CN106140184A - The preparation method of a kind of heavy oil floating bed hydrocracking catalyst and gained serosity thereof - Google Patents
The preparation method of a kind of heavy oil floating bed hydrocracking catalyst and gained serosity 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/485—Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/50—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using organic liquids
- B01J38/56—Hydrocarbons
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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
- 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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- 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
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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
- C10G2300/70—Catalyst aspects
- C10G2300/701—Use of spent catalysts
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- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
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Abstract
The present invention relates to the preparation method of heavy oil floating bed hydrocracking catalyst, and serosity obtained by this method.The method of the invention includes: waste acetic acid carries out coke-burning regeneration, grinds, and prepares waste acetic acid powder, and measures its water absorption rate；Take acid solution by 1～1.2 times of waste acetic acid hole saturated impregnation liquid volume, add nickel-molybdenum ore powder, stir 1.5～2.5h, obtain liquid-solid mixture；Adding waste acetic acid powder in liquid-solid mixture to impregnate, after mix homogeneously, standing 1.5～2.5h, drying and roasting, obtain the mixture after roasting；Mixture after roasting adds binding agent and water, makes serosity, serosity is carried out spray shaping and is dried, i.e. prepare heavy oil floating bed hydrocracking catalyst.Catalyst prepared by the present invention is relatively cheap, and hydrogenation activity and cracking activity are all largely increased, it is adaptable to heavy oil floating bed hydrogenation, and can continue to recycle according to the method for the present invention by this catalyst.
Description
Technical field
The present invention relates to hydrocracking catalyst field, particularly relate to a kind of be prepared heavy oil by waste acetic acid and hang
The method of floating bed hydrocracking catalyst, and the serosity obtained by the method.
Background technology
Suspension bed hydrocracking heavy oil refers to, heavy oil under facing hydrogen and fully dispersed catalyst concurrent conditions in high temperature,
The process of the raw hydrocracking reaction of elevated pressure.Raw material can be residual oil extremely inferior, it is also possible to be the mixing of coal and residual oil
Thing.Along with the heaviness day by day of crude oil, and some produced during the alternative energy source finding fossil energy are unconventional bad
Matter oil product (such as coal tar etc.), causes traditional processing of heavy oil means (such as residual hydrogenation, RFCC) to be difficult to enter it
Row processes.And heavy oil floating bed hydrocracking technology is owing to it has, and adaptability to raw material is wide, catalyst use efficiency is high, economic effect
The feature that benefit is high, shows prominent advantage.
The catalyst that conventional heavy oil floating bed hydrocracking technique uses has solid particle class catalyst, oil-soluble to be catalyzed
Agent, water-soluble catalytic etc., or the combination of several catalyst.Catalytic effect best for oil-soluble catalyst, therein add
Hydrogen activity component is oil-soluble metal Co, Mo, Ni, W etc..Although this oil-soluble catalyst is hydrogenated with effective, but cost is relatively
Height, and more difficult recycling.Therefore, for the mink cell focus that processing the degree of inferiority is high, cheap, its economic benefit is poor.
Based on the problems referred to above, prior art discloses a kind of inferior heavy oil suspension bed hydrogenation catalyst and preparation thereof and use
Method, the method is with the bauxite powder activated as carrier, loads the one in molybdenum, nickel, cobalt, tungsten and ferrum or several thereon
Kind, in terms of metal oxide weight, load capacity is 0.5%～15%.Preparation method is by bauxite powder and sub-molten salt medium
Thermal activation after (NaOH-H2O and/or KOH-H2O) mixing, through deionized water wash, after drying as catalyst carrier, will prepare
Carrier loaded transition metal after be dried, roasting, thus obtain inferior heavy oil suspension bed hydrogenation catalyst.But, the method institute
The cracking activity preparing catalyst is relatively low.
Prior art two discloses a kind of hydrocracking catalyst for suspension bed and its preparation method and application, and the method is selected
Waste acetic acid as carrier, one or more of carrying transition metal molybdenum, nickel, tungsten and ferrum, metal load thereon
Amount is 3%～5%.Preparation method be using particle diameter < waste acetic acid of 150 μm is dried, after roasting as carrier, utilize
Solution containing metal precursor prepares catalyst after carrying out incipient impregnation, then drying, roasting.But, bear in this process
Active metal relatively costly carried, the economic benefit causing this technology is poor.
Summary of the invention
It is desirable to provide a kind of side being prepared heavy oil floating bed hydrocracking catalyst by waste acetic acid
Method, improves hydrogenation and the cracking performance of catalyst, effectively solves the recycling problem of waste acetic acid.
For achieving the above object, the invention provides the preparation method of a kind of heavy oil floating bed hydrocracking catalyst, bag
Include following steps:
Step A, carries out coke-burning regeneration by waste acetic acid, by the waste acetic acid grounds travel after regeneration
Broken, prepare waste acetic acid powder, and measure its water absorption rate；
Step B, takes acid solution by 1～1.2 times of waste acetic acid hole saturated impregnation liquid volume, and addition is ready to
Nickel-molybdenum ore powder, stir 1.5～2.5h, obtain liquid-solid mixture；
Step C, adds described waste acetic acid powder in described liquid-solid mixture and impregnates, and mixing is all
Stand 1.5～2.5h after even, be then dried roasting, obtain the mixture after roasting；
Step D, adds binding agent and water, makes serosity, carry out this serosity afterwards in the mixture after described roasting
Spray shaping is dried, and i.e. prepares heavy oil floating bed hydrocracking catalyst.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, in described step A, waste acetic acid
The particle size of powder is below 5 μm, preferably 2～3 μm.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, in described step B, nickel-molybdenum ore is ground
Pulverizing and obtain nickel-molybdenum ore powder, the particle size of this powder is below 5 μm, preferably 2～3 μm.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, in described nickel-molybdenum ore powder containing 1wt%～
The molybdenum of 8wt% and the nickel (wt% is weight percentage) of 1wt%～7wt%.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, the acid solution in described step B include sulphuric acid,
Nitric acid；The concentration of described acid solution is: 1～6mol/L.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, solid material includes nickel-molybdenum ore powder, gives up and urge
Fluidized cracking catalysts powder and binding agent, described solid material accounts for the percentage ratio of total solid raw material and is: nickel-molybdenum ore powder is
30wt%～50wt%, waste acetic acid powder is 40wt%～60wt%, and binding agent is 10wt%；Described step D
Serosity in, it is 44wt%～46wt% that solid material accounts for the percentage ratio of described serosity.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, in described step C, the temperature of roasting is 400
～450 DEG C, roasting time is 4～6h.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, in described step D, heavy oil floating bed hydrogenation splits
Changing catalyst size is 75～150 μm.
In the preparation method of above-mentioned heavy oil floating bed hydrocracking catalyst, described binding agent is Alumina gel；In described step
Before rapid A, also described waste acetic acid is carried out pretreatment: utilize toluene extracting to remove this waste acetic acid
The oil product adsorbed, and be dried at 100～120 DEG C, drying time is 1.5～2.5h.
Present invention also offers a kind of by the serosity obtained by said method, in described serosity, solid material accounts for described serosity
Percentage ratio be 44wt%～46wt%, wherein said solid material includes: nickel-molybdenum ore, waste acetic acid, binding agent；
Each component by accounting for the percentages of solid material in described serosity is:
Nickel-molybdenum ore, accounts for 30wt%～50wt%；
Waste acetic acid, accounts for 40wt%～60wt%；
Binding agent, accounts for 10wt%.
Catalyst prepared by the present invention is relatively cheap, and hydrogenation activity and cracking activity are all greatly improved, it is adaptable to weight
Oil floating bed hydrogenation, and can continue to recycle according to the method for the present invention by this catalyst.
Accompanying drawing explanation
Fig. 1 is the preparation method schematic flow sheet of a kind of heavy oil floating bed hydrocracking catalyst of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the detailed description of the invention of the present invention is described in more details, in order to energy
The advantage being enough more fully understood that the solution of the present invention and its various aspects.But, specific embodiments described below and reality
Executing example is only descriptive purpose rather than limitation of the present invention.
As it is shown in figure 1, the method that the present invention prepares heavy oil floating bed hydrocracking catalyst comprises the steps:
Step A, prepares waste acetic acid powder: carry out making charcoal by pretreated waste acetic acid again
Raw, then the catalytic cracking catalyst after regeneration is ground, and measure its water absorption rate.
Above-mentioned preprocessing process by: utilize toluene extracting to remove the oil product that adsorbed of this waste acetic acid, and
100～120 DEG C are dried 1.5～2.5h.
The method that coke-burning regeneration process is nitrogen-air regenesis used in the embodiment of the present invention: useless catalytic cracking is urged
Agent is placed in regenerator, is passed through nitrogen and replaces, and temperature is slowly raised to 250～350 DEG C, after constant temperature 3～4h slowly
Being passed through air, the oxygen content controlled in regenerator is 0.3%～0.5%, and heating rate is 10～20 DEG C/h, and temperature rises to 400
Constant temperature 2～3h after DEG C, temperature rises to 500 DEG C of constant temperature to end of making charcoal, and starts to cool to room after continuing constant temperature 6h after end of making charcoal
Temperature.By this coke-burning regeneration process, major part can be removed and cover the carbon deposit on waste acetic acid active center, favorably
In recovering its cracking activity, and improve pore passage structure.
After the ground pulverizing of above-mentioned waste acetic acid, the particle size obtained is below 5 μm, and the present invention is real
The preferred size executing example is 2～3 μm.
Step B, prepares liquid-solid mixture: nickel-molybdenum ore grinds prepared nickel-molybdenum ore powder, is then added to acid
In solution, stir 1.5～2.5h, prepare liquid-solid mixture.
Above-mentioned acid solution includes that sulphuric acid, nitric acid etc., the volume of taken acid solution are the saturated leaching in waste acetic acid hole
Long-pending 1～1.2 times of stain liquid, concentration is 1～6mol/L.
Molybdenum containing 1wt%～8wt% and the nickel of 1wt%～7wt% in above-mentioned nickel-molybdenum ore, and mostly with the shape of sulphided state
Formula exists.After grinding, the particle size obtained is below 5 μm, and the preferred size of the embodiment of the present invention is 2～3 μm.
Step C, drying and roasting: add waste acetic acid powder in above-mentioned liquid-solid mixture, after mix homogeneously,
Carry out drying and roasting after standing 1.5～2.5h, obtain the mixture after roasting.Described sintering temperature is 400～450 DEG C, roasting
Time is 4～6h.
In above-mentioned liquid-solid mixture, the nickel in nickel-molybdenum ore and molybdenum element can be leached by acid solution with the form of metallic salt,
Then it is carried on waste acetic acid powder, after roasting, generates nickel oxide and the molybdenum oxidation with hydrogenation activity
Thing.Further, acid solution can improve the metal deposit problem on waste acetic acid and pore passage structure, improves it cracking
Energy.
Still containing the nickel not leached and molybdenum element in nickel-molybdenum ore slag, its dispersibility is improved, and vulcanizes through roasting
After can be as the generation of active center catalytic heavy hydrocracking reaction.
Step D, serosity molding: add binding agent and water in the mixture after above-mentioned roasting, make serosity, by spraying
After drying machine drying and moulding, i.e. prepare hydrocracking catalyst for suspension bed.
In above-mentioned serosity, it is 44wt%～46wt% that solid material accounts for the percentage ratio of serosity.Wherein, solid material includes:
Nickel-molybdenum ore, waste acetic acid, binding agent, each component by the percentages accounting for total solid material is: nickel-molybdenum ore
30wt%～50wt%, waste acetic acid 40wt%～60wt%, binding agent 10wt%.
The hydrocracking catalyst for suspension bed prepared by above-mentioned steps, its particle size should control in 75～150 μm.
Embodiment 1
Select waste acetic acid, use toluene extracting to remove the oil product of dead catalyst absorption, 120 DEG C of dry 2h
After, catalyst is carried out coke-burning regeneration, measures the water absorption rate of regenerated catalyst, catalyst is ground to 2～3 μm, weighs 60g.
Calculate volume by saturated infusion process, take the sulfuric acid solution that concentration is 6mol/L of 1.2 times of volumes, 30g nickel-molybdenum ore powder is added
In sulfuric acid solution, mix and blend 2.5h.In liquid-solid mixture, add waste acetic acid powder, stand after mix homogeneously
2h, after sample drying, 450 DEG C of roasting 4h.Mixture adds 10g Alumina gel and 120ml water after baking, makes serosity
After, make, by spray drying, the fresh catalyst that particle diameter is 75～150 μm.
Embodiment 2
Select waste acetic acid, use toluene extracting to remove the oil product of dead catalyst absorption, 120 DEG C of dry 2h
After, catalyst is carried out coke-burning regeneration, measures the water absorption rate of regenerated catalyst, catalyst is ground to 2～3 μm, weighs 40g.
Calculate volume by saturated infusion process, take the sulfuric acid solution that concentration is 5mol/L of 1.2 times of volumes, 50g nickel-molybdenum ore powder is added
In sulfuric acid solution, mix and blend 2h.In liquid-solid mixture, add waste acetic acid powder, stand after mix homogeneously
2.5h, after sample drying, 450 DEG C of roasting 5h.Mixture adds 10g Alumina gel and 120ml water after baking, makes serosity
After, make, by spray drying, the fresh catalyst that particle diameter is 75～150 μm.
Embodiment 3
Select waste acetic acid, use toluene extracting to remove the oil product of dead catalyst absorption, 100 DEG C of dry 2.5h
After, catalyst is carried out coke-burning regeneration, measures the water absorption rate of regenerated catalyst, catalyst is ground to 2～3 μm, weighs 50g.
Calculating volume by saturated infusion process, taking isopyknic concentration is 3mol/L sulfuric acid solution, 40g nickel-molybdenum ore powder is added sulphuric acid molten
In liquid, mix and blend 2.5h.In liquid-solid mixture, add waste acetic acid powder, after mix homogeneously, stand 2.5h,
After sample drying, 400 DEG C of roasting 6h.Mixture adds 10g Alumina gel and 120ml water after baking, after making serosity, logical
Cross spray drying and make the fresh catalyst that particle diameter is 75～150 μm.
Embodiment 4
Select waste acetic acid, use toluene extracting to remove the oil product of dead catalyst absorption, 110 DEG C of dry 1.5h
After, catalyst is carried out coke-burning regeneration, measures the water absorption rate of regenerated catalyst, catalyst is ground to 2～3 μm, weighs 40g.
Calculating volume by saturated infusion process, taking isopyknic concentration is 1mol/L sulfuric acid solution, 50g nickel-molybdenum ore powder is added sulphuric acid molten
In liquid, mix and blend 2h.In liquid-solid mixture, add waste acetic acid powder, after mix homogeneously, stand 2.5h, will
After sample drying, 400 DEG C of roasting 6h.Mixture adds 10g Alumina gel and 120ml water after baking, after making serosity, passes through
It is spray-dried and makes the fresh catalyst that particle diameter is 75～150 μm.
Comparative example
Select waste acetic acid, use toluene extracting to remove the oil product of dead catalyst absorption, 120 DEG C of dry 2h
After, catalyst is carried out coke-burning regeneration, and catalyst is ground to 2～3 μm, weigh 60g.By 30g nickel-molybdenum ore baking after grinding,
Mixing with dead catalyst powder, add 10g Alumina gel and 120mL water, after making serosity, making particle diameter by spray drying is 75
～150 fresh catalysts of μm.
Table 1 below is the composition of waste acetic acid and nickel-molybdenum ore.Prepared catalyst is carried out in autoclave
Coal tar hydrocracking is tested, with the activity of comparative example for 100, and the relative activity evaluation result of other gained catalyst such as table 2
Shown in.
Table 1 waste acetic acid and the composition of nickel-molybdenum ore
| Analysis project | Nickel content, wt% | Molybdenum content, wt% | Coke content, wt% |
| Waste acetic acid | 3.4 | 8 | 15.3 |
| Nickel-molybdenum ore | 3.1 | 7.3 | -- |
Table 2 catalyst activity evaluation result
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example |
| Desulfurization degree | 102 | 103 | 102 | 101 | 100 |
| > 370 DEG C of conversion ratios | 108 | 106 | 105 | 103 | 100 |
As shown in Table 2, the inventive method the regenerated catalyst prepared has preferable Hydrogenation and cracking performance, can have
Effect converts the macromolecular components in coal tar, and removes a part of hetero atom, produces the oil product meeting fixed bed hydrogenation charging, this
Inventive method is particularly well-suited to be prepared coal tar suspension bed hydrocracking catalyst by waste acetic acid.
It is last that it is noted that obviously above-described embodiment is only for clearly demonstrating example of the present invention, and also
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out change or the variation of other multi-form.Here without also cannot all of embodiment be given exhaustive.And thus drawn
What Shen went out obviously changes or changes among still in protection scope of the present invention.
Claims (10)
1. a preparation method for heavy oil floating bed hydrocracking catalyst, comprises the steps:
Step A, carries out coke-burning regeneration by waste acetic acid, is ground by the waste acetic acid after regeneration,
Prepare waste acetic acid powder, and measure its water absorption rate；
Step B, takes acid solution by 1～1.2 times of waste acetic acid hole saturated impregnation liquid volume, adds ready nickel
Molybdenum ore powder, stirs 1.5～2.5h, obtains liquid-solid mixture；
Step C, adds described waste acetic acid powder in described liquid-solid mixture and impregnates, after mix homogeneously
Stand 1.5～2.5h, be then dried roasting, obtain the mixture after roasting；
Step D, adds binding agent and water, makes serosity, spray this serosity afterwards in the mixture after described roasting
Shaping and drying, i.e. prepares heavy oil floating bed hydrocracking catalyst.
Method the most according to claim 1, it is characterised in that in described step A, waste acetic acid powder
Particle size is below 5 μm, preferably 2～3 μm.
Method the most according to claim 1, it is characterised in that in described step B, is ground nickel-molybdenum ore pulverizing and obtaining
To nickel-molybdenum ore powder, the particle size of this powder is below 5 μm, preferably 2～3 μm.
Method the most according to claim 3, it is characterised in that in described nickel-molybdenum ore powder containing 1wt%～8wt% molybdenum and
The nickel of 1wt%～7wt%.
Method the most according to claim 1, it is characterised in that the acid solution in described step B includes sulphuric acid, nitric acid；Institute
The concentration stating acid solution is 1～6mol/L.
Method the most according to claim 1, it is characterised in that solid material includes that nickel-molybdenum ore powder, useless catalytic cracking are urged
Agent powder and binding agent, described solid material accounts for the percentage ratio of total solid raw material and is: nickel-molybdenum ore powder be 30wt%～
50wt%, waste acetic acid powder is 40wt%～60wt%, and binding agent is 10wt%；In the serosity of described step D,
It is 44wt%～46wt% that solid material accounts for the percentage ratio of described serosity.
Method the most according to claim 1, it is characterised in that in described step C, the temperature of roasting is 400～450 DEG C,
Roasting time is 4～6h.
Method the most according to claim 1, it is characterised in that in described step D, heavy oil floating bed hydrocracking catalyst
A size of 75～150 μm.
Method the most according to claim 1, it is characterised in that described binding agent is Alumina gel；Before described step A,
Also described waste acetic acid is carried out pretreatment: utilize toluene extracting to remove what this waste acetic acid was adsorbed
Oil product, and be dried at 100～120 DEG C, drying time is 1.5～2.5h.
10. the serosity prepared according to the method one of claim 1 to 9 Suo Shu, in described serosity, solid material accounts for described
The percentage ratio of serosity is 44wt%～46wt%, and wherein said solid material includes: nickel-molybdenum ore, waste acetic acid, viscous
Knot agent；Each component by accounting for the percentages of solid material in described serosity is:
Nickel-molybdenum ore, accounts for 30wt%～50wt%；
Waste acetic acid, accounts for 40wt%～60wt%；
Binding agent, accounts for 10wt%.
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| CN1609174A (en) * | 2003-10-24 | 2005-04-27 | 中国石油化工股份有限公司 | Prepn process of catalyst for residual oil hydrocracking in suspension bed |
| CN101543783A (en) * | 2008-03-27 | 2009-09-30 | 中国石油化工股份有限公司 | Suspension bed hydrocracking catalyst and preparation method and application thereof |
| CN105126815A (en) * | 2015-07-16 | 2015-12-09 | 福州大学 | Poor-quality heavy oil suspended bed hydrogenation catalyst, preparation method and use method thereof |
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