CN110449149A - 一种碳网络固载贵金属纳米颗粒材料的制备方法 - Google Patents
一种碳网络固载贵金属纳米颗粒材料的制备方法 Download PDFInfo
- Publication number
- CN110449149A CN110449149A CN201910570848.0A CN201910570848A CN110449149A CN 110449149 A CN110449149 A CN 110449149A CN 201910570848 A CN201910570848 A CN 201910570848A CN 110449149 A CN110449149 A CN 110449149A
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- China
- Prior art keywords
- chloride
- potassium
- acid
- sodium
- platinum
- Prior art date
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 33
- 239000002253 acid Substances 0.000 claims description 25
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 20
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 18
- 239000011591 potassium Substances 0.000 claims description 18
- 229910052700 potassium Inorganic materials 0.000 claims description 18
- 235000002639 sodium chloride Nutrition 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 15
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- 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 13
- 239000011734 sodium Substances 0.000 claims description 13
- 229910052708 sodium Inorganic materials 0.000 claims description 13
- XXVRGGCHZUCJCX-UHFFFAOYSA-N [Cl].[Rh] Chemical compound [Cl].[Rh] XXVRGGCHZUCJCX-UHFFFAOYSA-N 0.000 claims description 12
- 229910052763 palladium Inorganic materials 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- SIEBMRITFODZNV-UHFFFAOYSA-N Cl.[K].[Ru] Chemical compound Cl.[K].[Ru] SIEBMRITFODZNV-UHFFFAOYSA-N 0.000 claims description 3
- NZIGZHDIUCTKQH-UHFFFAOYSA-N Cl[Ru+2].[NH4+] Chemical compound Cl[Ru+2].[NH4+] NZIGZHDIUCTKQH-UHFFFAOYSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- HWNXEHYDQGFUNE-UHFFFAOYSA-N [Na].Cl.[Ru] Chemical compound [Na].Cl.[Ru] HWNXEHYDQGFUNE-UHFFFAOYSA-N 0.000 claims description 3
- WSLMHVFKYRAUMK-UHFFFAOYSA-N acetic acid;iridium Chemical compound [Ir].CC(O)=O WSLMHVFKYRAUMK-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- -1 chlorauride Chemical compound 0.000 claims description 3
- NQNFKQOIDNMNBB-UHFFFAOYSA-L dichloroplatinum;triphenylphosphane Chemical compound Cl[Pt]Cl.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NQNFKQOIDNMNBB-UHFFFAOYSA-L 0.000 claims description 3
- JQTYQMMCROYLPI-UHFFFAOYSA-N dipotassium;platinum(2+);tetracyanide;trihydrate Chemical compound O.O.O.[K+].[K+].[Pt+2].N#[C-].N#[C-].N#[C-].N#[C-] JQTYQMMCROYLPI-UHFFFAOYSA-N 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 claims description 3
- WDZVNNYQBQRJRX-UHFFFAOYSA-K gold(iii) hydroxide Chemical compound O[Au](O)O WDZVNNYQBQRJRX-UHFFFAOYSA-K 0.000 claims description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- 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 3
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 3
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 claims description 3
- 229910001630 radium chloride Inorganic materials 0.000 claims description 3
- 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 3
- 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 claims description 3
- YWFDDXXMOPZFFM-UHFFFAOYSA-H rhodium(3+);trisulfate Chemical compound [Rh+3].[Rh+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YWFDDXXMOPZFFM-UHFFFAOYSA-H 0.000 claims description 3
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940071536 silver acetate Drugs 0.000 claims description 3
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 3
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 3
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 claims description 3
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 3
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- AOFZMTDNRXMXOR-UHFFFAOYSA-L Cl[Pt](Cl)C1=CC=CC=C1 Chemical compound Cl[Pt](Cl)C1=CC=CC=C1 AOFZMTDNRXMXOR-UHFFFAOYSA-L 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- RPOYPGDEQYFZNE-UHFFFAOYSA-J [Cl-].[Na+].[Ir+3].[Cl-].[Cl-].[Cl-] Chemical compound [Cl-].[Na+].[Ir+3].[Cl-].[Cl-].[Cl-] RPOYPGDEQYFZNE-UHFFFAOYSA-J 0.000 claims description 2
- HKSGQTYSSZOJOA-UHFFFAOYSA-N potassium argentocyanide Chemical compound [K+].[Ag+].N#[C-].N#[C-] HKSGQTYSSZOJOA-UHFFFAOYSA-N 0.000 claims description 2
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 claims description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- ARHBWGMHXPPGCZ-UHFFFAOYSA-N [K].[Au](C#N)(C#N)C#N Chemical compound [K].[Au](C#N)(C#N)C#N ARHBWGMHXPPGCZ-UHFFFAOYSA-N 0.000 claims 1
- 229960002737 fructose Drugs 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000003054 catalyst Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000005715 Fructose Substances 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZDPCYBPGTYHQJT-UHFFFAOYSA-N N(=O)[Pt](N)N Chemical compound N(=O)[Pt](N)N ZDPCYBPGTYHQJT-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RBNNPWUKDNRSMD-UHFFFAOYSA-N [Cl].[Ir] Chemical compound [Cl].[Ir] RBNNPWUKDNRSMD-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 235000017168 chlorine Nutrition 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- NEYLGXVZJUUZMY-UHFFFAOYSA-K potassium;trichlorogold Chemical compound [K].Cl[Au](Cl)Cl NEYLGXVZJUUZMY-UHFFFAOYSA-K 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/23—
-
- B01J35/33—
-
- B01J35/393—
-
- B01J35/399—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B01J37/088—Decomposition of a metal salt
Abstract
本发明涉及一种碳网络固载贵金属纳米颗粒材料的制备方法,包括下列步骤:将水溶盐、碳源、贵金属前驱体按照一定配比溶于水,得到混合溶液;干燥得到混合粉末;将(2)中所得粉末,在保护气和氢气的混合气氛下,加热到350~1200℃,保温一段时间后,进行碳源的碳化及贵金属前驱体的分解,随炉冷却至室温,得到粉末状混合物;将(3)中混合物清洗后干燥,得到碳网络固载贵金属纳米颗粒的复合材料。
Description
技术领域
本发明涉及一种碳网络固载贵金属纳米颗粒材料的制备方法,属于先进材料领域。
背景技术
贵金属(如铂、铑、钯、钌、金等)是重要的催化剂,在化工、能源、环保等领域都有着重要应用。为了提高催化剂的反应活性,目前主流方法是减小催化剂的颗粒尺寸,从而提升活性表面积,提高催化剂利用效率。在化工合成,水解产氢,有机物分解,燃料电池等领域,都可以见到贵金属纳米颗粒催化剂的应用。比如,氢气燃料电池用的铂催化剂要求其纳米颗粒粒径在3~5纳米。
然而,纳米颗粒存在很多问题,包括制备环节不易分散,使用过程会发生团聚,并且离散的纳米颗粒也存在着电子传导效率差等不足。因此,可采用将催化剂纳米颗粒负载于特定载体的方式,改善如上问题。
催化剂载体作为催化剂活性组分的骨架,负责支撑活性组分,使活性组分得到分散,同时还可以增加催化剂的强度。常用的载体有氧化铝、硅胶、活性碳等。然而金属或者无机物载体往往受限于反应体系的酸碱环境,不易做成通用型载体。与之相比,碳材料的化学稳定性较好。目前,常见的贵金属催化剂载体有活性碳、炭黑等。然而,这些传统的碳材料孔结构分布多为微孔,无法充分与液态、气态反应物接触,并存在离子传输效率低等问题。而且,这些材料的制备成本较高,结构可控性差。
碳网络是一种具有三维连通纳米结构的碳材料,兼具大比表面积、高导电性等特点。相较于传统碳材料,碳网络的连通结构特别适合于反应物的充分接触,并可改善离子的传质过程。这些优势使得碳网络材料成为一种极具潜力的催化剂载体。
综上,开发一种碳网络固载贵金属纳米颗粒的复合材料,其中比表面积高、孔径分布优良碳网络载体可充分发挥贵金属纳米颗粒的催化性能。该材料将具有很高的应用价值。
发明内容
本发明目的是开发一种碳网络固载贵金属纳米颗粒的复合材料制备方法,具体技术方法是利用水溶盐作为模板,结合高温碳化工艺实现目标材料制备。技术方案如下:
一种碳网络固载贵金属纳米颗粒材料的制备方法,包括下列步骤:
(1)将水溶盐、碳源、贵金属前驱体按照一定配比溶于水,得到混合溶液;
(2)将(1)中所得混合溶液进行干燥得到混合粉末;
(3)将(2)中所得粉末,在保护气和氢气的混合气氛下,加热到350~1200℃,保温一段时间后,进行碳源的碳化及贵金属前驱体的分解,随炉冷却至室温,得到粉末状混合物;
(4)将(3)中混合物清洗后干燥,得到碳网络固载贵金属纳米颗粒的复合材料。
(1)中将水溶盐、碳源、贵金属前驱体按照(0.5~50):(0.01~10):(0.01~10)的比例溶于水。水溶盐为氯化钠、碳酸钠、硅酸钠、硫酸钠、氯化钾、硫酸钾、硫酸钙、碳酸钾、氯化钙、碳酸钙的一种或多种组合。所述碳源包括葡萄糖,蔗糖,果糖、柠檬酸,聚乙烯醇,酒石酸,明胶中的一种或多种组合。(1)中所述贵金属前驱体包括氯铂酸、氯铂酸钾、氯铂酸钠、氯铂酸铵、铂硫醇盐、四铂***、二亚硝基二氨铂、氰化铂、硝酸铂、氯化铂、二腈苯基二氯化铂、三苯基膦氯化铂、氯化铑、三氯化铑、氯铑酸、硫酸铑、硝酸铑、醋酸铑、氯铑酸钾、氯铑酸钠、氯铑酸铵、硝酸钯、氯化钯、硫酸钯、氯钯酸钾、氯钯酸钠、氯钯酸铵、氯化钌、三氯化钌、氯钌酸钾、氯钌酸钠、氯钌酸铵、氯铱酸、三氯化铱、醋酸铱、氯铱酸铵、氯铱酸钾、氯铱酸钠、氯化金、氯金酸、氢氧化金、氯金酸钾、氯金酸铵、氯金酸钠、氰化金钾,硝酸银、氯化银、醋酸银、碳酸银、硫酸银、磷酸银、氰化银钾的一种或多种组合。(3)中加热到500-700℃。
与现有技术相比,本发明的有益效果是:所用原料丰富、工艺简单、产量高。所制得的材料中贵金属纳米粒颗粒分布均匀,颗粒的直径在0.5~100nm范围内可控,充分发挥贵金属纳米颗粒的催化性能;碳网络具有大比表面积和超薄的纳米片层结构,这种碳结构作为贵金属颗粒的载体,可以防止其团聚,并同时改善离子传输和电子传导过程。
附图说明
图1为本发明实施例一所制备碳网络固载铂纳米颗粒材料的实物图
图2为本发明实施例一所制得碳网络固载铂纳米颗粒材料的透射电子显微镜图
图3为本发明实施例一所制得碳网络上所固载铂纳米颗粒的透射电子显微镜图
图4为本发明实施例一所制备碳网络固载铂纳米颗粒材料在1M KOH溶液中测得析氢反应电化学性能图
具体实施方式
首先对本发明的技术路线进行说明:将盐类分散于水中,然后加入碳源和贵金属催化剂前驱体,混合均匀后,通过干燥,高温煅烧,水洗去除盐等工艺,得到所述复合材料,工艺如下:
(1)将水溶盐、碳源、贵金属前驱体按照质量比(0.5~50):(0.01~10):(0.01~10)的比例溶于水,得到混合溶液。所述水溶盐类包括但不限于氯化钠、碳酸钠、硅酸钠、硫酸钠、氯化钾、硫酸钾、硫酸钙、碳酸钾、氯化钙、碳酸钙的一种或多种组合;所述碳源包括但不限于葡萄糖,蔗糖,果糖、柠檬酸,聚乙烯醇,酒石酸,明胶中的一种或多种组合;所述贵金属前驱体包括但不限于氯铂酸、氯铂酸钾、氯铂酸钠、氯铂酸铵、铂硫醇盐、四铂***、二亚硝基二氨铂、氰化铂、硝酸铂、氯化铂、二腈苯基二氯化铂、三苯基膦氯化铂、氯化铑、三氯化铑、氯铑酸、硫酸铑、硝酸铑、醋酸铑、氯铑酸钾、氯铑酸钠、氯铑酸铵、硝酸钯、氯化钯、硫酸钯、氯钯酸钾、氯钯酸钠、氯钯酸铵、氯化钌、三氯化钌、氯钌酸钾、氯钌酸钠、氯钌酸铵、氯铱酸、三氯化铱、醋酸铱、氯铱酸铵、氯铱酸钾、氯铱酸钠、氯化金、氯金酸、氢氧化金、氯金酸钾、氯金酸铵、氯金酸钠、氰化金钾,硝酸银、氯化银、醋酸银、碳酸银、硫酸银、磷酸银、氰化银钾的一种或多种组合。
(2)将(1)中所得混合溶液进行干燥得到混合粉末。所述干燥方式包括如下:①冷冻干燥:将混合溶液置于-5~-200℃进行冷冻,随后将冷冻所得固体置于冷冻干燥机中,在真空环境中进行冷冻干燥12~72小时;②加热烘干:将混合溶液置于50~100℃烘箱中12~200小时;③喷雾干燥:将混合溶液通过80~200℃的喷雾干燥方式去除水份。
(3)将(2)中所得粉末置于管式炉中,在氩气、氮气、氢气的一种或多种混合气氛下,以0.5~500℃/min的升温速率加热到350~1200℃,保温0.01~12小时,进行碳源的碳化及贵金属前驱体的分解,随炉冷却至室温,得到粉末状混合物。
(4)将(3)中混合物使用去离子水抽滤洗涤,并将抽滤产物在50~100℃干燥箱中干燥5~72小时,得到碳网络固载贵金属纳米颗粒的复合材料。
下面结合实施例对本发明作进一步描述,这些实施例只是用于说明本发明,并不限制本发明。
实施例一
将氯化钠、葡萄糖、氯铂酸钾按照质量比2:0.1:0.05的比例溶于水,得到混合溶液。将混合溶液置于液氮中进行冷冻,并转移至冷冻干燥机(真空度<50Pa,冷阱温度-50℃)中,进行冷冻干燥12小时,得到混合固体粉末。将该固体粉末置于管式炉中,在200ml/min的氩气气氛下,以50℃/min的升温速率加热到650℃,保温10分钟,进行碳源的碳化及铂前驱体的分解,随炉冷却至室温,得到粉末状混合物。混合物使用去离子水抽滤洗涤,并将抽滤产物在60℃干燥箱中干燥48小时,得到碳网络固载铂纳米颗粒材料。
实施例二
将氯化钙、蔗糖、氯钯酸钠、水按照质量比1:0.5:0.01的比例溶于水,得到混合溶液。将混合溶液置于80℃烘箱中72小时,得到混合固体粉末。将该固体粉末置于管式炉中,在50ml/min氩气与50ml/min氢气的混合气氛下,以5℃/min的升温速率加热到700℃,保温1小时,进行碳源的碳化及铂前驱体的分解,随炉冷却至室温,得粉末状混合物。混合物使用去离子水抽滤洗涤,并将抽滤产物在80℃干燥箱中干燥24小时,得到碳网络固载钯纳米颗粒材料。
实施例三
将氯化钠、蔗糖、硝酸银、水按照质量比1:0.5:0.1的比例溶于水,得到混合溶液。将混合溶液通过150℃的喷雾干燥方式去除水份。将该固体粉末置于管式炉中,在100ml/min的氢气气氛下,以10℃/min的升温速率加热到600℃,保温2小时,进行碳源的碳化及铂前驱体的分解,随炉冷却至室温,得到粉末状混合物。混合物使用去离子水抽滤洗涤,并将抽滤产物在90℃干燥箱中干燥12小时,得到碳网络固载银纳米颗粒材料。
Claims (6)
1.一种碳网络固载贵金属纳米颗粒材料的制备方法,包括下列步骤:
(1)将水溶盐、碳源、贵金属前驱体按照一定配比溶于水,得到混合溶液。
(2)将(1)中所得混合溶液进行干燥得到混合粉末;
(3)将(2)中所得粉末,在保护气和氢气的混合气氛下,加热到350~1200℃,保温一段时间后,进行碳源的碳化及贵金属前驱体的分解,随炉冷却至室温,得到粉末状混合物;
(4)将(3)中混合物清洗后干燥,得到碳网络固载贵金属纳米颗粒的复合材料。
2.根据权利要求1所述的制备方法,其特征在于,(1)中将水溶盐、碳源、贵金属前驱体按照(0.5~50):(0.01~10):(0.01~10)的比例溶于水。
3.根据权利要求1所述的制备方法,其特征在于,(1)中,水溶盐为氯化钠、碳酸钠、硅酸钠、硫酸钠、氯化钾、硫酸钾、硫酸钙、碳酸钾、氯化钙、碳酸钙的一种或多种组合。
4.根据权利要求1所述的制备方法,其特征在于,(1)中所述碳源包括葡萄糖,蔗糖,果糖、柠檬酸,聚乙烯醇,酒石酸,明胶中的一种或多种组合。
5.根据权利要求1所述的制备方法,其特征在于,(1)中所述贵金属前驱体包括氯铂酸、氯铂酸钾、氯铂酸钠、氯铂酸铵、铂硫醇盐、四铂***、二亚硝基二氨铂、氰化铂、硝酸铂、氯化铂、二腈苯基二氯化铂、三苯基膦氯化铂、氯化铑、三氯化铑、氯铑酸、硫酸铑、硝酸铑、醋酸铑、氯铑酸钾、氯铑酸钠、氯铑酸铵、硝酸钯、氯化钯、硫酸钯、氯钯酸钾、氯钯酸钠、氯钯酸铵、氯化钌、三氯化钌、氯钌酸钾、氯钌酸钠、氯钌酸铵、氯铱酸、三氯化铱、醋酸铱、氯铱酸铵、氯铱酸钾、氯铱酸钠、氯化金、氯金酸、氢氧化金、氯金酸钾、氯金酸铵、氯金酸钠、氰化金钾,硝酸银、氯化银、醋酸银、碳酸银、硫酸银、磷酸银、氰化银钾的一种或多种组合。
6.根据权利要求1所述的制备方法,其特征在于,(3)中加热到500-700℃。
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