CN105400545B - A kind of heavy oil separating method and its processing system - Google Patents
A kind of heavy oil separating method and its processing system Download PDFInfo
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Abstract
The invention provides a kind of heavy oil separating method and its processing system, the separation method is provided with the extraction tower of multiple packing sections using upper area, and distributor is provided between adjacent packing section, supercritical solvent from supercritical solvent recovery tower is introduced by distributor, the heavy constituent in the depitching oil phase on the extraction tower top is further separated.Heavy oil separating method of the present invention can effectively solve the inapparent problem of heavy oil feed separating effect in extraction separation process in prior art, so as to obtain the target product of high income, good properties.
Description
Technical field
The present invention relates to a kind of heavy oil separating method and its processing system, belong to Petroleum Processing Technology field.
Background technology
Solvent deasphalting is the technology for removing out by the heavy component Colophonium in petroleum heavy oil, it is adaptable to which exploitation is obtained
Mink cell focus, the various normal pressures obtained in oil sands bitumen and petroleum refining process and decompression residuum process, this kind of mink cell focus
Density (20 DEG C)>0.934g/cm3Or boiling point is higher than 350 DEG C.Deasphalted oil after removing Colophonium is mainly for the production of lubricating oil
Base oil as catalytic cracking or is hydrocracked (be not limited to) raw material of following process, and the Colophonium of removing can be dripped as road
Blue or green, building asphalt or gasified raw material etc..
Existing solvent deasphalting techniques mainly have two grades or three-stage process.In two grades of extraction separation processes, in first order mistake
Be divided into light, weight in journey after solvent and heavy oil feed mixing biphase, it is light phase to become depitching oil phase, by solvent and be dissolved it is de-
Coal tar (Deasphalted Oil-DAO) is constituted, and heavy phase is referred to as Colophonium phase, by de-oiled asphalt (Deoiled Asphalt-
DOA) and certain content solvent composition.Colophonium heat phase is to flash distillation removing wherein most solvent after higher temperature, then uses water
Steam strips residual solvent therein, obtains de-oiled asphalt.During the second level, depitching oil phase is heated in the near of solvent
Most solvents are reclaimed under critical or super critical condition, then obtain depitching after residual solvent therein being stripped with vapor
Oil；In three-level extraction separation process, one section of removing oil (glue again between aforementioned extraction tower and supercritical solvent recovery tower, is increased
Matter) knockout tower, from depitching oil phase heated intensification or the blood pressure lowering again of extraction tower, to reduce the solvability of solvent so as to
In removing oil again settle down in the separation of the second level, the frivolous oil phase of tower top enters supercritical tower recycling design, again removing oil phase
Stripping removes remaining solvent respectively again with frivolous oil phase, obtains so-called heavy removing oil (or claiming colloid) and frivolous oil.
According to the solvent de-asphalting process of prior art, either two grades or three-stage process, extraction tower and again removing oil point
Settlement separate effect served to raw material thing only from tower, and extraction tower and the top of removing oil knockout tower and the bottom temperature difference again
Very little, unobvious to the separating effect of heavy oil feed.Therefore, a kind of new heavy oil separating method how is developed, is had
The separating effect for improving mink cell focus of effect is always people's problem demanding prompt solution.
The content of the invention
Technical problem underlying solved by the invention is to provide a kind of heavy oil separating method and its processing system, this point
The inapparent problem of heavy oil feed separating effect in extraction separation process in prior art can effectively be solved from method,
So as to obtain the target product of high income, good properties.
The invention provides a kind of heavy oil separating method, is provided with the extraction tower of multiple packing sections using upper area, and
Distributor is provided between adjacent packing section, the supercritical solvent from supercritical solvent recovery tower is introduced by distributor, is made
Heavy constituent in the depitching oil phase on the extraction tower top is further separated, and the separation method includes：
Heavy oil feed is mixed in static mixer with main solvent, and from giving less than the region for being provided with packing section
Enter the extraction tower, the main solvent is 1.5-5.0 with the mass flowrate ratio of the heavy oil feed:1, and control blender
Temperature is 50-200 DEG C, and pressure is 3.0-10.0MPa；
Secondary solvent is passed through with main solvent mixed material entry zone from the extraction tower bottom and less than heavy oil feed
Distributor is sent in tower, and with the de-oiled asphalt phase counter current contacting isolated, the matter of the secondary solvent and the heavy oil feed
Amount flow rate ratio is 0.1-1.0:1；
Supercritical solvent is introduced in the extraction tower by the distributor between packing section, and with the depitching isolated
Oil phase contact mixing, the supercritical solvent are 0.1-1 with the mass flowrate ratio of the heavy oil feed:1；
The depitching oil phase that heavy oil feed is separated in the extraction tower is gone out from extraction tower top row, is separated
Deasphalted oil is collected, the de-oiled asphalt that extraction tower bottom is discharged mutually is stripped, solvent is isolated, and is collected de-oiled asphalt；
Wherein, extraction temperature 50-200 DEG C in extraction tower is controlled, pressure is 3.0-10.0MPa, and the tower top of extraction tower
Temperature is higher than 5-50 DEG C of column bottom temperature.
Above-mentioned heavy oil feed partition method be the second-order separation method, inventor research find：Heavy oil feed is being entered
Before extraction tower, which is carried out into premix process with main solvent, can effectively reduce the viscosity of heavy oil feed, be conducive to mink cell focus
Separating effect of the raw material in extraction tower.Additionally, upper area of the present invention in extraction tower is provided with multiple packing sections, Ke Yida
To the detached purpose of mono-tower multi-stage, the separating effect of heavy oil feed is effectively increased, while also improving depitching oil phase
Yield.At the same time, invention also uses supercritical solvent is to the Colophonium phase carried secretly in depitching oil phase and other heavy constituents
Eluting is carried out, it is achieved thereby that the purpose of idetified separation.Moreover, as the supercritical from supercritical solvent recovery tower is molten
The temperature of agent is higher, so as to thermograde is set up in extraction tower, is conducive to the extract and separate of heavy oil feed, is in particular in
Extraction tower head temperature is higher than bottom temp, and the temperature difference is between 5-50 DEG C.
For the second-order separation method of above-mentioned heavy oil feed, also comprise the steps：
The depitching oil phase that extraction tower top row is gone out and the mixture of solvent send into supercritical solvent recovery tower recycling design,
Make solvent be separated with deasphalted oil in the supercritical state, and the supercritical solvent for obtaining is returned into static mixer and extraction
Tower.
For the separation of heavy oil feed, the present invention can also be further to the deasphalted oil for obtaining by three-level partition method
Process, isolate removing oil phase again and frivolous oil phase, the property of depitching oil phase not only can be improved, while can also high degree
The frivolous oil phase of lifting yield.Thus, on the basis of heavy oil feed the second-order separation method of the present invention, can also include following
Step：
Mixture of the depitching oil phase isolated with solvent is gone out and is sent into removing oil knockout tower again, institute from extraction tower top row
State removing oil knockout tower upper area again and be provided between multiple packing sections, and adjacent packing section and be provided with distributor, supercritical is molten
Agent introduces the heavy removing oil knockout tower by the distributor between packing section；
The frivolous oil phase that depitching oil phase is separated in the heavy removing oil knockout tower is from removing oil knockout tower top row again
Go out, carry out separation and collect frivolous oil, the removing oil again that bottom of towe is discharged mutually is stripped, solvent is isolated, and is collected removing oil again；Institute
The mass flowrate ratio that supercritical solvent is stated with the heavy oil feed is 0.1-1:1, the tower top temperature of the heavy removing oil knockout tower
Higher than 5-50 DEG C of column bottom temperature, and to control the temperature of the heavy removing oil knockout tower be 50-200 DEG C, and pressure is 3.0-10.0MPa.
The present invention program can also be the three-level partition method for heavy oil feed, also comprise the steps：
The frivolous oil phase that removing oil knockout tower top row again is gone out and the mixture feeding supercritical solvent recovery tower of solvent, make molten
Agent in the supercritical state with frivolous separation of oil, and the supercritical solvent for obtaining is returned into static mixer, extraction tower and weight
Removing oil knockout tower.
In the specific embodiment of the present invention, the pressure of extraction tower described in the pressure ratio of the supercritical solvent recovery tower
High 0.1-1MPa, the temperature in the supercritical solvent recovery tower are higher 10-150 DEG C than the temperature in the extraction tower.
In the specific embodiment of the present invention, implement the bar of supercritical recovery solvent in the supercritical solvent recovery tower
Part is：Pressure 3.0-10.0MPa, temperature 94-280 DEG C, and reduced temperature Tr=T/TCBetween 0.992-1.20 (TC, iFor the critical temperature of solvent, xiFor each component molar fraction, T is supercritical tower temperature degree, TcIt is referred to as false
Critical temperature, temperature unit are K).
No matter separation method of the present invention to heavy oil feed, used setting filler using two grades or three-level partition method
The extraction tower of section and again removing oil knockout tower, the upper area filling 3-5 section packing sections in extraction tower and again removing oil knockout tower, its
Filler mode is random packing or structured packing, the specific surface area >=150m of filler2/m3, voidage >=0.95, and packing section it
Jian Fen 2-4 roads introduce supercritical solvent via distributor, keep each road solvent incoming direction identical, can up or down simultaneously.
The selection of filler can for example be Pall ring filler, ripple packing (orifice plate/calendering), Intalox metal tower packing, θ ring fillers etc..
Heavy oil feed used in the present invention includes the mink cell focus and oil sands bitumen, PETROLEUM PROCESSING mistake that oil exploitation obtains
The residual oil obtained in journey or the coal tar asphalt obtained during catalytic cracked oil pulp or Coal Chemical Industry, and the heavy oil feed
Density ＞ 0.934g/cm at 20 DEG C3Or boiling point is higher than 350 DEG C.
Main solvent used in the present invention, secondary solvent and supercritical solvent, are the convenience of production operation, can adopt
Identical solvent, such as key component can be C3-C5 alkane and cycloalkane, for example propane, normal butane, iso-butane, positive penta
Alkane, isopentane and Pentamethylene. or its mixture.
Present invention also offers the processing system of above-mentioned heavy oil separating method can be implemented, the processing system includes quiet
State blender, extraction tower, solvent tank and stripper；
The static mixer has main solvent import and heavy oil feed import and mixed material outlet, and main solvent enters
The mouth connection solvent tank, the material inlet of mixed material outlet extraction tower；
The extraction tower internal upper part is provided with multiple packing sections, and in the middle part of tower body, tower body bottom sets for mixed material import
There is secondary colvent inlet, so as to contact into the secondary solvent in tower with de-oiled asphalt realize extraction, tower internal upper part arranges packing section
Region be provided with supercritical solvent entrance and be communicated between adjacent packing section by distributor so that supercritical solvent extraction
Take Ta Nei to contact with deasphalted oil mixing, at the top of tower body, be provided with the outlet of depitching oil phase, tower body bottom is provided with de-oiled asphalt phase
Floss hole；
The de-oiled asphalt phase floss hole of the extraction tower bottom connects the stripper, so that the solvent in de-oiled asphalt phase
It is separated.
Further, the processing system also includes supercritical solvent recovery tower, the thing of the supercritical solvent recovery tower
Depitching oil phase outlet at the top of material import and extraction tower, the supercritical solvent outlet of the supercritical solvent recovery tower
Connect with the supercritical solvent entrance of static mixer and extraction tower, the supercritical solvent recovery tower bottom of towe is provided with deasphalted oil
Phase floss hole.
Further, the processing system also includes deasphalted oil stripper and de-oiled asphalt flash distillation stripper；
The depitching oil phase floss hole that the supercritical solvent recovery tower is isolated connects the deasphalted oil stripper
Material inlet, the solvent outlet of the deasphalted oil stripper pass through pipeline connection to the solvent tank；
The de-oiled asphalt phase floss hole of the extraction tower is communicated to the material inlet of the de-oiled asphalt flash distillation stripper, institute
The solvent outlet for stating de-oiled asphalt flash distillation stripper passes through pipeline connection to the solvent tank.
Further, the processing system also includes removing oil knockout tower again, and the heavy removing oil knockout tower upper area is provided with
Distributor is provided between multiple packing sections, and adjacent packing section, the region of tower body setting packing section is provided with supercritical solvent and enters
Mouth is simultaneously communicated between adjacent packing section by distributor, and the heavy removing oil knockout tower is set less than supercritical solvent entrance area
Depitching oil phase entrance, and the depitching oil phase outlet with extraction tower top are put, bottom of towe is provided with removing oil again and mutually exports.
Further, the processing system also includes supercritical solvent recovery tower, and the frivolous oil phase of removing oil knockout tower goes out again
Mouth is connected with the material inlet of the supercritical solvent recovery tower, the supercritical solvent outlet of the supercritical solvent recovery tower
Respectively with static mixer, extraction tower and the supercritical solvent entrance of removing oil knockout tower is connected again, the supercritical solvent is reclaimed
Tower bottom of towe is provided with frivolous oil phase floss hole.
Further, the processing system also includes frivolous oil and gas stripper, again removing oil stripper and de-oiled asphalt flash steam
Stripper；
The frivolous oil phase floss hole that the supercritical solvent recovery tower is isolated connects the material of the frivolous oil and gas stripper
Import, the solvent outlet of the frivolous oil and gas stripper pass through pipeline connection to the solvent tank；
The phase of the removing oil again floss hole that the heavy removing oil knockout tower is isolated connects the material inlet of the heavy removing oil stripper,
The solvent outlet of the heavy removing oil stripper is by pipeline connection to the solvent tank；
The de-oiled asphalt phase floss hole of the extraction tower is communicated to the material inlet of the de-oiled asphalt flash distillation stripper, institute
The solvent outlet for stating de-oiled asphalt flash distillation stripper passes through pipeline connection to the solvent tank.
In the heavy oil separating method of the present invention, installed additional by the upper area in the extraction tower and mink cell focus knockout tower
Multiple packing sections, and supercritical solvent is introduced by the distributor arranged between packing section, heavy oil feed is entered so as to reach
The detached purpose of row mono-tower multi-stage, effectively increases the separating effect of heavy oil feed.Moreover, due to molten from supercritical
The temperature of the supercritical solvent of agent recovery tower is higher, is introduced into and temperature ladder can be set up in extraction tower and again removing oil knockout tower
Degree, effectively solves the inapparent problem of heavy oil feed separating effect in extraction process in prior art, so as to obtain
The target product of high income, good properties.
Description of the drawings
Fig. 1 is the process chart of heavy oil feed the second-order separation method of the present invention.
Fig. 2 is the process chart of heavy oil feed three-level partition method of the present invention.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below in the embodiment of the present invention
Technical scheme is clearly and completely described, it is clear that described embodiment is a part of embodiment of the invention, rather than entirely
The embodiment in portion.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The every other embodiment for being obtained, belongs to the scope of protection of the invention.
The heavy oil feed that the present invention is adopted includes the mink cell focus and oil sands bitumen that oil exploitation obtains, petroleum refining process
In the dregs of fat that obtain or the coal tar asphalt obtained during catalytic cracked oil pulp, and Coal Chemical Industry, and the heavy oil feed
Density ＞ 0.934g/cm at 20 DEG C3Or boiling point is higher than 350 DEG C.
In a particular embodiment, the key component of main solvent used in the present invention, secondary solvent and supercritical solvent
The alkane and cycloalkane of C3-C5 can be, propane, normal butane, iso-butane, pentane, isopentane and Pentamethylene. is specifically as follows
Or its mixture.
First, the second-order separation method of mink cell focus, detailed process can be described as follows：
As shown in figure 1, static mixer 1 connects extraction tower 2, solvent tank 6 is connected with static mixer 1 by pipeline,
After main solvent is mixed into static mixer 1 with heavy oil feed, de-oiled asphalt phase and de- drip in sending into extraction tower 2, are isolated
Blue or green oil phase；Wherein, main solvent and the mass flowrate ratio of heavy oil feed are 1.5-5.0:1；The temperature for controlling static mixer 1 is
50-200 DEG C, pressure is 3.0-10.0MPa；
The tower body bottom of extraction tower 2 is provided with secondary colvent inlet, and the solvent in solvent tank 6 passes through pair of the pipeline from extraction tower 2
Colvent inlet mutually carries out counter-current extraction to de-oiled asphalt into extraction tower 2；Wherein, the mass flowrate of secondary solvent and heavy oil feed
Than for 0.1-1.0:1；Top in extraction tower 2 arranges the region of packing section and is provided with supercritical solvent entrance, and supercritical solvent is returned
The supercritical solvent received in tower 3 enters extraction tower 2 by the supercritical solvent entrance；
Upper area in extraction tower 2 is provided with 3-5 packing section, and which can be random packing or structured packing, its filler
Specific surface area >=150m2/m3, between voidage >=0.95, and adjacent packing section, it is provided with distributor, supercritical solvent recovery tower 3
In supercritical solvent is introduced in extraction tower 2 by the distributor between packing section so that supercritical solvent in extraction tower 2 and
Deasphalted oil contacts mixing, isolates depitching oil phase and de-oiled asphalt phase；Wherein, supercritical solvent and heavy oil feed
Mass flowrate ratio is 0.1-1:1；The temperature of extraction tower 2 is 50-200 DEG C, and pressure is 3.0-10.0, and the tower top temperature of extraction tower 2
Degree is higher than 5-50 DEG C of column bottom temperature；
The outlet of depitching oil phase is provided with the top of extraction tower 2, the outlet is connected with supercritical solvent recovery tower 3, by extraction tower 2
The depitching oil phase that overhead stream goes out and recycling design in the mixture feeding supercritical solvent recovery tower 3 of solvent, make solvent face super
It is separated with deasphalted oil under boundary's state, the solvent isolated returns extraction tower 2 and static mixing from supercritical solvent recovery tower 3
Device 1；Wherein, the 0.1-1MPa higher than the pressure of extraction tower 2 of supercritical solvent recovery tower 3, temperature is high 10-150 DEG C, and reduced temperature
Tr=T/TCBetween 0.992-1.20 (TC, iFor the critical temperature of solvent, xiFor each component molar fraction, T
For supercritical tower temperature degree, TcReferred to as pseudocritical temperature, temperature unit is K)；
3 bottom of supercritical solvent recovery tower is provided with the outlet of depitching oil phase, and depitching oil phase enters depitching from the outlet
Oil and gas stripper 5, is further separated out solvent by stripping；Deasphalted oil stripper 5 is provided with discharge of materials mouth and solvent discharge mouth,
The solvent that Jing deasphalted oils stripper 5 is isolated returns to solvent tank 6 by pipeline from solvent discharge mouth；
In Jing extraction towers 2, detached de-oiled asphalt is mutually exported from the de-oiled asphalt that 2 bottom of extraction tower is arranged and enters removing oil
Colophonium flash distillation stripper 4, is further separated out solvent by stripping；De-oiled asphalt flash distillation stripper 4 be provided with discharge of materials mouth and
Solvent discharge mouth, the solvent that Jing de-oiled asphalt flash distillations stripper 4 is isolated return to solvent tank by pipeline from solvent discharge mouth
6。
2nd, mink cell focus three-level partition method, detailed process are as follows：
As shown in Fig. 2 static mixer 01 connects extraction tower 02, solvent tank 08 is connected with static mixer 01 by pipeline
It is logical, after main solvent is mixed into static mixer 01 with heavy oil feed, in sending into extraction tower 02, isolate de-oiled asphalt phase
With depitching oil phase；Wherein, main solvent and the mass flowrate ratio of heavy oil feed are 1.5-5.0:1；Control static mixer
Temperature is 50-200 DEG C, and pressure is 3.0-10.0MPa；
The tower body bottom of extraction tower 02 is provided with the entrance of secondary solvent, and the solvent in solvent tank 08 is by pipeline from extraction tower 02
Secondary colvent inlet counter-current extraction is mutually carried out to de-oiled asphalt into extraction tower 02；The quality of wherein secondary solvent and heavy oil feed
Flow rate ratio is 0.1-1.0:1；Top in extraction tower 02 arranges the region of packing section and is provided with supercritical solvent entrance, and supercritical is molten
Supercritical solvent in agent recovery tower 04 enters extraction tower 02 by the supercritical solvent entrance；
Upper area in extraction tower 02 is provided with 3-5 packing section, and which can be random packing or structured packing, its filler
Specific surface area >=150m2/m3, between voidage >=0.95, and adjacent packing section, it is provided with distributor, supercritical solvent recovery tower
Supercritical solvent in 04 is introduced in extraction tower 02 by the distributor between packing section, so that supercritical solvent is in extraction tower 02
In contact with deasphalted oil mixing, isolate depitching oil phase and de-oiled asphalt phase；Wherein, supercritical solvent recovery tower 4 compares
The high 0.1-1MPa of pressure of extraction tower 2, temperature is high 10-150 DEG C, and reduced temperature Tr=T/TCBetween 0.992-1.20 (TC, iFor the critical temperature of solvent, xiFor each component molar fraction, T is supercritical tower temperature degree, TcReferred to as vacation is faced
Boundary's temperature, temperature unit are K), supercritical solvent is 0.1-1 with the mass flowrate ratio of heavy oil feed:1；The temperature of extraction tower 02
Spend for 50-200 DEG C, pressure is 3.0-10.0, and the tower top temperature of extraction tower 02 is higher than 5-50 DEG C of column bottom temperature；
The outlet of depitching oil phase is provided with the top of extraction tower 02, the outlet is connected with removing oil knockout tower 03 again, makes extraction tower 02
In depitching oil phase enter removing oil knockout tower 03 again.Upper area in removing oil knockout tower 03 is provided with 3-5 packing section again, its
Can be random packing or structured packing, the specific surface area >=150m of its filler2/m3, voidage >=0.95, and adjacent packing section it
Between be provided with distributor, the supercritical solvent in supercritical solvent recovery tower 04 is introduced by the distributor between packing section and is taken off again
In separating of oil tower 03 so that supercritical solvent in removing oil knockout tower 03 again with deasphalted oil phase counter current contacting, isolate frivolous
Oil phase and again removing oil phase.Wherein, supercritical solvent and the mass flowrate ratio of heavy oil feed are 0.1-1:1；Control removing oil point again
Temperature from tower is 50-200 DEG C, and pressure is 3.0-10.0MPa, and the tower top temperature of removing oil knockout tower 03 is higher than column bottom temperature again
5-50℃；
It is provided with frivolous oil phase outlet again at the top of removing oil knockout tower 03, the outlet is connected with supercritical solvent recovery tower 04, will
The frivolous oil phase that 03 overhead stream of removing oil knockout tower goes out again and recycling design in the mixture feeding supercritical solvent recovery tower 04 of solvent,
Make solvent in the supercritical state with frivolous separation of oil, the solvent isolated returns extraction respectively from supercritical solvent recovery tower 04
Take tower 02 and removing oil knockout tower 03 again；Wherein, the 0.1-1MPa higher than the pressure of extraction tower 02 of supercritical solvent recovery tower 04, temperature
It is high 10-150 DEG C；
03 bottom of removing oil knockout tower is provided with removing oil again and mutually exports again, and removing oil again enters removing oil stripper again from the outlet
06, solvent is further separated out by stripping；Removing oil stripper 06 is provided with discharge of materials mouth and solvent discharge mouth, Jing removing oils again again
The solvent that stripper 06 is isolated returns to solvent tank 08 by pipeline from solvent discharge mouth；
04 bottom of supercritical solvent recovery tower is provided with frivolous oil phase outlet, and frivolous oil phase is carried from the outlet into frivolous oil and gas
Tower 07, is further separated out solvent by stripping；Frivolous oil and gas stripper 07 is provided with discharge of materials mouth and solvent discharge mouth, and Jing is frivolous
The solvent that oil and gas stripper 07 is isolated returns to solvent tank 08 by pipeline from solvent discharge mouth；
In Jing extraction towers 02, detached de-oiled asphalt mutually exports removing oil drip from the de-oiled asphalt that 02 bottom of extraction tower is arranged
Blue or green flash distillation stripper 05, is further separated out solvent by stripping；De-oiled asphalt flash distillation stripper 05 be provided with discharge of materials mouth and
Solvent discharge mouth, the solvent that Jing de-oiled asphalt flash distillations stripper 05 is isolated return to solvent tank by pipeline from solvent discharge mouth
08。
Embodiment 1
Using petroleum residual oil (boiling point>420 DEG C) for raw material, using C3-C4 mixed solvents (wherein, main solvent, secondary solvent and
Supercritical solvent is all the mixed solvent), the composition of the mixed solvent is as follows：
| Component | Propane | Iso-butane | Normal butane |
| Composition, m% | 25 | 50 | 25 |
As shown in Fig. 2 being separated to petroleum residual oil using three-level partition method, its detailed process refer to above-mentioned three fraction
From method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of petroleum residual oil are 2.4：1；
2) secondary solvent and the mass flowrate ratio of petroleum residual oil are 0.1:1；
3) temperature that petroleum residual oil is mixed with main solvent is 120 DEG C, and pressure is 4.6MPa；
4) 3 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap θ ring fillers, the specific surface area of its filler
150m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels and enters extraction by the distributor
Take in tower 02, keep each road solvent incoming direction upwards, and 02 head temperature of extraction tower is higher than 8 DEG C of bottom temp, supercritical
Solvent is 0.25 with the mass flowrate ratio of petroleum residual oil:1；
5) 3 sections of fillers are loaded again in 03 internal upper part region of removing oil knockout tower, filler is scattered heap θ ring fillers, the ratio of its filler
Surface area 150m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distributor
Into in removing oil knockout tower 03 again, keep each road solvent incoming direction upwards, and 03 head temperature of removing oil knockout tower is higher than again
10 DEG C of bottom temp, supercritical solvent are 0.25 with the mass flowrate ratio of petroleum residual oil:1；
6) the pressure 4.3MPa of extraction tower 02,125 DEG C of temperature；The temperature of removing oil knockout tower is 135 DEG C again, and pressure is
4.2MPa。
7) the pressure 4.9MPa of supercritical solvent recovery tower 04,165 DEG C of temperature, reduced temperature Tr=1.094.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, has comparability, comparative example total solvent circulating load (total solvent circulating load identical with the present embodiment to make result
=main solvent+pair solvent+extraction tower introduces the removing oil knockout tower of supercritical solvent+again and introduces supercritical solvent, due in comparative example
Without supercritical solvent is introduced in extraction tower and again removing oil knockout tower, higher than embodiment, following example is identical for main solvent ratio),
Other relevant parameters are identical with the present embodiment.Table 1 is the comparison of embodiment 1 and frivolous oil phase in comparative example：
The comparison of frivolous oil phase in table 1, embodiment 1 and comparative example
| Property | Raw material | The frivolous oil of comparative example | The frivolous oil of embodiment |
| Yield, m% | 100 | 42.69 | 49.77 |
| Density (20 DEG C), g/cm3 | 0.9801 | 0.9272 | 0.9254 |
| Carbon residue, m% | 14.40 | 1.56 | 1.62 |
| S, m% | 2.08 | 1.8 | 1.7 |
| N, m% | 0.76 | 0.19 | 0.19 |
| C7 asphalitines, μ g/g | 5.45 | 0.085 | 0.050 |
| Ni, μ g/g | 39.7 | 1.2 | 0.8 |
| V, μ g/g | 156 | 3.0 | 2.0 |
As shown in Table 1：The yield of the frivolous oil phase of target product in embodiment 1 is higher than comparative example, and C7 asphalt contents
Decline, Ni and V content decline, it is seen that during the three-level partition method of embodiment 1 efficiently solves prior art, heavy oil feed is extracting
The inapparent problem of separating effect during taking, obtains the frivolous oil phase of high income, good properties.
Embodiment 2
Using petroleum residual oil (boiling point>420 DEG C) for raw material, using C4 mixed solvents (wherein, main solvent, secondary solvent and super
Critical solvent is all the mixed solvent), the composition of the mixed solvent is as follows：
| Component | Iso-butane | Normal butane |
| Composition, m% | 25 | 75 |
As shown in Fig. 2 being separated to petroleum residual oil using three-level partition method, its detailed process refer to above-mentioned three fraction
From method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of petroleum residual oil are 2.8：1；
2) secondary solvent and the mass flowrate ratio of petroleum residual oil are 0.2:1；
3) petroleum residual oil and main solvent mixing temperature are 100 DEG C, and pressure is 4.3MPa；
4) 4 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap Pall ring filler, the specific surface of its filler
Product 219m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels and is entered by the distributor
In extraction tower 02, keep each road solvent incoming direction downward, and 02 head temperature of extraction tower is higher than 15 DEG C of bottom temp, it is super to face
Boundary's solvent is 0.5 with the mass flowrate ratio of petroleum residual oil:1；
5) 4 sections of fillers are loaded again in 03 internal upper part region of removing oil knockout tower, filler is scattered heap Pall ring filler, its filler
Specific surface area 219m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels by the distribution
Device is entered in removing oil knockout tower 03 again, keeps each road solvent incoming direction downward, and 03 head temperature of removing oil knockout tower is high again
In 15 DEG C of bottom temp, supercritical solvent is 0.5 with the mass flowrate ratio of petroleum residual oil:1；
6) the pressure 4.3MPa of extraction tower 02,110 DEG C of temperature；The temperature of removing oil knockout tower is 125 DEG C again, and pressure is
4.1MPa。
7) the pressure 4.6MPa of supercritical solvent recovery tower 04,180 DEG C of temperature, reduced temperature Tr=1.077.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 2 is the ratio of embodiment 2 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 2, embodiment 2 and comparative example
| Property | Raw material | The frivolous oil of comparative example | The frivolous oil of embodiment |
| Yield, m% | 100 | 68.26 | 75.68 |
| Density (20 DEG C), g/cm3 | 0.9801 | 0.9347 | 0.9362 |
| Carbon residue, m% | 14.40 | 4.3 | 3.5 |
| S, m% | 2.08 | 1.9 | 1.9 |
| N, m% | 0.76 | 0.26 | 0.26 |
| C7 asphalitines, m% | 5.45 | 0.2 | 0.12 |
| Ni, μ g/g | 39.7 | 3.4 | 4.3 |
| V, μ g/g | 156 | 11.4 | 11.8 |
As shown in Table 2：The yield of the frivolous oil phase of target product in embodiment 2 is higher than comparative example, and C7 asphalt contents
Decline, quite, carbon residue is reduced, it is seen that the three-level partition method of embodiment 2 efficiently solves mink cell focus in prior art for Ni and V content
Not significant enough the problem of raw material separating effect in extraction process, obtains the frivolous oil phase of high income, good properties.
Embodiment 3
Tower bottom product (the reduced crude) (boiling point obtained using Canadian oil sands bitumen Jing air-distillations>350 DEG C, 20 DEG C
When density ＞ 1.0g/cm3) for raw material, using C5 mixed solvents, (wherein, main solvent, secondary solvent and supercritical solvent are all this
Mixed solvent), the composition of the mixed solvent is as follows：
| Component | Isopentane | Pentane |
| Composition, m% | 25 | 75 |
As shown in Fig. 2 being separated to reduced crude using three-level partition method, its detailed process refer to above-mentioned three fraction
From method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of reduced crude are 2.75：1；
2) secondary solvent and the mass flowrate ratio of reduced crude are 0.25:1；
3) reduced crude and main solvent mixing temperature are 170 DEG C, and pressure is 4.0MPa；
4) 3 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap Intalox Saddle, the ratio of its filler
Surface area 185m2/m3, voidage 0.96 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distributor
Into in extraction tower 02, each road solvent incoming direction is kept upwards, and 02 head temperature of extraction tower is higher than 8 DEG C of bottom temp,
Supercritical solvent is 0.25 with the mass flowrate ratio of petroleum residual oil:1；
5) again in 03 internal upper part region of removing oil knockout tower load 4 sections of fillers, filler be perforated plate corrugated structured packing, its filler
Specific surface area 250m2/m3, voidage 0.984 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels by described
Distributor is entered again in removing oil knockout tower 03, keeps each road solvent incoming direction upwards, and temperature at the top of removing oil knockout tower 03 again
Degree is 0.5 with the mass flowrate ratio of petroleum residual oil higher than 15 DEG C of bottom temp, supercritical solvent:1；
6) the pressure 4.3MPa of extraction tower 02,175 DEG C of temperature；The temperature of removing oil knockout tower is 185 DEG C again, and pressure is
4.1MPa。
7) the pressure 4.5MPa of supercritical solvent recovery tower 04,250 DEG C of temperature, reduced temperature Tr=1.12.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 3 is the ratio of embodiment 3 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 3, embodiment 3 and comparative example
| Property | Raw material | The frivolous oil of comparative example | The frivolous oil of embodiment |
| Yield, m% | 100 | 84 | 87 |
| Density (20 DEG C), g/cm3 | 1.0217 | 0.9792 | 0.9754 |
| Carbon residue, m% | 13 | 6 | 5.5 |
| S, m% | 5 | 4.2 | 4.2 |
| N, m% | 0.78 | 0.33 | 0.30 |
| C7 asphalitines, m% | 15.0 | 0.3 | 0.1 |
| Ni, μ g/g | 80 | 30 | 25 |
| V, μ g/g | 220 | 90 | 78 |
As shown in Table 3：The yield of the frivolous oil phase of target product in embodiment 3 is higher than comparative example, and C7 asphalt contents
Decline, quite, carbon residue is reduced, it is seen that in embodiment 3, three-level partition method efficiently solves mink cell focus in prior art for Ni and V content
Not significant enough the problem of raw material separating effect in extraction process, obtains the frivolous oil phase of high income, good properties.
Embodiment 4
Using the decompression residuum (boiling point of Canadian oil sands bitumen>524 DEG C, density ＞ 1.0596g/cm when 20 DEG C3, C7
Asphalitine is up to 18.1m%) for raw material, using pentane, used as solvent, (wherein, main solvent, secondary solvent and supercritical solvent be all
For the solvent)；
As shown in Fig. 2 being separated to decompression residuum using three-level partition method, its detailed process refer to above-mentioned three fraction
From method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of decompression residuum are 3.0：1；
2) secondary solvent and the mass flowrate ratio of decompression residuum are 0.5:1；
3) decompression residuum and main solvent mixing temperature are 160 DEG C, and pressure is 7.0MPa；
4) 3 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap metal step ring filler, the ratio of its filler
Surface area 221m2/m3, voidage 0.951 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distribution
Device is entered in extraction tower 02, keeps each road solvent incoming direction downward, and 02 head temperature of extraction tower is higher than bottom temp 10
DEG C, supercritical solvent is 0.4 with the mass flowrate ratio of petroleum residual oil:1；
5) 4 sections of fillers are loaded again in 03 internal upper part region of removing oil knockout tower, to dissipate heap metal step ring filler, which fills out filler
Specific surface area 221m of material2/m3, voidage 0.951 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels by institute
State distributor to enter again in removing oil knockout tower 03, keep each road solvent incoming direction downward, and again at the top of removing oil knockout tower 03
Temperature is higher than 12 DEG C of bottom temp, and supercritical solvent is 0.6 with the mass flowrate ratio of petroleum residual oil:1；
6) the pressure 7.0MPa of extraction tower 02,165 DEG C of temperature；The temperature of removing oil knockout tower is 176 DEG C again, and pressure is
6.7MPa。
7) the pressure 7.6MPa of supercritical solvent recovery tower 04,275 DEG C of temperature, reduced temperature Tr=1.17.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 4 is the ratio of embodiment 4 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 4, embodiment 4 and comparative example
| Property | Raw material | The frivolous oil of comparative example | The frivolous oil of embodiment |
| Yield, m% | 100 | 65 | 72 |
| Density (20 DEG C), g/cm3 | 1.0596 | 0.9990 | 1.000 |
| Carbon residue, m% | 24.9 | 12 | 10.5 |
| S, m% | 6.1 | 4.9 | 4.9 |
| N, m% | 0.63 | 0.5 | 0.5 |
| C7 asphalitines, m% | 18.1 | 0.2 | ＜ 0.1 |
| Ni, μ g/g | 104 | 39.1 | 35 |
| V, μ g/g | 280 | 85.4 | 80 |
As shown in Table 4：The yield of the frivolous oil phase of target product in embodiment 4 is higher than comparative example, and C7 asphalt contents
Decline, quite, carbon residue is reduced, it is seen that in embodiment 4, three-level partition method efficiently solves mink cell focus in prior art for Ni and V content
Not significant enough the problem of raw material separating effect in extraction process, obtains the frivolous oil phase of high income, good properties.
Embodiment 5
Using the super mink cell focus (boiling point of Venezuela>420 DEG C, density ＞ 1.0g/cm when 20 DEG C3) for raw material, using C5
Mixed solvent (wherein, main solvent, secondary solvent and supercritical solvent are all the mixed solvent), the composition of the mixed solvent is as follows：
| Component | Pentane | Pentamethylene. |
| Composition, m% | 88 | 12 |
As shown in Fig. 2 being separated to mink cell focus using three-level partition method, its detailed process refer to above-mentioned three-level and separate
Method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of mink cell focus are 2.4：1；
2) secondary solvent and the mass flowrate ratio of mink cell focus are 0.2:1；
3) mink cell focus and main solvent mixing temperature are 160 DEG C, and pressure is 5.0MPa；
4) 3 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is calendering corrugated regular filler, the ratio table of its filler
Area 500m2/m3, voidage 0.975 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distributor
Into in extraction tower 02, keep each road solvent incoming direction downward, and 02 head temperature of extraction tower be higher than 10 DEG C of bottom temp,
Supercritical solvent is 0.3 with the mass flowrate ratio of petroleum residual oil:1；
5) again in 03 internal upper part region of removing oil knockout tower load 4 sections of fillers, filler be perforated plate corrugated structured packing, its filler
Specific surface area 250m2/m3, voidage 0.984 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels by described
Distributor is entered again in removing oil knockout tower 03, keeps each road solvent incoming direction downward, and temperature at the top of removing oil knockout tower 03 again
Degree is 0.6 with the mass flowrate ratio of petroleum residual oil higher than 15 DEG C of bottom temp, supercritical solvent:1；
6) the pressure 5.0MPa of extraction tower 02,165 DEG C of temperature；The temperature of removing oil knockout tower is 178 DEG C again, and pressure is
4.8MPa。
7) the pressure 5.6MPa of supercritical solvent recovery tower 04,250 DEG C of temperature, reduced temperature Tr=1.075.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 5 is the ratio of embodiment 5 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 5, embodiment 5 and comparative example
| Property | Raw material | The frivolous oil of comparative example | The frivolous oil of embodiment |
| Yield, m% | 100 | 76.6 | 79.8 |
| Density (20 DEG C), g/cm3 | 1.0281 | 0.9967 | 0.9890 |
| Viscosity (100 DEG C), mPa.s | 2966.3 | 295 | 200 |
| Carbon residue, m% | 21.05 | 9.92 | 9.42 |
| Asphalitine, m% | 12.05 | 0.79 | 0.25 |
| S, m% | 4.0 | 3.5 | 3.6 |
| N, m% | 0.76 | 0.27 | 0.27 |
| Ni, μ g/g | 118 | 38.3 | 28 |
| V, μ g/g | 531 | 147.7 | 111 |
As shown in Table 5：The yield of the frivolous oil phase of target product in embodiment 5 is higher than comparative example, and C7 asphalt contents
Decline, quite, carbon residue is reduced, it is seen that in embodiment 5, three-level partition method efficiently solves mink cell focus in prior art for Ni and V content
Not significant enough the problem of raw material separating effect in extraction process, obtains the frivolous oil phase of high income, good properties.
Embodiment 6
Certain catalytic cracked oil pulp is adopted for raw material, (wherein, main solvent, secondary solvent and supercritical are molten using C4 mixed solvents
Agent is all the mixed solvent), the composition of the mixed solvent is as follows：
| Component | Iso-butane | Normal butane |
| Composition, m% | 25 | 75 |
As shown in figure 1, being separated to mink cell focus using the second-order separation method, its detailed process refer to above-mentioned the second-order separation
Method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of catalytic cracked oil pulp are 3.2：1；
2) secondary solvent and the mass flowrate ratio of catalytic cracked oil pulp are 0.3:1；
3) catalytic cracked oil pulp and main solvent mixing temperature are 100 DEG C, and pressure is 4.3MPa；
4) 3 sections of fillers are loaded in 2 internal upper part region of extraction tower, filler is calendering corrugated regular filler, the ratio table of its filler
Area 500m2/m3, voidage 0.975 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distributor
Into in extraction tower 02, keep each road solvent incoming direction downward, and 2 head temperature of extraction tower be higher than 13 DEG C of bottom temp,
Supercritical solvent is 0.5 with the mass flowrate ratio of petroleum residual oil:1；
5) the pressure 4.3MPa of extraction tower 02,107 DEG C of temperature.
6) the pressure 4.6MPa of supercritical solvent recovery tower 3,190 DEG C of temperature, reduced temperature Tr=1.10.
According to prior art solvent de-asphalting process as a comparison case, be added without supercritical in extraction tower in comparative example
Solvent, the upper area in extraction tower do not set up multistage packing section, and tower top and bottom do not have the temperature difference, other relevant parameters with
The present embodiment is identical.Table 6 is the comparison of embodiment 6 and depitching oil phase in comparative example：
The comparison of depitching oil phase in table 6, embodiment 6 and comparative example
As shown in Table 6：The yield of the target product depitching oil phase in embodiment 6 contains higher than comparative example, and C7 asphalitines
Amount is remarkably decreased, and tenor is slightly reduced, and arene content increases compared with comparative example, and product is more beneficial for as production high-quality
Material with carbon element raw material.
Embodiment 7
Certain catalytic cracked oil pulp is adopted for raw material, (wherein, main solvent, secondary solvent and supercritical are molten using C4 mixed solvents
Agent is all the mixed solvent), the composition of the mixed solvent is as follows：
| Component | Iso-butane | Normal butane |
| Composition, m% | 90 | 10 |
As shown in Fig. 2 being separated to catalytic cracked oil pulp using three-level partition method, its detailed process refer to above-mentioned three
Level partition method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of catalytic cracked oil pulp are 2.85：1；
2) secondary solvent and the mass flowrate ratio of catalytic cracked oil pulp are 0.35:1；
3) catalytic cracked oil pulp and main solvent mixing condition are 90 DEG C for temperature, and pressure is 4.3MPa；
4) 3 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap Pall ring filler, the specific surface of its filler
Product 219m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels and is entered by the distributor
In extraction tower 02, keep each road solvent incoming direction downward, and 02 head temperature of extraction tower is higher than 10 DEG C of bottom temp, it is super to face
Boundary's solvent is 0.25 with the mass flowrate ratio of petroleum residual oil:1；
5) 4 sections of fillers are loaded again in 03 internal upper part region of removing oil knockout tower, filler is calendering corrugated regular filler, its filler
Specific surface area 450m2/m3, voidage 0.97 arranges distributor between packing section, supercritical solvent is divided into 3 tunnels by described point
Cloth device is entered in removing oil knockout tower 03 again, keeps each road solvent incoming direction downward, and 03 head temperature of removing oil knockout tower again
Higher than 20 DEG C of bottom temp, supercritical solvent is 1 with the mass flowrate ratio of petroleum residual oil:1；
6) the pressure 4.3MPa of extraction tower 02,95 DEG C of temperature；The temperature of removing oil knockout tower is 110 DEG C again, and pressure is
4.2MPa。
7) the pressure 4.6MPa of supercritical solvent recovery tower 04,180 DEG C of temperature, reduced temperature Tr=1.105.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 7 is the ratio of embodiment 7 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 7, embodiment 7 and comparative example
As shown in Table 7：The yield of the frivolous oil phase of target product in embodiment 7 is higher than comparative example, and C7 asphalt contents
Decline, quite, carbon residue is reduced for Ni and V content, and saturated hydrocarbon content is higher, be more beneficial for splitting as bunker fuel oil and return catalysis
Raw oil is turned to, the density of removing oil phase increases again, can be used as high quality carbon material feedstock.
Embodiment 8
Using certain coal tar asphalt (boiling point>350 DEG C) for raw material, using pentane as solvent (wherein, main solvent, pair
Solvent and supercritical solvent are all the solvent)；
As shown in Fig. 2 being separated to coal tar asphalt using three-level partition method, its detailed process refer to above-mentioned three-level
Partition method.The technological parameter that each step of the method is related to is as follows：
1) main solvent and the mass flowrate ratio of coal tar asphalt are 2.3：1；
2) secondary solvent and the mass flowrate ratio of coal tar asphalt are 0.1:1；
3) coal tar asphalt and main solvent mixing condition are 150 DEG C for temperature, and pressure is 6.0MPa；
4) 2 sections of fillers are loaded in 02 internal upper part region of extraction tower, filler is scattered heap Pall ring filler, the specific surface of its filler
Product 219m2/m3, voidage 0.95 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels and is entered by the distributor
In extraction tower 02, each road solvent incoming direction is kept upwards, and 02 head temperature of extraction tower is higher than 5 DEG C of bottom temp, it is super to face
Boundary's solvent is 0.2 with the mass flowrate ratio of petroleum residual oil:1；
5) 3 sections of fillers are loaded again in 03 internal upper part region of removing oil knockout tower, filler is scattered heap Pall ring filler, its filler
Specific surface area 300m2/m3, voidage 0.97 arranges distributor between packing section, supercritical solvent is divided into 2 tunnels by the distribution
Device is entered in removing oil knockout tower 03 again, keeps each road solvent incoming direction upwards, and 03 head temperature of removing oil knockout tower is high again
In 10 DEG C of bottom temp, supercritical solvent is 0.4 with the mass flowrate ratio of petroleum residual oil:1；
6) the pressure 6.0MPa of extraction tower 02,153 DEG C of temperature；The temperature of removing oil knockout tower is 163 DEG C again, and pressure is
5.7MPa。
7) the pressure 6.5MPa of supercritical solvent recovery tower 04,230 DEG C of temperature, reduced temperature Tr=1.072.
According to prior art solvent de-asphalting process as a comparison case, extraction tower and removing oil knockout tower again in comparative example
In be added without supercritical solvent, the upper area in extraction tower and again removing oil knockout tower does not set up multistage packing section, tower top and
Bottom does not have the temperature difference, and other relevant parameters are identical with the present embodiment.Table 8 is the ratio of embodiment 8 and frivolous oil phase in comparative example
Compared with：
The comparison of frivolous oil phase in table 8, embodiment 8 and comparative example
As shown in Table 8：The yield of the frivolous oil phase of target product in embodiment 8 is higher than comparative example, and C7 asphalt contents
Decline, it is seen that during in embodiment 8, three-level partition method efficiently solves prior art, heavy oil feed separates effect in extraction process
Not significant enough the problem of fruit, obtains the frivolous oil phase of high income, good properties.
Finally it should be noted that：Above example only to illustrate technical scheme, rather than a limitation；Although
With reference to the foregoing embodiments the present invention has been described in detail, it will be understood by those within the art that：Which still may be used
To modify to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical scheme spirit and
Scope.
Claims (13)
1. a kind of heavy oil separating method, it is characterised in that the extraction tower of multiple packing sections is provided with using upper area, and it is adjacent
Distributor is provided between packing section, the supercritical solvent from supercritical solvent recovery tower is introduced by distributor, made described
Heavy constituent in the depitching oil phase on extraction tower top is further separated, and the separation method includes：
Heavy oil feed is mixed with main solvent in static mixer, and institute is sent into from less than the region for being provided with packing section
Extraction tower is stated, the main solvent is 1.5-5.0 with the mass flowrate ratio of the heavy oil feed:1, and control the temperature of blender
For 50-200 DEG C, pressure is 3.0-10.0MPa；
By secondary solvent from the extraction tower bottom and less than heavy oil feed and main solvent mixed material entry zone by distribution
Device is sent in tower, and with the de-oiled asphalt phase counter current contacting isolated, the quality stream of the secondary solvent and the heavy oil feed
Rate ratio is 0.1-1.0:1；
Supercritical solvent is introduced in the extraction tower by the distributor between packing section, and with the depitching oil phase isolated
Contact mixing, the supercritical solvent are 0.1-1 with the mass flowrate ratio of the heavy oil feed:1；
The depitching oil phase that heavy oil feed is separated in the extraction tower is gone out from extraction tower top row, separation is carried out and is collected
Deasphalted oil, mutually strips to the de-oiled asphalt that extraction tower bottom is discharged, isolates solvent, and collect de-oiled asphalt；
Wherein, extraction temperature 50-200 DEG C in extraction tower is controlled, pressure is 3.0-10.0MPa, and the tower top temperature of extraction tower
Higher than 5-50 DEG C of column bottom temperature；
Mixture of the depitching oil phase isolated with solvent is gone out and is sent into removing oil knockout tower again from extraction tower top row, it is described heavy
Removing oil knockout tower upper area is provided between multiple packing sections, and adjacent packing section and is provided with distributor, and supercritical solvent is led to
The distributor crossed between packing section introduces the heavy removing oil knockout tower；
The frivolous oil phase that depitching oil phase is separated in the heavy removing oil knockout tower is gone out from removing oil knockout tower top row again, is entered
Frivolous oil is collected in row separation, the removing oil again that bottom of towe is discharged mutually is stripped, solvent is isolated, and is collected removing oil again；It is described super
Critical solvent is 0.1-1 with the mass flowrate ratio of the heavy oil feed:1, the tower top temperature of the heavy removing oil knockout tower is higher than
5-50 DEG C of column bottom temperature, and control the heavy removing oil knockout tower temperature be 50-200 DEG C, pressure is 3.0-10.0MPa.
2. heavy oil separating method according to claim 1, it is characterised in that methods described also includes：
The depitching oil phase that extraction tower top row is gone out and the mixture feeding supercritical solvent recovery tower recycling design of solvent, make molten
Agent is separated with deasphalted oil in the supercritical state, and the supercritical solvent for obtaining is returned static mixer and extraction tower.
3. heavy oil separating method according to claim 1, it is characterised in that methods described also includes：
The frivolous oil phase that removing oil knockout tower top row again is gone out and the mixture feeding supercritical solvent recovery tower of solvent, make solvent exist
With frivolous separation of oil under supercriticality, and the supercritical solvent for obtaining is returned into static mixer, extraction tower and removing oil again
Knockout tower.
4. the heavy oil separating method according to Claims 2 or 3, it is characterised in that the supercritical solvent recovery tower
The high 0.1-1MPa of pressure of extraction tower described in pressure ratio, the temperature in the supercritical solvent recovery tower is than in the extraction tower
Temperature is high 10-150 DEG C.
5. heavy oil separating method according to claim 4, it is characterised in that implement in the supercritical solvent recovery tower
The condition of supercritical recovery solvent is：Pressure 3.0-10.0MPa, temperature 94-280 DEG C, and reduced temperature Tr=T/TCIn 0.992-
1.20 between；Wherein,
TC, iFor the critical temperature of solvent, xiFor each component molar fraction, T is supercritical tower temperature degree, TcReferred to as
Pseudocritical temperature, temperature unit are K.
6. heavy oil separating method according to claim 1, it is characterised in that described filler section is 3-5 sections, filler mode
For random packing or structured packing, the specific surface area >=150m of described filler2/m3, voidage >=0.95.
7. heavy oil separating method according to claim 1, it is characterised in that the heavy oil feed includes oil exploitation
During the mink cell focus for obtaining and the residual oil obtained in oil sands bitumen, petroleum refining process or catalytic cracked oil pulp or Coal Chemical Industry
The coal tar asphalt for obtaining, and density ＞ 0.934g/cm of the heavy oil feed at 20 DEG C3Or boiling point is higher than 350 DEG C.
8. heavy oil separating method according to claim 1, it is characterised in that the main solvent, secondary solvent and super face
The key component of boundary's solvent is the alkane and cycloalkane of C3-C5.
9. the processing system of heavy oil separating method described in any one of claim 1-8 is implemented, it is characterised in that the processing system
System includes static mixer, extraction tower, solvent tank and stripper；
The static mixer has main solvent import and heavy oil feed import and mixed material outlet, and main solvent import connects
Lead to the solvent tank, the material inlet of mixed material outlet extraction tower；
The extraction tower internal upper part is provided with multiple packing sections, and in the middle part of tower body, tower body bottom is provided with pair for mixed material import
Colvent inlet, so as to contact into the secondary solvent in tower with de-oiled asphalt realize extraction, tower internal upper part arranges the area of packing section
Domain is provided with supercritical solvent entrance and is communicated between adjacent packing section by distributor, so that supercritical solvent is in extraction tower
The interior mixing that contacts with deasphalted oil, is provided with the outlet of depitching oil phase at the top of tower body, tower body bottom is provided with de-oiled asphalt and mutually discharges
Mouthful；
The de-oiled asphalt phase floss hole of the extraction tower bottom connects the stripper, so that the solvent in de-oiled asphalt phase is divided
Separate out and；
The processing system also includes removing oil knockout tower again, and the heavy removing oil knockout tower upper area is provided with multiple packing sections, and
Distributor is provided between adjacent packing section, tower body arranges the region of packing section and is provided with supercritical solvent entrance and by distributor
It is communicated between adjacent packing section, the heavy removing oil knockout tower arranges depitching oil phase less than supercritical solvent entrance area and enters
Mouthful, the heavy removing oil separates tower top and is provided with frivolous oil phase outlet, and bottom of towe is provided with removing oil again and mutually exports.
10. processing system according to claim 9, it is characterised in that the processing system is also returned including supercritical solvent
Receive tower, the depitching oil phase outlet at the top of the material inlet of the supercritical solvent recovery tower and extraction tower is described super to face
The supercritical solvent outlet of boundary's solvent recovery tower is connected with the supercritical solvent entrance of static mixer and extraction tower, described super
Critical solvent recovery tower bottom of towe is provided with depitching oil phase floss hole.
11. processing systems according to claim 10, it is characterised in that the processing system is also stripped including deasphalted oil
Tower and de-oiled asphalt flash distillation stripper；
The depitching oil phase floss hole that the supercritical solvent recovery tower is isolated connects the material of the deasphalted oil stripper
Import, the solvent outlet of the deasphalted oil stripper pass through pipeline connection to the solvent tank；
The de-oiled asphalt phase floss hole of the extraction tower is communicated to the material inlet of the de-oiled asphalt flash distillation stripper, described de-
The solvent outlet of oil asphalt flash distillation stripper is by pipeline connection to the solvent tank.
12. processing systems according to claim 9, it is characterised in that the processing system is also returned including supercritical solvent
Receive tower, the frivolous oil phase outlet of removing oil knockout tower again connect with the material inlet of the supercritical solvent recovery tower, it is described surpass face
The supercritical solvent outlet of boundary's solvent recovery tower is molten with the supercritical of static mixer, extraction tower and removing oil knockout tower again respectively
Agent entrance is connected, and the supercritical solvent recovery tower bottom of towe is provided with frivolous oil phase floss hole.
13. processing systems according to claim 12, it is characterised in that the processing system is also carried including frivolous oil and gas
Tower, again removing oil stripper and de-oiled asphalt flash distillation stripper；
The frivolous oil phase floss hole that the supercritical solvent recovery tower is isolated connects the material inlet of the frivolous oil and gas stripper,
The solvent outlet of the frivolous oil and gas stripper is by pipeline connection to the solvent tank；
The phase of the removing oil again floss hole that the heavy removing oil knockout tower is isolated connects the material inlet of the heavy removing oil stripper, described
The solvent outlet of removing oil stripper passes through pipeline connection to the solvent tank again；
The de-oiled asphalt phase floss hole of the extraction tower is communicated to the material inlet of the de-oiled asphalt flash distillation stripper, described de-
The solvent outlet of oil asphalt flash distillation stripper is by pipeline connection to the solvent tank.
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| CN107177378B (en) * | 2017-04-21 | 2018-06-29 | 北京和利凯石化技术有限公司 | The supercritical extract of heavy oil feedstock and the combined system of floating bed hydrogenation and method |
| CN107177373B (en) * | 2017-04-21 | 2018-06-19 | 北京和利凯石化技术有限公司 | A kind of overcritical residual oil and/or catalytic slurry processing system and processing method |
| CN110964338B (en) * | 2018-09-30 | 2021-12-31 | 广东怡和科洁科技有限公司 | Method for preparing aromatic oil-lignocellulose asphalt regenerant by using supercritical technology |
| CN109679674A (en) * | 2019-01-07 | 2019-04-26 | 李刚 | A kind of needle-shape coke raw material pretreating process |
| CN114426860A (en) * | 2020-09-22 | 2022-05-03 | 中国石油化工股份有限公司 | Heavy oil supercritical extraction separation method and device |
| CN114907876A (en) * | 2021-02-09 | 2022-08-16 | 中国石油化工股份有限公司 | Method and apparatus for solvent recovery |
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| CN1083513A (en) * | 1993-09-24 | 1994-03-09 | 中国石油化工总公司 | A kind of method of separating petroleum heavy oil |
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| CN1410510A (en) * | 2001-09-26 | 2003-04-16 | 石油大学(北京) | Solvent extraction technology for removing high softening point asphalt in petroleum slag and its equipment |
| CN1891784A (en) * | 2005-07-05 | 2007-01-10 | 中国石油大学(北京) | Method for realizing heavy oil deep-step separation by coupled residue granulating |
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| CN1083513A (en) * | 1993-09-24 | 1994-03-09 | 中国石油化工总公司 | A kind of method of separating petroleum heavy oil |
| CN1410510A (en) * | 2001-09-26 | 2003-04-16 | 石油大学(北京) | Solvent extraction technology for removing high softening point asphalt in petroleum slag and its equipment |
| CN1891784A (en) * | 2005-07-05 | 2007-01-10 | 中国石油大学(北京) | Method for realizing heavy oil deep-step separation by coupled residue granulating |
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