, stirring for 5min, standing, phase-separating and separating an oil phase and a water phase to obtain a platinum stripping solution, wherein the concentration of Pt in the stripping solution (V =98 ml) is 25.3g/L after sample feeding detection, and the stripping rate of platinum is 99.1%; adjusting the pH of the platinum stripping solution to be =8, filtering, and returning acid to be at the pH of = 0.5; and (3) precipitating platinum in the obtained solution by ammonium chloride to obtain ammonium chloroplatinate, then calcining and reducing to obtain a platinum product, and analyzing to obtain the final platinum product with the mass of 99.99%.
Example 2
The concentration of Pt and Rh in the platinum-rhodium alloy extraction liquid is 26.3g/L, the concentration of Rh is 0.09g/L, 50L of the platinum-rhodium alloy extraction liquid is placed in a glass extraction barrel, 50L of tributyl phosphate is added, stirring is carried out for 25min, the mixture is poured into a separating funnel after stirring, standing is carried out, and a platinum-carrying organic phase is obtained after phase splitting is carried out; NaCl and NaHCO3、Na2CO3Mixing the raw materials according to the mass ratio of 1:0.5:0.5 to prepare a 30% solution used as a back extractant; mixing the platinum-loaded organic phase and the prepared stripping agent according to the ratio of O: A =1:1, mixing in a glass extraction barrel, stirring for 5min, standing, phase-separating and separating an oil phase and a water phase to obtain a platinum stripping solution, wherein the concentration of Pt in the stripping solution (V =50.5L) after sample sending detection is 25.9g/L, and the stripping rate of platinum is 99.4%; adjusting the pH of the platinum stripping solution to be 10 =10, filtering, and returning acid to be 1 = pH; and (3) precipitating platinum in the obtained solution by ammonium chloride to obtain ammonium chloroplatinate, then calcining and reducing to obtain a platinum product, and analyzing to obtain the final platinum product with the mass of 99.99%.
Example 3
Putting 10L of platinum-rhodium alloy extract liquor into a beaker, adding 10L of tributyl phosphate, stirring for 25min, pouring the mixture into a glass extraction barrel after stirring, standing, and carrying out phase separation to obtain a platinum-loaded organic phase, wherein the concentration of Pt and Rh in the platinum-rhodium alloy extract liquor is 15g/L, and the concentration of Rh in the platinum-rhodium alloy extract liquor is 1.64 g/L; mixing NaCl, NaHCO3 and Na2CO3 in a mass ratio of 1:0.8:1 to prepare a 30% solution serving as a back extractant; mixing the platinum-loaded organic phase and the prepared stripping agent according to the ratio of O: A =1:1, mixing in a glass extraction barrel, stirring for 5min, standing, phase-separating and separating an oil phase and a water phase to obtain a platinum stripping solution, wherein the concentration of Pt in the stripping solution (V = 14.5L) after sample sending detection is 10.26g/L, and the stripping rate of platinum is 99.2%; adjusting the pH of the platinum stripping solution to be =11, filtering, and returning acid to be at the pH of = 0.8; and (3) precipitating platinum in the obtained solution by ammonium chloride to obtain ammonium chloroplatinate, then calcining and reducing to obtain a platinum product, and analyzing to obtain the final platinum product with the mass of 99.99%.
Claims (5)
1. A method for extracting platinum from TBP extraction liquid is characterized by comprising the following steps:
(1) mixing the platinum-rhodium alloy solution and tributyl phosphate according to the ratio of O: A =1:1, then extracting in a glass extraction barrel, wherein the stirring time is 20-30 min during single-stage extraction, and obtaining a platinum-loaded organic phase after extraction;
(2) NaCl and NaHCO3、Na2CO3Mixing the raw materials according to the mass ratio of 1: 0.5-1 to prepare a 30% solution used as a stripping agent;
(3) putting the platinum-loaded organic phase and the stripping agent prepared in the step (2) into a glass extraction barrel according to the ratio of O: A =1:1, mixing, stirring for 5-10 min, standing, phase-separating and separating an oil phase and a water phase to obtain platinum stripping liquid;
(4) adjusting the pH of the platinum back extraction solution obtained in the step (3) to be 8-11, filtering, and returning acid to be 0.5-1;
(5) and (4) carrying out ammonium chloride platinum precipitation on the solution obtained in the step (4) to obtain ammonium chloroplatinate, and then calcining and reducing to obtain a platinum product.
2. The method for extracting platinum from TBP extraction liquid as claimed in claim 1, wherein the ratio of the platinum-rhodium alloy solution to tributyl phosphate in step (1) is 1:1, and the extraction stirring time is 20-30 min.
3. The method for extracting platinum from TBP extract as claimed in claim 1, wherein NaCl and NaHCO are used in step (2)3、Na2CO3The mixing ratio of (1: 0.5) - (1), and after mixing, preparing a 30% solution to be used as a stripping agent.
4. The method for extracting platinum from TBP extraction liquid according to claim 1, wherein the ratio of the platinum-carrying organic phase in the step (3) to the stripping agent prepared in the step (2) is 1:1, and the stirring time is 5-10 min.
5. The method for extracting platinum from TBP extract as claimed in claim 1, wherein in step (4), the pH of the platinum strip solution in step (3) is adjusted to be 8-11, and the solution is filtered and then returned to acid to be pH = 0.5-1.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2520275A1 (en) * | 2004-09-21 | 2006-03-21 | North-West University | Recovery of one or more platinum group metals from a source of one or more platinum group metals |
CN101260469A (en) * | 2008-04-21 | 2008-09-10 | 上海大学 | Method for reclaiming and purifying platinum and rhodium from waste material containing platinum and rhodium |
EP2169085A1 (en) * | 2008-09-29 | 2010-03-31 | Nippon Mining & Metals Co., Ltd. | Method of separating rhodium from platinum and/or palladium |
CN102417981A (en) * | 2011-11-22 | 2012-04-18 | 中国科学院过程工程研究所 | Method for extracting and separating platinum, palladium and rhodium by using ionic liquid-based three-liquid phase system |
JP2014133227A (en) * | 2012-12-11 | 2014-07-24 | Tosoh Corp | Platinum separating agents and platinum ion separating methods |
CN107574314A (en) * | 2017-08-25 | 2018-01-12 | 金川集团股份有限公司 | A kind of method of refined platinum in strip liquor from platinum |
-
2022
- 2022-04-25 CN CN202210437482.1A patent/CN114717428A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2520275A1 (en) * | 2004-09-21 | 2006-03-21 | North-West University | Recovery of one or more platinum group metals from a source of one or more platinum group metals |
CN101260469A (en) * | 2008-04-21 | 2008-09-10 | 上海大学 | Method for reclaiming and purifying platinum and rhodium from waste material containing platinum and rhodium |
EP2169085A1 (en) * | 2008-09-29 | 2010-03-31 | Nippon Mining & Metals Co., Ltd. | Method of separating rhodium from platinum and/or palladium |
CN102417981A (en) * | 2011-11-22 | 2012-04-18 | 中国科学院过程工程研究所 | Method for extracting and separating platinum, palladium and rhodium by using ionic liquid-based three-liquid phase system |
JP2014133227A (en) * | 2012-12-11 | 2014-07-24 | Tosoh Corp | Platinum separating agents and platinum ion separating methods |
CN107574314A (en) * | 2017-08-25 | 2018-01-12 | 金川集团股份有限公司 | A kind of method of refined platinum in strip liquor from platinum |
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Application publication date: 20220708 |