CN108435193A - Reproducible removing organochlorine catalyst of one kind and preparation method thereof - Google Patents
Reproducible removing organochlorine catalyst of one kind and preparation method thereof Download PDFInfo
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- CN108435193A CN108435193A CN201810325562.1A CN201810325562A CN108435193A CN 108435193 A CN108435193 A CN 108435193A CN 201810325562 A CN201810325562 A CN 201810325562A CN 108435193 A CN108435193 A CN 108435193A
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- catalyst
- organochlorine
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- 239000003054 catalyst Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical group [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 150000000703 Cerium Chemical class 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 150000002751 molybdenum Chemical class 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 2
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical group [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 150000003863 ammonium salts Chemical class 0.000 claims 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229910001629 magnesium chloride Inorganic materials 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000460 chlorine Substances 0.000 abstract description 13
- 229910052801 chlorine Inorganic materials 0.000 abstract description 13
- 239000003921 oil Substances 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 15
- 238000006298 dechlorination reaction Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 10
- 239000003463 adsorbent Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- 101100494773 Caenorhabditis elegans ctl-2 gene Proteins 0.000 description 4
- 101100112369 Fasciola hepatica Cat-1 gene Proteins 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 101100005271 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) cat-1 gene Proteins 0.000 description 4
- 235000018660 ammonium molybdate Nutrition 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 235000014121 butter Nutrition 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000010779 crude oil Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical class [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 150000002823 nitrates Chemical class 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 101100208039 Rattus norvegicus Trpv5 gene Proteins 0.000 description 3
- 101150019148 Slc7a3 gene Proteins 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical class [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- 235000011147 magnesium chloride Nutrition 0.000 description 3
- 229910001510 metal chloride Inorganic materials 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 101100392078 Caenorhabditis elegans cat-4 gene Proteins 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical class CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910017315 Mo—Cu Inorganic materials 0.000 description 1
- NBFQLHGCEMEQFN-UHFFFAOYSA-N N.[Ni] Chemical compound N.[Ni] NBFQLHGCEMEQFN-UHFFFAOYSA-N 0.000 description 1
- 101100005280 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) cat-3 gene Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000382 dechlorinating effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 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
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000010458 rotten stone Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- LIXPXSXEKKHIRR-UHFFFAOYSA-M tetraethylphosphanium;bromide Chemical compound [Br-].CC[P+](CC)(CC)CC LIXPXSXEKKHIRR-UHFFFAOYSA-M 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- 239000010457 zeolite 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—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
- B01J23/8871—Rare earth metals or actinides
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/617—500-1000 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of reproducible removing organochlorine catalyst and preparation method thereof.The composite oxides that the catalyst is synthesized using silicon source, silicon source and magnesium source is carriers, using Ni, Mo, Cu, Ce as active component.Based on the mass percent of catalyst, NiO contents are 6.2 15.6% in active component, and CuO contents are 16.1 25.4%, MoO3Content is 1.7 4.6%, CeO2Content is 1.5 2.5%, remaining is carrier；Using composite oxides as carrier, there is the preferable dispersed active metal of energy the catalyst orderly pore passage structure, special pore size distribution, hole to hold larger.Organochlorine can be effectively removed, avoids subsequent device by inorganic chlorine corrosion, improves the quality of oil product.The catalyst energy constant regeneration simultaneously reduces the shutting down time, reduces production cost.
Description
Technical field
The present invention relates to a kind of reproducible for removing the catalyst of organic chloride and its preparation in naphtha containing chlorine
Method belongs to oil refinery field.
Background technology
The exploitation later stage in oil field can be increased to increase the yield in oil field using some auxiliary agents containing organic chloride
Add tar productivity, lead in the crude oil of part that chloride content is higher, chlorine-containing compound is mainly enriched in naphtha.Chlorine in naphtha
Compound is mainly chloralkane, such as：Chloroform, dichloromethane, trichloroethanes etc..The desalinating process of crude oil at present, can only
The butter in crude oil is removed, organic chloride therein cannot be removed.Naphtha is as ethylene production and catalytic reforming
Raw material, organic chloride does not generate equipment corrosion in naphtha, but during carrying out pre-add hydrogen, organochlorine is in high temperature
Chemical reaction production hydrogen chloride occurs under the conditions of high pressure and hydrogen are existing, hydrogenation system upstream device can be corroded.Such as：Corrosion
Air cooling apparatus, the water cooling equipment of pre- hydrogenation system；Hydrogen chloride and the ammonia reaction for adding hydrogen to generate generate ammonium chloride, block pipeline；Very
To the entrance for entering pre-add hydrogen circulating hydrogen compressor, the normal operation of circulating hydrogen compressor is seriously affected.Organochlorine in order to prevent
The corrosion that hydrogen chloride causes equipment is converted into crude oil processing, many researchers develop a plurality of types of dechlorinations
Agent, commercial Application has been for many years for some antichlors.But these antichlors are concentrated mainly on to butter in distillate
Removing, is also rarely reported for the antichlor of the removing of organochlorine.US5928500, which is described, micro in a kind of removing the hydrocarbon component to be had
The method of machine chloride, this method do the gold of carrier, Ni, Co or iron and its mixture using the tripoli of porosity high-specific surface area
Belong to or metal oxide is the adsorbent of active component, converts organic chloride to metal chloride to be removed.
A kind of adsorbent of removing organic chloride is described in CN200810049261 patents, this adsorbent uses porosity object
Matter, such as molecular sieve, aluminium oxide, activated carbon are the mixed of carrier, impregnating metal chloride or metal chloride and metal sulfate
Close object.The adsorbent can convert organic chloride to butter under conditions of aqueous, the side being then washed with water
Method removes butter, this will increase dechlorinating refined step, causes technique cumbersome and also relates to the laggard one-step removal of washing
The problem of moisture.Although infusion process is prepared simply, the surface area of adsorbent and hole can be caused to hold drop acutely, to influence to move
State adsorption effect and bed service life.US3864243 discloses a kind of method removing chloride and other impurity in olefin component,
Under room temperature, condition of normal pressure, chloride in the hydrocarbon component can be adsorbed with 13X the or 10X zeolite molecular sieves of aperture 8A or so de-
It removes.Influence of the silica alumina ratio of molecular sieve to the organic HCl content of removing is disclosed in US20120190906 patents, the results showed that sial
There is higher organochlorine adsorption capacity than the 13X molecular sieves less than 1.25.Although 13X molecular sieves have centainly organochlorine
Removal effect, but total adsorption capacity is limited and Dynamic Adsorption rate is low, and service life is short.
Invention content
Present invention is generally directed to remove the deficiencies of catalyst chlorosity of organochlorine is low, non-renewable place in naphtha, open
Send out a kind of reproducible catalyst for removing organic chloride in the oil products such as naphtha containing chlorine.The present invention provides one kind
The catalyst and preparation method thereof of reproducible removing organochlorine.Catalyst of the present invention has good removing organochlorine performance, and
Renewable recycling.
Catalyst of the present invention is the composite oxides that are synthesized using silicon source, silicon source and magnesium source as carrier, is with Ni, Mo, Cu, Ce
A kind of reproducible removing organochlorine catalyst is made in active component.
The catalyst, it is characterised in that：The composite oxides of the silicon source, silicon source and the synthesis of magnesium source, by quality
Percentages SiO2Content is 3% ~ 10%, and content of MgO is 9.2 ~ 18.9%, remaining is Al2O3。
The catalyst activity component content is in terms of catalyst gross mass, and NiO contents are 6.2- in active component
15.6%, CuO content are 16.1-25.4%, MoO3Content is 1.7-4.6%, CeO2Content is 1.5-2.5%.
The catalyst, it is characterised in that：The specific surface area of the catalyst is 430 ~ 526m2/ g, Kong Rongwei 0.85 ~
1.1ml/g, aperture 4-10nm.
The preparation method of the catalyst, it is characterised in that：By a certain amount of silicon source, silicon source, magnesium source, soluble nickel
Salt, surfactant and water are uniformly mixed, and obtain sealing in starting sol gel mixture immigration synthesis reactor, at 150 ~ 220 DEG C
Crystallization 8 ~ 24 hours.The pH value of crystal slurries is adjusted to neutrality, be added into reaction kettle a certain amount of solubility molybdenum salt, can
The mantoquita of dissolubility and soluble cerium salt, carry out 8 ~ 28h of ion-exchange reactions.To the end of reaction, above-mentioned slurries are added and are flocculated
Agent precipitates, is filtered, washed, drying, extruded moulding, and filtered fluid reuse is used for lower secondary response.Through 100 ~ 150 DEG C dry 2 ~ 4
Hour, 500 ~ 700 DEG C of roastings obtain a kind of reproducible removing organochlorine catalyst after 3 ~ 6 hours.
According to catalyst provided by the invention, the pore volume, specific surface area, bore dia are surveyed using nitrogen low-temperature adsorption
It is fixed.
A kind of renewable removing organochlorine catalyst prepared according to the method provided by the invention is suitable for containing organochlorine
Distillate is handled, and organochlorine can be effectively removed, and produces the distillate containing relatively low chlorine.
The above-mentioned technical proposal of the present invention has the following advantages compared with prior art：
（1）For this catalyst from the angle of Molecular Design, the catalyst prepared has orderly pore passage structure, particular bore
Diameter, hole hold larger.The performance of organochlorine is desorbed using catalyst cryogenic absorption organochlorine, pyrolytic conversion, solves previous catalyst
By simple adsorbing and removing inorganic chlorine activity can not adsorbent organic chlorine the drawbacks of, while solve organochlorine absorption class catalyst chlorine
Hold too low the problem of can not regenerating.
（2）Magnesium silicate, adsorbin have preferable adsorption capacity, two kinds of objects to the organic chloride in naphtha
Matter can regard MgOSiO as2、Al2O3 .SiO2, that is, loaded the silica of metal oxide.In mixed adsorbent, magnesia
There is synergistic effect with two kinds of metal oxides of aluminium oxide, the polarity of adsorbent is increased, to improve adsorbent to stone brain
The adsorption capacity of chloride in oil.
（3）Ce preferably disperses on the surface of the carrier conducive to Ni-Mo-Cu isoreactivities component, inhibits the growth of crystal grain, catalysis
The specific surface area of agent and hole, which hold, to increase, and chlorosity increases.Ce during catalyst roasts3+Oxidation is appraised at the current rate as Ce4+, and Ce4+Tool
Have stronger that electronic capability, i.e. L acid amount increase, the total acid content increase of Ce modified catalysts can effectively inhibit oil product alkene
Polymerization, prevents catalyst coking, improves the anti-coking performance of catalyst, extend the dechlorination service life of catalyst.
（4）Environmentally friendly nickel-ammonia solution is used as template, successfully urges active component nickel insertion micropore
In agent presoma, for the guarantee that provides of synthesis that subsequent Ni-Mo-Cu-Ce is active constituent catalyst.Since nickel insertion is micro-
Kong Zhong can preferably protect nickle atom when the temperature rises, while nickel activates the Active Chlorine of absorption on a catalyst, passes through original
Sub- transferance allows it to be desorbed from catalyst；And ensure the nickel on catalyst from poisoning, renewable recycling.
Example is embodied：
With reference to specific implementation case come the characteristics of catalyst of the present invention is described in detail, preparation method and its catalytic performance, but this
Invention is not limited only to these examples, does not also constitute any restriction to invention practical range.
Embodiment 1：
By 197g Aluminum sols（Al2O3Content 22%）, 33.3g Ludox（SiO2Content 30%）, 38.1g nickel nitrates, 2.5g tetra-
Ethyl phosphonium bromide ammonium and 300g water stir 6h, are uniformly mixed, and obtain starting sol gel mixture, and starting sol gel masses move
Enter in synthesis reactor and seal, in 220 DEG C of crystallization 8 hours.The pH value of crystal slurries is adjusted to neutrality with 0.5mol/L urea, is added
4.28g ammonium molybdates, 59.7g copper nitrates and 6.3g cerous nitrates carry out ion-exchange reactions 8h.To the end of reaction, by above-mentioned slurries
Be added flocculant precipitate, be filtered, washed, drying, extruded moulding, filtered fluid reuse is for lower secondary response.Through 150 DEG C of dryings
2 hours, 500 DEG C roasting 6 hours after obtain renewable absorption dechlorination catalyst Cat1.
Embodiment 2：
By 179g Aluminum sols, 10g Ludox, 44.6g magnesium chlorides, 15.1g nickel nitrates, 2.5g cetyl trimethylammonium bromides and
300g water stirs 10h, is uniformly mixed, and obtains starting sol gel mixture, and starting sol gel masses move into close in synthesis reactor
Envelope, in 150 crystallization 8 hours.The pH value of crystal slurries is adjusted to neutrality with 0.5mol/L urea, addition 6.26g ammonium molybdates,
59.7g copper nitrates and 6.3g cerous nitrates carry out ion-exchange reactions 28h.To the end of reaction, above-mentioned slurries addition flocculant is sunk
It forms sediment, be filtered, washed, drying, extruded moulding, filtered fluid reuse is used for lower secondary response.It is 4 hours, 500 DEG C dry through 120 DEG C
Roasting obtains renewable absorption dechlorination catalyst Cat2 after 6 hours.
Embodiment 3
By 192.5g Aluminum sols, 23g Ludox, 33g magnesium chlorides, 26.6g nickel nitrates, 2.5g tetraethylammonium bromides and 300g water,
6h is stirred, is uniformly mixed, obtains starting sol gel mixture, starting sol gel masses are moved into synthesis reactor and sealed, 220
DEG C crystallization 20 hours.The pH value of crystal slurries is adjusted to neutrality with 0.5mol/L urea, 4.28g ammonium molybdates, 48.7g nitre is added
Sour copper and 5.1g cerous nitrates carry out ion-exchange reactions 20h.To the end of reaction, flocculant precipitation, mistake is added in above-mentioned slurries
Filter, washing, dry, extruded moulding, filtered fluid reuse are used for lower secondary response.It is 3 hours dry through 120 DEG C, 600 DEG C of roastings 5
Renewable absorption dechlorination catalyst Cat3 is obtained after hour.
Embodiment 4：
By 244g Aluminum sols, 23g Ludox, 21.7g magnesium chlorides, 26.6g nickel nitrates, 2.5g cetyl trimethylammonium bromides and
300g water stirs 6h, is uniformly mixed, and obtains starting sol gel mixture, and starting sol gel masses move into close in synthesis reactor
Envelope, in 180 DEG C of crystallization 20 hours.The pH value of crystal slurries is adjusted to neutrality with 0.5mol/L urea, addition 2.3g ammonium molybdates,
37.8g copper nitrates and 3.78g cerous nitrates carry out ion-exchange reactions 28h.To the end of reaction, flocculant is added in above-mentioned slurries
It precipitates, be filtered, washed, drying, extruded moulding, filtered fluid reuse is used for lower secondary response.It is 4 hours dry through 100 DEG C, 700
DEG C roasting 3 hours after obtain renewable absorption dechlorination catalyst Cat4.
Embodiment 5：
The present embodiment is to the dechlorination catalyst of above-described embodiment 1~4 and the catalyst Cat5 activity comparative determinations of the prior art.
The porous and Acidity of the said goods and coker gasoline desilicification catalyst are analyzed, analysis result such as table 1
The physico-chemical property of 1 different catalysts of table
MgO is introduced in the carriers of catalyst Cat2 ~ 4 provided by the invention as can be seen from Table 1, compared to the Cat1 for being not introduced into MgO
There is more preferably specific surface area and Kong Rong.Catalyst Cat1 ~ 4 provided by the invention are by specific preparation process, compared to same
γ-Al under equal compositions2O3Aperture with bigger and Kong Rong.
Catalyst prepared by each embodiment is taken to the reaction tube of 27 × 3.5mm of 30ml loading Φ, catalyst bed floor height respectively
48mm is spent, raw materials used oil is that naphtha property is shown in Table 2.
2 naphtha property of table
| Project | Density, g/cm3 | Total chlorine, μ g/g |
| Naphtha | 0.64 | 246 |
Analysis about Selection instrument：KY-200 microcoulomb chlorinity titrators measure organochlorine in oil.30ml catalyst is taken to be packed into fixed bed
Reactor carries out activation in device, is passed through hydrogen, adjustment system pressure is 0.7MPa, amounts of hydrogen 50mL/min, with 10 DEG C/min
230 DEG C, constant temperature 2h are warming up to, is then warming up to 400 DEG C again with identical heating rate, constant temperature 4h makes catalyst activate completely.It is living
After change, device is replaced into nitrogen, is pumped into feedstock oil naphtha, and oil inlet air speed is 1.5h-1, reaction temperature is 150 DEG C, reaction
Pressure is 0.7MPa, and nitrogen is gas/oil to compare 100:1 carries out dechlorination experiment, and product is organic through washing removing inorganic chlorine post analysis after dechlorination
Chlorinity.After the dechlorination effect of catalyst declines, catalyst is warming up to 250 DEG C with 10 DEG C/min, reaction pressure improve to
1.4 MPa, are purged with nitrogen, are waited for that reactor outlet gas detection chlorinity is zero, are stopped regeneration.Reaction temperature is cooled to
150 DEG C, pressure is down to 0.7MPa, re-starts dechlorination experiment.Sampling analysis after a certain period of time is reacted, reaction result such as table is recorded
Shown in 3.
The 3 total chlorine of dechlorination determination of activity result of table, μ g/g
From the data of table 3 it is found that tetra- kinds of dechlorination catalysts of Cat1, Cat2, Cat3, Cat4 are in about 240 μ of naphtha content of organic chloride
Removing organochlorine experiment is carried out in g/g raw materials, organochlorine removing reaches 97.9% or more, and comparative catalyst Cat5 is in organochlorine
It is poor that organochlorine effect is removed in existing environment.To catalyst below performance in order to further appreciate that catalyst of the present invention
Cat 3 carries out regeneration tests, and experimental result is shown in Table 3.The experimental results showed that：Catalyst Cat3 catalyst can effective adsorbing and removing
Organochlorine, and can regenerate, it reuses.Inventor additionally use the above method to the catalyst obtained by other each embodiments into
It has gone long period experiment, can obtain preferable as a result, showing that catalyst of the present invention has preferable activity and stability.
Claims (9)
1. a kind of catalyst of reproducible removing organochlorine, it is characterised in that：The catalyst is closed with silicon source, silicon source and magnesium source
At composite oxides be carrier, using Ni, Mo, Cu, Ce as active component.
2. catalyst described in accordance with the claim 1, it is characterised in that：The composite oxide carrier, by mass percentage
Count SiO2Content is 3% ~ 10%, and content of MgO is 9.2 ~ 18.9%, remaining is Al2O3。
3. catalyst described in accordance with the claim 1, it is characterised in that：The silicon source is Aluminum sol；Silicon source is Ludox；Magnesium
Source is magnesium chloride.
4. catalyst according to claim 1, it is characterised in that：The specific surface area of the catalyst is 430 ~ 526m2/ g, hole
Hold is 0.85 ~ 1.1ml/g, aperture 4-10nm.
5. catalyst described in accordance with the claim 1, it is characterised in that：Catalyst activity component content is with catalyst gross mass
It counts, NiO contents are 6.2-15.6% in active component, and CuO contents are 16.1-25.4%, MoO3Content is 1.7-4.6%, CeO2
Content is 1.5-2.5%.
6. according to the preparation method of claim 1 ~ 5 any one of them catalyst, it is characterised in that：A kind of reproducible removing
The preparation method of organochlorine catalyst is as follows：
A certain amount of silicon source, silicon source, magnesium source, soluble nickel salt, surfactant and water are uniformly mixed, starting sol is obtained
Gel mixture was moved into synthesis reactor and is sealed, in 150 ~ 220 DEG C of crystallization 8 ~ 24 hours；During the pH value of crystal slurries is adjusted to
Property, the molybdenum salt of a certain amount of solubility, the cerium salt of soluble mantoquita and solubility are added into reaction kettle, carries out ion exchange
React 8 ~ 28h；To the end of reaction, above-mentioned slurries addition flocculant is precipitated, be filtered, washed, is dried, extruded moulding, after filtering
Liquid reuse is used for lower secondary response；2 ~ 4 hours dry through 100 ~ 150 DEG C, 500 ~ 700 DEG C of roastings obtain one kind after 3 ~ 6 hours can
Regenerated removing organochlorine catalyst.
7. the preparation method of catalyst according to claim 6, it is characterised in that：The surfactant is tetraethyl
Ammonium bromide or cetyl trimethylammonium bromide.
8. the preparation method of catalyst according to claim 6, it is characterised in that：With urea by the pH value tune of crystal slurries
It saves to neutrality.
9. the preparation method of catalyst according to claim 6, it is characterised in that：Soluble molybdenum salt, mantoquita and cerium salt
For its ammonium salt or nitrate.
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