WO1999061553A1 - New silicoaluminophosphates having an ael structure, a method for their preparation and their use as fcc catalysts - Google Patents
New silicoaluminophosphates having an ael structure, a method for their preparation and their use as fcc catalysts Download PDFInfo
- Publication number
- WO1999061553A1 WO1999061553A1 PCT/US1999/011470 US9911470W WO9961553A1 WO 1999061553 A1 WO1999061553 A1 WO 1999061553A1 US 9911470 W US9911470 W US 9911470W WO 9961553 A1 WO9961553 A1 WO 9961553A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silicon
- molecular sieve
- sapo
- molar percent
- catalyst
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
- C01B37/08—Silicoaluminophosphates (SAPO compounds), e.g. CoSAPO
-
- 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
- B01J29/005—Mixtures of molecular sieves comprising at least one molecular sieve which is not an aluminosilicate zeolite, e.g. from groups B01J29/03 - B01J29/049 or B01J29/82 - B01J29/89
-
- 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
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates (SAPO compounds)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
-
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
- C10G45/64—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
-
- 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
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/20—C2-C4 olefins
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S423/00—Chemistry of inorganic compounds
- Y10S423/30—Alpo and sapo
Definitions
- the molecular sieve has a first number of Si atoms coordinated as Si(4Si),
- the invention is a fluidized catalytic cracking method comprising injecting a feed into an FCC riser reactor having a reaction zone and catalytically cracking the feed in the reaction zone under catalytic cracking conditions in the presence of a cracking catalyst in order to form a cracked product, the cracking catalyst containing a molecular sieve having a framework tetrahedra of silicon, aluminum, and phosphorus, a total silicon amount ranging from above about 4 molar percent to about 20 molar percent, a total aluminum amount ranging from about 40 molar percent to about 55 molar percent, and a total phosphorus amount ranging from about 30 molar percent to about 50 molar percent, the molar percents being based on the total amount of aluminum, phosphorus, and silicon present in the composition, and the molecular sieve having the topology AEL and being isostructural with conventional SAPO-11, wherein
- the molecular sieve has a first number of Si atoms coordinated as Si(4Si)
- the conventional SAPO-11 with the Si amount has a second number of Si atoms coordinated as Si(4Si)
- Figure 5 shows powder x-ray diffraction data from AEL-type SAPOs of examples 5 through 8.
- SAPO materials having the AEL structure and designated ECR-42 herein may be prepared as small crystals with high silicon concentration and without undesirable silicon island formation,
- Section A describes the preferred molecular sieve synthesis processes
- Section B describes the preferred molecular sieve catalysts
- Section C describes the physical differences between the preferred ECR-42 and conventional SAPO-11
- Section D describes the use of the preferred ECR-42 molecular sieve catalysts in catalytic cracking processes.
- a lattice site occupied by a silicon 4+ cation i.e., a "silicon site”
- the four nearest neighbor lattice sites may therefore be occupied by one silicon and three aluminum cations, two silicon and two aluminum cations, three silicon and one aluminum cations, four silicon cations, or four aluminum cations.
- conventional AEL-type SAPOs with increased silicon concentration, above about 4 molar % contain undesirable silicon islands, i.e., silicon atoms in the framework having four silicon atom nearest neighbors.
- the silicon atoms in the preferred composition are physically distributed so that the silicon island concentration is greatly reduced compared with conventional SAPO-1 1 (i.e., SAPO- 11 prepared in accordance with the methods disclosed in the prior art) having the same total silicon concentration.
- the preferred molecular sieve compositions have both a desirably high silicon concentration and a desirable silicon atom dispersion (i.e. a smaller number of silicon islands than would be present in conventional SAPO-11 with the same silicon content) may be formed in accordance with conventional molecular sieve synthesis techniques.
- the preferred ECR-42 synthesis processes commence with the formation of a silicoaluminophosphate gel having the formula
- Non-limiting examples of useful surfactants include one or more of long chain alkylamines such as hexadecylamine, tetradecylamine, dodecylamine, decylamine, or octylamine, or dimethyl alkylamine compounds such as dimethylhexadecylammine or dimethyloctylamine, or trimethylalkylammonium salts such as trimethy lhexadecy lammounium chloride .
- long chain alkylamines such as hexadecylamine, tetradecylamine, dodecylamine, decylamine, or octylamine
- dimethyl alkylamine compounds such as dimethylhexadecylammine or dimethyloctylamine
- trimethylalkylammonium salts such as trimethy lhexadecy lammounium chloride .
- the S0L:A1 2 0 3 molar ratio in the synthesis solution preferably ranging from about 0 to about 30, and more preferably ranging from about 4 to about 20, and the Si0 2 :Al 2 0 3 molar ratio preferably ranging from about 0.01 to about 2.0, and more preferably ranging from about 0.1 to about 0.8.
- the synthesis solution may then be subjected to gel formation conditions in order to provide the silicoaluminophosphate gel.
- the ingredients of the synthesis solution, surfactant solution, and alumino phosphate mixture may be mixed in any order.
- the organic silicon source may be added to a mixture of phosphoric acid and the water-soluble organic solvent.
- the template and the surfactant may then be added, with the water and aluminum source being added last.
- the preferred ECR-42 molecular sieve compositions are crystalline, and may be prepared with crystal sizes ranging from about 0.001 micrometers to about 1.0 micrometers. Preferably, crystal size ranges from about 0.01 micrometers to about 0.5 micrometers.
- the synthesis may be adjusted to prepare crystals of decreased size by diluting the synthesis solution with surfactant, co- solvent, and mixtures thereof. Small crystals may also be prepared by conventional methods such as seeding and high shear agitation rates.
- the ECR-42 molecular sieve materials prepared in accordance with these methods are useful as catalytic materials. While not wishing to be bound, it is believed that the silicon distribution within the molecular sieve crystal, as measured for example by Si NMR, is one important characteristic influencing catalytic activity in SAPO materials. Since silicon is responsible for the acidity in SAPO materials, it is desirable that silicon be well dispersed in the aluminophosphate framework for high catalytic activity. Conventional SAPO molecular sieves may contain large silicon islands in the molecular sieve framework. Large silicon islands are undesirable because those silicon atoms at the interior of the islands are catalytically inactive.
- the molecular sieve material formed from the gel as set forth above may be calcined to remove the template.
- the sample may then be allowed to cool, preferably in a dry environment.
- the preferred molecular sieves may contain Si concentrations as low as about 1 wt.%. It is often difficult to obtain high quality NMR data from samples of such a low concentration over the whole range of chemical shifts, and consequently some degree of uncertainty may be introduced into the deconvolutions required to determine the number of Si atoms with zero, one, two, three and four nearest neighbors. Nevertheless, the intensity of the -109 to -115 ppm region is sufficient in molecular sieve materials of even 1 wt.% to determine the approximate molar percent of Si framework atoms having four Si atom nearest neighbors, i.e., Si atoms located in the center of Si islands.
- the conventional FCC catalyst may be a composition of catalyst particles and other reactive and non-reactive components, such catalysts are described in European patent document No. 0 600 686A1, incorporated by reference herein.
- the SAPO catalyst may be in the form of particles, and may include fines, inert particles, particles containing a metallic species, and mixtures thereof.
- Inert particles may contain species such as silica, alumina, clay, and mixtures thereof.
- More than one type of catalyst particle may be present in the catalyst.
- individual catalyst particles may contain large pore molecular sieve catalyst, the ECR-42 molecular sieve catalyst, other shape selective molecular sieve such as zeolite, and mixtures thereof.
- Conventional FCC catalysts useful in the invention also include catalysts containing a zeolite Y, zeolite beta, mixtures thereof, and catalysts containing a mixture of zeolite Y and a shape selective molecular sieve species such as ZSM- 5, or a mixture of an amorphous acidic material and ZSM-5.
- Such catalysts are described in U.S. Patent No. 5,318,692, incorporated by reference herein.
- the zeolite portion of the catalyst particle will typically contain from about 5 wt.% to 95 wt.% zeolite-Y (or alternatively the amorphous acidic material) and the balance of the zeolite portion being ZSM-5.
- the large pore and shape selective catalysts may include "crystalline admixtures" which are thought to be the result of faults occurring within the crystal or crystalline area during the synthesis of the zeolites.
- crystalline admixtures of ZSM-5 and ZSM-11 are disclosed in U.S. Patent No. 4,229,424 which is incorporated herein by reference.
- the crystalline admixtures are themselves medium pore, i.e., shape selective, size zeolites and are not to be confused with physical admixtures of zeolites in which distinct crystals of crystallites of different zeolites are physically present in the same catalyst composite or hydrothermal reaction mixtures.
- one aspect of the invention is the use of an effective amount of the ECR-42 molecular sieve catalysts of the invention in catalytic cracking processes, especially in FCC processes for producing naphtha and C 2 to C 4 olefins.
- Suitable FCC conditions and the types of feeds that may be used therein are as follows.
- CA hexadecylamine
- the conventional SAPO-11 showed lower activity than the ZSM-5 additive catalyst, as is shown by the naphtha yield reduction of 0.9 wt.% when the conventional SAPO-11 was used as an FCC additive. This contrasts with the ZSM-5 additive, which reduced naphtha yield by 4.0 wt.%. From these data, one can estimate that the ZSM-5 additive catalyst is about four times more active than conventional SAPO-11. As can be seen from Table 3, the preferred ECR-42 material prepared in example 5 is substantially more active than conventional SAPO-1 1.
Abstract
Description
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Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP99925797A EP1062295A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, a method for their preparation and their use as fcc catalysts |
AU42014/99A AU4201499A (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, a method for their preparation and their use as fcc catalysts |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US8668198P | 1998-05-26 | 1998-05-26 | |
US60/086,681 | 1998-05-26 |
Publications (2)
Publication Number | Publication Date |
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WO1999061553A1 true WO1999061553A1 (en) | 1999-12-02 |
WO1999061553A9 WO1999061553A9 (en) | 2000-02-24 |
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Family Applications (7)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/011466 WO1999061555A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in naphtha cracking |
PCT/US1999/011469 WO1999061372A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, and their preparation |
PCT/US1999/011470 WO1999061553A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, a method for their preparation and their use as fcc catalysts |
PCT/US1999/011472 WO1999061559A1 (en) | 1998-05-26 | 1999-05-25 | Silicoaluminophosphates having an ael structure and a method for their preparation and their use |
PCT/US1999/011467 WO1999061556A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, a method for their preparation and their use as naphtha cracking catalysts |
PCT/US1999/011465 WO1999061552A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in catalytic cracking |
PCT/US1999/011468 WO1999061558A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in hydroprocessing |
Family Applications Before (2)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/011466 WO1999061555A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in naphtha cracking |
PCT/US1999/011469 WO1999061372A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, and their preparation |
Family Applications After (4)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/011472 WO1999061559A1 (en) | 1998-05-26 | 1999-05-25 | Silicoaluminophosphates having an ael structure and a method for their preparation and their use |
PCT/US1999/011467 WO1999061556A1 (en) | 1998-05-26 | 1999-05-25 | New silicoaluminophosphates having an ael structure, a method for their preparation and their use as naphtha cracking catalysts |
PCT/US1999/011465 WO1999061552A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in catalytic cracking |
PCT/US1999/011468 WO1999061558A1 (en) | 1998-05-26 | 1999-05-25 | New catalytic silicoaluminophosphates having an ael structure, and their use in hydroprocessing |
Country Status (5)
Country | Link |
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US (10) | US6300537B1 (en) |
EP (7) | EP1062300A1 (en) |
AU (7) | AU4201399A (en) |
TW (2) | TW473540B (en) |
WO (7) | WO1999061555A1 (en) |
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US6867341B1 (en) | 2002-09-17 | 2005-03-15 | Uop Llc | Catalytic naphtha cracking catalyst and process |
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