SG186401A1 - Recovery method for high purity platinum - Google Patents
Recovery method for high purity platinum Download PDFInfo
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- SG186401A1 SG186401A1 SG2012093555A SG2012093555A SG186401A1 SG 186401 A1 SG186401 A1 SG 186401A1 SG 2012093555 A SG2012093555 A SG 2012093555A SG 2012093555 A SG2012093555 A SG 2012093555A SG 186401 A1 SG186401 A1 SG 186401A1
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- SG
- Singapore
- Prior art keywords
- platinum
- ruthenium
- high purity
- aqua regia
- recovery method
- Prior art date
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 302
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 140
- 238000011084 recovery Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 90
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 87
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 55
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 27
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 22
- 229910001260 Pt alloy Inorganic materials 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000000696 magnetic material Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 abstract description 15
- 239000010941 cobalt Substances 0.000 abstract description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052804 chromium Inorganic materials 0.000 abstract description 13
- 239000011651 chromium Substances 0.000 abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052802 copper Inorganic materials 0.000 abstract description 8
- 239000010949 copper Substances 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 6
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 5
- 238000005477 sputtering target Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 43
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 13
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 150000003057 platinum Chemical class 0.000 description 8
- 230000003247 decreasing effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 150000003303 ruthenium Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- -1 platinum group metals Chemical class 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- XUXNAKZDHHEHPC-UHFFFAOYSA-M sodium bromate Chemical compound [Na+].[O-]Br(=O)=O XUXNAKZDHHEHPC-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-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
- C22B11/04—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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/025—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper, or baths
-
- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- 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
RECOVERY METHOD FOR HIGH PURITY PLATINUMA high purity platinum recovery method including the steps of dissolving a platinum alloy containing ruthenium in aqua regia and eliminating residue, thereaftercausing acid with platinum dissolved therein and an ammonium chloride solution to react so as to deposit chloroplatinic ammonium salt, and reducing the chloroplatinic ammonium salt to obtain a platinum sponge. The method is characterized in that acid with platinum dissolved therein and the ammonium chloride solution are caused to react at a temperature of 40°C or higher. Provided is a method which enables recovery, at a high yield, of high purity platinum which can be reused in a platinum and a platinum-containing target as a result of efficiently eliminating ruthenium, cobalt, chromium, copper, iron, nickel, silicon and the like which become included in a spent platinum alloy sputtering target, particularly a magnetic material target, and in scraps such as mill ends, sawdust, and surface grinding scraps generated during theproduction process of such a target.
Description
WQ2012/029379 ; PCT/JP2011/064006
RECOVERY METHOD FOR HIGH PURITY PLATINUM
[0001]
The present invention relates to a recovery method of high purity platinum for recovering high purity platinum, at a high yield, from a platinum alloy containing platinum and ruthenium as components, and in particular from scraps of a magnetic material target or the like.
[0002]
In recent years, pursuant to the considerable advancement of semiconductor integrated circuits, various thin films are being formed for circuit design and the formation of various electrical and electronic devices. Among the ih above, an alloy sputtering target containing platinum is also used for forming a specific thin film for use as a magnetic thin film for a recording medium or as a semiconductor material. This kind of platinum alloy target often also contains ruthenium as an alloy element.
These thin films are formed by sputtering an alloy target containing platinum or the like in an inert atmosphere of argon gas or the like.
[0003] During the stage that this kind of target is produced, a large amount of mill ends such as sawdust is generated. All of such mill ends become scraps. And the spent target also becomes a scrap.
During the production process of the target, as a result of the plastic working such as forging/rolling or mechanical processing such as cutting of the ingot after the ingot is melted and cast, and due to the process of bonding the target to the backing plate, the portion that comes into contact with the target becomes contaminated. In particular, contamination is severe which is caused by heavy metals and the like from the material configuring the cutting tools used for the 3 mechanical processing and peripheral processing tools is severe.
Since platinum is an expensive material, it is necessary to recover and reuse the same, but there is a problem in that a material containing the foregoing contaminants cannot be used as is.
WQ2012/028379 , PCT/JP2011/0640096
[0004] The foregoing impurities may cause the deterioration of performance of recording mediums, hard disks and semiconductor device elements, as well as cause the deterioration of performance of thin films as a result of generating splashes, abnormal discharges, particles and the like during the sputtering process.
Normally, platinum is recovered by dissolving platinum-containing scraps in acid such as aqua regia to eliminate residue, thereafter causing the acid with platinum dissolved therein and an ammonium chloride solution to react so as to precipitate/recover the product as ammonium hexachloroplatinate, and additionally roasting the ammonium hexachloroplatinate. 10005] A magnetic thin film containing platinum as its main component of the constituent elements or as a part of the constituent elements often contains ruthenium also as a part of the constituent elements. Since ruthenium is a platinum group element, in addition to the properties being similar, there is also the problem of platinum and ruthenium being difficult to separate.
Excluding special cases where the inclusion of ruthenium in platinum will not cause any particular problem to the material properties, unless platinum and ruthenium are separated, ruthenium will become an impurity. Since platinum itself is an extremely expensive material, platinum must be recovered at a high yield.
Several techniques for recovering platinum have been proposed in patent documents, and these are introduced below. However, it cannot be said that these patent documents offer an efficient recovery method for separating ruthenium from platinum and recovering high purity platinum.
[0006] Patent Document 1 below discloses, upon precipitating platinum as an ammonium chloride salt and extracting platinum, technology of adjusting the pH of a chioride-containing aqueous solution which contains gold and platinum group metals and performing two-stage neutralization and filtering to separate tellurium.
Patent Document 2 below discloses technology of eliminating ruthenium as an impurity by heating ammonium hexachloroplatinate or platinum to a high temperature in an oxygen gas airflow.
[0007] Patent Document 3 below discloses, upon separating ruthenium from a solution containing a platinum group via oxidation/distillation, technology of adjusting the pH of the solution, and thereafter using sodium bromate to transform ruthenium into ruthenium tetroxide and performing oxidation/distiliation thereto so as to
W02012/029379 3 PCT/JP2011/064096 separate/recover ruthenium.
Patent Document 4 below discloses, upon forming ammonium hexachloroplatinate, a method of producing a platinum powder by using a dispersion stabilization agent in an ammonium chloride solution to obtain fine ammonium hexachloroplatinate, and burning the ammonium hexachloroplatinate at a low temperature.
[0008] Patent Document 5 below discloses a high purity platinum recovery method including the steps of dissolving platinum-containing scraps in acid, thereafter causing the product to react with an ammonium chloride solution, 1} precipitating/recovering the product as ammonium hexachloroplatinate, and roasting the ammonium hexachloroplatinate to obtain a platinum sponge.
Patent Document 8 below describes technology of dissolving platinum- containing scraps in acid, thereafter causing the product to react with an ammonium chloride solution, precipitating/recovering the product as ammonium hexachloroplatinate, and thereafter recovering the platinum remaining in the liquid by using ion-exchange resin and activated carbon.
[0009] [Patent Document 1] Japanese Unexamined Patent Application Publication No. H10- 102156 [Patent Document 2] Japanese Unexamined Patent Application Publication No. 2006-183099 [Patent Document 3] Japanese Unexamined Patent Application Publication No. 2006-161096 [Patent Document 4] Japanese Unexamined Patent Application Publication No. 2008-106349 [Patent Document 5] Japanese Unexamined Patent Application Publication No. 2003-27154 [Patent Document 6] Japanese Unexamined Patent Application Publication No. 2003-129145
[Problems to be Solved by the Invention]
WQ2012/028379 4 PCT/JP2011/064096
[0010] Based on the above, the present invention provides a method of enabling recovery of high purity platinum as a resuit of efficiently eliminating cobalt, chromium, copper, iron, nickel, silicon and the like which become included in a platinum alloy used for sputtering particularly in a target scrap (spent target) containing platinum used for forming a magnetic thin film or in scraps such as mill ends, sawdust, and surface grinding scraps generated in the production process of such a target.
Especially, since it is possible to separate ruthenium contained in the platinum alloy scraps used for sputtering, recovery of high purity platinum which can be reused in platinum and a platinum-containing target can be achieved at a high yield and at a 14 low cost. [Means for Solving the Problems]
[0011] The present invention provides: 1) A high purity platinum recovery method including the steps of dissolving a platinum alloy containing ruthenium in aqua regia and eliminating residue, thereafter ia causing acid with platinum dissolved therein and an ammonium chloride solution to react so as to deposit chloroplatinic ammonium salt, and reducing the chloroplatinic ammonium salt to obtain a platinum sponge, wherein the acid with platinum dissolved therein and the ammonium chloride solution are caused to react at a temperature of 40°C or higher; 2) The high purity platinum recovery method according to 1) above, wherein a platinum concentration of a liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 15 g/L or more; and 3) The high purity platinum recovery method according to 1) or 2) above, wherein a ruthenium concentration of a liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 6 g/L or less.
[0012] The present invention additionally provides: 4) The high purity platinum recovery method according to any one of 1) to 3) above, wherein a ruthenium content as an impurity in the platinum sponge obtained by roasting the chloroplatinic ammonium salt is 2% or less; 5) The high purity platinum recovery method according to 4) above, wherein the ruthenium content is 1% or less; and 6) The high purity platinum recovery method according to any one of 1) to 5) above, wherein the platinum alloy containing ruthenium is a scrap of a magnetic
WO02012/029379 5 PCT/JP2011/064006 material target, and a platinum recovery rate from the scrap is 99% or higher. [Effect of the Invention]
[0013] The present invention yields a superior effect of being able to eliminate, with a relatively simple process, cobalt, chromium, copper, iron, nickel, silicon and the like which become included in a platinum-containing target scrap (spent target) for use in sputtering or in scraps such as mill ends, sawdust, and surface grinding scraps generated during the production process of such a target, and efficiently separate, from platinum, ruthenium as a platinum group element contained in the 1 magnetic material target.
[0014] The present invention foremost dissolves, in acid, scraps containing ih platinum and ruthenium and additionally containing cobalt, chromium, copper, iron, nickel, silicon and the like as impurity elements. Aqua regia is used as the acid for dissolving the scraps. While other acids can also be used for dissolving the scraps, for instance, if hydrochloric acid is used for dissolving the scraps, the dissolution will be incomplete. In addition, hydrogen will be generated; which is a possibility of hydrogen explosion.
Sufficient dissolution can be achieved by using aqua regia, and there is an advantage in that there is no danger of the hydrogen becoming diluted and exploding since nitrogen oxide and hydrogen are simultaneously generated during the dissolution. When aqua regia is used, while platinum will not dissolve easily at 2a first, platinum will gradually dissolve more easily.
[0015] After dissolving the platinum-containing scraps in acid, impurities such as tantalum oxide (Ta,0s) and boron oxide (BOs), as residue, are eliminated.
After eliminating the residue, caustic alkali such as sodium hydroxide (NaOH) is added to the solution containing platinum, the pH is adjusted to be 310 6 20 to achieve neutralization, cobalt, copper and the like are precipitated as hydroxide, and these are filtered and eliminated.
When the solution contains palladium, hydroxides of cobalt, copper and the like are precipitated and eliminated, and palladium is extracted via solvent
W02012/029379 5 PCT/JP2011/064006 extraction. After palladium is extracted, the exiracted palladium is subject to back extraction with ammonia, and the palladium-containing fluid is reduced with a reducing agent such as hydrazine so as to recover a high purity palladium sponge.
[0018] Subsequently, the acid with platinum dissolved therein and an ammonium chloride solution are caused to react so as to precipitate ammonium hexachloroplatinate ((NH,):PtCls) crystals. In the foregoing case, desirably, aqua regia that dissolved the platinum is added to the ammonium chloride solution.
Normally, common knowledge is to add an ammonium chloride solution to the aqua regia with platinum dissolved therein, but when this technique is adopted, 0 ammonium hexachloroplatinate becomes re-dissclved and cannot be deposited easily; thus phenomena are observed in that platinum remains in the solution and the yield of platinum deteriorates.
[0017] Accordingly, in order to increase the yield of platinum, it is important to add the aqua regia that dissolved the platinum to the ammonium chloride solution.
Subsequently, the ammonium hexachloroplatinate ((NHs).PtCle) crystals obtained as described above are roasted at 600 to 1000°C to obtain a high purity platinum sponge. Consequently, the yield of platinum reaches 97%, and high purity platinum can be recovered at a high yield with a relatively simple method. The foregoing process is a method that is disclosed in Patent Document 6 developed by
Nikko Materials, which is the name of the predecessor of the Applicant before the name change, and is an efficient recovery method for high purity platinum.
[0018] The problem is that the separation of ruthenium is not considered in the foregoing scraps. This is because the separation of ruthenium was not considered a major problem since the addition of ruthenium for forming a magnetic film or as a ¢5 constituent element of the target was not being conducted generally. Nevertheless, the separation of ruthenium is an urgent necessity under the current circumstances.
Meanwhile, since ruthenium is a platinum group element as described above, it cannot be separated from platinum easily. The present invention provides technology for easily and efficiently separating ruthenium from platinum.
[0019] The high purity platinum recovery method of the present invention includes the steps of dissolving a platinum alloy containing ruthenium in aqua regia and eliminating residue, thereafter causing acid with platinum dissolved therein and an ammonium chloride solution to react so as to deposit chloroplatinic ammonium
W02012/029379 7 PCT/JIP2011/064096 salt, and reducing the chloroplatinic ammonium salt fo obtain a platinum sponge, wherein the acid with platinum dissolved therein and the ammonium chloride solution are caused to react at a temperature of 40°C or higher.
While there is no particular limit in the upper limit of the temperature, it could be said that the temperature is preferably 100°C or less where the solution does not evaporate.
[0020] It could be said that, up to the process of obtaining the sponge, conventional technology may be used. Nevertheless, it is difficult to separate ruthenium, and the intended separation could not be realized. Nevertheless, by i raising the temperature by merely 10 to 20°C or so higher than ordinary temperature, the platinum recovery rate improved, and it became possible to reduce the content rate of ruthenium in the platinum salt. This was an extremely unexpected result. [0021) in other words, the technique of reducing the foregoing chloroplatinic ammonium salt and obtaining a platinum sponge is a relatively simple and efficient i5 production process, and the separation of ruthenium became possible as an extension of the foregoing technology.
While this may appear to be simple, as described above, it is difficult to anticipate this result, and a dramatic effect was obtained.
[0022] Moreover, with the high purity platinum recovery method of the present invention, preferably, the platinum concentration of the liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 15 g/L or more. This is because the solubility of the platinum salt will increase and the platinum recovery rate from scraps will deteriorate (to less than 99%), if the platinum concentration is reduced to less than 15 g/L.
The platinum content rate in the scraps is usually 30 wt% or higher, and, when the scraps are dissolved in aqua regia under normal conditions, the platinum concentration in the solution becomes a concentration that becomes considerably greater than 15 g/L; the concentration will not fall below 15 g/L unless the product is diluted in a large volume of water. However, in cases where the ruthenium content rate is high and the platinum content rate is relatively low, and the concentration will fall below 15 g/L as is, it will suffice to mix the scraps with scraps having a high platinum content rate and dissolve the scraps in aqua regia.
[0023] With the high purity platinum recovery method of the present invention,
WQ2012/029379 8 PCT/JP2011/064096 preferably, the ruthenium concentration of the liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 6 g/L or less. in addition to the foregoing reaction temperature being affected, this is because ruthenium tends to easily enter into the deposit when the ruthenium concentration exceeds 6 g/L. In order to lower the ruthenium concentration, dilution with water will suffice. Nevertheless, mutual adjustment is required since dilution will contrarily lower the platinum concentration of the liquid.
[0024] Based on the above, the high purity platinum recovery method of the present invention can cause the ruthenium content as an impurity in the platinum sponge, which is obtained by roasting the chloroplatinic ammonium salt, to be 2% or less, and even 1% or less. In addition, the present invention can achieve a platinum recovery rate of 99% or higher from scraps of a magnetic material target containing a platinum alloy containing ruthenium. The present invention provides this kind of high purity platinum recovery method.
[0028] [Examples]
The present invention is now explained based on the following Examples.
Note that these Examples are described for facilitating the understanding of the present invention, and the present invention is not limited by the Examples. in other words, the present invention is only limited by the ensuing patent claims and the technical concept described in this specification.
[0026] (Example 1)
In Example 1, scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were dissolved in aqua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having a platinum concentration of 30 g/L and a ruthenium concentration of 5 g/L.
The aqua regia solution and ammonium chloride were caused fo react at 45°C to obtain chloroplatinic ammonium salt ((NH.),PtCls) crystals. Subsequently, a0 the crystals were roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured. The results are shown in Table 1.
WO02012/029379 9 PCT/IP2011/064096 [Table 1] platinum recovery rate ruthenium content rate
CC %) | in the platinum salt (wt%) — Example 1 i 995 05
Example 3 99.2 17 = 0.6 ”
Comparative Example 2 _ 99.5 ER 2.3
[0028] As shown in Table 1, the platinum recovery rate reached 99.5%, and the ruthenium content rate in the platinum salt decreased to 0.5 wt%. This ruthenium content was sufficiently decreased to use the recycled platinum as a target.
Moreover, similar platinum purity and ruthenium reduction could be achieved as long as the reaction temperature of the aqua regia solution and ammonium chloride was 40°C or higher. Note that there is no particular limitation to the roast temperature and may be adjusted as needed, and the temperature capable of normally obtaining a platinum sponge may be arbitrarily selected; hereinafter the same.
[0029] (Example 2) in Example 2, scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were dissolved in aqua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having a platinum concentration of 18 g/L and a ruthenium concentration of 3 g/L.
The aqua regia solution and ammonium chloride were caused to react at 80°C to deposit chloroplatinic ammonium salt, and the deposited chloroplatinic ammonium salt was roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured. The results are shown in Table 1. 10030} As shown in Table 1, the platinum recovery rate reached 98.3 %, and the ruthenium content rate in the platinum salt decreased to 0.3 wi%. This ruthenium content was sufficiently decreased fo use the recycled platinum as a target.
Moreover, similar platinum purity and ruthenium reduction could be achieved so as long as the reaction temperature of the aqua regia solution and ammonium chloride
WQ2012/029379 10 PCT/JP2011/064086 was 40°C or higher.
[0031] (Example 3) in Example 3, scraps of a magnetic material target containing platinum, & cobalt, chromium, and ruthenium were dissolved in aqua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having a platinum concentration of 16 g/L and a ruthenium concentration of 5 g/l.
The aqua regia solution and ammonium chloride were caused to react at 1 50°C to deposit chloroplatinic ammonium salt, and the deposited chloroplatinic ammonium salt was roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured. The results are shown in Table 1.
[0032] As shown in Table 1, the platinum recovery rate reached 99.2 %, and the ruthenium content rate in the platinum salt decreased to 1.7 wi%. This ruthenium content was sufficiently decreased to use the recycled platinum as a target.
Moreover, similar platinum purity and ruthenium reduction could be achieved so as long as the reaction temperature of the aqua regia solution and ammonium chloride was 40°C or higher.
[0033] (Comparative Example 1)
Scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were dissolved in aqua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having 2h a platinum concentration of 12 g/L. and a ruthenium concentration of 2 g/L. In the foregoing case, the platinum concentration was low and lower than the 15 g/L of the present invention.
The aqua regia solution and ammonium chloride were caused to react at 70°C to deposit chloroplatinic ammonium salt, and the deposited chioroplatinic ammonium salt was roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured.
[0034] The results are shown in Table 1. As shown in Table 1, the ruthenium
WQ02012/029379 » PCT/JP2011/064096 content rate in the platinum salt decreased to 0.6 wi% and the ruthenium content satisfied the conditions of the object of the present invention, but the platinum recovery rate deteriorated to 96.0%. It was confirmed that a low platinum concentration is unfavorable since it deteriorates the platinum recovery rate.
[0035] (Comparative Example 2)
Scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were dissolved in agua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having 14 a platinum concentration of 48 g/L. and a ruthenium concentration of 8 g/L. In the foregoing case, the ruthenium concentration exceeded 6 g/L, which is the upper limit of the present invention.
The aqua regia solution and ammonium chloride were caused to react at 70°C to deposit chloroplatinic ammonium salt, and the deposited chloroplatinic ammonium salt was roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured.
[0036] The results are shown in Table 1. As shown in Table 1, while the platinum recovery rate was high at 99.5%, the ruthenium content rate in the platinum 24 salt increased to 2.3 wi%. It was confirmed that a high ruthenium concentration in the aqua regia solution is unfavorable.
[0037] (Comparative Example 3)
Scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were dissolved in aqua regia and residue was eliminated, and the resulting product was diluted in water to obtain an aqua regia solution having a platinum concentration of 30 g/L and a ruthenium concentration of 5 g/l. The aqua regia solution and ammonium chloride were caused to react at 30°C to deposit chioroplatinic ammonium salt, and the deposited chloroplatinic ammonium salt was 50 roasted at 800°C to obtain a platinum sponge, and the platinum recovery rate from the aqua regia solution and the ruthenium content rate as an impurity were measured.
In the foregoing case, the temperature for causing the aqua regia solution and ammonium chloride to react did not satisfy 40°C or higher, which is a condition of the
WQ2012/029379 + PCT/JP2011/0684086 present invention.
[0038] The results are shown in Table 1. As shown in Table 1, while the platinum recovery rate was high at 99.2%, the ruthenium content rate in the platinum salt increased to 3.5 wt%. It was confirmed that a low temperature for causing the aqua regia solution and ammonium chloride to react is unfavorable since it increases the ruthenium content.
[0039] Accordingly, in addition to platinum, cobalt, chromium, and ruthenium as the magnetic materials as scraps, it was possible to eliminate most of the numerous other impurities such as copper, iron, nickel, silicon and the like that result from the mill ends, sawdust, and surface grinding scraps arising during the production process of a target containing platinum, and the platinum yield of obtaining high purity platinum reached 99%.
Moreover, it was also possible to yield an effect of being able to reduce ruthenium, which is difficult to separate from platinum.
In the foregoing description, while scraps of a magnetic material target containing platinum, cobalt, chromium, and ruthenium were used for explaining the present invention, the present invention can be similarly applied to scraps containing other impurities. [Industrial Applicability]
[0040] The present invention yields a superior effect of being able to eliminate, with a relatively simple process, cobalt, chromium, copper, iron, nickel, silicon and the like which become included in scraps such as mill ends, sawdust, and surface grinding scraps generated during the production process of a platinum and platinum- containing target for use in sputtering, and recover, at a high yield, high purity platinum that can be reused as platinum or as a target containing platinum.
Moreover, since the present invention also yields an effect of being able to reduce ruthenium, which is said to be difficult to separate from platinum, using a relatively simple method, the present invention can provide a method that is useful for recovering high purity platinum at a low cost and at a high yield.
Claims (6)
1. A high purity platinum recovery method including the steps of dissolving a platinum alloy containing ruthenium in aqua regia and eliminating residue, thereafter causing acid with platinum dissolved therein and an ammonium chloride solution to react so as to deposit chloroplatinic ammonium salt, and reducing the chloroplatinic ammonium salt to obtain a platinum sponge, wherein the acid with platinum dissolved therein and the ammonium chloride solution are caused to react at a temperature of 40°C or higher.
2. The high purity platinum recovery method according to claim 1, wherein a platinum concentration of a liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 15 g/L or more.
3. The high purity platinum recovery method according to claim 1 or claim 2, wherein a ruthenium concentration of a liquid resulting from dissolving the platinum alloy containing ruthenium in the aqua regia is 6 g/L or less.
4. The high purity platinum recovery method according to any one of claims 1 to 3, wherein a ruthenium content as an impurity in the platinum sponge obtained by roasting the chloroplatinic ammonium salt is 2% or less.
5. The high purity platinum recovery method according to claim 4, wherein the ruthenium content is 1% or less.
6. The high purity platinum recovery method according to any one of claims 1 to 5, wherein the platinum alloy containing ruthenium is a scrap of a magnetic material target, and a platinum recovery rate from the scrap is 99% or higher.
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DE102013203743A1 (en) * | 2013-03-05 | 2014-09-11 | Heraeus Precious Metals Gmbh & Co. Kg | Process for the preparation of high purity platinum powder and platinum powder obtainable by this process and use |
CN103627902B (en) * | 2013-04-25 | 2015-12-23 | 上海派特贵金属环保科技有限公司 | A kind of method reclaiming rhodium from inactive noble metal catalyst |
FR3026110B1 (en) * | 2014-09-24 | 2016-11-18 | Commissariat Energie Atomique | PROCESS FOR RECOVERING THE PLATINUM PRESENT IN A MEMBRANE-ELECTRODE ASSEMBLY |
TWI623623B (en) * | 2017-04-17 | 2018-05-11 | 國立中山大學 | Treating method for recycling noble metal |
DE102019217188A1 (en) * | 2019-11-07 | 2021-05-12 | Robert Bosch Gmbh | Process for the extraction of platinum and / or ruthenium |
CN110964912A (en) * | 2019-12-20 | 2020-04-07 | 有研亿金新材料有限公司 | Method for recovering and purifying platinum from platinum-tungsten alloy |
CN111676371A (en) * | 2020-04-27 | 2020-09-18 | 励福(江门)环保科技股份有限公司 | Method for separating and purifying platinum from tungsten crucible |
CN111690819A (en) * | 2020-06-24 | 2020-09-22 | 广东金正龙科技有限公司 | Platinum purification method and reaction kettle |
CN111926195B (en) * | 2020-06-24 | 2022-03-08 | 重庆材料研究院有限公司 | Method for preparing high-purity platinum powder from platinum alloy waste |
CN112126789A (en) * | 2020-09-17 | 2020-12-25 | 朱俊 | Chloroplatinic acid solution concentration process and equipment |
CN115125398A (en) * | 2022-08-09 | 2022-09-30 | 顾秀华 | Preparation process of semi-metallic compound of metal platinum |
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JP3079034B2 (en) * | 1996-05-27 | 2000-08-21 | 日鉱金属株式会社 | How to recover platinum |
JP4865156B2 (en) * | 2001-07-18 | 2012-02-01 | Jx日鉱日石金属株式会社 | Method for recovering high-purity platinum and palladium |
JP2003129145A (en) * | 2001-10-22 | 2003-05-08 | Nikko Materials Co Ltd | Method for recovering platinum |
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JP5327420B2 (en) * | 2007-12-12 | 2013-10-30 | 三菱マテリアル株式会社 | Platinum recovery method |
CN101358287A (en) * | 2008-09-10 | 2009-02-04 | 灵宝市金源矿业有限责任公司 | Separation method of gold, silver and platinum metals from refractory alloy gold |
JP5408412B2 (en) * | 2009-03-20 | 2014-02-05 | 三菱マテリアル株式会社 | Platinum recovery process |
JP5339068B2 (en) * | 2009-03-20 | 2013-11-13 | 三菱マテリアル株式会社 | Ruthenium purification and recovery method |
CN101797649B (en) * | 2010-01-19 | 2012-09-05 | 兰州大学 | Method and device for preparing high-purity ruthenium |
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CN102959103A (en) | 2013-03-06 |
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