CN105441693A - Method for separating and extracting platinum group metals - Google Patents
Method for separating and extracting platinum group metals Download PDFInfo
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- CN105441693A CN105441693A CN201510797547.3A CN201510797547A CN105441693A CN 105441693 A CN105441693 A CN 105441693A CN 201510797547 A CN201510797547 A CN 201510797547A CN 105441693 A CN105441693 A CN 105441693A
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- platinum
- palladium
- ammonium
- ammonium chloroplatinate
- extraction
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 21
- 239000002184 metal Substances 0.000 title claims abstract description 21
- -1 platinum group metals Chemical class 0.000 title claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 139
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 136
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 68
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 67
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 54
- 238000000605 extraction Methods 0.000 claims abstract description 43
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000012074 organic phase Substances 0.000 claims abstract description 17
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 15
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 30
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 26
- 239000000460 chlorine Substances 0.000 claims description 26
- 229910052801 chlorine Inorganic materials 0.000 claims description 26
- 239000006210 lotion Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 18
- 238000010792 warming Methods 0.000 claims description 14
- 239000000284 extract Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 150000003863 ammonium salts Chemical class 0.000 claims description 6
- 238000007689 inspection Methods 0.000 claims description 6
- KIDPOJWGQRZHFM-UHFFFAOYSA-N platinum;hydrate Chemical compound O.[Pt] KIDPOJWGQRZHFM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- 239000010970 precious metal Substances 0.000 abstract description 3
- LIAWOTKNAVAKCX-UHFFFAOYSA-N hydrazine;dihydrochloride Chemical compound Cl.Cl.NN LIAWOTKNAVAKCX-UHFFFAOYSA-N 0.000 abstract 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 238000011946 reduction process Methods 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 241000628997 Flos Species 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
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
- C22B11/06—Chloridising
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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)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for separating and extracting platinum group metals. The method comprises the steps that the palladium concentration of feed liquid containing the platinum group metals is controlled to be 1.5-5.5g/L, the electric potential of the feed liquid is controlled to be 850-950mv, palladium is extracted by means of S201 organic phases, and palladium is extracted from the palladium-loaded organic phases through the following process. Ammonium chloride is added into palladium extraction raffinate to deposit platinum, obtained ammonium chloroplatinate is subjected to reduction and dissolution by being added with hydrazine dihydrochloride solution and is heated to 90-95 DEG C, and chlorine gas is introduced; after the obtained ammonium chloroplatinate is repeatedly subjected to the hydrazine dihydrochloride reduction process for 2-3 times, and high-purity platinum black can be obtained by reducing the ammonium chloroplatinate through the hydrazine dihydrochloride according to the mass ratio of 1:1. Compared with the prior art, the method has the advantages that the process is simple, the precious metal separation efficiency is high, generation of a larger amount of ammonia-contained waste gas is avoided in the process of reducing ammonium chloroplatinate through hydrazine hydrate, and no nitrogen oxide pollution is produced.
Description
Technical field
The invention belongs to metal separation technical field, the method for separation and Extraction platinum in liquid more than the extraction palladium being specifically related to a kind of platinum group metallic solution, slag or secondary resource.
Background technology
At present, adopt the refinery practice of multiplex aqua regia dissolution-ammonium chloride repeated precipitation in platinum refining process, the method is the refinery practice of the most ancient classics, and catch up with nitre, catch up with in sour process, part platinum can be dispersed in flue gas with flue gas; And in 1% dissolving with hydrochloric acid insoluble slag, platinum content is higher, causes the dispersion of platinum.Catch up with acid, catch up with nitre process operation loaded down with trivial details, the production cycle is long, and cost is high.Aqua regia dissolution and hydrochloric acid catch up with the oxynitride produced in nitre process, not only have a strong impact on the operating environment of post worker, and the more difficult absorption process of oxynitride, cause environmental protection pressure large.
The separation and Extraction of platinum palladium also can adopt extraction process, i.e. the first S of platinum group metal feed liquid
201extraction of palladium, N
235extraction platinum, then extracts platinum palladium from extracted organic phase.Due to the existence of base metal and other impurity, there is line clogging in operation, the third phase of the floss that becomes turbid, aqueous phase carry organic equal phenomenon secretly often to cause continuous print to extract, and causes extraction efficiency to reduce.In addition, platinum strip liquor still needs to be incorporated to aqua regia dissolution-ammonium chloride and sinks platinum group system and carry out refining treatment, can output qualified product.
Summary of the invention
Technical problem to be solved by this invention is the method providing separation and Extraction platinum liquid more than a kind of extraction palladium from platinum group metallic solution, slag or secondary resource for shortcoming of the prior art, and the present invention has that flow process is simple, precious metal separation efficiency is high, avoid a large amount of ammonia-contaminated gas produced in hydrazine hydrate reduction ammonium chloroplatinate process, the advantage not producing nitrogen oxides pollution.
Following technical scheme is adopted for solving technical problem of the present invention:
A method for separation and Extraction platinum metals, comprises following technique: controlling palladium concentration in platinum group metal feed liquid is 1.5-5.5g/L, and platinum concentration is 10-15g/L, and current potential is 850 ~ 950mv, uses S
201organic phase extraction palladium, carry palladium organic phase and then extract palladium through subsequent technique, more than extraction palladium, liquid adds ammonium chloride and sinks platinum, the ammonium chloroplatinate obtained dissolves by adding hydrazine hydrochloride solution reduction, and be warming up to 90-95 DEG C, logical chlorine catches up with chlorine, after the ammonium chloroplatinate of gained repeats hydrazine hydrochloride reducing process 2-3 time, just can obtain high purity platinum black by the reduction of 1:1 hydrazine hydrochloride in mass ratio ammonium chloroplatinate, after vacuum-drying, obtain spongy platinum product.
The method of above-mentioned separation and Extraction platinum metals, comprises the following steps:
In step a, control platinum group metal feed liquid, palladium concentration is 1.5-5.5g/L, and platinum concentration is 10-15g/L, and current potential is 850-950mv, and acidity is 1-2mol/L, with S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase;
Step b, liquid more than extraction palladium is filtered after be warming up to and boil, add chloride solid to filter to saturated ammonium chloride solution inspection without after obvious sediment, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion use conventional zinc dust precipitation technique to reclaim platinum;
Step c, filter gained ammonium chloroplatinate weigh after be that the hydrochloric acid intensification pulp of 1:9-12 3.5-4.5mol/L is to 85-90 DEG C according to solid-to-liquid ratio, preparation acidity is 3.5-4.5mol/L, mass concentration is the hydrazine hydrochloride solution of 50-55g/L, adds hydrazine hydrochloride solution cold filtration after fully dissolving;
Steps d, filtrate are warming up to 90-95 DEG C, within logical chlorine 15-25 minute, until no longer include ammonium salt precipitation, catch up with chlorine 15-20 minute, cold filtration, the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion use conventional zinc dust precipitation technique to reclaim platinum;
After step e, repeating step c, steps d 2-3 time, ammonium chloroplatinate is according to the dilute hydrochloric acid solution pulp of solid-to-liquid ratio 1:4-6 pH=1-2, slowly add with the hydrazine hydrochloride solution of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain spongy platinum product.
The add-on of hydrazine hydrochloride solution described in described step c is 0.3 times of ammonium chloroplatinate quality.
In described steps d, the intake of chlorine is 40-50L/h.
The present invention is the method for separation and Extraction platinum liquid more than a kind of extraction palladium from platinum group metallic solution, slag or secondary resource, and the present invention has that flow process is simple, precious metal separation efficiency is high, avoid a large amount of ammonia-contaminated gas produced in hydrazine hydrate reduction ammonium chloroplatinate process, the advantage not producing nitrogen oxides pollution.Compared with prior art, there is following beneficial effect: 1. the present invention does not re-use the chloroazotic acid of severe corrosive, and operation process does not discharge nitrous oxides exhaust gas; 2. Pt, Pd separating effect of the present invention is better, reaches as high as more than 99%; 3. present invention, avoiding the drawback of manually catching up with nitre in aqua regia dissolution process, greatly save labour intensity; 4. the method cost is low, good operational environment, and throughput is large, and direct yield is high; 5. the present invention uses 1:1 hydrazine hydrochloride reduction ammonium chloroplatinate, greatly reduces the ammonia-contaminated gas produced in hydrazine hydrate reduction ammonium chloroplatinate process, environment-friendly high-efficiency.This technology has been successfully applied to the production of platinum metals separating-purifying, and output meets spongy platinum and the palladium sponge product of national standard.
Accompanying drawing explanation
Fig. 1 is flow process figure of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Controlling palladium concentration in platinum group metal feed liquid is 1.5g/L, and platinum concentration is 10g/L, and volume is 1L, and current potential is 850mv, and acidity is 1mol/L, with S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase; Platinum concentration 9.4g/L, palladium concentration 0.092g/L, volume 1L in liquid more than extraction palladium, carry a palladium organic phase and then after back extraction, extract palladium; Be warming up to after liquid more than extraction palladium is filtered and boil, add chloride solid 25g and filter without after obvious sediment to saturated ammonium chloride solution inspection, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion recovery platinum; Filter gained ammonium chloroplatinate 30g, according to the hydrochloric acid 270mL intensification pulp to 85 DEG C that solid-to-liquid ratio is 1:9 3.5mol/L, preparation acidity is 3.5mol/L, mass concentration is the hydrazine hydrochloride solution of 50g/L, be that 0.3 times of ammonium chloroplatinate quality slowly adds hydrazine hydrochloride solution 9g according to hydrazine hydrochloride quality, cold filtration after fully dissolving; Filtrate is warming up to 90 DEG C, and logical chlorine 15 minutes is until no longer include ammonium salt precipitation, and chlorine intake is that 45L/h catches up with chlorine 15 minutes, cold filtration, and the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion reclaim platinum; Repeating hydrazine hydrochloride reduction ammonium chloroplatinate-Tong chlorine sinks after platinum 3 times; By the dilute hydrochloric acid solution pulp according to the pH=1 of solid-to-liquid ratio 1:4 112mL of the 28g ammonium chloroplatinate that obtains, slowly add with the hydrazine hydrochloride solution 28g of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain the spongy platinum product of 99.99%.
Embodiment 2:
Controlling palladium concentration in platinum group metal feed liquid is 5.5g/L, and platinum concentration is 20g/L, and volume is 1L, and current potential is 950mv, and acidity is 1.2mol/L, with S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase; Platinum concentration 19.8g/L, palladium concentration 0.041g/L, volume 1L in liquid more than extraction palladium, carry a palladium organic phase and then after back extraction, extract palladium; Be warming up to after liquid more than extraction palladium is filtered and boil, add chloride solid 40g and filter without after obvious sediment to saturated ammonium chloride solution inspection, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion recovery platinum; Filter gained ammonium chloroplatinate 35g, according to the hydrochloric acid 600mL intensification pulp to 90 DEG C that solid-to-liquid ratio is 1:10 4.0mol/L, preparation acidity is 4.5mol/L, mass concentration is the hydrazine hydrochloride solution of 55g/L, be that 0.3 times of ammonium chloroplatinate quality slowly adds hydrazine hydrochloride solution 10.5g according to hydrazine hydrochloride quality, cold filtration after fully dissolving; Filtrate is warming up to 95 DEG C, and logical chlorine 20 minutes is until no longer include ammonium salt precipitation, and chlorine intake is that 50L/h catches up with chlorine 15 minutes, cold filtration, and the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion reclaim platinum; Repeating hydrazine hydrochloride reduction ammonium chloroplatinate-Tong chlorine sinks after platinum 2 times; By the dilute hydrochloric acid solution pulp according to the pH=2 of solid-to-liquid ratio 1:5 165mL of the 33g ammonium chloroplatinate that obtains, slowly add with the hydrazine hydrochloride solution 33g of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain the spongy platinum product of 99.99%.
Embodiment 3
Controlling palladium concentration in platinum group metal feed liquid is 2.5g/L, and platinum concentration is 15g/L, and volume is 1L, and current potential is 900mv, and acidity is 1.5mol/L, with S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase; Platinum concentration 14.1g/L, palladium concentration 0.012g/L, volume 1L in liquid more than extraction palladium, carry a palladium organic phase and then after back extraction, extract palladium; Be warming up to after liquid more than extraction palladium is filtered and boil, add chloride solid 30g and filter without after obvious sediment to saturated ammonium chloride solution inspection, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion recovery platinum; Filter gained ammonium chloroplatinate 30g, according to the hydrochloric acid 330mL intensification pulp to 90 DEG C that solid-to-liquid ratio is 1:11 4.5mol/L, preparation acidity is 4.5mol/L, mass concentration is the hydrazine hydrochloride solution of 55g/L, according to 0.3 times that hydrazine hydrochloride quality is ammonium chloroplatinate quality, slowly add hydrazine hydrochloride solution 9g, cold filtration after fully dissolving; Filtrate is warming up to 91 DEG C, and logical chlorine 15 minutes is until no longer include ammonium salt precipitation, and chlorine intake is that 40L/h catches up with chlorine 20 minutes, cold filtration, and the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion reclaim platinum; Repeating hydrazine hydrochloride reduction ammonium chloroplatinate-Tong chlorine sinks after platinum 3 times; By the dilute hydrochloric acid solution pulp according to the pH=1 of solid-to-liquid ratio 1:6 142mL of the 27g ammonium chloroplatinate that obtains, slowly add with the hydrazine hydrochloride solution 27g of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain the spongy platinum product of 99.99%.
Embodiment 4
In the chlorated liquid of adjustment platinum metals, palladium concentration is 4.0g/L, and platinum concentration is 15g/L, volume 920mL, and controlling potential is after 918mv acidity 1.8mol/L, through S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase; Platinum concentration 14.1g/L, palladium concentration 0.012g/L, volume 900mL in liquid more than extraction palladium, carry a palladium organic phase and then after back extraction, extract palladium; Be warming up to after liquid more than extraction palladium is filtered and boil, add chloride solid 29g and filter without after obvious sediment to saturated ammonium chloride solution inspection, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion recovery platinum; Filter gained ammonium chloroplatinate 25g, according to the hydrochloric acid 250mL intensification pulp to 90 DEG C that solid-to-liquid ratio is 1:10 4.5mol/L, preparation acidity is 4.5mol/L, mass concentration is the hydrazine hydrochloride solution of 53g/L, according to 0.3 times that hydrazine hydrochloride quality is ammonium chloroplatinate quality, slowly add hydrazine hydrochloride solution 7.5g, cold filtration after fully dissolving; Filtrate is warming up to 91 DEG C, and logical chlorine 15 minutes is until no longer include ammonium salt precipitation, and chlorine intake is 45L/h, catches up with chlorine 20 minutes, cold filtration, and the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion reclaim platinum; Repeating hydrazine hydrochloride reduction ammonium chloroplatinate-Tong chlorine sinks after platinum 3 times; By the dilute hydrochloric acid solution pulp according to the pH=2 of solid-to-liquid ratio 1:6 138mL of the 23g ammonium chloroplatinate that obtains, slowly add with the hydrazine hydrochloride solution 23g of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain the spongy platinum product of 99.99%.
Claims (4)
1. a method for separation and Extraction platinum metals, is characterized in that comprising following technique: controlling palladium concentration in platinum group metal feed liquid is 1.5-5.5g/L, and platinum concentration is 10-15g/L, and current potential is 850 ~ 950mv, uses S
201organic phase extraction palladium, carry palladium organic phase and then extract palladium through subsequent technique, more than extraction palladium, liquid adds ammonium chloride and sinks platinum, the ammonium chloroplatinate obtained dissolves by adding hydrazine hydrochloride solution reduction, and be warming up to 90-95 DEG C, logical chlorine catches up with chlorine, after the ammonium chloroplatinate of gained repeats hydrazine hydrochloride reducing process 2-3 time, just can obtain high purity platinum black by the reduction of 1:1 hydrazine hydrochloride in mass ratio ammonium chloroplatinate, after vacuum-drying, obtain spongy platinum product.
2. the method for a kind of separation and Extraction platinum metals according to claim 1, is characterized in that comprising the following steps:
In step a, control platinum group metal feed liquid, palladium concentration is 1.5-5.5g/L, and platinum concentration is 10-15g/L, and current potential is 850-950mv, and acidity is 1-2mol/L, with S
201extracting and separating palladium, extracts palladium after carrying the back extraction of palladium organic phase;
Step b, liquid more than extraction palladium is filtered after be warming up to and boil, add chloride solid and filter without after obvious sediment to saturated ammonium chloride solution inspection, after the ammonium chloroplatinate ammonium chloride solution washing obtained is neutrality to washing lotion, filtrate and washing lotion recovery platinum;
Step c, filter gained ammonium chloroplatinate weigh after be that the hydrochloric acid intensification pulp of 1:9-12 3.5-4.5mol/L is to 85-90 DEG C according to solid-to-liquid ratio, preparation acidity is 3.5-4.5mol/L, mass concentration is the hydrazine hydrochloride solution of 50-55g/L, adds hydrazine hydrochloride solution cold filtration after fully dissolving;
Steps d, filtrate are warming up to 90-95 DEG C, within logical chlorine 15-25 minute, until no longer include ammonium salt precipitation, catch up with chlorine 15-20 minute, cold filtration, the ammonium chloroplatinate ammonium chloride solution obtained washs, and washs after being neutrality to washing lotion, and filtrate and washing lotion use conventional zinc dust precipitation technique to reclaim platinum;
After step e, repeating step c, steps d 2-3 time, ammonium chloroplatinate is according to the dilute hydrochloric acid solution pulp of solid-to-liquid ratio 1:4-6 pH=1-2, slowly add with the hydrazine hydrochloride solution of ammonium chloroplatinate mass ratio 1:1 until when judging in solution platinum and precipitate completely, pure water platinum black, after vacuum-drying, obtain spongy platinum product.
3. the method for a kind of separation and Extraction platinum metals according to claim 1 and 2, is characterized in that: the add-on of hydrazine hydrochloride solution described in described step c is 0.3 times of ammonium chloroplatinate quality.
4. the method for a kind of separation and Extraction platinum metals according to claim 1 and 2, is characterized in that: in described steps d, the intake of chlorine is 40-50L/h.
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| CN107058731A (en) * | 2017-05-12 | 2017-08-18 | 江西铜业集团公司 | A kind of technique that platinum palladium product is produced by raw material of Pt Pd concentrate |
| CN107217143A (en) * | 2017-05-12 | 2017-09-29 | 江西铜业集团公司 | A kind of method of processing platinum group metal chloride precipitation slag |
| 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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| CN114182106A (en) * | 2021-11-25 | 2022-03-15 | 北京科技大学 | Method for separating and purifying platinum group metal in iron alloy |
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| CN106148724A (en) * | 2016-08-29 | 2016-11-23 | 金川集团股份有限公司 | A kind of platinum refinery practice |
| CN106148724B (en) * | 2016-08-29 | 2018-04-10 | 金川集团股份有限公司 | A kind of platinum refinery practice |
| CN107058731A (en) * | 2017-05-12 | 2017-08-18 | 江西铜业集团公司 | A kind of technique that platinum palladium product is produced by raw material of Pt Pd concentrate |
| CN107217143A (en) * | 2017-05-12 | 2017-09-29 | 江西铜业集团公司 | A kind of method of processing platinum group metal chloride precipitation slag |
| 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 |
| CN107574314B (en) * | 2017-08-25 | 2019-05-10 | 金川集团股份有限公司 | A method of the refined platinum from platinum strip liquor |
| CN110684902A (en) * | 2019-10-23 | 2020-01-14 | 金川集团股份有限公司 | Process for extracting noble metal by silver capture of high-alumina oil catalyst |
| CN110684902B (en) * | 2019-10-23 | 2021-06-08 | 金川集团股份有限公司 | Process for extracting noble metal by silver capture of high-alumina oil catalyst |
| CN112442599A (en) * | 2020-11-24 | 2021-03-05 | 金川集团股份有限公司 | Method for efficiently separating platinum and palladium from gold extraction residual liquid |
| CN114182106A (en) * | 2021-11-25 | 2022-03-15 | 北京科技大学 | Method for separating and purifying platinum group metal in iron alloy |
| CN114959289A (en) * | 2022-04-25 | 2022-08-30 | 金川集团股份有限公司 | Method for recovering platinum from palladium extraction organic phase |
| CN114959289B (en) * | 2022-04-25 | 2023-09-29 | 金川集团股份有限公司 | Method for recovering platinum in palladium extraction organic phase |
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