CN115418490A - Method for recovering platinum and palladium from waste liquid containing trace precious metals - Google Patents
Method for recovering platinum and palladium from waste liquid containing trace precious metals Download PDFInfo
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 137
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 69
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 66
- 239000007788 liquid Substances 0.000 title claims abstract description 54
- 239000002699 waste material Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000010970 precious metal Substances 0.000 title claims abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000012074 organic phase Substances 0.000 claims abstract description 57
- 238000000605 extraction Methods 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 36
- 229910052742 iron Inorganic materials 0.000 claims abstract description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004448 titration Methods 0.000 claims abstract description 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 229910000510 noble metal Inorganic materials 0.000 claims description 14
- YZHUMGUJCQRKBT-UHFFFAOYSA-M sodium chlorate Chemical class [Na+].[O-]Cl(=O)=O YZHUMGUJCQRKBT-UHFFFAOYSA-M 0.000 claims description 5
- 238000010586 diagram Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims 5
- CMHKGULXIWIGBU-UHFFFAOYSA-N [Fe].[Pt] Chemical compound [Fe].[Pt] CMHKGULXIWIGBU-UHFFFAOYSA-N 0.000 claims 1
- 239000008346 aqueous phase Substances 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- -1 Platinum group metals Chemical class 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000005843 Thiram Substances 0.000 description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 2
- 229960002447 thiram Drugs 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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Classifications
-
- 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
-
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/30—Oximes
-
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
-
- 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
Abstract
The invention discloses a method for recovering platinum and palladium from waste liquid containing trace precious metals, which comprises the following steps: adjusting the potential of the waste liquid, and determining the acidity of the solution by a NaOH titration method to obtain a solution to be extracted; extracting the adjusted waste liquid by using a mixed liquid of an extracting agent LIX84-I and Solveso150 to obtain an organic phase carrying palladium and iron; washing the organic phase with dilute hydrochloric acid to obtain a palladium-loaded organic phase; carrying out back extraction on the palladium-loaded organic phase by using concentrated hydrochloric acid to obtain a palladium-containing solution; extracting raffinate by using the mixture of tri-n-octylamine and tributyl phosphate to obtain a platinum and iron-loaded organic phase; washing the loaded organic phase by using dilute hydrochloric acid to obtain a platinum-loaded organic phase; and (3) carrying out back extraction on the platinum-carrying organic phase by using thiourea to obtain a platinum-containing solution. The method has simple process, the extractant has higher selectivity to platinum and palladium, and the treated waste liquid can be directly merged into a conventional sewage treatment plant for treatment, thereby realizing the reclamation of the waste water and effectively solving the problem of environmental protection.
Description
Technical Field
The invention relates to the field of wastewater resource utilization, in particular to a comprehensive recovery method of platinum and palladium in precious metal refining wastewater.
Background
Platinum group metals have the advantages of excellent corrosion resistance, strong high-temperature oxidation resistance, good catalytic activity and the like, and are often used in the fields of catalysis, microelectronic materials, medicines, energy sources, jewelry and the like, however, because the global platinum group metals have small reserves and low ore grades, the separation and purification of the platinum group metals are difficult, and the price of the platinum group metals is high. The content of noble metals in waste such as waste electrons and waste catalysts is 80 times higher than that in ore deposits, so the secondary resource of rare noble metals becomes an important source of platinum group metals.
The waste liquid produced by the precious metal refinery contains a trace amount of platinum-palladium precious metals, and the direct discharge can cause great economic loss and is not favorable for environmental protection requirements. At present, methods for treating wastewater containing trace noble metals in noble metal refineries mainly comprise a metal replacement method, a precipitation method, an incineration method, an extraction method, an adsorption method, an electrolysis method, a redox method and the like. The metal replacement method can enrich and recover precious metals, and simultaneously, the recovery slag is polluted by various reagents, so that the precious metal refining process is 2-3 times long, and the refining times are 3-4 times more. Although resin adsorption has the advantages of simple operation, small labor amount and the like, the resin is expensive and has small treatment capacity, so that the condition of industrial application is not met.
The precipitation method is to adjust the properties of wastewater containing a trace amount of precious metals and then to recover the precious metals by selecting the precipitation method, for example, the method disclosed in the chinese patent: a method for treating a waste liquid containing a noble metal of the platinum group, 202111089525.3, which comprises adjusting the waste liquid containing the noble metal of the platinum group to be acidic using hydrochloric acid; then, sodium thiram, thiram and platinum group metal chlorine complex anion are added into the waste liquid to carry out coordination reaction, precipitate is generated, and thus the platinum group noble metal is separated from the waste liquid. However, the precipitation method has high requirements on the properties of the waste liquid, the metal cannot be completely recovered due to improper treatment, and the precipitation method needs multiple times of precipitation to completely recover the metal. And because the concentration of the metal in the wastewater is low, the concentration is needed to be carried out on the metal which is difficult to directly treat and recover by selecting the traditional precipitation method and the traditional replacement method, the energy consumption is high, and the process cost is increased. Therefore, it is necessary to develop a method for treating wastewater with high recovery rate, short recovery process and simple operation.
Disclosure of Invention
In order to solve the problems of incomplete precious metal precipitation and low recovery rate of waste water generated in the precious metal refining process by adopting methods such as metal replacement, chemical precipitation or resin adsorption and the like, the invention provides the method for recovering the platinum and the palladium from the waste liquid containing trace precious metals, which has the advantages of simple operation, short recovery flow and high recovery rate.
The invention is realized by the following technical scheme: a method for recovering platinum and palladium from waste liquid containing trace precious metals comprises the following steps:
(1) According to a potential pH diagram, adjusting the potential of the waste liquid to be more than 1000mv, controlling the metal valence state of the solution, and adjusting the acidity of the solution to be 0.1Mol/L by a NaOH titration method to obtain a solution to be extracted;
(2) Extracting the solution to be extracted of step (1) by adding an extractant A which is a mixture of 2-5% LIX84-I and 95-98% Solvesso 150%;
(3) Washing the palladium-carrying and part of iron-carrying organic phase obtained in the step (2) for three times by using 1-2 mol/L diluted hydrochloric acid, and allowing iron to enter a water phase to obtain a palladium-carrying organic phase;
(4) Carrying out back extraction on the palladium-loaded organic phase by using 10mol/L dilute hydrochloric acid, wherein the volume ratio of the water phase to the organic phase is 1:3, palladium enters the water phase to obtain a palladium-containing solution, and the back extraction rate of the palladium reaches 99.47-99.9%;
(5) Adding an extracting agent B into the raffinate extracted in the step (2), wherein the extracting agent B is a mixed phase of 5-95% of tri-n-octylamine and 95-5% of tributyl phosphate, and extracting to obtain a platinum and iron-loaded organic phase;
(6) Washing the platinum-and-iron-loaded organic phase obtained in the step (5) with dilute hydrochloric acid with the concentration of 0.0001-0.001 mol/L, and allowing iron to enter a water phase to obtain a platinum-loaded organic phase;
(7) And (4) performing back extraction on the platinum-loaded organic phase in the step (6), wherein platinum enters the water phase to obtain a platinum-containing solution, and the back extraction rate of the platinum reaches 99.6-99.9%.
Preferably, the step (1) adopts saturated sodium chlorate to adjust the potential of the waste liquid.
Preferably, the extraction time in the step (2) is 5min, and the volume ratio of the extracting agent A to the waste liquid is 1:1-2:1.
Preferably, the stripping time of the step (4) is 5min, and the number of stripping stages is three.
Preferably, the extraction time in the step (5) is 5min, and the volume ratio of the extracting agent B to the waste liquid is 1:1-3: 1.
preferably, the stripping agent in the step (7) is 0.5mol/L thiourea, the stripping time is 5min, and the number of stripping stages is three.
Compared with the prior art, the invention has the following advantages: (1) compared with a precipitation method or a displacement method, the method can extract the platinum and the palladium in the low-concentration precious metal waste liquid by only one-time extraction and three-stage back extraction, and has the advantages of shorter process flow and simpler operation. The method can efficiently realize the separation and recovery of noble metals, has the recovery rate of platinum and palladium of more than 99.9 percent, and is green and environment-friendly.
(2) The platinum and palladium solution obtained by the method has extremely low base metal content, the purity of the platinum and palladium solution is over 99 percent, and the platinum and palladium solution can be directly linked to refining.
(3) The invention has good platinum-palladium separation effect, and impurities are hardly extracted and the extraction phase separation is good when extracting palladium and platinum. The primary extraction rate E (%) of palladium is more than or equal to 99.9%, the primary extraction rate E (%) of platinum is more than or equal to 99.5%, the back extraction solution is subjected to traditional refining processes of concentration, reduction calcination and the like to obtain palladium powder and platinum powder with the purity of 99.99%, and the back extracted organic phase is washed by deionized water, balanced by hydrochloric acid, and still good in separation effect after repeated extraction and use.
Drawings
FIG. 1 is a graph of the effect of LIX84-1 volume fraction on palladium extraction.
FIG. 2 is a diagram showing the effect of extracting palladium by comparing the volume ratio of the extractant A to the waste liquid.
FIG. 3 is a graph of the effect of volume fraction of tri-n-octylamine in extractant B on platinum extraction.
FIG. 4 is a graph of the effect of extractant B on the volume ratio of raffinate palladium on platinum extraction.
FIG. 5 shows an infrared spectrum of the organic phase.
Detailed Description
Experimental example 1: a method for recovering platinum and palladium from waste liquid containing trace precious metals comprises the following steps:
(1) Taking 500ml of waste liquid, adding saturated sodium chlorate to adjust the potential of the waste liquid to be more than 1000mv according to a potential pH diagram, controlling the metal valence state of the solution, and adjusting the acidity of the solution to be 0.1Mol/L by a NaOH titration method to obtain a solution to be extracted;
(2) Adding an extracting agent A into the liquid to be extracted in the step (1) for extraction for 5min, wherein the extracting agent A is a mixed liquid which is formed by 2 percent of LIX84-I and 98 percent of Solvesso150, and the volume ratio of the extracting agent to the waste liquid is 1:1, palladium and a small amount of iron enter an extracting agent A to obtain an organic phase carrying palladium and part of iron, and platinum is left in raffinate;
(3) Washing the palladium-loaded and part of iron-loaded organic phase obtained in the step (2) for three times by using 1mol/L hydrochloric acid, and allowing impurity iron to enter a water phase to obtain a palladium-loaded organic phase;
(4) Carrying out three-stage back extraction on the palladium-loaded organic phase by using 10mol/L hydrochloric acid, wherein each time is 5min, the volume ratio of the water phase to the organic phase is 1:3, palladium enters the water phase to obtain a palladium-containing solution, and the back extraction rate of the palladium reaches 99.9%;
(5) Adding an extracting agent B into the raffinate extracted in the step (2), wherein the extracting agent B is a mixed phase of 5% of tri-n-octylamine and 95% of tributyl phosphate, the volume ratio of the extracting agent B to the waste liquid is 1:1, and platinum and iron enter an organic phase to obtain a platinum and iron-loaded organic phase;
(6) Washing the platinum-and-iron-loaded organic phase obtained in the step (5) with dilute hydrochloric acid with the concentration of 0.0001mol/L for 5min, and allowing iron to enter the water phase to obtain a platinum-loaded organic phase;
the washing conditions are given in the following table:
(7) And (3) adding 0.5mol/L thiourea into the platinum-loaded organic phase obtained in the step (6) to perform three-stage back extraction, wherein the back extraction time is 5min, platinum enters a water phase to obtain a platinum-containing solution, and the back extraction rate of the platinum reaches 99.9%.
Example 2: a method for recovering platinum and palladium from waste liquid containing trace precious metals comprises the following steps:
(1) Adding saturated sodium chlorate into 1000ml of waste liquid to adjust the potential of the waste liquid to be more than 1000mv, controlling the metal valence state of the solution, and adjusting the acidity of the solution to be 0.1Mol/L by a NaOH titration method to obtain a solution to be extracted;
(2) Adding an extracting agent A into the liquid to be extracted in the step (1) for extraction for 5min, wherein the extracting agent A is a mixed liquid which is formed by 5 percent of LIX84-I and 95 percent of Solvesso150, and the volume ratio of the extracting agent to the waste liquid is 2:1, palladium and a small amount of iron enter an extracting agent A to obtain an organic phase carrying palladium and part of iron, and platinum is left in raffinate;
(3) Washing the palladium-loaded and part of iron-loaded organic phase obtained in the step (2) for three times by using 2mol/L hydrochloric acid, and allowing impurity iron to enter a water phase to obtain a palladium-loaded organic phase;
(4) Carrying out three-stage back extraction on the palladium-loaded organic phase by using 10mol/L hydrochloric acid, wherein each time is 5min, the volume ratio of the water phase to the organic phase is 1:3, palladium enters the water phase to obtain a palladium-containing solution, and the back extraction rate of the palladium reaches 99.47%;
(5) Adding an extracting agent B into the raffinate extracted in the step (2), wherein the extracting agent B is a mixed phase of 5% of tri-n-octylamine and 95% of tributyl phosphate, the volume ratio of the extracting agent B to the waste liquid is 2:1, and platinum and iron enter an organic phase to obtain a platinum and iron-loaded organic phase;
(6) Washing the platinum-and-iron-loaded organic phase obtained in the step (5) with dilute hydrochloric acid with the concentration of 0.001mol/L for 5min, and allowing iron to enter the water phase to obtain a platinum-loaded organic phase;
the wash conditions are given in the following table:
(7) And (3) adding 0.5mol/L thiourea into the platinum-loaded organic phase obtained in the step (6) to perform three-stage back extraction, wherein the back extraction time is 5min, platinum enters a water phase to obtain a platinum-containing solution, and the back extraction rate of the platinum reaches 99.8%.
Example 3: a method for recovering platinum and palladium from waste liquid containing trace precious metals comprises the following steps:
(1) Taking 800ml of waste liquid, adding saturated sodium chlorate to adjust the potential of the waste liquid to be more than 1000mv, controlling the metal valence state of the solution, and adjusting the acidity of the solution to be 0.1Mol/L by a NaOH titration method to obtain a solution to be extracted;
(2) Adding an extracting agent A into the liquid to be extracted in the step (1) for extraction for 5min, wherein the extracting agent A is a mixed liquid which is formed by 4 percent of LIX84-I and 96 percent of Solvesso150, and the volume ratio of the extracting agent to the waste liquid is 1:1, palladium and a small amount of iron enter an extracting agent A to obtain an organic phase carrying palladium and part of iron, and platinum is left in raffinate;
(3) Washing the palladium-loaded and part of iron-loaded organic phase obtained in the step (2) for three times by using 1mol/L hydrochloric acid, and allowing impurity iron to enter a water phase to obtain a palladium-loaded organic phase;
(4) Carrying out three-stage back extraction on the palladium-loaded organic phase by using 10mol/L hydrochloric acid, wherein each time is 5min, the volume ratio of the water phase to the organic phase is 1:3, palladium enters the water phase to obtain a palladium-containing solution, and the back extraction rate of the palladium reaches 99.8%;
(5) Adding an extracting agent B into the raffinate extracted in the step (2), wherein the extracting agent B is a mixed phase of 60% of tri-n-octylamine and 40% of tributyl phosphate, the volume ratio of the extracting agent B to the waste liquid is 3:1, and platinum and iron enter an organic phase to obtain a platinum and iron-loaded organic phase;
(6) Washing the platinum-and-iron-loaded organic phase obtained in the step (5) with dilute hydrochloric acid with the concentration of 0.001mol/L for 5min, and allowing iron to enter the water phase to obtain a platinum-loaded organic phase;
the wash conditions are given in the following table:
(7) And (3) adding 0.5mol/L thiourea into the platinum-loaded organic phase obtained in the step (6) to perform three-stage back extraction, wherein the back extraction time is 5min, platinum enters a water phase to obtain a platinum-containing solution, and the back extraction rate of the platinum reaches 99.78%.
Claims (7)
1. A method for recovering platinum and palladium from waste liquid containing trace precious metals is characterized by comprising the following steps:
(1) According to a potential pH diagram, adjusting the potential of the waste liquid to be more than 1000mv, controlling the metal valence state of the solution, and adjusting the acidity of the solution to be 0.1Mol/L by a NaOH titration method to obtain a solution to be extracted;
(2) Adding an extracting agent A into the liquid to be extracted in the step (1) for extraction, wherein the extracting agent A is a mixed solution formed by 2-5% of LIX84-I and 95-98% of Solvesso150, palladium and a small amount of iron enter the extracting agent A to obtain an organic phase loaded with palladium and part of iron, and platinum is remained in raffinate;
(3) Washing the palladium-loaded and part of iron-loaded organic phase obtained in the step (2) for three times by using 1-2 mol/L diluted hydrochloric acid to obtain a palladium-loaded organic phase;
(4) And (3) carrying out back extraction on the palladium-loaded organic phase by using 10mol/L diluted hydrochloric acid, wherein the volume ratio of the aqueous phase to the organic phase is 1:3, allowing palladium to enter a water phase to obtain a palladium-containing solution, wherein the back extraction rate of the palladium reaches 99.47-99.9%;
(5) Adding an extracting agent B into the raffinate extracted in the step (2), wherein the extracting agent B is a mixed phase of 5-95% of tri-n-octylamine and 95-5% of tributyl phosphate, and extracting to obtain a platinum and iron-loaded organic phase;
(6) Washing the platinum-and iron-loaded organic phase obtained in the step (5) with dilute hydrochloric acid with the concentration of 0.0001-0.001 mol/L, and allowing iron to enter a water phase to obtain a platinum-loaded organic phase;
(7) And (4) performing back extraction on the platinum-loaded organic phase in the step (6), wherein platinum enters the water phase to obtain a platinum-containing solution, and the back extraction rate of the platinum reaches 99.6-99.9%.
2. The method for recovering platinum and palladium from waste liquid containing trace noble metals as claimed in claim 1, wherein the step (1) adopts saturated sodium chlorate to adjust the potential of the waste liquid.
3. The method for recovering platinum and palladium from waste liquid containing trace noble metals as claimed in claim 1, wherein the extraction time in the step (2) is 5min, and the volume ratio of the extracting agent A to the waste liquid is 1:1-2:1.
4. The method for recovering platinum and palladium from a waste liquid containing trace noble metals according to any one of claims 1 to 3, wherein the stripping time in the step (4) is 5min, and the number of stripping stages is three.
5. The method for recovering platinum and palladium from waste liquid containing trace noble metals as claimed in any one of claims 1 to 3, wherein the extraction time in the step (5) is 5min, and the volume ratio of the extracting agent B to the waste liquid is 1:1-3:1.
6. The method for recovering platinum and palladium from waste liquid containing trace noble metals according to claim 4, wherein the stripping agent in the step (7) is 0.5mol/L thiourea, the stripping time is 5min, and the number of stripping stages is three.
7. The method for recovering platinum and palladium from waste liquid containing trace noble metals according to claim 5, wherein the stripping agent in the step (7) is 0.5mol/L thiourea, the stripping time is 5min, and the number of stripping stages is three.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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