CN106635157A - Inferior crude oil lightweighting method - Google Patents
Inferior crude oil lightweighting method Download PDFInfo
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- CN106635157A CN106635157A CN201510717262.4A CN201510717262A CN106635157A CN 106635157 A CN106635157 A CN 106635157A CN 201510717262 A CN201510717262 A CN 201510717262A CN 106635157 A CN106635157 A CN 106635157A
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Abstract
The invention relates to the field of oil refining, and discloses an inferior raw oil lightweighting method. The method comprises the following steps: introducing a reaction material in a slurry bed reactor for a hydrocracking reaction to obtain a hydrocracking mixture; separating the hydrocracking mixture to obtain heavy distillate oil containing a hydrogenation catalyst; introducing the heavy distillate oil in a hydrocyclone separator for separating the heavy distillate oil to obtain the low-density distillate oil of a poor solid content component and high-density tail oil of a rich solid content component; then introducing the low-density distillate oil in a fixed bed hydrotreatment apparatus for a hydrogenation reaction, fractionating the hydrogenation reaction products to obtain hydrogenation tail oil; and circulating the high-density tail oil to the inner space of the slurry bed reactor. The method can efficiently convert the inferior raw oil such as deoiled asphalt and/or high aromatic hydrocarbon component such as ethylene tar, catalytic cracking recycle oil and catalytic cracking slurry to the lightweight distillate oil.
Description
Technical field
The present invention relates to refining art, in particular it relates to a kind of lightening method of inferior feedstock oil.
Background technology
In Conventional refinery, solvent de-asphalting process is mainly used in producing high viscosity lubrication from decompression residuum
Oil base oil, wherein deasphalting process Main Function be slough the pitch in residual oil with reduce its carbon residue and
Improve color and luster.But the crude oil degree of heaviness that modern refinery is processed is deepened, and causes RFCC
And the raw material carbon residue of the device such as fixed bed residual hydrogenation raise, tenor increase, and then affect above-mentioned
The service cycle of device.It is and the metal impurities in residual oil are concentrated mainly in asphalitine component therefore logical
Cross the asphalitine that solvent de-asphalting process more can be removed thoroughly in feedstock oil so that deasphalted oil
Carbon residue and tenor are greatly lowered such that it is able to used as RFCC, residual hydrocracking
And the quality raw materials of residual hydrocracking.
Solvent deasphalting process produces a certain amount of de-oiled asphalt simultaneously.De-oiled asphalt is a kind of more special
Colloidal solution, due to being enriched residual oil in the overwhelming majority asphalitine and weight colloid so that its molecule knot
Structure height aromatisation, processability extreme difference, and be difficult to become road asphalt product.With conventional vacuum
Residual oil is compared, and the coking tendency of de-oiled asphalt is even more serious.At present, de-oiled asphalt is mainly used in refinery
The fuel of recirculating fluidized bed and boiler of power plant, fuel oil blend component and Pitch Water Slurry raw material, make to resource
Into certain waste.
Contain substantial amounts of heavy arene in ethylene bottom oil, catalytic cracking recycle oil and catalytic cracked oil pulp,
It is difficult to be processed further in existing refinery's flow process.For example, different type is mentioned in CN101531924B
Heavy charge to there is optimal conversion in catalytic cracking unit interval, Jiao can be reduced in the interval
The generation of charcoal and dry gas；If the unconverted heavy oil containing a large amount of aromatic hydrocarbons is further in catalytic cracking unit
Conversion, it will cause steeply rising for dry gas and coke yield, it is necessary to take other technological approaches conversions.
CN101531924B and CN101531923B disclose a kind of RFCC and hydrotreating group
Technique is closed, the charging that will be processed as fixed bed hydrogenation more than 260 DEG C of cuts in catalytic cracking fractionating tower,
And hydrogenation tail oil then enters catalytic cracking unit.Although the technique can reduce the generation of dry gas and coke,
But still can produce a certain amount of slurry oil.
Additionally, containing a large amount of catalyst fineses in catalytic cracked oil pulp, easily it is deposited on beds,
Bed pressure drop is caused to raise and block so as to traditional fixed bed hydrogenation technique lighting cannot be adopted.Mesh
Before, above-mentioned high aromatic component is mainly used in fuel oil, modified pitch, needle coke, carbon black and pitch base carbon
Preparation of fiber etc., cannot equally realize comprehensive effectively utilizes of resource.
CN1195822C discloses a kind of viscosity breaking method of de-oiled asphalt.The prior art is by de-oiling
After pitch and catalytic cracked oil pulp are according to certain ratio blending, using the prolonged mode of operation of low temperature,
On the basis of the operation cycle is ensured, the viscosity of raw material is effectively reduced.Fractionating out a small amount of visbreaking gas
After body and visbreaking gasoline, generation can be used as the visbreaking residue of heavy oil.The major product of the method
For visbreaking residue, value of the product is relatively low, and uses as heavy oil and also can cause to environment one to be fixed
Ring, it is impossible to which the economical and efficient for realizing raw material is utilized.
CN102234536A then refer to a kind of solvent deasphalting-RFCC-asphalt gasification-pitch
The group technology of mediation.Wherein a de-oiled asphalt part is used to produce chemical fertilizer as the raw material of asphalt gasification,
Another part reconciles production asphalt for high grade road together with the catalytic cracked oil pulp through plug.Although should
Group technology realizes the efficient utilization of asphaltic products, but for de-asphalting processes process and de-oiled asphalt
Property have clear and definite restrictive condition, the accommodation of raw material is narrower, while light ends cannot be met
The needs of oil production.
Prior art cannot both realize the contour virtue of ethylene bottom oil, catalytic cracking recycle oil and catalytic cracked oil pulp
The complete lighting of hydrocarbon component, cannot adapt to again raw material in poor quality trend and highly-efficient processing de-oiled asphalt.
Accordingly, it would be desirable to a kind of brand-new conversion process is developed, by de-oiled asphalt of different nature and/or high aromatic hydrocarbons group
It is point most or all of to be converted into light ends oil, the need growing to traffic fuel to meet China
Ask.
The content of the invention
The purpose of the present invention is that, for the deficiencies in the prior art, solution includes de-oiled asphalt and/or high aromatic hydrocarbons
Component (ethylene bottom oil, catalytic cracking recycle oil and catalytic cracked oil pulp etc.) interior inferior feedstock oil without
Method Efficient Conversion is the problem of light ends oil.
To achieve these goals, the present invention provides a kind of lightening method of inferior feedstock oil, the method
Including：Paste state bed reactor will be introduced including the reaction mass of inferior feedstock oil, hydrogenation catalyst and hydrogen
In carry out hydrocracking reaction, obtain being hydrocracked mixture；The mixture that is hydrocracked is carried out point
From, obtain first gas, the first light ends oil and the heavy distillate containing hydrogenation catalyst；By institute
State heavy distillate and be introduced in cyclone hydraulic separators and separated, obtain the low density fraction of lean solid content component
The high density tail oil of oil and rich solid content component；Then it is the low density fraction is oily with first lightweight
Distillate is introduced in fixed bed hydrogenation processing meanss carries out hydrogenation reaction, and by the hydrogenation reaction product for obtaining
It is fractionated, is obtained second gas, the second light ends oil and hydrogenation tail oil；And by the high density
Tail oil is looped back in paste state bed reactor inner chamber.
The said method of the present invention can efficiently by including de-oiled asphalt and/or high aromatic component (ethene
Tar, catalytic cracking recycle oil and catalytic cracked oil pulp etc.) it is converted into lightweight in interior inferior feedstock oil and evaporates
Divide oil.
The method of the present invention is combined paste state bed reactor and fixed bed residual hydrocracking device, can keep away
Exempt from catalyst inactivation and bed blockage problem in fixed bed, it is thus possible to highly-efficient processing high metal content, height
The poor quality material such as de-oiling pitch of carbon residue and high asphalt content, improves the integral light cut of refinery
Oil yield, and then improve its economic benefit.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute the part of specification, with
Detailed description below is used to explain the present invention together, but is not construed as limiting the invention.
In accompanying drawing：
Fig. 1 is a kind of structural representation of the cyclone hydraulic separators of preferred embodiment of the present invention.
Fig. 2 is a kind of process chart of preferred embodiment of the present invention.
Fig. 3 is a kind of structural representation of the paste state bed reactor of preferred embodiment of the present invention.
Description of reference numerals
1st, reactor shell 2, cyclone hydraulic separators inner chamber
3rd, sleeve 4, spin liquid separator entrance
5th, gaseous phase outlet 6, underflow pipe
7th, gas distributor 8, reactor inner chamber
9th, gas outlet 10, product oil export
11st, air inlet 12, unload agent mouth
13rd, agent mouth 14, raw material oil-in are added
15th, discharging opening 1a, inferior feedstock oil and hydrogenation catalyst
2a, force (forcing) pump 3a, heat exchanger
4a, paste state bed reactor 5a, the first hot high score
6a, cyclone hydraulic separators 7a, hydrogen to be clean
8a, fixed bed hydrogenation processing meanss 9a, the second hot high score
10a, destilling tower 11a, high density tail oil
12a, recycle oil 13a, oil is got rid of outward
14a, recycle hydrogen 15a, fresh hydrogen
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of lightening method of inferior feedstock oil, the method includes：Will be including inferior
The reaction mass of feedstock oil, hydrogenation catalyst and hydrogen is introduced in paste state bed reactor to carry out being hydrocracked instead
Should, obtain being hydrocracked mixture；The mixture that is hydrocracked is separated, obtain first gas,
First light ends oil and the heavy distillate containing hydrogenation catalyst；The heavy distillate is introduced and is revolved
Separated in liquid/gas separator, obtained the low density fraction oil and rich solid content component of lean solid content component
High density tail oil；Then the oily fixed bed that introduces oily with first light ends of the low density fraction is added
Hydrogenation reaction is carried out in hydrogen processing meanss, and the hydrogenation reaction product for obtaining is fractionated, obtain second
Gas, the second light ends oil and hydrogenation tail oil；And that the high density tail oil is looped back into slurry bed system is anti-
In answering device inner chamber.
In the present invention, in case of no particular description, described first, second etc. it is for area
Divide and do not indicate that precedence.Those skilled in the art should not be construed as the limit to technical scheme
System.
In the present invention, the reaction mass and be not specific to only containing inferior feedstock oil, hydrogenation catalyst and
The material of hydrogen, reaction mass herein refers to the property for participating in inferior feedstock oil lighting process
Material, including solid phase, gas phase and liquid phase material, also including reactant, product etc..
It is preferred that inferior feedstock oil is carried out to be re-introduced into being carried out in the paste state bed reactor after heat pre-treatment
Hydrocracking reaction.The heat pre-treatment is in order that into the reaction in the paste state bed reactor
Logistics can more efficiently carry out hydrocracking reaction.It is preferred that the condition of the heat pre-treatment includes temperature
Spend for 320-380 DEG C.
The present invention can also in advance be mixed the inferior feedstock oil with the hydrogenation catalyst, be formed
It is re-introduced into into the paste state bed reactor after uniform slurries.
By it is described be hydrocracked mixture and carry out detached method can have various, those skilled in the art can
With using conventional use of various methods in the art, as long as be hydrocracked mixture described in enabling to entering
The isolated first gas of row, the first light ends oil and the heavy distillate containing hydrogenation catalyst are
Can.For example, by it is described be hydrocracked mixture carry out detached method can for introduce high pressure hot separator
In separated, it is under conditions of 300-380 DEG C that the high pressure hot separator is separated preferably in temperature range
Carry out, pressure is 10-30MPa.
Can contain unconverted tail oil in the heavy distillate of the present invention.
It is preferred that the first gas for obtaining are carried out into removal of impurities purification and concentration, and will obtain after concentration
Hydrogen-rich gas is introduced to carry out hydrogenation reaction in follow-up fixed bed hydrogenation processing meanss.
Cyclone hydraulic separators can be directly entered by the isolated heavy distillate to separate, it is also possible to
First it is depressured, enters back in cyclone hydraulic separators separated after pressure reduction.
It is preferred that the solid content in the low density fraction oil of the lean solid content component is not higher than 0.5 weight %；
It is preferred that the range of solid content in the high density tail oil of the rich solid content component is 5-50 weight %, more preferably
For 10-40 weight %.
Slurry bed system can be obtained after oil mixes with the low density fraction by first light ends are oily
The feedstock oil of hydrotreater, into follow-up fixed bed hydrogenation processing meanss, the slurry bed hydroprocessing
Solid content is less than 200ppm in the feedstock oil of processing meanss, and Ni+V is not more than 80ppm, asphalt content
No more than 5 weight %.
To the species of the fixed bed hydrogenation processing meanss, there is no particular limitation, those skilled in the art's energy
It is enough to adopt conventional use of various fixed bed hydrogenation processing meanss in the art.
The no spy of concrete operation method of the hydrogenation reaction to carrying out in the fixed bed hydrogenation processing meanss
Different restriction, can be conventional use of various concrete operation methods in the art.
To the actual conditions that is fractionated the hydrogenation reaction product for obtaining, there is no particular limitation, as long as energy
It is enough to cause to obtain second gas, the second light ends oil and hydrogenation tail oil by the fractionation.This
The cut point of the oily and described hydrogenation tail oil of bright preferably described second light ends is 330-380 DEG C.
The paste state bed reactor inner chamber is the inner space being made up of paste state bed reactor housing.
It is preferred that gas (hydrogen) is anti-into slurry bed system from the air inlet positioned at paste state bed reactor housing bottom
In answering the reaction mass of device inner chamber, cause reaction mass that relative motion is carried out in paste state bed reactor inner chamber
The carrying out reacted in so as to be conducive to paste state bed reactor.
It is preferred that the cyclone hydraulic separators include spin liquid separator entrance, cyclone hydraulic separators inner chamber, gaseous phase outlet,
Product oil export and underflow pipe.Material is entered in cyclone hydraulic separators inner chamber by spin liquid separator entrance and utilized
The centrifugal force of itself is separated, and isolated gas gas-phase objects lead to the spinning liquid point from the gaseous phase outlet
Outside device, the less component of isolated solid content is from the product oil export positioned at cyclone hydraulic separators top
Lead to outside the cyclone hydraulic separators, the larger component of isolated solid content is from positioned at rotary filter press
The underflow pipe of device bottom is led to outside the cyclone hydraulic separators.
A kind of preferred embodiment of the invention, cyclone hydraulic separators of the present invention is as schemed
Shown in 1, specifically：
The cyclone hydraulic separators include spin liquid separator entrance 4, cyclone hydraulic separators inner chamber 2, gaseous phase outlet 5,
Product oil export 10 and underflow pipe 6.Material enters cyclone hydraulic separators inner chamber by spin liquid separator entrance 4
Centrifugal force in 2 using itself is separated, and isolated gas gas-phase objects lead to from the gaseous phase outlet 5
Outside the cyclone hydraulic separators, the less component of isolated solid content is from positioned at cyclone hydraulic separators top
Product oil export 10 is led to outside the cyclone hydraulic separators, the larger component of isolated solid content
Lead to outside the cyclone hydraulic separators from the underflow pipe 6 positioned at cyclone hydraulic separators bottom.
It is preferred that the cyclone hydraulic separators is arranged on beyond the paste state bed reactor inner chamber, the heavy end
Oil is introduced to be separated in cyclone hydraulic separators inner chamber from spin liquid separator entrance, and isolated is described low
Density distillate is led in the fixed bed hydrogenation processing meanss from the product oil export of cyclone hydraulic separators,
The isolated high density tail oil is drawn from the underflow pipe of the cyclone hydraulic separators bottom, and by institute
State high density tail oil to loop back in the paste state bed reactor inner chamber, preferably get rid of outside the tail oil of part.
The paste state bed reactor is any suitable reactor in slurry bed system hydrocracking heavy oil.It is preferred that
Ground, is provided with so that the reaction mass is in the paste state bed reactor inner chamber in the paste state bed reactor
In carry out the sleeve of interior circulation, the bottom of the sleeve is by the way that internal diameter is less than the sleeve diameter and stretches into institute
The conduit for stating sleeve inner is connected with the air inlet on paste state bed reactor housing, and the hydrogen is by described
Air inlet is introduced to successively in the conduit and the sleeve.By arranging the sleeve, and hydrogen from
The air inlet is entered in the sleeve so that the Gas content in reaction mass in sleeve substantially compares sleeve
Gas content in outer reaction mass is high, so as to promote the reaction mass in sleeve to move upwards, and covers
Reaction mass outside cylinder is moved relatively downward, so forms interior circulation in paste state bed reactor inner chamber, is promoted
Reacting to each other between gas in reaction mass, solid, liquid three-phase is entered such that it is able to improve reaction efficiency.
The internal diameter for requiring the conduit of guiding hydrogen is in order that the slurry less than the internal diameter of the sleeve
Reaction mass in bed reactor inner chamber can be entered in the sleeve from the bottom of the sleeve.Therefore,
Those skilled in the art can determine therefrom that the ratio of the internal diameter of the conduit and the sleeve.
The sleeve is one or at least two, at least the conduit of the lower cartridge of two and institute
State and be provided between air inlet gas distributor；The hydrogen is introduced to successively described by the air inlet
In gas distributor, the conduit and the sleeve.Being disposed to of the gas distributor can make
The hydrogen that must be entered in the paste state bed reactor inner chamber can be distributed more uniformly across, hydrogen Jing gases point
Cloth device is evenly distributed to each built-in sleeve bottom, and the gas distributor herein is dispersed into hydrogen little
Bubble, the bubble in each sleeve is moved up, and the Gas content in sleeve is contained more than the gas outside sleeve
Amount.By the difference of fluid density inside and outside sleeve, pressure reduction is formed in certain vertical distance range, should
Pressure reduction promotes sleeve outer fluid to flow downward, and the fluid flows upward in sleeve is thusly-formed interior circulation.
That what is reacted in so as to be conducive to paste state bed reactor inner chamber is efficiently carried out.
Preferably, the length of the sleeve is the 2/5 to 4/5 of the length of the paste state bed reactor inner chamber.
The length of the paste state bed reactor inner chamber can with the ratio of the internal diameter of the paste state bed reactor inner chamber
Think 5-20：1；Preferably 8-15：1.
Preferably, the internal diameter of the paste state bed reactor inner chamber is 50-6000mm, more preferably
300-5000mm。
Preferably, the internal diameter of the sleeve be the internal diameter of the paste state bed reactor inner chamber 1/100 to
3/4。
Preferably, the length that the conduit stretches into the sleeve inner is the 1/1000 of the length of the sleeve
To 1/10.
A kind of preferred embodiment of the invention, paste state bed reactor of the present invention is such as
Shown in Fig. 3, specifically, the paste state bed reactor includes：
Reactor shell 1, the bottom of the reactor shell is provided with unloads agent mouth 12, air inlet 11 and original
Material oil-in 14, the top of the reactor shell is provided with gas outlet 9, adds agent mouth 13, discharging opening 15；
The inner space of the reactor shell 1 constitutes reactor inner chamber 8 and (is alternatively referred to as slurry herein
Bed reactor inner chamber).The bottom of the reactor inner chamber 8 is provided with so that reaction mass is in the reactor
The sleeve 3 of interior circulation is carried out in inner chamber 8, the bottom of the sleeve 3 is less than in the sleeve by internal diameter
Footpath and stretch into the conduit of the sleeve inner and connect with the air inlet 11 of the reactor shell 1.Also,
The sleeve 3 is 1 or at least two, and the cyclone hydraulic separators is set to 1 grade, the institute of lower cartridge
State and gas distributor 7 is provided between conduit and the air inlet 11.
It is preferred that the condition of control hydrocracking reaction so that the heavy distillate accounts for paste state bed reactor and enters
40-60 weight % of material (i.e. inferior feedstock oil).
It is preferred that the heavy distillate is tangentially entered from spin liquid separator entrance, flow rate exists
Between 5-15m/s, preferably between 7-12m/s, rotary motion is formed in cyclone hydraulic separators, relied on
Centrifugal force is separated to the heavy distillate.
The method of the present invention is applied to the condition of conventional use of hydrocracking reaction in the art, but special
Not, the condition of the hydrocracking reaction of the invention relatively relaxes, the preferred hydrocracking reaction
Condition includes：Pressure is 10-30MPa；Temperature is 380-450 DEG C；Volume space velocity is 0.1-2.0h during liquid-1,
Hydrogen to oil volume ratio is 200-5000.The condition of the more preferably hydrocracking reaction includes：Pressure is
18-25MPa；Temperature is 410-440 DEG C；Volume space velocity is 0.2-1.0h during liquid-1, hydrogen to oil volume ratio is
1000-2500。
It is described in terms of the tenor in the hydrogenation catalyst relative to inferior feedstock oil described in every g
The consumption of hydrogenation catalyst can be 0.05-5 weight %, preferably 0.1-3 weight %.
Preferably, in a first aspect, hydrogenation catalyst of the present invention can be high-dispersion nano level support type
Catalyst, the hydrogenation catalyst includes carrier and metal active constituent, and the metal active constituent is selected from
At least one in nano level Mo, Ni, Co and V, the carrier is coal dust, activated carbon, graphite
With at least one carbon-based material in carbon black；It is preferred that
In the hydrogenation catalyst, the average grain diameter of the metal active constituent is 10-100nm, excellent
Elect 20-50nm as；More preferably
In the hydrogenation catalyst, the average grain diameter of the carrier is 20-200 μm, preferably
50-120μm。
According to described in a first aspect, in the hydrogenation catalyst, the specific surface area of the carrier is
50-1000m2/ g, preferably 300-800m2/g；It is preferred that
In the hydrogenation catalyst, the aperture of the carrier is 2-100nm, preferably 3-50nm；More
Plus preferably
The average grain diameter of the carrier of the hydrogenation catalyst is 60-100 μm.
Preferably, second aspect, containing carrier and active metallic element in hydrogenation catalyst of the present invention,
The carrier includes silica-alumina and aluminum oxide, and the active metallic element includes iron, calcium and molybdenum,
The catalyst is microspheric, and average grain diameter is 20-200 μm；Preferably 50-120 μm；More preferably
For 60-100 μm.
According to the second aspect, with the gross weight meter of the catalyst, the active metallic element is with oxygen
The content of compound meter is 10-40 weight %；It is preferred that
With the gross weight meter of the hydrogenation catalyst, the content of calcium and molybdenum in terms of oxide is respectively 0.1-1
Weight % and 5-10 weight %.
The carrier of hydrogenation catalyst has abundant pore structure and larger specific surface area, one side active metal
High degree of dispersion can be obtained on its surface, improve the reactivity of hydrogenation catalyst；On the other hand, it is bad
The macromoleculars such as asphalitine and colloid in matter feedstock oil can be entered inside carrier duct, with hydrogenation catalyst
Agent is spread in reaction system inner height, prevents the aggregation of green coke presoma, reduces the generation of coke.
There is no particular limitation for preparation method of the method for the present invention to the hydrogenation catalyst, can adopt
Conventional use of such as infusion process in the art etc. is prepared, and the present invention will not be described here.
Hydrogenation catalyst be well mixed with inferior feedstock oil after together be hydrogenated with into paste state bed reactor
Cracking reaction, after reaction system balance, from the high density tail oil portion that the hydrocyclone underflow pipe flows out
Reaction system is exceptionally thrown away, the portion in paste state bed reactor hydrocracking reaction system is removed with given pace
Divide the hydrogenation catalyst of inactivation, while fresh hydrogenation catalyst is supplemented in raw material by phase same rate, make
Obtain the catalyst content in the paste state bed reactor to be maintained in the aforementioned range of the present invention.
The relative density of the inferior feedstock oil of the present invention is larger, the macromolecular such as colloid and asphalitine, sulphur
Nitrogen heteroatom and tenor are high.
In the present invention, it is preferred to the inferior feedstock oil be Atmospheric vacuum residual oil, de-oiled asphalt, high aromatic oil,
At least one in heavy crude, super heavy crude, oil-sand, bitumen, shale oil and coal tar.
More preferably the inferior feedstock oil is Atmospheric vacuum residual oil, de-oiled asphalt, high aromatic oil, heavy original
At least one in oil, super heavy crude, oil-sand, bitumen, shale oil and coal tar.
More preferably the inferior feedstock oil is de-oiled asphalt and/or high aromatic oil.
The particularly preferably inferior feedstock oil is de-oiled asphalt and high aromatic oil, the de-oiled asphalt and described
The weight ratio of high aromatic oil can be 0.1-10：1.
The high aromatic oil can be in ethylene bottom oil, catalytic cracking recycle oil and catalytic cracked oil pulp
Plant or several, 350 DEG C of initial boiling point ＞, wherein arene content are generally higher than 80 weight %.
It is preferred that containing hydrotreating catalyst in the fixed bed hydrogenation processing meanss, the hydrotreating is urged
Agent refers to residuum hydrogenating and metal-eliminating, hydrodesulfurization, hydrodenitrogeneration and is hydrocracked the catalysis of function
Agent series.
It is preferred that the hydrotreating catalyst include as carrier Woelm Alumina and be supported on the load
At least one active metallic element in vib, VIIB races and group VIII on body.
Specifically, the active metallic element in the hydrotreating catalyst can be molybdenum, tungsten, cobalt, nickel
In one or more, the grading method of the hydrotreating catalyst is preferably so that the fixed bed hydrogenation
Reaction stream in processing meanss passes sequentially through Hydrodemetalation catalyst, Hydrobon catalyst, hydrogenation
Denitrification catalyst and hydrocracking catalyst.
In a particular embodiment, those skilled in the art can be according to the property of feedstock oil and slurry bed system
The hydrogenation result of reactor, adjusts at the process conditions and hydrogenation therein in fixed bed hydrogenation processing meanss
The loadings and level of reason catalyst match somebody with somebody mode.
It is preferred that the condition of hydrogenation reaction is carried out in the fixed bed hydrogenation processing meanss including：Hydrogen dividing potential drop is
8-15MPa；Temperature is 350-410 DEG C；Volume space velocity is 0.2-1.0h during liquid-1；Hydrogen to oil volume ratio is
200-1000。
The second light ends oil resulting during in the present invention hydrogenation reaction product for obtaining is fractionated
Preferably include gasoline fraction and diesel oil distillate.
The cut point of more preferably described gasoline fraction and the diesel oil distillate is 180 DEG C.
Especially, the hydrogenation tail oil and the cut point of second light ends oil can be 350 DEG C.
A kind of preferred embodiment of the invention, the present invention the inferior feedstock oil it is light
Qualitative method is carried out according to the process chart shown in Fig. 2, specifically：
Force (forcing) pump 2a will be passed sequentially through including the reaction mass of inferior feedstock oil and hydrogenation catalyst 1a and change
Hot device 3a is introduced in paste state bed reactor 4a carries out hydrocracking reaction, obtains being hydrocracked mixture；
By it is described be hydrocracked mixture and be introduced in the first hot high score 5a separated, obtain first gas,
One light ends oil and the heavy distillate containing hydrogenation catalyst；The heavy distillate is introduced into spinning liquid
Separated in separator 6a, obtained the low density fraction oil and rich solid content component of lean solid content component
High density tail oil 11a, and obtain hydrogen 7a to be clean, the hydrogen 7a to be clean rich in hydrogen
Loop back in reaction system as recycle hydrogen 14a and fresh hydrogen 15a after separated removal of impurities；Then will be described
The oily introducing in fixed bed hydrogenation processing meanss 8a with first light ends oil of low density fraction carries out adding
Hydrogen react, and the hydrogenation reaction product for obtaining is introduced into successively in the second hot high score 9a separated and
It is introduced in destilling tower 10a and is fractionated, obtains second gas, the second light ends oil and hydrogenation tail oil；
And a part for the high density tail oil is looped back into paste state bed reactor inner chamber as recycle oil 12a
In, and the high density tail oil of remainder is carried out into outer getting rid of as oily 13a is got rid of outward.
Specifically, the method for the present invention has the advantage that：
1st, using paste state bed reactor mild hydrogenation technique, can by de-oiled asphalt, catalytic cracked oil pulp,
Metal and/or asphalitine in the inferior feedstock oil such as catalytic cracking recycle oil and ethylene bottom oil is sloughed so as to full
The requirement of foot fixed bed residual hydrogenation charging, expands the raw material sources of fixed bed residual hydrogenation；
2nd, de-oiled asphalt is the peptization system of a complexity, compared with common decompression residuum, drip therein
The dispersion phase molecule such as blue or green matter condenses Du Genggao, and polarity is higher, and content is more, and the continuous phase content such as colloid
It is relatively low, thus be inclined to higher coking；The introducing of high aromatic oil, on the one hand can be efficient with its solution
Processing problems, it is often more important that improve the relative stability of de-oiled asphalt system, prevent green coke presoma
Existence, so as to effectively inhibit paste state bed reactor hydrogenation process in coke generation, extend device
Cycle of oparation；
3rd, paste state bed reactor hydrogenation process only sloughs the metal in charging using the operating condition for relaxing
And asphalitine, and do not pursue cracking conversion rate, so as to reduce paste state bed reactor during coke life
Into, it is ensured that the property of heavy distillate；
4th, the useless hydrotreating in fixed bed hydrogenation processing meanss can be used in paste state bed reactor
Catalyst, advantageously reduces the running cost of device, increases economic benefit；
5th, heavy distillate is separated using cyclone hydraulic separators, it is ensured that most hydrogenation catalysts enter
In entering high density tail oil, it is to avoid its bed blockage problem caused into fixed bed hydrogenation processing meanss；
6th, the present invention is realized by the circulation by high density tail oil in slurry bed system hydrotreater
The full conversion of inferior raw material, except arrange outside a small amount of waste residue, do not produce reluctant tail oil inferior, have
Resource utilization is high, eco-friendly advantage.
Hereinafter will be described the present invention by embodiment.
From de-oiled asphalt A and Zhenghai catalytic cracked oil pulp as inferior feedstock oil, specific property such as table
Shown in 1.
In the case where contrary explanation is not made, the gas for using and the volumetric quantities of liquid are 25 DEG C and 1
The numerical value of individual normal atmosphere pressure.
Table 1
| De-oiled asphalt A | Zhenghai slurry oil | |
| Softening point/DEG C | 165 | — |
| (carbon residue)/weight % | 46 | 9.68 |
| (asphalitine)/weight % | 41.9 | 4.1 |
| (S)/weight % | 10.9 | 1.0 |
| (N)/weight % | 0.29 | 0.22 |
| (Ni+V)/(μg/g) | 430 | 19.8 |
Embodiment 1-7 is used for the lightening method of the inferior feedstock oil for illustrating the present invention.
Embodiment 1-3
Hydrogenation catalyst used in embodiment 1-3 is identical, is Mo system supported catalysts, specifically
Consist of：In terms of active metal, Mo (average grain diameter is 45nm) content is 10 weight %, and remaining is
Carrier active carbon, the average grain diameter of hydrogenation catalyst is 100 μm.
It is described in terms of the tenor in the hydrogenation catalyst relative to inferior feedstock oil described in every g
The consumption of hydrogenation catalyst is as shown in table 2.
Inferior feedstock oil used in embodiment 1-3 is identical, is weight ratio for 7：3 de-oiled asphalt A
With Zhenghai catalytic cracked oil pulp.
Test fixed bed hydrogenation processing meanss used in embodiment 1-3 to add for single reactor small fixed
Hydrogen production device, loads successively guard catalyst, catalyst for demetalation, desulphurization catalyst and denitrification catalyst,
The trade mark of hydrotreating catalyst used is followed successively by RG-20A, RDM-2B, RMS-1 and RSN-2,
By the production of sinopec Chang Ling catalyst plant；The admission space ratio of 4 kinds of catalyst is 5：30：20：45.
The concrete grammar of embodiment 1-3 is：
Aforementioned inferior feedstock oil, hydrogenation catalyst and hydrogen are introduced in paste state bed reactor to carry out hydrogenation and splits
Change reaction, hydrocracking reaction condition as shown in table 2, obtains being hydrocracked mixture；Add described
Hydrogen cracking compounds temperature be 300 DEG C, pressure be 20MPa under the conditions of carry out flash separation, obtain the
One gas, the first light ends oil and the heavy distillate containing hydrogenation catalyst, by the heavy end
Oil is introduced in cyclone hydraulic separators and is separated, and the low density fraction oil and richness for obtaining lean solid content component contains admittedly
The high density tail oil of amount component, wherein, speed V of the heavy distillate at spin liquid separator entrance,
The solid content of low density fraction oil and the solid content of high density tail oil are as shown in table 2 respectively；Then by institute
State low density fraction oil and introduce solid as fixed bed hydrogenation processing meanss feedstock oil with the first light ends oil
Hydrogenation reaction, the property of the fixed bed hydrogenation processing meanss feedstock oil are carried out in fixed bed hydrotreater
3 are shown in Table, the condition of hydrogenation reaction as shown in table 4, and the hydrogenation reaction product for obtaining is fractionated,
Obtain second gas, the second light ends oil and hydrogenation tail oil；And loop back the high density tail oil
In paste state bed reactor inner chamber.
Paste state bed reactor and cyclone hydraulic separators used in embodiment 1-3 is respectively identical, and structure point
Not as shown in Fig. 3 and Fig. 1.
Specifically, the length of sleeve is the 3/5 of the length of paste state bed reactor inner chamber；
The internal diameter of sleeve is 300mm.
The internal diameter of reactor inner chamber is 5000mm.
It is 200mm that the conduit stretches into the length of the sleeve inner.
The length of underflow pipe is 100mm.
The length of the paste state bed reactor inner chamber is with the ratio of the internal diameter of the paste state bed reactor inner chamber
10：1.
The volume of cyclone hydraulic separators is 1 with the ratio of the volume of paste state bed reactor inner chamber：600.
The Mean Speed that flow downward of the reaction mass in paste state bed reactor inner chamber outside sleeve be
0.2m/s。
Speed of the reaction mass in the entrance through the cyclone hydraulic separators is 8m/s.
Table 2
Table 3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Density (20 DEG C)/(g/cm3) | 0.958 | 0.953 | 0.940 |
| (carbon residue)/weight % | 8.2 | 7.7 | 6.4 |
| (S)/weight % | 3.1 | 2.9 | 1.8 |
| (N)/weight % | 0.12 | 0.08 | 0.06 |
| (Ni+V)/(μg/g) | 54.0 | 48.2 | 30.7 |
| (four components)/weight % | |||
| Saturated hydrocarbons | 18.6 | 18.7 | 26.4 |
| Aromatic hydrocarbons | 57.4 | 59.6 | 60.4 |
| Colloid | 19.2 | 17.5 | 14.2 |
| Asphalitine | 4.8 | 4.2 | 2.8 |
Table 4
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Reaction condition | |||
| Pressure/MPa | 15 | 14.0 | 15 |
| Temperature/DEG C | 390 | 400 | 400 |
| Volume space velocity/h during liquid-1 | 0.2 | 0.2 | 0.5 |
| Hydrogen to oil volume ratio | 600 | 800 | 600 |
| Product slates/weight % | |||
| Second gas (C1-C4) | 1.21 | 2.83 | 0.85 |
| Gasoline fraction (C5-180℃) | 13.01 | 14.1 | 12.78 |
| Diesel oil distillate (180-350 DEG C) | 17.88 | 19.88 | 15.35 |
| Hydrogenation tail oil (350 DEG C of ＞) | 68.57 | 64.59 | 71.98 |
| The property of hydrogenation tail oil | |||
| (Ni+V)/(μg/g) | 19.68 | 13.42 | 11.52 |
| (carbon residue)/weight % | 4.42 | 3.45 | 3.55 |
Embodiment 4-5
Embodiment 4-5 carries out hydrocracking reaction using method same as Example 2, except that,
Differ in reaction temperature in the fixed bed hydrogenation processing meanss and embodiment 2, it is concrete such as table 5
Shown in.
Table 5
| Embodiment 4 | Embodiment 5 | |
| Reaction condition | ||
| Pressure/MPa | 14.0 | 14.0 |
| Temperature/DEG C | 390 | 410 |
| Volume space velocity/h during liquid-1 | 0.2 | 0.2 |
| Hydrogen to oil volume ratio | 800 | 800 |
| Product slates/weight % | ||
| Second gas (C1-C4) | 2.18 | 3.24 |
| Gasoline fraction (C5-180℃) | 13.4 | 16.35 |
| Diesel oil distillate (180-350 DEG C) | 18.58 | 21.42 |
| Hydrogenation tail oil (350 DEG C of ＞) | 66.48 | 60.73 |
| Hydrogenation tail oil property | ||
| (Ni+V)/(μg/g) | 18.13 | 9.52 |
| (carbon residue)/weight % | 4.29 | 3.17 |
Can be seen that with the rising of reaction temperature from the result of embodiment 2, embodiment 4 and embodiment 5,
Hydrogenation tail oil yield is reduced, while the property of hydrogenation tail oil improves, can be split as the heavy-oil catalytic of high-quality
Change raw material.
Embodiment 6-7
The present embodiment carries out hydrocracking reaction using inferior feedstock oil and device same as Example 1,
Except that, the average grain diameter of the hydrogenation catalyst for using is 80 μm, and wherein active component is with oxygen
The content of compound meter is respectively Fe relative to the gross weight of the hydrogenation catalyst：25 weight %, Mo：
10 weight %, Ca：1 weight %.Specific reaction condition is as shown in table 6.
Table 6
| Embodiment 6 | Embodiment 7 | |
| Reaction condition | ||
| Pressure/MPa | 18 | 18 |
| Temperature/DEG C | 430 | 440 |
| Hydrogenation catalyst consumption/μ g/g | 2000 | 2000 |
| Volume space velocity/h during liquid-1 | 0.2 | 0.2 |
| Hydrogen to oil volume ratio | 1500 | 1500 |
| Reaction result/weight % | ||
| First gas yield | 8.07 | 8.45 |
| Slurry bed system generates oil yield | 81.29 | 83.54 |
| High density tail oil yield | 10.51 | 7.96 |
| Coking yield | 1.43 | 1.85 |
| V/m/s | 8 | 8 |
| Solid content | ||
| Low density fraction oil/μ g/g | 25.68 | 23.15 |
| High density tail oil/weight % | 7.6 | 10.03 |
Comparative example 1-3
The hydrocracking reaction of comparative example 1-3 is corresponding with the hydrocracking reaction condition of embodiment 1-3 respectively
It is identical, and inferior feedstock oil is identical, comparative example 1-3 is respectively adopted and embodiment 1-3 identical slurry bed system
Reactor carries out hydrocracking reaction, and the liquid product to obtaining after paste state bed reactor reaction steams
Cutting is evaporated, and does not adopt cyclone hydraulic separators of the present invention to be separated, the product that distillation cutting is obtained
The property of distillate is shown in Table 7.Although product cut oil disclosure satisfy that the requirement that fixed bed feeds, and produce
The yield of product is relatively low, increased the load of paste state bed reactor, also increases production cost.
The cut oil yield wherein in table 7 is referred to can enter follow-up fixed bed hydrogenation hydrotreating
The yield of the oil phase of device.
Table 7
| Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Reaction condition | |||
| Pressure/MPa | 18 | 20 | 22 |
| Temperature/DEG C | 420 | 420 | 420 |
| Hydrogenation catalyst consumption/μ g/g | 800 | 1000 | 2000 |
| Volume space velocity/h during liquid-1 | 0.2 | 0.5 | 1.5 |
| Hydrogen to oil volume ratio | 1500 | 1500 | 2000 |
| Reaction result/weight % | |||
| Gas recovery ratio (C1-C4) | 6.02 | 8.07 | 5.43 |
| Cut oil yield (IBP-500 DEG C) | 69.05 | 72.29 | 76.45 |
| Yield of residual oil | 24.26 | 19.71 | 19.74 |
| Coking yield | 1.62 | 1.43 | 0.78 |
It can be seen from the results above that the said method provided using the present invention can efficiently by including de-
Oil asphalt and/or high aromatic component (ethylene bottom oil, catalytic cracking recycle oil and catalytic cracked oil pulp etc.) exist
Interior inferior feedstock oil is converted into light ends oil.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the present invention, can be to the technical side of the present invention
Case carries out various simple variants, and these simple variants belong to protection scope of the present invention.
It is further to note that each particular technique described in above-mentioned specific embodiment is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, the present invention is no longer separately illustrated to various possible combinations.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as its
Without prejudice to the thought of the present invention, it should equally be considered as content disclosed in this invention.
Claims (15)
1. a kind of lightening method of inferior feedstock oil, the method includes：Will including inferior feedstock oil,
The reaction mass of hydrogenation catalyst and hydrogen is introduced in paste state bed reactor carries out hydrocracking reaction, obtains
It is hydrocracked mixture；The mixture that is hydrocracked is separated, first gas, first light are obtained
Matter distillate and the heavy distillate containing hydrogenation catalyst；The heavy distillate is introduced into rotary filter press
Separated in device, obtained the low density fraction oil of lean solid content component and the high density of rich solid content component
Tail oil；Then the oily fixed bed hydrogenation that introduces oily with first light ends of the low density fraction is processed
Hydrogenation reaction is carried out in device, and the hydrogenation reaction product for obtaining is fractionated, obtain second gas,
Second light ends oil and hydrogenation tail oil；And the high density tail oil is looped back in paste state bed reactor
In chamber.
2. method according to claim 1, wherein, the cyclone hydraulic separators is arranged on the slurry
Beyond state bed reactor inner chamber, the heavy distillate is introduced to cyclone hydraulic separators from spin liquid separator entrance
Separated in inner chamber, the oily product oil export from cyclone hydraulic separators of the isolated low density fraction
In leading to the fixed bed hydrogenation processing meanss, the isolated high density tail oil is from rotary filter press
The underflow pipe of device bottom is drawn and is looped back in the paste state bed reactor inner chamber.
3. method according to claim 1, wherein, being provided with the paste state bed reactor makes
Obtain the reaction mass carries out the sleeve of interior circulation in the paste state bed reactor inner chamber, the sleeve
Bottom is less than the sleeve diameter and stretches into the conduit and the slurry bed system of the sleeve inner by internal diameter
Air inlet connection on the housing of reactor, the hydrogen is introduced to successively described leading by the air inlet
In pipe and the sleeve.
4. method according to claim 3, wherein, the sleeve is one or at least two,
Gas distributor is provided between the conduit and the air inlet of at least lower cartridge of two；
The hydrogen is introduced to successively the gas distributor, the conduit and the sleeve by the air inlet
In.
5. the method according to claim 3 or 4, wherein, the length of the sleeve is the slurry
The 2/5 to 4/5 of the length of state bed reactor inner chamber；It is preferred that
The internal diameter of the paste state bed reactor inner chamber is 50-6000mm, more preferably
300-5000mm。
6. the method according to any one in claim 3-5, wherein, the internal diameter of the sleeve
For the 1/100 to 3/4 of the internal diameter of the paste state bed reactor inner chamber；It is preferred that
The conduit stretches into the 1/1000 to 1/10 of the length that the length of the sleeve inner is the sleeve.
7. the method according to any one in claim 1-6, wherein, it is described be hydrocracked it is anti-
The condition answered includes：Pressure is 10-30MPa；Temperature is 380-450 DEG C；Volume space velocity is during liquid
0.1-2.0h-1, hydrogen to oil volume ratio is 200-5000：1；It is preferred that
The condition of the hydrocracking reaction includes：Pressure is 18-25MPa；Temperature is 410-440 DEG C；
Volume space velocity is 0.2-1.0h during liquid-1, hydrogen to oil volume ratio is 1000-2500：1.
8. the method according to any one in claim 1-6, wherein, relative to described in every g
Inferior feedstock oil, in terms of the tenor in the hydrogenation catalyst, the consumption of the hydrogenation catalyst is
0.05-5 weight %, preferably 0.1-3 weight %.
9. the method according to any one in claim 1-6, wherein, the hydrogenation catalyst
For high-dispersion nano level loaded catalyst, the hydrogenation catalyst includes carrier and metal active constituent,
At least one of the metal active constituent in nano level Mo, Ni, Co and V, the carrier
At least one carbon-based material in for coal dust, activated carbon, graphite and carbon black；It is preferred that
In the hydrogenation catalyst, the average grain diameter of the metal active constituent is 10-100nm, excellent
Elect 20-50nm as；More preferably
In the hydrogenation catalyst, the average grain diameter of the carrier is 20-200 μm, preferably
50-120μm。
10. method according to claim 9, wherein, in the hydrogenation catalyst, the load
The specific surface area of body is 50-1000m2/ g, preferably 300-800m2/g；It is preferred that
In the hydrogenation catalyst, the aperture of the carrier is 2-100nm, preferably 3-50nm；More
Plus preferably
The average grain diameter of the carrier of the hydrogenation catalyst is 60-100 μm.
11. methods according to any one in claim 1-6, wherein, the hydrogenation catalyst
In containing carrier and active metallic element, the carrier includes silica-alumina and aluminum oxide, described
Active metallic element includes iron, calcium and molybdenum, and the hydrogenation catalyst is microspheric, and average grain diameter is
20-200μm；Preferably 50-120 μm；More preferably 60-100 μm.
12. methods according to claim 11, wherein, with the gross weight of the hydrogenation catalyst
Meter, the content that the active metallic element is counted with oxide is as 10-40 weight %；It is preferred that
With the gross weight meter of the hydrogenation catalyst, the content of calcium and molybdenum in terms of oxide is respectively 0.1-1
Weight % and 5-10 weight %.
13. methods according to any one in claim 1-6, wherein, the inferior feedstock oil
For Atmospheric vacuum residual oil, de-oiled asphalt, high aromatic oil, heavy crude, super heavy crude, oil-sand, natural
At least one in pitch, shale oil and coal tar；It is preferred that
The inferior feedstock oil is de-oiled asphalt and high aromatic oil, the de-oiled asphalt and the high aromatic oil
Weight ratio be 0.1-10：1.
14. methods according to any one in claim 1-6, wherein, the fixed bed hydrogenation
Contain hydrotreating catalyst in processing meanss, the hydrotreating catalyst includes the porous as carrier
Aluminum oxide and load on the carrier in vib, VIIB races and group VIII extremely
A kind of few active metallic element；It is preferred that
In the hydrotreating catalyst, the active metallic element is in molybdenum, tungsten, cobalt and nickel
It is at least one.
15. methods according to any one in claim 1-6, wherein, the fixed bed hydrogenation
The condition of hydrogenation reaction is carried out in processing meanss to be included：Hydrogen dividing potential drop is 8-15MPa；Temperature is
350-410℃；Volume space velocity is 0.2-1.0h during liquid-1；Hydrogen to oil volume ratio is 200-1000.
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| CN110813295A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | Preparation method and application of slurry bed hydrogenation catalyst |
| CN111996034A (en) * | 2020-08-18 | 2020-11-27 | 胡友超 | Method for clean utilization of inferior heavy oil |
| CN112391200A (en) * | 2020-10-22 | 2021-02-23 | 中国科学院大连化学物理研究所 | Method for hydrogenating ethylene cracking tar |
| CN112771138A (en) * | 2018-09-26 | 2021-05-07 | 环球油品有限责任公司 | Process for making and using metal catalysts for slurry hydrocracking |
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| CN110813295A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | Preparation method and application of slurry bed hydrogenation catalyst |
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| CN111996034A (en) * | 2020-08-18 | 2020-11-27 | 胡友超 | Method for clean utilization of inferior heavy oil |
| CN112391200A (en) * | 2020-10-22 | 2021-02-23 | 中国科学院大连化学物理研究所 | Method for hydrogenating ethylene cracking tar |
| CN116162487A (en) * | 2021-11-25 | 2023-05-26 | 中国石化工程建设有限公司 | Method and system for hydrogenating heavy raw oil of liquid-phase non-hydrogen slurry bed |
| CN114045179A (en) * | 2021-11-30 | 2022-02-15 | 陕西延长石油（集团）有限责任公司 | Multiphase flow residual oil hydro-upgrading and catalytic cracking combined process and system |
| CN114292665A (en) * | 2021-12-13 | 2022-04-08 | 中国海洋石油集团有限公司 | Heavy oil modification method and heavy oil modification system |
| CN115475622A (en) * | 2022-08-24 | 2022-12-16 | 宁波中金石化有限公司 | Preparation method and application of slurry bed hydrogenation catalyst based on waste porcelain powder carrier |
| CN115475622B (en) * | 2022-08-24 | 2023-08-25 | 宁波中金石化有限公司 | Preparation method and application of slurry bed hydrogenation catalyst based on waste porcelain powder carrier |
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