CN105441693B - A kind of method of separation and Extraction platinum group metal - Google Patents
A kind of method of separation and Extraction platinum group metal Download PDFInfo
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- CN105441693B CN105441693B CN201510797547.3A CN201510797547A CN105441693B CN 105441693 B CN105441693 B CN 105441693B CN 201510797547 A CN201510797547 A CN 201510797547A CN 105441693 B CN105441693 B CN 105441693B
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- platinum
- palladium
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- ammonium
- ammonium chloroplatinate
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 238000000605 extraction Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- 238000000926 separation method Methods 0.000 title claims abstract description 17
- 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 58
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 54
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 38
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 claims abstract description 35
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000460 chlorine Substances 0.000 claims abstract description 27
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 16
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 15
- 238000010792 warming Methods 0.000 claims abstract description 12
- 239000000284 extract Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims description 25
- 239000006210 lotion Substances 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 23
- 239000000706 filtrate Substances 0.000 claims description 18
- 230000007935 neutral effect Effects 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- 150000003863 ammonium salts Chemical class 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 12
- 239000007789 gas Substances 0.000 abstract description 5
- 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
- 239000010970 precious metal Substances 0.000 abstract description 3
- KIDPOJWGQRZHFM-UHFFFAOYSA-N platinum;hydrate Chemical compound O.[Pt] KIDPOJWGQRZHFM-UHFFFAOYSA-N 0.000 description 5
- 239000013049 sediment Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 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
Abstract
A kind of new method of separation and Extraction platinum group metal, its step are：It is 1.5 5.5g/L to control palladium concentration in platinum group metal feed liquid, and current potential is 850 950mv, uses S201Organic phase extracts palladium, carries palladium organic phase then by subsequent technique extraction palladium.Extract palladium extraction raffinate and add ammonium chloride and sink platinum, obtained ammonium chloroplatinate is dissolved by adding hydrazine hydrochloride solution reduction, is warming up to 90 95 DEG C, leads to chlorine, after the ammonium chloroplatinate of gained repeats hydrazine hydrochloride reducing process 23 times, passes through in mass ratio 1:1, it can obtain high-purity platinum black using hydrazine hydrochloride reduction ammonium chloroplatinate.Compared with prior art, the present invention there is flow simple, precious metal separation efficiency high, avoid hydrazine hydrate reduction ammonium chloroplatinate during caused a large amount of ammonia-contaminated gas, do not produce the advantages of nitrogen oxides pollution.
Description
Technical field
The invention belongs to metal separation technology field, and in particular to a kind of platinum group metallic solution, slag or secondary resource
Extract the method for separation and Extraction platinum in palladium extraction raffinate.
Background technology
At present, the refinery practice of multi-purpose aqua regia dissolution-ammonium chloride repeated precipitation is adopted in platinum refining process, this method is the most
Ancient classical refinery practice, during catching up with nitre, catching up with acid, part platinum can be dispersed in flue gas with flue gas；And 1% dissolving with hydrochloric acid not
Platinum content is higher in molten slag, causes the scattered of platinum.Catch up with acid, flooding process cumbersome, production cycle length, cost height.Chloroazotic acid
Caused nitrogen oxides in dissolving and hydrochloric acid flooding process, not only have a strong impact on the operating environment of post worker, and nitrogen oxygen
The more difficult absorption processing of compound, causes environmental protection pressure big.
The separation and Extraction of platinum palladium can also use extraction process, i.e. platinum group metal feed liquid elder generation S201Extraction of palladium, N235Extract platinum, so
Afterwards platinum palladium is extracted from extraction organic phase.Due to the presence of base metal and other impurity, cause continuously to extract operation and send out often
Raw line clogging, the third phase for the floccule that becomes turbid, aqueous phase carry organic equal phenomenon secretly, cause extraction efficiency to reduce.In addition,
Platinum strip liquor still needs to be incorporated to the heavy platinum group system progress refining treatment of aqua regia dissolution-ammonium chloride, can output qualified products.
The content of the invention
The technical problems to be solved by the invention are provided a kind of from platinum group metal the shortcomings that being directed in the prior art
Solution, slag or secondary resource extraction palladium extraction raffinate in separation and Extraction platinum method, the present invention has that flow is simple, precious metal separation effect
Rate is high, avoid hydrazine hydrate reduction ammonium chloroplatinate during caused a large amount of ammonia-contaminated gas, do not produce the excellent of nitrogen oxides pollution
Point.
Adopted the following technical scheme that to solve the technical problem of the present invention：
A kind of method of separation and Extraction platinum group metal, including following technique：The palladium concentration in platinum group metal feed liquid is controlled to be
1.5-5.5g/L, platinum concentration 10-15g/L, current potential are 850 ~ 950mv, use S201Organic phase extracts palladium, carries palladium organic phase and then passes through
Subsequent technique extraction palladium is crossed, extraction palladium extraction raffinate adds the heavy platinum of ammonium chloride, and obtained ammonium chloroplatinate is by adding hydrazine hydrochloride solution reduction
Dissolving, is warming up to 90-95 DEG C, and logical chlorine catches up with chlorine, after the ammonium chloroplatinate of gained repeats hydrazine hydrochloride reducing process 2-3 times, passes through
In mass ratio 1:1 hydrazine hydrochloride reduction ammonium chloroplatinate can obtain high-purity platinum black, after vacuum dried, obtain spongy platinum product.
The method of above-mentioned separation and Extraction platinum group metal, comprises the following steps：
Step a, it is 1.5-5.5g/L to control in platinum group metal feed liquid palladium concentration, platinum concentration 10-15g/L, and current potential is
850-950mv, acidity 1-2mol/L, with S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；
Step b, it will extract to be warming up to after palladium extraction raffinate filters and boil, and add chloride solid and extremely examined with saturated ammonium chloride solution
Without being filtered after obvious sediment, obtained ammonium chloroplatinate is washed to washing lotion in after neutral with ammonium chloride solution, and filtrate and washing lotion use
Conventional zinc dust precipitation technique reclaims platinum；
Step c, filtering gained ammonium chloroplatinate weigh after according to solid-to-liquid ratio be 1:9-12 3.5-4.5mol/L hydrochloric acid liter
To 85-90 DEG C, preparation acidity is 3.5-4.5mol/L for warm pulp, and mass concentration is 50-55g/L hydrochloric acid hydrazine solution, adds salt
Sour hydrazine solution cold filtration after abundant dissolving；
Step d, filtrate is warming up to 90-95 DEG C, leads to chlorine 15-25 minutes until there is no ammonium salt precipitation, catches up with chlorine 15-20
Minute, cold filtration, obtained ammonium chloroplatinate is washed with ammonium chloride solution, is washed after being in neutral to washing lotion, filtrate and washing lotion make
Platinum is reclaimed with conventional zinc dust precipitation technique；
Step e, after repeat step c, step d2-3 times, ammonium chloroplatinate is according to solid-to-liquid ratio 1:4-6 pH=1-2 watery hydrochloric acid
Solution pulp, it is slowly added to and ammonium chloroplatinate mass ratio 1:1 hydrochloric acid hydrazine solution is until judge that the platinum in solution precipitates completely
When, pure water platinum black, after vacuum dried, obtain spongy platinum product.
The addition of hydrochloric acid hydrazine solution described in the step c is 0.3 times of ammonium chloroplatinate quality.
The intake of chlorine is 40-50L/h in the step d.
The present invention is a kind of side of separation and Extraction platinum in extraction palladium extraction raffinate from platinum group metallic solution, slag or secondary resource
Method, the present invention has flow simple, precious metal separation efficiency high, avoid hydrazine hydrate reduction ammonium chloroplatinate during it is caused big
Amount ammonia-contaminated gas, the advantages of nitrogen oxides pollution is not produced.Compared with prior art, have the advantages that：1. the present invention
The chloroazotic acid of severe corrosive is not used, and operation process does not discharge nitrous oxides exhaust gas；2. Pt, Pd separating effect of the present invention compared with
It is good, reach as high as more than 99%；3. the drawbacks of present invention, avoiding nitre is manually caught up with during aqua regia dissolution, greatly save work
Intensity；4. this method cost is low, good operational environment, production capacity is big, and direct yield is high；5. the present invention uses 1:1 hydrazine hydrochloride reduces
Ammonium chloroplatinate, greatly reduce caused ammonia-contaminated gas during hydrazine hydrate reduction ammonium chloroplatinate, environment-friendly high-efficiency.The technology into
Work(is applied to the production of platinum group metal separating-purifying, and output meets the spongy platinum and palladium sponge product of national standard.
Brief description of the drawings
Fig. 1 is flow process figure of the present invention.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
It is 1.5g/L, platinum concentration 10g/L, volume 1L to control palladium concentration in platinum group metal feed liquid, and current potential is
850mv, acidity 1mol/L, with S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；Extract platinum concentration in palladium extraction raffinate
9.4g/L, palladium concentration 0.092g/L, volume 1L, carry palladium organic phase and palladium is then extracted after back extraction；It will be heated up after extraction palladium extraction raffinate filtering
To boiling, add chloride solid 25g and examined to saturated ammonium chloride solution without being filtered after obvious sediment, obtained ammonium chloroplatinate
Washed with ammonium chloride solution after being in neutral to washing lotion, filtrate and washing lotion recovery platinum；Filtering gained ammonium chloroplatinate 30g, according to solid-liquid
Than for 1:9 heat up pulp to 85 DEG C with 3.5mol/L hydrochloric acid 270mL, and preparation acidity is 3.5mol/L, mass concentration 50g/L
Hydrochloric acid hydrazine solution, be slowly added to hydrochloric acid hydrazine solution 9g for 0.3 times of ammonium chloroplatinate quality according to hydrazine hydrochloride quality, treat fully molten
Cold filtration after solution；Filtrate is warming up to 90 DEG C, leads to chlorine 15 minutes until there is no ammonium salt precipitation, chlorine intake is 45L/h
Catch up with chlorine 15 minutes, cold filtration, obtained ammonium chloroplatinate is washed with ammonium chloride solution, is washed after being in neutral to washing lotion, filtrate
And washing lotion recovery platinum；After repeating hydrazine hydrochloride reduction ammonium chloroplatinate-heavy platinum of logical chlorine 3 times；By obtained 28g ammonium chloroplatinates according to
Solid-to-liquid ratio 1:4 use the dilute hydrochloric acid solution pulp of 112mL pH=1, are slowly added to and ammonium chloroplatinate mass ratio 1:1 hydrazine hydrochloride is molten
Liquid 28g pure water platinum black, after vacuum dried, obtains 99.99% sea when the platinum judged in solution precipitates completely
Continuous platinum product.
Embodiment 2：
It is 5.5g/L, platinum concentration 20g/L, volume 1L to control palladium concentration in platinum group metal feed liquid, and current potential is
950mv, acidity 1.2mol/L, with S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；Extract platinum concentration in palladium extraction raffinate
19.8g/L, palladium concentration 0.041g/L, volume 1L, carry palladium organic phase and palladium is then extracted after back extraction；It will be heated up after extraction palladium extraction raffinate filtering
To boiling, add chloride solid 40g and examined to saturated ammonium chloride solution without being filtered after obvious sediment, obtained ammonium chloroplatinate
Washed with ammonium chloride solution after being in neutral to washing lotion, filtrate and washing lotion recovery platinum；Filtering gained ammonium chloroplatinate 35g, according to solid-liquid
Than for 1:10 heat up pulp to 90 DEG C with 4.0mol/L hydrochloric acid 600mL, and preparation acidity is 4.5mol/L, mass concentration 55g/
L hydrochloric acid hydrazine solution, hydrochloric acid hydrazine solution 10.5g is slowly added to according to 0.3 times of hydrazine hydrochloride quality for ammonium chloroplatinate quality, waits to fill
Divide cold filtration after dissolving；Filtrate is warming up to 95 DEG C, and logical chlorine 20 minutes is until there is no ammonium salt precipitation, chlorine intake to be
50L/h catches up with chlorine 15 minutes, cold filtration, and obtained ammonium chloroplatinate is washed with ammonium chloride solution, washs after being in neutral to washing lotion,
Filtrate and washing lotion recovery platinum；After repeating hydrazine hydrochloride reduction ammonium chloroplatinate-heavy platinum of logical chlorine 2 times；The 33g ammonium chloroplatinates that will be obtained
According to solid-to-liquid ratio 1:5 use the dilute hydrochloric acid solution pulp of 165mL pH=2, are slowly added to and ammonium chloroplatinate mass ratio 1:1 hydrochloric acid
Hydrazine solution 33g pure water platinum black, after vacuum dried, obtains 99.99% when the platinum judged in solution precipitates completely
Spongy platinum product.
Embodiment 3
It is 2.5g/L, platinum concentration 15g/L, volume 1L to control palladium concentration in platinum group metal feed liquid, and current potential is
900mv, acidity 1.5mol/L, with S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；Extract platinum concentration in palladium extraction raffinate
14.1g/L, palladium concentration 0.012g/L, volume 1L, carry palladium organic phase and palladium is then extracted after back extraction；It will be heated up after extraction palladium extraction raffinate filtering
To boiling, add chloride solid 30g and examined to saturated ammonium chloride solution without being filtered after obvious sediment, obtained ammonium chloroplatinate
Washed with ammonium chloride solution after being in neutral to washing lotion, filtrate and washing lotion recovery platinum；Filtering gained ammonium chloroplatinate 30g, according to solid-liquid
Than for 1:11 heat up pulp to 90 DEG C with 4.5mol/L hydrochloric acid 330mL, and preparation acidity is 4.5mol/L, mass concentration 55g/
L hydrochloric acid hydrazine solution, according to 0.3 times that hydrazine hydrochloride quality is ammonium chloroplatinate quality, hydrochloric acid hydrazine solution 9g is slowly added to, is treated fully
Cold filtration after dissolving；Filtrate is warming up to 91 DEG C, leads to chlorine 15 minutes until there is no ammonium salt precipitation, chlorine intake is 40L/
H catches up with chlorine 20 minutes, cold filtration, and obtained ammonium chloroplatinate is washed with ammonium chloride solution, washs after being in neutral to washing lotion, filtrate
And washing lotion recovery platinum；After repeating hydrazine hydrochloride reduction ammonium chloroplatinate-heavy platinum of logical chlorine 3 times；By obtained 27g ammonium chloroplatinates according to
Solid-to-liquid ratio 1:6 use the dilute hydrochloric acid solution pulp of 142mL pH=1, are slowly added to and ammonium chloroplatinate mass ratio 1:1 hydrazine hydrochloride is molten
Liquid 27g pure water platinum black, after vacuum dried, obtains 99.99% sea when the platinum judged in solution precipitates completely
Continuous platinum product.
Embodiment 4
It is 4.0g/L, platinum concentration 15g/L, volume 920mL to adjust palladium concentration in the chlorated liquid of platinum group metal, and controlling potential is
After 918mv acidity 1.8mol/L, through S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；Extract platinum concentration in palladium extraction raffinate
14.1g/L, palladium concentration 0.012g/L, volume 900mL, carry palladium organic phase and palladium is then extracted after back extraction；After the filtering of palladium extraction raffinate will be extracted
It is warming up to and boils, adds chloride solid 29g and examined to saturated ammonium chloride solution without being filtered after obvious sediment, obtained chlorine platinum
Sour ammonium is washed to washing lotion in after neutral with ammonium chloride solution, filtrate and washing lotion recovery platinum；Filtering gained ammonium chloroplatinate 25g, according to
Solid-to-liquid ratio is 1:10 heat up pulp to 90 DEG C with 4.5mol/L hydrochloric acid 250mL, and preparation acidity is 4.5mol/L, and mass concentration is
53g/L hydrochloric acid hydrazine solution, according to 0.3 times that hydrazine hydrochloride quality is ammonium chloroplatinate quality, hydrochloric acid hydrazine solution 7.5g is slowly added to,
The cold filtration after abundant dissolving；Filtrate is warming up to 91 DEG C, leads to chlorine 15 minutes until there is no ammonium salt precipitation, chlorine intake
For 45L/h, chlorine is caught up with 20 minutes, cold filtration, obtained ammonium chloroplatinate is washed with ammonium chloride solution, is washed to washing lotion in neutrality
Afterwards, filtrate and washing lotion recovery platinum；After repeating hydrazine hydrochloride reduction ammonium chloroplatinate-heavy platinum of logical chlorine 3 times；The 23g chloroplatinic acids that will be obtained
Ammonium is according to solid-to-liquid ratio 1:6 use the dilute hydrochloric acid solution pulp of 138mL pH=2, are slowly added to and ammonium chloroplatinate mass ratio 1:1 salt
Sour hydrazine solution 23g pure water platinum black, after vacuum dried, is obtained when the platinum judged in solution precipitates completely
99.99% spongy platinum product.
Claims (4)
- A kind of 1. method of separation and Extraction platinum group metal, it is characterised in that including following technique：Control in platinum group metal feed liquid Palladium concentration is 1.5-5.5g/L, and platinum concentration 10-15g/L, current potential is 850 ~ 950mv, uses S201Organic phase extracts palladium, and carrying palladium has Machine phase is then by subsequent technique extraction palladium, and extraction palladium extraction raffinate adds the heavy platinum of ammonium chloride, and obtained ammonium chloroplatinate is by adding hydrazine hydrochloride Solution reduction dissolves, and is warming up to 90-95 DEG C, and logical chlorine catches up with chlorine, and the ammonium chloroplatinate of gained repeats hydrazine hydrochloride reducing process 2-3 times Afterwards, in mass ratio 1 is passed through:1 hydrazine hydrochloride reduction ammonium chloroplatinate can obtain high-purity platinum black, after vacuum dried, obtain sponge Platinum product.
- 2. the method for a kind of separation and Extraction platinum group metal according to claim 1, it is characterised in that comprise the following steps：Step a, it is 1.5-5.5g/L, platinum concentration 10-15g/L, current potential 850- to control palladium concentration in platinum group metal feed liquid 950mv, acidity 1-2mol/L, with S201Extracting and separating palladium, palladium is extracted after carrying the back extraction of palladium organic phase；Step b, it will be warming up to and boil after extraction palladium extraction raffinate filtering, add chloride solid and examined to saturated ammonium chloride solution without bright Filtered after aobvious precipitation, obtained ammonium chloroplatinate is washed to washing lotion in after neutral with ammonium chloride solution, filtrate and washing lotion recovery platinum；Step c, filtering gained ammonium chloroplatinate weigh after according to solid-to-liquid ratio be 1:9-12 is heated up with 3.5-4.5mol/L hydrochloric acid to be starched Change to 85-90 DEG C, preparation acidity is 3.5-4.5mol/L, and mass concentration is 50-55g/L hydrochloric acid hydrazine solution, adds hydrazine hydrochloride Solution cold filtration after abundant dissolving；Step d, filtrate is warming up to 90-95 DEG C, leads to chlorine 15-25 minutes until there is no ammonium salt precipitation, catches up with 15-20 points of chlorine Clock, cold filtration, obtained ammonium chloroplatinate are washed with ammonium chloride solution, are washed after being in neutral to washing lotion, and filtrate and washing lotion use Conventional zinc dust precipitation technique reclaims platinum；Step e, after repeat step c, step d 2-3 times, ammonium chloroplatinate is according to solid-to-liquid ratio 1:4-6 pH=1-2 dilute hydrochloric acid solution Pulp, it is slowly added to and ammonium chloroplatinate mass ratio 1:1 hydrochloric acid hydrazine solution is pure when the platinum judged in solution precipitates completely Water washing platinum black, after vacuum dried, obtain spongy platinum product.
- A kind of 3. method of separation and Extraction platinum group metal according to claim 2, it is characterised in that：Salt in the step c The addition of sour hydrazine solution is 0.3 times of ammonium chloroplatinate quality.
- A kind of 4. method of separation and Extraction platinum group metal according to claim 2, it is characterised in that：Chlorine in the step d The intake of gas is 40-50L/h.
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| CN106148724B (en) * | 2016-08-29 | 2018-04-10 | 金川集团股份有限公司 | A kind of platinum refinery practice |
| CN107058731B (en) * | 2017-05-12 | 2019-02-01 | 江西铜业集团公司 | A kind of technique that platinum palladium product is produced as raw material using 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 |
| 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 |
| 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 |
| CN114182106B (en) * | 2021-11-25 | 2022-08-19 | 北京科技大学 | Method for separating and purifying platinum group metal in iron alloy |
| 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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| JP2820289B2 (en) * | 1989-10-13 | 1998-11-05 | 田中貴金属工業株式会社 | Method for producing potassium tetrachloroplatinate |
| JP3479483B2 (en) * | 1999-12-28 | 2003-12-15 | 日鉱金属株式会社 | Recovery method of high purity platinum |
| JP4323492B2 (en) * | 2006-03-31 | 2009-09-02 | 日鉱金属株式会社 | Method for recovering platinum in waste liquid containing selenium using hydrazine |
| CN101279772B (en) * | 2008-05-15 | 2011-01-19 | 金川集团有限公司 | Preparation of potassium platinochloride |
| CN102797018B (en) * | 2012-08-30 | 2015-09-23 | 贵研资源（易门）有限公司 | A kind of method adopting controlling potential separating-purifying platinum |
| CN103484687B (en) * | 2013-10-11 | 2014-07-16 | 金川集团股份有限公司 | Platinum refining technology |
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