Classifications

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  • 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
  • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
  • B01J29/7007—Zeolite Beta
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  • B01J35/00—Catalysts, in general, characterised by their form or physical properties
  • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
  • B01J35/391—Physical properties of the active metal ingredient
  • B01J35/394—Metal dispersion value, e.g. percentage or fraction
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  • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
  • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
  • B01J21/08—Silica
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  • 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
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  • B01J29/00—Catalysts comprising molecular sieves
  • B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
  • B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B01J29/00—Catalysts comprising molecular sieves
  • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
  • B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • 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
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  • B01J35/00—Catalysts, in general, characterised by their form or physical properties
  • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • 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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  • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
  • B01J35/63—Pore volume
  • B01J35/638—Pore volume more than 1.0 ml/g
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  • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
  • B01J35/64—Pore diameter
  • B01J35/643—Pore diameter less than 2 nm
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  • B01J35/647—2-50 nm
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  • B01J35/80—Catalysts, in general, characterised by their form or physical properties characterised by their amorphous structures
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • 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
• • C—CHEMISTRY; METALLURGY
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  • 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
  • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
  • C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
  • C10G1/086—Characterised by the catalyst used
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  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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  • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
  • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
  • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
  • C10G45/12—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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  • 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
• • C—CHEMISTRY; METALLURGY
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  • C10G47/10—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used with catalysts deposited on a carrier
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  • C10G47/14—Inorganic carriers the catalyst containing platinum group metals or compounds thereof
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  • 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
  • C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
  • C10G47/02—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used
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  • C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
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  • C10G49/02—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used
  • C10G49/08—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00 characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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  • 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
  • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
  • B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
  • B01J29/74—Noble metals
  • B01J29/7415—Zeolite Beta
• • 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
  • C10G2400/06—Gasoil
• • 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
  • C10G2400/10—Lubricating oil

Definitions

• the present invention relates to a bifunctional catalyst having both hydrogenation and acidic functions.
• zeolite catalysts are well known in the art and possess well-arranged pore systems with uniform pore sizes. However, these materials tend to possess either only micropores or only mesopores. Micropores are defined as ppres having a diameter less than about 2 nm. Mesopores are defined as pores having a diameter ranging from about 2 nm to about 50 nm. [004] Because such hydrocarbon processing reactions are mass-transfer limited, a catalyst with an ideal pore size will facilitate transport of the reactants to active catalyst sites and transport the products out of the catalyst. [005] There is yet need for an improved material having functionalized sites within a porous framework for processes directed to the catalytic conversion and/or adsorption of hydrocarbons and other organic compounds.
• a catalyst for hydrocarbon conversion comprising at least three components (1) at least one element with a hydrogenation function, (2) at least one type of microporous zeolite, and (3) a porous, noncrystalline inorganic oxide having randomly interconnected mesopores and having an X-ray reflection in 2 ⁇ between 0.5 degrees to 2.5 degrees.
• FIG. 1 depicts X-ray diffraction (XRD) patterns of pure zeolite beta and zeolite beta/TUD-1 as prepared in Examples 1, 2 and 3;
• FIG. 2 depicts the mesoporosity of pure zeolite beta and zeolite beta/TUD-
• FIG. 3 depicts XRD patterns for mesoporous material, MCM-22 zeolite, and the composite prepared in Example 4;
• FIG. 4 illustrates the mesopore size distribution of the composite zeolite/TUD-1 prepared in Example 4.
• FIG. 5 depicts XRD patterns of pure zeolite Y and of Sample 5 prepared in Example 5.
• the inventive catalyst has a novel composition essentially comprising three active components: (1) at least one metal selected from group VIII, IB, IIB, VIEB and VD3 in the periodic table of the elements; (2) at least one type of microporous zeolite providing some acidic function; and (3) a noncrystalline inorganic oxide having randomly interconnected mesopores ranging from 1.5 to 25 run in diameter.
• the catalyst can also optionally include boron and/or phosphorus as another component.
• the catalyst may further comprise a binder.
• the metal is mainly selected from transition metals, noble metals and their combinations. These metals include titanium, vanadium, zirconium, manganese, zinc, copper, gold, lanthanum, chromium, molybdenum, nickel, cobalt, iron, tungsten, palladium, rhodium, ruthenium and platinum. Some of the metals can be located on the pore surface of the mesoporous, inorganic oxide; some of them can be incorporated within the zeolite framework as substitutions of lattice atoms and/or located inside the zeolite micropores. Also, some of the metal can be located on the catalyst binder.
• the metal content in the catalyst ranges from 0.3 wt. % to 30 wt. % based on the weight of the catalyst.
• its contents preferably ranges from 0.2 to 5wt%
• transition metals its contents preferably ranges from 3 to 30 wt.%.
• the zeolite described herein includes a microporous zeolite embedded in a non-crystalline, porous inorganic oxide.
• the microporous zeolite can be any type of microporous zeolite. Some examples are zeolite Beta, zeolite Y (including "ultra stable Y” ⁇ USY), mordenite, Zeolite L, ZSM-5, ZSM-11, ZSM-12, ZSM-20, Theta-1, ZSM-23, ZSM-34, ZSM-35, ZSM-48, SSZ-32, PSH-3, MCM-22, MCM-49, MCM-56, ITQ-I, ITQ-2, ITQ-4, ITQ-21, SAPO-5, SAPO-Il, SAPO-37, Breck-6 (also known as EMT), ALPO 4 -5, etc.
• the zeolite can be incorporated into the inorganic oxide or can be in-situ synthesized in the noncrystalline porous oxide.
• the catalyst's zeolite content can range from less than about 1% by weight to more than about 99% by weight or any range therebetween. However, it is preferably from about 3% by weight to 90% by weight, and more preferably from about 4% by weight to about 80% by weight.
• the catalyst with zeolite included preferably contains no more than about 10 volume percent of micropores.
• the noncrystalline, porous inorganic oxide is preferably a three- dimensional, mesoporous inorganic oxide material containing at least 97 volume percent mesopores (i.e., no more than 3 volume percent micropores) based on micropores and mesopores of the inorganic oxide material (i.e., without any zeolite incorporated therein), and generally at least 98 volume percent mesopores.
• This material is described in U.S. Pat. No. 6,358,486, and it is denoted as TUD-I .
• a method for making a preferred porous inorganic oxide is disclosed in US patent 6,358,486 and U.S. patent application serial No: 10/764,797.
• the main chemical composition of the preferred porous inorganic oxide includes, but is not limited to, silica, alumina, silica-alumina, titanium oxide, zirconium oxide, magnesium oxide and their combination.
• the porous inorganic oxide TUD-I can further comprise vanadium, zinc, copper, gold, gallium, lanthanum, chromium, molybdenum, nickel, cobalt, iron and tungsten.
• TUD-I is a noncrystalline material (i.e., no crystallinity is observed by presently available x-ray diffraction techniques). Its average mesopore size, as determined from N 2 -porosimetry, ranges from about 2 nm to about 25 nm.
• the mesoporous inorganic oxide is generally prepared by heating a mixture of (1) a precursor of the inorganic oxide, and (2) an organic templating agent that mixes well with the oxide precursor or the oxide species generated from the precursor.
• the starting material is generally an amorphous material and may be comprised of one or more inorganic oxides such as silicon oxide or aluminum oxide, with or without additional metal oxides.
• the silicon atoms may be replaced in part by other metal atoms.
• metals include, but are not limited to, aluminum, titanium, vanadium, zirconium, gallium, boron, manganese, zinc, copper, gold, lanthanum, chromium, molybdenum, nickel, cobalt, iron, tungsten, palladium and platinum. These metals can be incorporated into the inorganic oxide inside mesopore wall and/or on the mesopore surface. The additional metals may optionally be incorporated into the material prior to initiating the process for producing a structure that contains mesopores. Also after preparation of the material, cations in the system may optionally be replaced with other ions such as those of an alkali metal (e.g., sodium, potassium, lithium, etc.)
• an alkali metal e.g., sodium, potassium, lithium, etc.
• the organic templating agent a mesopore-forming organic compound
• the organic templating agent has a boiling point of at least about 15O 0 C.
• zeolite In order to incorporate zeolite into the porous inorganic oxide, the preferred process is described in US 6,762,143 and US patent publication 2004/0138051.
• the preformed zeolite and/or pretreated zeolite are suspended in a mixture with water.
• the suspension is mixed with an inorganic oxide or a precursor of an inorganic oxide, and at least one mesopore-forming organic compound to form a mixture.
• the mixture preferably forms gel by ageing and/or stirring at certain temperature from room temperature to 100°C and/or by drying at a temperature from 60-120°C.
• the gel is heated up to a temperature from 140 to 200°C and for a period of time sufficient to form a mesoporous inorganic oxide structure.
• the organic pore-forming agent is removed by extraction or extraction together with calcination to obtain a composition having zeolite incorporated into a noncrystalline, porous inorganic oxide.
• U.S. patent application serial No 10/764,797 discloses a method to prepare the noncrystalline, porous inorganic oxide by using complexes.
• Complexes such as, e.g., silitrane, alumatrane, titanatrane, and particularly, silicon- triethanolamine, aluminum-triethanolamine and their mixture can be used as the precursor of the noncrystalline, porous inorganic oxide.
• silitrane, alumatrane, titanatrane, and particularly, silicon- triethanolamine, aluminum-triethanolamine and their mixture can be used as the precursor of the noncrystalline, porous inorganic oxide.
• a composition having zeolite incorporated into a noncrystalline, porous inorganic oxide (TUD-I) can be obtained.
• the said metal having a hydrogenation function can be introduced into the catalyst in different stages of catalyst preparation.
• the metal can be loaded by conventional impregnation and ion exchange. It is also possible that the metal is introduced into zeolite before zeolite incorporated into the porous inorganic oxide (TUD-I) by impregnation or ion exchange.
• the zeolite/TUD-1 is preferable to be shaped using certain binders, such as alumina. After catalyst shaping, the metal can be introduced to the catalyst.
• the composite zeolite/TUD-1 impregnates with at least one solution containing at least one element from group VIB, VIEB, IB, IEB and VIII.
• Sources of group VIB elements that can be used are well known to the skilled person.
• molybdenum and tungsten sources are oxides and hydroxides, molybdic acids and tungstic acids and their salts, in particular ammonium salts such as ammonium molybdate, ammonium heptamolybdate, ammonium tungstate, phosphomolybdic acid, phosphotungstic acid and their salts, silicomolybdic acid, silicotungstic acid and their salts.
• oxides and ammonium salts are used, such as ammonium molybdate, ammonium heptamolybdate and ammonium metatungstate.
• the sources of the group VIII, VIIB, IB and BOB elements that can be used are well known to the skilled person.
• sources of nonnoble metals are nitrates, sulfates, phosphates, halides, for example chlorides, bromides and fluorides, and carboxylates, for example acetates and carbonates.
• sources of noble metals are halides, for example chlorides, nitrates, acids such as chloroplatmic acid, and oxychlorides such as ammoniacal ruthenium oxychloride.
• the catalysts obtained in the present invention are formed into grains of different shapes and dimensions.
• the catalyst can be used in hydrocracking, hydrotreating, and hydroisomerization, in which all catalysts are bifunctional, combining an acid function and a hydrogenating function. It is important to balance these two functions in a certain process.
• the metal selected from transition metal and noble metal offers hydrogenation function.
• the incorporated zeolite offers acid function.
• the noncrystalline porous oxide, TUD-I can offer acid function and/or hydrogenation function, depending the chemical composition of the oxide.
• the porous oxide is a mixed oxide, silica-alumina, and then it supplies acid function.
• the porous oxide is silica containing nickel and molybdenum; it offers hydrogenation function.
• the porous oxide may not offer any acid and hydrogenation function, for example, if the porous oxide is pure silica. So this novel catalyst has a great deal of flexibility to adjust acid function and hydrogenation function.
• Another important feature of this catalyst offers high mesoporosity by using the noncrystalline porous oxide, significantly enhancing mass-transfer and consequently improves the catalytic performance.
• intraparticle mass-transfer limitations reduce catalyst utilization and lower overall catalytic performance.
• Introduction of mesoporosity will boost the overall catalytic performance.
• many refining processes are using heavy petroleum feeds, which need large pores to facilitate the big molecules into and out the catalytic particles.
• Petroleum feeds can include, for example, undeasphalted petroleum residua, deasphalted petroleum residua, tar sands bitumen, shale oil and coal liquid.
• the noncrystalline, porous oxide TUD-I having mesopores size from 1.5 to 30 run can fulfill the need to enhance the mass-transfer.
• the noncrystalline, porous oxide has not only tunable mesopores, but also has randomly interconnected mesopores.
• its randomly interconnected mesopores structure distinguishes from other mesoporous materials, such as MCM-41.
• the randomly interconnected mesopores reduce the chance of pore blockage compared to the materials with one- or two-dimensional pore system.
• the novel catalyst will have a longevity advantage regarding pore blockage deactivation.
• the catalyst preferably have noncrystalline silica-aluminas as porous material, have zeolites selected from zeoliteY, ZSM-5, zeolite Beta, MCM-56 and/or MCM-22, and have metals selected from group VIII and/or VIB in the periodic table. It is even preferable that, given a significant, heteroatomic poison content in the feed, some metals of group VIB and VIII are in the sulfided or oxysulfided form.
• One conventional sulfiding method which is well known to the skilled person consists of heating in the presence of hydrogen sulfide (pure or, for example, in a stream of a hydrogen/hydrogen sulfide mixture or a nitrogen/hydrogen sulfide mixture) to a temperature in the range 15O 0 C to 800 0 C, preferably in the range 25O 0 C to 600 0 C, generally in a traversed bed reaction zone.
• the hydrocracking process conditions e.g. temperature, pressure, hydrogen circulation rate, and space velocity
• the temperature is generally over 200 0 C, and usually in the range 25O 0 C to 48O 0 C.
• the pressure is over 0.1 MPa and usually over 1 MPa.
• the quantity of hydrogen is a minimum of 50 liters of hydrogen per liter of feed and usually in the range 80 to 5000 liters of hydrogen per liter of feed.
• the hourly space velocity is generally in the range 0.1 to 20 volumes of feed per volume of catalyst per hour.
• Hydrocracking products can include, for example, middle distillates with a boiling range of from about 15O 0 C to about 400 0 C, diesel fuel and lube base oil.
• hydroisomerization catalyst e.g. for upgrading a Fischer-ray
• Tropsch product (disclosed in US 6,570,047), comprises one or more Group VIII catalytic metal components supported on an acidic metal oxide support to give the catalyst both a hydrogenation function and an acid function for hydroisomerizing the hydrocarbons.
• Hydroisomerization conditions typically include a temperature of from about 150 0 C to about 500 0 C, a pressure from about 1 bar to about 240 bars, and a LHSV from about 0.1 to about 20.
• the catalytic metal component may comprise a Group VIII noble metal, such as Pt or Pd, and preferably Pt.
• the catalytic metal component comprise one or more less expensive, non-noble Group VIII metals, such as Co, Ni and Fe, which will typically also include a Group VIB metal (e.g., Mo or W) oxide promoter.
• the catalyst may also have a Group IB metal, such as copper, as a hydrogenolysis suppressant. Phosphorus may also be included to enhance the solubility of the metals and to aid in overall stability.
• the cracking and hydrogenating activity of the catalyst is determined by its specific composition, as is known.
• the present invention provides a preferred catalyst composition having catalytically active metal, e.g. cobalt and molybdenum, the oxide support or carrier including silica, alumina, silica-alumina, silica-alumina-phosphates, titania, zirconia, vanadia, and other Group II, FV 5 V or VI oxides, as well as acidic zeolite, such as zeolite Y (including USY), zeolite Beta and ZSM-5.
• the oxide support or carrier including silica, alumina, silica-alumina, silica-alumina-phosphates, titania, zirconia, vanadia, and other Group II, FV 5 V or VI oxides
• acidic zeolite such as zeolite Y (including USY), zeolite Beta and ZSM-5.
• This example demonstrates the incorporation of zeolite Beta into silica TUD-I .
• 4.6 parts calcined zeolite Beta with a SiO 2 ZAl 2 O 3 molar ratio of 75 and an average particle size of 0.2 ⁇ m were suspended in 51 parts water and stirred for 30 minutes. Then 23 parts triethanolamine were added to the suspension while stirring. After continuous stirring for another 30 minutes, 63.5 parts tetraethyl orthosilicate ("TEOS”) were added. After stirring again for another 30 minutes, 12.6 parts tetraethylammonium hydroxide aqueous solution (35%) were added drop-wise to the mixture. After stirring for about 2 hours, the mixture formed a thick, nonflowing gel.
• TEOS tetraethyl orthosilicate
• This gel was aged at room temperature under static conditions for 24 hours. Next, the gel was dried in air at 100°C for 24 hours. The dried gel was transferred into autoclaves and hydro thermally treated at 180°C for 4 hours. Finally, it was calcined at 600°C for 10 hours in air with a heating rate of l°C/min.
• the XRD pattern of the resultant product, designated as Sample 1 is shown in FIG. 1, which clearly shows two characteristic peaks of zeolite beta. There is about 20wt % zeolite beta in the final composite. Nitrogen adsorption revealed its surface area of about 730 m 2 /g, pore volume of about 1.08 cm 3 /g. The mesopore size distribution of Sample 1 is shown in FIG. 2.
• EXAMPLE 2 [040] The zeolite Beta used here is the same as that in Example 1. First, 12.2 parts zeolite Beta were suspended in 51 parts water and stirred for 30 minutes. Then 23 parts triethanolamine were added to the suspension with stirring. After continuous stirring for another 30 minutes, 63.5 parts TEOS were added. After stirring again for another 30 minutes, 12.7 parts tetraethylammonium hydroxide aqueous solution (35%) were added drop-wise to the mixture. The same procedure was followed as described in Example 1. After calcination, its XRD pattern (corresponding to Sample 2) is shown in FIG. 1, which clearly shows two characteristic peaks of zeolite Beta.
• This example illustrates incorporation of MCM-22.
• 2.4 parts as- synthesized zeolite MCM-22 with a SiO 2 AAl 2 O 3 molar ratio of 6.4 and an average particle size of 2,5 ⁇ m were suspended in 10.5 parts water and stirred for 30 minutes. Then 9.2 parts triethanolamine were added to the above suspension under stirring. After continuous stirring for another 30 minutes, 12.7 parts TEOS were added. After stirring again for another 30 minutes, 2.52 parts tetraethylammonium hydroxide aqueous solution (35%) were added drop-wise to the mixture. After stirring for about 2 hours, the mixture formed a thick, nonflowing gel. This gel was aged at room temperature under static conditions for 24 hours.
• the XRD pattern of the resultant product designated as Sample 4 and shown as the uppermost plot in FIG. 3, clearly shows characteristic peaks of zeolite MCM-22 (middle plot) and mesoporous material (lowest plot). There is about 40wt % zeolite MCM-22 in Sample 4, and elemental analysis confirmed this number based on aluminum content, assuming no aluminum from siliceous mesoporous material.
• Nitrogen adsorption revealed its surface area of about 686 m 2 /g, pore volume of about 0.82 cm 3 /g. Its mesopore size distribution centered around 10 nm in FIG. 4. Argon adsorption showed micropores centered at 0.5 nm.
• the XRD pattern of Sample 5 is shown as the upper plot in FIG. 5, which clearly shows two characteristic peaks of zeolite Y and mesostructure material.
• the lower plot depicts an XRD pattern of zeolite Y.
• Nitrogen adsorption revealed its surface area of about 694 m 2 /g, pore volume of about 1.1 cmVg.
• This example demonstrates catalyst extrusion using alumina as binder.
• the proton form (i.e. H + ) of the Sample 5 was obtained by ion exchange, mixing one part of Composite 5 with ten parts of 1 N ammonium nitrate solution at 6O 0 C for 6 hours while stirring.
• the solid material was filtered, washed and dried at 11O 0 C to get a white powder. After a second ion exchange, the solid material was calcined at 55O 0 C for 6 hours in air.
• This example demonstrates the preparation of silica precursor, silica- triethanolamine complexes.
• 250 parts of silica gel, 697 parts of triethanolamine (TEA) and 286 parts of ethylene glycol (EG) were loaded into a flask equipped with a condenser. After the contents of the flask were mixed well with a mechanical stirrer, the mixture was heated up to 200-210 0 C while stirring. This setup removed most of water generated during reaction together with a small portion of EG from the top of the condenser. Meanwhile, most of the EG and TEA remained in the reaction mixture. After about six hours, heating was stopped; and the reaction mixture was collected after cooling down to 55°C. This reaction mixture was slightly brown, denoted as silica- triethanolamine complexes.
• This example demonstrates the zeolite/TUD-1 preparation using silica- triethanolamine complexes as a silica source.
• the final zeolite/TUD-1 composite contains 45 wt% of zeolite. Nitrogen gas adsorption showed that it has a BET surface area of about 560 m 2 /g, total pore volume of 1.2 cnrVg and average mesopore size of about 5.7 nm.
• Example 6 This is an example showing metals incorporation into the catalyst.
• the extrudate obtained in Example 6 is further functionalized by impregnation with Ni and W.
• Five (5) parts of nickel nitrate aqueous solution (14 wt % Ni) is mixed with 8.4 parts of ammonium metatungstate solution (39.8 wt % W) under stirring.
• the mixture is then diluted with 9 parts of water under stirring.
• 12.5 Parts of extrudate obtained in Example 6 are impregnated with the above Ni/W solution, dried at 118 0 C for 2 hours and calcined at 500 0 C for 2 hours.
• the resulting modified extrudates contains 4.0 wt % of Ni and 18.7 wt % W.
• zeolite/TUD-1 0.3wt% platinum/zeolite-TUD-1 by incipient wetness.
• the zeolite/TUD-1 obtained in Example 2 is impregnated with an aqueous solution comprising 0.42 parts of tetraammine platinum nitrate, 12.5 parts of aqueous solution of tetraammine palladium nitrate (5% Pd) and 43 parts of water. Impregnated zeolite/TUD-1 is aged at room temperature for 5 hours before dried at 90°C for 2 hours. The dried material is finally calcined in air at 350 0 C for 4 hours with a heating rate of l°C/min.
• Noble metal dispersion is measured using CO chemisorption; the powder is then reduced in a hydrogen stream at 100 0 C for 1 hr followed by heating to 35O 0 C at 5°C/min and is maintained at this temperature for 2 hr. A dispersion of 51% is measured for the metal assuming a Pt:CO stoichiometry of 1.
• EXAMPLE Il This example demonstrates catalyst preparation of 0.90wt% iridium/zeolite/TUD-1 by incipient wetness. 0.134 Parts of iridium (III) chloride are dissolved in 5.3 parts of deionized water. This solution is added to 8 parts of zeolite/TUD-1 obtained in Example 4 with mixing. The powder was dried at 25 0 C. [054] For dispersion measurement using CO chemisorption, the powder is then reduced in a hydrogen stream at 100 0 C for 1 hr followed by heating to 35O 0 C at 5°C/min and is maintained at this temperature for 2 hr. CO chemisorption showed a 78% dispersion for the metal assuming an Ir: CO stoichiometry of 1.
• Example 9 This example illustrates the use of the catalyst obtained in Example 9 as a hydrocracking catalyst, which is evaluated for middle distillates selectivity in hydrocracking.
• the evaluation is carried out in a flow reactor with presulfided form (in a conventional way) using a hydrotreated heavy vacuum gas oil as a feedstock. It is operated at LHSV of 1.5 kg /liter hour, total pressure of 140 bar (partial pressure OfH 2 S of 5.5 bar, and a partial pressure of ammonia of 0.075 bar) and a gas/feed ratio of 1500 NL/kg.
• the properties of feedstock are shown in Table 1.
• the composite zeolite/TUD-1 obtained in Example 6 is impregnated with tetraammine platinum nitrate as described in Example 9, and the final catalyst has about 0.6 wt% Pt.
• a typical, deoiled wax feed has the composition shown in Table 2 below. This deoiled wax is obtained from the solvent (MEK) dewaxing of a 300 SUS (65 cst) neutral oil obtained from an Arab Light crude.
• the total liquid product from the hydrocracking step is further upgraded and hydroisomerized by processing over a low acidity Pt/zeolite Beta/TUD-1 catalyst obtained to effectively hydroisomerize and convert most of the unconverted wax to very high quality, very high VI lube oil containing essentially all isoparaffms, primarily singly branched.
• the waxy total liquid product is processed over the catalyst at 400 psia H 2 partial pressure, 2500 SCFfB hydrogen, and 0.5 LHSV over a range of conversion levels.
• the total liquid product is then distilled to a nominal 700° F+ cut- point.
• the waxy bottoms are then solvent dewaxed to produce lube oils having improved lube yield.
• Table 3 contains results of these experiments using zeolite containing hydrocracking catalyst.

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