JP2007533428A - ゼオライトのインサイチュ結晶化で生じさせたfcc触媒 - Google Patents
ゼオライトのインサイチュ結晶化で生じさせたfcc触媒 Download PDFInfo
- Publication number
- JP2007533428A JP2007533428A JP2006532935A JP2006532935A JP2007533428A JP 2007533428 A JP2007533428 A JP 2007533428A JP 2006532935 A JP2006532935 A JP 2006532935A JP 2006532935 A JP2006532935 A JP 2006532935A JP 2007533428 A JP2007533428 A JP 2007533428A
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- JP
- Japan
- Prior art keywords
- microspheres
- catalyst
- kaolin
- zeolite
- alumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 199
- 239000010457 zeolite Substances 0.000 title claims abstract description 116
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 111
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 238000002425 crystallisation Methods 0.000 title description 30
- 230000008025 crystallization Effects 0.000 title description 30
- 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 abstract description 171
- 239000004005 microsphere Substances 0.000 claims abstract description 148
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 129
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 129
- 238000001354 calcination Methods 0.000 claims abstract description 23
- 238000004231 fluid catalytic cracking Methods 0.000 claims abstract description 11
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract 2
- 239000011159 matrix material Substances 0.000 claims description 75
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 61
- 238000000034 method Methods 0.000 claims description 55
- 239000011148 porous material Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 29
- 238000005336 cracking Methods 0.000 claims description 17
- 239000012013 faujasite Substances 0.000 claims description 16
- 229930195733 hydrocarbon Natural products 0.000 claims description 16
- 150000002430 hydrocarbons Chemical class 0.000 claims description 16
- 229910001593 boehmite Inorganic materials 0.000 claims description 15
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 238000001694 spray drying Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 239000004215 Carbon black (E152) Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- 230000001747 exhibiting effect Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 29
- 230000000694 effects Effects 0.000 description 28
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 25
- 229910052863 mullite Inorganic materials 0.000 description 25
- 239000011230 binding agent Substances 0.000 description 24
- 239000000571 coke Substances 0.000 description 22
- 239000000047 product Substances 0.000 description 20
- 239000004115 Sodium Silicate Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 19
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 19
- 229910052911 sodium silicate Inorganic materials 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000000203 mixture Substances 0.000 description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 239000011734 sodium Substances 0.000 description 15
- 239000003999 initiator Substances 0.000 description 14
- 229910052596 spinel Inorganic materials 0.000 description 14
- 239000011029 spinel Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 238000010304 firing Methods 0.000 description 11
- 230000006872 improvement Effects 0.000 description 11
- 238000000354 decomposition reaction Methods 0.000 description 10
- 229910052761 rare earth metal Inorganic materials 0.000 description 10
- 239000007921 spray Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- -1 ammonium ions Chemical class 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 6
- 238000002161 passivation Methods 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 239000004927 clay Substances 0.000 description 5
- 230000006870 function Effects 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 229910052720 vanadium Inorganic materials 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000008186 active pharmaceutical agent Substances 0.000 description 3
- 238000004523 catalytic cracking Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 230000000670 limiting effect Effects 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005906 dihydroxylation reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000012035 limiting reagent Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000001935 peptisation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- UVPKUTPZWFHAHY-UHFFFAOYSA-L 2-ethylhexanoate;nickel(2+) Chemical compound [Ni+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O UVPKUTPZWFHAHY-UHFFFAOYSA-L 0.000 description 1
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical group [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000012084 conversion product Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005414 inactive ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007518 monoprotic acids Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000012690 zeolite precursor Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0045—Drying a slurry, e.g. spray drying
-
- 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
-
- 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
-
- 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
- B01J29/084—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
- B01J37/08—Heat treatment
-
- 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
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
- C10G11/04—Oxides
- C10G11/05—Crystalline alumino-silicates, e.g. molecular sieves
-
- 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
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/14—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts
- C10G11/18—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils with preheated moving solid catalysts according to the "fluidised-bed" technique
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/005—Spinels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- 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
- B01J2229/42—Addition of matrix or binder particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
Description
「マトリックスはシーブの中に存在するナトリウムの掃きだめとして働くことでマトリックス触媒の中のゼオライト粒子に安定性を加えると言われている。前記マトリックスは下記の追加的機能を果たす:ゼオライトを希釈する機能;それを熱および蒸気および機械的摩滅に対して安定にする機能;ゼオライトを最大能力で使用することができかつ再生を容易に行うことができるように高い間隙率を与える機能;そして最後に、再生および分解中の伝熱そして大規模な接触分解中の熱貯蔵にとって重要であるバルク特性(bulk properties)を与える機能。」
従来技術の流動接触分解触媒では、下記の2つの一般的技術の中の1つを用いて活性ゼオライト系成分を当該触媒の微小球の中に取り込ませている。1つの技術では、ゼオライト系成分を結晶化させた後に個別の段階で微小球の中に取り込ませる。2番目の技術、即ちインサイチュ技術では、最初に微小球を生じさせた後にゼオライト系成分を前記微小球自身の中で結晶化を起こさせることでゼオライト系成分と非ゼオライト系成分の両方を含有する微小球を生じさせる。
本発明に従い、反応性メタカオリンと不活性な含水カオリンを含有する前駆体である反応性微小球を生じさせることを通して、新規なマクロ多孔性インサイチュ生成ゼオライト触媒を生じさせる。前記微小球をアルカリ性シリケート溶液と反応させることでゼオライト触媒を生じさせる。前記含水カオリンをマトリックス前駆体として存在させると上述した同時係属中の出願である米国連続番号09/956,250に開示したマクロ多孔構造に似かよったマクロ多孔構造がもたらされることを見いだした。前記同時係属中の出願では、焼成を受けさせた超微細な含水カオリンをマトリックス前駆体として用いてそのようなマクロ多孔性構造を達成している。本発明の触媒は、金属不動態化に有用であることを確認した焼成ベーマイトアルミナばかりでなく、また、ある程度ではあるが、特徴的な発熱を経る焼成を受けたカオリンに由来するマトリックスも含有している可能性がある。
(発明の詳細な説明)
水和カオリンとメタカオリンと結合剤、例えばシリカゾルまたはケイ酸ナトリウムなどの供給材料混合物に噴霧乾燥を受けさせることで本発明の触媒を製造する。その噴霧乾燥微小球に場合により酸による中和を受けさせかつ洗浄を受けさせることでナトリウム含有量を低くしてもよい。その噴霧乾燥微小球に好適には後で焼成を受けさせることで前駆体である多孔質微小球を生じさせる。本発明で重要なことは、含水カオリン成分がメタカオリンに吸熱変化しないように焼成を低い方の温度で行うことで前記含水カオリンが不活性な成分として保持されるようにすることである。前記噴霧乾燥微小球に焼成を受けさせる時に用いる焼成温度は1000度F未満、好適には800度F未満であってもよい。
(実施例2および3)
実施例1の微小球の中にゼオライトを成長させる目的で、ゼオライト含有量の調整でメタカオリン含有量が100%の微小球を添加した場合と添加しない場合の2つの反応を実施した。各実施例の反応成分を表4に示す。
実施例4および5の微小球には特徴的発熱を経る焼成を受けた超微細カオリン[Ansilex 93(商標)]を含有させ、それに噴霧乾燥を車型噴霧器が備わっているパイロットプラントで受けさせた。噴霧乾燥を受けさせるスラリーを生じさせる時に用いた各成分の重量パーセントを表5に示す。各カオリン成分の重量パーセントは結合剤無し基準が基になっている。
(実施例6および7)
実施例4および5の微小球を用いてゼオライトを成長させる目的で2つの反応を実施した。各実施例の反応成分を表6に示す。
(実施例8および9)
これらの実施例では、金属耐性アルミナを含有させた微小球の調製を開示する。一般的には、最初に高分散性の金属耐性ベーマイトに焼成を1450度Fで2時間受けさせることでガンマアルミナにした。次に、そのガンマアルミナを水性媒体中で粉砕してAPSが約2ミクロンになるまで小さくした。その粉砕したガンマアルミナスラリーに解膠を受けさせるか或は受けさせないでそれをCowlesミキサーに入れておいたメタカオリンと含水カオリンとAnsilex−93(商標)(適用可能な場合)が入っているスラリーに加えた。次に、前記スラリーにケイ酸ナトリウム(SiO2/Na2Oが3.22)を噴霧に適した混合物が生じるに充分な量の水と一緒に加えた。前記スラリーに噴霧乾燥を車型噴霧器が備わっているパイロットプラントで受けさせた。前記スラリーに入っている各成分の重量パーセントを表7に示す。再び、アルミナ成分のパーセントは結合剤無し基準が基になっている。
(実施例10および11)
実施例8および9の微小球を表8に示す成分と反応させた。
これらの実施例では、本発明の触媒(実施例3、6および7)が示す性能を2つの比較実施例のそれと対比させて測定する。その2つの比較実施例は米国連続番号09/956,250の触媒(比較1)および米国特許第5,395,908号の触媒(比較2)に相当する。これらの触媒サンプルを実験室で1450度Fの100%蒸気中で4時間失活させた。次に、その失活させた触媒をインジェクターの高さが1.125”のACE(商標)流動床試験装置に入れてコンラドソン炭素が約6%の芳香族供給材料を用いた試験を970度Fで受けさせた。活性FCC触媒の量を変えることで活性を変化させた。前記ACE装置に入れる不活性微小球と活性触媒の総量を12.0gに一定に保持した。変換率が70%の時の収率を報告する。
(実施例17−21)
以下に示す実施例では、本発明の触媒(実施例10および11)が示す性能を米国連続番号09/956,250の触媒(比較3)、2001年10月17日付けで出願した米国連続番号09/978,180の触媒(比較4)および2002年6月6日付けで出願した米国連続番号10/164,488の触媒(比較5)のそれに対比させて測定する。比較触媒4および5は残渣分解に適する種類の触媒に相当する。これらの触媒サンプルに前以て蒸気処理を1350度Fの100%蒸気中で2時間受けさせておいた後、オクタン酸ニッケルおよびナフテン酸バナジウムを用いて3000/3000PPMのニッケルとバナジウムを湿り開始で添加した後、後蒸気処理を蒸気が90%で空気が10%の混合物中で1450度Fにおいて4時間受けさせた。次に、この上に示した実施例に記述したプロトコルに従ってACEを用いて各触媒が示す性能を測定した。変換率が70%の時の収率を比較した。
(実施例22−24)
これらの実施例でもまた本発明の触媒が示す金属不動態化の方が比較5の触媒および商業的残渣用触媒(比較6)よりも向上していることを示す。実施例17−21の様式に比べて異なる様式で失活させた触媒を用いてACEデータを得た。3サンプルを実験室で前以て蒸気で失活させておき、ニッケルおよびバナジウムに関する流動床分解、後蒸気処理による失活プロトコルを実施した。NiおよびVの典型的な充填率はそれぞれ2800PPMおよび3600PPMであった。次に、その失活させた触媒をインジェクターの高さが2.125”のACE装置に入れてそれらにこの上に示した実施例で用いた供給材料と同じ供給材料を用いた試験を8WHSVにおいて998度Fの分解温度で受けさせた。前記ACE装置に入れる触媒の量を一定に9.0gにしそして送り込む油の量を変えることで活性を変化させた。変換率が75%の時の生成物収率を示す。
Claims (10)
- ゼオライト系流動接触分解触媒であって、
(a)メタカオリン含有反応性微小球からインサイチュで結晶化したアルミノケイ酸塩ゼオライトを少なくとも約15重量%、および
(b)前記反応性微小球に含まれていた含水カオリンから生じたアルミナ含有マトリックス、
を含んで成る触媒。 - 前記反応性微小球が前記アルミナ含有成分を基準にして含水カオリンを5−80重量%、メタカオリンを20−50重量%、焼成ベーマイトを0−30重量%および特徴的発熱を経る焼成を受けたカオリンを0−40重量%含んで成る請求項1記載の触媒。
- 前記反応性微小球が前記アルミナ含有成分の重量を基準にして含水カオリンを10−75重量%、メタカオリンを25−45重量%、焼成ベーマイトを10−25重量%および前記焼成カオリンを5−30重量%含んで成る請求項1記載の触媒。
- 孔径が40−20,000オングストロームの範囲内の水銀細孔容積が0.25cc/gより大きい請求項1記載の触媒。
- メタカオリン含有反応性微小球からインサイチュで結晶化したY−ファウジャサイトを含有する触媒微小球を含んで成る流動接触分解触媒であって、前記反応性微小球に含まれていた含水カオリンから生じた非ゼオライト系アルミナ含有マトリックスを含んで成っていて直径が40−20,000オングストロームの範囲内の孔に関して約0.15cc/gより大きい水銀間隙率を示す触媒微小球を含んで成る流動接触分解触媒。
- 更に、前記アルミナ含有マトリックスが57%固体未満のインシピエントスラリー点を示すアルミナ含有前駆体から生じたものである請求項5記載の流動接触分解触媒。
- 流動接触分解触媒を生じさせる方法であって、
(a)含水カオリンとメタカオリンを含んで成る水性スラリーを噴霧乾燥させることで直径が20−150ミクロンの範囲内の反応性微小球を生じさせ、
(b)前記噴霧乾燥微小球とアルカリ性シリケート水溶液を前記反応性微小球からインサイチュで結晶化したY−ファウジャサイトが生じるような温度でそのような時間反応させる、
ことを含んで成る方法。 - 前記噴霧乾燥微小球を前記アルカリ性シリケート水溶液と反応させる前に前記噴霧乾燥微小球に焼成を1000度F未満の温度で受けさせておく請求項7記載の方法。
- 前記水性スラリーが含水カオリンを5−80重量%、メタカオリンを20−50重量%、焼成ベーマイトを0−30重量%および前記焼成カオリンを0−40重量%含有するようにする請求項8記載の方法。
- 炭化水素原料をFCC条件下で分解させる方法であって、前記炭化水素原料を請求項1の触媒に接触させることを含んで成る方法。
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Also Published As
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CA2524548C (en) | 2012-07-17 |
WO2004103558A1 (en) | 2004-12-02 |
EP1624965A1 (en) | 2006-02-15 |
CA2524548A1 (en) | 2004-12-02 |
WO2004103558B1 (en) | 2005-04-14 |
MXPA05012340A (es) | 2006-01-30 |
JP5337343B2 (ja) | 2013-11-06 |
US6942783B2 (en) | 2005-09-13 |
KR101042413B1 (ko) | 2011-06-16 |
KR20060010819A (ko) | 2006-02-02 |
BRPI0410764A (pt) | 2006-06-27 |
AU2004240913A1 (en) | 2004-12-02 |
TW200505572A (en) | 2005-02-16 |
CN100528351C (zh) | 2009-08-19 |
US20040235642A1 (en) | 2004-11-25 |
CN1795048A (zh) | 2006-06-28 |
BRPI0410764B1 (pt) | 2016-07-05 |
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