CN110833835B - 一种碳包覆金属颗粒锚定纳米催化材料的制备方法 - Google Patents
一种碳包覆金属颗粒锚定纳米催化材料的制备方法 Download PDFInfo
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- CN110833835B CN110833835B CN201911132691.XA CN201911132691A CN110833835B CN 110833835 B CN110833835 B CN 110833835B CN 201911132691 A CN201911132691 A CN 201911132691A CN 110833835 B CN110833835 B CN 110833835B
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- Prior art keywords
- salt
- chloride
- ammonium
- cobalt
- nickel
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 47
- 239000002923 metal particle Substances 0.000 title claims abstract description 41
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 84
- 239000002184 metal Substances 0.000 claims abstract description 84
- 239000012266 salt solution Substances 0.000 claims abstract description 61
- 239000000243 solution Substances 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 32
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 238000006073 displacement reaction Methods 0.000 claims abstract description 12
- 238000005530 etching Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 74
- 239000008367 deionised water Substances 0.000 claims description 68
- 229910021641 deionized water Inorganic materials 0.000 claims description 68
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 64
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 59
- 238000002156 mixing Methods 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 37
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 37
- 239000001257 hydrogen Substances 0.000 claims description 37
- 229910052739 hydrogen Inorganic materials 0.000 claims description 37
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 34
- -1 polytetrafluoroethylene Polymers 0.000 claims description 33
- 229910052786 argon Inorganic materials 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 31
- 150000003839 salts Chemical class 0.000 claims description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 17
- 229910052700 potassium Inorganic materials 0.000 claims description 17
- 239000011591 potassium Substances 0.000 claims description 17
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Chemical group COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 238000006722 reduction reaction Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- IGJQUJNPMOYEJY-UHFFFAOYSA-N 2-acetylpyrrole Chemical compound CC(=O)C1=CC=CN1 IGJQUJNPMOYEJY-UHFFFAOYSA-N 0.000 claims description 8
- 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 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 8
- 150000001868 cobalt Chemical class 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 150000002815 nickel Chemical class 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical group NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical group CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 6
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 6
- 229910052703 rhodium Inorganic materials 0.000 claims description 6
- 239000010948 rhodium Substances 0.000 claims description 6
- SVOOVMQUISJERI-UHFFFAOYSA-K rhodium(3+);triacetate Chemical compound [Rh+3].CC([O-])=O.CC([O-])=O.CC([O-])=O SVOOVMQUISJERI-UHFFFAOYSA-K 0.000 claims description 6
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 5
- 150000002503 iridium Chemical class 0.000 claims description 5
- 150000002940 palladium Chemical class 0.000 claims description 5
- 150000003057 platinum Chemical class 0.000 claims description 5
- 150000003283 rhodium Chemical class 0.000 claims description 5
- 150000003303 ruthenium Chemical class 0.000 claims description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 5
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims description 5
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims description 5
- 150000003681 vanadium Chemical class 0.000 claims description 5
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 4
- VYXHVRARDIDEHS-UHFFFAOYSA-N 1,5-cyclooctadiene Chemical compound C1CC=CCCC=C1 VYXHVRARDIDEHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000004912 1,5-cyclooctadiene Substances 0.000 claims description 4
- ICSNLGPSRYBMBD-UHFFFAOYSA-N 2-aminopyridine Chemical compound NC1=CC=CC=N1 ICSNLGPSRYBMBD-UHFFFAOYSA-N 0.000 claims description 4
- CUYKNJBYIJFRCU-UHFFFAOYSA-N 3-aminopyridine Chemical compound NC1=CC=CN=C1 CUYKNJBYIJFRCU-UHFFFAOYSA-N 0.000 claims description 4
- FKNQCJSGGFJEIZ-UHFFFAOYSA-N 4-methylpyridine Chemical compound CC1=CC=NC=C1 FKNQCJSGGFJEIZ-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical group CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical group CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 claims description 4
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methylaniline Chemical group CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 claims description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical group C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical group NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- XKGMHABTFTUWDV-UHFFFAOYSA-N [W+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] Chemical compound [W+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] XKGMHABTFTUWDV-UHFFFAOYSA-N 0.000 claims description 4
- FQNHWXHRAUXLFU-UHFFFAOYSA-N carbon monoxide;tungsten Chemical group [W].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] FQNHWXHRAUXLFU-UHFFFAOYSA-N 0.000 claims description 4
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 4
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 4
- KZLHPYLCKHJIMM-UHFFFAOYSA-K iridium(3+);triacetate Chemical compound [Ir+3].CC([O-])=O.CC([O-])=O.CC([O-])=O KZLHPYLCKHJIMM-UHFFFAOYSA-K 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 150000002751 molybdenum Chemical class 0.000 claims description 4
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 4
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- UBQKCCHYAOITMY-UHFFFAOYSA-N pyridin-2-ol Chemical compound OC1=CC=CC=N1 UBQKCCHYAOITMY-UHFFFAOYSA-N 0.000 claims description 4
- WRHZVMBBRYBTKZ-UHFFFAOYSA-N pyrrole-2-carboxylic acid Chemical compound OC(=O)C1=CC=CN1 WRHZVMBBRYBTKZ-UHFFFAOYSA-N 0.000 claims description 4
- OJLCQGGSMYKWEK-UHFFFAOYSA-K ruthenium(3+);triacetate Chemical compound [Ru+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OJLCQGGSMYKWEK-UHFFFAOYSA-K 0.000 claims description 4
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000004729 solvothermal method Methods 0.000 claims description 4
- 150000003657 tungsten Chemical class 0.000 claims description 4
- 125000005287 vanadyl group Chemical group 0.000 claims description 4
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Chemical group CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 claims description 2
- MBVAQOHBPXKYMF-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;rhodium Chemical compound [Rh].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O MBVAQOHBPXKYMF-LNTINUHCSA-N 0.000 claims description 2
- IYWJIYWFPADQAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;ruthenium Chemical compound [Ru].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O IYWJIYWFPADQAN-LNTINUHCSA-N 0.000 claims description 2
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical group CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 2
- VGZCKCJMYREIKA-UHFFFAOYSA-N 1-(2,4-dimethyl-1h-pyrrol-3-yl)ethanone Chemical compound CC(=O)C=1C(C)=CNC=1C VGZCKCJMYREIKA-UHFFFAOYSA-N 0.000 claims description 2
- WDQFELCEOPFLCZ-UHFFFAOYSA-N 1-(2-hydroxyethyl)pyrrolidin-2-one Chemical compound OCCN1CCCC1=O WDQFELCEOPFLCZ-UHFFFAOYSA-N 0.000 claims description 2
- DNDPLEAVNVOOQZ-UHFFFAOYSA-N 2,3,4,5,6-pentachloropyridine Chemical compound ClC1=NC(Cl)=C(Cl)C(Cl)=C1Cl DNDPLEAVNVOOQZ-UHFFFAOYSA-N 0.000 claims description 2
- MFFMQGGZCLEMCI-UHFFFAOYSA-N 2,4-dimethyl-1h-pyrrole Chemical compound CC1=CNC(C)=C1 MFFMQGGZCLEMCI-UHFFFAOYSA-N 0.000 claims description 2
- PAJMKGZZBBTTOY-UHFFFAOYSA-N 2-[[2-hydroxy-1-(3-hydroxyoctyl)-2,3,3a,4,9,9a-hexahydro-1h-cyclopenta[g]naphthalen-5-yl]oxy]acetic acid Chemical compound C1=CC=C(OCC(O)=O)C2=C1CC1C(CCC(O)CCCCC)C(O)CC1C2 PAJMKGZZBBTTOY-UHFFFAOYSA-N 0.000 claims description 2
- ZEYKLMDPUOVUCR-UHFFFAOYSA-N 2-chloro-5-(trifluoromethyl)benzenesulfonyl chloride Chemical compound FC(F)(F)C1=CC=C(Cl)C(S(Cl)(=O)=O)=C1 ZEYKLMDPUOVUCR-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Chemical group CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 2
- NYPYPOZNGOXYSU-UHFFFAOYSA-N 3-bromopyridine Chemical compound BrC1=CC=CN=C1 NYPYPOZNGOXYSU-UHFFFAOYSA-N 0.000 claims description 2
- RZJPBQGRCNJYBU-UHFFFAOYSA-N 3-chloropyridin-2-amine Chemical compound NC1=NC=CC=C1Cl RZJPBQGRCNJYBU-UHFFFAOYSA-N 0.000 claims description 2
- PWRBCZZQRRPXAB-UHFFFAOYSA-N 3-chloropyridine Chemical compound ClC1=CC=CN=C1 PWRBCZZQRRPXAB-UHFFFAOYSA-N 0.000 claims description 2
- FPFSGDXIBUDDKZ-UHFFFAOYSA-N 3-decyl-2-hydroxycyclopent-2-en-1-one Chemical compound CCCCCCCCCCC1=C(O)C(=O)CC1 FPFSGDXIBUDDKZ-UHFFFAOYSA-N 0.000 claims description 2
- CELKOWQJPVJKIL-UHFFFAOYSA-N 3-fluoropyridine Chemical compound FC1=CC=CN=C1 CELKOWQJPVJKIL-UHFFFAOYSA-N 0.000 claims description 2
- XXSPKSHUSWQAIZ-UHFFFAOYSA-L 36026-88-7 Chemical compound [Ni+2].[O-]P=O.[O-]P=O XXSPKSHUSWQAIZ-UHFFFAOYSA-L 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Chemical group CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- YILMOQBPBZHHFY-UHFFFAOYSA-L C(C)(C)[Ru](C1=CC=CC=C1)(Cl)Cl Chemical compound C(C)(C)[Ru](C1=CC=CC=C1)(Cl)Cl YILMOQBPBZHHFY-UHFFFAOYSA-L 0.000 claims description 2
- JEKHZWKDISRMDQ-UHFFFAOYSA-N C1=CC=NC(C2=CC=CC=N2)=C1.C1=CC=NC(C2=CC=CC=N2)=C1.C1=CC=NC(C2=CC=CC=N2)=C1.Cl Chemical compound C1=CC=NC(C2=CC=CC=N2)=C1.C1=CC=NC(C2=CC=CC=N2)=C1.C1=CC=NC(C2=CC=CC=N2)=C1.Cl JEKHZWKDISRMDQ-UHFFFAOYSA-N 0.000 claims description 2
- QICBZCXKJSWKQI-UHFFFAOYSA-N ClC=1C(=C(C=CC=1)[Ru+])Cl Chemical class ClC=1C(=C(C=CC=1)[Ru+])Cl QICBZCXKJSWKQI-UHFFFAOYSA-N 0.000 claims description 2
- ARDXCNKWEOUEKB-UHFFFAOYSA-H Cl[Rh](Cl)(Cl)(Cl)(Cl)Cl.N.O Chemical compound Cl[Rh](Cl)(Cl)(Cl)(Cl)Cl.N.O ARDXCNKWEOUEKB-UHFFFAOYSA-H 0.000 claims description 2
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims description 2
- PAPNRQCYSFBWDI-UHFFFAOYSA-N DMP Natural products CC1=CC=C(C)N1 PAPNRQCYSFBWDI-UHFFFAOYSA-N 0.000 claims description 2
- PAEYAKGINDQUCT-UHFFFAOYSA-N Ethyl 2-pyrrolecarboxylate Chemical compound CCOC(=O)C1=CC=CN1 PAEYAKGINDQUCT-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- RKBOHILEOXOBOF-UHFFFAOYSA-K FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F.[Rh+3].FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F.FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F Chemical class FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F.[Rh+3].FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F.FC(C(C(C(=O)[O-])(F)F)(F)F)(F)F RKBOHILEOXOBOF-UHFFFAOYSA-K 0.000 claims description 2
- 229910003767 Gold(III) bromide Inorganic materials 0.000 claims description 2
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical group CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 2
- VYRZVNZTWPARPF-UHFFFAOYSA-M N.[Cl-].[Rh+3] Chemical compound N.[Cl-].[Rh+3] VYRZVNZTWPARPF-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Chemical group 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Chemical group CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Chemical group 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- RSBNPUNXBGVNNB-UHFFFAOYSA-M S(=O)(=O)([O-])[O-].[NH4+].[Co+] Chemical compound S(=O)(=O)([O-])[O-].[NH4+].[Co+] RSBNPUNXBGVNNB-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910021550 Vanadium Chloride Inorganic materials 0.000 claims description 2
- 229910021552 Vanadium(IV) chloride Inorganic materials 0.000 claims description 2
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical compound [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 claims description 2
- UCFIGPFUCRUDII-UHFFFAOYSA-N [Co](C#N)C#N.[K] Chemical compound [Co](C#N)C#N.[K] UCFIGPFUCRUDII-UHFFFAOYSA-N 0.000 claims description 2
- YMXQRQIZILQVGU-UHFFFAOYSA-H [K].Cl[Rh](Cl)(Cl)(Cl)(Cl)Cl Chemical compound [K].Cl[Rh](Cl)(Cl)(Cl)(Cl)Cl YMXQRQIZILQVGU-UHFFFAOYSA-H 0.000 claims description 2
- XJIPZQRDWCIXPA-UHFFFAOYSA-N [Mo+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] Chemical compound [Mo+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] XJIPZQRDWCIXPA-UHFFFAOYSA-N 0.000 claims description 2
- FBAZCZFUGZHBMZ-UHFFFAOYSA-O [NH4+].[Ni].[O-][N+]([O-])=O Chemical compound [NH4+].[Ni].[O-][N+]([O-])=O FBAZCZFUGZHBMZ-UHFFFAOYSA-O 0.000 claims description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 2
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 2
- DAPUDVOJPZKTSI-UHFFFAOYSA-L ammonium nickel sulfate Chemical compound [NH4+].[NH4+].[Ni+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DAPUDVOJPZKTSI-UHFFFAOYSA-L 0.000 claims description 2
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 claims description 2
- MMCPOSDMTGQNKG-UJZMCJRSSA-N aniline;hydrochloride Chemical compound Cl.N[14C]1=[14CH][14CH]=[14CH][14CH]=[14CH]1 MMCPOSDMTGQNKG-UJZMCJRSSA-N 0.000 claims description 2
- AQBOUNVXZQRXNP-UHFFFAOYSA-L azane;dichloropalladium Chemical compound N.N.N.N.Cl[Pd]Cl AQBOUNVXZQRXNP-UHFFFAOYSA-L 0.000 claims description 2
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 claims description 2
- WPEJSSRSFRWYJB-UHFFFAOYSA-K azanium;tetrachlorogold(1-) Chemical compound [NH4+].[Cl-].[Cl-].[Cl-].[Cl-].[Au+3] WPEJSSRSFRWYJB-UHFFFAOYSA-K 0.000 claims description 2
- 239000004202 carbamide Chemical group 0.000 claims description 2
- GGRQQHADVSXBQN-FGSKAQBVSA-N carbon monoxide;(z)-4-hydroxypent-3-en-2-one;rhodium Chemical compound [Rh].[O+]#[C-].[O+]#[C-].C\C(O)=C\C(C)=O GGRQQHADVSXBQN-FGSKAQBVSA-N 0.000 claims description 2
- LPEOOPATWLDBQS-UHFFFAOYSA-N carbonyl dichloride;iridium;triphenylphosphane Chemical compound [Ir].ClC(Cl)=O.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 LPEOOPATWLDBQS-UHFFFAOYSA-N 0.000 claims description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 2
- 229960001231 choline Drugs 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 229910000152 cobalt phosphate Inorganic materials 0.000 claims description 2
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 claims description 2
- AVWLPUQJODERGA-UHFFFAOYSA-L cobalt(2+);diiodide Chemical compound [Co+2].[I-].[I-] AVWLPUQJODERGA-UHFFFAOYSA-L 0.000 claims description 2
- BSUSEPIPTZNHMN-UHFFFAOYSA-L cobalt(2+);diperchlorate Chemical compound [Co+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O BSUSEPIPTZNHMN-UHFFFAOYSA-L 0.000 claims description 2
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 claims description 2
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims description 2
- MJABMRHBVCGGOG-UHFFFAOYSA-L cobalt(2+);sulfite Chemical compound [Co+2].[O-]S([O-])=O MJABMRHBVCGGOG-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- BZRRQSJJPUGBAA-UHFFFAOYSA-L cobalt(ii) bromide Chemical compound Br[Co]Br BZRRQSJJPUGBAA-UHFFFAOYSA-L 0.000 claims description 2
- YCYBZKSMUPTWEE-UHFFFAOYSA-L cobalt(ii) fluoride Chemical compound F[Co]F YCYBZKSMUPTWEE-UHFFFAOYSA-L 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 2
- RKBAPHPQTADBIK-UHFFFAOYSA-N cobalt;hexacyanide Chemical compound [Co].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] RKBAPHPQTADBIK-UHFFFAOYSA-N 0.000 claims description 2
- PNNCIXRVXCLADM-UHFFFAOYSA-L cyclohexane-1,2-diamine;dichloroplatinum Chemical compound Cl[Pt]Cl.NC1CCCCC1N PNNCIXRVXCLADM-UHFFFAOYSA-L 0.000 claims description 2
- DMRVBCXRFYZCPR-UHFFFAOYSA-L cycloocta-1,5-diene;ruthenium(2+);dichloride Chemical compound Cl[Ru]Cl.C1CC=CCCC=C1 DMRVBCXRFYZCPR-UHFFFAOYSA-L 0.000 claims description 2
- UOPIRNHVGHLLDZ-UHFFFAOYSA-L dichlororhodium Chemical compound Cl[Rh]Cl UOPIRNHVGHLLDZ-UHFFFAOYSA-L 0.000 claims description 2
- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 claims description 2
- XOLNQIIEFUNTQC-UHFFFAOYSA-H dipotassium;hexachlororuthenium(2-) Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[K+].[K+].[Ru+4] XOLNQIIEFUNTQC-UHFFFAOYSA-H 0.000 claims description 2
- LMABILRJNNFCPG-UHFFFAOYSA-L ethane-1,2-diamine;platinum(2+);dichloride Chemical compound [Cl-].[Cl-].[Pt+2].NCCN LMABILRJNNFCPG-UHFFFAOYSA-L 0.000 claims description 2
- FCNXGBYXGSKCDG-UHFFFAOYSA-N ethylferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.CC[C-]1C=CC=C1 FCNXGBYXGSKCDG-UHFFFAOYSA-N 0.000 claims description 2
- 229960002413 ferric citrate Drugs 0.000 claims description 2
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 229940062993 ferrous oxalate Drugs 0.000 claims description 2
- 229910001922 gold oxide Inorganic materials 0.000 claims description 2
- OVWPJGBVJCTEBJ-UHFFFAOYSA-K gold tribromide Chemical compound Br[Au](Br)Br OVWPJGBVJCTEBJ-UHFFFAOYSA-K 0.000 claims description 2
- OTCKNHQTLOBDDD-UHFFFAOYSA-K gold(3+);triacetate Chemical compound [Au+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OTCKNHQTLOBDDD-UHFFFAOYSA-K 0.000 claims description 2
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 claims description 2
- WDZVNNYQBQRJRX-UHFFFAOYSA-K gold(iii) hydroxide Chemical compound O[Au](O)O WDZVNNYQBQRJRX-UHFFFAOYSA-K 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- HLYTZTFNIRBLNA-LNTINUHCSA-K iridium(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ir+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O HLYTZTFNIRBLNA-LNTINUHCSA-K 0.000 claims description 2
- HTFVQFACYFEXPR-UHFFFAOYSA-K iridium(3+);tribromide Chemical compound Br[Ir](Br)Br HTFVQFACYFEXPR-UHFFFAOYSA-K 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Chemical group CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 2
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- UQPSGBZICXWIAG-UHFFFAOYSA-L nickel(2+);dibromide;trihydrate Chemical compound O.O.O.Br[Ni]Br UQPSGBZICXWIAG-UHFFFAOYSA-L 0.000 claims description 2
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical compound [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 claims description 2
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 2
- QEKXARSPUFVXIX-UHFFFAOYSA-L nickel(2+);triphenylphosphane;dibromide Chemical compound [Ni+2].[Br-].[Br-].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QEKXARSPUFVXIX-UHFFFAOYSA-L 0.000 claims description 2
- ZBRJXVVKPBZPAN-UHFFFAOYSA-L nickel(2+);triphenylphosphane;dichloride Chemical compound [Cl-].[Cl-].[Ni+2].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 ZBRJXVVKPBZPAN-UHFFFAOYSA-L 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 2
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical group CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- PBDBXAQKXCXZCJ-UHFFFAOYSA-L palladium(2+);2,2,2-trifluoroacetate Chemical compound [Pd+2].[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F PBDBXAQKXCXZCJ-UHFFFAOYSA-L 0.000 claims description 2
- JUBNUQXDQDMSKL-UHFFFAOYSA-N palladium(2+);dinitrate;dihydrate Chemical compound O.O.[Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O JUBNUQXDQDMSKL-UHFFFAOYSA-N 0.000 claims description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims 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 claims description 2
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 claims description 2
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Chemical group 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- NEYLGXVZJUUZMY-UHFFFAOYSA-K potassium;trichlorogold Chemical compound [K].Cl[Au](Cl)Cl NEYLGXVZJUUZMY-UHFFFAOYSA-K 0.000 claims description 2
- ZZYXNRREDYWPLN-UHFFFAOYSA-N pyridine-2,3-diamine Chemical compound NC1=CC=CN=C1N ZZYXNRREDYWPLN-UHFFFAOYSA-N 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- KXAHUXSHRWNTOD-UHFFFAOYSA-K rhodium(3+);triiodide Chemical compound [Rh+3].[I-].[I-].[I-] KXAHUXSHRWNTOD-UHFFFAOYSA-K 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 2
- UREFKUKELTYZEO-UHFFFAOYSA-N ruthenium;triphenylphosphane Chemical compound [Ru].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 UREFKUKELTYZEO-UHFFFAOYSA-N 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- CGOSIVYNVKVZBK-UHFFFAOYSA-K sodium cobalt(2+) trinitrite Chemical compound [Na+].[Co++].[O-]N=O.[O-]N=O.[O-]N=O CGOSIVYNVKVZBK-UHFFFAOYSA-K 0.000 claims description 2
- 239000000264 sodium ferrocyanide Substances 0.000 claims description 2
- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012247 sodium ferrocyanide Nutrition 0.000 claims description 2
- 229940080262 sodium tetrachloroaurate Drugs 0.000 claims description 2
- ABKQFSYGIHQQLS-UHFFFAOYSA-J sodium tetrachloropalladate Chemical compound [Na+].[Na+].Cl[Pd+2](Cl)(Cl)Cl ABKQFSYGIHQQLS-UHFFFAOYSA-J 0.000 claims description 2
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 2
- RNJPWBVOCUGBGY-UHFFFAOYSA-J tetraiodoplatinum Chemical compound [I-].[I-].[I-].[I-].[Pt+4] RNJPWBVOCUGBGY-UHFFFAOYSA-J 0.000 claims description 2
- AWDBHOZBRXWRKS-UHFFFAOYSA-N tetrapotassium;iron(6+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+6].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] AWDBHOZBRXWRKS-UHFFFAOYSA-N 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- QVJDTKXZVZTKLX-UHFFFAOYSA-K trichlorogold;triphenylphosphane Chemical compound Cl[Au](Cl)Cl.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QVJDTKXZVZTKLX-UHFFFAOYSA-K 0.000 claims description 2
- GCZKMPJFYKFENV-UHFFFAOYSA-K triiodogold Chemical compound I[Au](I)I GCZKMPJFYKFENV-UHFFFAOYSA-K 0.000 claims description 2
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 2
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 2
- JTJFQBNJBPPZRI-UHFFFAOYSA-J vanadium tetrachloride Chemical compound Cl[V](Cl)(Cl)Cl JTJFQBNJBPPZRI-UHFFFAOYSA-J 0.000 claims description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 2
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 claims 2
- 229910019142 PO4 Inorganic materials 0.000 claims 2
- 239000011261 inert gas Substances 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 2
- 239000010452 phosphate Substances 0.000 claims 2
- WVRNEYPEUSJKDG-UHFFFAOYSA-N cyclooctane;rhodium Chemical compound [Rh].C1CC=CCCC=C1.C1CC=CCCC=C1 WVRNEYPEUSJKDG-UHFFFAOYSA-N 0.000 claims 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims 1
- VHNQIURBCCNWDN-UHFFFAOYSA-N pyridine-2,6-diamine Chemical compound NC1=CC=CC(N)=N1 VHNQIURBCCNWDN-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004873 anchoring Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 38
- 239000007789 gas Substances 0.000 description 28
- 238000010438 heat treatment Methods 0.000 description 27
- 238000000967 suction filtration Methods 0.000 description 26
- 238000001291 vacuum drying Methods 0.000 description 25
- 239000003054 catalyst Substances 0.000 description 21
- 238000005406 washing Methods 0.000 description 17
- 238000000034 method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 150000004687 hexahydrates Chemical class 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- HSSMNYDDDSNUKH-UHFFFAOYSA-K trichlororhodium;hydrate Chemical compound O.Cl[Rh](Cl)Cl HSSMNYDDDSNUKH-UHFFFAOYSA-K 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229940032296 ferric chloride Drugs 0.000 description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 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
- WMQUKDQWMMOHSA-UHFFFAOYSA-N 1-pyridin-4-ylethanone Chemical compound CC(=O)C1=CC=NC=C1 WMQUKDQWMMOHSA-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- 229910021604 Rhodium(III) chloride Inorganic materials 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N Tetraethylene glycol, Natural products OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- MQLVWQSVRZVNIP-UHFFFAOYSA-L ferrous ammonium sulfate hexahydrate Chemical compound [NH4+].[NH4+].O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O MQLVWQSVRZVNIP-UHFFFAOYSA-L 0.000 description 1
- 229960000390 fludarabine Drugs 0.000 description 1
- GIUYCYHIANZCFB-FJFJXFQQSA-N fludarabine phosphate Chemical compound C1=NC=2C(N)=NC(F)=NC=2N1[C@@H]1O[C@H](COP(O)(O)=O)[C@@H](O)[C@@H]1O GIUYCYHIANZCFB-FJFJXFQQSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 description 1
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- GLOBUAZSRIOKLN-UHFFFAOYSA-N pentane-1,4-diol Chemical compound CC(O)CCCO GLOBUAZSRIOKLN-UHFFFAOYSA-N 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- MJRFDVWKTFJAPF-UHFFFAOYSA-K trichloroiridium;hydrate Chemical compound O.Cl[Ir](Cl)Cl MJRFDVWKTFJAPF-UHFFFAOYSA-K 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000010407 vacuum cleaning Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
本发明公开了碳包覆金属颗粒锚定纳米催化材料的制备方法，包含以下操作步骤：(1)配置金属盐溶液A，将有机碳源B溶液加入金属盐溶液A中，滴加还原剂反应，过滤、清洗，干燥后进行初步高温煅烧，得到的样品再加入强碱进行刻蚀，干燥后在混合气氛下高温煅烧，清洗、干燥后得到初级样品C；(2)配置金属盐溶液D，将步骤(1)所得初级样品C加入金属盐溶液D中，常温下进行置换反应，过滤、清洗、干燥，然后在混合气氛下高温煅烧，即得具有碳包覆金属颗粒锚定结构的纳米催化材料。本发明制备所得碳包覆金属颗粒锚定纳米催化材料中的金属颗粒大小分布均匀，制备工艺简单，可作为高效电催化材料，具有较好的电催化活性和电化学稳定性。
Description
技术领域
本发明涉及一种纳米催化材料的制备方法，特别涉及一种碳包覆金属颗粒锚定纳米催化材料的制备方法。
背景技术
随着科技的迅速发展，大量不可再生化石能源的消耗，导致环境污染问题日益严重。因此，发展燃料电池、电解水制氢等技术是解决当今社会能源短缺和环境污染的有效措施。在这些领域中，催化剂起到至关重要的作用。然而催化剂所用的贵金属资源稀少，同时成本高、活性低、稳定性差等系列问题又制约着这些技术领域的发展。纳米技术在催化领域凸显出巨大的发展潜力，运用纳米材料制备技术，可控地合成具有锚定结构的纳米催化材料，将大幅度降低催化剂的制备成本，提高催化剂的活性和稳定性。通过碳包覆技术可以进一步提高催化剂的稳定性，但现有的技术中得到稳定催化剂的工艺方法大多复杂成本高、耗时长，因此，亟需一种工艺简洁又能够制备得到稳定催化剂的方法。公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技术人员所公知的现有技术。
发明内容
本申请针对现有技术的不足，发明一种碳包覆金属颗粒锚定纳米催化材料的制备方法，通过本发明方法可得到一种简单可控、稳定、廉价、高效的电催化材料。
为实现上述目的，本发明提供的技术方案如下：
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，包含以下操作步骤：
(1)配置金属盐溶液A，将有机碳源B溶液加入金属盐溶液A中，然后滴加还原剂进行还原反应，过滤、清洗，干燥后进行高温煅烧，得到的样品再加入强碱进行刻蚀，干燥后在混合气氛下高温煅烧得到初级样品C，所述的还原反应的方式有液相反应或溶剂热反应；
(2)配置金属盐溶液D，将步骤(1)所得初级样品C加入金属盐溶液D中，常温下进行置换反应，过滤、清洗、干燥，然后在混合气氛下高温煅烧，即得碳包覆金属颗粒锚定纳米催化材料。
优选的是，步骤(1)中所述的金属盐溶液A为金属盐A溶于水中得到金属盐溶液；所述的金属盐A为铁盐、钴盐、镍盐、钨盐、钼盐、钒盐中的至少一种，两种及两种以上混合时比例任意，其中有铁盐、钴盐或镍盐参与混合时三者中任一种混合比例不为零；所述的铁盐为氯化亚铁、三氯化铁、乙酰丙酮铁、铁***、亚铁***、亚硝基亚铁***、二茂铁、硝酸铁、柠檬酸铁、柠檬酸铁铵、草酸高铁铵、草酸亚铁、六氰合铁酸钾、硫酸铁、硫酸亚铁、硫酸亚铁铵、硫酸高铁铵、乙基二茂铁、十二羰基三铁、醋酸铁或醋酸亚铁中的一种；所述的钴盐为氯化钴、乙酸钴、磷酸钴、酞菁钴、钴***、六氰钴酸钾、六氨基氯化钴、高氯酸钴、硝酸钴、氟化钴、碘化钴、溴化钴、亚硝酸钴钠、草酸钴、硫酸钴、硫酸亚钴、硫酸钴铵、环烷酸钴或乙酰丙酮钴中的一种；所述的镍盐为氯化镍、乙酰丙酮镍、乙酰丙酮酸镍、乙酸镍、溴化镍、碘化镍、硫酸镍、硝酸镍、硫酸镍铵、次磷酸镍、硝酸镍铵、氨基磺酸镍、碱式碳酸镍、甲酸镍、二茂镍、二(三苯基膦)溴化镍或双(三苯基膦)氯化镍中的一种；所述的钨盐为六羰基钨、异丙醇钨、偏钨酸铵、钨酸铵、钨酸钾、钨酸钠、磷钨酸、磷钨酸钠、钨硅酸、六氯化钨、六羰基钨、异丙醇钨或偏钨酸铵中的一种；所述的钼盐为六羰基钼、乙酰丙酮钼、异丙醇钼、四钼酸铵、七钼酸铵、二钼酸铵、钼酸钠、磷钼酸、磷钼酸铵、磷钼酸钠、氯化钼、钼酸锂或钼酸钾中的一种；所述的钒盐为三异丙醇氧钒、乙酰丙酮氧钒、三异丙氧基氧化钒、氧化二乙酰丙酮合钒、偏钒酸铵、偏钒酸钠、偏钒酸钾、正钒酸钠、氯化钒、氧化钒、四氯化钒或钒酸钠中的一种。
优选的是，步骤(1)中所述的金属盐A与还原剂成摩尔比1:2～10。
优选的是，步骤(1)中所述的有机碳源B溶液与为有机碳源B与去离子水的体积比为1:2～4混合后所得；所述的有机碳源B为乙二醇、甲醇、乙醇、异丙醇、丙三醇、正丁醇、N,N-二甲基甲酰胺、油胺、油酸、聚乙二醇、甲苯、乙腈、N,N-二甲基乙酰胺、二甲基亚砜、吡啶、吡咯、尿素、苯胺、N-甲基苯胺、N,N-二甲基苯胺、N-乙基苯胺、N,N-二乙基苯胺、二苯胺、盐酸苯胺、二氧二甲基嘌呤、苯丙氨酸、2-羟基吡啶、2-氨基吡啶、2,6-二氨基吡啶2-甲基吡啶、3-氨基吡啶、4-甲基吡啶、五氯吡啶、3-氯吡啶、3-氟吡啶、3-溴吡啶、2,3-二氨基吡啶、2-氨基-3-氯吡啶、2-吡咯烷酮、2-吡咯羧酸、3-乙酰基-2,4-二甲基吡咯、羟乙基吡咯烷酮、2-乙酰基吡咯、1-甲基吡咯、四氢吡咯、吡咯-2-羧酸乙酯、2,4-二甲基吡咯、4-乙酰吡啶、2-乙酰吡咯、N-甲基吡咯单磷酸氟达拉滨、1-丁基-3-甲基咪唑六氟磷酸盐、1-丁基-3-甲基咪唑六氟磷酸盐或离子交换树脂中的一种或两种混合。
优选的是，步骤(1)中所述的液相反应为在室温下，将还原剂滴入到有机碳源B和金属盐溶液A的混合溶液中，然后搅拌2～12小时。
优选的是，步骤(1)中所述的溶剂热反应为将还原剂滴入到有机碳源B和金属盐溶液A的混合溶液中，搅拌均匀，然后将混合溶液转移到聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在100～180摄氏度下反应6～12小时，冷却至室温后取出所得物质。
优选的是，步骤(1)中所述的还原剂为硼氢化钠、水合肼、硼氢化钾、乙二醇、聚乙烯吡咯烷酮、正丙醇、正丁醇、乙醇、三甘醇、四甘醇、1,2-十六二醇、1,4-丁二醇、1,4-戊二醇、对苯二酚、甲醛、苯甲醛、乙酸、草酸、苹果酸、抗坏血酸、维生素、柠檬酸、甲酸、联氨、羟胺、苯胺、吡啶、N,N-二甲基甲酰胺(DMF)或N,N-二甲基乙酰胺(DMAC)中的一种。
优选的是，步骤(1)中所述的清洗后的样品与强碱的质量与之比为1:2～10。
优选的是，步骤(1)中所述的强碱为碳酸钾、碳酸钠、氢氧化钠、氢氧化钾或胆碱中的至少一种，混合时比例任意。
优选的是，步骤(2)中所述的金属盐溶液D为金属盐D溶于水中得到金属盐溶液；所述的金属盐D为铂盐、铑盐、钯盐、金盐、钌盐、铱盐中的至少一种，两种及两种以上混合时比例任意；所述的铂盐为六氯铂酸铵、氯亚铂酸钾、二氯化铂、六氯铂酸钾、四氯化铂、四氨合氯化铂、二氯化铂、四碘化铂、四氨合硝酸铂、二亚硝基二氨铂、(1,2-二氨基环己烷)二氯化铂、氯化铂、四氰基铂酸钾、六氯代铂酸钠、顺-二胺二氯铂、氢化六氯铂酸盐、双(2,4-戊二酮酸)铂、乙酰丙酮铂、乙二胺氯化铂、(1,5-环辛二烯)二氯或氯亚铂酸铵中的一种；所述的铑盐为乙酰丙酮铑、氯化铑、醋酸铑、碘化铑、辛酸铑、氯铑酸铵、二羰基乙酰丙酮铑、四(三苯基膦)氢化铑、二(1,5-环辛二烯)四氟硼酸铑、(1,5-环辛二烯)氯铑四羰基二氯化二铑、辛酸铑二聚体、三乙酰丙酮铑、双环辛烯氯化铑二聚体、六氯铑酸钾、二-Μ-氯-四羰基二铑、水合五氯铑酸铵、乙酸铑二聚物、六氯代铑酸钠、水合六氯铑酸铵、双(三苯基膦)合氯化羰基铑或七氟丁酸铑二聚体中的一种；所述的钯盐为醋酸钯、碘化钯、乙酸钯、硝酸钯、硫酸钯、二溴化钯、氯亚钯酸铵、乙酰丙酮钯、四氯钯酸钠、氯钯酸钾、二氯二氨钯、四溴钯酸钾、六氟乙酰丙酮钯、二水硝酸钯、二氯四氨钯、溴化钯、氯钯酸钠、三氟乙酸钯、1,2-双(二环己基)乙烷钯氯化物或双(乙二胺)氯化钯中的一种；所述的金盐为乙酸金、碘化金、四氯铂酸钾、(三苯基膦)氯化金、氯化亚金、四氯金酸钠、溴化金、四氯金酸铵水合物、氯化金钾、氯化金、氯金酸、氢氧化金、氧化金、二氯[(±)-BINAP]二金(I)或双(氯金(I))双(二苯基膦)甲烷中的一种；所述的钌盐为乙酰丙酮钌、醋酸钌、三氯化钌、氯钌酸铵、六氯钌酸铵、氧化钌、碳酰(二氢)三(三苯膦基)钌、二氯苯基钌(II)二聚体、异丙基苯基二氯化钌、氯化六氨合钌、亚硝酰硝酸钌、(1,5-环辛二烯)二氯化钌、氯化三(2,2′-联吡啶)、高钌(VII)酸钾或六氯钌酸钾中的一种；所述的铱盐为醋酸铱、乙酰丙酮铱、溴化铱、氯化铱、氯铱酸铵、2,4-戊二酮酸铱、羰基氯化双(三苯基磷)铱、乙酰丙酮酸二(2-苯基吡啶)铱或六氯铱(IV)酸钾中的一种。
优选的是，步骤(2)中初级样品C与金属盐D之间的摩尔比是5～20:1。
优选的是，步骤(1)和(2)中所述的高温煅烧为升温速度为1～20摄氏度/分钟，煅烧温度为300～1000摄氏度，保温时间1～6小时；所述的混合气氛为氢气与氮气、氩气或氦气中的一种或几种的混合物，按照任意体积比混合且氢气含量不为零。
与现有技术相比，本发明具有如下有益效果：
(1)本发明制备所得碳包覆金属颗粒锚定纳米催化材料中的金属颗粒大小分布均匀，制备工艺简单，可作为高效电催化材料，具有较好的电催化活性和电化学稳定性；
(2)本发明制备所得催化材料充分利用了载体材料对于金属颗粒的锚定作用，有效的缓解了在电化学加速过程中金属颗粒由于迁移、脱落造成的催化剂失活现象，提高了催化剂的稳定性和使用寿命；
(3)本发明制备所得催化材料可广泛应用于燃料电池、金属-空气电池、电解水、电解废水等领域，并且适合大规模生产。
附图说明
图1是本发明方法的工艺流程图。
图2是根据本发明制备所得碳包覆金属颗粒锚定纳米催化材料产品示意图。
图3是根据本发明制备所得碳包覆金属颗粒锚定纳米催化材料在0.1摩尔/升高氯酸溶液中的氧还原(ORR)极化曲线图(LSV)。
图4是根据本发明制备所得碳包覆金属颗粒锚定纳米催化材料在1.0摩尔/升氢氧化钾溶液中的析氢(HER)极化曲线图(LSV)。
具体实施方式
下面结合附图具体实施方式进行详细描述，但应当理解本发明的保护范围并不受具体实施方式的限制。
实施例1
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将4.756g(0.02mol)六水合氯化镍溶解于80ml的去离子水中后进行磁力搅拌，搅拌均匀后所得氯化镍溶液即为金属盐溶液A，将20ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加7.566g(0.2mol)还原剂硼氢化钠进行还原反应，持续搅拌8小时，然后进行抽滤、用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将得到的样品加入的氢氧化钾溶液(10g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.518g(0.001mol)六水合氯铂酸溶解于100ml的去离子水中，混合均匀后所得氯铂酸溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例2
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将1.9g(0.008mol)六水合氯化镍、1.904g(0.008mol)六水合氯化钴和1.08g(0.004mol)六水合氯化铁溶解于80ml的去离子水中后进行磁力搅拌，搅拌均匀后所得氯化镍、氯化钴和氯化铁溶液即为金属盐溶液A，将40ml乙二醇溶液(乙二醇与去离子水的体积比1:2混合所得)加入金属盐溶液A中混合，然后再缓慢滴加7.566g(0.2mol)还原剂硼氢化钠进行还原反应，持续搅拌12小时，然后进行抽滤、用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将得到的样品加入的氢氧化钾溶液(10g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.225g(0.001mol)乙酸钯溶解于100ml的去离子水中，混合均匀后所得乙酸钯溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例3
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将5.14g(0.02mol)乙酰丙酮镍溶解于80ml的去离子水中后进行磁力搅拌，搅拌均匀后所得乙酰丙酮镍溶液即为金属盐溶液A，将20ml异丙醇溶液(异丙醇与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加7.566g(0.2mol)还原剂硼氢化钠进行还原反应，持续搅拌6小时，然后进行抽滤、用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将得到的样品加入的氢氧化钾溶液(50g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.259g(0.0005mol)六水合氯铂酸和0.105g(0.0005mol)水合三氯化铑溶解于100ml的去离子水中，混合均匀后所得氯铂酸和三氯化铑溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至300摄氏度，保温6小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例4
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)1.189g(0.005mol)六水合氯化镍溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得氯化镍溶液即为金属盐溶液A，将4ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)和0.375ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加1.892g(0.05mol)还原剂硼氢化钠进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在180摄氏度下反应12小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，将得到的样品加入的氢氧化钠溶液(10g NaOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得样品真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，将所粉末品清洗、真空干燥12小时后即得初级样品C；
(2)将0.518g(0.001mol)六水合氯铂酸溶解于100ml的去离子水中，混合均匀后所得氯铂酸溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例5
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将4.756g(0.02mol)六水合氯化镍溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得氯化镍溶液即为金属盐溶液A，将4ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)和0.375ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加10ml(0.2mol)还原剂水合肼进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在160摄氏度下反应8小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，将得到的样品加入的碳酸钾溶液(10g K2CO3溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.5564g(0.002mol)醋酸钌溶解于100ml的去离子水中，混合均匀后所得醋酸钌溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以10℃/min的速度升温至650摄氏度，保温2小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例6
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将0.1242g(0.005mol)四水合醋酸镍溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得醋酸镍溶液即为金属盐溶液A，将4ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)和0.375ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加2.5ml(0.5mol)还原剂水合肼进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在180摄氏度下反应6小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以20℃/min的速度升温至1000摄氏度，保温1小时后自然降温，将得到的样品加入的氢氧化钾溶液(20g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以20℃/min的速度升温至1000摄氏度，保温1小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将1.554g(0.003mol)六水合氯铂酸溶解于100ml的去离子水中，混合均匀后所得氯铂酸溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以20℃/min的速度升温至1000摄氏度，保温1小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例7
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将1.64g(0.005mol)乙酰丙酮钼、0.5623g(0.002mol)七水合硫酸钴和0.27g(0.001mol)六水合氯化铁溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得乙酰丙酮钼、硫酸钴和氯化铁混合溶液即为金属盐溶液A，将4ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)和0.375ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加2.5ml(0.05mol)还原剂水合肼进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在100摄氏度下反应12小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将得到的样品加入的氢氧化钾溶液(10g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.518g(0.001mol)六水合氯铂酸和0.105g(0.0005mol)水合三氯化铑溶解于100ml的去离子水中，混合均匀后所得氯铂酸和三氯化铑的混合溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例8
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将0.475g(0.002mol)六水合氯化镍、0.66g(0.002mol)二水钨酸钠和0.117g(0.001mol)偏钒酸铵溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得氯化镍、钨酸钠和偏钒酸铵的混合溶液即为金属盐溶液A，将4ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)和0.375ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加5ml(0.05mol)还原剂1,4-丁二醇进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在140摄氏度下反应8小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将得到的样品加入的氢氧化钾溶液(30g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.559g(0.001mol)醋酸铱和0.105g(0.0005mol)水合三氯化铑溶解于100ml的去离子水中，混合均匀后所得醋酸铱和三氯化铑的混合溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至450摄氏度，保温1小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例9
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将0.412g(0.002mol)钼酸钠、0.66g(0.002mol)二水钨酸钠和0.117g(0.001mol)偏钒酸铵溶解于80ml的去离子水中后进行磁力搅拌，搅拌均匀后所得钼酸钠、钨酸钠和偏钒酸铵的混合溶液即为金属盐溶液A，将19.5ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)、0.5ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加2.5ml(0.05mol)还原剂水合肼进行还原反应，持续搅拌2小时，然后进行抽滤、用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至650摄氏度，保温2小时后自然降温，将得到的样品加入的氢氧化钾溶液(10g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.317g(0.001mol)氯化铱和0.207g(0.0005mol)氯化钌溶解于100ml的去离子水中，混合均匀后所得氯化铱和氯化钌的混合溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
实施例10
一种碳包覆金属颗粒锚定纳米催化材料的制备方法，具体操作步骤如下：
(1)将0.412g(0.002mol)钼酸钠、0.66g(0.002mol)二水钨酸钠和0.117g(0.001mol)偏钒酸铵溶解于35ml的去离子水中后进行磁力搅拌，搅拌均匀后所得钼酸钠、钨酸钠和偏钒酸铵的混合溶液即为金属盐溶液A，将14ml乙二醇溶液(乙二醇与去离子水的体积比1:4混合所得)、0.5ml吡啶溶液(吡啶与去离子水的体积比1:4混合所得)加入金属盐溶液A中混合，然后再缓慢滴加2.5ml(0.05mol)还原剂水合肼进行还原反应，搅拌均匀，然后将搅拌后所得物质移入50ml聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在150摄氏度下反应10小时，冷却至室温后取出所得物质进行抽滤，用去离子水清洗，干燥后将得到的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将得到的样品加入的氢氧化钾溶液(5g KOH溶解于20ml的去离子水中)中进行刻蚀，刻蚀6小时后将所得物质真空干燥12小时，将干燥后所得物质移入管式炉中高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，然后再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，将所得粉末清洗、真空干燥12小时后即得初级样品C；
(2)将0.317g(0.001mol)氯化铱水合物和0.207g(0.0005mol)氯化钌溶解于100ml的去离子水中，混合均匀后所得氯化铱和氯化钌的混合溶液即为金属盐溶液D，然后将步骤(1)中的初级样品C溶解于金属盐溶液D中，磁力搅拌12小时在常温下进行置换反应，然后抽滤、用去离子水清洗，将抽滤后所得滤渣真空干燥12小时；将干燥好的样品移入管式炉进行高温煅烧，即以0.2ml/min的速度通入混合气体(5％氢气和95％氩气)30分钟后，再以5℃/min的速度升温至450摄氏度，保温2小时后自然降温，即得碳包覆金属颗粒锚定纳米催化材料。
图2是根据本发明制备所得碳包覆金属颗粒锚定纳米催化材料的微观结构，图中A表示属于非贵金属，即铁盐、钴盐、镍盐、钨盐、钼盐或钒盐；图中D表示属于贵金属，即铂盐、铑盐、钯盐、金盐、钌盐或铱盐。
图3表明本发明制备所得碳包覆金属颗粒锚定纳米催化材料在经过1万圈的稳定性测试后，氧还原(ORR)的活性依然很高。
图4表明本发明制备所得碳包覆金属颗粒锚定纳米催化材料在析氢(HER)方面的活性比20％Pt/C的商业催化剂还要好。
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式，并且很显然，根据上述教导，可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用，从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。
本发明的范围意在由权利要求书及其等同形式所限定。
Claims (7)
1.一种碳包覆金属颗粒锚定纳米催化材料的制备方法，其特征在于，包含以下操作步骤：
（1）配置金属盐溶液A，将有机碳源B溶液加入金属盐溶液A中，然后滴加还原剂进行还原反应，过滤、清洗，干燥后进行初步高温煅烧，得到的样品再加入强碱进行刻蚀，干燥后在混合气氛下高温煅烧得到初级样品C，所述的还原反应的方式为溶剂热反应；所述的溶剂热反应为将还原剂滴入到有机碳源B和金属盐溶液A的混合溶液中，搅拌均匀，然后将混合溶液转移到聚四氟乙烯内衬不锈钢高压釜中，然后放置鼓风干燥箱中，并在100~180摄氏度下反应6~12小时，冷却至室温后取出所得物质；所述的金属盐溶液A为金属盐A溶于水中得到金属盐溶液；所述的金属盐A为铁盐、钴盐、镍盐、钨盐、钼盐、钒盐中的至少一种，两种及两种以上混合时比例任意，其中有铁盐、钴盐或镍盐参与混合时三者中任一种混合比例不为零；所述的有机碳源B溶液为有机碳源B与去离子水的体积比为1:2~4混合后所得；所述的有机碳源B为乙二醇、甲醇、乙醇、异丙醇、丙三醇、正丁醇、N,N-二甲基甲酰胺、油胺、油酸、聚乙二醇、甲苯、乙腈、N,N-二甲基乙酰胺、二甲基亚砜、吡啶、吡咯、尿素、苯胺、N-甲基苯胺、N,N-二甲基苯胺、N-乙基苯胺、N,N-二乙基苯胺、二苯胺、盐酸苯胺、二氧二甲基嘌呤、苯丙氨酸、2-羟基吡啶、2-氨基吡啶、2,6-二氨基吡啶、2-甲基吡啶、3-氨基吡啶、4-甲基吡啶、五氯吡啶、3-氯吡啶、3-氟吡啶、3-溴吡啶、2,3-二氨基吡啶、2-氨基-3-氯吡啶、2-吡咯烷酮、2-吡咯羧酸、3-乙酰基-2,4-二甲基吡咯、羟乙基吡咯烷酮、2-乙酰基吡咯、1-甲基吡咯、四氢吡咯、吡咯-2-羧酸乙酯、2,4-二甲基吡咯、4-乙酰吡啶、2-乙酰吡咯、N-甲基吡咯单磷酸氟达拉滨、1-丁基-3-甲基咪唑六氟磷酸盐、1-丁基-3-甲基咪唑六氟磷酸盐或离子交换树脂中的一种或两种混合；
（2）配置金属盐溶液D，将步骤（1）所得初级样品C加入金属盐溶液D中，常温下进行置换反应，过滤、清洗、干燥，然后在混合气氛下高温煅烧，即得碳包覆金属颗粒锚定纳米催化材料。
2.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述的金属盐A与还原剂成摩尔比1:2~10。
3.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述的还原剂为硼氢化钠、水合肼、1,4-丁二醇中的一种。
4.根据权利要求1所述的制备方法，其特征在于：步骤（1）中清洗后的样品与强碱的质量与之比为1:2~10；所述的强碱为碳酸钾、碳酸钠、氢氧化钠、氢氧化钾或胆碱中的至少一种，混合时比例任意。
5.根据权利要求1所述的制备方法，其特征在于：步骤（1）中所述的铁盐为氯化亚铁、三氯化铁、乙酰丙酮铁、铁***、亚铁***、亚硝基亚铁***、二茂铁、硝酸铁、柠檬酸铁、柠檬酸铁铵、草酸高铁铵、草酸亚铁、六氰合铁酸钾、硫酸铁、硫酸亚铁、硫酸亚铁铵、硫酸高铁铵、乙基二茂铁、十二羰基三铁、醋酸铁或醋酸亚铁中的一种；所述的钴盐为氯化钴、乙酸钴、磷酸钴、酞菁钴、钴***、六氰钴酸钾、六氨基氯化钴、高氯酸钴、硝酸钴、氟化钴、碘化钴、溴化钴、亚硝酸钴钠、草酸钴、硫酸钴、硫酸亚钴、硫酸钴铵、环烷酸钴或乙酰丙酮钴中的一种；所述的镍盐为氯化镍、乙酰丙酮镍、乙酰丙酮酸镍、乙酸镍、溴化镍、碘化镍、硫酸镍、硝酸镍、硫酸镍铵、次磷酸镍、硝酸镍铵、氨基磺酸镍、碱式碳酸镍、甲酸镍、二茂镍、二(三苯基膦)溴化镍或双(三苯基膦)氯化镍中的一种；所述的钨盐为六羰基钨、异丙醇钨、偏钨酸铵、钨酸铵、钨酸钾、钨酸钠、磷钨酸、磷钨酸钠、钨硅酸、六氯化钨、六羰基钨、异丙醇钨或偏钨酸铵中的一种；所述的钼盐为六羰基钼、乙酰丙酮钼、异丙醇钼、四钼酸铵、七钼酸铵、二钼酸铵、钼酸钠、磷钼酸、磷钼酸铵、磷钼酸钠、氯化钼、钼酸锂或钼酸钾中的一种；所述的钒盐为三异丙醇氧钒、乙酰丙酮氧钒、三异丙氧基氧化钒、氧化二乙酰丙酮合钒、偏钒酸铵、偏钒酸钠、偏钒酸钾、正钒酸钠、氯化钒、氧化钒、四氯化钒或钒酸钠中的一种；步骤（2）中所述的金属盐溶液D为金属盐D溶于水中得到金属盐溶液；所述的金属盐D为铂盐、铑盐、钯盐、金盐、钌盐、铱盐中的至少一种，两种及两种以上混合时比例任意；所述的铂盐为六氯铂酸铵、氯亚铂酸钾、二氯化铂、六氯铂酸钾、四氯化铂、四氨合氯化铂、二氯化铂、四碘化铂、四氨合硝酸铂、二亚硝基二氨铂、(1,2-二氨基环己烷)二氯化铂、氯化铂、四氰基铂酸钾、六氯代铂酸钠、顺-二胺二氯铂、氢化六氯铂酸盐、双(2,4-戊二酮酸)铂、乙酰丙酮铂、乙二胺氯化铂、(1,5-环辛二烯)二氯或氯亚铂酸铵中的一种；所述的铑盐为乙酰丙酮铑、氯化铑、醋酸铑、碘化铑、辛酸铑、氯铑酸铵、二羰基乙酰丙酮铑、四(三苯基膦)氢化铑、二(1,5-环辛二烯)四氟硼酸铑、(1,5-环辛二烯)氯铑四羰基二氯化二铑、辛酸铑二聚体、三乙酰丙酮铑、双环辛烯氯化铑二聚体、六氯铑酸钾、二-Μ-氯-四羰基二铑、水合五氯铑酸铵、乙酸铑二聚物、六氯代铑酸钠、水合六氯铑酸铵、双（三苯基膦）合氯化羰基铑或七氟丁酸铑二聚体中的一种；所述的钯盐为醋酸钯、碘化钯、乙酸钯、硝酸钯、硫酸钯、二溴化钯、氯亚钯酸铵、乙酰丙酮钯、四氯钯酸钠、氯钯酸钾、二氯二氨钯、四溴钯酸钾、六氟乙酰丙酮钯、二水硝酸钯、二氯四氨钯、溴化钯、氯钯酸钠、三氟乙酸钯、1,2-双(二环己基)乙烷钯氯化物或双(乙二胺)氯化钯中的一种；所述的金盐为乙酸金、碘化金、四氯铂酸钾、(三苯基膦)氯化金、氯化亚金、四氯金酸钠、溴化金、四氯金酸铵水合物、氯化金钾、氯化金、氯金酸、氢氧化金、氧化金、二氯[(±)-BINAP]二金(I)或双(氯金(I))双(二苯基膦)甲烷中的一种；所述的钌盐为乙酰丙酮钌、醋酸钌、三氯化钌、氯钌酸铵、六氯钌酸铵、氧化钌、碳酰(二氢)三(三苯膦基)钌、二氯苯基钌(II)二聚体、异丙基苯基二氯化钌、氯化六氨合钌、亚硝酰硝酸钌、(1,5-环辛二烯)二氯化钌、氯化三(2,2′-联吡啶)、高钌(VII)酸钾或六氯钌酸钾中的一种；所述的铱盐为醋酸铱、乙酰丙酮铱、溴化铱、氯化铱、氯铱酸铵、2,4-戊二酮酸铱、羰基氯化双(三苯基磷)铱、乙酰丙酮酸二(2-苯基吡啶)铱或六氯铱(IV)酸钾中的一种。
6.根据权利要求1所述的制备方法，其特征在于：步骤（2）中初级样品C与金属盐D之间的摩尔比是5~20:1。
7.根据权利要求1所述的制备方法，其特征在于：步骤（1）和（2）中所述的高温煅烧为升温速度为1~20摄氏度/分钟，煅烧温度为300~1000摄氏度，保温时间1~6小时；所述的混合气氛为氢气与惰性气体混合所得，按照任意体积比混合且氢气含量不为零；所述的惰性气体为氮气、氩气或氦气中的一种或几种的混合物。
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