CN108079999A - A kind of method of continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst - Google Patents
A kind of method of continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst Download PDFInfo
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- CN108079999A CN108079999A CN201711278563.7A CN201711278563A CN108079999A CN 108079999 A CN108079999 A CN 108079999A CN 201711278563 A CN201711278563 A CN 201711278563A CN 108079999 A CN108079999 A CN 108079999A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 66
- 239000002184 metal Substances 0.000 title claims abstract description 66
- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 36
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000011148 porous material Substances 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 77
- 150000003839 salts Chemical class 0.000 claims abstract description 25
- 239000012266 salt solution Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000012216 screening Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000001099 ammonium carbonate Substances 0.000 claims description 8
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000009938 salting Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910000856 hastalloy Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 14
- 239000002048 multi walled nanotube Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000005352 clarification Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 4
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 229960001545 hydrotalcite Drugs 0.000 description 4
- 229910001701 hydrotalcite Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 241000257465 Echinoidea Species 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 125000005587 carbonate group Chemical group 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000021050 feed intake Nutrition 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 2
- 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 2
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J23/84—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
- B01J23/881—Molybdenum and 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
- 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
- B01J23/882—Molybdenum and 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
- B01J23/76—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
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8872—Alkali or alkaline earth metals
-
- B01J35/40—
-
- B01J35/60—
-
- 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
- B01J37/04—Mixing
-
- 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
- B01J37/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to the technical fields of the synthesis of multi-metal-oxide catalyst used in carbon nanotubes, the method of specially a kind of continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst, by the way that micro passage reaction continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst will not be used after homogeneous raw material preparation solution.The aqueous slkali of active metal salt solution and inert metal salt is continuously pumped into micro passage reaction, under certain condition, precipitation reaction is carried out in micro passage reaction and prepares presoma, reactant is filtered, washs, is dry, roasting, obtaining poly-metal deoxide hole catalyst after screening.Current traditional handicraft is compared, greatly improves the stability and uniformity of production catalyst, yield is improved；The expense of solvent is greatly reduced in reaction process, it is more environmentally-friendly；Its carbon nanotubes Diameter distribution being catalyzed is concentrated, and indices collimation is good, improves the competitiveness of product in market.
Description
Technical field
The present invention relates to the technical fields of the synthesis of multi-metal-oxide catalyst used in carbon nanotubes, are specially a kind of company
The continuous method for preparing carbon nanotubes poly-metal deoxide pore space structure catalyst, by that will not be adopted after homogeneous raw material preparation solution
With micro passage reaction continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst.
Background technology
Micro passage reaction has obvious advantage in terms of mass transfer, heat exchange, can strengthen mixing and accurate temperature controlling, also
The cycle of craft screening and technique amplification can be greatly shortened.Miniature chemical industry equipment have it is simple in structure, without enlarge-effect, operation
Condition is easily controllable and the advantages that intrinsic safety, causes the very big concern of numerous researchers.
Carbon nanotubes has excellent physical mechanical property, mainly has hexagonal row as monodimension nanometer material
The carbon atom of row forms several layers to tens of layers of coaxial pipe.It has very big draw ratio, diameter usually 1-100nm it
Between, length is at a few micrometers to hundreds of microns.Just because of its big draw ratio, carbon nanotubes is in mechanics, electricity, electrical and thermal conductivity
Energy aspect all shows very excellent.Since it is with excellent performance, carbon nanotubes is in catalyst carrier, rubber plastic composite wood
The numerous areas such as material, electrochemical material, photoelectric sensing all have wide, potential application prospect.
Carbon nanotubes carry out catalytic chemistry vapor phase deposition catalysts technology of preparing, be all traditionally coprecipitation and
Gel method.Wherein coprecipitation is artificial or form control flow velocity is added dropwise in metering pump, can not accurately be controlled, obtained forerunner
Body product is uneven, and lot stability is slightly poor, and obtained catalyst granules and yield uniformity is poor, the carbon nanometer that final production goes out
Pipe Diameter distribution is wide, and specific surface area gap is big.
Patent CN201510671278.6《It is a kind of continuously to prepare sea urchin shape Ag-ZnO nano-particles using micro passage reaction
Method》, a kind of method that sea urchin shape Ag-ZnO nano-particles are continuously prepared using micro passage reaction of the disclosure of the invention.Tool
Body is will be by AgNO3, sodium citrate, lauryl sodium sulfate, H2O2The mixed solution of composition with by NaBH4With NaOH compositions
Mixed solution is passed through micro passage reaction simultaneously, is reacted under certain temperature and residence time, and reaction mass should from microchannel plate
After device outlet outflow, being directly entered capillary microreactor, the reaction was continued, generates monodisperse Silver nanodisks.The monodisperse silver nanoparticle
Disk is directly entered a micro passage reaction with 3 entrances, the microchannel plate after capillary microreactor outlet outflow
Other two entrance of device is answered to each lead into Zn (NO3)2Solution and NaOH solution, reaction mass are flowed out from micro passage reaction
Afterwards, aging is carried out at a certain temperature, and sea urchin shape Ag-ZnO nano-particles are finally prepared.
Patent CN201620272546.7,《A kind of micro passage reaction for producing nanometer sulfate》Disclose a kind of production
The micro passage reaction of nanometer sulfate, belongs to chemical reaction device technical field.The micro passage reaction of the patent passes through three
The setting of layer structure and reaction of high order unit enables to charging more accurate, and reaction mass mixing is more uniform, overcomes feed liquid
The laminar flow phenomenon occurred in the reaction process that clashes makes reaction be more nearly plume state, and reaction process contact is more abundant, reaction
More thoroughly, the nanometer sulfate of head-on collision reaction generation can effectively be avoided to reunite again, product is made to keep nano shape and grain size
Uniformly, so be made high quality nanometer sulfate product.
Patent CN201510158737.0《A kind of method that copper zinc catalyst is prepared using micro passage reaction》It discloses
A kind of method that copper zinc catalyst is prepared using micro passage reaction, the process for preparing the catalyst are in micro passage reaction
Middle progress, the micro passage reaction at least possess two entrances and corresponding mixing section, and the equivalent diameter of mixing section exists
0.01-5mm.The invention solves the problems, such as that nucleus is easily reunited during coprecipitation preparation, is easy to get smaller to large specific surface area, grain size
Catalyst crystal grain.
Patent CN201410108682.8《A kind of side for preparing nano-titanium dioxide with the precipitation method using microreactor
Method》A kind of method for preparing nano-titanium dioxide with the precipitation method using microreactor is disclosed, by the inorganic matter nothing of titaniferous
Water-ethanol dissolves, then that the ethanol solution of the aqueous solution of inorganic base and titaniferous inorganic matter is pumped into microchannel moduleization simultaneously respectively is anti-
It answers in device, keeps residence time 15s-1min, reacted at room temperature, reaction product is centrifuged, precipitation distillation washing
It washs 3 times, and it is dry in vacuum desiccator, then 600 DEG C of roasting 2h in Muffle furnace, obtain final products nano-titanium dioxide.
Patent CN201310690832.6《A kind of method that micro passage reaction prepares carbonate form nano hydrotalcite》It is public
A kind of preparation method of carbonate form nano hydrotalcite is opened.The invention uses coprecipitation, by mixed salt solution and contains
The mixed ammonium/alkali solutions for having carbonate are continuously passed through micro passage reaction after heat exchange, under certain temperature in micro passage reaction
It carries out precipitation reaction and hydrotalcite precursor is prepared, then by precursor pulp through follow-up aging or hydro-thermal process, and wash dry
It is dry to obtain carbonate form hydrotalcite product.
Above-mentioned patent, which concentrates on, continuously prepares basic chemical industry raw material, single substance nano particle and sheet metal oxygen
The fields such as compound there is no the pore space structure catalyst for the catalyzing carbon nanotube that a new generation is prepared using microchannel reaction technology at present
Precedent and report, the present invention compensate for this blanking technique and method, and accurate continuous producing carbon nano-tube is catalyzed with pore space structure
Agent.
The content of the invention
For carbon nano-tube catalyst industry Situation at present both at home and abroad, it is more to provide a kind of continuous producing carbon nano-tube use
The method of metal oxide hole structure catalyst makes up its continuous batch precision system for carbon nanotubes pore space structure catalyst
Technological gap.Using micro passage reaction, reaction raw materials reach being mixed for micron even Nano grade, react abundant ring
Guarantor is efficient, and the catalyst granules prepared is homogeneous, active site is evenly distributed, and catalytic activity is stablized, and carbon nanotubes production is greatly improved
The quality and the market competitiveness of product.
Pore space structure catalyst of the present invention, the poly-metal deoxide pore space structure for catalyzing carbon nanotube growth are urged
Agent.The method is continuous preparation method, including successive soln charging and the discharging of continuous nozzle.
The technical scheme is that：
A kind of method of continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst, by active metal salt and go from
Sub- water is configured to active metal salt solution and inert metal salt and is configured to the aqueous slkali of inert metal salt with lye to be continuously pumped into
Reaction member under certain condition, carries out precipitation reaction and prepares presoma in the reaction cell, and reactant is filtered, washing, dry
It obtains preparing carbon nanotubes poly-metal deoxide pore space structure catalyst after dry, roasting, screening.
A kind of continuous producing carbon nano-tube method of poly-metal deoxide pore space structure catalyst, is as follows,
Including：
（1）Active metal salt and deionized water are configured to solution A, and A liquid is active metal salt solution, mass fraction 5%-60%；
（2）Inert metal salt and Alkali liquid compounding are into solution B, and B liquid is the aqueous slkali of inert metal salt, mass fraction 2%-60%；
（3）A and B solution are continuously delivered continuously to reaction member by accurate measurement pump, and the flow volume ratio of wherein A and B are A：B
=0.7-1.5:1；
（4）Reaction temperature is 15 DEG C -80 DEG C, reaction pressure 0.05Mpa-0.2Mpa, and material carries out in micro passage reaction
Reaction, the residence time is in 3-8s, then continuous ejection；
（5）Material is filtered, washing, and overnight, 350-700 DEG C of roasting, screening obtains product for 70-150 DEG C of drying.
The features of the present invention also has：
The step（3）Reaction member for micro passage reaction, micro passage reaction for covering 1nm-50mm single channel,
One or more combinations in multichannel, Parallel Unit, the parallel system of highly dense, micro passage reaction material are carbonization
Silicon ceramics, glass, quartz, stainless steel, Hastelloy or graphite.
The active metal salt is the one or more of iron, nickel, cobalt, manganese, platinum, aluminium, the nitrate of magnesium or sulfate,
The mass fraction of active metal salt solution is preferably 20%-50%；The high active metal salt solution reaction rate of concentration faster, is reduced
The volume of reaction system, short preparation period, but excessively high rear precipitate speed is accelerated, easy blocking pipeline, the present invention rationally control
Active metal salt solution concentration processed.
Inert metal salt is ammonium molybdate, the one or more of ammonium carbonate；Lye for sodium hydroxide or ammonium hydroxide it is a kind of or
Person mixes；The preferred 5%-50% of mass fraction of the aqueous slkali of inert metal salt, the high active metal salt solution reaction rate of concentration
Faster, the volume of reaction system, short preparation period are reduced, but excessively high rear precipitate speed is accelerated, easy blocking pipeline, this hair
The concentration of the aqueous slkali of bright reasonable control inert metal salt.
The flow volume ratio of the active metal salt solution and inert metal salting liquid is 0.7：1 - 1.5:1, be preferably
0.9-1.3:1, further preferably 1:1, rational usage ratio so that two kinds of solution of A and B mix more uniform stabilization.
The step（5）Drying temperature for 100-120 DEG C, calcination temperature is 400 DEG C -600 DEG C；Drying temperature is in 100-
During 120 DEG C of sections, drying efficiency is faster and the material hardness of generation is moderate；Calcination temperature can ensure to imitate at 400-600 DEG C
The active site section of narrow distribution is obtained on the premise of rate.
The beneficial effects of the invention are as follows：
The present invention can reach accurate control pH value in reaction by the flow of fine adjustments two kinds of solution of A and B, be accurate to
0.01；（PH is a passive index parameter, is what is realized by adjusting the flow-rate ratio of AB）；By the residence time for controlling reaction
3-8s realizes that catalyst granules is evenly distributed, and specific surface area of catalyst and micropore data are uniform, and uniformity is strong, obtained catalysis
Agent yield multiplying power has 30% raising than before.
The data target of the multi-walled carbon nanotube prepared is catalyzed, including Diameter distribution, heap density, SSA, volume resistivity etc.
Lot stability is good.
In short, the accurate control of the invention by that can reach pH to the conversion of different flow, compares current traditional work
Skill, greatly improves the stability and uniformity of production catalyst, and yield is improved；Solvent is greatly reduced in reaction process
Expense, it is more environmentally-friendly；Its carbon nanotubes Diameter distribution being catalyzed is concentrated, and indices collimation is good, improves product
The market competitiveness.
Description of the drawings
Hole catalyst prepared by Fig. 1 present invention；
Catalyst granules figure prepared by Fig. 2 present invention；
Carbon nanotubes SEM pictures prepared by Fig. 3 conventional methods synthesis Fe-series catalyst（It is distributed caliber 8.98-30.6nm）；
Carbon nanotubes SEM pictures prepared by Fig. 4 present invention synthesis Fe-series catalysts（It is distributed caliber 12.9-23.2nm）；
Carbon nanotubes SEM pictures prepared by Fig. 5 present invention synthesis nickel catalysts（It is distributed caliber 14.1-27.7nm）.
Specific embodiment
Below in conjunction with the content in the embodiment of the present invention, apparent and completion is carried out to technical scheme and is explained
It states.Obviously, described embodiment is only the part of the embodiment of the present invention, and is not whole experiment case studies.It is based on
The embodiment of the present invention.Remaining embodiment that those skilled in the art are obtained, all belong to the scope of protection of the present invention within.
Embodiment 1：In the present embodiment, Fe-series catalyst is prepared using the method for the present invention.Formula is as follows：
A active metal salt solutions
Nine water aluminum nitrate 1350g, nine water ferric nitrate 610g, deionized water 4000g；The deionization of 4000g is added in 10L beakers
Water, successively adds in the nine water aluminum nitrates of 1350g and the nine water ferric nitrates of 610g, and heating mantle is warming up to 50 DEG C -55 DEG C, uses glass bar
It is spare after stirring to dissolved clarification.
The aqueous slkali of B inert metal salt
Four water ammonium heptamolybdate 40g, ammonium carbonate 550g, 17% ammonium hydroxide 190g, deionized water 3500g.
Preparation method：The deionized water of 3500g is added in 10L beakers, successively adds in the ammonium carbonate of 550g and four water of 40g
Ammonium heptamolybdate, heating mantle are warming up to 40 DEG C -50 DEG C, are stirred with glass bar to dissolved clarification, add in 17% ammonium hydroxide of 190g, and stirring is equal
It is spare after even.
Concrete operations are：
Using Shanghai Tauto Biotechnology Co., Ltd. TBP2H02S type constant-flux pumps, by active metal salt solution A and inertia
Metal saline solution B is continuously passed through the MCT of Guizhou Micro Technology Co., Ltd. with 105ml/min and 90ml/min flows respectively
Micro-mixer, 32 DEG C, pressure 0.2Mpa of controlling reaction temperature, material continuously spray at nozzle；Product carries out centrifugal filtration, uses
It is neutrality that deionized water, which is beaten to pH, and 110 DEG C of drying 10-12h, 450 DEG C of roasting 2h select 80-100 mesh to be urged for qualification after screening
Agent is weighed as 315g.
Carry out the catalysis of multi-walled carbon nanotube with it, a diameter of 50mm, length be 1400mm quartzy fluid bed in into
Row reaction, feed intake 2g, after hydrogen reducing, controls 680-690 DEG C of temperature, is passed through propylene：Nitrogen is 1000:The gas of 2000ml/min
Body 50min obtains multi-walled carbon nanotube product 87.3g；Its SEM picture is shown in attached drawing 4.
Embodiment 2 prepares nickel catalyst in the present embodiment, using the present invention.Formula is as follows：
A active metal salt solutions
Six water nickel nitrate 275g,
Magnesium nitrate hexahydrate 230g,
Deionized water 790g.
The deionized water of 790g is added in 2L beakers, successively adds in the six water nickel nitrates of 275g and the six water nitric acid of 230g
Magnesium, heating mantle are warming up to 50 DEG C -55 DEG C, spare after being stirred with glass bar to dissolved clarification.
The aqueous slkali of B inert metal salt
Four water ammonium heptamolybdate 19g,
Ammonium carbonate 350g,
17% ammonium hydroxide 120g,
Deionized water 680g.
Preparation method：The deionized water of 680g is added in 2L beakers, successively adds in the ammonium carbonate of 350g and four water seven of 19g
Ammonium molybdate, heating mantle are warming up to 40 DEG C -50 DEG C, are stirred with glass bar to dissolved clarification, add in 17% ammonium hydroxide of 120g, stir evenly
It is spare afterwards.
Concrete operations are：
Using Shanghai Tauto Biotechnology Co., Ltd. TBP1H02S type constant-flux pumps, by active metal salt solution A and inertia
The aqueous slkali B of metal salt is continuously passed through the MCT of Guizhou Micro Technology Co., Ltd. with 45ml/min and 55ml/min flows respectively
Micro-mixer, 41 DEG C, pressure 0.15Mpa of controlling reaction temperature, material continuously spray at nozzle；Product carries out centrifugal filtration,
It is neutral to be beaten with deionized water to pH, and 110 DEG C of drying 8-9h, 550 DEG C of roasting 3h select 80-100 mesh to be urged for qualification after screening
Agent is weighed as 104g.
Carry out the catalysis of multi-walled carbon nanotube with it, a diameter of 50mm, length be 1600mm quartzy fluid bed in into
Row reaction, feed intake 1g, after hydrogen reducing, controls 650-670 DEG C of temperature, is passed through propylene：Nitrogen is 1200:The gas of 1800ml/min
Body 60min obtains multi-walled carbon nanotube product 52.2g；Its SEM picture is shown in attached drawing 5.
Embodiment 3：In the present embodiment, cobalt series catalyst is prepared using traditional manual control dropwise addition.Formula is as follows：
A active metal salt solutions
Nine water aluminum nitrate 675g, cobalt nitrate hexahydrate 458g, deionized water 1900g.
Preparation method：The deionized water of 1900g is added in 5L beakers, successively adds in the nine water aluminum nitrates and 458g of 675g
Cobalt nitrate hexahydrate, heating mantle are warming up to 55 DEG C -60 DEG C, spare after being stirred with glass bar to dissolved clarification.
The aqueous slkali of B inert metal salt
Four water ammonium heptamolybdate 18g, ammonium carbonate 300g, 17% ammonium hydroxide 100g, deionized water 1800g.Preparation method：Add in 5L beakers
Enter the deionized water of 1800g, successively add in the ammonium carbonate of 300g and the four water ammonium heptamolybdates of 18g, heating mantle is warming up to 55 DEG C -60
DEG C, it is stirred with glass bar to dissolved clarification, adds in 17% ammonium hydroxide of 100g, stirred evenly rear spare.
Concrete operations are：
Laboratory 30L glass reaction kettle is as reaction vessel, using the constant pressure funnel of 3L in batches respectively by active metal
The aqueous slkali B of salting liquid A and inert metal salt, by way of manually adjusting, two kinds of solution of control are at the uniform velocity added dropwise, it is ensured that
It is added dropwise simultaneously.Reacting kettle jacketing leads to 30-35 DEG C of recirculated water controlling reaction temperature, and 1h is stirred after being added dropwise；Product carries out
Centrifugal filtration, it is neutral to be beaten with deionized water to pH, and 110 DEG C of drying 10-12h, 450 DEG C of roasting 2h select 80- after screening
100 mesh are qualified catalyst, are weighed as 91g.
Carry out the catalysis of multi-walled carbon nanotube with it, a diameter of 100mm, length in 1600mm stainless steel fluid beds into
Row reaction, feed intake 1.5g, after hydrogen reducing, controls 680-690 DEG C of temperature, is passed through propylene：Nitrogen is 1000:2000ml/min's
Gas 50min obtains multi-walled carbon nanotube product 34.8g；Its SEM picture is shown in attached drawing 3.
The data summarization comparison of each comparative example is shown in Table 1.
Table 1 is the data summary table of each comparative example
It can see by the comparison of Fig. 3, Fig. 4 and Fig. 5, iron system and nickel catalyst growth prepared by technical solution of the present invention
Carbon nanotubes, Diameter distribution section more concentrates, and the difference between pipe is small, and uniformity consistency is strong.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God and any modification, equivalent substitution, improvement and etc. within principle, done, should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of continuous producing carbon nano-tube method of poly-metal deoxide pore space structure catalyst, by active metal salt with going
Ionized water is configured to the continuous ground pump of aqueous slkali that active metal salt solution and inert metal salt are configured to inert metal salt with lye
Enter reaction member, under certain condition, carry out precipitation reaction in the reaction cell and prepare presoma, reactant is filtered, washing, dry
It obtains preparing carbon nanotubes poly-metal deoxide pore space structure catalyst after dry, roasting, screening.
2. a kind of side of continuous producing carbon nano-tube poly-metal deoxide pore space structure catalyst according to claim 1
Method, which is characterized in that it is as follows, including：
（1）Active metal salt and deionized water are configured to solution A, and A liquid is active metal salt solution, mass fraction 5%-60%；
（2）Inert metal salt and Alkali liquid compounding are into solution B, and B liquid is the aqueous slkali of inert metal salt, mass fraction 2%-60%；
（3）A and B solution are continuously delivered continuously to reaction member by accurate measurement pump, and the flow volume ratio of wherein A and B are A：B
=0.7-1.5:1；
（4）Reaction temperature is 15 DEG C -80 DEG C, reaction pressure 0.05Mpa-0.2Mpa, and material carries out in micro passage reaction
Reaction, the residence time is in 3-8s, then continuous ejection；
（5）Material is filtered, washing, and overnight, 350-700 DEG C of roasting, screening obtains product for 70-150 DEG C of drying.
3. a kind of continuous producing carbon nano-tube according to claim 1 or 2 poly-metal deoxide pore space structure catalyst
Method, which is characterized in that the reaction member is micro passage reaction, and micro passage reaction is covering 1nm-50mm
One or more combinations in single channel, multichannel, Parallel Unit, the parallel system of highly dense, micro passage reaction material
Matter is silicon carbide ceramics, glass, quartz, stainless steel, Hastelloy or graphite.
4. a kind of continuous producing carbon nano-tube according to claim 1 or 2 poly-metal deoxide pore space structure catalyst
Method, which is characterized in that the active metal salt is iron, nickel, cobalt, manganese, platinum, aluminium, the one of the nitrate of magnesium or sulfate
Kind is a variety of, and the mass fraction of active metal salt solution is preferably 20%-50%.
5. a kind of continuous producing carbon nano-tube according to claim 1 or 2 poly-metal deoxide pore space structure catalyst
Method, which is characterized in that inert metal salt for ammonium molybdate, the one or more of ammonium carbonate；Lye for sodium hydroxide or
Ammonium hydroxide is a kind of or mixes；The preferred 5%-50% of mass fraction of the aqueous slkali of inert metal salt.
6. a kind of continuous producing carbon nano-tube according to claim 1 or 2 poly-metal deoxide pore space structure catalyst
Method, which is characterized in that the flow volume ratio of the active metal salt solution and inert metal salting liquid is 0.7：1 -
1.5:1, it is preferably 0.9-1.3:1, further preferably 1:1.
7. a kind of continuous producing carbon nano-tube according to claim 1 or 2 poly-metal deoxide pore space structure catalyst
Method, which is characterized in that the step（5）Drying temperature for 100-120 DEG C, calcination temperature is 400 DEG C -600 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095927A (en) * | 2018-08-07 | 2018-12-28 | 山东金德新材料有限公司 | A kind of pressureless sintering silicon carbide microchannel reactor chip and preparation method thereof |
| CN112290021A (en) * | 2020-09-28 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon nano tube conductive agent for lithium ion battery |
| CN113663676A (en) * | 2021-08-26 | 2021-11-19 | 无锡碳谷科技有限公司 | Biological air-drying conversion catalyst and preparation method and application thereof |
| CN114618516A (en) * | 2022-03-17 | 2022-06-14 | 无锡东恒新能源科技有限公司 | Synthesis method of microspherical catalyst |
| CN116495725A (en) * | 2023-05-19 | 2023-07-28 | 重庆中润新材料股份有限公司 | Carbon nanotube growth system |
| WO2023173352A1 (en) * | 2022-03-17 | 2023-09-21 | 无锡东恒新能源科技有限公司 | Method for preparing carbon nanotube by catalytic cracking of methanol or propylene |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384358A (en) * | 2006-02-16 | 2009-03-11 | 拜尔材料科学股份公司 | Continuous preparation method of catalyst |
| CN101804459A (en) * | 2010-04-19 | 2010-08-18 | 南京工业大学 | Method for preparing nanometer nickel powder by micro passage reaction vessel |
| DE102010055399A1 (en) * | 2010-12-21 | 2012-06-21 | Süd-Chemie AG | Use of a catalyst comprising a mixed oxide in a basic heterogeneous catalyzed chemical reaction e.g. triglyceride transesterification to prepare biodiesel, where the catalyst is obtained by calcining a bilayer metal hydroxide |
-
2017
- 2017-12-06 CN CN201711278563.7A patent/CN108079999A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384358A (en) * | 2006-02-16 | 2009-03-11 | 拜尔材料科学股份公司 | Continuous preparation method of catalyst |
| CN101804459A (en) * | 2010-04-19 | 2010-08-18 | 南京工业大学 | Method for preparing nanometer nickel powder by micro passage reaction vessel |
| DE102010055399A1 (en) * | 2010-12-21 | 2012-06-21 | Süd-Chemie AG | Use of a catalyst comprising a mixed oxide in a basic heterogeneous catalyzed chemical reaction e.g. triglyceride transesterification to prepare biodiesel, where the catalyst is obtained by calcining a bilayer metal hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| 贾斌: ""Fe/Mo/Al2O3催化剂火焰热解法合成碳纳米管的实验研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095927A (en) * | 2018-08-07 | 2018-12-28 | 山东金德新材料有限公司 | A kind of pressureless sintering silicon carbide microchannel reactor chip and preparation method thereof |
| CN112290021A (en) * | 2020-09-28 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon nano tube conductive agent for lithium ion battery |
| CN112290021B (en) * | 2020-09-28 | 2022-09-06 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon nano tube conductive agent for lithium ion battery |
| CN113663676A (en) * | 2021-08-26 | 2021-11-19 | 无锡碳谷科技有限公司 | Biological air-drying conversion catalyst and preparation method and application thereof |
| CN114618516A (en) * | 2022-03-17 | 2022-06-14 | 无锡东恒新能源科技有限公司 | Synthesis method of microspherical catalyst |
| CN114618516B (en) * | 2022-03-17 | 2023-06-02 | 无锡东恒新能源科技有限公司 | Synthesis method of microspherical catalyst |
| WO2023173352A1 (en) * | 2022-03-17 | 2023-09-21 | 无锡东恒新能源科技有限公司 | Method for preparing carbon nanotube by catalytic cracking of methanol or propylene |
| CN116495725A (en) * | 2023-05-19 | 2023-07-28 | 重庆中润新材料股份有限公司 | Carbon nanotube growth system |
| CN116495725B (en) * | 2023-05-19 | 2023-12-19 | 重庆中润新材料股份有限公司 | Carbon nanotube growth system |
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