CN114904561A - 一种制氯气用的催化剂及其应用 - Google Patents
一种制氯气用的催化剂及其应用 Download PDFInfo
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- CN114904561A CN114904561A CN202210490583.5A CN202210490583A CN114904561A CN 114904561 A CN114904561 A CN 114904561A CN 202210490583 A CN202210490583 A CN 202210490583A CN 114904561 A CN114904561 A CN 114904561A
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- catalyst
- copper
- elements
- arsenic
- compound
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- Granted
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- 239000003054 catalyst Substances 0.000 title claims abstract description 109
- 239000000460 chlorine Substances 0.000 title claims abstract description 37
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 33
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 239000010949 copper Substances 0.000 claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 16
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 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 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 239000011777 magnesium Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 239000010936 titanium Substances 0.000 claims abstract description 9
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052788 barium Inorganic materials 0.000 claims abstract description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 8
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 7
- 150000003624 transition metals Chemical class 0.000 claims abstract description 7
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 6
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 4
- 239000002808 molecular sieve Substances 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002651 NO3 Inorganic materials 0.000 claims description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 2
- 150000002602 lanthanoids Chemical class 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 16
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 238000002791 soaking Methods 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 150000001642 boronic acid derivatives Chemical class 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000002909 rare earth metal compounds Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/16—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J29/166—Y-type faujasite
-
- 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
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/04—Preparation of chlorine from hydrogen chloride
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/20—After treatment, characterised by the effect to be obtained to introduce other elements in the catalyst composition comprising the molecular sieve, but not specially in or on the molecular sieve itself
-
- 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
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/40—Special temperature treatment, i.e. other than just for template removal
-
- 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
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
本发明涉及一种制氯气用的催化剂及其应用。基于催化剂的总重计,本催化剂含有1~25wt%的铜,0.50~0.75wt%的砷,0.1~15wt%的碱金属元素,0.1~10wt%的一种或两多种稀土元素,0~12wt%镁、钙、钡、锰、铁、镍、钴、锌、钌或钛元素的一种或多种。采用先在载体上浸渍含铜化合物、任选的含除铜以外的过渡金属、碱金属、碱土金属和稀土金属的化合物于水中,经过干燥焙烧得到初期催化剂,然后再浸渍含砷元素的化合物。采用本发明所述的催化剂,在用于氯化氢氧化制氯气的反应时具有很高的转化率和很好的稳定性同时克服在流化床反应过程中使用的催化剂存在耐磨损性较差,长周期运行时活性组分易脱落粉化造成的催化剂活性降低的问题。
Description
技术领域
本发明属于催化剂领域,具体涉及一种制氯气用的催化剂及应用。
背景技术
氯气是一种重要的化工原料,广泛应用于纺织、医药、石油化工、饮水消毒和环保工业等众多领域。当氯气应用于化学品合成时,多数涉氯反应对氯原子利用率偏低,造成大量氯资源损失,这些损失的氯资源多以副产氯化氢的形式存在。据相关文献统计,随着中国化工行业的发展,聚氯乙烯、MDI、TDI、甲烷氯化物、三氯乙烯等产品生产规模的扩大,副产氯化氢总量已超过500万t/a,以甲苯二异氰酸酯(toluene-2,4-diisocyanate,TDI)为例,1分子TDI的产生将伴随4分子副产氯化氢的生成:CH3C6H3(NH2)2+2COCl2 CH3C6H3(NCO)2+4HCl。氯原子的利用率为零,所有氯原子均转变成氯化氢副产物。由于氯化氢市场受限、需求量小,同时环境代价大,末端处理成本高;若不充分回收利用,不利于绿色化学的发展。因此人们迫切希望找到一种经济适用的氯化氢制氯气过程,实现氯元素的闭路循环和零排放,此项研究意义十分重大。
早在十九世纪,国外研究人员就已开始对氯化氢制氯气工艺进行研究。到目前为止,涉及的方法主要有三种:电解法、直接氧化法和催化氧化法。其中,能耗较低、操作简单的催化氧化法备受相关行业青睐,成为近年来的研究热点。催化氧化法是以O2为氧化剂,在催化剂的作用下,使HCl转化为Cl2,反应式如下:
4HCl+O2→2H2O+2Cl2
该反应为可逆反应,受平衡制约,且反应温度较高,因此对催化剂的要求较为苛刻。如何获得高活性、高稳定性的催化剂一直是该领域的研究核心。氯化氢催化氧化法制氯气使用的催化剂主要有铜基、铬基和钌基催化剂,以及近年来开发的铈基催化剂等。其中,铜基催化剂活性优良,成本较低,容易再生,工业应用前景广阔,研究者们对其进行了广泛而深入地研究。
专利CN201710071745.0开发了一种多组分的铜基催化剂,掺杂了Cs、Re、Ir等较为少见的元素为助剂,该催化剂具有低温高活性、寿命长的优点,在220℃常压下反应,氯化氢的转化率能达到90%以上,可稳定反应25000h,但其操作复杂,不适用于工业化。
专利CN201610625612.9将B、Nb、P等元素为铜基催化剂助剂,其B元素的加入极大减缓了Cu组分的流失,延长了催化剂寿命,同时获得了良好的催化性能,但氯化氢转化率仅为80%。
专利CN201711220899.8中催化剂活性组分采用钌组分,将活性组分通过双氧水处理,制得催化剂,其氯化氢转化率仅为35.9%,且采用贵金属钌元素。
专利CA920775则以孔径的分子筛作为氯化氢氧化载体,负载氯化铜为活性组分,在V(HCl)∶V(O2)=1∶0.25,HCl空速80V·V-1·h-1,反应温度482℃的条件下,氯化氢的最高转化率为69%。
纵观现有的针对氯化氢氧化催化剂方面的研究,都存在催化剂活性组分流失导致催化剂活性降低的问题。
发明内容
本发明针对现有技术中存在的上述缺点,在铜系催化剂中加入了砷,对催化剂进行改性处理并通过催化剂制备方式的改进得到该催化剂,克服在流化床反应过程中使用的催化剂存在耐磨损性较差,长周期运行时活性组分易脱落粉化造成的催化剂活性降低的问题。
此外,本发明的另一目的是提供一种新的氯化氢氧化催化剂的制备方法,使该催化剂具有较好的反应活性以及良好的导热性,有利于保持催化剂床层反应温度的均一性,减小反应器工程放大热效应。
本发明的再一个目的在于提供上述催化剂的应用途径,该催化剂应用于氯化氢氧化制备氯气的反应中,具有优异的催化反应活性和稳定性,选择性及收率高。
为解决上述技术问题,本发明的技术方案如下:
本发明的催化剂包括载体和活性组分,基于催化剂总重计,所述催化剂包含的活性组分如下:1~25wt%、优选6~25wt%、更优选8~12wt%的铜;0.5~0.75wt%、优选0.6~0.75wt%、更优选0.65~0.75wt%的砷;0.1~15wt%、优选2~13wt%、更优选2.5~8wt%的碱金属元素;0.1~10wt%、优选3~9wt%、更优选4~9wt%的一种或多种稀土元素;0~12wt%、优选0~10wt%、更优选3~6wt%的选自镁、钙、钡、锰、铁、镍、钴、锌和钛的元素的一种或多种,其中镁、钙、钡、锰、铁、镍、钴、锌和钛的元素的含量可以为0或不为0;60~80wt%的载体,优选为60~70wt%的载体。所述的催化剂的总重指载体与施用于其上的金属盐或氧化物的重量总和。
其中所述碱金属元素为锂、钠、钾、铯中的一种,优选为钠或钾。所述的稀土元素为镧系元素中的至少一种,优选为铈、镧、镨和钕。
所述载体为分子筛、高岭土、硅藻土、二氧化硅、氧化铝、二氧化钛、二氧化锆中的一种或多种,优选为分子筛或高岭土,其中分子筛更优选为Y型分子筛。
本发明的催化剂制备过程包括如下步骤:1)溶解所需的含铜化合物、任选的含除铜以外的过渡金属、碱金属、碱土金属和稀土金属的化合物于水中,加入载体浸渍,干燥;
2)将步骤1中干燥后的固体,在200~300℃焙烧1~3h得到初期催化剂;3)将含砷化合物溶解于水中,加入步骤2中得到初期催化剂,重新浸渍,干燥。4)将步骤3中干燥后的固体在450~650℃焙烧3~5h得到催化剂。
作为优选的方案,上述制备步骤中(1)步和(3)步载体在金属溶液中浸渍8~16h,再在70~110℃下干燥12~24h。
本催化剂制备过程中用到的含铜化合物为铜的可溶性盐,优选是选自硝酸铜、氯化铜和乙酸铜当中的一种或多种,一般情况下,当使用两种或多种时它们按照任意比例的组合,优选为硝酸铜和氯化铜;含除铜以外的过渡金属的化合物是锰、铁、镍、钴、锌、钛的可溶性盐,优选锰、铁、镍、钴、锌、钛元素对应的硝酸盐、氯化物或乙酸盐中的一种或多种,更优选锰、铁、钴、锌元素对应的硝酸盐、氯化物或乙酸盐中的一种或多种;含砷化合物为三氧化二砷;碱金属化合物为锂、钠、钾中的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐中的一种或多种;优选钠或钾的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐;碱土金属化合物为镁、钙、钡的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐中的一种或多种,优选镁或钙的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐;稀土金属化合物为铈、镧、镨和钕的硝酸盐或氯化盐,优选硝酸盐。
本发明的催化剂应用于氯化氢催化氧化制氯气的反应在流化床反应器中进行。反应条件为:反应温度为320~460℃,优选为360~400℃;反应压力为0.1~0.6Mpa,优选为0.1~0.35Mpa;氯化氢与氧气的摩尔比为0.5~9∶1,优选为1~4∶1;氯化氢的质量空速为0.1~2.5h-1,优选为0.5~2h-1。反应产物用过量的碘化钾溶液吸收,反应生成的氯气用碘量法进行测定,未反应的氯化氢则通过酸碱滴定得到,由此计算得到氯气的收率。
最后,本发明提供了该催化剂在催化以氯化氢为原料制氯气反应中的用途。
本发明提供的催化剂具有制备工艺简单的特点,同时,与金、钌系催化剂相比价格相对低廉。与现有含铜催化剂相比,本发明还进一步引入了砷元素,对催化剂进行改性处理,与现有的组分相比有较强氧化性且具有较强的离子键特性,砷元素与骨架铝形成As-O-Al化学键,提高比表面积的同时由于在催化剂制备的时候采用分步,先在载体上浸渍含铜化合物、任选的含除铜以外的过渡金属、碱金属、碱土金属和稀土金属的化合物于水中,经过干燥焙烧得到初期催化剂,然后再浸渍含砷元素的化合物对催化剂进行改性处理这样可以降低催化剂中心的酸密度与酸强度,给晶格氧离子的快速体相迁移提供了物质基础与场所,保证反应向高选择性方向进行的同时增强了催化剂的寿命。
具体实施方式
以下通过实例来进一步阐述本发明,但绝不仅限于以下实施例。
实施例1
用50ml含有13.68gCuCl2·2H2O的水溶液浸渍60g HY分子筛12h,然后在90℃干燥10h,260℃焙烧2h,将得到的固体重新分散在50ml含有0.86g As2O3、4.13gNaCl、7.08gCe(NO3)3·6H2O、6.9gNd(NO3)3·6H2O、23.15gMg(NO3)2·6H2O的水溶液中,浸渍12h,然后在90℃干燥10h,550℃焙烧4h,得到活性催化剂。压片成型制得30~60目催化剂颗粒。将6g30~60目催化剂装入固定床反应器中,在氯化氢和氧气流速均为100ml/min,反应温度为380℃,反应压力为0.18Mpa的条件下反应。反应4小时后的氯气收率为89.2%,反应100小时后的氯气收率为88.9%,催化剂活性保持稳定。
实施例2
用50ml含有18.33gCuCl2·2H2O的水溶液浸渍60g HY分子筛12h,然后在90℃干燥10h,260℃焙烧2h,将得到的固体重新分散在50ml含有0.94g As2O3、7.28gNaCl、12.76gCe(NO3)3·6H2O、11.15gNd(NO3)3·6H2O、36.5gMg(NO3)2·6H2O的水溶液中,浸渍12h,然后在90℃干燥10h,550℃焙烧4h,得到活性催化剂。压片成型制得30~60目催化剂颗粒。将6g30~60目催化剂装入固定床反应器中,在氯化氢和氧气流速均为100ml/min,反应温度为380℃,反应压力为0.18Mpa的条件下反应。反应4小时后的氯气收率为89.1%,反应100小时后的氯气收率为89.6%,催化剂活性保持稳定。
实施例3
用50ml含有23.75gCuCl2·2H2O的水溶液浸渍60g HY分子筛12h,然后在90℃干燥10h,260℃焙烧2h,将得到的固体重新分散在50ml含有1g As2O3、12.76gNaCl、19.33gCe(NO3)3·6H2O、18.82gNd(NO3)3·6H2O、86.22gMg(NO3)2·6H2O的水溶液中,浸渍12h,然后在90℃干燥10h,550℃焙烧4h,得到活性催化剂。压片成型制得30~60目催化剂颗粒。将6g30~60目催化剂装入固定床反应器中,在氯化氢和氧气流速均为100ml/min,反应温度为380℃,反应压力为0.18Mpa的条件下反应。反应4小时后的氯气收率为88.5%,反应100小时后的氯气收率为88.1%,催化剂活性保持稳定。
实施例4
用50ml含有13.68gCuCl2·2H2O的水溶液浸渍60g HY分子筛12h,然后在90℃干燥10h,260℃焙烧2h,将得到的固体重新分散在50ml含有0.86g As2O3、3.01gKCl、7.04gPr(NO3)3·6H2O、7.12gLa(NO3)3·6H2O、8.37gNi(NO3)2·6H2O的水溶液中,浸渍12h,然后在90℃干燥10h,550℃焙烧4h,得到活性催化剂。压片成型制得30~60目催化剂颗粒。将6g30~60目催化剂装入固定床反应器中,在氯化氢和氧气流速均为100ml/min,反应温度为380℃,反应压力为0.18Mpa的条件下反应。反应4小时后的氯气收率为89.5%,反应100小时后的氯气收率为89.0%,催化剂活性保持稳定。
实施例5
用50ml含有18.33gCuCl2·2H2O的水溶液浸渍60g HY分子筛12h,然后在90℃干燥10h,260℃焙烧2h,将得到的固体重新分散在50ml含有0.94g As2O3、5.27gKCl、11.42gCe(NO3)3·6H2O、11.37gPr(NO3)3·6H2O、12.31gCo(NO3)2·6H2O的水溶液中,浸渍12h,然后在90℃干燥10h,550℃焙烧4h,得到活性催化剂。压片成型制得30~60目催化剂颗粒。将6g30~60目催化剂装入固定床反应器中,在氯化氢和氧气流速均为100ml/min,反应温度为380℃,反应压力为0.18Mpa的条件下反应。反应4小时后的氯气收率为88.9%,反应100小时后的氯气收率为88.6%,催化剂活性保持稳定。
对比例1
催化剂制备参照实施例1:不同之处仅在于活性组分负载时不添加三氧化二砷组分,其他操作与实施例1相同,制得催化剂。反应4小时后的氯气收率为80.1%,反应100小时后的氯气收率为75.6%。
对比例2
催化剂制备参照实施例1:不同之处仅在于添加0.13g三氧化二砷,其他操作与实施例1相同,制得催化剂。反应4小时后的氯气收率为80.5%,反应100小时后的氯气收率为76.5%。
对比例3
催化剂制备参照实施例1:不同之处仅在于添加1.31g三氧化二砷,其他操作与实施例1相同,制得催化剂。反应4小时后的氯气收率为81.5%,反应100小时后的氯气收率为76.9%。
通过实施例1与对比例1对比发现,通过在活性组分中添加三氧化二砷,对催化剂进行改性处理,其氯气的收率以及活性都有所提高
通过实施例1与对比例2和对比例3对比发现砷的含量在特定的范围内制备的催化剂可以提高氯气的收率以及有很好的活性。
Claims (10)
1.一种用于氯化氢氧化制氯气的催化剂,该催化剂包括载体及施用于其上的金属盐或氧化物,其特征在于:基于催化剂的总重,所述金属盐或氧化物施用于载体上使得催化剂含有:1~25wt%的铜,0.50~0.75wt%的砷,0.1~15wt%的碱金属元素,0.1~10wt%的一种或多种稀土元素,0~12wt%镁、钙、钡、锰、铁、镍、钴、锌、钌或钛元素的一种或多种。
2.根据权利要求1所述的氯化氢氧化制氯气的催化剂,其特征在于,基于催化剂的总重,所述的催化剂含有6~25wt%的铜,0.60~0.75wt%的砷,2~13wt%的碱金属元素,3~9wt%的一种或多种稀土元素,0~10wt%的镁、钙、钡、锰、铁、镍、钴、锌、钌或钛元素的一种或多种,60~80wt%的载体。
3.根据权利要求1或2所述的催化剂,其特征在于,所述的载体为分子筛、高岭土、硅藻土、二氧化硅、氧化铝、二氧化钛、二氧化锆中的一种或多种。
4.根据权利要求1或2所述的催化剂,其特征在于,所述的碱金属元素为钠、钾或铯中的一种或多种。
5.根据权利要求1或2所述的催化剂,其特征在于,所述的稀土元素为镧系元素中的一种或多种。
6.根据权利要求5所述的催化剂,其特征在于,所述的稀土元素为铈、镧、镨和钕中的一种或多种。
7.一种如权利要求1~6任一项所述的催化剂的制备方法,其特征在于,所述的催化剂按以下方法制备:
1)溶解所需的含铜化合物、任选的含除铜以外的过渡金属、碱金属、碱土金属和稀土金属的化合物于水中,加入载体浸渍,干燥;
2)将步骤1中干燥后的固体,在200~300℃焙烧1~3h得到初期催化剂;
3)将所需的含砷化合物溶解于水中,加入步骤2中得到初期催化剂,重新浸渍,干燥。
4)将步骤3中干燥后的固体在450~650℃焙烧3~5h得到催化剂。
8.根据权利要求7所述的氯化氢氧化制氯气催化剂的制备方法,其特征在于,所述的含铜化合物为铜的可溶性盐;含除铜以外的过渡金属的化合物是锰、铁、镍、钴、锌、钌或钛的可溶性盐;含砷化合物为砷的可溶性化合物;含碱金属的化合物为钠或钾的可溶性盐;含碱土金属的化合物为镁、钙、钡的可溶性盐;含稀土元素的化合物为稀土元素的可溶性盐。
9.根据权利7或8所述的催化剂的制备方法,其特征在于,所述的含铜化合物为硝酸铜、氯化铜、乙酸铜的一种或多种;含砷化合物为三氧化二砷;含除铜以外的过渡金属的化合物为锰、铁、镍、钴、锌、钛元素的硝酸盐、氯化物或乙酸盐中的一种或多种;含碱金属的化合物为钠或钾的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐中的一种或多种;含碱土金属的化合物为镁、钙、钡中的氯化物、硝酸盐、乙酸盐、碳酸盐或硼酸盐中的一种或多种;含稀土元素的化合物为铈、镧、镨、钕的硝酸盐或氯化物中的一种或多种。
10.如权利要求1-6所述的催化剂或如权利要求7-9所述的催化剂的制备方法制备的催化剂在催化以氯化氢为原料制氯气反应中的用途。
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