WO2018192520A1 - Catalyseur optimisé d'hydrocraquage de diesel et son procédé de préparation - Google Patents

Catalyseur optimisé d'hydrocraquage de diesel et son procédé de préparation Download PDF

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Publication number
WO2018192520A1
WO2018192520A1 PCT/CN2018/083510 CN2018083510W WO2018192520A1 WO 2018192520 A1 WO2018192520 A1 WO 2018192520A1 CN 2018083510 W CN2018083510 W CN 2018083510W WO 2018192520 A1 WO2018192520 A1 WO 2018192520A1
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molecular sieve
modified
hydrocracking catalyst
aluminum
preparing
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Chinese (zh)
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明卫星
石友良
许莉
杨伟光
赖波
王春锋
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Wuhan Kaidi Engineering Technology Research Institute Co Ltd
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Wuhan Kaidi Engineering Technology Research Institute Co Ltd
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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
    • B01J35/615—100-500 m2/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
    • 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
    • B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
    • B01J29/14—Iron group metals or copper
    • B01J29/146—Y-type faujasite
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    • B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
    • B01J29/16—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • B01J29/42—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing iron group metals, noble metals or copper
    • B01J29/46—Iron group metals or copper
    • 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
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • B01J29/48—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing arsenic, antimony, bismuth, vanadium, niobium tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • 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
    • B01J29/06—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
    • B01J29/7284—TON-type, e.g. Theta-1, ISI-1, KZ-2, NU-10 or ZSM-22
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J29/00—Catalysts comprising molecular sieves
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    • 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
    • B01J29/76—Iron group metals or copper
    • B01J29/7615—Zeolite Beta
    • 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
    • B01J29/06—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
    • B01J29/76—Iron group metals or copper
    • B01J29/7684—TON-type, e.g. Theta-1, ISI-1, KZ-2, NU-10 or ZSM-22
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—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
    • B01J29/76—Iron group metals or copper
    • B01J29/7692—MTT-type, e.g. ZSM-23, KZ-1, ISI-4 or EU-13
    • 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
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J29/7815—Zeolite Beta
    • 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
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J29/7884—TON-type, e.g. Theta-1, ISI-1, KZ-2, NU-10 or ZSM-22
    • 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
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J29/7892—MTT-type, e.g. ZSM-23, KZ-1, ISI-4 or EU-13
    • 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
    • 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
    • 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
    • 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
    • C10G47/12—Inorganic carriers
    • C10G47/16—Crystalline alumino-silicate carriers
    • C10G47/20—Crystalline alumino-silicate carriers the catalyst containing other metals or 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
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1037—Hydrocarbon fractions
    • 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
    • C10G2300/70—Catalyst aspects

Definitions

  • the invention relates to a catalyst, in particular to an optimized diesel hydrocracking catalyst and a preparation method thereof.
  • Hydrocracking is a very important technology for the efficient conversion of heavy oil and clean oil production in the refining industry. It can process heavy crude oil with high sulfur and high metal. It has wide source of raw materials, great production flexibility, good product quality and middle distillate. High oil yield. Hydrocracking technology can directly produce low aromatics, low sulfur and low nitrogen high quality middle distillate products from reduced pressure diesel (VGO), which can meet increasingly stringent environmental requirements, and catalysts play a central role in hydrocracking reactions. The key to hydrocracking technology is the development and improvement of catalysts.
  • the conventional preparation methods of the hydrocracking catalyst mainly include a dipping method, a coprecipitation method and a kneading method.
  • the preparation process of the kneading method is the simplest, and the requirements for the process and the catalyst dosing are not high, but the preparation process is relatively extensive, the catalyst The dispersibility of each component is not good, and some metal hydrogenation active centers are covered, which can not exert its activity better. It is usually used for catalysts with less hydrogenation performance; the preparation process of coprecipitation method is the most complicated.
  • the impregnation method is the most widely used method for preparing hydrocracking catalysts. Firstly, the carrier which meets the performance requirements of the catalyst, such as the shape, mechanical strength, specific surface and acidity of the carrier, is prepared, and then the metal group is supported by a saturated or supersaturated impregnation method. The metal component is enriched in the catalyst to make the catalyst have higher mechanical strength and fully exert its Hydrogen performance.
  • the hydrocracking catalyst prepared by the prior method has simple mechanical mixing between the components, and the components in the catalyst are easily agglomerated into secondary particles, so that the dispersibility of the active component is poor, and the prepared catalyst is difficult to prepare.
  • the best performance is achieved, and there are also problems with complicated preparation processes and high costs.
  • CN98114489.6 discloses a hydrocracking catalyst, amorphous silico-alumina and Y-type molecular sieves as cracking components, and Group VIB and Group VIII metal oxides as hydrogenation components, using a series of hydrocracking.
  • the middle distillate oil is produced, and the catalyst has good nitrogen resistance, but the preparation method is complicated and the preparation cost is high.
  • CN1393521A discloses a medium oil type hydrocracking catalyst and a preparation method thereof, wherein the carrier used for the catalyst is amorphous silicon aluminum, aluminum oxide and Y and ⁇ composite molecular sieve, wherein the composite molecular sieve is after the ⁇ molecular sieve raw powder is burned to the template.
  • the carrier used for the catalyst is amorphous silicon aluminum, aluminum oxide and Y and ⁇ composite molecular sieve, wherein the composite molecular sieve is after the ⁇ molecular sieve raw powder is burned to the template.
  • CN1351121A discloses a hydrocracking catalyst containing modified ⁇ molecular sieve and amorphous silicon aluminum and a preparation method thereof, wherein the modified ⁇ molecular sieve directly exchanges the synthesized molecular sieve slurry with ammonium, and then roasts deammonium, acid
  • the modified ⁇ molecular sieve is obtained by treatment and hydrothermal treatment. Since a large amount of non-skeletal aluminum is retained in the pores of the molecular sieve, the acidity and diffusion property of the modified molecular sieve are affected, which ultimately affects the yield and properties of the diesel product.
  • the object of the present invention is to provide an optimized diesel hydrocracking catalyst and a preparation method thereof, which can significantly reduce the freezing point of the diesel fraction and increase the cetane number of the diesel fuel under the premise of ensuring the diesel oil yield.
  • the technical scheme adopted by the present invention is: an optimized diesel hydrocracking catalyst comprising the following components and their weight percentages: 1 to 25% of modified molecular sieves, 10 to 65% ⁇ -Al 2 O 3 , 15 to 70% amorphous silicon aluminum, 9 to 40% binder and 10 to 35% active metal oxide; the catalyst has a specific surface area of 200 to 400 m 2 /g, The total pore volume is from 0.30 to 0.65 cm 3 /g.
  • the catalyst raw material comprises the following components and their weight percentages: 3.3 to 5.4% modified molecular sieve, 21.6 to 27% ⁇ -Al 2 O 3 , 29.7 to 35% amorphous silicon aluminum, 15 to 25 % binder and 20-28% active metal oxide; the catalyst has a specific surface area of 341-375 m 2 /g, and a total pore volume of 0.49-0.57 cm 3 /g; the catalyst is columnar and the length is 3 to 8 mm.
  • the modified molecular sieve is one of a modified ⁇ molecular sieve, a modified Y molecular sieve, a modified MOR molecular sieve, a modified ZSM-5 molecular sieve, a modified ZSM-22 molecular sieve, and a modified ZSM-23 molecular sieve or Several.
  • the active metal in the active metal oxide is one or more of W, Mo, Ni, and Co.
  • the modified ⁇ molecular sieve has a specific surface area of 450 to 750 m 2 /g and a total pore volume of 0.3 to 0.5 cm 3 /g.
  • the modified Y-type molecular sieve has a specific surface area of 750 to 860 m 2 /g and a total pore volume of 0.35 to 0.55 cm 3 /g.
  • the modified MOR molecular sieve has a specific surface area of 300 to 560 m 2 /g and a total pore volume of 0.3 to 0.45 cm 3 /g.
  • a method for preparing the above optimized diesel hydrocracking catalyst comprises the following steps:
  • step 2) preparing modified molecular sieve and ⁇ -Al 2 O 3 composite material: adding the modified molecular sieve obtained in step 1) to a mixed solution of aluminum salt and alkali for precipitation, fully precipitating, and then taking the slurry to be sequentially dried and calcined, and then changed.
  • Molecular sieve and ⁇ -Al 2 O 3 composite
  • the ammonium exchange condition is: the temperature is 60 to 90 ° C, and the ammonium salt used is 0.4 to 0.6 mol/L of ammonium chloride or ammonium nitrate.
  • the hydrothermal treatment conditions are: a temperature of 630 to 750 ° C, a treatment time of 1 to 4 hours, and a gauge pressure of 0.05 to 0.4 MPa.
  • the aluminum salt treatment condition is: the aluminum salt solution used has an Al 3+ concentration of 0.5 to 1.5 mol/L, and the mass ratio of the aluminum salt to the modified molecular sieve is 4 to 30:1.
  • the temperature is 70 to 100 ° C, and the treatment time is 1 to 5 hours.
  • the modified molecular sieve is a modified ⁇ molecular sieve
  • the crystallization temperature is 135 to 145 ° C
  • the calcination de-template treatment conditions are: after the temperature rise rate is 2 ° C / min, the temperature is raised to 540-560 ° C, Roasted for 7 to 9 hours.
  • the aluminum source is one or more of pseudoboehmite, aluminum sulfate and sodium metaaluminate
  • the silicon source is one of white carbon black, silica sol and water glass. Or several.
  • the aluminum salt is one or more of aluminum sulfate, aluminum nitrate and aluminum chloride;
  • the base is one or more of ammonium oxalate, ammonia water, sodium hydroxide and potassium hydroxide.
  • the control temperature is 50-70 ° C
  • the pH is 3-7
  • the drying temperature is 110-130 ° C
  • the baking temperature is 300-600 ° C
  • the baking time is 2 ⁇ . 4 hours.
  • the drying temperature is 100 to 120 ° C
  • the time is 18 to 22 hours
  • the activation temperature is 450 to 600 ° C
  • the activation time is 4 to 6 hours.
  • the present invention has the following advantages:
  • a modified molecular sieve is added to the aluminum salt solution for preparing ⁇ -Al 2 O 3 , and after adding a precipitating agent, the precipitate of aluminum hydroxide is deposited and the modified molecular sieve is wrapped, and the precipitate is dried, After calcination, the cracking active component can be uniformly dispersed into the alumina.
  • the catalyst of the invention has a more uniform acidity center, suitable acidity, large specific surface area and pore volume, and alumina in the catalyst. Molecular sieves are more closely contacted, which facilitates the rapid transfer of reactants and product molecules between the acid center and the cracking center, so that there is better synergy between the cracking and hydrogenation active components.
  • the hydrocracking catalyst of the invention has suitable cracking action and good isomerization effect on long-chain alkyl groups of long-chain alkanes, aromatic hydrocarbons and naphthenes, good middle distillate selectivity and high catalytic activity. Under the premise of ensuring diesel oil yield, the freezing point of diesel fraction is obviously reduced, and the cetane number of diesel is improved.
  • the invention optimizes the matching between the hydrogenation function and the acidic function, forms a combination of strong hydrogenation function and medium acid or weak acid function, and the positive carbon ion can be more hydrogenated and saturated at the hydrogenation active center.
  • the direction of the formation proceeds, reducing the secondary cracking of the cracked product.
  • the specific surface area and pore volume are measured by low temperature liquid nitrogen physical adsorption, the molar ratio of silicon to aluminum is determined by chemical method, and the framework silica aluminum is determined by NMR; the amount of infrared acid, B acid and L acid are adsorbed by pyridine.
  • the spectroscopy method, the sodium content is determined by plasma emission spectroscopy, and the relative crystallinity of the molecular sieve is determined by the XRD method.
  • modified ⁇ molecular sieve by hydrothermal synthesis method (specific surface area: 450-750 m 2 /g, total pore volume: 0.3-0.5 cm 3 /g), modified Y-type molecular sieve (specific surface area of 750-860 m 2 / g, total pore volume is 0.35-0.55 cm 3 /g), modified MOR molecular sieve (specific surface area is 300-560 m 2 /g, total pore volume is 0.3-0.45 cm 3 /g), modified ZSM-5 molecular sieve, One or more of the modified ZSM-22 molecular sieve and the modified ZSM-23 molecular sieve, according to the molecular sieve compounding molar ratio, the template or the guiding agent, the aluminum salt, and the water are mixed and stirred to a clear solution (where the modified Y The molecular sieve needs to adjust the alkalinity of the mixed solution with hydrochloric acid, and then the silicon source is added to the obtained clear solution under stirring,
  • the catalyst material the modified molecular sieve and the alumina composite material, the amorphous silicon aluminum, the active metal oxide and the binder are mixed, compacted, formed, dried and activated to obtain a catalyst, and the rolling time is obtained.
  • the strip is extruded into a column shape, the length is 3 to 8 mm, dried at 120 ° C for 20 hours, and calcined at 450 to 600 ° C for 5 to 6 hours to obtain a catalyst.
  • the ammonium exchange was carried out twice at a concentration of 0.5 mol/L ammonium chloride solution at 80 ° C, and the liquid-solid ratio was 10:1. Further, hydrothermal treatment is carried out at a water vapor pressure of 0.15 MPa, a treatment temperature of 600 ° C, and a treatment time of 2.5 hours, followed by treatment with an aluminum salt, and the hydrothermally treated molecular sieve is placed in a flask with a reflux device and can be sealed, and added.
  • the composite material of molecular sieve and ⁇ -Al 2 O 3 was 195.5 g (dry basis 93%), amorphous silicon aluminum 238.6 g (dry basis 88%), MoO 3 90.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6wt%) 116.7g, binder 360g (dry basis 25%) were mixed, crushed in a wheel mill for 40 minutes, crushed into a squeezeable paste, extruded into strips, The shape is columnar, the length is 3-8 mm, and dried at 120 ° C for 20 hours, and calcined at 500 ° C for 5-6 hours to obtain a hydrocracking catalyst, numbered C-1, and the properties are shown in Table 2.
  • the modified molecular sieve was the same as the ⁇ modified molecular sieve in Example 1; the molecular sieve and the ⁇ -Al 2 O 3 composite were the same as in Example 1; the composite material was 195.5 g (dry basis 93%), amorphous silicon aluminum 204.5 g (dry basis) 88%), MoO 3 is 108.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6 wt%) is 163.4 g, and binder 360 g (dry basis 25%) is mixed.
  • the roller mill is rolled for 40 minutes, crushed into a squeezing paste, extruded into strips, and shaped into a column shape, having a length of 3 to 8 mm, dried at 120 ° C for 20 hours, and calcined at 500 ° C for 5 to 6 hours to obtain Hydrocracking catalyst, numbered C-2, properties are shown in Table 2.
  • the modified molecular sieve was the same as the ⁇ -modified molecular sieve in Example 1; 140 g of ammonium oxalate and 3000 ml of aluminum chloride solution (concentration: 1.5 mol/L) were weighed and mixed in a 5000 ml beaker to modify 52.6 g (dry basis 98%). Molecular sieves were added to the mixture, kept at a constant temperature of 70 ° C, and continuously added with 2 mol/L of ammonia water until the pH was 4, and evaporated at 85 ° C. The aspirated white solid was dried at 100 ° C for 3 hours and calcined at 500 ° C for 4 hours to obtain a molecular sieve.
  • the ⁇ -Al 2 O 3 composite material was 272.8 g (dry basis 93%), and the conversion rate was 72.3%.
  • the composite material of molecular sieve and ⁇ -Al 2 O 3 was 173.2 g (dry basis 93%), amorphous silicon aluminum 238.6 g (dry basis 88%), MoO 3 was 108.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6wt%) was 116.7g, binder 360g (dry basis 25%) was mixed, crushed in a wheel mill for 40 minutes, crushed into a squeezing paste, extruded
  • the molding has a columnar shape and a length of 3 to 8 mm, and is dried at 120 ° C for 20 hours and calcined at 500 ° C for 5 to 6 hours to obtain a hydrocracking catalyst, which is numbered C-3, and the properties are shown in Table 2.
  • the modified molecular sieve was the same as the ⁇ modified molecular sieve in Example 1; the composite material of molecular sieve and ⁇ -Al 2 O 3 was the same as in Example 3, and the composite material was 173.2 g (dry basis 93%) and amorphous silicon aluminum 204.5 g (dry). 88%), MoO 3 is 108.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6 wt%) is 233.4 g, and binder 360 g (dry basis 25%) is mixed.
  • the modified molecular sieve was the same as the ⁇ -modified molecular sieve of Example 1; 20.5 g of modified molecular sieve (dry basis 98%), alumina 169.8 g (dry basis 96%), amorphous silica aluminum 238.6 g ( Dry base 88%), MoO 3 is 90.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6 wt%) is 116.7 g, and binder 360 g (dry basis 25%) is mixed.
  • the modified molecular sieve was the same as the ⁇ -modified molecular sieve of Example 1; 33.4 g of modified molecular sieve (dry basis 98%), alumina 135.3 g (dry basis 96%), amorphous silica aluminum 238.6 g ( Dry base 88%), MoO 3 is 108.5 g (99.1 wt%), Ni(NO 3 ) 2 ⁇ 6H 2 O (NiO, 26.6 wt%) is 116.7 g, and binder 360 g (dry basis 25%) is mixed.
  • Example 1 The catalysts of Example 1 and Comparative Example 1 were evaluated on a fixed bed hydrogenation experimental apparatus under the following conditions: a total reaction pressure of 10 MPa, a hydrogen oil volume ratio of 1000, a volumetric space velocity of 1.0 h -1 , and a reduced pressure.
  • Distillate oil (VGO) is a feedstock oil, and the properties of the feedstock oil are shown in Table 3.
  • Catalysts C-1 and C-5 were evaluated under the same process conditions, and the evaluation results are shown in Table 4.
  • the catalyst of Example 1 had better middle distillate oil under the same process conditions.
  • Raw material oil Vacuum distillate Density (20 ° C), kg / m 3 912.3 Distillation range, °C IBP/10% 315/403 30%/50% 442/461 70%/90% 495/526 95%/EBP 532/544 Freezing point, °C 32 Nitrogen, ⁇ g/g 1568 Carbon, wt% 84.53 Hydrogen, wt% 11.72 Carbon residue, wt% 0.32 BMCI value 43

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Abstract

L'invention concerne un catalyseur optimisé d'hydrocraquage de diesel et son procédé de préparation. Les matières premières comprennent les constituants suivants en pourcentage en poids : 1 à 25 % de tamis moléculaire modifié, 10 à 65 % de γ-Al2O3, 15 à 70 % de silice-alumine amorphe, 9 à 40 % de liant et 10 à 35 % d'oxyde métallique actif. La surface spécifique du catalyseur est comprise entre 200 et 450 m2/g, et le volume poreux total est compris entre 0,30 et 0,65 cm3/g. Afin d'obtenir un support, un tamis moléculaire modifié est ajouté à une solution de sel d'aluminium inorganique utilisée pour la préparation de γ-Al2O3, et une précipitation, un séchage et une calcination sont effectués afin d'obtenir un composite de tamis moléculaire et de γ-Al2O3 ; puis les matières restantes sont mélangées avec le composite selon la proportion de matières du catalyseur, et un laminage, un formage, un séchage et une activation sont effectués afin d'obtenir le catalyseur. Le tamis moléculaire dans le support de catalyseur présente un rapport silice/alumine élevé et une surface spécifique élevée et il est dispersé de manière élevée dans le support ; ainsi, le support présente des sites acides plus uniformes et l'alumine est en contact plus étroit avec le tamis moléculaire ; par conséquent, le catalyseur peut réduire considérablement le point d'écoulement d'une fraction diesel et améliorer l'indice de cétane du diesel, garantissant en même temps un rendement de diesel élevé.
PCT/CN2018/083510 2017-04-21 2018-04-18 Catalyseur optimisé d'hydrocraquage de diesel et son procédé de préparation Ceased WO2018192520A1 (fr)

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