CN108745392B - Hydrodemetallization catalyst and preparation method thereof - Google Patents
Hydrodemetallization catalyst and preparation method thereof Download PDFInfo
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—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
- C10G45/06—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 nickel or cobalt metal, or compounds thereof
- C10G45/08—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 nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
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- 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
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
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- 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
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
- C10G2300/206—Asphaltenes
Abstract
The invention belongs to a hydrodemetallization catalyst, and particularly relates to a hydrodemetallization catalyst with bimodal pore distribution and a preparation method thereof. The hydrogenation active metal component contained in the catalyst is selected from at least one metal component of VIB group and at least one metal component of VIII group. The preparation method comprises the steps of mixing the precursor of the alumina with the extrusion aid, adding a metal salt solution containing the hydrogenation active metal component, kneading, molding, drying, and then carrying out hydrothermal treatment, drying and roasting. Compared with the prior invention, the preparation method of the catalyst provided by the invention has the advantages of easy control of the bimodal pore channel structure of the catalyst, shortened preparation process, simple method, easy operation, capability of reducing the production cost of the catalyst and easy industrial use. The prepared catalyst can be used as a hydrogenation deasphalting and demetalization catalyst for heavy oil such as residual oil and the like.
Description
Technical Field
The invention belongs to a hydrodemetallization catalyst, and particularly relates to a hydrodemetallization catalyst with bimodal pore distribution and a preparation method thereof.
Background
Crude oil heaviness and deterioration are increasingly obvious, and environmental regulations are increasingly strict. The deep processing of inferior heavy oil such as residual oil can not only improve the utilization rate of the crude oil, but also reduce the environmental pollution. The poor heavy oil such as residual oil contains a large amount of metals such as Fe, Ni and V, and hydrogenation removal is required to be carried out firstly, so as to avoid poisoning downstream hydrodesulfurization, hydrodenitrogenation, catalytic cracking catalysts and the like. Metals in heavy oils such as residual oil mainly exist in macromolecular compounds such as colloids and asphaltenes. The part of the substance has complex structure, large molecular size and difficult diffusion, and the metal is deposited on the surface of the catalyst and in the pore channel after being removed. Therefore, in order to maximize the performance of residual oil hydrogenation for deasphalting and demetallization, the catalyst is required to have good reaction activity and excellent diffusion performance. At present, the catalyst for residual oil hydrogenation deasphalting and demetalization generally requires pore diameter bimodal distribution, and has two pore channels of macropores (pore diameter is more than 50 nm) and mesopores (pore diameter is less than 50 nm), wherein the macropores can provide channels for diffusion of macromolecules containing metal such as asphaltene and the like, rapid diffusion and deposition of impurities to the internal pore channels of the catalyst are promoted, the utilization rate of the catalyst is improved, and the mesopores can provide a specific surface as large as possible for reaction, promote removal of the impurities and uniform deposition in the pore channels, so that the hydrogenation catalyst has high demetalization activity and high impurity capacity, and is beneficial to prolonging the running period of the residual oil hydrogenation catalyst.
In order to improve the pore structure of the hydrodemetallization catalyst, a pore-expanding agent is generally added or a complex catalyst preparation process is adopted at present. In the prior art, the patent art of bimodal pore size distribution catalysts is disclosed as follows:
CN100496738C discloses an alumina carrier with bimodal pores, a catalyst and a preparation method thereof. The carrier adopts the precursor of alumina and a nitrogen-containing compound except acid to be mixed, molded and dried, and the temperature is in 750-800 DEG CoAnd C, roasting to obtain the catalyst. The pore-expanding agent used in the method is a nitrogen-containing compound, comprises ammonium citrate, ammonium bicarbonate, ammonium oxalate, urea and the like, has high dosage (20-50% of the mass of an alumina precursor), and generates a large amount of NO in the roasting processxThe method is easy to cause environmental pollution, and the production cost of the catalyst is high. Meanwhile, the nitrogen-containing compound has low thermal stability and is volatile or decomposed in the drying process, so that the hole expanding effect and the repeatability of the product are influenced.
CN103357445A discloses a hydrogenation deasphalted catalyst and a preparation method thereof. The catalyst consists of a carrier with a bimodal pore structure and cobalt and/or nickel and molybdenum and/or tungsten components loaded on the carrier. The preparation method of the carrier used for the catalyst comprises the steps of modifying water containing pseudo-boehmite and alumina P1, then mixing, molding, drying and roasting P1 and a modified product P2 thereof, and then impregnating, drying and roasting. The whole preparation process of the catalyst is complex.
Disclosure of Invention
The invention aims to provide a novel hydrodemetallization catalyst with bimodal pore distribution and a preparation method thereof, aiming at the defects in the existing preparation method of the hydrodemetallization catalyst with bimodal pore distribution. Compared with the prior art, the invention adopts a brand-new method for preparing the catalyst with bimodal pore distribution, simplifies the preparation process of the catalyst, realizes clean preparation and is easier to be applied in industry. The catalyst prepared by the method can be used as a hydrogenation deasphalting and demetalization catalyst for heavy oil such as residual oil and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the hydrodemetallization catalyst with bimodal pore distribution contains hydrogenation active metal components selected from at least one VIB group metal component and at least one VIII group metal component, wherein the content of the VIB group metal component is 0.1-12 wt% and the content of the VIII group metal component is 0.1-3 wt% calculated by oxides and based on the catalyst. The catalyst contains an auxiliary phosphorus, the content of which is 0 to 3 wt.%, calculated as oxide and based on the catalyst.
The pore volume of the catalyst is 0.6-1.4 mL/g and the specific surface area is 50-300 m measured by mercury intrusion method2The pore volume with the pore diameter less than 50 nm accounts for 40-80% of the total pore volume, and the pore volume with the pore diameter more than 50 nm accounts for 20-60% of the total pore volume.
The invention also provides a preparation method of the bimodal pore distribution heavy oil hydrodemetallization catalyst, which comprises the steps of kneading, forming, drying, hydrothermal treatment, drying and roasting.
The preparation of the catalyst precursor is that the precursor of the alumina is mixed with the extrusion assistant, and then the mixture is added with the metal salt solution containing the hydrogenation active metal component for kneading, molding and drying.
The precursor of the alumina is one or a mixture of more of gibbsite, pseudo-boehmite, boehmite and amorphous aluminum hydroxide, and can be a commercial product or a product prepared by any method in the prior art. Preferably pseudoboehmite.
The extrusion aid is one or more of sesbania powder, methyl cellulose, starch and polyvinyl alcohol, and the addition amount of the extrusion aid is 0.5-5% of the amount of the alumina dry matrix.
The metal salt solution may or may not be added with an acid. If acid is added, the acid is one or more of inorganic acid such as hydrochloric acid, sulfuric acid or nitric acid, and the addition amount is 0-3% of the amount of the alumina dry matrix; or one or more of organic acid such as formic acid, acetic acid, tartaric acid, oxalic acid or citric acid, and the addition amount is 0-3% of the dry matrix of alumina.
The hydrogenation active metal component is selected from the combination of at least one group VIB metal component and at least one group VIII metal component.
The forming method adopts any one of tabletting, rolling ball, oil column forming or strip extruding. The shape of the carrier can be made into spherical, spheroidal, cylindrical, clover-shaped or clover-shaped according to different requirements. The drying temperature is 60-150 ℃, and the drying time is 0.1-12 h. The dried catalyst precursor still contains part of water, and the dry basis of the catalyst precursor is 50-90 wt%.
The hydrothermal treatment refers to heating the partially dried catalyst precursor to a certain temperature under a closed condition, and then carrying out hydrothermal treatment at the temperature for a period of time. The temperature of the hydrothermal treatment is 150-300 ℃, and the time is 1-24 h. The water used in the hydrothermal treatment is water carried by the partially dried catalyst precursor, and the mass of the water is 10-100% of the dry mass of the catalyst.
The preparation method of the catalyst also comprises the steps of drying and roasting the sample after the hydrothermal treatment. The drying temperature is 80-200 ℃, and the drying time is 1-24 h. The roasting temperature is 400-800 ℃, and the roasting time is 1-8 h.
The invention has the following remarkable advantages:
the invention provides a novel method for preparing a heavy oil hydrodemetallization catalyst, and the obtained catalyst has a structure with mesoporous and macroporous bimodal pore distribution. And (3) modulating the mesoporous aperture of the catalyst by adopting hydrothermal treatment.
The advantages are that: compared with the prior invention, the preparation method of the catalyst provided by the invention has the advantages of easy control of the bimodal pore channel structure of the catalyst, shortened preparation process, simple method, easy operation, capability of reducing the production cost of the catalyst and easy industrial use.
The catalyst prepared by the method can be used as a hydrogenation deasphalting and demetalization catalyst for heavy oil such as residual oil and the like.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Examples 1-3 illustrate catalysts having bimodal pore distributions and methods of making the same provided by the present invention.
Example 1
165 g of commercial pseudoboehmite (73 wt% on a dry basis) was weighed, 3.6 g of sesbania powder was added, and mixed well. 226 mL of 20.7 g/L MoO containing 4.2 g/L NiO was added3，2.9 g/L P2O5The Ni-Mo-P solution is kneaded into plastic bodies, and then the plastic bodies are extruded into clover-shaped strips with the diameter of 1.3 mm on a strip extruding machine. The wet strands were dried at 100 ℃ for 30 minutes to give strands having a dry basis of 65% by mass. And (3) placing the strips into a hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into an oven, heating to 250 ℃, and carrying out thermostatic hydrothermal treatment for 3 hours. And drying the sample subjected to the hydrothermal treatment at 120 ℃ for 12 h, and keeping the temperature of the sample in a roasting furnace at 600 ℃ for 2 h to obtain the catalyst A1. The catalyst channel structure and metal loading are shown in table 1.
Example 2
165 g of commercial pseudoboehmite (73 wt% on a dry basis) was weighed, 3.6 g of sesbania powder was added, and mixed well. 226 mL of 20.7 g/L MoO containing 4.2 g/L NiO was added3，2.9 g/L P2O5The Ni-Mo-P solution is kneaded into plastic bodies, and then the plastic bodies are extruded into clover-shaped strips with the diameter of 1.3 mm on a strip extruding machine. The wet strands were dried at 120 ℃ for 30 minutes to give strands having a dry basis of 74% by mass. And (3) placing the strips into a hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into an oven, heating to 220 ℃, and carrying out thermostatic hydrothermal treatment for 3 hours. And drying the sample subjected to the hydrothermal treatment at 120 ℃ for 12 h, and keeping the temperature of the sample in a roasting furnace at 600 ℃ for 2 h to obtain the catalyst A2. The catalyst channel structure and metal loading are shown in table 1.
Example 3
A commercial pseudoboehmite was weighed at 165 g (dry)73 wt%), 3.6 g sesbania powder was added and mixed well. 226 mL of 31.1 g/L MoO containing 6.3 g/L NiO was added3，4.4 g/L P2O5The Ni-Mo-P solution is kneaded into plastic bodies, and then the plastic bodies are extruded into clover-shaped strips with the diameter of 1.3 mm on a strip extruding machine. The wet strands were dried at 100 ℃ for 30 minutes to give strands having a dry basis of 68% by mass. And (3) placing the strips into a hydrothermal kettle, sealing the hydrothermal kettle, putting the hydrothermal kettle into an oven, heating to 250 ℃, and carrying out thermostatic hydrothermal treatment for 3 hours. And drying the sample subjected to the hydrothermal treatment at 120 ℃ for 12 h, and keeping the temperature of the sample in a roasting furnace at 600 ℃ for 2 h to obtain the catalyst A3. The catalyst channel structure and metal loading are shown in table 1.
Comparative example 1
165 g of commercial pseudoboehmite (73 wt% on a dry basis) was weighed, 3.6 g of sesbania powder was added, and mixed well. 226 mL of 20.7 g/L MoO containing 4.2 g/L NiO was added3，2.9 g/L P2O5The Ni-Mo-P solution is kneaded into plastic bodies, and then the plastic bodies are extruded into clover-shaped strips with the diameter of 1.3 mm on a strip extruding machine. The wet strip sample is dried at 120 ℃ for 12 h and kept at 600 ℃ for 2 h in a roasting furnace to obtain the catalyst B1. The catalyst pore structure and metal loading are shown in table 1.
Comparative example 2
165 g of commercial pseudoboehmite (73 wt% on a dry basis) was weighed, 3.6 g of sesbania powder was added, and mixed well. 230 g of a dilute acetic acid solution (containing 2.0 g of acetic acid) was added thereto, kneaded to give a plastic mass, and then extruded into a clover-type strand having a diameter of 1.3 mm on a plodder. And drying the wet strip at 120 ℃ for 12 h, and keeping the temperature of the wet strip in a roasting furnace at 600 ℃ for 2 h to obtain the alumina carrier. Taking 100 g of alumina carrier, using 118 mL of alumina carrier containing 10.0 g/L NiO and 49.6 g/L MoO3，7.0 g/L P2O5The Ni-Mo-P solution is soaked for 1 hour, dried for 12 hours at the temperature of 120 ℃, and kept constant at the temperature of 500 ℃ for 2 hours in a roasting furnace to obtain a catalyst B2. The catalyst pore structure and metal loading are shown in table 1.
TABLE 1
Examples 4 to 6
Examples 4-6 provide specific embodiments of the resid hydrotreating process of the present invention and illustrate the resid hydrodemetallization performance of the catalysts of the above examples.
The catalyst was evaluated on a 100 mL small fixed bed reactor using a residual oil having a nickel content of 27 ppm, a vanadium content of 98 ppm, a sulfur content of 4.65%, a carbon residue of 13.2%, and a nitrogen content of 3240 ppm as a raw material, and the results are shown in Table 2.
The catalyst loading volume was 100 mL. The process conditions used to evaluate each catalyst were the same. The reaction conditions are as follows: the reaction temperature is 380 ℃, the hydrogen partial pressure is 15 MPa, and the liquid hourly space velocity is 1.0 h-1The volume ratio of hydrogen to oil is 760, and a sample is taken after 300 hours of reaction. Inductively coupled plasma emission spectrometry (ICP-AES) was used to determine the nickel and vanadium content of the oil before and after hydrotreating (see RIPP124-90 for a specific method). The mass fraction of asphaltenes in the oil before and after hydrotreating was analyzed by a petroleum asphalt component determination method (for a specific method, see NB/SH/T0509-2010). The metal and asphaltene removal rates were calculated according to the following formula:
the evaluation results are shown in Table 2.
Comparative examples 3 to 4
The deasphalted mass fraction and demetallization fraction of the catalysts B1 and B2 were evaluated according to the methods of examples 4 to 6. The results are shown in Table 2.
TABLE 2
The results shown in Table 2 are the results obtained after the reaction was evaluated for 300 hours, and it can be seen from the comparison that the hydrodemetallization activity and the hydrodeasphaltene activity of the hydrodemetallization catalyst provided by the present invention are higher than those of the reference catalyst.
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 (9)
1. A preparation method of a hydrodemetallization catalyst is characterized by comprising the following steps: the catalyst contains a hydrogenation active metal component; the hydrogenation active metal component is selected from at least one metal component of VIB group and at least one metal component of VIII group; calculated as oxides and based on the catalyst, the content of the metal component of the VIB group is 0.1-12 wt%, and the content of the metal component of the VIII group is 0.1-3 wt%; the preparation method of the catalyst comprises the steps of mixing a precursor of alumina with an extrusion aid, adding a metal salt solution containing a hydrogenation active metal component, kneading, molding, drying, and then carrying out hydrothermal treatment, drying and roasting.
2. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the catalyst has a bimodal pore distribution structure, the pore volume of the catalyst is 0.6-1.4 mL/g, and the specific surface area of the catalyst is 50-300 m2The pore volume with the pore diameter less than 50 nm accounts for 40-80% of the total pore volume, and the pore volume with the pore diameter more than 50 nm accounts for 20-60% of the total pore volume.
3. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the catalyst also contains auxiliary phosphorus, and the content of the oxide of the auxiliary phosphorus is 0-3 wt% calculated by oxide and taking the catalyst as a reference.
4. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the precursor of the alumina is pseudo-boehmite.
5. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that:
the extrusion aid is one or more of sesbania powder, methyl cellulose, starch and polyvinyl alcohol, and the addition amount of the extrusion aid is 0.5-5% of the amount of the alumina dry matrix.
6. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the metal salt solution is added with or without acid.
7. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the acid is added, and the acid is inorganic acid or organic acid; wherein the inorganic acid is one or more of hydrochloric acid, sulfuric acid or nitric acid, and the addition amount is 0-3% of the amount of the alumina dry matrix; the organic acid is one or more of formic acid, acetic acid, tartaric acid, oxalic acid or citric acid, and the addition amount is 0-3% of the amount of the alumina dry matrix.
8. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that: the forming method adopts any one of tabletting, rolling ball, oil column forming or strip extruding; the shape of the carrier is made into a spherical shape, a spherical-like shape, a cylindrical shape, a clover shape or a clover shape according to different requirements; the drying temperature is 60-150 ℃, and the drying time is 0.1-12 h; the dried catalyst precursor still contains part of water, and the dry basis of the catalyst precursor is 50-90 wt%.
9. The method for preparing a hydrodemetallization catalyst according to claim 1, characterized in that:
the temperature of the hydrothermal treatment is 150-300 ℃, and the time is 1-24 h; the water used in the hydrothermal treatment is water carried by a partially dried catalyst precursor, and the mass of the water is 10-100% of the mass of a dry base of the catalyst; the drying temperature after the hydrothermal treatment is 80-200 ℃, and the drying time is 1-24 h; the roasting temperature is 400-800 ℃, and the roasting time is 1-8 h.
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| CN111821991B (en) * | 2019-04-17 | 2022-07-12 | 中国石油化工股份有限公司 | Preparation method of hydrodesulfurization catalyst |
| CN110227481B (en) * | 2019-06-25 | 2022-06-10 | 中化泉州石化有限公司 | Heavy oil hydrotreating catalyst and preparation method thereof |
| CN111001411A (en) * | 2019-11-27 | 2020-04-14 | 浙江石油化工有限公司 | Residual oil hydrotreating catalyst and preparation method thereof |
| CN113088329B (en) * | 2019-12-23 | 2023-02-24 | 中国石油天然气股份有限公司 | Method and device for viscosity reduction and modification of inferior heavy oil |
| CN111905838A (en) * | 2020-08-19 | 2020-11-10 | 中化泉州石化有限公司 | Method for preparing hydrodemetallization catalyst by using residual oil hydrogenation deactivated catalyst |
| CN114100645A (en) * | 2021-11-24 | 2022-03-01 | 中化泉州能源科技有限责任公司 | Multi-channel and hollow hydrogenation active proppant and preparation method thereof |
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