EP3749792A1 - Verfahren zur hydrometallurgischen aufarbeitung einer edelmetall-zinn-legierung - Google Patents
Verfahren zur hydrometallurgischen aufarbeitung einer edelmetall-zinn-legierungInfo
- Publication number
- EP3749792A1 EP3749792A1 EP18753327.8A EP18753327A EP3749792A1 EP 3749792 A1 EP3749792 A1 EP 3749792A1 EP 18753327 A EP18753327 A EP 18753327A EP 3749792 A1 EP3749792 A1 EP 3749792A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- noble metal
- metal
- tin
- tin alloy
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 45
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 38
- 239000011135 tin Substances 0.000 claims abstract description 34
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052718 tin Inorganic materials 0.000 claims abstract description 33
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 32
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010931 gold Substances 0.000 claims abstract description 26
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 25
- 229910052737 gold Inorganic materials 0.000 claims abstract description 24
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 17
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004332 silver Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 10
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 22
- 229910000510 noble metal Inorganic materials 0.000 claims description 19
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 17
- 239000010970 precious metal Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 239000002699 waste material Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 12
- 239000002893 slag Substances 0.000 claims description 12
- 238000005275 alloying Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 239000011819 refractory material Substances 0.000 claims description 4
- -1 Hybobromites Chemical class 0.000 claims description 3
- 239000003082 abrasive agent Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 238000010626 work up procedure Methods 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical class [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Chemical class [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- 235000012255 calcium oxide Nutrition 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 235000011132 calcium sulphate Nutrition 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical class OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 claims description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical class Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 2
- GEOVEUCEIQCBKH-UHFFFAOYSA-N hypoiodous acid Chemical class IO GEOVEUCEIQCBKH-UHFFFAOYSA-N 0.000 claims description 2
- ICIWUVCWSCSTAQ-UHFFFAOYSA-N iodic acid Chemical class OI(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-N 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 235000013980 iron oxide Nutrition 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical class OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000010802 sludge Substances 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- 239000010793 electronic waste Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 15
- 239000002253 acid Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000009853 pyrometallurgy Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- CQVDKGFMVXRRAI-UHFFFAOYSA-J Cl[Au](Cl)(Cl)Cl Chemical compound Cl[Au](Cl)(Cl)Cl CQVDKGFMVXRRAI-UHFFFAOYSA-J 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 230000002146 bilateral effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000010792 electronic scrap Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- CUILPNURFADTPE-UHFFFAOYSA-N hypobromous acid Chemical class BrO CUILPNURFADTPE-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010414 supernatant solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0438—Nitric acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C11/00—Alloys based on lead
- C22C11/04—Alloys based on lead with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
- C22C3/005—Separation of the constituents of alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Definitions
- the invention relates to a process for the hydrometallurgical work-up of certain of (i) gold and / or platinum, (ii) palladium, silver and / or copper, (iii) tin and optionally (iv) one or more other elements of existing alloys with a particular gold and / or platinum: tin weight ratio.
- Gold, platinum, palladium and silver are precious metals; Copper and tin are non-noble metals.
- Gold and / or platinum on the one hand and palladium, silver and / or copper on the other hand containing alloys are usually worked up hydrometallurgically by first being treated in a first step with nitric acid, whereby the less noble metals palladium, silver or copper than nitrate go into solution compared to gold and platinum.
- Gold or platinum in the remaining residue can be brought into solution in a subsequent step with a medium comprising hydrochloric acid and suitable oxidizing agent as tetrachloroauric or hexachloroplatinic acid. If said alloys also contain tin, this separation process can often not be carried out without further ado.
- the invention relates to a process for the hydrometallurgical workup of a noble metal-tin alloy consisting of (i) 0.45 to 25 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 35 to 99.2 Wt .-% of at least one metal B selected from the group consisting of palladium, silver and copper, (iii) 0.3 to 30 wt .-% tin and (iv) 0 to 50 wt .-% of at least one of gold , Platinum, palladium, silver, copper and tin different element with a metal A: tin weight ratio of>
- the method comprises the steps:
- the noble metal-tin alloy in process step (a1) is selected in a targeted manner or in process step (a2) specifically prepared so that it is from the constituents (i) 0.45 to 25 wt .-%, preferably 3 to 20 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 35 to 99.2 wt .-%, preferably 40 to 95 wt .-% of at least one metal B selected from the group consisting of palladium, silver and copper, (iii) 0.3 to 30% by weight, preferably 2 to 17.5% by weight of tin and (iv) 0 to 50% by weight of at least one of gold, Platinum, palladium, silver, copper and tin of various elements composed to 100 wt .-% and at the same time a metal A: tin weight ratio of> 0.7: 1, preferably in the range of 1: 1 to 10: 1. It will be apparent to those skilled in the art that given the weight ratio
- the noble metal-tin alloy consists of (i) 3 to 20 wt .-% of at least one metal A selected from the group consisting of gold and platinum, (ii) 40 to 95 wt .-% of at least one metal B selected from Group consisting of palladium, silver and copper, (iii) 2 to 17.5% by weight of tin and (iv) 0 to 50% by weight of at least one of gold, platinum, Palladium, silver, copper and tin different element with a metal A: tin weight ratio ranging from 1: 1 to 10: 1.
- noble metal-tin alloys assembled as mentioned above are noble metal-tin alloys composed essentially according to the invention, also referred to herein as "noble-metal-tin alloy of the invention essentially composed type" or as "the noble metal-tin alloy” , Obviously, the essential composition of the precious metal-tin alloy according to the invention forms an essential prerequisite for a successful and uncomplicated implementation of the method according to the invention with avoidance of the aforementioned problems in solid-liquid separation.
- the noble metal-tin alloy is selected specifically, in particular under noble metal-tin alloys.
- the targeted selection takes place in such a way that the above-mentioned conditions according to the invention are fulfilled with regard to composition and, concomitantly, also the metal A: tin weight ratio. Accordingly, the noble metal-tin alloy of the type essentially composed according to the invention can already be ready and can be worked up by hydrometallurgy in process steps (b) to (d).
- the noble metal-tin alloy is initially produced in a targeted manner such that the abovementioned conditions essential to the invention are fulfilled with respect to composition and, concomitantly, also the metal A: tin weight ratio.
- the noble metal-tin alloy can be prepared by alloying the metals or elements making up it.
- the precious metal-tin alloy is generally not preferably prepared directly by alloying the metals or elements constituting it.
- the noble metal-tin alloy in process step (a2) can be prepared in a targeted manner by one of the following methods (a2-1) to (a2-5) known to the person skilled in the art.
- the person skilled in the art knows how to skilfully select and combine the starting materials according to type and quantity in each case in order to arrive at a precious metal-tin alloy of the type essential to the invention.
- the procedure (a2-1) comprises or consists of melting at least one recyclable material to be recycled to form a multiphase system comprising a lower A molten noble metal-tin alloy phase of the type essential to the invention and an upper phase of lower density molten slag, optionally with the addition of collector metal and / or slag former and / or reducing agent, and separating the upper phase from the catalyst lower phase, taking advantage of the difference in density, followed by cooling and solidification of the melt separated from each other, and take-up of the solidified noble metal-tin alloy.
- the recyclable material to be recycled may be a single recyclable material or a mixture of different recyclables.
- the at least one recyclable material to be recycled may comprise not only noble metal and non-noble metal but also at least one substance different therefrom, the latter in particular selected from inorganic refractory materials, i. Inorganic non-metallic at high temperatures, for example in the range of 200 to 650 ° C physically and chemically not or practically non-changing materials.
- inorganic refractory materials include silica, alumina, calcia, iron oxide, calcium sulfate, calcium phosphate and tin dioxide.
- the at least one substance other than noble metal and non-noble metal may be, for example, a constituent, if appropriate sole constituent of ceramic filter materials, blasting agents, abrasives and / or inorganic support materials, for example catalyst support materials.
- the at least one recyclable material to be recycled can come from one or more different sources. It may be mine concentrate and / or one or more wastes or waste mixtures. Examples of types of waste include waste from the
- the procedure (a2-2) comprises or consists in treating a molten alloy different from the noble metal-tin alloy of the type substantially composed of the invention with an oxidizing agent such as, in particular, oxygen to form a multiple A phase system comprising a lower phase of molten noble metal-tin alloy of the invention essentially composed type and an upper phase of molten slag of lower density in which formed oxidation products are found, optionally with the addition of collector metal and / or slag formers, and separating the above From the lower phase, taking advantage of the density difference, followed by cooling and solidification of the separated melts, and take-up of the solidified noble metal-tin alloy.
- an oxidizing agent such as, in particular, oxygen
- the procedure (a2-3) comprises or consists in alloying at least two mutually different alloys, if appropriate by alloying at least one element, for example metal, to form a noble metal-tin alloy of the invention essentially composed type.
- the at least two mutually different alloys may be at least two different noble metal-tin alloys of the invention substantially composite type or at least two different from each other and of the invention substantially composite type different noble metal-tin alloys or at least one noble metal-tin alloy of Actively composed of the essential type and at least one of the invention substantially composite type different noble metal-tin alloy act.
- at least one of the at least two mutually different alloys is not a noble metal-tin alloy. Often, none of the at least two different alloys is a noble metal-tin alloy.
- the procedure (a2-4) comprises or consists in alloying at least one element, for example a metal, to form an alloy with the formation of a noble metal-tin alloy of the type essential to the invention.
- a noble metal-tin alloy of the type essential to the invention may itself already be a noble metal-tin alloy of the type substantially of the invention. in general, however, it is not a noble metal-tin alloy of the invention essential composite type.
- the procedure (a2-5) comprises or consists in distilling off tin, for example excess tin, from an alloy, if appropriate with the aid of vacuum or under reduced pressure with formation of a noble metal-tin alloy, from the inventive essential type.
- tin for example excess tin
- the alloy undergoing distilling off of tin itself may already be a precious metal-tin alloy of the type essentially composed according to the invention; In general, however, it is not a noble metal-tin alloy of the type essential to the invention.
- step (b) of the process according to the invention nitric acid-soluble or salicylic acid-soluble constituents of the noble metal-tin alloy purposely selected in step (a1) or produced in step (a2) are reacted with nitric acid to form a nitric acid - solved solution comprising the at least one metal B dissolved as dissolved nitrate and an undissolved residue.
- the nitric acid used in step (b) has an oxidizing effect and has a concentration, for example, in the range from 10 to 67% by weight.
- Step (b) can be carried out at temperatures, for example in the range of 20 ° C to boiling temperature.
- the undissolved residue comprising gold or platinum does not require any additional chemical treatment or separation step before carrying out process step (d).
- the undissolved residue is not associated with interfering tin dioxide, or at least substantially none, or is free thereof.
- step (c) of the process according to the invention the undissolved residue formed in step (b) is separated from the nitric acid solution.
- customary solid-liquid separation processes known to the person skilled in the art, for example decantation, removal, filtration or suitable combinations of such separation processes.
- step (d) of the process according to the invention the undissolved residue removed in step (c) from the nitric acid solution is dissolved in a medium comprising hydrochloric acid and at least one oxidizing agent.
- a medium comprising hydrochloric acid and at least one oxidizing agent.
- it is possible to form a solution comprising hexachlorotinic acid and tetrachloroauric acid or hexachlorotinic acid, as well as hexachloroplatinic acid or hexachlorotinic acid, and tetrachloroauric acid and hexachloroplatinic acid.
- the hydrochloric acid used in step (d) has a concentration, for example, in the range of 3 to 12 mol / L.
- the at least one oxidizing agent may in particular be selected from the group consisting of nitric acid, chlorates, nitrates, bromates, iodates, chlorites, bromites, iodites, hypochlorites, hypobromites, hypoiodites, perchlorates, ozone, ozonides, superoxides, oxygen, chlorine, bromine , iodine, peroxo compounds, permanganates and chromates.
- Step (d) may be carried out at temperatures, for example, in the range of 20 ° C to boiling temperature.
- Alloys with the composition given in the table below were each admixed with 4 ml of 53% strength by weight nitric acid per gram of alloy and carefully heated from room temperature to 100 ° C. with stirring. The alloys were partially dissolved by the formation of a black to shiny metallic residue and NOx gas. The absence of NOx evolution signaled the end of the dissolution reaction (duration between 2 and 7 hours). After cooling, the respective resulting mixture was filtered over a period of 10 to 60 minutes and the residue was washed several times with water.
- the washed residue was treated either with aqua regia (mixture of 75 ml of 10M hydrochloric acid and 25 ml of 53% strength by weight nitric acid) or made up to a total volume of 100 ml with 6M hydrochloric acid.
- the mixture was heated with stirring to 80 ° C and, if not done so, mixed with 53 wt .-% nitric acid until no further change in the reaction mixture and no further NOx formation can be seen on further addition was (10 to 20 ml of the 53 wt .-% nitric acid).
- the residue dissolved to give a yellow to orange colored clear solution. After cooling, the respective mixture obtained was filtered for a period of 10 to 60 minutes and the residue was washed with 6M hydrochloric acid.
- Alloys with the composition given in the table below were each admixed with 4 ml of 53% strength by weight nitric acid per gram of alloy and carefully heated from room temperature to 100 ° C. with stirring. The alloys partially dissolved under bilateral fertilize a purple voluminous residue and NOx gas. The absence of NOx evolution signaled the end of the dissolution reaction (duration between 2 and 7 hours). After cooling, the respective resulting mixture was filtered over a period of 10 to 60 minutes and the residue was washed several times with water.
- the purple color of the residue indicated the formation of Au particles in the tin dioxide matrix ("Cassius gold purple”).
- Phase analysis on a sample of the residue by X-ray diffractometry revealed tin dioxide as the major phase.
- the leached residue was made up to 200 ml with 6M hydrochloric acid, heated to 80 ° C. with stirring, and either 4.5M sodium chlorate solution or 53% strength by weight nitric acid was added dropwise until the redox potential of the mixture was> 900 mV vs. Ag / AgCl standard electrode. The mixture turned from purple to yellow and a milky suspension formed.
- the mixture was allowed to cool and filtered through a Blauband paper filter. In this case, a clear filtrate was never obtained because fine white particles penetrated through the filter. The filtration was slow and in no case feasible within a period of less than 6 hours. At times, the mixture formed a stable suspension with a gel-like to slimy consistency that clogged the filter and did not allow solid / liquid separation.
- the metal button was cut and in each case a fragment of about 10 g in a beaker and poured with 4 ml of 53 wt.% Nitric acid per gram of alloy and diluted with water by%. and to obtain ⁇ -concentrated nitric acid:
- the mixture was stirred overnight at room temperature, then at 100 ° C for a further 3 hours. At first there was a reaction after heating, then not anymore. It was allowed to cool with stirring. The supernatant solution was filtered through blue band filter. The residues were added directly to a beaker and made up to about 100 ml with 6M hydrochloric acid. While stirring, 4.5M sodium chlorate solution was added dropwise at 60 ° C. After 0.2 ml of addition, the mixture had each discolored from purple to milky yellow. A total of 1 mL sodium chlorate solution was added. The mixture was stirred for 1.5 hours, then the excess chlorate was boiled and the solution was allowed to cool. The mixtures were filtered, again to give a white precipitate which was fine enough to penetrate through the filter.
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EP18155948 | 2018-02-09 | ||
PCT/EP2018/070531 WO2019154530A1 (de) | 2018-02-09 | 2018-07-30 | Verfahren zur hydrometallurgischen aufarbeitung einer edelmetall-zinn-legierung |
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EP3749792A1 true EP3749792A1 (de) | 2020-12-16 |
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US (1) | US20210071284A1 (de) |
EP (1) | EP3749792B1 (de) |
CN (1) | CN111630193B (de) |
TW (1) | TWI685571B (de) |
WO (1) | WO2019154530A1 (de) |
ZA (1) | ZA202004852B (de) |
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CN114807624B (zh) * | 2022-04-07 | 2023-10-13 | 北京电子科技职业学院 | 一种抗氧化耐磨贵金属首饰的制备装置及方法 |
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US4293332A (en) * | 1977-06-08 | 1981-10-06 | Institute Of Nuclear Energy Research | Hydrometallurgical process for recovering precious metals from anode slime |
FR2498682B1 (fr) * | 1981-01-23 | 1986-08-08 | Industeler | Silencieux en matiere inoxydable pour pot d'echappement pour vehicule automobile |
JPS58107438A (ja) * | 1981-12-18 | 1983-06-27 | Ishifuku Kinzoku Kogyo Kk | 歯科用低カラツト焼付合金 |
US4906293A (en) * | 1985-09-03 | 1990-03-06 | Eldred Daniel S | Hydrometallurgical process for extracting metals from ocean-mined ferromanganese nodules |
JP3251899B2 (ja) * | 1998-02-13 | 2002-01-28 | 財団法人電気磁気材料研究所 | 耐摩耗性高透磁率合金および磁気記録再生ヘッド |
JP2000119772A (ja) * | 1998-10-15 | 2000-04-25 | Soichi Nagasawa | 装身具用銀合金 |
SG10201502960YA (en) * | 2010-04-15 | 2015-06-29 | Entegris Inc | Method for recycling of obsolete printed circuit boards |
CN103451432B (zh) * | 2013-08-27 | 2015-08-05 | 江西南城鑫业环保处置有限公司 | 一种从含贵金属废催化剂中提取铅和贵金属的方法 |
GB2518223A (en) * | 2013-09-16 | 2015-03-18 | Itri Innovation Ltd | Recovery of metals |
CN104630479B (zh) * | 2013-11-07 | 2016-08-17 | 中国科学院宁波材料技术与工程研究所 | 一种从电子废弃物中回收多种金属的方法 |
CN103966450B (zh) * | 2014-05-23 | 2016-03-30 | 江西理工大学 | 一种铜阳极泥的全湿法预处理方法 |
WO2015193515A1 (de) * | 2014-11-10 | 2015-12-23 | Heraeus Deutschland GmbH & Co. KG | Verfahren zur aufarbeitung edelmetall-haltiger materialien |
PL2985354T3 (pl) * | 2014-11-10 | 2017-04-28 | Heraeus Deutschland Gmbh & Co Kg | Sposób usuwania metalu szlachetnego z kształtek katalizatora zawierających metal szlachetny |
CN105886769B (zh) * | 2015-01-26 | 2018-11-13 | 昆明冶金高等专科学校 | 一种硝酸溶解多金属合金物料集贵金属的方法 |
CN104711573A (zh) * | 2015-03-27 | 2015-06-17 | 章平传 | 一种多酸复合型退锡溶液 |
CN105200243B (zh) * | 2015-10-12 | 2017-06-20 | 湖南金旺铋业股份有限公司 | 一种金银合金分离提纯的工艺 |
TWI585238B (zh) * | 2016-03-09 | 2017-06-01 | 賀陳弘 | 利用鹽酸回收印刷電路板中金屬之方法 |
CN105803206A (zh) * | 2016-03-28 | 2016-07-27 | 河南工信环保科技有限公司 | 一种无害化深度处理废旧线路板回收金属的方法 |
CN105842102B (zh) * | 2016-06-22 | 2018-04-20 | 大冶有色设计研究院有限公司 | 一种银阳极泥中金银的快速分析方法 |
CN107034363B (zh) * | 2017-04-28 | 2019-03-19 | 西北有色金属研究院 | 一种从含锡镀金电子废料中快速回收金箔的方法 |
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2018
- 2018-07-30 EP EP18753327.8A patent/EP3749792B1/de active Active
- 2018-07-30 CN CN201880086297.4A patent/CN111630193B/zh not_active Expired - Fee Related
- 2018-07-30 WO PCT/EP2018/070531 patent/WO2019154530A1/de unknown
- 2018-07-30 US US16/963,661 patent/US20210071284A1/en not_active Abandoned
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TWI685571B (zh) | 2020-02-21 |
WO2019154530A1 (de) | 2019-08-15 |
TW201934765A (zh) | 2019-09-01 |
US20210071284A1 (en) | 2021-03-11 |
EP3749792B1 (de) | 2021-06-09 |
ZA202004852B (en) | 2022-04-28 |
CN111630193B (zh) | 2022-05-03 |
CN111630193A (zh) | 2020-09-04 |
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