CN107252682A - A kind of preparation method and applications for being used for organic carbon vapor phase growth for the catalyst of carbide - Google Patents
A kind of preparation method and applications for being used for organic carbon vapor phase growth for the catalyst of carbide Download PDFInfo
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- CN107252682A CN107252682A CN201710434753.7A CN201710434753A CN107252682A CN 107252682 A CN107252682 A CN 107252682A CN 201710434753 A CN201710434753 A CN 201710434753A CN 107252682 A CN107252682 A CN 107252682A
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- Prior art keywords
- catalyst
- compound
- organic carbon
- vapor phase
- carbide
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- 239000003054 catalyst Substances 0.000 title claims abstract description 102
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000001947 vapour-phase growth Methods 0.000 title claims abstract description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000007921 spray Substances 0.000 claims abstract description 30
- 230000003197 catalytic effect Effects 0.000 claims abstract description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 239000011777 magnesium Substances 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008139 complexing agent Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 230000001376 precipitating effect Effects 0.000 claims abstract description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 8
- 239000011733 molybdenum Substances 0.000 claims abstract description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010703 silicon Substances 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 24
- -1 acylate compound Chemical class 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 150000003377 silicon compounds Chemical class 0.000 claims description 4
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical group C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 239000004471 Glycine Substances 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
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 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
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000005323 carbonate salts Chemical class 0.000 claims description 2
- 238000005336 cracking Methods 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims 2
- 229940077388 benzenesulfonate Drugs 0.000 claims 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 239000008187 granular material Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 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 description 8
- 239000000463 material Substances 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 238000000975 co-precipitation Methods 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 3
- 239000001099 ammonium carbonate Substances 0.000 description 3
- 235000012501 ammonium carbonate Nutrition 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000007233 catalytic pyrolysis Methods 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N dimethylmethane Natural products CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical group [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000011787 zinc oxide 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
- B01J23/70—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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/10—Magnesium; Oxides or hydroxides thereof
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/75—Cobalt
-
- 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
- B01J23/755—Nickel
-
- 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
- B01J23/76—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
- B01J23/78—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 alkali- or alkaline earth metals
-
- 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
- B01J23/76—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
- B01J23/83—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 rare earths or actinides
-
- B01J35/613—
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a kind of for preparation method and applications of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：Into compound or compound containing catalytic elements, precipitating reagent or complexing agent or dispersant or precipitating reagent and dispersant or complexing agent and dispersant are added, the compound or compound containing catalytic elements are containing compound or their compound more than one or both of rare earth element, iron, cobalt, nickel, molybdenum, zirconium, copper, zinc, magnesium, aluminium, silicon；Synthesized by one or both of the precipitation method, complexometry, hydro-thermal method, high pressure hydro-thermal method, sol-gal process above method and the mixed liquor containing above-mentioned catalytic elements is made, mixed liquor is spray-dried by spray dryer and quickly removes the catalyst precursor that solvent formation catalytic elements nanomorphic is distributed, and catalyst precursor obtains the catalyst for organic carbon vapor phase growth for carbide after high-temperature calcination.
Description
Technical field
The present invention relates to a kind of preparation method of catalyst, and in particular to it is carbide that one kind, which is used for organic carbon vapor phase growth,
Catalyst preparation method, and its application.
Background technology
CNT, graphene or their compound are the important materials formed by carbon, and basic structural unit is
The carbene hexatomic ring that carbon atom is formed with sp2 hybrid forms, its mechanics, electricity and chemical property are excellent, are widely used.
At present, it is exactly catalytic pyrolysis and the carbon member by carbon containing organic gas to prepare one of main method of above-mentioned material
The deposition growing of element, this method yield is high, and preparation condition is controllable, is had an optimistic view of by people.Carbon containing organic gas catalytic pyrolysis chemical gaseous phase
In sedimentation, catalyst is mostly important factor, is widely studied.Patent CN02100709.8 passes through coprecipitation, height
Pressure hydro-thermal reaction, high-temperature calcination prepare CNT Fe-series catalyst；Patent CN03117874.X is prepared for containing by complexometry
Rare earth element iron system CNT Fe-series catalyst；CN201310370268.X is prepared for magnesium through-stone ink by high pressure hydro-thermal reaction
Alkene catalyst.Above-mentioned patent has all been successfully prepared out the catalyst of CNT, graphene, but catalyst preparation process is all adopted
With washing, filtering, evaporation, grinding, crushing common process, catalyst granules form is uncontrollable, and catalytic elements are because for a long time
The skewness that technological operation and the evaporation of slow solvent easily form state of aggregation and caused, and thus largely pollute the useless of environment
Liquid, dust the like waste.
The content of the invention
The technical problems to be solved by the invention be in view of the shortcomings of the prior art there is provided a kind of technique it is simple and environmentally-friendly, urge
Catalyst particles form is controllable, catalytic elements are evenly distributed is used for preparation side of the organic carbon vapor phase growth for the catalyst of carbide
Method.
The technical problems to be solved by the invention are to additionally provide the application of Above-mentioned catalytic agent.
The technical problems to be solved by the invention are realized by following technical scheme, and the present invention is that one kind is used for
Organic carbon vapor phase growth is the preparation method of the catalyst of carbide, is characterized in, this method includes：
Into compound or compound containing catalytic elements, add precipitating reagent or complexing agent or dispersant or precipitating reagent and
Dispersant or complexing agent and dispersant, the compound or compound containing catalytic elements be containing rare earth element, iron, cobalt, nickel,
More than one or both of molybdenum, zirconium, copper, zinc, magnesium, aluminium, silicon compound or their compound；Compound or they answer
Compound is all solution, and its complexing agent presses the 20%-300% proportionings of required catalytic elements theoretical stoichiometric, preferably 50%-200%；
Precipitating reagent presses the 50%-150% of required catalytic elements theoretical stoichiometric proportioning, preferably 80%-120%；Dispersant presses solution matter
The 0.1%-10% proportionings of amount, preferably 0.25%-5%；Pass through the precipitation method, complexometry, hydro-thermal method, high pressure hydro-thermal method, sol-gal process
One or both of above method synthesis the mixed liquor containing above-mentioned catalytic elements is made, mixed liquor sprayed by spray dryer
The quick catalyst precursor for removing solvent formation catalytic elements nanomorphic distribution is dried, catalyst precursor passes through high-temperature calcination
The catalyst for organic carbon vapor phase growth for carbide is obtained afterwards.The Rare Earths in Catalyst element, iron, cobalt, nickel, molybdenum, zirconium,
Copper, the one or more of zinc oxide account for the ratio 0.01% ~ 95% of gross mass, magnesium, aluminium, Si oxide it is one or two kinds of with
On account for the ratio 5% ~ 100% of gross mass, 50 ~ 1500 microns of catalyst particle size scope, 10 ~ 1000 ㎡ of specific surface area/g.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
State be used for organic carbon vapor phase growth for carbide catalyst preparation method in, the rare earth element, iron, cobalt, nickel, molybdenum,
More than one or both of zirconium, copper, zinc, magnesium, aluminium, silicon compound or their compound be rare earth element, iron, cobalt, nickel,
Molybdenum, zirconium, copper, zinc, magnesium, aluminium, the oxide of silicon, hydroxide, chloride, cyanide, fluoride, nitrate, sulfate, silicic acid
More than one or both of salt, acylate compound or their compound.Acylate is ferric acetate or copper acetate.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, and the solute of the compound or compound is dense
Degree or solid content are 0.5%-95%, preferably 2%-50%.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, and the precipitating reagent is soluble hydroxide
It is more than one or both of thing, soluble carbonate salt and bicarbonate, soluble ammonium salt, ammonia, urea；The complexing agent is lemon
It is more than one or both of lemon acid, tartaric acid, glycine, the amine tetraacethyl of second two；The dispersant is sodium metaphosphate, alkylbenzene
Sodium sulfonate, polyvinyl alcohol, polyethylene glycol oxide, one polyoxypropylene of polyoxyethylene one polyoxyethylene-type three sections of copolymers, polyethylene adjoin
It is one or more kinds of in pyrrolidone.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, and the temperature of the spray dryer is 120
DEG C -400 DEG C, preferably 200 DEG C -300 DEG C.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, and the spray dryer is centrifugal spray dryer
One kind in dry machine, Pressuresprayingdrier or two/tri- fluid spray dryers.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, the catalyst precursor particle size range
50-1000 microns.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
That states is used in preparation method of the organic carbon vapor phase growth for the catalyst of carbide, the temperature of the high-temperature calcination for 300 DEG C-
1200 DEG C, calcination time is 1-24 hours.
In the preparation method for organic carbon vapor phase growth for the catalyst of carbide, made described in any of the above-described
The purposes of CNT, graphene or their compound is made in standby obtained catalyst in vapour deposition process.
The technical problems to be solved by the invention can also further be realized by following technical scheme, institute of the present invention
In the purposes stated, the root catalyst is placed in high-temperature service, is passed through seven carbon and following organic gas and inert gas, reproducibility
The mixture of gas, temperature control is at 600 DEG C -1200 DEG C, and organic carbon is through cracking deposition growing in catalyst surface, by separation
Purification, is made CNT, graphene or their compound, wherein high-temperature service is roller kilns, rotary furnace, fixed bed, shifting
Dynamic bed or fluid bed.
Compared with prior art, mixed liquor, Ran Houtong is first made in compound or compound containing catalytic elements by the present invention
Cross and be spray-dried the quick catalyst precursor for removing solvent formation catalytic elements nanomorphic distribution, organic carbon is obtained after high-temperature calcination
The catalyst of deposition growing is cracked, the processes such as washing, filtering, evaporation, grinding, crushing in customary preparation methods are eliminated, saved
About production cost, while make catalyst form controllable, avoids catalytic elements because of long-time technological operation and slow molten in addition
The uneven distribution to form state of aggregation and cause is evaporated in agent, and thus generation waste liquid, dust the like waste pollute asking for environment
Topic, its technique is simple and environmentally-friendly, it is easy to commercial introduction, using the catalyst can efficiently prepare CNT, graphene and it
Compound.
Brief description of the drawings
Fig. 1 is CNT high power transmission electron microscope photo obtained by the catalyst of embodiment 1；
Fig. 2 is CNT, graphene and its compound high power transmission electron microscope photo obtained by the catalyst of embodiment 5；
Fig. 3 is graphene high power transmission electron microscope photo obtained by the catalyst of embodiment 6；
Fig. 4 is CNT high power transmission electron microscope photo obtained by the catalyst of embodiment 7；
Fig. 5 is CNT, graphene and its compound high power transmission electron microscope photo obtained by the catalyst of embodiment 9；
Fig. 6 is CNT high power transmission electron microscope photo obtained by the catalyst of embodiment 10.
Embodiment
Concrete technical scheme of the invention described further below, in order to which those skilled in the art is further understood that
The present invention, without constituting the limitation to its right.
Embodiment 1, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
30% sodium hydroxide and 5% neopelex are added into 30% ferric nitrate containing catalytic elements by coprecipitation, high pressure
The mixed liquor of iron-containing catalyst precursor is made in hydro-thermal method, and the percentage of above material is mass percent concentration, mixed liquor
It is added in drying machine with centrifugal spray, is spray-dried at a temperature of 240 DEG C, the cyclone separator and cloth bag of drying machine with centrifugal spray
Deduster collection catalyst precursor, 60-150 microns of catalyst precursor particle diameter, after forged by rotary furnace at a temperature of 450 DEG C
Burn 3 hours, obtain 50-120 microns of particle diameter, specific surface area 90m2/ g catalyst granules, it is iron oxidation that catalyst, which is mainly constituted,
Thing (95%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 600-800 DEG C, be passed through methane and
The mixed gas of argon gas, you can CNT is made.
Embodiment 2, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
15% ammonium carbonate, 5% sodium phosphate are added into 10% cobalt chloride containing catalytic elements must be contained by coprecipitation, high pressure hydro-thermal legal system
The mixed liquor of Co catalysts precursor, the percentage of above material is mass percent concentration, and mixed liquor is added to centrifugation spray
In mist drying machine, it is spray-dried at a temperature of 280 DEG C, the cyclone separator and sack cleaner of drying machine with centrifugal spray, which are collected, urges
Agent precursor, 80-200 microns of catalyst precursor particle diameter, after by rotary furnace in 400 DEG C of temperature lower calcinations 2 hours, obtain
60-150 microns of particle diameter, specific surface area 60m2/ g catalyst granules, it is cobalt/cobalt oxide (90%) that catalyst, which is mainly constituted,.
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control is passed through ethene alkane at 650-850 DEG C
With the mixed gas of argon gas, you can CNT is made.
Embodiment 3, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
30% ammonium carbonate, 5% sodium metaphosphate are added into 20% nickel nitrate containing catalytic elements, 10% cobalt nitrate, by coprecipitation, high pressure
Iron content, the mixed liquor of Co catalysts precursor is made in hydro-thermal method, and the percentage of above material is mass percent concentration, mixing
Liquid is added in twin-fluid spray dryer, is spray-dried at a temperature of 220 DEG C, the cyclone separator of twin-fluid spray dryer
With sack cleaner collection catalyst precursor, 70-40 microns of catalyst precursor particle diameter, after by rotary furnace in 400 DEG C of temperature
The lower calcining of degree 2 hours, obtains 50 ~ 110 microns of particle diameter, specific surface area 100m2/ g catalyst granules, catalyst, which is mainly constituted, is
Iron, cobalt/cobalt oxide (98%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control is passed through propane alkane at 700-900 DEG C
With the mixed gas of nitrogen, you can CNT is made.
Embodiment 4, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
20% sodium hydroxide, 5% neopelex are added into 40% nickel nitrate containing catalytic elements, 20% magnesia, by altogether
The precipitation method, high pressure hydro-thermal legal system obtain the mixed liquor of nickeliferous Mg catalyst precursor, and the percentage of above material is quality percentage
Specific concentration, mixed liquor is added in drying machine with centrifugal spray, is spray-dried at a temperature of 250 DEG C, the rotation of drying machine with centrifugal spray
Wind separator and sack cleaner collection catalyst precursor, 60-120 microns of catalyst precursor particle diameter, after pass through rotary furnace
In 400 DEG C of temperature lower calcinations 2 hours, 50-110 microns of particle diameter, specific surface area 180m are obtained2/ g catalyst granules, catalyst master
Constitute is nickel, magnesium oxide (94%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control is passed through acetylene alkane at 650-850 DEG C
With the mixed gas of argon gas, you can CNT is made.
Embodiment 5, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
20% sodium hydroxide, 5% urea, the polyoxy of 5% polyoxyethylene one are added into 10% ferric nitrate containing catalytic elements, 20% magnesium acetate
Propylene one polyoxyethylene-type, three sections of copolymers, by coprecipitation, high pressure hydro-thermal legal system obtain iron content, Mg catalyst precursor mixing
Liquid, the percentage of above material is mass percent concentration, and mixed liquor is added in drying machine with centrifugal spray, in 260 DEG C of temperature
Degree is lower to be spray-dried, the cyclone separator and sack cleaner collection catalyst precursor of drying machine with centrifugal spray, before catalyst
Body is 60-120 micron of particle diameter, after by rotary furnace in 400 DEG C of temperature lower calcinations 2 hours, obtain 50-110 microns of particle diameter, compare
Surface area 200m2/ g catalyst granules, it is iron, magnesium oxide (90%) that catalyst, which is mainly constituted,.
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 700-1000 DEG C, be passed through methane and
The mixed gas of argon gas, you can CNT, graphene and its compound is made.
Embodiment 6, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
20% ammonium carbonate, 5% urea, 5% APEO are added to 30% aluminum nitrate containing catalytic elements, 30% magnesium sulfate, by co-precipitation
Method, high pressure hydro-thermal legal system must contain aluminium, the mixed liquor of Mg catalyst precursor, and the percentage of above material is that mass percent is dense
Degree, mixed liquor is added in three fluid spray dryers, is spray-dried at a temperature of 260 DEG C, the rotation of three fluid spray dryers
Wind separator and sack cleaner collection catalyst precursor, 50-150 microns of catalyst precursor particle diameter, after pass through rotary furnace
In 600 DEG C of temperature lower calcinations 2 hours, 50-100 microns of particle diameter, specific surface area 90m are obtained2/ g catalyst granules, catalyst is main
Composition is aluminium, magnesium oxide (90%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 700-1000 DEG C, be passed through methane and
The mixed gas of argon gas, you can graphene is made.
Embodiment 7, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
By ferric nitrate, nickel nitrate, citric acid in mass ratio 1：3：5 are made the iron content of solutes content 50%, the catalyst precursor of nickel
Mixed liquor, mixed liquor is added in drying machine with centrifugal spray, is spray-dried at a temperature of 240 DEG C, and drying machine with centrifugal spray thinks rotation
Wind separator and sack cleaner collection catalyst precursor, 60-150 microns of catalyst precursor particle diameter, after pass through rotary furnace
In 450 DEG C of temperature lower calcinations 3 hours, 50-120 microns of particle diameter, specific surface area 120m are obtained2/ g catalyst granules, catalyst master
Constitute is iron, nickel oxide (95%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 600 ~ 800 DEG C, be passed through methane and
The mixed gas of argon gas, you can CNT is made.
Embodiment 8, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
By lanthanum nitrate, ferric nitrate, nickel nitrate, citric acid in mass ratio 5：1：3：5 be made solutes content 40% containing lanthanum, iron, nickel
Catalyst precursor mixed liquor, mixed liquor is added in Pressuresprayingdrier, is spray-dried at a temperature of 240 DEG C, pressure spray
The cyclone separator and sack cleaner collection catalyst precursor of mist drying machine, the particle diameter 90-200 of catalyst precursor are micro-
Rice, after by rotary furnace in 400 DEG C of temperature lower calcinations 2 hours, obtain 70-150 microns of particle diameter, specific surface area 70m2/ g catalyst
Particle, it is lanthanum, iron, nickel oxide (89%) that catalyst, which is mainly constituted,.
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 600-800 DEG C, be passed through ethane and
The mixed gas of argon gas, you can CNT is made.
Embodiment 9, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
By nickel nitrate, magnesium nitrate, citric acid in mass ratio 1：4：6, which are made solutes content 30%, is made iron content, Mg catalyst precursor
Mixed liquor, mixed liquor is added in drying machine with centrifugal spray, is spray-dried at a temperature of 260 DEG C, drying machine with centrifugal spray
Cyclone separator and sack cleaner collection catalyst precursor, 60-120 microns of catalyst precursor particle diameter, after pass through revolution
Stove obtained 50-110 microns of particle diameter, specific surface area 200m in 400 DEG C of temperature lower calcinations 2 hours2/ g catalyst granules, catalyst
Main composition is nickel, magnesium oxide (95%).
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 700-1000 DEG C, be passed through methane and
The mixed gas of nitrogen, you can CNT, graphene and its compound is made.
Embodiment 10, a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, this method includes：
By aluminum nitrate, magnesium nitrate, citric acid in mass ratio 1：1：2, which are made solutes content 60%, is made containing aluminium, Mg catalyst precursor
Mixed liquor, mixed liquor is added in twin-fluid spray dryer, is spray-dried at a temperature of 260 DEG C, and two fluid sprays are dried
The cyclone separator and sack cleaner collection catalyst precursor of machine, 50-150 microns of catalyst precursor particle diameter, after be passed through
Into rotary furnace in 600 DEG C of temperature lower calcinations 2 hours, 50-100 microns of particle diameter, specific surface area 90m are obtained2/ g catalyst granules,
It is aluminium, magnesium oxide (90%) that catalyst, which is mainly constituted,.
When catalyst is applied, above-mentioned catalyst is placed in fixed bed, temperature control at 700-1000 DEG C, be passed through methane and
The mixed gas of argon gas, you can graphene is made.
Claims (10)
1. it is a kind of for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, it is characterised in that this method includes：
Into compound or compound containing catalytic elements, precipitating reagent or complexing agent or dispersant or precipitating reagent are added and scattered
Agent or complexing agent and dispersant, the compound or compound containing catalytic elements be containing rare earth element, iron, cobalt, nickel, molybdenum,
More than one or both of zirconium, copper, zinc, magnesium, aluminium, silicon compound or their compound；Its complexing agent is urged as required
Change the 20%-300% proportionings of element theory stoichiometry, preferably 50%-200%；Precipitating reagent is based on required catalytic elements theoretical chemistry
The 50%-150% of amount proportioning, preferably 80%-120%；Dispersant is matched by the 0.1%-10% of solution quality, preferably 0.25%-5%；
It is made by the synthesis of one or both of the precipitation method, complexometry, hydro-thermal method, high pressure hydro-thermal method, sol-gal process above method
Mixed liquor containing above-mentioned catalytic elements, mixed liquor is received by the quick solvent formation catalytic elements that remove of spray dryer spray drying
The catalyst precursor of rice state distribution, it is carbon that catalyst precursor obtains being used for organic carbon vapor phase growth after high-temperature calcination
The catalyst of compound.
2. it is according to claim 1 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
Be, more than one or both of the rare earth element, iron, cobalt, nickel, molybdenum, zirconium, copper, zinc, magnesium, aluminium, silicon compound or it
Compound be rare earth element, iron, cobalt, nickel, molybdenum, zirconium, copper, zinc, magnesium, aluminium, the oxide of silicon, hydroxide, chloride, cyanogen
More than one or both of compound, fluoride, nitrate, sulfate, silicate, acylate compound or they answer
Compound.
3. it is according to claim 2 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
It is, the solute concentration or solid content of the compound or compound are 0.5%-95%, preferably 2%-50%.
4. it is according to claim 1 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
It is, during the precipitating reagent is soluble hydroxide, soluble carbonate salt and bicarbonate, soluble ammonium salt, ammonia, urea
It is one or more kinds of；The complexing agent be one or both of citric acid, tartaric acid, glycine, the amine tetraacethyl of second two with
On；The dispersant is sodium metaphosphate, sodium alkyl benzene sulfonate, polyvinyl alcohol, polyethylene glycol oxide, the polyoxypropylene one of polyoxyethylene one
Three sections of copolymers of polyoxyethylene-type, polyethylene adjoin one or more kinds of in pyrrolidone.
5. it is according to claim 1 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
It is, the temperature of the spray dryer is 120 DEG C -400 DEG C, preferably 200 DEG C -300 DEG C.
6. being used for preparation method of the organic carbon vapor phase growth for the catalyst of carbide according to claim 1 or 5, it is special
Levy and be, the spray dryer is in drying machine with centrifugal spray, Pressuresprayingdrier or two/tri- fluid spray dryer
It is a kind of.
7. it is according to claim 1 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
It is, 50-1000 microns of the catalyst precursor particle size range.
8. it is according to claim 1 for preparation method of the organic carbon vapor phase growth for the catalyst of carbide, its feature
It is, the temperature of the high-temperature calcination is 300 DEG C -1200 DEG C, and calcination time is 1-24 hours.
9. CNT, graphene is made in the catalyst prepared described in claim any one of 1-8 in vapour deposition process
Or the purposes of their compound.
10. purposes according to claim 9, it is characterised in that：The catalyst is placed in high-temperature service, be passed through seven carbon and
Following organic gas and inert gas, the mixture of reducibility gas, temperature control is at 600 DEG C -1200 DEG C, and organic carbon is through cracking
Deposition growing is in catalyst surface, by separating-purifying, and CNT, graphene or their compound, its high temperature is made
Equipment is roller kilns, rotary furnace, fixed bed, moving bed or fluid bed.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107570160A (en) * | 2017-10-18 | 2018-01-12 | 哈尔滨金纳科技有限公司 | A kind of medical stone is method for preparing catalyst, catalyst and the application that carrier is used for CNT production |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184425A (en) * | 2013-03-13 | 2013-07-03 | 无锡格菲电子薄膜科技有限公司 | Method for growing graphene film by using low-temperature chemical vapor deposition |
| CN103721750A (en) * | 2014-01-09 | 2014-04-16 | 深圳市三顺中科新材料有限公司 | Catalyst for preparing long-pipe-diameter carbon nano tubes and preparation method of catalyst |
| CN104870363A (en) * | 2013-09-30 | 2015-08-26 | Lg化学株式会社 | Carbon nanotube having high specific surface area and method for manufacturing same |
| CN105964268A (en) * | 2016-05-17 | 2016-09-28 | 深圳市河科科技有限公司 | Metal catalyst preparation method and preparation method of carbon nanotube |
| CN106629672A (en) * | 2016-09-30 | 2017-05-10 | 潍坊昊晟碳材料有限公司 | Carbon nanotube-graphene composite material and preparation method thereof |
-
2017
- 2017-06-10 CN CN201710434753.7A patent/CN107252682A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184425A (en) * | 2013-03-13 | 2013-07-03 | 无锡格菲电子薄膜科技有限公司 | Method for growing graphene film by using low-temperature chemical vapor deposition |
| CN104870363A (en) * | 2013-09-30 | 2015-08-26 | Lg化学株式会社 | Carbon nanotube having high specific surface area and method for manufacturing same |
| CN103721750A (en) * | 2014-01-09 | 2014-04-16 | 深圳市三顺中科新材料有限公司 | Catalyst for preparing long-pipe-diameter carbon nano tubes and preparation method of catalyst |
| CN105964268A (en) * | 2016-05-17 | 2016-09-28 | 深圳市河科科技有限公司 | Metal catalyst preparation method and preparation method of carbon nanotube |
| CN106629672A (en) * | 2016-09-30 | 2017-05-10 | 潍坊昊晟碳材料有限公司 | Carbon nanotube-graphene composite material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 刘广文: "《喷雾干燥实用技术大全》", 31 October 2001, 中国轻工业出版社 * |
| 秦柄权: "《上海化学工业志》", 30 June 1997, 上海社会科学院出版社 * |
| 贾瑛: "《轻质碳材料的应用》", 30 November 2013, 国防工业出版社 * |
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| CN107626334A (en) * | 2017-10-19 | 2018-01-26 | 焦作集越纳米材料技术有限公司 | A kind of preparation method of carbon nano-tube catalyst |
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| CN109280425A (en) * | 2018-11-02 | 2019-01-29 | 杭州超探新材料科技有限公司 | A kind of preparation method of floor heating electric hot plate |
| CN109647410A (en) * | 2019-01-08 | 2019-04-19 | 燕山大学 | For handling the preparation method of the support type expandable graphite catalyst of EDTA-Cu waste water |
| CN109734081A (en) * | 2019-03-18 | 2019-05-10 | 新奥石墨烯技术有限公司 | Mesoporous template and preparation method thereof, three-dimensional meso-hole graphene and preparation method thereof, energy storage material and battery |
| CN111514903A (en) * | 2019-12-25 | 2020-08-11 | 江西悦安新材料股份有限公司 | Method for preparing iron-based array carbon tube catalyst in large scale |
| CN115215324A (en) * | 2021-09-16 | 2022-10-21 | 哈尔滨工业大学 | Method for preparing carbon nano tube by pyrolyzing organic micromolecule crosslinking precursor at high temperature |
| WO2023173357A1 (en) * | 2022-03-14 | 2023-09-21 | 无锡东恒新能源科技有限公司 | Method for synthesizing thin-walled carbon nanotube |
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