CN105400545A

CN105400545A - Heavy oil separation method and treatment system thereof

Info

Publication number: CN105400545A
Application number: CN201410458235.5A
Authority: CN
Inventors: 赵锁奇; 许志明; 孙学文; 徐春明
Original assignee: China University of Petroleum Beijing
Current assignee: China University of Petroleum Beijing
Priority date: 2014-09-10
Filing date: 2014-09-10
Publication date: 2016-03-16
Anticipated expiration: 2034-09-10
Also published as: CN105400545B

Abstract

The present invention provides a heavy oil separation method and a treatment system thereof. According to the separation method, an extraction tower with a plurality of filler sections arranged on the upper portion region is used, distributors are arranged between the adjacent filler sections, and a supercritical solvent from a supercritical solvent recovery tower is introduced through the distributors so as to further separate the heavy components in the deasphalted oil phase on the upper portion of the extraction tower. With the separation method of the present invention, the problem that the heavy oil raw material separation effect is not significant during the extraction separation process in the prior art can be effectively solved so as to obtain the target product with characteristics of high yield and excellent property.

Description

Heavy oil separation method and treatment system thereof

Technical Field

The invention relates to a heavy oil separation method and a treatment system thereof, belonging to the technical field of petroleum processing.

Background

Solvent deasphalting is a technology for removing heavy component asphalt in petroleum heavy oil, and is suitable for heavy oil and oil sand obtained by miningTreatment of bitumen and of the various atmospheric and vacuum residues obtained during petroleum processing, the density of such heavy oils (20 ℃ C.)>0.934g/cm³Or a boiling point above 350 ℃. The deasphalted asphalt oil is mainly used for producing lubricating oil base oil or used as a raw material for catalytic cracking or hydrocracking (not limited to) subsequent processing, and the deasphalted asphalt can be used as road asphalt, building asphalt or gasification raw materials and the like.

The prior solvent deasphalting technology mainly comprises a second-level or third-level process. In the second-stage extraction separation process, the solvent and the heavy oil raw material are mixed and then divided into a light phase and a heavy phase in the first-stage process, the light phase becomes a deasphalted oil phase and consists of the solvent and dissolved deasphalted oil (Deasphal-DAO), and the heavy phase is called an asphalt phase and consists of the deasphalted asphalt (DeoildAsphalt-DOA) and a certain content of the solvent. Heating the asphalt phase to a higher temperature, removing most of the solvent by flash evaporation, and stripping the residual solvent by steam to obtain the deoiled asphalt. In the second stage, heating the deasphalted oil phase to recover most of the solvent under the near-critical or supercritical condition of the solvent, and steam stripping the residual solvent to obtain deasphalted oil; in the three-stage extraction separation process, a section of heavy deoiling (colloid) separation tower is additionally arranged between the extraction tower and the supercritical solvent recovery tower, the deasphalted oil phase from the extraction tower is heated or depressurized to reduce the dissolving capacity of the solvent, so that the heavy deoiled phase is settled in the second-stage separation, the light deoiled oil phase at the tower top enters the supercritical tower to recover the solvent, and the heavy deoiled oil phase and the light deoiled oil phase are stripped to remove the residual solvent respectively to obtain the heavy deoiled (or called colloid) and the light deoiled oil.

According to the solvent deasphalting process in the prior art, no matter a two-stage process or a three-stage process, the extraction tower and the heavy deoiling and separating tower only play a role in settling and separating raw materials, the temperature difference between the top and the bottom of the extraction tower and the heavy deoiling and separating tower is very small, and the separation effect on the heavy oil raw materials is not obvious. Therefore, how to develop a new heavy oil separation method and effectively improve the separation effect of heavy oil is a problem to be solved urgently.

Disclosure of Invention

The invention provides a heavy oil separation method and a treatment system thereof, which can effectively solve the problem that the separation effect of heavy oil raw materials in the extraction separation process is not obvious in the prior art, so that a target product with high yield and excellent properties is obtained.

The invention provides a heavy oil separation method, which adopts an extraction tower with a plurality of packing sections in the upper area, a distributor is arranged between the adjacent packing sections, and a supercritical solvent from a supercritical solvent recovery tower is introduced through the distributor to further separate heavy components in a deasphalted oil phase at the upper part of the extraction tower, wherein the separation method comprises the following steps:

mixing a heavy oil raw material and a main solvent in a static mixer, and feeding the mixture into the extraction tower from a region lower than a region in which a filling section is arranged, wherein the mass flow rate ratio of the main solvent to the heavy oil raw material is 1.5-5.0:1, the temperature of the mixer is controlled to be 50-200 ℃, and the pressure is controlled to be 3.0-10.0 MPa;

feeding a secondary solvent into the extraction tower from the lower part of the extraction tower and below the inlet area of the mixed material of the heavy oil raw material and the main solvent through a distributor, and carrying out countercurrent contact on the secondary solvent and the separated deoiled asphalt, wherein the mass flow rate ratio of the secondary solvent to the heavy oil raw material is 0.1-1.0: 1;

introducing a supercritical solvent into the extraction tower through a distributor between the packing sections, and contacting and mixing the supercritical solvent with the separated deasphalted oil, wherein the mass flow rate ratio of the supercritical solvent to the heavy oil raw material is 0.1-1: 1;

discharging the deasphalted oil phase separated from the heavy oil raw material in the extraction tower from the top of the extraction tower, separating to collect deasphalted oil, stripping the deasphalted asphalt phase discharged from the bottom of the extraction tower to separate a solvent, and collecting the deoiled asphalt;

wherein the extraction temperature in the extraction tower is controlled to be 50-200 ℃, the pressure is controlled to be 3.0-10.0MPa, and the temperature of the top of the extraction tower is 5-50 ℃ higher than the temperature of the bottom of the extraction tower.

The heavy oil raw material separation method is a two-stage separation method, and the inventor of the present invention finds that: the heavy oil raw material and the main solvent are premixed before entering the extraction tower, so that the viscosity of the heavy oil raw material can be effectively reduced, and the separation effect of the heavy oil raw material in the extraction tower is facilitated. In addition, the upper area in the extraction tower is provided with a plurality of packing sections, so that the aim of single-tower multi-stage separation can be fulfilled, the separation effect of the heavy oil raw material is effectively improved, and the yield of the deasphalted oil phase is also improved. Meanwhile, the invention also uses the supercritical solvent to elute the asphalt phase and other heavy components carried in the deasphalted oil phase, thereby realizing the purpose of strengthening separation. Moreover, because the temperature of the supercritical solvent from the supercritical solvent recovery tower is higher, a temperature gradient is established in the extraction tower, which is beneficial to the extraction and separation of the heavy oil raw material, and the temperature difference is between 5 and 50 ℃ when the temperature at the top of the extraction tower is higher than that at the bottom of the extraction tower.

The two-stage separation method for the heavy oil raw material also comprises the following steps:

and (3) sending the mixture of the deasphalted oil phase and the solvent discharged from the top of the extraction tower into a supercritical solvent recovery tower to recover the solvent, separating the solvent from the deasphalted oil phase in a supercritical state, and returning the obtained supercritical solvent to the static mixer and the extraction tower.

For the separation of heavy oil raw materials, the invention can further process the obtained deasphalted oil by a three-stage separation method to separate a heavy deasphalted oil phase and a light deasphalted oil phase, thereby not only improving the properties of the deasphalted oil phase, but also greatly improving the yield of the light deasphalted oil phase. Therefore, on the basis of the two-stage separation method of the heavy oil raw material, the method also comprises the following steps:

discharging a mixture of the separated deasphalted oil phase and the solvent from the top of the extraction tower and sending the mixture into a heavy deoiling and separating tower, wherein a plurality of filler sections are arranged in the upper area of the heavy deoiling and separating tower, a distributor is arranged between every two adjacent filler sections, and the supercritical solvent is introduced into the heavy deoiling and separating tower through the distributor between the filler sections;

discharging the light deoiled phase separated from the deasphalted oil phase in the heavy deoiling and separating tower from the top of the heavy deoiling and separating tower, separating to collect light deoiled oil, steam stripping the heavy deoiled phase discharged from the bottom of the heavy deoiling tower to separate out solvent and collect heavy deoiled oil; the mass flow rate ratio of the supercritical solvent to the heavy oil raw material is 0.1-1:1, the temperature of the top of the heavy deoiling and separating tower is 5-50 ℃ higher than the temperature of the bottom of the heavy deoiling and separating tower, the temperature of the heavy deoiling and separating tower is controlled to be 50-200 ℃, and the pressure is 3.0-10.0 MPa.

The scheme of the invention can also be a three-stage separation method for heavy oil raw materials, and further comprises the following steps:

and (3) sending the mixture of the light deoiling phase and the solvent discharged from the top of the heavy deoiling separation tower into a supercritical solvent recovery tower, separating the solvent from the light deoiling phase in a supercritical state, and returning the obtained supercritical solvent to the static mixer, the extraction tower and the heavy deoiling separation tower.

In a specific embodiment of the present invention, the pressure of the supercritical solvent recovery column is 0.1 to 1MPa higher than the pressure of the extraction column, and the temperature in the supercritical solvent recovery column is 10 to 150 ℃ higher than the temperature in the extraction column.

In a specific embodiment of the present invention, the supercritical solvent recovery conditions in the supercritical solvent recovery column are as follows: pressure 3.0-10.0MPa, temperature 94-280 deg.C, and contrast temperature T_r＝T/T_CBetween 0.992 and 1.20: (T_c，iIs the critical temperature of the solvent, x_iIs the mole fraction of each component, T is the supercritical tower temperature, T_cReferred to as the pseudo-critical temperature in K).

The invention is a counterweightThe separation method of the heavy oil raw material adopts an extraction tower and a heavy deoiling separation tower which are provided with filler sections no matter a two-stage or three-stage separation method is adopted, the upper areas in the extraction tower and the heavy deoiling separation tower are filled with 3-5 sections of filler sections, the filler mode is random packing or regular packing, the specific surface area of the packing is more than or equal to 150m²/m³The void ratio is more than or equal to 0.95, and the supercritical solvent is introduced into the filler sections through the distributor in 2-4 ways, and the introduction directions of all the ways of solvent are kept the same, and the solvents can be simultaneously upwards or downwards. The packing can be selected, for example, from pall ring packing, corrugated packing (perforated plate/calendering), intalox ring packing, theta ring packing, and the like.

The heavy oil raw material used in the invention comprises heavy oil and oil sand asphalt obtained by petroleum exploitation, residual oil or catalytic cracking slurry oil obtained in the petroleum processing process, or coal tar asphalt obtained in the coal chemical industry process, and the density of the heavy oil raw material at 20 ℃ is more than 0.934g/cm³Or a boiling point above 350 ℃.

The main solvent, the secondary solvent and the supercritical solvent used in the present invention can be the same solvent for the convenience of production operation, for example, alkane and cycloalkane each having a main component of C3-C5, such as propane, n-butane, isobutane, n-pentane, isopentane and cyclopentane or a mixture thereof.

The invention also provides a treatment system capable of implementing the heavy oil separation method, wherein the treatment system comprises a static mixer, an extraction tower, a solvent tank and a stripping tower;

the static mixer is provided with a main solvent inlet, a heavy oil raw material inlet and a mixed material outlet, the main solvent inlet is communicated with the solvent tank, and the mixed material outlet is communicated with the material inlet of the extraction tower;

the extraction tower is characterized in that a plurality of filler sections are arranged at the upper part in the extraction tower, a mixed material inlet is formed in the middle of the tower body, an auxiliary solvent inlet is formed in the lower part of the tower body so that an auxiliary solvent entering the extraction tower is contacted with deoiled asphalt to realize extraction, a supercritical solvent inlet is formed in the area, where the filler sections are arranged, at the upper part in the extraction tower, and is communicated between the adjacent filler sections through a distributor so that the supercritical solvent is contacted and mixed with the deasphalted oil in the extraction tower, a deasphalted oil phase outlet is formed in the top of the tower body, and a deoiled asphalt phase outlet is formed in the;

and a deoiled asphalt phase discharge port at the bottom of the extraction tower is connected with the stripping tower, so that the solvent in the deoiled asphalt phase is separated.

Furthermore, the treatment system also comprises a supercritical solvent recovery tower, a material inlet of the supercritical solvent recovery tower is communicated with a deasphalted oil phase outlet at the top of the extraction tower, a supercritical solvent outlet of the supercritical solvent recovery tower is communicated with the static mixer and a supercritical solvent inlet of the extraction tower, and a deasphalted oil phase outlet is arranged at the bottom of the supercritical solvent recovery tower.

Further, the treatment system also comprises a deasphalted oil stripping tower and a deasphalted asphalt flash stripping tower;

a deasphalted oil phase discharge port separated by the supercritical solvent recovery tower is communicated with a material inlet of the deasphalted oil stripping tower, and a solvent outlet of the deasphalted oil stripping tower is communicated with the solvent tank through a pipeline;

and a deoiled asphalt phase discharge port of the extraction tower is communicated with a material inlet of the deoiled asphalt flash stripping tower, and a solvent outlet of the deoiled asphalt flash stripping tower is communicated with the solvent tank through a pipeline.

Furthermore, the processing system also comprises a heavy deoiling separation tower, wherein a plurality of filler sections are arranged in the upper area of the heavy deoiling separation tower, a distributor is arranged between the adjacent filler sections, a supercritical solvent inlet is arranged in the area where the filler sections are arranged on the tower body and communicated between the adjacent filler sections through the distributor, a deasphalted oil phase inlet is arranged in the area, which is lower than the supercritical solvent inlet, of the heavy deoiling separation tower and communicated with a deasphalted oil phase outlet at the top of the extraction tower, and a heavy deoiling phase outlet is arranged at the bottom of the extraction tower.

Furthermore, the treatment system also comprises a supercritical solvent recovery tower, a light deoiling phase outlet of the heavy deoiling separation tower is communicated with a material inlet of the supercritical solvent recovery tower, a supercritical solvent outlet of the supercritical solvent recovery tower is respectively communicated with a supercritical solvent inlet of the static mixer, the extraction tower and the heavy deoiling separation tower, and a light deoiling phase outlet is arranged at the bottom of the supercritical solvent recovery tower.

Further, the treatment system also comprises a light deoiling stripping tower, a heavy deoiling stripping tower and a deoiled asphalt flash stripping tower;

the light deoiling phase discharge port separated by the supercritical solvent recovery tower is communicated with the material inlet of the light deoiling stripping tower, and the solvent outlet of the light deoiling stripping tower is communicated with the solvent tank through a pipeline;

a heavy deoiling phase discharge port separated by the heavy deoiling separation tower is communicated with a material inlet of the heavy deoiling stripping tower, and a solvent outlet of the heavy deoiling stripping tower is communicated with the solvent tank through a pipeline;

In the heavy oil separation method, a plurality of filler sections are additionally arranged in the upper areas of the extraction tower and the heavy oil separation tower, and the supercritical solvent is introduced by the distributor arranged between the filler sections, so that the aim of performing single-tower multistage separation on the heavy oil raw material is fulfilled, and the separation effect of the heavy oil raw material is effectively improved. Moreover, because the temperature of the supercritical solvent from the supercritical solvent recovery tower is higher, the introduction of the supercritical solvent can establish a temperature gradient in the extraction tower and the heavy deoiling and separating tower, and the problem that the separation effect of the heavy oil raw material in the extraction process is not obvious in the prior art is effectively solved, so that the target product with high yield and excellent properties is obtained.

Drawings

FIG. 1 is a process flow diagram of the two-stage separation of a heavy oil feedstock according to the present invention.

FIG. 2 is a process flow diagram of the three stage separation of a heavy oil feedstock according to the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The heavy oil raw material adopted by the invention comprises heavy oil and oil sand asphalt obtained by petroleum exploitation, oil residue or catalytic cracking oil slurry obtained in the petroleum processing process and coal tar asphalt obtained in the coal chemical industry process, and the density of the heavy oil raw material at 20 ℃ is more than 0.934g/cm³Or a boiling point above 350 ℃.

In a specific embodiment, the main components of the main solvent, the secondary solvent and the supercritical solvent used in the present invention can be alkanes and cycloalkanes of C3-C5, and can be propane, n-butane, isobutane, n-pentane, isopentane and cyclopentane or their mixtures.

The first two-stage separation process of heavy oil includes the following steps:

as shown in fig. 1, a static mixer 1 is connected with an extraction tower 2, a solvent tank 6 is communicated with the static mixer 1 through a pipeline, so that a main solvent and a heavy oil raw material enter the static mixer 1 to be mixed, and then are sent into the extraction tower 2 to separate a deasphalted asphalt phase and a deasphalted oil phase; wherein the mass flow rate ratio of the main solvent to the heavy oil raw material is 1.5-5.0: 1; controlling the temperature of the static mixer 1 to be 50-200 ℃ and the pressure to be 3.0-10.0 MPa;

an auxiliary solvent inlet is arranged at the lower part of the extraction tower body 2, and a solvent in the solvent tank 6 enters the extraction tower 2 from the auxiliary solvent inlet of the extraction tower 2 through a pipeline to carry out countercurrent extraction on the deoiled asphalt phase; wherein the mass flow rate ratio of the secondary solvent to the heavy oil raw material is 0.1-1.0: 1; a supercritical solvent inlet is arranged in the area of the upper part in the extraction tower 2, which is provided with the filler section, and the supercritical solvent in the supercritical solvent recovery tower 3 enters the extraction tower 2 through the supercritical solvent inlet;

the upper region in the extraction tower 2 is provided with 3-5 packing sections which can be random packing or regular packing, and the specific surface area of the packing is more than or equal to 150m²/m³The void ratio is more than or equal to 0.95, a distributor is arranged between the adjacent filler sections, and the supercritical solvent in the supercritical solvent recovery tower 3 is introduced into the extraction tower 2 through the distributor between the filler sections, so that the supercritical solvent is contacted and mixed with the deasphalted oil in the extraction tower 2, and a deasphalted oil phase and a deasphalted asphalt phase are separated; wherein the mass flow rate ratio of the supercritical solvent to the heavy oil feedstock is from 0.1 to 1: 1; the temperature of the extraction tower 2 is 50-200 ℃, the pressure is 3.0-10.0, and the temperature of the top of the extraction tower 2 is 5-50 ℃ higher than the temperature of the bottom of the extraction tower;

the top of the extraction tower 2 is provided with a deasphalted oil phase outlet which is connected with a supercritical solvent recovery tower 3, the mixture of the deasphalted oil phase and the solvent flowing out from the top of the extraction tower 2 is sent into the supercritical solvent recovery tower 3 to recover the solvent, so that the solvent is separated from the deasphalted oil phase in a supercritical state, and the separated solvent returns to the extraction tower 2 and the static mixer 1 from the supercritical solvent recovery tower 3; wherein the supercritical solvent recovery tower 3 has a pressure 0.1-1MPa higher than that of the extraction tower 2, a temperature 10-150 deg.C higher than that of the extraction tower 2, and a comparative temperature T_r＝T/T_CBetween 0.992 and 1.20: (T_c，iIs the critical temperature of the solvent, x_iIs the mole fraction of each component, T is the supercritical tower temperature, T_cReferred to as the pseudo-critical temperature, in units of K);

the bottom of the supercritical solvent recovery tower 3 is provided with a deasphalted oil phase outlet, the deasphalted oil phase enters a deasphalted oil stripping tower 5 from the deasphalted oil phase outlet, and the solvent is further separated by steam stripping; the deasphalted oil stripping tower 5 is provided with a material discharge port and a solvent discharge port, and the solvent separated by the deasphalted oil stripping tower 5 returns to the solvent tank 6 from the solvent discharge port through a pipeline;

the deoiled asphalt phase separated in the extraction tower 2 enters a deoiled asphalt flash evaporation stripping tower 4 from a deoiled asphalt phase outlet arranged at the bottom of the extraction tower 2, and the solvent is further separated through stripping; the deoiled asphalt flash evaporation stripping tower 4 is provided with a material discharge port and a solvent discharge port, and the solvent separated by the deoiled asphalt flash evaporation stripping tower 4 returns to the solvent tank 6 from the solvent discharge port through a pipeline.

Secondly, a heavy oil three-stage separation method comprises the following specific processes:

as shown in fig. 2, the static mixer 01 is connected with the extraction tower 02, the solvent tank 08 is communicated with the static mixer 01 through a pipeline, so that the main solvent and the heavy oil raw material enter the static mixer 01 to be mixed, and then are sent into the extraction tower 02 to separate a deasphalted asphalt phase and a deasphalted oil phase; wherein the mass flow rate ratio of the main solvent to the heavy oil raw material is 1.5-5.0: 1; controlling the temperature of the static mixer to be 50-200 ℃ and the pressure to be 3.0-10.0 MPa;

the lower part of the tower body of the extraction tower 02 is provided with an auxiliary solvent inlet, and the solvent in the solvent tank 08 enters the extraction tower 02 from the auxiliary solvent inlet of the extraction tower 02 through a pipeline to carry out countercurrent extraction on the deoiled asphalt phase; wherein the mass flow rate ratio of the secondary solvent to the heavy oil feedstock is from 0.1 to 1.0: 1; a supercritical solvent inlet is arranged in the area of the upper part in the extraction tower 02, which is provided with the filler section, and the supercritical solvent in the supercritical solvent recovery tower 04 enters the extraction tower 02 through the supercritical solvent inlet;

the upper region in the extraction tower 02 is provided with 3-5 packing sections which can be random packing or regular packing, and the specific surface area of the packing is more than or equal to 150m²/m³Void ratio is not less than 0.95, a distributor is arranged between adjacent packing sections, and the supercritical solvent in the supercritical solvent recovery tower 04Introducing the critical solvent into the extraction tower 02 through a distributor between the packing sections so that the supercritical solvent is contacted and mixed with the deasphalted oil in the extraction tower 02 to separate a deasphalted oil phase and a deasphalted asphalt phase; wherein the supercritical solvent recovery tower 4 has a pressure 0.1-1MPa higher than that of the extraction tower 2, a temperature 10-150 deg.C higher than that of the extraction tower 2, and a comparative temperature T_r＝T/T_CBetween 0.992 and 1.20: (T_c，iIs the critical temperature of the solvent, x_iIs the mole fraction of each component, T is the supercritical tower temperature, T_cReferred to as pseudo-critical temperature in units of K), the mass flow ratio of supercritical solvent to heavy oil feedstock is 0.1-1: 1; the temperature of the extraction tower 02 is 50-200 ℃, the pressure is 3.0-10.0, and the temperature of the top of the extraction tower 02 is 5-50 ℃ higher than the temperature of the bottom of the extraction tower 02;

the top of the extraction tower 02 is provided with an deasphalted oil phase outlet which is connected with the heavy deoiling and separating tower 03, so that the deasphalted oil phase in the extraction tower 02 enters the heavy deoiling and separating tower 03. The upper region in the heavy deoiling and separating tower 03 is provided with 3-5 packing sections which can be random packing or regular packing, and the specific surface area of the packing is more than or equal to 150m²/m³The void ratio is more than or equal to 0.95, a distributor is arranged between the adjacent packing sections, and the supercritical solvent in the supercritical solvent recovery tower 04 is introduced into the heavy deoiling and separating tower 03 through the distributor between the packing sections, so that the supercritical solvent is in countercurrent contact with the deasphalted oil phase in the heavy deoiling and separating tower 03 to separate out a light deoiled phase and a heavy deoiled phase. Wherein the mass flow rate ratio of the supercritical solvent to the heavy oil feedstock is from 0.1 to 1: 1; controlling the temperature of the heavy deoiling and separating tower at 50-200 ℃ and the pressure at 3.0-10.0MPa, wherein the temperature of the top of the heavy deoiling and separating tower 03 is 5-50 ℃ higher than the temperature of the bottom of the tower;

the top of the heavy deoiling and separating tower 03 is provided with a light deoiling phase outlet which is connected with the supercritical solvent recovery tower 04, the mixture of the light deoiling phase and the solvent flowing out of the top of the heavy deoiling and separating tower 03 is sent into the supercritical solvent recovery tower 04 to recover the solvent, so that the solvent is separated from the light deoiling phase in a supercritical state, and the separated solvent returns to the extraction tower 02 and the heavy deoiling and separating tower 03 from the supercritical solvent recovery tower 04 respectively; wherein the pressure of the supercritical solvent recovery tower 04 is 0.1-1MPa higher than that of the extraction tower 02, and the temperature is 10-150 ℃;

the bottom of the heavy deoiling and separating tower 03 is provided with a heavy deoiling phase outlet, a heavy deoiling phase enters a heavy deoiling and stripping tower 06 from the heavy deoiling and separating tower, and a solvent is further separated through stripping; the heavy deoiling stripping tower 06 is provided with a material discharge port and a solvent discharge port, and the solvent separated by the heavy deoiling stripping tower 06 returns to the solvent tank 08 through a pipeline from the solvent discharge port;

the bottom of the supercritical solvent recovery tower 04 is provided with a light deoiling phase outlet, the light deoiling phase enters a light deoiling stripping tower 07 from the light deoiling phase outlet, and the solvent is further separated through stripping; the light deoiling stripping tower 07 is provided with a material discharge port and a solvent discharge port, and the solvent separated by the light deoiling stripping tower 07 returns to the solvent tank 08 through a pipeline from the solvent discharge port;

the solvent is further separated by stripping through a deoiled asphalt phase separated in the extraction tower 02 from a deoiled asphalt phase flash evaporation stripping tower 05 arranged at the bottom of the extraction tower 02; the deoiled asphalt flash stripping tower 05 is provided with a material discharge port and a solvent discharge port, and the solvent separated by the deoiled asphalt flash stripping tower 05 returns to the solvent tank 08 through a pipeline from the solvent discharge port.

Example 1

Petroleum residuum (boiling point >420 ℃) is adopted as a raw material, and a C3-C4 mixed solvent (wherein, the main solvent, the auxiliary solvent and the supercritical solvent are all the mixed solvent) is adopted, and the composition of the mixed solvent is as follows:

components	Propane	Isobutane	N-butane
				Composition, m%	25	50	25

As shown in fig. 2, the petroleum residual oil is separated by a three-stage separation method, and the specific process refers to the three-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the petroleum residue is 2.4: 1;

2) the mass flow rate ratio of the secondary solvent to the petroleum residue is 0.1: 1;

3) the temperature for mixing the petroleum residual oil and the main solvent is 120 ℃, and the pressure is 4.6 MPa;

4) 3 sections of packing are filled in the upper area in the extraction tower 02, the packing is random theta ring packing, and the specific surface area of the packing is 150m²/m³The porosity is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths, the 2 paths of solvents pass through the distributor and enter the extraction tower 02, the introduction directions of the solvents are kept upward, the temperature of the top of the extraction tower 02 is 8 ℃ higher than that of the bottom of the extraction tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.25: 1;

5) 3 sections of packing are filled in the upper area in the heavy deoiling and separating tower 03, the packing is random theta ring packing, and the specific surface area of the packing is 150m²/m³The void ratio is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths and enters the heavy deoiling and separating tower 03 through the distributor, the introduction direction of each path of solvent is kept upward, and the temperature at the top of the heavy deoiling and separating tower 03 is highThe mass flow rate ratio of the supercritical solvent to the petroleum residuum is 0.25:1 at a bottom temperature of 10 ℃;

6) the pressure of the extraction tower 02 is 4.3MPa, and the temperature is 125 ℃; the temperature of the heavy deoiling and separating tower is 135 ℃, and the pressure is 4.2 MPa.

7) The pressure of the supercritical solvent recovery column 04 was 4.9MPa, the temperature was 165 ℃, and the comparative temperature Tr was 1.094.

According to the solvent deasphalting process of the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper area of the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom is avoided, the total solvent circulation amount of the comparative example is the same as that of the embodiment (the total solvent circulation amount is the main solvent, the auxiliary solvent, the supercritical solvent introduced into the extraction tower and the supercritical solvent introduced into the heavy deoiling and separating tower, the main solvent ratio is higher than that of the embodiment because the supercritical solvent is not introduced into the extraction tower and the heavy deoiling and separating tower, and the following examples are the same), and other relevant parameters are the same as those of the embodiment. Table 1 compares the light de-oiled phases of example 1 and the comparative example:

TABLE 1 comparison of light deoiled phases in example 1 and comparative example

Properties of	Raw materials	Comparative example light deoiling	Examples light deoiling
				Yield, m%	100	42.69	49.77
Density (20 ℃ 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 asphaltenes, μ g/g	5.45	0.085	0.050
				Ni，μg/g	39.7	1.2	0.8
V，μg/g	156	3.0	2.0

As can be seen from Table 1: the yield of the target product light deoiled phase in the example 1 is higher than that of the comparative example, the content of C7 asphaltene is reduced, and the content of Ni and V is reduced, so that the three-stage separation method in the example 1 effectively solves the problem that the separation effect of the heavy oil raw material in the extraction process is not obvious in the prior art, and the light deoiled phase with high yield and excellent property is obtained.

Example 2

Petroleum residuum (boiling point >420 ℃) is adopted as a raw material, and a C4 mixed solvent is adopted (wherein, the main solvent, the auxiliary solvent and the supercritical solvent are all the mixed solvent), and the composition of the mixed solvent is as follows:

components	Isobutane	N-butane
			Composition, m%	25	75

1) the mass flow rate ratio of the main solvent to the petroleum residue is 2.8: 1;

2) the mass flow rate ratio of the secondary solvent to the petroleum residue is 0.2: 1;

3) the mixing temperature of the petroleum residual oil and the main solvent is 100 ℃, and the pressure is 4.3 MPa;

4) 4 sections of packing are filled in the upper area in the extraction tower 02, the packing is random pall ring packing, and the specific surface area of the packing is 219m²/m³The porosity is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 3 paths, the 3 paths of solvents pass through the distributor and enter the extraction tower 02, the introduction direction of each path of solvent is kept downward, the temperature of the top of the extraction tower 02 is 15 ℃ higher than that of the bottom, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.5: 1;

5) 4 sections of packing are filled in the upper region in the heavy deoiling and separating tower 03, the packing is random pall ring packing, and the specific surface area of the packing is 219m²/m³The void ratio is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 3 paths, the 3 paths of solvents pass through the distributor and enter the heavy deoiling and separating tower 03, the introduction direction of each path of solvent is kept downward, the temperature of the top of the heavy deoiling and separating tower 03 is 15 ℃ higher than the temperature of the bottom of the heavy deoiling and separating tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.5: 1;

6) the pressure of the extraction tower 02 is 4.3MPa, and the temperature is 110 ℃; the temperature of the heavy deoiling and separating tower is 125 ℃, and the pressure is 4.1 MPa.

7) The pressure of the supercritical solvent recovery column 04 is 4.6MPa, the temperature is 180 ℃, and the comparative temperature Tr is 1.077.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 2 compares the light de-oiled phases of example 2 and the comparative example:

TABLE 2 comparison of the light deoiled phases in example 2 and comparative example

Properties of	Raw materials	Comparative example light deoiling	Examples light deoiling
				Yield, m%	100	68.26	75.68
Density (20 ℃ 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

[0090]

C7 asphaltenes, m%	5.45	0.2	0.12
				Ni，μg/g	39.7	3.4	4.3
V，μg/g	156	11.4	11.8

As can be seen from Table 2: the yield of the target product light deoiled phase in the example 2 is higher than that of the comparative example, the content of C7 asphaltene is reduced, the contents of Ni and V are equivalent, and the carbon residue is reduced, so that the three-stage separation method in the example 2 effectively solves the problem that the separation effect of the heavy oil raw material in the extraction process in the prior art is not obvious enough, and the light deoiled phase with high yield and excellent property is obtained.

Example 3

Bottoms (atmospheric residuum) (boiling point) from atmospheric distillation of canadian oil sand bitumen>The density at 350 ℃ and 20 ℃ is more than 1.0g/cm³) Mixing with C5A mixed solvent (wherein, the main solvent, the secondary solvent and the supercritical solvent are the mixed solvent), and the composition of the mixed solvent is as follows:

components	Isopentane	N-pentane
			Composition, m%	25	75

As shown in fig. 2, the atmospheric residue is separated by a three-stage separation method, and the specific process refers to the three-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the atmospheric residue was 2.75: 1;

2) the mass flow rate ratio of the secondary solvent to the atmospheric residue is 0.25: 1;

3) the mixing temperature of the atmospheric residue and the main solvent is 170 ℃, and the pressure is 4.0 MPa;

4) the upper area in the extraction tower 02 is filled with 3 sections of packing which is random metal intalox saddle ring packing, and the specific surface area of the packing is 185m²/m³The porosity is 0.96, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths, the 2 paths of solvents pass through the distributor and enter the extraction tower 02, the introduction directions of the solvents are kept upward, the temperature of the top of the extraction tower 02 is 8 ℃ higher than the temperature of the bottom of the extraction tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.25: 1;

5) 4 sections of packing are filled in the upper region in the heavy deoiling and separating tower 03, the packing is pore plate corrugated regular packing, and the specific surface area of the packing is 250m²/m³The void ratio is 0.984, a distributor is arranged between the filler sections, the supercritical solvent is divided into 3 paths, the 3 paths of solvents pass through the distributor and enter the heavy deoiling and separating tower 03, the introduction direction of each path of solvent is kept upward, the temperature of the top of the heavy deoiling and separating tower 03 is 15 ℃ higher than the temperature of the bottom, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.5: 1;

6) the pressure of the extraction tower 02 is 4.3MPa, and the temperature is 175 ℃; the temperature of the heavy deoiling and separating tower is 185 ℃, and the pressure is 4.1 MPa.

7) The pressure of the supercritical solvent recovery column 04 was 4.5MPa, the temperature was 250 ℃, and the comparative temperature Tr was 1.12.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 3 is a comparison of the light de-oiled phases in example 3 and the comparative example:

TABLE 3 comparison of the light deoiled phases in example 3 with the comparative examples

Properties of	Raw materials	Comparative example light deoiling	Examples light deoiling
				Yield, m%	100	84	87
Density (20 ℃ 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 asphaltenes, m%	15.0	0.3	0.1
				Ni，μg/g	80	30	25
V，μg/g	220	90	78

As can be seen from Table 3: the yield of the target product light deoiled phase in the example 3 is higher than that of the comparative example, the content of C7 asphaltene is reduced, the contents of Ni and V are equivalent, and the carbon residue is reduced, so that the problem that the separation effect of the heavy oil raw material in the extraction process in the prior art is not obvious enough is effectively solved by the three-stage separation method in the example 3, and the light deoiled phase with high yield and excellent property is obtained.

Example 4

Vacuum residuum (boiling point) from canadian oil sand bitumen>The density at 524 ℃ and 20 ℃ is more than 1.0596g/cm³C7 asphaltene is up to 18.1 m%) as raw material, and n-pentane is used as solvent (wherein, the main solvent, the auxiliary solvent and the supercritical solvent are all the solvents);

as shown in fig. 2, the vacuum residue is separated by a three-stage separation method, and the specific process refers to the three-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the vacuum residue was 3.0: 1;

2) the mass flow rate ratio of the secondary solvent to the vacuum residue is 0.5: 1;

3) the mixing temperature of the vacuum residue and the main solvent is 160 ℃, and the pressure is 7.0 MPa;

4) 3 sections of packing are filled in the upper region in the extraction tower 02, the packing is random metal stepped ring packing, and the specific surface area of the packing is 221m²/m³The porosity is 0.951, a distributor is arranged between the packing sections, the supercritical solvent is divided into 2 paths and enters the extraction tower 02 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the extraction tower 02 is 10 ℃ higher than that of the bottom of the extraction tower 02, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.4: 1;

5) heavy deoiling separation4 sections of packing are filled in the upper area in the tower 03, the packing is random metal stepped ring packing, and the specific surface area of the packing is 221m²/m³The void ratio is 0.951, a distributor is arranged between the packing sections, the supercritical solvent is divided into 3 paths and enters the heavy deoiling and separating tower 03 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the heavy deoiling and separating tower 03 is 12 ℃ higher than the temperature of the bottom, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.6: 1;

6) the pressure of the extraction tower 02 is 7.0MPa, and the temperature is 165 ℃; the temperature of the heavy deoiling and separating tower is 176 ℃, and the pressure is 6.7 MPa.

7) The pressure of the supercritical solvent recovery column 04 was 7.6MPa, the temperature was 275 ℃, and the comparative temperature Tr was 1.17.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 4 compares the light de-oiled phases of example 4 and the comparative example:

TABLE 4 comparison of the light deoiled phases in example 4 and comparative example

Properties of	Raw materials	Comparative example light deoiling	Examples light deoiling
				Yield, m%	100	65	72
Density (20 ℃ 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 asphaltenes, m%	18.1	0.2	＜0.1
				Ni，μg/g	104	39.1	35
V，μg/g	280	85.4	80

As can be seen from Table 4: the yield of the target product light deoiled phase in the example 4 is higher than that of the comparative example, the content of C7 asphaltene is reduced, the contents of Ni and V are equivalent, and the carbon residue is reduced, so that the problem that the separation effect of the heavy oil raw material in the extraction process in the prior art is not obvious enough is effectively solved by the three-stage separation method in the example 4, and the light deoiled phase with high yield and excellent property is obtained.

Example 5

Using Venezuela extra heavy oil (boiling point)>The density at 420 ℃ and 20 ℃ is more than 1.0g/cm³) The preparation method comprises the following steps of (1) taking a C5 mixed solvent as a raw material (wherein a main solvent, a secondary solvent and a supercritical solvent are all the mixed solvent), wherein the mixed solvent comprises the following components:

components	N-pentane	Cyclopentane
			Composition, m%	88	12

As shown in fig. 2, the heavy oil is separated by a three-stage separation method, and the specific process refers to the three-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the heavy oil is 2.4: 1;

2) the mass flow rate ratio of the secondary solvent to the heavy oil is 0.2: 1;

3) the mixing temperature of the heavy oil and the main solvent is 160 ℃, and the pressure is 5.0 MPa;

4) 3 sections of packing are filled in the upper area in the extraction tower 02, the packing is calendering corrugated regular packing, and the specific surface area of the packing is 500m²/m³The porosity is 0.975, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths and enters the extraction tower 02 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the extraction tower 02 is 10 ℃ higher than that of the bottom of the extraction tower 02, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.3: 1;

5) 4 sections of packing are filled in the upper region in the heavy deoiling and separating tower 03, the packing is pore plate corrugated regular packing, and the specific surface area of the packing is 250m²/m³The porosity is 0.984, a distributor is arranged between the filler sections, the supercritical solvent is divided into 3 paths and enters the heavy deoiling and separating tower 03 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the heavy deoiling and separating tower 03 is 15 ℃ higher than the temperature of the bottom, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.6: 1;

6) the pressure of the extraction tower 02 is 5.0MPa, and the temperature is 165 ℃; the temperature of the heavy deoiling and separating tower is 178 ℃, and the pressure is 4.8 MPa.

7) The pressure of the supercritical solvent recovery column 04 is 5.6MPa, the temperature is 250 ℃, and the comparison temperature Tr is 1.075.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 5 compares the light de-oiled phases of example 5 and the comparative example:

TABLE 5 comparison of light deoiled phases in example 5 and comparative example

Properties of	Raw materials	Comparative example light deoiling	Examples light deoiling
				Yield, m%	100	76.6	79.8
Density (20 ℃ C.), g/cm³	1.0281	0.9967	0.9890
				Viscosity (100 ℃ C.), mPa.s	2966.3	295	200
Carbon residue, m%	21.05	9.92	9.42
				Asphaltenes, m%	12.05	0.79	0.25
S，m％	4.0	3.5	3.6
				N，m％	0.76	0.27	0.27
Ni，μg/g	118	38.3	28
				V，μg/g	531	147.7	111

As can be seen from Table 5: the yield of the target product light deoiled phase in the example 5 is higher than that of the comparative example, the content of C7 asphaltene is reduced, the contents of Ni and V are equivalent, and the carbon residue is reduced, so that the problem that the separation effect of the heavy oil raw material in the extraction process in the prior art is not obvious enough is effectively solved by the three-stage separation method in the example 5, and the light deoiled phase with high yield and excellent property is obtained.

Example 6

The method adopts certain catalytic cracking slurry oil as a raw material, adopts a C4 mixed solvent (wherein, the main solvent, the auxiliary solvent and the supercritical solvent are all the mixed solvent), and the composition of the mixed solvent is as follows:

components	Isobutane	N-butane
			Composition, m%	25	75

As shown in fig. 1, the heavy oil is separated by a two-stage separation method, and the specific process refers to the two-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the catalytic cracking slurry oil is 3.2: 1;

2) the mass flow rate ratio of the secondary solvent to the catalytic cracking slurry oil is 0.3: 1;

3) the mixing temperature of the catalytic cracking slurry oil and the main solvent is 100 ℃, and the pressure is 4.3 MPa;

4) 3 sections of packing are filled in the upper region in the extraction tower 2, the packing is calendering corrugated regular packing, and the specific surface area of the packing is 500m²/m³The porosity is 0.975, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths and enters the extraction tower 02 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the extraction tower 2 is higher than the temperature of the bottom by 13 ℃, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.5: 1;

5) the pressure of the extraction column 02 was 4.3MPa and the temperature was 107 ℃.

6) The pressure of the supercritical solvent recovery column 3 was 4.6MPa, the temperature was 190 ℃, and the comparative temperature Tr was 1.10.

According to the prior art, the solvent deasphalting process is taken as a comparative example, in the comparative example, a supercritical solvent is not added into an extraction tower, a multi-section filling section is not additionally arranged in the upper area in the extraction tower, the temperature difference between the top and the bottom is avoided, and other relevant parameters are the same as those in the embodiment. Table 6 is a comparison of the deasphalted oil phases of example 6 and the comparative example:

TABLE 6 comparison of deasphalted oil phases in example 6 and comparative examples

As can be seen from Table 6: the yield of the deasphalted oil phase of the target product in the example 6 is higher than that of the comparative example, the content of C7 asphaltene is obviously reduced, the content of metal is slightly reduced, the content of aromatic hydrocarbon is improved compared with that of the comparative example, and the product is more favorable for being used as a raw material for producing high-quality carbon materials.

Example 7

components

Isobutane

N-butane

[0153]

Composition, m%

90

10

As shown in fig. 2, a three-stage separation method is used to separate the catalytic cracking slurry oil, and please refer to the three-stage separation method. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the catalytic cracking slurry oil is 2.85: 1;

2) the mass flow rate ratio of the secondary solvent to the catalytic cracking slurry oil is 0.35: 1;

3) the mixing condition of the catalytic cracking slurry oil and the main solvent is that the temperature is 90 ℃ and the pressure is 4.3 MPa;

4) 3 sections of packing are filled in the upper region in the extraction tower 02, the packing is random pall ring packing, and the specific surface area of the packing is 219m²/m³The porosity is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths, the 2 paths of solvents pass through the distributor and enter the extraction tower 02, the introduction direction of each path of solvent is kept downward, the temperature of the top of the extraction tower 02 is 10 ℃ higher than the temperature of the bottom of the extraction tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.25: 1;

5) 4 sections of packing are filled in the upper region in the heavy deoiling and separating tower 03, the packing is calendering corrugated regular packing, and the specific surface area of the packing is 450m²/m³The void ratio is 0.97, a distributor is arranged between the filler sections, the supercritical solvent is divided into 3 paths and enters the heavy deoiling and separating tower 03 through the distributor, the introduction direction of each path of solvent is kept downward, the temperature of the top of the heavy deoiling and separating tower 03 is higher than the temperature of the bottom by 20 ℃, and the supercritical solvent and the petroleum residual oil are mixedThe mass flow ratio is 1: 1;

6) the pressure of the extraction tower 02 is 4.3MPa, and the temperature is 95 ℃; the temperature of the heavy deoiling and separating tower is 110 ℃, and the pressure is 4.2 MPa.

7) The pressure of the supercritical solvent recovery column 04 was 4.6MPa, the temperature was 180 ℃, and the comparative temperature Tr was 1.105.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 7 compares the light de-oiled phases of example 7 and the comparative example:

TABLE 7 comparison of light deoiled phases in example 7 and comparative example

As can be seen from Table 7: the yield of the target product in the example 7 in the light deoiling phase is higher than that in the comparative example, the content of C7 asphaltene is reduced, the contents of Ni and V are equivalent, the carbon residue is reduced, the content of saturated hydrocarbon is higher, the method is more favorable for being used as bunker fuel oil and returning to catalytic cracking to be used as raw oil, the density of the heavy deoiling phase is improved, and the heavy deoiling phase can be used as a high-quality carbon material.

Example 8

The method comprises the following steps of (1) adopting certain coal tar pitch (the boiling point is more than 350 ℃) as a raw material and adopting n-pentane as a solvent (wherein a main solvent, an auxiliary solvent and a supercritical solvent are all the solvents);

as shown in fig. 2, a three-stage separation method is used to separate coal tar pitch, and please refer to the three-stage separation method for the specific process. The method comprises the following steps of:

1) the mass flow rate ratio of the main solvent to the coal tar pitch is 2.3: 1;

2) the mass flow rate ratio of the secondary solvent to the coal tar pitch is 0.1: 1;

3) the mixing condition of the coal tar pitch and the main solvent is that the temperature is 150 ℃ and the pressure is 6.0 MPa;

4) 2 sections of packing are filled in the upper area in the extraction tower 02, the packing is random pall ring packing, and the specific surface area of the packing is 219m²/m³The porosity is 0.95, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths, the 2 paths of solvents pass through the distributor and enter the extraction tower 02, the introduction directions of the solvents are kept upward, the temperature of the top of the extraction tower 02 is 5 ℃ higher than that of the bottom of the extraction tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.2: 1;

5) 3 sections of packing are filled in the upper region in the heavy deoiling and separating tower 03, the packing is random pall ring packing, and the specific surface area of the packing is 300m²/m³The void ratio is 0.97, a distributor is arranged between the filler sections, the supercritical solvent is divided into 2 paths, the 2 paths of solvents pass through the distributor and enter the heavy deoiling and separating tower 03, the introduction direction of each path of solvent is kept upward, the temperature of the top of the heavy deoiling and separating tower 03 is 10 ℃ higher than the temperature of the bottom of the heavy deoiling and separating tower, and the mass flow rate ratio of the supercritical solvent to the petroleum residual oil is 0.4: 1;

6) the pressure of the extraction tower 02 is 6.0MPa, and the temperature is 153 ℃; the temperature of the heavy deoiling and separating tower is 163 ℃ and the pressure is 5.7 MPa.

7) The pressure of the supercritical solvent recovery column 04 is 6.5MPa, the temperature is 230 ℃, and the comparison temperature Tr is 1.072.

According to the solvent deasphalting process in the prior art as a comparative example, in the comparative example, no supercritical solvent is added into an extraction tower and a heavy deoiling and separating tower, a multi-section packing section is not additionally arranged in the upper areas in the extraction tower and the heavy deoiling and separating tower, the temperature difference between the top and the bottom of the tower is avoided, and other relevant parameters are the same as those in the embodiment. Table 8 compares the light de-oiled phases of example 8 and the comparative example:

TABLE 8 comparison of light deoiled phases in example 8 and comparative example

As can be seen from Table 8: the yield of the target product light deoiled phase in the example 8 is higher than that of the comparative example, and the content of C7 asphaltene is reduced, so that the problem that the separation effect of the heavy oil raw material in the extraction process in the prior art is not obvious enough is effectively solved by the three-stage separation method in the example 8, and the light deoiled phase with high yield and excellent property is obtained.

Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims

1. A heavy oil separation method is characterized in that an extraction tower with a plurality of packing sections arranged in the upper area is adopted, a distributor is arranged between the adjacent packing sections, and supercritical solvent from a supercritical solvent recovery tower is introduced through the distributor to further separate heavy components in a deasphalted oil phase at the upper part of the extraction tower, wherein the separation method comprises the following steps:

2. The heavy oil separation process of claim 1, further comprising:

3. The heavy oil separation process of claim 1, wherein the separated mixture of deasphalted oil phase and solvent is discharged from the top of the extraction column and fed to a heavy deoiling and separating column, the heavy deoiling and separating column being provided in an upper region thereof with a plurality of packing sections with distributors disposed between adjacent packing sections, and the supercritical solvent is introduced into the heavy deoiling and separating column through the distributors between the packing sections;

4. The heavy oil separation process of claim 3, further comprising:

5. A heavy oil separation method according to claim 2 or 4, wherein the pressure of the supercritical solvent recovery column is 0.1 to 1MPa higher than the pressure of the extraction column, and the temperature in the supercritical solvent recovery column is 10 to 150 ℃ higher than the temperature in the extraction column.

6. A heavy oil separation method according to claim 5, wherein the supercritical recovery of solvent is carried out in the supercritical solvent recovery column under conditions such that: pressure 3.0-10.0MPa, temperature 94-280 deg.C, and contrast temperature T_r＝T/T_CBetween 0.992 and 1.20; wherein,

T_c，iis the critical temperature of the solvent, x_iIs the mole fraction of each component, T is the supercritical tower temperature, T_cReferred to as the pseudo-critical temperature, in units of K.

7. The method of claim 1 or 3The heavy oil separation method is characterized in that the filling section is 3-5 sections, the filling mode is random packing or regular packing, and the specific surface area of the packing is more than or equal to 150m²/m³The porosity is more than or equal to 0.95.

8. The heavy oil separation process of claim 1, wherein the heavy oil feedstock comprises heavy oil and oil sand bitumen obtained from oil recovery, residual oil or catalytically cracked oil slurry obtained from petroleum processing, or coal tar pitch obtained from coal chemical engineering processes, and has a density of > 0.934g/cm at 20 ℃³Or a boiling point above 350 ℃.

9. The heavy oil separation process of claim 1, wherein the major components of the primary, secondary and supercritical solvents are both C3-C5 alkanes and cycloalkanes.

10. A processing system for performing a heavy oil separation process according to any one of claims 1-9, wherein the processing system comprises a static mixer, an extraction column, a solvent tank, and a stripping column;

11. The processing system according to claim 10, further comprising a supercritical solvent recovery tower, wherein the material inlet of the supercritical solvent recovery tower is communicated with the deasphalted oil phase outlet at the top of the extraction tower, the supercritical solvent outlet of the supercritical solvent recovery tower is communicated with the static mixer and the supercritical solvent inlet of the extraction tower, and the deasphalted oil phase outlet is arranged at the bottom of the supercritical solvent recovery tower.

12. The processing system of claim 11, further comprising a deasphalted oil stripper and a deasphalted asphalt flash stripper;

13. The treatment system according to claim 10, further comprising a heavy deoiling separation tower, wherein a plurality of packing sections are arranged at the upper region of the heavy deoiling separation tower, a distributor is arranged between the adjacent packing sections, a supercritical solvent inlet is arranged at the region of the tower body where the packing sections are arranged and communicated between the adjacent packing sections through the distributor, a deasphalted oil phase inlet is arranged below the supercritical solvent inlet region of the heavy deoiling separation tower, a light deoiled phase outlet is arranged at the top of the heavy deoiling separation tower, and a heavy deoiled phase outlet is arranged at the bottom of the heavy deoiling separation tower.

14. The treatment system according to claim 13, further comprising a supercritical solvent recovery tower, wherein the light deoiling phase outlet of the heavy deoiling separation tower is communicated with the material inlet of the supercritical solvent recovery tower, the supercritical solvent outlet of the supercritical solvent recovery tower is respectively communicated with the supercritical solvent inlets of the static mixer, the extraction tower and the heavy deoiling separation tower, and the bottom of the supercritical solvent recovery tower is provided with a light deoiling phase outlet.

15. The process system of claim 14, further comprising a light de-oiling stripper, a heavy de-oiling stripper, and a de-oiled asphalt flash stripper;