CN108927154A - 一种金属间化合物纳米催化剂的制备方法 - Google Patents
一种金属间化合物纳米催化剂的制备方法 Download PDFInfo
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- CN108927154A CN108927154A CN201810635342.9A CN201810635342A CN108927154A CN 108927154 A CN108927154 A CN 108927154A CN 201810635342 A CN201810635342 A CN 201810635342A CN 108927154 A CN108927154 A CN 108927154A
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- 229910000765 intermetallic Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 11
- -1 salt salt Chemical class 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 40
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 28
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 claims description 8
- PDZGAEAUKGKKDE-UHFFFAOYSA-N lithium;naphthalene Chemical compound [Li].C1=CC=CC2=CC=CC=C21 PDZGAEAUKGKKDE-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- URXNVXOMQQCBHS-UHFFFAOYSA-N naphthalene;sodium Chemical compound [Na].C1=CC=CC2=CC=CC=C21 URXNVXOMQQCBHS-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052752 metalloid Inorganic materials 0.000 claims description 3
- 150000002738 metalloids Chemical class 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 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 2
- JJHHIJFTHRNPIK-UHFFFAOYSA-N Diphenyl sulfoxide Chemical compound C=1C=CC=CC=1S(=O)C1=CC=CC=C1 JJHHIJFTHRNPIK-UHFFFAOYSA-N 0.000 claims description 2
- 239000012448 Lithium borohydride Substances 0.000 claims description 2
- 229910016285 MxNy Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 150000002344 gold compounds Chemical class 0.000 claims 1
- 229910052745 lead Inorganic materials 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 229910052718 tin Inorganic materials 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 238000010992 reflux Methods 0.000 abstract 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 51
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000005406 washing Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000002604 ultrasonography Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000006228 supernatant Substances 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 5
- 239000000084 colloidal system Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910000907 nickel aluminide Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229910006119 NiIn Inorganic materials 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 241000251730 Chondrichthyes Species 0.000 description 1
- 229910019043 CoSn Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- 229910003310 Ni-Al Inorganic materials 0.000 description 1
- 229910001005 Ni3Al Inorganic materials 0.000 description 1
- 229910000943 NiAl Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000007868 Raney catalyst Substances 0.000 description 1
- 229910000564 Raney nickel Inorganic materials 0.000 description 1
- 229910008336 SnCo Inorganic materials 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- QNZRVYCYEMYQMD-UHFFFAOYSA-N copper;pentane-2,4-dione Chemical compound [Cu].CC(=O)CC(C)=O QNZRVYCYEMYQMD-UHFFFAOYSA-N 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000010742 number 1 fuel oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 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 description 1
- 239000000123 paper Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/825—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with gallium, indium or thallium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/44—Hydrogenation of the aromatic hydrocarbons
- C10G45/46—Hydrogenation of the aromatic hydrocarbons characterised by the catalyst used
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- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/44—Hydrogenation of the aromatic hydrocarbons
- C10G45/46—Hydrogenation of the aromatic hydrocarbons characterised by the catalyst used
- C10G45/48—Hydrogenation of the aromatic hydrocarbons characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/44—Hydrogenation of the aromatic hydrocarbons
- C10G45/46—Hydrogenation of the aromatic hydrocarbons characterised by the catalyst used
- C10G45/52—Hydrogenation of the aromatic hydrocarbons characterised by the catalyst used containing platinum group metals or compounds thereof
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种金属间化合物纳米催化剂的制备方法，属于催化新材料技术领域。将金属M对应盐与金属N对应盐以摩尔比1:3‑3:1溶解在醚类溶剂中。然后向双金属盐溶液中快速或缓慢加入强还原剂，其中强还原剂物质的量过量10％‑50％。对还原产物直接洗涤或转移至高沸点溶剂回流后洗涤。所得产品经真空干燥，得到金属间化合物纳米催化剂材料。本方法制备工艺简单易行，粒径小，活性位点暴露多，所得纳米级金属间化合物催化剂对芳香烃化合物具有高选择加氢性能。
Description
技术领域
本发明属于催化新材料技术领域，具体来说，属于一种纳米级金属间化合物催化剂的制备方法。
背景技术
当前，随着各国工业化水平飞速发展，能源消耗速率与日剧增，全球化石资源短缺匮乏，迫使人类必须提高化石能源的利用率且积极寻找新型可替代能源。在液煤和柴油中存在的萘，会降低燃料的稳定。萘的异构氢化反应可以提升液煤和柴油燃料质量。四氢萘,是一种非常有用的精细化学品，广泛用于油漆、涂料、油墨、医药、和纸张领域。将萘高效转化为四氢萘，该工艺不仅可以提高燃料的稳定性，而且可降低有害固体颗粒的排放，符合资源高效利用，且有利于保护环境。
在目前科学研究中，有各种类型的催化剂用于芳香烃及炔烃化合物的选择加氢反应中。金属间化合物作为一种具有高效选择性的催化剂，其在选择加氢中的应用也越来越广泛。金属间化合物可以通过粉末冶金法、电弧融化法、感应加热法制备。在催化反应中时，常常需要获得大比表面积，以增加活性位点，因此通常还要经过球磨或者粉碎等后处理，但是一般情况下仍旧无法制备出纳米级材料。因此，材料晶粒尺寸的纳米化有望大幅改善材料的力学性能及催化性能等，例如纳米化可以解决金属间化合物的室温脆性问题，并且可以增加材料的活性位点，提高催化剂性能。通常情况下，制备金属间化合物往往需要经过高温处理，而高温处理带来的必然是金属间化合物的晶粒增大。因此能在常温下制备纳米级金属间化合物成为新的挑战和研究热点。
中国专利CN102477503公开了一种纳米晶镍铝金属间化合物制备方法，以重量分数分别为66-92％镍，11-33％铝的粉状混合物，球磨6-13h后，在350℃-450℃下保温，通入6-8Mpa惰性气体后引燃。该方法虽然反应迅速，但是在高温条件下较为耗能，且引入的引燃剂中含有铝粉，对于镍铝金属间化合物的化学计量比无法精准控制，引燃剂也为后续分离带来繁琐的处理工作。
中国专利CN104415753公开了一种直接合成双金属纳米材料的方法，主要在醋酸、水中的一种或两种以上的溶剂，以包覆金属间化合物、内核金属化合物、表面活性剂为原料，通过氢气还原，在1～160℃下合成双金属纳米材料的方法。该方法虽然实现了一步合成，但是引入了表面活性剂，在后续处理过程中并未去除，即制得的纳米催化剂材料不够纯净。
中国专利CN101343043A公开了一种两性金属化合物纳米材料制备方法，该方法在制备过程中需要加入表面活性剂(十六烷基三甲基氯化铵、聚乙二醇等)作为分散剂，且纳米颗粒尺寸由5-50nm不定，纳米棒直径为10-100纳米，纳米片厚度为5-100纳米，纳米单元组成的纳米球直径为0.2微米至3微米，制备的力度尺寸较为不均。
发明内容
本发明提供了一种金属间化合物纳米催化剂的制备方法。针对目前金属间化合物需在高温下合成提供一种简单有效的解决办法，该方法利用共还原原理，获得纯度高，形貌均一，催化性能优越的PtCu，PtIn，PdIn，NiAl，NiIn等金属间化合物纳米材料。与其他方法相比，优势在于室温条件下合成，对于金属间化合物的尺寸有较好的控制，避免高温下金属间化合物发生团聚导致的粒径增大等问题。
本发明的技术方案：
一种金属间化合物纳米催化剂的制备方法，所述的金属间化合物纳米催化剂为MxNy，其中M、N为Mo、Re、Rh、Pt、Fe、Ni、Cu等过渡金属及Al、In、Si、Pb、P、Sb等第ⅢA-第ⅤA金属与准金属，M、N不同；步骤如下：(1)将金属M对应的盐与金属N对应的盐按照摩尔比为1:3-3:1溶解在四氢呋喃、二甘醇二甲醚或乙二醇二甲醚中，混合均匀，得到双金属盐溶液；(2)将萘基锂、萘基钠、硼氢化钠、硼氢化钾、硼氢化锂或三乙基硼氢化锂中的一种强还原剂缓慢或快速加入至双金属盐溶液中，形成金属间化合物；其中，强还原剂物质的量过量10％-50％；(3)对步骤(2)中形成的金属间化合物先用正己烷洗涤，然后用甲醇、四氢呋喃、乙醇、水中的一种与正己烷的混合液洗涤，二者的体积比为3:1；未形成金属间化合物的转移至角鲨烷、二辛醚、二苯砜、二苯亚砜中的一种高沸点溶剂中回流，再对其洗涤，所得产品经真空干燥，得到金属间化合物纳米催化剂。
对于制备方法步骤(1)在于所述金属盐可为氯化物、乙酰丙酮络合物、乙酸络合物中的一种可溶金属盐，两种金属对应的盐相同或不同。
制备所得金属间化合物纳米催化剂主要用于芳香烃化合物的选择加氢反应。
本发明的有益效果：本方法制备工艺简单易行，粒径小，粒子分散良好，活性位点暴露多，所得纳米级金属间化合物催化剂对芳香烃化合物具有高选择加氢性能。
附图说明
图1为本发明产物PtCu的XRD衍射谱图。
图2为本发明产物PtIn的TEM图。
图3为本发明产物PdIn的XRD衍射谱图。
图4为铝化镍金属间化合物催化剂对萘的选择加氢数据图。
具体实施方式
下面将通过实施例来详述本发明，下面描述的实施例是示例性的，仅用于解释本发明，但本发明并不局限于这些实施例。
实施例1
取0.1309g(0.5mmol)乙酰丙酮铜与0.1967g(0.5mmol)乙酰丙酮铂加入15ml四氢呋喃中，搅拌。待其溶解后，取4.4mL 0.5mmol/L(10％过量)还原剂萘基锂快速加入到上述溶液中，反应3h，得到灰黑色胶体；利用氮气吹扫，油浴40℃下将四氢呋喃溶液蒸干；然后加入50ml正己烷洗涤，超声后离心；加入30ml甲醇与10ml正己烷混合液，超声洗涤并离心，重复此步骤3次，倒掉上清液，所得产品经真空干燥，得到PtCu金属间化合物纳米粒子。
该样品的XRD衍射如图1所示，与标准图谱完全一致，经根据谢乐公式计算分析可得平均粒径约为2.1nm，具有立方晶形。
实施例2
重复实施例一中的步骤,不同之处在于:取3.5mL 0.5mmol/L(10％过量)萘基锂，乙酰丙酮铂质量改为0.07866g(0.2mmol)，乙酰丙酮铜质量改为0.0157g(0.6mmol)，得到PtCu3金属间化合物纳米粒子。
实施例3
取0.0983g(0.25mmol)乙酰丙酮铂与0.0553g(0.25mmol)氯化铟加入20ml二甘醇二甲醚中，搅拌。待其溶解后，取3.0mL 0.5mmol/L(20％过量)还原剂萘基钠快速加入到上述溶液中，反应3h，得到灰黑色胶体；利用氮气吹扫，油浴60℃下将二甘醇二甲醚溶液蒸干；然后加入50ml正己烷洗涤，超声后离心；加入30ml四氢呋喃与10ml正己烷混合液，超声洗涤并离心，重复此步骤4次，倒掉上清液；所得产品经真空干燥，得到PtIn金属间化合物纳米粒子。
透射电镜图如图2所示，表征结果显示PtIn金属间化合物纳米粒子分散良好，形状均匀，平均粒径为3nm。
实施例4
取0.0914g(0.30mmol)乙酰丙酮钯与0.0664g(0.30mmol)氯化铟加入20ml乙二醇二甲醚中，搅拌。待其溶解后，取3.3mL 0.5mmol/L(10％过量)还原剂萘基钠快速加入到上述溶液中，反应3h，得到灰黑色胶体；利用氮气吹扫，油浴60℃下将乙二醇二甲醚溶液蒸干；然后加入50ml正己烷洗涤，超声后离心；加入30ml四氢呋喃与10ml正己烷混合液，超声洗涤并离心，重复此步骤3次；倒掉上清液；所得产品经真空干燥，得到PdIn金属间化合物纳米粒子。
该样品的XRD衍射如图3所示，与标准图谱完全一致，经根据谢乐公式计算分析可得平均粒径约为2.8nm，具有立方晶形。
实施例5
取0.2360g(0.60mmol)氯化镍与0.0664g(0.30mmol)氯化铟加入30ml四氢呋喃中，搅拌。待其溶解后，取5.5mL 0.5mmol/L(30％过量)还原剂萘基锂快速加入到上述溶液中，反应3h，得到灰黑色胶体；重复利用氮气吹扫，油浴40℃下将四氢呋喃溶液蒸干；然后加入30ml角鲨烷于300℃下回流3h，收集固体，加入正己烷洗涤，超声后离心；加入30ml乙醇与10ml正己烷混合液，超声洗涤并离心，重复此步骤3次，倒掉上清液；所得产品经真空干燥，得到NiIn金属间化合物纳米粒子。
实施例6
取0.0810g(0.60mmol)氯化镍与0.0258g(0.20mmol)氯化铝加入30ml四氢呋喃中，搅拌。待其溶解后，取5.0mL 0.5mmol/L(40％过量)还原剂萘基锂快速加入到上述溶液中，反应3h，得到灰黑色胶体；重复利用氮气吹扫，油浴40℃下将四氢呋喃溶液蒸干；然后加入30ml二辛醚于300℃下回流3h，收集固体，加入正己烷洗涤，超声后离心；加入30ml四氢呋喃与10ml正己烷混合液，超声洗涤并离心，重复此步骤4次，倒掉上清液；所得产品经真空干燥，得到Ni3Al金属间化合物纳米粒子。
实施例7
取0.0521g(0.20mmol)氯化锡与0.0260g(0.20mmol)氯化钴加入20m二甘醇二甲醚中，搅拌。待其溶解后，取0.0170g(50％过量)还原剂硼氢化钠缓慢加入到上述溶液中，反应4h，离心收集固体，加入正己烷洗涤，超声后离心；加入60ml水与20ml正己烷混合液，超声洗涤并离心，重复此步骤3次，倒掉上清液；所得产品经真空干燥，得到CoSn金属间化合物纳米粒子。
实施例8
取0.0546g(0.20mmol)氯化钼与0.0260g(0.20mmol)氯化钴加入20m乙二醇二甲醚中，搅拌。待其溶解后，取0.0283g(50％过量)还原剂硼氢化钾缓慢加入到上述溶液中，反应4h，离心收集固体，加入正己烷洗涤，超声后离心；加入60ml乙醇与20ml正己烷混合液，超声洗涤并离心，重复此步骤3次，倒掉上清液；所得产品经真空干燥，得到CoMo金属间化合物纳米粒子。
实施例9
取0.0811g(0.50mmol)氯化铁与0.0667g(0.50mmol)氯化铝加入40mL四氢呋喃中，搅拌。待其溶解后，取3.6mL 1mmol/L(20％过量)还原剂三乙基硼氢化锂溶液，缓慢加入到上述溶液中，反应4h，离心收集固体，加入正己烷洗涤，超声后离心；加入30ml四氢呋喃醇与10ml正己烷混合液，超声洗涤并离心，重复此步骤3次，倒掉上清液；所得产品经真空干燥，得到FeAl金属间化合物纳米粒子。
实施例10
化学计量比可控的纳米铝化镍金属间化合物催化剂在萘选择加氢反应中的催化性能研究。
以3wt％的萘为模型化合物进行选择加氢反应。反应在固定床中进行。
反应条件为：催化剂铝化镍：0.2g，反应压力4MPa，反应温度180～340℃,质量空速：1.88gcath gnaph -1，氢油比1:400。产物分析采用气相色谱，氢火焰检测器。铝化镍催化剂在450℃,100sccmAr气氛下煅烧3h，切换至氢气，充压至4Mpa于450℃下活化两小时。分别在不同温度下进行选择加氢反应，探究其催化活性，在反应温度为240℃，接触时间为1.88gcath gnaph -1，反应压力4MPa，氢油比1:400，转化率可达98％，选择性在99％。反应结果如图4所示。
实施例11
重复实施例十中的步骤,不同之处在于，以5wt％的萘为模型化合物考察CoMo金属间化合物催化剂的选择加氢反应。结果显示其在反应温度为300℃，接触时间为1.88gcathgnaph -1，反应压力4MPa，氢油比1:400，转化率可达85％，选择性达99％。
实施例12
重复实施例十中的步骤,不同之处在于，以3wt％的萘为模型化合物考察SnCo金属间化合物催化剂选择加氢反应。结果显示其在反应温度为240℃，接触时间2.56gcath gnaph -1，反应压力4MPa，氢油比1:400，转化率可达92％，选择性在98％以上。
Claims (5)
1.一种金属间化合物纳米催化剂的制备方法，其特征在于，所述的金属间化合物纳米催化剂为MxNy，M、N为过渡金属、第ⅢA-第ⅤA金属与准金属，M与N不相同；步骤如下：(1)将金属M对应的盐与金属N对应的盐按照摩尔比为1:3-3:1溶解在四氢呋喃、二甘醇二甲醚或乙二醇二甲醚中，混合均匀，得到双金属盐溶液；(2)将萘基锂、萘基钠、硼氢化钠、硼氢化钾、硼氢化锂或三乙基硼氢化锂中的一种强还原剂缓慢或快速加入至双金属盐溶液中，形成金属间化合物；其中，强还原剂物质的量过量10％-50％；(3)对步骤(2)中形成的金属间化合物先用正己烷洗涤，然后用甲醇、四氢呋喃、乙醇、水中的一种与正己烷的混合液洗涤，二者的体积比为3:1；未形成金属间化合物的转移至角鲨烷、二辛醚、二苯砜、二苯亚砜中的一种高沸点溶剂中回流，再对其洗涤，所得产品经真空干燥，得到金属间化合物纳米催化剂。
2.根据权利要求1所述的金属间化合物纳米催化剂的制备方法，其特征在于，其中M、N为Mo、W、Re、Fe、Co、Rh、Pt、Pd、Fe、Ni、Cu、Au、Ag、Al、In、Sn、Pb与准金属，M、N不同。
3.根据权利要求1或2所述的金属间化合物纳米催化剂的制备方法，其特征在于，所述金属对应的盐为氯化物、乙酰丙酮络合物、乙酸络合物中的任意一种可溶金属盐，两种金属对应的盐相同或不同。
4.根据权利要求1或2所述的金属间化合物纳米催化剂的制备方法，其特征在于，制备所得的金属间化合物纳米催化剂用于芳香烃化合物的选择加氢反应。
5.根据权利要求3所述的金属间化合物纳米催化剂的制备方法，其特征在于，制备所得的金属间化合物纳米催化剂用于芳香烃化合物的选择加氢反应。
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