JP6673756B2 - Method of manufacturing or collecting single substance - Google Patents
Method of manufacturing or collecting single substance Download PDFInfo
- Publication number
- JP6673756B2 JP6673756B2 JP2016117710A JP2016117710A JP6673756B2 JP 6673756 B2 JP6673756 B2 JP 6673756B2 JP 2016117710 A JP2016117710 A JP 2016117710A JP 2016117710 A JP2016117710 A JP 2016117710A JP 6673756 B2 JP6673756 B2 JP 6673756B2
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- Japan
- Prior art keywords
- compound
- flask
- gold
- dissolved
- aqueous solution
- Prior art date
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- 239000000126 substance Substances 0.000 title claims description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 49
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- 239000002904 solvent Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 11
- VDCSGNNYCFPWFK-UHFFFAOYSA-N diphenylsilane Chemical compound C=1C=CC=CC=1[SiH2]C1=CC=CC=C1 VDCSGNNYCFPWFK-UHFFFAOYSA-N 0.000 claims description 8
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 claims description 6
- 230000001603 reducing effect Effects 0.000 claims description 6
- APRDARTZFVUGQN-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5-decakis-phenylpentasilolane Chemical compound C1=CC=CC=C1[Si]1(C=2C=CC=CC=2)[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 APRDARTZFVUGQN-UHFFFAOYSA-N 0.000 claims description 5
- DHUSVFRVDIOOKD-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5-decamethylhexasilinane Chemical compound C[Si]1(C)[SiH2][Si](C)(C)[Si](C)(C)[Si](C)(C)[Si]1(C)C DHUSVFRVDIOOKD-UHFFFAOYSA-N 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims 1
- 239000004305 biphenyl Substances 0.000 claims 1
- 125000006267 biphenyl group Chemical group 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 description 59
- 229910052737 gold Inorganic materials 0.000 description 54
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 53
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 39
- 239000000843 powder Substances 0.000 description 38
- 238000006722 reduction reaction Methods 0.000 description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 36
- 238000011084 recovery Methods 0.000 description 27
- 239000002253 acid Substances 0.000 description 21
- 206010065042 Immune reconstitution inflammatory syndrome Diseases 0.000 description 19
- QCAWEPFNJXQPAN-UHFFFAOYSA-N methoxyfenozide Chemical compound COC1=CC=CC(C(=O)NN(C(=O)C=2C=C(C)C=C(C)C=2)C(C)(C)C)=C1C QCAWEPFNJXQPAN-UHFFFAOYSA-N 0.000 description 19
- RTCLHEHPUHREBC-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6-dodecamethylhexasilinane Chemical compound C[Si]1(C)[Si](C)(C)[Si](C)(C)[Si](C)(C)[Si](C)(C)[Si]1(C)C RTCLHEHPUHREBC-UHFFFAOYSA-N 0.000 description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 13
- 125000000217 alkyl group Chemical group 0.000 description 10
- 125000003118 aryl group Chemical group 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 239000010948 rhodium Substances 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 229910052703 rhodium Inorganic materials 0.000 description 5
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 4
- XJWOWXZSFTXJEX-UHFFFAOYSA-N phenylsilicon Chemical compound [Si]C1=CC=CC=C1 XJWOWXZSFTXJEX-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 150000002344 gold compounds Chemical class 0.000 description 3
- 150000003058 platinum compounds Chemical class 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- -1 technetium ion Chemical class 0.000 description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910021606 Palladium(II) iodide Inorganic materials 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- WRYNUJYAXVDTCB-UHFFFAOYSA-M acetyloxymercury Chemical compound CC(=O)O[Hg] WRYNUJYAXVDTCB-UHFFFAOYSA-M 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N bismuth(III) nitrate Inorganic materials [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- QTMDXZNDVAMKGV-UHFFFAOYSA-L copper(ii) bromide Chemical compound [Cu+2].[Br-].[Br-] QTMDXZNDVAMKGV-UHFFFAOYSA-L 0.000 description 2
- ORMNPSYMZOGSSV-UHFFFAOYSA-N dinitrooxymercury Chemical compound [Hg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ORMNPSYMZOGSSV-UHFFFAOYSA-N 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 150000002504 iridium compounds Chemical class 0.000 description 2
- 229940100892 mercury compound Drugs 0.000 description 2
- 150000002731 mercury compounds Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 229910052762 osmium Inorganic materials 0.000 description 2
- 150000002908 osmium compounds Chemical class 0.000 description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 2
- HNNUTDROYPGBMR-UHFFFAOYSA-L palladium(ii) iodide Chemical compound [Pd+2].[I-].[I-] HNNUTDROYPGBMR-UHFFFAOYSA-L 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 125000003367 polycyclic group Chemical group 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000003586 protic polar solvent Substances 0.000 description 2
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 2
- 150000003304 ruthenium compounds Chemical class 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 2
- 229940071536 silver acetate Drugs 0.000 description 2
- 229940100890 silver compound Drugs 0.000 description 2
- 150000003379 silver compounds Chemical class 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052713 technetium Inorganic materials 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 150000003498 tellurium compounds Chemical class 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- 125000001637 1-naphthyl group Chemical group [H]C1=C([H])C([H])=C2C(*)=C([H])C([H])=C([H])C2=C1[H] 0.000 description 1
- 125000001622 2-naphthyl group Chemical group [H]C1=C([H])C([H])=C2C([H])=C(*)C([H])=C([H])C2=C1[H] 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- 229910021589 Copper(I) bromide Inorganic materials 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910021595 Copper(I) iodide Inorganic materials 0.000 description 1
- 229910021590 Copper(II) bromide Inorganic materials 0.000 description 1
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 229910003767 Gold(III) bromide Inorganic materials 0.000 description 1
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021638 Iridium(III) chloride Inorganic materials 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910021604 Rhodium(III) chloride Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- BMSYAGRCQOYYMZ-UHFFFAOYSA-N [As].[As] Chemical compound [As].[As] BMSYAGRCQOYYMZ-UHFFFAOYSA-N 0.000 description 1
- MBQYUMXAJCFWGL-UHFFFAOYSA-N [Na+].[Pt+4] Chemical compound [Na+].[Pt+4] MBQYUMXAJCFWGL-UHFFFAOYSA-N 0.000 description 1
- 229940045985 antineoplastic platinum compound Drugs 0.000 description 1
- 125000000223 arsonoyl group Chemical group [H][As](*)(*)=O 0.000 description 1
- 125000003828 azulenyl group Chemical group 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- CZKMPDNXOGQMFW-UHFFFAOYSA-N chloro(triethyl)germane Chemical compound CC[Ge](Cl)(CC)CC CZKMPDNXOGQMFW-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- RFKZUAOAYVHBOY-UHFFFAOYSA-M copper(1+);acetate Chemical compound [Cu+].CC([O-])=O RFKZUAOAYVHBOY-UHFFFAOYSA-M 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 description 1
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 description 1
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 1
- 125000006165 cyclic alkyl group Chemical group 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 125000001995 cyclobutyl group Chemical group [H]C1([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000001559 cyclopropyl group Chemical group [H]C1([H])C([H])([H])C1([H])* 0.000 description 1
- 150000001354 dialkyl silanes Chemical class 0.000 description 1
- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical class [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 description 1
- SRRYZMQPLOIHRP-UHFFFAOYSA-L dipotassium;tellurate Chemical compound [K+].[K+].[O-][Te]([O-])(=O)=O SRRYZMQPLOIHRP-UHFFFAOYSA-L 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000002291 germanium compounds Chemical class 0.000 description 1
- OVWPJGBVJCTEBJ-UHFFFAOYSA-K gold tribromide Chemical compound Br[Au](Br)Br OVWPJGBVJCTEBJ-UHFFFAOYSA-K 0.000 description 1
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- 125000003392 indanyl group Chemical group C1(CCC2=CC=CC=C12)* 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002497 iodine compounds Chemical class 0.000 description 1
- HTFVQFACYFEXPR-UHFFFAOYSA-K iridium(3+);tribromide Chemical compound Br[Ir](Br)Br HTFVQFACYFEXPR-UHFFFAOYSA-K 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 229910001987 mercury nitrate Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- NALMPLUMOWIVJC-UHFFFAOYSA-N n,n,4-trimethylbenzeneamine oxide Chemical compound CC1=CC=C([N+](C)(C)[O-])C=C1 NALMPLUMOWIVJC-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- DRXYRSRECMWYAV-UHFFFAOYSA-N nitrooxymercury Chemical compound [Hg+].[O-][N+]([O-])=O DRXYRSRECMWYAV-UHFFFAOYSA-N 0.000 description 1
- 150000002941 palladium compounds Chemical class 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- HZEBHPIOVYHPMT-UHFFFAOYSA-N polonium atom Chemical compound [Po] HZEBHPIOVYHPMT-UHFFFAOYSA-N 0.000 description 1
- 150000003069 polonium compounds Chemical class 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 239000001230 potassium iodate Substances 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
- 229940093930 potassium iodate Drugs 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003284 rhodium compounds Chemical class 0.000 description 1
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- JUDUFOKGIZUSFP-UHFFFAOYSA-M silver;4-methylbenzenesulfonate Chemical compound [Ag+].CC1=CC=C(S([O-])(=O)=O)C=C1 JUDUFOKGIZUSFP-UHFFFAOYSA-M 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011697 sodium iodate Substances 0.000 description 1
- 235000015281 sodium iodate Nutrition 0.000 description 1
- 229940032753 sodium iodate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- GKLVYJBZJHMRIY-UHFFFAOYSA-N technetium atom Chemical compound [Tc] GKLVYJBZJHMRIY-UHFFFAOYSA-N 0.000 description 1
- 150000003496 technetium compounds Chemical class 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229940071240 tetrachloroaurate Drugs 0.000 description 1
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 description 1
- QFJIELFEXWAVLU-UHFFFAOYSA-H tetrachloroplatinum(2+) dichloride Chemical compound Cl[Pt](Cl)(Cl)(Cl)(Cl)Cl QFJIELFEXWAVLU-UHFFFAOYSA-H 0.000 description 1
- 125000005329 tetralinyl group Chemical group C1(CCCC2=CC=CC=C12)* 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003799 water insoluble solvent Substances 0.000 description 1
Classifications
-
- 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
Description
本発明は、単体を製造若しくは回収する方法に関する。より詳細に、本発明は、単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物から単体を製造する方法若しくは前記化合物を含有する水溶液から単体を回収する方法に関する。 The present invention relates to a method for producing or recovering a simple substance. More specifically, the present invention provides a method for producing a simple substance from a water-soluble compound in which a standard electrode potential in a reduction half reaction for producing a simple substance is higher than a potential of a standard hydrogen electrode, or a simple substance from an aqueous solution containing the compound. And a method for collecting the same.
ポリシランは金属イオンの還元能を持つことが知られている(非特許文献1)。また、ポリシランの層をAu、Ag、Pt、Pd等の金属イオンの還元剤として利用して金属層を形成できることが知られている(非特許文献2)。
特許文献1は、標準電極電位が0Vよりも大きい元素のイオンをプロトン性溶媒に溶解してなる溶液と、前記プロトン性溶媒に対して難溶性のポリシランとを混合して、標準電極電位が0Vよりも大きい元素のイオンから、該元素の粒子を製造する方法を開示している。この方法で得られる粒子はポリシランに吸着して複合体を形成する。
特許文献2は、親水性ポリマーとポリシランとのブロック共重合体から得られる前記ポリシランをミセル内面に有し、該ミセルのシェル部が架橋されている親水性ミセルを用い金属イオンを該ミセルを還元剤として還元することにより該金属の単分散微粒子を調製する方法を開示している。
It is known that polysilane has the ability to reduce metal ions (Non-Patent Document 1). It is also known that a metal layer can be formed using a polysilane layer as a reducing agent for metal ions such as Au, Ag, Pt, and Pd (Non-Patent Document 2).
Patent Literature 1 discloses that a solution obtained by dissolving an ion of an element having a standard electrode potential higher than 0 V in a protic solvent and a polysilane that is hardly soluble in the protic solvent are mixed to obtain a standard electrode potential of 0 V. A method is disclosed for producing particles of an element from ions of a larger element. The particles obtained by this method adsorb to the polysilane to form a complex.
Patent Document 2 discloses that a polysilane obtained from a block copolymer of a hydrophilic polymer and a polysilane is provided on the inner surface of a micelle, and the micelle is reduced by a hydrophilic micelle in which a shell portion of the micelle is crosslinked. It discloses a method for preparing monodispersed fine particles of the metal by reduction as an agent.
本発明の目的は、単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物から単体を高効率で製造する方法若しくは前記化合物を含有する水溶液から単体を高効率で回収する方法を提供することである。 An object of the present invention is to provide a method for producing a simple substance from a water-soluble compound in which the standard electrode potential in the reduction half reaction for producing the simple substance is higher than the potential of the standard hydrogen electrode, or from an aqueous solution containing the compound. An object of the present invention is to provide a method for recovering a simple substance with high efficiency.
本発明は以下の形態を包含する。 The present invention includes the following embodiments.
〔1〕 水および水に非相溶な溶媒からなる不均一液媒体中にて、
水に難溶で且つ水に非相溶な溶媒に可溶なポリシランの存在下に、
単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物を還元することを含む、前記化合物から単体を製造する方法。
[1] In a heterogeneous liquid medium comprising water and a solvent immiscible with water,
In the presence of polysilane that is hardly soluble in water and soluble in a solvent that is incompatible with water,
A method for producing a simple substance from said compound, comprising reducing a compound soluble in water, wherein a standard electrode potential in a reduction half reaction for producing a simple substance is higher than a potential of a standard hydrogen electrode.
〔2〕 単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物を含有する水溶液と、水に非相溶な溶媒と、水に難溶で且つ水に非相溶な溶媒に可溶なポリシランとを含有する不均一反応液を得、
該反応液において前記化合物を還元することを含む、
前記化合物を含有する水溶液から単体を回収する方法。
[2] The standard electrode potential in the reduction half-reaction for forming a simple substance is higher than the potential of the standard hydrogen electrode and contains an aqueous solution containing a compound soluble in water, a solvent incompatible with water, and a water-insoluble solvent. And to obtain a heterogeneous reaction solution containing a polysilane soluble in a solvent incompatible with water,
Reducing the compound in the reaction solution.
A method for recovering a simple substance from an aqueous solution containing the compound.
本発明に係る方法にしたがって、単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物を不均一液媒体中でポリシランを用いて還元すると、生成した単体がポリシランや他の物質に吸着しないので、ポリシランを用いた従来の還元法に比べて効率的に単体を製造若しくは回収することができる。 According to the method of the present invention, when the standard electrode potential in the reduction half-reaction for producing a simple substance is higher than the potential of the standard hydrogen electrode and a compound soluble in water is reduced using polysilane in a heterogeneous liquid medium, Since the obtained simple substance does not adsorb to polysilane or other substances, the simple substance can be produced or recovered more efficiently than the conventional reduction method using polysilane.
本発明は、以下に述べる化合物(基質)から単体を製造する方法、または該化合物(基質)を含有する水溶液から単体を回収する方法である。 The present invention is a method for producing a simple substance from a compound (substrate) described below, or a method for recovering a simple substance from an aqueous solution containing the compound (substrate).
本発明において用いられる化合物(基質)は、水に可溶な化合物である。該化合物(基質)の水への溶解度は、好ましくは0.001質量%以上、より好ましくは0.1質量%以上である。
本発明において用いられる化合物(基質)は、単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きい化合物、好ましくは前記標準電極電位が標準水素電極の電位よりも0.2V以上大きい化合物、より好ましくは前記標準電極電位が標準水素電極の電位よりも0.7V以上大きい化合物である。標準電極電位は、標準水素電極と測定対象化学種の電極を組み合わせて作製された電池の標準状態における起電力(emf)と等しい。
The compound (substrate) used in the present invention is a compound that is soluble in water. The solubility of the compound (substrate) in water is preferably 0.001% by mass or more, more preferably 0.1% by mass or more.
The compound (substrate) used in the present invention is a compound having a standard electrode potential higher than the potential of the standard hydrogen electrode in the reduction half reaction for producing a simple substance, preferably the standard electrode potential is 0.2 V higher than the potential of the standard hydrogen electrode. A compound having a larger potential than the above, more preferably a compound whose standard electrode potential is 0.7 V or more higher than the potential of the standard hydrogen electrode. The standard electrode potential is equal to an electromotive force (emf) in a standard state of a battery prepared by combining a standard hydrogen electrode and an electrode of a chemical species to be measured.
本発明において用いられる化合物(基質)の具体例としては、
(銅)
Cu2++2e-=Cu(E*(25℃)=0.340V)で表される還元半反応を引き起こす銅化合物(酢酸銅(II)、臭化銅(II)、塩化銅(II)、ヨウ化銅(II)、硝酸銅(II)、ビス(2,4−ペンタンジオネート)銅(II)など)、
Cu++e-=Cu(E*(25℃)=0.520V)で表される還元半反応を引き起こす銅化合物(例えば、酢酸銅(I)、臭化銅(I)、塩化銅(I)、ヨウ化銅(I)など)、
Specific examples of the compound (substrate) used in the present invention include:
(copper)
Copper compounds (copper (II) acetate, copper (II) bromide, copper (II) chloride, etc.) which cause a reduction half reaction represented by Cu 2+ + 2e − = Cu (E * (25 ° C.) = 0.340 V); Copper (II) iodide, copper (II) nitrate, bis (2,4-pentanedionate) copper (II), etc.),
A copper compound (for example, copper (I) acetate, copper (I) bromide, copper (I) chloride) that causes a reduction half reaction represented by Cu + + e − = Cu (E * (25 ° C.) = 0.520 V) , Copper (I) iodide),
(ルテニウム)
RuO2+4H++4e-=Ru+2H2O(E*(25℃)=0.68V)で表される還元半反応を引き起こすルテニウム化合物(酸化ルテニウム(IV))、
RuO4+4H++4e-=RuO2+H2O(E*(25℃)=1.387V)で表される還元半反応を引き起こすルテニウム化合物(酸化ルテニウム(VIII))、
(ruthenium)
A ruthenium compound (ruthenium (IV) oxide) that causes a reduction half reaction represented by RuO 2 + 4H + + 4e − = Ru + 2H 2 O (E * (25 ° C.) = 0.68 V);
A ruthenium compound (ruthenium oxide (VIII)) that causes a reduction half reaction represented by RuO 4 + 4H + + 4e − = RuO 2 + H 2 O (E * (25 ° C.) = 1.387 V);
(テクネチウム)
Tc2++2e-=Tc(E*(25℃)=0.400V)で表される還元半反応を引き起こすテクネチウム化合物(テクネチウムイオン)、
(technetium)
A technetium compound (technetium ion) that causes a reduction half reaction represented by Tc 2+ + 2e − = Tc (E * (25 ° C.) = 0.400 V);
(テルル)
TeO2+4H++4e-=Te+2H2O(E*(25℃)=0.521V)で表される還元半反応を引き起こすテルル化合物(酸化テルル(IV))、
H2TeO4+6H++2e-=Te4++2H2O(E*(25℃)=0.926V)で表される還元半反応を引き起こすテルル化合物(テルル酸ナトリウム(VI)、テルル酸カリウム(VI))
(tellurium)
A tellurium compound (tellurium (IV) oxide) that causes a reduction half reaction represented by TeO 2 + 4H + + 4e − = Te + 2H 2 O (E * (25 ° C.) = 0.521 V);
H 2 TeO 4 + 6H + + 2e − = Te 4+ + 2H 2 O (E * (25 ° C.) = 0.926 V) tellurium compound (sodium (VI) tellurium, potassium tellurate (VI) VI))
(ロジウム)
Rh3++3e-=Rh(E*(25℃)=0.758V)で表される還元半反応を引き起こすロジウム化合物(塩化ロジウム(III)、硝酸ロジウム(III))、
(rhodium)
A rhodium compound (rhodium (III) chloride, rhodium (III) nitrate) which causes a reduction half reaction represented by Rh 3+ + 3e − = Rh (E * (25 ° C.) = 0.758 V);
(パラジウム)
Pd2++2e-=Pd(E*(25℃)=0.915V)で表される還元半反応を引き起こすパラジウム化合物(酢酸パラジウム(II)、硝酸パラジウム(II)、塩化パラジウム(II)、臭化パラジウム(II)、ヨウ化パラジウム(II))、
(palladium)
Palladium compound (palladium acetate (II), palladium (II) nitrate, palladium (II) chloride, palladium (II), which causes a reduction half reaction represented by Pd 2+ + 2e − = Pd (E * (25 ° C.) = 0.915 V) Palladium (II) iodide, palladium (II) iodide),
(銀)
Ag++e-=Ag(E*(25℃)=0.799V)で表される還元半反応を引き起こす銀化合物(酢酸銀(I)、硝酸銀(I)、トリフルオロメタンスルホン酸銀(I)、p−トルエンスルホン酸銀(I))、
[Ag(NH3)2]++e-=Ag+2NH3(E*(25℃)=0.373V)で表される還元半反応を引き起こす銀化合物(塩化ジアンミン銀(I))、
(Silver)
Ag + + e − = Ag (E * (25 ° C.) = 0.799 V) A silver compound (silver acetate (I), silver nitrate (I), silver trifluoromethanesulfonate (I), silver (I) p-toluenesulfonate),
A silver compound (silver diammine chloride (I)) that causes a reduction half-reaction represented by [Ag (NH 3 ) 2 ] + + e − = Ag + 2NH 3 (E * (25 ° C.) = 0.373 V);
(オスミウム)
OsO2+4H++4e-=Os+2H2O(E*(25℃)=0.687V)で表される還元半反応を引き起こすオスミウム化合物、
OsO4+8H++8e-=Os+4H2O(E*(25℃)=0.84V)で表される還元半反応を引き起こすオスミウム化合物(酸化オスミウム(VIII))
(osmium)
An osmium compound which causes a reduction half reaction represented by OsO 2 + 4H + + 4e − = Os + 2H 2 O (E * (25 ° C.) = 0.687 V);
Osmium compound (osmium (VIII) oxide) that causes a reduction half reaction represented by OsO 4 + 8H + + 8e − = Os + 4H 2 O (E * (25 ° C.) = 0.84 V)
(白金)
Pt2++2e-=Pt(E*(25℃)=1.188V)で表される還元半反応を引き起こす白金化合物(塩化白金(II))
[PtCl6]4-+2e-=[PtCl4]2-+2Cl-(E*(25℃)=0.726V)で表される還元半反応を引き起こす白金化合物(ヘキサクロロ白金(IV)酸カリウム、ヘキサクロロ白金(IV)酸ナトリウム、ヘキサクロロ白金(IV)酸(=塩化白金(IV)の塩酸溶液))
[PtCl4]2-+2e-=Pt+4Cl-(E*(25℃)=0.758V)で表される還元半反応を引き起こす白金化合物(テトラクロロ白金(II)酸カリウム)
(platinum)
Pt 2+ + 2e − = Pt (E * (25 ° C.) = 1.188 V) Platinum compound (platinum (II) chloride) which causes a reduction half reaction
Platinum compounds (potassium hexachloroplatinate (IV), hexachloroplatinum) that cause a reduction half-reaction represented by [PtCl 6 ] 4- + 2e − = [PtCl 4 ] 2- + 2Cl − (E * (25 ° C.) = 0.726 V) Sodium platinum (IV) acid, hexachloroplatinic (IV) acid (= platinum (IV) chloride solution in hydrochloric acid)
A platinum compound (potassium tetrachloroplatinate (II)) which causes a reduction half-reaction represented by [PtCl 4 ] 2- + 2e − = Pt + 4Cl − (E * (25 ° C.) = 0.758 V)
(イリジウム)
[IrCl6]3-+3e-=Ir+6Cl-(E*(25℃)=0.86V)で表される還元半反応を引き起こすイリジウム化合物
Ir3++3e-=Ir(E*(25℃)=1.156V)で表される還元半反応を引き起こすイリジウム化合物(塩化イリジウム(III)、臭化イリジウム(III))
(iridium)
[IrCl 6 ] 3- + 3e − = Ir + 6Cl − (E * (25 ° C.) = 0.86 V) An iridium compound that causes a reduction half reaction Ir 3+ + 3e − = Ir (E * (25 ° C.) = 1) Iridium compound (iridium (III) chloride, iridium (III) bromide) which causes a reduction half reaction represented by .156V)
(金)
[AuCl4]-+3e-=Au+4Cl-(E*(25℃)=1.002V)で表される還元半反応を引き起こす金化合物(テトラクロロ金(III)酸)、
Au3++3e-=Au(E*(25℃)=1.52V)で表される還元半反応を引き起こす金化合物(塩化金(III)、臭化金(III))、
Au++e-=Au(E*(25℃)=1.83V)で表される還元半反応を引き起こす金化合物(塩化金(I))
(Money)
[AuCl 4 ] − + 3e − = Au + 4Cl − (E * (25 ° C.) = 1.002 V) A gold compound (tetrachloroaurate (III) acid) that causes a reduction half reaction,
Au 3+ + 3e − = Au (E * (25 ° C.) = 1.52 V), a gold compound (gold (III) chloride, gold (III) bromide) which causes a reduction half reaction,
Au + + e − = Au (E * (25 ° C.) = 1.83 V) A gold compound which causes a reduction half reaction (gold (I) chloride)
(水銀)
Hg2 2++2e-=2Hg(l)(E*(25℃)=0.796V)で表される還元半反応を引き起こす水銀化合物(酢酸水銀(I)、塩化水銀(I)、硝酸水銀(I))
2Hg2++2e-=Hg2 2+(E*(25℃)=0.9110V)で表される還元半反応を引き起こす水銀化合物(塩化水銀(II)、酢酸水銀(II)、硝酸水銀(II))
(mercury)
Hg 2 2+ + 2e − = 2Hg (l) (E * (25 ° C.) = 0.796 V) A mercury compound (mercury acetate (I), mercury chloride (I), mercury nitrate ( I))
2Hg 2+ + 2e − = Hg 2 2+ (E * (25 ° C.) = 0.110 110 V) Mercury compounds (mercury chloride (II), mercury acetate (II), mercuric nitrate (II) ))
(鉛)
PbO2(α)+H2O+2e-=Pb(red)+2OH-(E*(25℃)=0.249V)で表される還元半反応を引き起こす鉛化合物、
(lead)
A lead compound which causes a reduction half-reaction represented by PbO 2 (α) + H 2 O + 2e − = Pb (red) + 2OH − (E * (25 ° C.) = 0.249 V);
(ゲルマニウム)
Ge2++2e-=Ge(E*(25℃)=0.247V)で表される還元半反応を引き起こすゲルマニウム化合物
(germanium)
Ge 2+ + 2e − = Ge (E * (25 ° C.) = 0.247 V) Germanium compound causing reduction half reaction
(ヒ素)
HAsO2+3H++3e-=As+2H2O(E*(25℃)=0.248V)で表される還元半反応を引き起こすヒ素化合物
(Arsenic)
Arsenic compound that causes a reduction half-reaction represented by HAsO 2 + 3H + + 3e − = As + 2H 2 O (E * (25 ° C.) = 0.248 V)
(ビスマス)
Bi3++3e-=Bi(E*(25℃)=0.317V)で表される還元半反応を引き起こすビスマス化合物(硝酸ビスマス(III)、塩化ビスマス(III)、臭化ビスマス(III))、
(Bismuth)
Bi 3+ + 3e − = Bi (E * (25 ° C.) = 0.317 V) Bismuth compound that causes a reduction half reaction (bismuth (III) nitrate, bismuth (III) chloride, bismuth (III) bromide) ,
(ポロニウム)
Po2++2e-=Po(E*(25℃)=0.368V)で表される還元半反応を引き起こすポロニウム化合物、
(polonium)
A polonium compound which causes a reduction half-reaction represented by Po 2+ + 2e − = Po (E * (25 ° C.) = 0.368 V),
(ヨウ素)
2IO3 -+12H++10e-=I2+6H2O(E*(25℃)=1.195V)で表される還元半反応を引き起こすヨウ素化合物(ヨウ素酸ナトリウム(V)、ヨウ素酸カリウム(V))
(Iodine)
2IO 3 − + 12H + + 10e − = I 2 + 6H 2 O (E * (25 ° C.) = 1.195 V) An iodine compound (sodium iodate (V), potassium iodate (V)) that causes a reduction half reaction )
(臭素)
2HBrO+2H++2e-=Br2(l)+2H2O(E*(25℃)=1.604V)で表される還元半反応を引き起こす臭素化合物、
(bromine)
A bromine compound which causes a reduction half-reaction represented by 2HBrO + 2H + + 2e − = Br 2 (l) + 2H 2 O (E * (25 ° C.) = 1.604 V);
〔塩素)
2HClO(aq)+2H++2e-=Cl2(g)+2H2O(E*(25℃)=1.630V)で表される還元半反応を引き起こす塩素化合物、
〔chlorine)
2HClO (aq) + 2H + + 2e − = Cl 2 (g) + 2H 2 O (E * (25 ° C.) = 1.630 V);
(硫黄)
H2SO3+4H++4e-=S+3H2O(E*(25℃)=0.500V)で表される還元半反応を引き起こす硫黄化合物、
SO4 2-+4H++2e-=H2SO3+H2O(E*(25℃)=0.158V)硫酸ナトリウム(VI)、硫酸カリウム(VI)
などを挙げることができる。
(sulfur)
A sulfur compound which causes a reduction half reaction represented by H 2 SO 3 + 4H + + 4e − = S + 3H 2 O (E * (25 ° C.) = 0.500 V);
SO 4 2- + 4H + + 2e − = H 2 SO 3 + H 2 O (E * (25 ° C.) = 0.158 V) Sodium sulfate (VI), potassium sulfate (VI)
And the like.
本発明に用いられる不均一系液媒体は、水と、水に非相溶な溶媒からなるものである。
ここで、非相溶な溶媒とは、等体積の水と当該溶媒とを混ぜ合わせたときに2相に分離する溶媒である。よって、当該溶媒が水に多少溶解するものでも、または水が当該溶媒に多少溶解するものであってもよい。水に非相溶な溶媒としては、オクタン、クロロホルム、ジクロロメタン、1,2-ジクロロエタン、クロロベンゼン、トルエン、アニソール、ジn−ブチルエーテル、メチルイソブチルケトンなどを挙げることができる。
The heterogeneous liquid medium used in the present invention is composed of water and a solvent immiscible with water.
Here, the incompatible solvent is a solvent that separates into two phases when an equal volume of water and the solvent are mixed. Thus, the solvent may be slightly soluble in water or water may be slightly soluble in the solvent. Examples of the solvent incompatible with water include octane, chloroform, dichloromethane, 1,2-dichloroethane, chlorobenzene, toluene, anisole, di-n-butyl ether, and methyl isobutyl ketone.
本発明に用いられるポリシランは、水に難溶で且つ水に非相溶な溶媒に可溶なものである。「水に難溶」とは、室温の水に対するポリシランの溶解度が1重量%未満であることを意味する。「溶媒に可溶」とは、室温の溶媒に対するポリシランの溶解度が 重量%以上であることを意味する。 The polysilane used in the present invention is hardly soluble in water and soluble in a solvent that is incompatible with water. "Slightly soluble in water" means that the solubility of polysilane in water at room temperature is less than 1% by weight. "Soluble in solvent" means that the solubility of polysilane in a solvent at room temperature is at least% by weight.
ポリシランは、Si−Si結合で連なる重合体である。ポリシランの分子鎖は、直鎖状、環状、分岐鎖状、網目状などになっていてもよい。また、ポリシランは、1種のシランモノマーのみからなるホモポリマーであってもよいし、2種以上のシランモノマーからなるコポリマーであってもよい。 Polysilane is a polymer connected by Si-Si bonds. The molecular chain of the polysilane may be linear, cyclic, branched, or network-like. The polysilane may be a homopolymer composed of only one type of silane monomer or a copolymer composed of two or more types of silane monomers.
ポリシランとしては、例えば、式(1)で表される構造単位を有する分子鎖からなるものが挙げられる。 Examples of the polysilane include those composed of a molecular chain having a structural unit represented by the formula (1).
R1およびR2は、特に限定されないが、それぞれ独立に、アルキル基、またはアリール基であることができる。
直鎖状ポリシランの具体例としては、ポリ(ジアルキルシラン)、ポリ(アルキルアリールシラン)、ポリ(ジアリールシラン)などが挙げられる。
R 1 and R 2 are not particularly limited, but can be each independently an alkyl group or an aryl group.
Specific examples of the linear polysilane include poly (dialkylsilane), poly (alkylarylsilane), and poly (diarylsilane).
分岐鎖または網目状のポリシランは、例えば、式(2)または式(3)で表される構造単位などを分子鎖の分岐部として有する。
R3は、特に限定されないが、それぞれ独立に、アルキル基、またはアリール基であることができる。
分子鎖の末端には、式(4)で表される構造単位を有することができる。
R4およびR6は、特に限定されないが、それぞれ独立に、アルキル基、またはアリール基であることができる。R5は、水素原子、アルキル基、またはアリール基であることができる。
The branched or network-like polysilane has, for example, a structural unit represented by the formula (2) or the formula (3) as a branched portion of a molecular chain.
R 3 is not particularly limited, but can be each independently an alkyl group or an aryl group.
The terminal of the molecular chain can have a structural unit represented by the formula (4).
R 4 and R 6 are not particularly limited, but may be each independently an alkyl group or an aryl group. R 5 can be a hydrogen atom, an alkyl group, or an aryl group.
R1、R2、R3、R4、R5、又はR6におけるアルキル基は、直鎖アルキル基、分岐鎖アルキル基、および環状アルキル基のいずれであってもよい。該アルキル基は、それを構成する炭素原子の数が、好ましくは8個以下、より好ましくは6個以下である。
アルキル基の具体例としては、メチル基、エチル基、n−プロピル基、i−プロピル基、n−ブチル基、i−ブチル基、s−ブチル基、t−ブチル基、n−ペンチル基、n−へキシル基、シクロプロピル基、シクロブチル基、シクロペンチル基、シクロヘキシル基などを挙げることができる。これらのうち、炭素数1〜6の直鎖アルキル基が好ましい。
The alkyl group for R 1 , R 2 , R 3 , R 4 , R 5 , or R 6 may be any of a linear alkyl group, a branched alkyl group, and a cyclic alkyl group. The alkyl group has preferably eight or less carbon atoms, more preferably six or less carbon atoms.
Specific examples of the alkyl group include methyl group, ethyl group, n-propyl group, i-propyl group, n-butyl group, i-butyl group, s-butyl group, t-butyl group, n-pentyl group, and n -Hexyl, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and the like. Among these, a linear alkyl group having 1 to 6 carbon atoms is preferable.
R1、R2、R3、R4、R5、又はR6におけるアリール基は、単環であっても、多環であってもよい。多環アリール基は、少なくとも一つの環が芳香環であれば、残りの環が飽和環、不飽和環又は芳香環のいずれであってもよい。当該アリール基は、それを構成する炭素原子の数が、好ましくは6〜10個である。アリール基の具体例としては、フェニル基、1−ナフチル基、2−ナフチル基、アズレニル基、インダニル基、テトラリニル基を挙げることができる。これらのうち、フェニル基が好ましい。 The aryl group represented by R 1 , R 2 , R 3 , R 4 , R 5 , or R 6 may be monocyclic or polycyclic. As long as at least one ring of the polycyclic aryl group is an aromatic ring, the remaining ring may be a saturated ring, an unsaturated ring, or an aromatic ring. The aryl group preferably has 6 to 10 carbon atoms. Specific examples of the aryl group include a phenyl group, a 1-naphthyl group, a 2-naphthyl group, an azulenyl group, an indanyl group, and a tetralinyl group. Of these, a phenyl group is preferred.
本発明に好ましく用いられるポリシランとしては、ジメチルポリシラン、ジフェニルポリシラン、デカメチルシクロヘキサシラン(式(a)参照)、デカフェニルシクロペンタシラン(式(b〕参照)、ポリメチルフェニルシラン(式(c)参照)、ジメチルシランとモノフェニルシランのポリマー(式(e)参照)、ジフェニルシランとモノメチルシランのポリマー(式(g)参照)、ジフェニルシランとモノフェニルシランのポリマー(式(f)参照)、ジメチルシランとジフェニルシランのポリマー(式(d)参照)を挙げることができる。これらのうち、ドデカメチルシクロヘキサシラン、デカフェニルシクロペンタシランが好ましい。これらポリシランは1種を単独で若しくは2種以上を組み合わせて用いることができる。 Examples of the polysilane preferably used in the present invention include dimethylpolysilane, diphenylpolysilane, decamethylcyclohexasilane (see formula (a)), decaphenylcyclopentasilane (see formula (b)), and polymethylphenylsilane (formula (c) )), Polymer of dimethylsilane and monophenylsilane (see formula (e)), polymer of diphenylsilane and monomethylsilane (see formula (g)), polymer of diphenylsilane and monophenylsilane (see formula (f)) And a polymer of dimethylsilane and diphenylsilane (see formula (d)), of which dodecamethylcyclohexasilane and decaphenylcyclopentasilane are preferred, and these polysilanes may be used alone or in combination. These can be used in combination.
なお、式(d)、(e)、(f)および(g)中のxおよびyは括弧内の構造単位の繰り返し数を表す。 Note that x and y in the formulas (d), (e), (f) and (g) represent the number of repetitions of the structural unit in parentheses.
本発明に用いられるポリシランは、その重量平均分子量が、1000〜10000であることが好ましい。なお、ポリシランの重量平均分子量は、ゲル浸透クロマトグラフまたは超高温ゲル浸透クロマトグラフにより得られるクロマトグラムを標準ポリスチレンの分子量に換算することによって得られる値である。 The polysilane used in the present invention preferably has a weight average molecular weight of 1,000 to 10,000. The weight average molecular weight of polysilane is a value obtained by converting a chromatogram obtained by gel permeation chromatography or ultra-high temperature gel permeation chromatography into the molecular weight of standard polystyrene.
ポリシランは、特許文献1や2に記載のとおり、還元性を有する。このポリシランの還元性によって、前述した基質が還元され単体を生成する。この還元反応は、通常、10〜99℃の温度で行うことが好ましい。基質は水に溶解しており、ポリシランは水に非相溶な溶媒に溶解しているので、基質とポリシランとを接触させるために、不均一系溶媒を撹拌することが好ましい。 Polysilane has a reducing property as described in Patent Documents 1 and 2. By the reducing property of this polysilane, the above-mentioned substrate is reduced to generate a simple substance. Usually, this reduction reaction is preferably performed at a temperature of 10 to 99 ° C. Since the substrate is dissolved in water and the polysilane is dissolved in a solvent incompatible with water, it is preferable to stir the heterogeneous solvent to bring the substrate and the polysilane into contact.
この還元反応で得られる単体は、水および水に非相溶な溶媒からなる不均一系液媒体に難溶なものであることが好ましい。具体的には、金、白金、水銀、銀、パラジウム、ロジウムが好ましい。
難溶な単体は、不均一系液媒体中にて、析出し、粒状の固体として回収することができる。ポリシランは、既に述べたように水に非相溶な溶媒に可溶であるので、析出した単体がポリシランに付着することなく、濾過などの固液分離操作で容易にポリシランと単体とを分離することができ、そのため、比重差などを利用しての固固分離操作や、ポリシランの焼却処理操作を行う必要がない。
The simple substance obtained by this reduction reaction is preferably hardly soluble in a heterogeneous liquid medium composed of water and a solvent incompatible with water. Specifically, gold, platinum, mercury, silver, palladium, and rhodium are preferred.
The hardly soluble simple substance precipitates in the heterogeneous liquid medium and can be recovered as a granular solid. Since polysilane is soluble in a solvent that is incompatible with water as described above, the precipitated simple substance does not adhere to the polysilane, and the polysilane and the simple substance can be easily separated by a solid-liquid separation operation such as filtration. Therefore, there is no need to perform a solid-solid separation operation using a specific gravity difference or the like or an incineration operation of polysilane.
本発明の方法は、ポリシランと単体とを固液分離操舵で分離することができ、且つポリシランを焼却しないでもよいので、ポリシランの再利用が可能である。本発明の方法は、工場排液や生活排液等に含まれる希少元素の回収に好適である。また、海、湖沼、河川、土壌等の自然界からの希少元素の回収にも好適である。 According to the method of the present invention, polysilane and a simple substance can be separated by solid-liquid separation steering, and the polysilane does not need to be incinerated, so that the polysilane can be reused. The method of the present invention is suitable for recovering rare elements contained in factory wastewater, domestic wastewater, and the like. It is also suitable for recovering rare elements from the natural world such as the sea, lakes, marshes, rivers and soil.
以下、実施例を示し、本発明を更に詳細に説明するが、本発明はこれら実施例に限定されるものでない。 Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.
(金の回収)
実施例1
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン30mLに溶解させた。塩化金酸を塩酸に溶解させて、金100mgを含む水溶液10mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(100mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。該粉末は純度100%の金であった。金としての回収率は100%であった。
(Collection of gold)
Example 1
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 30 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 10 mL of an aqueous solution containing 100 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (100 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The powder was 100% pure gold. The recovery rate as gold was 100%.
(金の回収)
実施例2
フラスコにてドデカメチルシクロヘキサシラン1gをオクタン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(28mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は93%であった。
(Collection of gold)
Example 2
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of octane. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (28 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 93%.
(金の回収)
実施例3
フラスコにてドデカメチルシクロヘキサシラン1gをクロロホルム20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を60℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 3
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of chloroform. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 60 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
。
(金の回収)
実施例4
フラスコにてドデカメチルシクロヘキサシラン1gをジn−ブチルエーテル20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(27mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は90%であった。
.
(Collection of gold)
Example 4
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of di-n-butyl ether. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (27 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 90%.
(金の回収)
実施例5
フラスコにてドデカメチルシクロヘキサシラン1gをアニソール20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(27mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は90%であった。
(Collection of gold)
Example 5
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of anisole. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (27 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 90%.
(金の回収)
実施例6
フラスコにてドデカメチルシクロヘキサシラン1gをモノクロロベンゼン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を30℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 6
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of monochlorobenzene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 30 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
(金の回収)
実施例7
フラスコにてドデカメチルシクロヘキサシラン1gをメチルイソブチルケトン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を90℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(24mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は80%であった。
(Collection of gold)
Example 7
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of methyl isobutyl ketone. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 90 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (24 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 80%.
(金の回収)
比較例1
塩化金酸を塩酸に溶解させて、金100mgを含む水溶液10mLを得た。フラスコに、前記水溶液10mLと、ドデカメチルシクロヘキサシラン1gと、テトラヒドロフラン20mLとを入れた。当該フラスコ内を80℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を得ることができなかった。金としての回収率は0%であった。
(Collection of gold)
Comparative Example 1
Chloroauric acid was dissolved in hydrochloric acid to obtain 10 mL of an aqueous solution containing 100 mg of gold. The flask was charged with 10 mL of the aqueous solution, 1 g of dodecamethylcyclohexasilane, and 20 mL of tetrahydrofuran. The inside of the flask was heated to 80 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. Filtrate could not be obtained. The recovery rate as gold was 0%.
(金の回収)
比較例2
塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。フラスコに前記水溶液30mLと、ドデカメチルシクロヘキサシラン1gと、メタノール30mLとを入れた。当該フラスコ内を80℃に加熱して、5時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を得ることができなかった。金としての回収率は0%であった。
(Collection of gold)
Comparative Example 2
Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. The flask was charged with 30 mL of the aqueous solution, 1 g of dodecamethylcyclohexasilane, and 30 mL of methanol. The inside of the flask was heated to 80 ° C. and stirred for 5 hours. After returning to room temperature, the obtained liquid was filtered. Filtrate could not be obtained. The recovery rate as gold was 0%.
(金の回収)
比較例3
塩化金酸を塩酸に溶解させて、金100mgを含む水溶液10mLを得た。フラスコに、前記水溶液10mLと、ドデカメチルシクロヘキサシラン1gと、アセトン20mLとを入れた。当該フラスコ内を50℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を得ることができなかった。金としての回収率は0%であった。
(Collection of gold)
Comparative Example 3
Chloroauric acid was dissolved in hydrochloric acid to obtain 10 mL of an aqueous solution containing 100 mg of gold. The flask was charged with 10 mL of the aqueous solution, 1 g of dodecamethylcyclohexasilane, and 20 mL of acetone. The inside of the flask was heated to 50 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. Filtrate could not be obtained. The recovery rate as gold was 0%.
。
(金の回収)
比較例4
フラスコに、塩化金酸47mg(金として23mg)と、ドデカメチルシクロヘキサシラン1gと、テトラヒドロフラン20mLとを入れた。当該フラスコ内を80℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(13mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は56%であった。
.
(Collection of gold)
Comparative Example 4
A flask was charged with 47 mg of chloroauric acid (23 mg as gold), 1 g of dodecamethylcyclohexasilane, and 20 mL of tetrahydrofuran. The inside of the flask was heated to 80 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (13 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 56%.
(銀の回収)
実施例8
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン20mLに溶解させた。酢酸銀を酢酸に溶解させて、銀30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。次いで、1%水酸化ナトリウム水溶液を加えてpH9に調整した。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。灰色の粉末(8mg)を得た。この粉末をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。銀としての回収率は27%であった。
(Recovery of silver)
Example 8
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of toluene. Silver acetate was dissolved in acetic acid to obtain 30 mL of an aqueous solution containing 30 mg of silver. This aqueous solution was added to the flask. Then, the pH was adjusted to 9 by adding a 1% aqueous sodium hydroxide solution. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A gray powder (8 mg) was obtained. This powder was analyzed by an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as silver was 27%.
(白金の回収)
実施例9
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン30mLに溶解させた。塩化白金酸を塩酸に溶解させて、白金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。次いで、1%水酸化ナトリウム水溶液を加えてpH12に調整した。当該フラスコ内を97℃に加熱して、48時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。灰色の粉末(14mg)を得た。この粉末をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。白金としての回収率は46%であった。
(Platinum recovery)
Example 9
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 30 mL of toluene. Chloroplatinic acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of platinum. This aqueous solution was added to the flask. Then, the pH was adjusted to 12 by adding a 1% aqueous sodium hydroxide solution. The inside of the flask was heated to 97 ° C. and stirred for 48 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A gray powder (14 mg) was obtained. This powder was analyzed by an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as platinum was 46%.
(パラジウムの回収)
実施例10
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン20mLに溶解させた。酢酸パラジウムを酢酸に溶解させて、パラジウム32mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。黒色の粉末(29mg)を得た。この粉末をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。パラジウムとしての回収率は90%であった。
(Recovery of palladium)
Example 10
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of toluene. Palladium acetate was dissolved in acetic acid to obtain 30 mL of an aqueous solution containing 32 mg of palladium. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A black powder (29 mg) was obtained. This powder was analyzed by an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery as palladium was 90%.
(ロジウムの回収)
実施例11
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン20mLに溶解させた。塩化ロジウムを硝酸に溶解させて、ロジウム24mgを含む水溶液24mLを得た。この水溶液をフラスコに加えた。次いで、1%水酸化ナトリウム水溶液を加えてpH13に調整した。当該フラスコ内を97℃に加熱して、4時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。黄色〜茶色の粉末(24mg)を得た。この粉末をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。ロジウムとしての回収率は100%であった。
(Recovery of rhodium)
Example 11
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of toluene. Rhodium chloride was dissolved in nitric acid to obtain 24 mL of an aqueous solution containing 24 mg of rhodium. This aqueous solution was added to the flask. Subsequently, the pH was adjusted to 13 by adding a 1% aqueous sodium hydroxide solution. The inside of the flask was heated to 97 ° C. and stirred for 4 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A yellow-brown powder (24 mg) was obtained. This powder was analyzed by an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as rhodium was 100%.
(水銀の回収)
実施例12
フラスコにてドデカメチルシクロヘキサシラン1gをトルエン20mLに溶解させた。塩化水銀を硝酸に溶解させて、水銀30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。次いで、1%水酸化ナトリウム水溶液を加えてpH14に調整した。当該フラスコ内を97℃に加熱して、5時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。銀色の粉末(23mg)を得た。この粉末をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。白金としての回収率は76%であった。
(Recovery of mercury)
Example 12
In a flask, 1 g of dodecamethylcyclohexasilane was dissolved in 20 mL of toluene. Mercuric chloride was dissolved in nitric acid to obtain 30 mL of an aqueous solution containing 30 mg of mercury. This aqueous solution was added to the flask. Then, the pH was adjusted to 14 by adding a 1% aqueous sodium hydroxide solution. The inside of the flask was heated to 97 ° C. and stirred for 5 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A silver powder (23 mg) was obtained. This powder was analyzed by an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as platinum was 76%.
(金の回収)
実施例13
フラスコにてデカフェニルシクロペンタシラン1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、3時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(28mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は93%であった。
(Collection of gold)
Example 13
In a flask, 1 g of decaphenylcyclopentasilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 3 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (28 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 93%.
(金の回収)
実施例14
フラスコにてポリメチルフェニルシラン1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 14
In a flask, 1 g of polymethylphenylsilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
(金の回収)
実施例15
フラスコにてジメチルシランとジフェニルシランの50:50モル%のポリマー1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、1時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 15
In a flask, 1 g of a 50:50 mol% polymer of dimethylsilane and diphenylsilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 1 hour. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
(金の回収)
実施例16
フラスコにてジメチルシランとモノフェニルシランの50:50モル%のポリマー1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。次いで、1%水酸化ナトリウム水溶液を加えてpH13に調整した。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 16
In a flask, 1 g of a 50:50 mol% polymer of dimethylsilane and monophenylsilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. Subsequently, the pH was adjusted to 13 by adding a 1% aqueous sodium hydroxide solution. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
(金の回収)
実施例17
フラスコにてジフェニルシランとモノメチルシランの50:50モル%のポリマー1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 17
In a flask, 1 g of a 50:50 mol% polymer of diphenylsilane and monomethylsilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
(金の回収)
実施例18
フラスコにてジフェニルシランとモノフェニルシランの50:50モル%のポリマー1gをトルエン20mLに溶解させた。塩化金酸を塩酸に溶解させて、金30mgを含む水溶液30mLを得た。この水溶液をフラスコに加えた。当該フラスコ内を97℃に加熱して、2時間撹拌した。室温に戻した後、得られた液を濾過した。濾物を60℃で乾燥させた。金色〜茶色の粉末(30mg)を得た。この粉末を王水に溶かした溶液をICP発光分析装置IRIS Intrepid II XDL(Thermo Elemental社製)にて分析した。金としての回収率は100%であった。
(Collection of gold)
Example 18
In a flask, 1 g of a 50:50 mol% polymer of diphenylsilane and monophenylsilane was dissolved in 20 mL of toluene. Chloroauric acid was dissolved in hydrochloric acid to obtain 30 mL of an aqueous solution containing 30 mg of gold. This aqueous solution was added to the flask. The inside of the flask was heated to 97 ° C. and stirred for 2 hours. After returning to room temperature, the obtained liquid was filtered. The residue was dried at 60 ° C. A golden-brown powder (30 mg) was obtained. A solution of this powder dissolved in aqua regia was analyzed using an ICP emission spectrometer IRIS Intrepid II XDL (manufactured by Thermo Elemental). The recovery rate as gold was 100%.
以上の結果から、本発明の方法は、生成した単体がポリシランや他の物質に吸着しないので、ポリシランを用いた従来の還元法に比べて効率的に単体を製造若しくは回収できることがわかる。 From the above results, it can be seen that in the method of the present invention, since the produced simple substance does not adsorb to polysilane or other substances, the simple substance can be produced or recovered more efficiently than the conventional reduction method using polysilane.
Claims (2)
ジメチルポリシラン、ジフェニルポリシラン、デカメチルシクロヘキサシラン、デカフェニルシクロペンタシラン、ポリメチルフェニルシラン、またはジメチルシランとジフェニルシランのポリマーの存在下に、
単体を生成する還元半反応における標準電極電位が標準水素電極の電位よりも大きく且つ水に可溶な化合物を還元することを含む、
前記化合物から単体を製造する方法。 In a heterogeneous liquid medium consisting of water and a solvent incompatible with water,
In the presence of dimethylpolysilane, diphenylpolysilane, decamethylcyclohexasilane, decaphenylcyclopentasilane, polymethylphenylsilane, or a polymer of dimethylsilane and diphenylsilane ,
Reducing the compound soluble in water, wherein the standard electrode potential in the reduction half reaction to produce a simple substance is larger than the potential of the standard hydrogen electrode, and
A method for producing a simple substance from the compound.
水に非相溶な溶媒と、
ジメチルポリシラン、ジフェニルポリシラン、デカメチルシクロヘキサシラン、デカフェニルシクロペンタシラン、ポリメチルフェニルシラン、またはジメチルシランとジフェニルシランのポリマーと
を含有する不均一反応液を得、
該反応液において前記化合物を還元することを含む、
前記化合物を含有する水溶液から単体を回収する方法。 An aqueous solution containing a compound in which the standard electrode potential in the reduction half-reaction that produces a simple substance is larger than the potential of the standard hydrogen electrode and is soluble in water,
A solvent incompatible with water,
Dimethyl polysilane, diphenyl polysilane, decamethylcyclohexasilane, decaphenylcyclopentasilane, polymethylphenylsilane, or obtain a heterogeneous reaction solution containing dimethylsilane and diphenylsilane polymer ,
Reducing the compound in the reaction solution.
A method for recovering a simple substance from an aqueous solution containing the compound.
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