CN115739141A - Mesoporous structure catalyst and preparation method and application thereof - Google Patents
Mesoporous structure catalyst and preparation method and application thereof Download PDFInfo
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- CN115739141A CN115739141A CN202211529967.XA CN202211529967A CN115739141A CN 115739141 A CN115739141 A CN 115739141A CN 202211529967 A CN202211529967 A CN 202211529967A CN 115739141 A CN115739141 A CN 115739141A
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- catalyst
- nitrate
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- concentrated solution
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- 239000003054 catalyst Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000017 hydrogel Substances 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052796 boron Inorganic materials 0.000 claims abstract description 5
- 239000011575 calcium Chemical group 0.000 claims abstract description 5
- 229910052791 calcium Chemical group 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 5
- 239000011777 magnesium Chemical group 0.000 claims abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 5
- 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 abstract description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 239000011591 potassium Substances 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 239000011734 sodium Chemical group 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 5
- 239000010937 tungsten Substances 0.000 claims abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 20
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- 238000001694 spray drying Methods 0.000 claims description 16
- 239000012018 catalyst precursor Substances 0.000 claims description 14
- LAQPNDIUHRHNCV-UHFFFAOYSA-N isophthalonitrile Chemical compound N#CC1=CC=CC(C#N)=C1 LAQPNDIUHRHNCV-UHFFFAOYSA-N 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 9
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 8
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- PLMFYJJFUUUCRZ-UHFFFAOYSA-M decyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCC[N+](C)(C)C PLMFYJJFUUUCRZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000000499 gel Substances 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 4
- 238000009718 spray deposition Methods 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- DQUVZAJXJOPXIR-UHFFFAOYSA-N boric acid;manganese Chemical compound [Mn].OB(O)O DQUVZAJXJOPXIR-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 3
- DFULNEJUIZSEEC-UHFFFAOYSA-N copper;nitric acid Chemical compound [Cu].O[N+]([O-])=O.O[N+]([O-])=O DFULNEJUIZSEEC-UHFFFAOYSA-N 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- WFLYOQCSIHENTM-UHFFFAOYSA-N molybdenum(4+) tetranitrate Chemical compound [N+](=O)([O-])[O-].[Mo+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] WFLYOQCSIHENTM-UHFFFAOYSA-N 0.000 claims description 3
- 229920001983 poloxamer Polymers 0.000 claims description 3
- 229960000502 poloxamer Drugs 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 238000010438 heat treatment Methods 0.000 description 19
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000003756 stirring Methods 0.000 description 10
- 239000000693 micelle Substances 0.000 description 8
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 8
- 229940117975 chromium trioxide Drugs 0.000 description 7
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 235000006408 oxalic acid Nutrition 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 235000011056 potassium acetate Nutrition 0.000 description 4
- -1 Aromatic nitriles Chemical class 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 230000002538 fungal effect Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 239000005747 Chlorothalonil Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- IECPWNUMDGFDKC-UHFFFAOYSA-N Fusicsaeure Natural products C12C(O)CC3C(=C(CCC=C(C)C)C(O)=O)C(OC(C)=O)CC3(C)C1(C)CCC1C2(C)CCC(O)C1C IECPWNUMDGFDKC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920006121 Polyxylylene adipamide Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000003934 aromatic aldehydes Chemical class 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- IECPWNUMDGFDKC-MZJAQBGESA-N fusidic acid Chemical compound O[C@@H]([C@@H]12)C[C@H]3\C(=C(/CCC=C(C)C)C(O)=O)[C@@H](OC(C)=O)C[C@]3(C)[C@@]2(C)CC[C@@H]2[C@]1(C)CC[C@@H](O)[C@H]2C IECPWNUMDGFDKC-MZJAQBGESA-N 0.000 description 1
- 229960004675 fusidic acid Drugs 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920006391 phthalonitrile polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920006123 polyhexamethylene isophthalamide Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Catalysts (AREA)
Abstract
The invention provides a mesoporous structure catalyst and a preparation method and application thereof, belonging to the technical field of catalyst preparation. The catalyst comprises a template agent, a carrier, a main catalyst and a cocatalyst; the template agent is a nonionic macromolecular surfactant; the carrier is silicon dioxide hydrogel; the active component composition of the catalyst is represented as follows: VCr b P c D d E e O x (ii) a Wherein D is boron, molybdenum, zirconium, tungsten, titanium, nickel, copper, manganese, iron or cobalt; e is potassium, lithium, sodium, magnesium or calcium; wherein b = 0.5-2.5; c =0.1 to 1.5; d =0 to 0.8; e =0 to 0.6; x is determined according to the content of each element in the valence state balance. The catalytic effect of the catalyst provided by the inventionHigh efficiency, long service life and high selectivity.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a mesoporous structure catalyst, and a preparation method and application thereof.
Background
Aromatic nitriles (AN for short) are chemical intermediates with high added value and wide application, cyano (CN) on AN Aromatic ring has good reaction activity, can perform various chemical reactions such as hydrolysis, hydrogenation, reduction, substitution, addition, polymerization and the like to generate corresponding fine chemicals such as phthalein amine, fusidic acid, aromatic amine, aromatic aldehyde and the like, can be used for preparing pesticides, plastics, resins, rubbers, dyes, medicines, lubricants, films, photo materials and the like, is one of essential raw materials in the fields of modern medicines, fine chemicals and the like, and has extremely high economic value.
Isophthalonitrile, the most demanding aromatic nitrile, is widely used in a number of applications, of which the two main uses are the larger: firstly, 2,4,5, 6-tetrachloro-1, 3-benzenedinitrile (chlorothalonil) is synthesized through chlorination reaction, can destroy metabolism of fungal cells to prevent the fungal cells from propagating, and is an efficient broad-spectrum low-toxicity mildew-proof bactericide; and secondly, synthesizing m-xylylenediamine (MXDA) through hydrogenation reaction, and then performing polycondensation reaction with adipic acid to obtain the polyhexamethylene isophthalamide (MXD 6), so that the defects of strong water absorption, low glass transition temperature, high processing difficulty and the like of the traditional nylon are overcome, and the high-performance barrier nylon resin is widely applied to the fields of structural materials, engineering plastics and the like.
The commonly used method for preparing isophthalonitrile is a 'gas phase ammoxidation' method which takes m-xylene, air and ammonia as raw materials and prepares the isophthalonitrile under the action of a catalyst. The method is simple and economical, and has the advantages of normal pressure operation, medium reaction temperature, no need of special solvent, no pollution discharge, low investment and the like. However, the existing catalyst has small specific surface area, no obvious pore structure and low porosity, when the catalyst is reacted in a fluidized bed, active components are easy to lose, the catalyst is easy to be coked and inactivated, and the activity of the catalyst is reduced to a certain degree, so that the service life of the catalyst is influenced.
Disclosure of Invention
The invention provides a mesoporous structure catalyst, a preparation method and application thereof.
In order to achieve the above object, the present invention provides a catalyst with a mesoporous structure, which comprises a template and a carrierA main catalyst and an auxiliary catalyst; the template agent is a nonionic macromolecular surfactant; the carrier is silicon dioxide hydrogel; the active component composition of the catalyst is represented as follows: VCr b P c D d E e O x (ii) a Wherein D is boron, molybdenum, zirconium, tungsten, titanium, nickel, copper, manganese, iron or cobalt; e is potassium, lithium, sodium, magnesium or calcium; wherein b = 0.5-2.5; c =0.1 to 1.5; d =0 to 0.8; e =0 to 0.6; x is determined according to the content of each element in the valence state balance.
Preferably, the nonionic macromolecular surfactant comprises one or more of poloxamer, polyoxyethylene-polyoxypropylene-polyoxyethylene, cetyltrimethylammonium bromide, sodium lauryl sulfate, DTAB, cetyltrimethylammonium bromide and sodium lauryl sulfate.
Preferably, the content of the active component in the catalyst is 30-70% by weight.
Preferably, the catalyst is of a microsphere structure, and the diameter of the catalyst is 50-200 mu m.
The invention provides a preparation method of the mesoporous structure catalyst, which comprises the following steps:
1) Conversion to form the catalyst active component VCr b P c D d E e O x Mixing the precursors, reacting, adding a template agent and silicon dioxide hydrogel, and concentrating to obtain a concentrated solution;
2) Aging the concentrated solution to form gel, and then performing spray drying and forming; or directly spray drying the concentrated solution for molding;
3) Drying after molding to obtain a catalyst precursor;
4) And sintering the catalyst precursor to obtain the catalyst.
Preferably, the precursor in step 1) comprises vanadium pentoxide; chromium oxide; phosphoric or phosphotungstic acid; sodium nitrate; zirconium nitrate; cobalt nitrate; boric acid; manganese nitrate; lithium nitrate; nickel acetate; magnesium carbonate; potassium nitrate; calcium carbonate; copper nitric acid; molybdenum nitrate.
Preferably, the inlet temperature of the spray drying is 200-300 ℃, and the outlet temperature is 60-130 ℃; the temperature during sintering is 300-900 ℃, and the time is 8-12 h.
The invention provides application of the mesoporous structure catalyst in preparation of isophthalonitrile by an ammoxidation method.
Preferably, the isophthalonitrile is prepared by adopting a fluidized bed ammoxidation process, and the reaction temperature is 370-450 ℃.
Preferably, the space-time airflow rate for preparing isophthalonitrile by adopting a fluidized bed ammoxidation process is 50-400 ml/min; the flow rate of ammonia gas is 10-200 ml/min; the flow rate of the m-xylene is 10-150 mul/min.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the mesoporous structure catalyst provided by the invention, V, cr and P are used as main catalysts, a non-ionic macromolecular polymer is used as a template agent, and a part of catalyst auxiliaries are added, so that the specific surface area of the catalyst is increased, the activity and the conversion rate of the catalyst are increased, the possibility of catalyst inactivation is reduced, the reaction activity of the prepared catalyst is good, and the stable yield can be maintained for a long time.
Furthermore, the invention provides an m-phthalonitrile fluidized bed ammoxidation process, which is continuous and stable and is simple to operate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a mesoporous structure catalyst, which comprises a template agent, a carrier, a main catalyst and a cocatalyst; the template agent is a macromolecular surfactant; the carrier is silicon dioxide hydrogel; the active component composition of the catalyst is represented as follows: VCr b P c D d E e O x (ii) a Wherein D is boron, molybdenum, zirconium, tungsten, titanium, nickel, copper, manganese, iron or cobalt; e is potassium, lithium, sodium, magnesium or calcium; wherein b = 0.5-2.5; c =0.1 to 1.5; d =0 to 0.8; e =0 to 0.6; x is determined according to the content of each element in the valence state balance.
The mesoporous structure catalyst provided by the invention comprises a template agent; the template agent is a nonionic macromolecular surfactant; the nonionic macromolecular surfactant is preferably
One or more of F-127 (poloxamer), P123 (polyoxyethylene-polyoxypropylene-polyoxyethylene), CTAB (cetyltrimethylammonium bromide), K12 (sodium dodecyl sulfate), DTAB, cetyltrimethylammonium bromide, and sodium dodecyl sulfate. In the invention, the nonionic surfactant is used as an amphiphilic polymer, and a certain amount of the nonionic surfactant is added into water to form micelles. Because the hydrophilicity of one part of the block is stronger than that of the other part of the block, the micelle is formed in water, the hydrophobic end is used as an inner core, the hydrophilic end is used as a shell layer, the micelle is continuously added, the micelle can be further aggregated, the active ingredients of the catalyst are distributed around the micelle, and a mesoporous structure is formed after the surfactant is removed by high-temperature calcination, so that the specific surface area of the catalyst is increased, the exposure of active sites is increased, and the activity of the catalyst is improved.
The mesoporous structure catalyst provided by the invention comprises a carrier; the carrier is silica hydrogel.
The mesoporous structure catalyst provided by the invention comprises the following active components: VCr b P c D d E e O x (ii) a Wherein D is boron, molybdenum, zirconium, tungsten, titanium, nickel, copper, manganese, iron or cobalt; e is potassium, lithium, sodium, magnesium or calcium; wherein b = 0.5-2.5; c =0.1 to 1.5; d =0 to 0.8; e =0 to 0.6; x is determined according to the content of each element in the valence state balance. In the invention, vanadium, chromium and phosphorus are used as main catalysts, and D and E are used as auxiliary catalysts. In the invention, the catalyst has activity in weight percentageThe content of the property component is preferably 30% to 70%, more preferably 40% to 60%. The catalyst provided by the invention is of a microsphere structure, and the diameter of the catalyst is preferably 50-200 μm.
The invention takes nonionic surfactant as template agent, forms micelle in water, active ingredients of catalyst are distributed around the micelle along with the further aggregation of the micelle, and mesoporous structure is formed after the surfactant is removed by high-temperature calcination. And then, a small amount of the D auxiliary agent is added to reduce the generation of high-polymerization byproducts and improve the desorption effect of the byproducts on the surface of the catalyst, thereby reducing the phenomenon that the catalyst is easy to coke. Meanwhile, the addition of the auxiliary agent E increases the mechanical property of the catalyst and improves the wear resistance of the catalyst.
The invention provides a preparation method of the mesoporous structure catalyst, which comprises the following steps:
1) Conversion to form the catalyst active component VCr b P c D d E e O x Mixing the precursors, reacting, adding a template agent and silicon dioxide hydrogel, and concentrating to obtain a concentrated solution;
2) Aging the concentrated solution to form gel, and then performing spray drying and forming; or directly spray drying the concentrated solution for forming;
3) Drying after molding to obtain a catalyst precursor;
4) And sintering the catalyst precursor to obtain the catalyst.
The present invention forms the conversion into the catalyst active component VCr b P c D d E e O x After the precursors are mixed and react, a template agent and silicon dioxide hydrogel are added for concentration, and concentrated solution is obtained. In the present invention, the precursor preferably includes vanadium pentoxide; chromium oxide; phosphoric acid or phosphotungstic acid; sodium nitrate; zirconium nitrate; cobalt nitrate; boric acid; manganese nitrate; lithium nitrate; nickel acetate; magnesium carbonate; potassium nitrate; calcium carbonate; copper nitric acid; molybdenum nitrate. In the present invention, in the case of the present invention,preferably, vanadium pentoxide, chromium trioxide, oxalic acid and water are mixed for reaction to obtain a uniform liquid, and then other precursors are added into the uniform liquid for reaction. In the present invention, the concentration is preferably carried out at a temperature of 50 to 100 ℃ and preferably to 60 to 70% of the original solution so that the solution viscosity is 60 to 120 mPas.
After the concentrated solution is obtained, the concentrated solution is aged to form gel, and then spray drying forming is carried out, or the concentrated solution is directly spray dried and formed. In the present invention, the aging is preferably performed by standing at room temperature for 6 to 8 days. In the invention, the temperature of the spray drying is preferably 200-300 ℃ at the inlet and 60-130 ℃ at the outlet; the flow rate of the stream during the spray drying is preferably between 30 and 100ml/min.
After molding, the molded material is dried to obtain the catalyst precursor. In the present invention, the drying temperature is preferably 90 to 110 ℃ and the drying time is preferably 7 to 9 hours.
After the catalyst precursor is obtained, the catalyst precursor is sintered to obtain the catalyst. In the invention, the temperature during sintering is preferably 300-900 ℃, and more preferably 400-700 ℃; the time is preferably 8 to 12 hours, more preferably 10 hours.
The sources of the precursors of the active components, the template agent and the silicon dioxide hydrogel are not particularly limited in the invention, and the conventional commercial products in the field can be adopted.
The invention provides application of the mesoporous structure catalyst in preparation of isophthalonitrile by an ammoxidation method. In the present invention, isophthalonitrile is preferably produced by a fluidized bed ammoxidation process at a reaction temperature of preferably 370 to 450 ℃, more preferably 380 to 430 ℃, and most preferably 390 to 410 ℃. In the invention, the space-time airflow rate for preparing isophthalonitrile by adopting a fluidized bed ammoxidation process is preferably 50-400 ml/min, more preferably 80-300 ml/min, and most preferably 100-200 ml/min; the flow rate of the ammonia gas is preferably 10 to 200ml/min, more preferably 50 to 150ml/min, and most preferably 80 to 130ml/min; the meta-xylene feed flow rate is preferably 10 to 150. Mu.l/min, more preferably 20 to 100. Mu.l/min, most preferably 30 to 80. Mu.l/min. It can be understood that: when the fluidized bed ammoxidation process is adopted to prepare the isophthalonitrile, the raw materials can be fully contacted with the catalyst and fully reacted with the gas within the process parameters defined in the application.
In the invention, compared with the intermittent process such as a reaction kettle and the like, the fluidized bed ammoxidation process is adopted, and the movement of the fluidized bed gas and the catalyst ensures that the bed layer has good heat transfer performance, the temperature in the bed layer is uniform and is easy to control; the continuous regeneration and the circulation operation of the catalyst are convenient to carry out, the continuous feeding and the continuous output are realized, the efficiency is improved, and the cost is reduced. In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing 200g of vanadium pentoxide and 180g of chromium trioxide, adding 800g of oxalic acid and 800mL of water, stirring while heating until the mixture becomes a uniform liquid, then adding a solution consisting of 68g of potassium acetate, 190g of phosphoric acid, 80g of sodium nitrate and 100mL of water, stirring for half an hour, adding 80g of boric acid, adding 100g of F127, adding 1000g of silica hydrosol with the mass fraction of 30%, heating and concentrating at 80 ℃ until the concentration is 60% of the original solution and the viscosity is 75 mPa.s, carrying out spray drying molding on the obtained concentrated solution (the temperature of the inlet is 200, the outlet is 100 ℃, and the flow rate of the concentrated solution is 50 mL/min), drying the molded material in a 100 ℃ oven for 8h, placing the obtained catalyst precursor in a muffle furnace, gradually heating to 600 ℃ at the heating rate of 10 ℃/min, preserving heat for 10 hours, and cooling to room temperature to obtain the catalyst 1.
Example 2
Weighing 200g of vanadium pentoxide and 180g of chromium trioxide, adding 800g of oxalic acid and 800mL of water, stirring while heating until the vanadium pentoxide and the chromium trioxide become uniform liquid, then adding a solution consisting of 68g of potassium acetate, 200g of phosphotungstic acid, 80g of zirconium nitrate and 100mL of water, stirring for half an hour, adding 80g of boric acid, adding 100g of P123, adding 1000g of silica hydrosol with the mass fraction of 30%, heating and concentrating at 85 ℃ until the concentration is 70% of the original solution, aging the obtained concentrated solution for one week after the viscosity is 90 mPa.s, forming gel, performing spray drying and forming (the temperature inlet temperature is 250, the outlet temperature is 110 ℃, and the flow rate of the concentrated solution is 55 mL/min), placing the formed material into a 100 ℃ oven for drying for 8 hours, placing the obtained catalyst precursor into a muffle furnace, gradually heating to 600 ℃ at the heating rate of 10 ℃/min, preserving heat for 10 hours, and cooling to room temperature to obtain the catalyst 2.
Example 3
Weighing 200g of vanadium pentoxide and 180g of chromium trioxide, adding 800g of oxalic acid and 800mL of water, stirring while heating until the mixture becomes a uniform liquid, then adding a solution consisting of 68g of potassium acetate, 190g of phosphoric acid, 80g of cobalt nitrate and 120mL of water, stirring for half an hour, adding 80g of boric acid, adding 100g of DTAB, adding 1000g of silica hydrosol with the mass fraction of 30%, heating and concentrating at 60 ℃ until the concentration is 65% of the original solution, and the viscosity is 80 mPa.s, then carrying out spray drying molding on the obtained concentrated solution (the temperature inlet is 220, the outlet temperature is 80 ℃, and the flow rate of the concentrated solution is 75 mL/min), putting the molded material into a 100 ℃ oven for drying for 8 hours, putting the obtained catalyst precursor into a muffle furnace, gradually heating to 650 ℃ at the heating rate of 5 ℃, preserving heat for 10 hours, and cooling to room temperature to obtain the catalyst 3.
Example 4
Weighing 200g of vanadium pentoxide and 180g of chromium trioxide, adding 800g of oxalic acid and 800mL of water, stirring while heating until the mixture becomes a uniform liquid, then adding a solution consisting of 68g of nickel acetate, 190g of phosphoric acid, 80g of lithium nitrate and 120mL of water, stirring for half an hour, adding 80g of boric acid, adding 100g of DTAB, adding 1000g of silica hydrosol with the mass fraction of 30%, heating and concentrating at 60 ℃ until the concentration is 65% of the original solution and the viscosity is 80mPa · s, carrying out spray drying molding on the obtained concentrated solution (the inlet temperature is 230, the outlet temperature is 80 ℃, and the flow rate of the concentrated solution is 75 mL/min), drying the molded material in a 100 ℃ oven for 8 hours, placing the obtained catalyst precursor in a muffle furnace, gradually heating to 650 ℃ at the heating rate of 8 ℃, preserving heat for 10 hours, and cooling to room temperature to obtain the catalyst 4.
Comparative example 1
Weighing 200g of vanadium pentoxide and 180g of chromium trioxide, adding 800g of oxalic acid and 800mL of water, heating while stirring until the mixture becomes a uniform liquid, then adding a solution consisting of 68g of potassium acetate, 190g of phosphoric acid, 80g of sodium nitrate and 100mL of water, stirring for half an hour, adding 80g of boric acid, adding 1000g of silica hydrosol with the mass fraction of 30%, heating and concentrating to a certain concentration, carrying out spray drying molding in a spray dryer, then placing in a 100 ℃ oven for drying for 8 hours, placing a catalyst precursor in a muffle furnace, gradually heating to 600 ℃, keeping the temperature for 10 hours, and cooling to room temperature to obtain the catalyst 5.
The specific surface area analysis was performed on the catalysts prepared in examples 1 to 4 and comparative example 1, and the results are shown in Table 1.
TABLE 1 specific surface area of catalyst
It can be seen from table 1 that the addition of the macromolecular polymer as the template can effectively increase the specific surface area of the catalyst and increase the pore volume thereof, wherein the specific surface area of the catalyst to which F127 is added is the largest because F127 is an amphiphilic triblock copolymer, one end of which is hydrophilic and the other end of which is hydrophobic, in an aqueous solution, the hydrophobic ends aggregate, the hydrophilic ends disperse, and after calcination removal, the catalyst forms a mesoporous structure, increasing the specific surface area.
Example 5
40g of the catalyst prepared in each example was packed in each of porous high silica glass fluidized bed type reaction tubes having an inner diameter of 25mm, and at a reaction temperature of 410 ℃ and a reaction pressure of normal pressure, m-xylene (50 g) was fed into the reactor from the bottom at a rate of 2ml/min, and ammonia gas and air were fed into the reaction through another line, and the results of the reaction evaluation reaction were shown in Table 2, wherein the flow rate of ammonia gas was 30ml/min and the flow rate of air was 70 ml/min.
TABLE 2 results of catalytic reactions with different catalysts
As can be seen from Table 2, the catalyst provided by the invention has high selectivity and good cycle performance, and can still achieve the yield of more than 90% after 1000h of cycle.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The mesoporous structure catalyst is characterized by comprising a template, a carrier, a main catalyst and a cocatalyst; the template agent is a nonionic macromolecular surfactant; the carrier is silicon dioxide hydrogel; the active component composition of the catalyst is represented as follows: VCr b P c D d E e O x (ii) a Wherein D is boron, molybdenum, zirconium, tungsten, titanium, nickel, copper, manganese, iron or cobalt; e is potassium, lithium, sodium, magnesium or calcium; wherein b = 0.5-2.5; c =0.1 to 1.5; d =0 to 0.8; e =0 to 0.6; x is determined according to the content of each element in the formula according to the valence state balance.
2. The mesostructured catalyst of claim 1, wherein the non-ionic macromolecular surfactant comprises one or more of poloxamer, polyoxyethylene-polyoxypropylene-polyoxyethylene, cetyltrimethylammonium bromide, sodium dodecylsulfate, DTAB, cetyltrimethylammonium bromide, and sodium dodecylsulfate.
3. The mesostructured catalyst according to claim 1, wherein the content of the active component in the catalyst is 30-70 wt%.
4. The mesostructured catalyst according to claim 1, wherein the catalyst has a microsphere structure, and the diameter of the catalyst is 50-200 μm.
5. The method for preparing the mesostructured catalyst according to any one of claims 1 to 4, comprising the steps of:
1) Conversion to form the catalyst active component VCr b P c D d E e O x Mixing the precursors, reacting, adding a template agent and silicon dioxide hydrogel, and concentrating to obtain a concentrated solution;
2) Aging the concentrated solution to form gel, and then performing spray drying and forming; or directly spray drying the concentrated solution for molding;
3) Drying after molding to obtain a catalyst precursor;
4) And sintering the catalyst precursor to obtain the catalyst.
6. The production method according to claim 5, wherein the precursor in step 1) comprises vanadium pentoxide; chromium oxide; phosphoric or phosphotungstic acid; sodium nitrate; zirconium nitrate; cobalt nitrate; boric acid; manganese nitrate; lithium nitrate; nickel acetate; magnesium carbonate; potassium nitrate; calcium carbonate; copper nitric acid; molybdenum nitrate.
7. The method of claim 5, wherein the spray-drying has an inlet temperature of 200 to 300 ℃ and an outlet temperature of 60 to 130 ℃; the temperature during sintering is 300-900 ℃, and the time is 8-12 h.
8. Use of the mesostructured catalyst of any of claims 1 to 4 for the preparation of isophthalonitrile by ammoxidation.
9. The use of claim 8, wherein isophthalonitrile is prepared by a fluidized bed ammoxidation process at a temperature of 370-450 ℃.
10. The use according to claim 8, wherein the space-time gas flow rate in the preparation of isophthalonitrile by fluidized bed ammoxidation is 50 to 400ml/min; the flow rate of ammonia gas is 10-200 ml/min; the flow rate of the m-xylene feed is 10 to 150 mul/min.
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| CN1268399A (en) * | 1999-03-30 | 2000-10-04 | 中国石油化工集团公司 | Fluidized-bed catalyst for preparing isophthalonitrile |
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