CN108714434B - Light oil type hydrocracking catalyst and preparation method thereof - Google Patents

Light oil type hydrocracking catalyst and preparation method thereof Download PDF

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Publication number
CN108714434B
CN108714434B CN201810565969.1A CN201810565969A CN108714434B CN 108714434 B CN108714434 B CN 108714434B CN 201810565969 A CN201810565969 A CN 201810565969A CN 108714434 B CN108714434 B CN 108714434B
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light oil
parts
catalyst
hydrocracking catalyst
compound containing
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CN108714434A (en
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范文青
刘长坤
张黎
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Sinochem Corp
Sinochem Quanzhou Petrochemical Co Ltd
Sinochem Quanzhou Energy Technology Co Ltd
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Sinochem Quanzhou Petrochemical Co Ltd
Sinochem Quanzhou Energy Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/1608—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes the ligands containing silicon
    • 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
    • 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

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention discloses a light oil type hydrocracking catalyst and a preparation method thereof, wherein the hydrocracking catalyst is prepared from a compound containing VIII group metal elements, a compound containing VIB group metal elements, pseudo-boehmite, a molecular sieve and alkyl substituted siloxane containing modified groups. The obtained light oil type hydrocracking catalyst greatly improves the selectivity of light oil on the basis of improving the activity of the catalyst, the yield of liquid products is improved, the generation of gaseous hydrocarbon is reduced, and the output benefit of a light oil type hydrocracking device can be obviously improved.

Description

Light oil type hydrocracking catalyst and preparation method thereof
Technical Field
The invention relates to a light oil type hydrocracking catalyst and a preparation method thereof.
Background
The hydrocracking process is an oil refining process that converts high boiling feedstocks into low boiling naphtha and diesel fractions. Compared with catalytic cracking, the hydrocracking process has high raw material adaptability, high diesel fraction yield and good quality, but the octane number of naphtha is relatively low. With the increasing demand of society for clean transportation fuel oil, the hydrocracking process becomes one of the core processes of modern refineries.
The hydrocracking catalyst is the core of the overall hydrocracking process, which typically includes a bifunctional center: the first one is an acid center provided by a carrier, which basically determines the activity of the catalyst, and during the development of hydrocracking catalysts, materials such as halogenated (chlorine or fluorine) alumina, amorphous silica-alumina and molecular sieves have been used as acid components, and since the last 70 th century, with the development of molecular sieve preparation technology, silica-alumina molecular sieves gradually become the main component of the acid center in hydrocracking catalysts due to their definite structures and adjustable acidity. The second is a metal center which plays a hydrogenation/dehydrogenation role in the reaction process, provides a reaction raw material for the acid center, and timely saturates the acid center product to prevent deep cracking. The metal center is generally composed of a group VIB metal or a group VIB and VIIIB binary metal system, providing true hydrogenation/dehydrogenation activity in the form of sulfides. The close association of the acid center with the hydrogenation/dehydrogenation center and the coordination of the two is the key to the successful operation of the hydrocracking catalyst.
In order to meet the increasing demand of society for clean transportation fuel oil, high boiling point raw materials are fully utilized in the hydrocracking process to produce more naphtha and diesel oil products, and the production of low-value gaseous products (C1-C4) is reduced. Meanwhile, in order to reduce the operating cost of the production, the industrial production is expected to use a catalyst with higher activity to reduce the reaction temperature. Specifically, when the catalyst is designed, the acid center performance and the metal center performance of the catalyst are expected to be synchronously improved; the performance of the acid sites can be enhanced by increasing the acid strength of the acidic material (e.g., molecular sieve) or its amount used; the metal core performance is limited by the effective specific surface area provided by the carrier and the characteristics of the metal itself, and cannot be improved simply by increasing the amount used. Therefore, how to improve the performance of the metal center has been a hot spot of research in this field.
The surface of inorganic oxides, such as alumina, has a large number of hydroxyl groups, and the types of hydroxyl groups can be classified into five types depending on the coordination environment of aluminum atoms (reference: Catal Rev. Sci. Eng. 17(1), 31-70, 1978). The formation of Al-O-M chemical bonds by condensation of these hydroxyl groups is the key reason for the stronger interaction between the group VIB metal and the alumina support. The invention carries out surface modification on a hydrocracking catalyst carrier consisting of inorganic oxides, replaces strong hydroxyl on the surface of the hydrocracking catalyst carrier with other functional groups completely or partially, so that weak interaction is formed between the hydrocracking catalyst carrier and VI B metal, and even the strong hydroxyl directly participates in the vulcanization process of the VI B metal oxide, so that the interaction between the transition metal and the surface of the inorganic carrier is essentially changed, the full pre-vulcanization of the transition metal oxide is facilitated, the optimal hydrogenation/dehydrogenation performance is exerted in a hydrocracking reaction, particularly, the hydrocracking catalyst carrier is beneficial to the quick saturation of olefin intermediates, the deep cracking is reduced, the generation of C1-C4 gaseous hydrocarbons is reduced, and the yield of liquid products is improved.
Disclosure of Invention
In order to solve the problems of low light oil selectivity and low liquid product yield of the existing hydrocracking catalyst, the invention provides a novel light oil type hydrocracking catalyst and a preparation method thereof, and the catalyst has the characteristics of high activity, high light oil selectivity and high liquid yield.
In order to achieve the purpose, the invention adopts the following technical scheme:
a light oil type hydrocracking catalyst is prepared from the following raw materials:
(a) a compound containing a group VIII metal element;
(b) a compound containing a group VIB metal element;
(c) pseudo-boehmite;
(d) a molecular sieve;
(e) an alkyl-substituted siloxane containing a modifying group;
in the technical scheme, the amount of the raw material (a) is preferably 0.1-35 parts by weight, and more preferably 15-25 parts by weight; the preferred dosage of the raw material (b) is 0.1-15 parts, and the more preferred dosage is 4-8 parts; the amount of the raw material (c) is preferably 1-95 parts, and more preferably 20-60 parts; the preferred dosage of the raw material (d) is 1-80 parts, and the more preferred dosage is 10-40 parts; the amount of the raw material (e) is preferably 0.1 to 20 parts, more preferably 1 to 10 parts.
In the above technical solution, the group VIII metal element is selected from at least one of Co and Ni;
the VIB group metal element is at least one of Mo and W;
the structural formula of the alkyl substituted siloxane containing the modified group is as follows: X-R1-Si(OR2)3Wherein R is1And R2Independently selected from alkyl, aryl or substituted aryl, X is-H, -F, -NH2-SH, -CHO, -OH or-C (O) NH2Preferably, -SH.
The molecular sieve is a hydrogen type molecular sieve, specifically is at least one of a USY molecular sieve, a Beta molecular sieve, a ZSM-5 molecular sieve and an SSZ-32 molecular sieve, preferably is the USY molecular sieve, and has a specific surface area of 400-1000 m2Preferably 600 to 800 m/g2(ii)/g; the total pore volume is 0.45-1.00 cm3Preferably 0.50 to 0.80 ml/g; the mesoporous volume is 0.10-0.50 mL/g, preferably 0.20-0.40 mL/g; the Si/Al molar ratio is 2-30, and preferably 3-10; the unit cell size is 24.30 to 24.60
Figure DEST_PATH_IMAGE002
Preferably 24.40 to 24.55
Figure 190396DEST_PATH_IMAGE002
。
The preparation method of the light oil type hydrocracking catalyst comprises the following steps:
(1) uniformly mixing pseudo-boehmite and a molecular sieve, adding an acid solution, fully kneading and molding, drying and roasting to obtain a catalyst carrier;
(2) reacting alkyl substituted siloxane containing a modified group with the catalyst carrier obtained in the step (1), filtering and washing, and drying in vacuum to obtain a modified catalyst carrier;
(3) and (3) dispersing a compound containing VIB group metal elements and a compound containing VIII group metal elements in a solvent, impregnating the modified catalyst carrier obtained in the step (2), and then drying and roasting to obtain the light oil type hydrocracking catalyst.
In the above technical scheme, the concentration of the acid solution in the step (1) is 0.5wt% to 5wt%, preferably 1wt% to 3wt%, and the acid used may be inorganic acid such as sulfuric acid, hydrochloric acid, nitric acid, and the like, or organic acid such as formic acid, acetic acid, citric acid, and the like, preferably nitric acid.
The diameter of the extrudate kneaded and molded in the step (1) is 1.5-3.5 mm, the length of the extrudate is 3-12 mm, and the cross section of the extrudate is circular or clover-shaped.
The drying temperature in the step (1) is 80-200 ℃, and the drying time is 2-24 hours.
The roasting temperature in the step (1) is 400-650 ℃, and the roasting time is 2-10 h. Roasting the pseudo-boehmite at 500 ℃ for 4 h to obtain alumina with the specific surface area of 150-400 m2Preferably 200 to 320 m/g2(ii)/g; the pore volume is 0.2-0.8 cm3Preferably 0.40 to 0.65 cm/g3(ii)/g; the content of Na element is less than or equal to 0.1 percent, preferably less than or equal to 0.05 percent in percentage by weight.
The reaction conditions of the modified group-containing alkyl-substituted siloxane with the catalyst support in step (2) are not particularly limited and may be appropriately selected by those skilled in the art.
The temperature of vacuum drying in the step (2) is 60-150 ℃, and the time is 2-36 h.
The group VIB metal element-containing compound and the group VIII metal element-containing compound in step (3) are not particularly limited as long as the group VIB metal element, the group VIII metal element, or an oxide thereof can be supported on the modified catalyst support, and may be appropriately selected by those skilled in the art. The solvent used is also not particularly limited as long as impregnation loading can be achieved, and may be a single solvent, a mixed solvent, a solvent that is directly dissolved, or dissolved by adjusting pH, or a solvent that forms a colloid or achieves dissolution by adjusting pH.
The drying temperature in the step (3) is 80-200 ℃, and the drying time is 2-24 hours.
The reaction conditions for hydrocracking the VGO or the hydrocracking circulating oil by adopting the light oil type hydrocracking catalyst are as follows: in the presence of hydrogen, the reaction pressure is 12-18 MPa, the reaction temperature is 300-420 ℃, the volume ratio of hydrogen to oil is 450-1500, and the liquid hourly space velocity is 0.5-8.0 h-1。
Compared with the existing hydrocracking catalyst, the light oil type hydrocracking catalyst prepared by adopting the modified carrier provided by the invention greatly improves the light oil selectivity on the basis of improving the catalyst activity, the yield of liquid products is improved, the generation of gaseous hydrocarbon is reduced, and the output benefit can be obviously improved.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Divide USY intoThe sub-sieve powder and the catalyst powder can provide enough alumina (Al) in the final catalyst2O3) The pseudo-boehmite powder is evenly mixed, then 1.5wt% of nitric acid solution is added, after full kneading, the mixture is extruded into cylindrical particles with the length of 3-10 mm and the diameter of 2 mm, the cylindrical particles are dried for 12 hours at the temperature of 120 ℃, and then the cylindrical particles are roasted for 8 hours at the temperature of 550 ℃, so that the catalyst carrier S-0 is obtained, wherein Al is contained in the particles2O3The weight ratio of the USY molecular sieve is 60: 40.
Example 2
(1) 3-mercaptopropyltriethoxysilane which can provide enough modifying groups in the final catalyst is weighed and added into an ethanol solution with the mass fraction of 95%, and stirred for 30 minutes at room temperature to be fully dissolved. Then adding the carrier S-0 obtained in the example 1 into the solution, standing at room temperature for 12 hours, heating to 80 ℃, reacting for 4 hours, then filtering, washing with absolute ethyl alcohol, and vacuum drying at 70 ℃ for 24 hours to obtain the modified catalyst carrier S-1.
(2) Nickel nitrate (Ni (NO) that will provide sufficient NiO in the final catalyst3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for dipping the modified catalyst carrier S-1 obtained in the step (1), and then the modified catalyst carrier S-1 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-1. In parts by weight, the NiO in the catalyst is WO3The ratio of the modified carrier S-1 is 5:20: 75.
Example 3
(1) 2-mercaptoethyltriethoxysilane which provides sufficient modifying groups in the final catalyst is weighed out and added to a 95% by weight ethanol solution and stirred at room temperature for 30 minutes to dissolve it sufficiently. Then adding the carrier S-0 obtained in the example 1 into the solution, standing at room temperature for 12 hours, heating to 80 ℃, reacting for 4 hours, then filtering, washing with absolute ethyl alcohol, and vacuum drying at 70 ℃ for 24 hours to obtain the modified catalyst carrier S-2.
(3) Nickel nitrate (Ni (NO) that will provide sufficient NiO in the final catalyst3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for dipping the modified catalyst carrier S-2 obtained in the step (1), and then the modified catalyst carrier S-2 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-2. In parts by weight, the NiO in the catalyst is WO3The ratio of the modified carrier S-2 is 5:20: 75.
Example 4
(1) 3-mercaptopropyltrimethoxysilane which provided enough modifying groups in the final catalyst was weighed and added to a 95% ethanol solution by mass and stirred at room temperature for 30 minutes to be sufficiently dissolved. Then adding the carrier S-0 obtained in the example 1 into the solution, standing at room temperature for 12 hours, heating to 80 ℃, reacting for 4 hours, then filtering, washing with absolute ethyl alcohol, and vacuum drying at 70 ℃ for 24 hours to obtain the modified catalyst carrier S-3.
(2) Nickel nitrate (Ni (NO) that will provide sufficient NiO in the final catalyst3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for dipping the modified catalyst carrier S-3 obtained in the step (1), and then the modified catalyst carrier S-3 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-3. In parts by weight, the NiO in the catalyst is WO3The ratio of the modified carrier S-3 is 5:20: 75.
Example 5
(1) The methyltriethoxysilane which provided enough modifying groups in the final catalyst was weighed and added to a 95% by weight ethanol solution and stirred at room temperature for 30 minutes to dissolve it sufficiently. Then adding the carrier S-0 obtained in the example 1 into the solution, standing at room temperature for 15 hours, heating to 80 ℃, reacting for 6 hours, then filtering, washing with absolute ethyl alcohol, and vacuum drying at 70 ℃ for 24 hours to obtain the modified catalyst carrier S-4.
(2) Will be able to provide foot in the final catalystNiO-rich nickel nitrate (Ni (NO)3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for dipping the modified catalyst carrier S-4 obtained in the step (1), and then the modified catalyst carrier S-4 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-4. In parts by weight, the NiO in the catalyst is WO3The ratio of the modified carrier S-4 is 5:20: 75.
Example 6
(1) 3-aminopropyltriethoxysilane which provides sufficient modifying groups in the final catalyst is weighed and added to a 95% by weight ethanol solution and stirred at room temperature for 30 minutes to allow sufficient dissolution. Then adding the carrier S-0 obtained in the example 1 into the solution, standing at room temperature for 15 hours, heating to 80 ℃, reacting for 6 hours, then filtering, washing with absolute ethyl alcohol, and vacuum drying at 70 ℃ for 24 hours to obtain the modified catalyst carrier S-5.
(2) Nickel nitrate (Ni (NO) that will provide sufficient NiO in the final catalyst3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for dipping the modified catalyst carrier S-5 obtained in the step (1), and then the modified catalyst carrier S-5 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-5. In parts by weight, the NiO in the catalyst is WO3The ratio of the modified carrier S-5 is 5:20: 75.
Comparative example 1
Nickel nitrate (Ni (NO) that will provide sufficient NiO in the final catalyst3)2·6H2O) and sufficient tungsten trioxide WO3Ammonium metatungstate ((NH)4)10W12O41·xH2O) is dispersed in deionized water and used for impregnating the carrier S-0 obtained in example 1, and then the carrier S-0 is dried for 10 hours at the temperature of 100 ℃ and roasted for 5 hours at the temperature of 520 ℃ to obtain the catalyst C-0. In parts by weightMeasuring NiO in the catalyst, WO3The ratio of the carrier S-0 is 5:20: 75.
The catalyst performance was evaluated using a single-pass, 100 mL, small hydrogenation evaluation apparatus. H of 5% by volume was used before evaluation2S and 95% H2The catalyst is presulfurized by the formed mixed gas. The raw material used for evaluating the performance of the catalyst is hydrocracking cycle oil, and the properties and reaction process conditions of the hydrocracking cycle oil are shown in tables 1 and 2 respectively. The reaction temperature was adjusted as needed to ensure that the net conversion was maintained at 80% by mass over 100 hours. The net conversion is calculated as follows:
Figure DEST_PATH_IMAGE004
。
TABLE 1 Properties of the stock oils
Figure DEST_PATH_IMAGE006
TABLE 2 reaction Process conditions
Figure DEST_PATH_IMAGE008
The results of comparing the reaction properties of the respective catalysts are shown in Table 3.
TABLE 3 evaluation results of catalysts
Figure DEST_PATH_IMAGE010
The results in Table 3 show that, compared with the catalyst C-0, the reaction temperature of the catalysts C-1, C-2 and C-3 containing the-SH modified groups is at least 3 ℃ lower than that of the catalyst C-0, the light oil selectivity of C5-175 ℃ in the product is improved by at least 2 percent, the selectivity of gaseous hydrocarbons is reduced by at least 2 percent, and the yield of liquid products with more than C5 is also improved. The results show that the carrier is modified by the organic siloxane, so that the activity and selectivity of the catalyst for preparing light oil by hydrocracking wax oil can be improved, the generation of gaseous hydrocarbon is reduced, and the yield of liquid products is improved.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (6)

1. A light oil type hydrocracking catalyst is characterized in that: the feed is prepared from the following raw materials:
(a) a compound containing a group VIII metal element;
(b) a compound containing a group VIB metal element;
(c) pseudo-boehmite;
(d) a molecular sieve;
(e) an alkyl-substituted siloxane containing a modifying group;
the VIII group metal element is at least one selected from Co and Ni;
the VIB group metal element is at least one of Mo and W;
the structural formula of the alkyl substituted siloxane containing the modified group is as follows: X-R1-Si(OR2)3Wherein R is1And R2Independently selected from alkyl, aryl or substituted aryl, X is-SH;
the raw materials are as follows by weight: 0.1-35 parts of a compound containing VIII group metal elements, 0.1-15 parts of a compound containing VIB group metal elements, 1-95 parts of pseudo-boehmite, 1-80 parts of a molecular sieve and 0.1-20 parts of alkyl substituted siloxane containing modified groups;
the molecular sieve is specifically a USY molecular sieve.
2. The light oil hydrocracking catalyst according to claim 1, characterized in that: the raw materials are as follows by weight: 15-25 parts of a compound containing VIII group metal elements, 4-8 parts of a compound containing VIB group metal elements, 20-60 parts of pseudo-boehmite, 10-40 parts of a molecular sieve and 1-10 parts of alkyl substituted siloxane containing modified groups.
3. A process for the preparation of a light oil hydrocracking catalyst as claimed in any one of claims 1 to 2, characterized in that: the method comprises the following steps:
(1) uniformly mixing pseudo-boehmite and a molecular sieve, adding an acid solution, fully kneading and molding, drying and roasting to obtain a catalyst carrier;
(2) reacting alkyl substituted siloxane containing a modified group with the catalyst carrier obtained in the step (1), filtering and washing, and drying in vacuum to obtain a modified catalyst carrier;
(3) and (3) dispersing a compound containing VIB group metal elements and a compound containing VIII group metal elements in a solvent, impregnating the modified catalyst carrier obtained in the step (2), and then drying and roasting to obtain the light oil type hydrocracking catalyst.
4. The process for producing a light oil type hydrocracking catalyst according to claim 3, wherein: the concentration of the acid solution used in the step (1) is 0.5-5 wt%, and the acid is inorganic acid or organic acid;
the diameter of the kneaded and molded extrudate is 1.5-3.5 mm, the length of the kneaded and molded extrudate is 3-12 mm, and the section of the kneaded and molded extrudate is circular or clover-shaped;
the drying temperature is 80-200 ℃, and the drying time is 2-24 hours;
the roasting temperature is 400-650 ℃, and the roasting time is 2-10 h.
5. The process for producing a light oil type hydrocracking catalyst according to claim 3, wherein: and (3) drying in vacuum in the step (2) at the temperature of 60-150 ℃ for 2-36 h.
6. The process for producing a light oil type hydrocracking catalyst according to claim 3, wherein: the drying temperature in the step (3) is 80-200 ℃, and the time is 2-24 h.
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