CN108264934B

CN108264934B - Suspension bed hydrogenation process for treating heavy oil

Info

Publication number: CN108264934B
Application number: CN201611255873.2A
Authority: CN
Inventors: 李林; 林科
Original assignee: Beijing Huashi United Energy Technology and Development Co Ltd
Current assignee: Beijing Huashi United Energy Technology and Development Co Ltd
Priority date: 2016-12-30
Filing date: 2016-12-30
Publication date: 2020-03-17
Anticipated expiration: 2036-12-30
Also published as: CN108264934A; RU2681078C1

Abstract

The invention provides a suspension bed hydrogenation process for treating heavy oil, which mixes part of raw oil with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carries out primary shearing and secondary shearing on the mixture, so that high-dispersion mixing of the catalyst and the raw oil can be realized to obtain catalyst slurry, the catalyst can better exert the hydrogenation catalytic activity, and the conversion rate of the raw oil and the yield of light oil are improved; and then the catalyst slurry, the residual raw oil and hydrogen are mixed and then are fed into a suspension bed hydrogenation reactor, the suspension bed hydrogenation conditions are controlled to obtain a suspension bed hydrogenation product, and a reasonable separation process is adopted according to the composition and the properties of the suspension bed hydrogenation product, so that the hydrogenation load of the fixed bed is greatly reduced, more importantly, the yield and the quality of light oil are improved to the maximum extent, the service life of the fixed bed catalyst can be effectively prolonged, and the energy conservation and emission reduction of the whole process are facilitated.

Description

Suspension bed hydrogenation process for treating heavy oil

Technical Field

The invention relates to the technical field of coal and petrochemical industry, in particular to a suspension bed hydrogenation process for treating heavy oil.

Background

In recent years, with the increasing shortage of petroleum resources worldwide, the trend of heavy inferior crude oil is getting worse, the demand of heavy fuel oil in the market is rapidly reduced, and the demand of light fuel oil is continuously and rapidly increased, the deep processing technology of heavy inferior oil is promoted to become the key and difficult point of the development of the oil refining industry. In addition to the basic national conditions of poor oil and rich coal in China, some petrochemical products can be obtained from products such as coal gasification and dry distillation, and the like, so that the light oil and the chemical products are produced by utilizing the advanced coal conversion technology, the method not only has a positive promoting effect on adjusting the industrial structure and improving the industrial energy level of the chemical industry, but also is a strategic measure for lightening the dependence of China on petroleum import, developing the circular economy, reducing the environmental pollution and guaranteeing the energy safety and the economic sustainable development of China in the 21 st century.

The suspension bed hydrogenation process is one of the ideal methods for realizing the heavy oil lightening, and the process generally comprises the steps of uniformly mixing a dispersed catalyst and raw oil to form slurry, then feeding the slurry and high-pressure hydrogen into a suspension bed reactor together to perform catalytic hydrogenation and cracking reactions under the hydrogen condition, and finally preparing light oil products such as naphtha, light oil and the like. For example, chinese patent document CN104388117A discloses a method for producing high-quality fuel oil by hydrocracking heavy oil, which comprises the following steps: (1) mixing heavy oil with a suspension bed hydrocracking catalyst and hydrogen, and then feeding the mixture into a suspension bed hydrocracking reactor, wherein the operating pressure of the suspension bed hydrocracking reactor is 12-20MPa, the temperature is 400-^-1(ii) a (2) Separating the reactants of step (1) under high pressureSeparating in the reactor, directly feeding the gas-phase product into a fixed bed reaction device for hydrogenation reaction, and feeding the liquid-phase product into a reduced pressure distillation tower; the reduced pressure distillation tower obtains a light component product and a heavy component product, the light component product enters a fixed bed reaction device, and the heavy component is discharged; (3) and separating hydrogen and light hydrocarbon from the product obtained by the fixed bed reaction device, then feeding the product into a fractionating tower to obtain gasoline and diesel oil, and circulating the heavy component oil from the bottom of the fractionating tower into the fixed bed reaction device.

Although the above-mentioned technology can finally obtain high-quality light oil by carrying out fixed bed hydrocracking, refining and upgrading treatment again on the light components in the suspension bed hydrogenation product, the above-mentioned technology still has the following defects: 1) the heavy oil and the hydrocracking catalyst of the suspension bed are simply mixed and then are sent into a hydrocracking reactor of the suspension bed, if the density of the catalyst is higher, the heavy oil is easy to precipitate at the bottom of a container, and if the density of the catalyst is lower, the heavy oil is easy to float on the surface of an oil phase to form an encapsulated substance, the two conditions can influence the solid-liquid mixing effect, the hydrogenation performance of the suspension bed is further influenced, and finally the yield of light oil products is lower; 2) as only one suspension bed reactor is adopted, three reactions of cracking, hydrogenation and coke adsorption can not be ensured to be carried out under respective proper environmental conditions, incomplete cracking, insufficient hydrogenation and incomplete coke adsorption are caused, so that the liquid yield of the whole process is low, the coke yield is high, the tendency of oil product condensation coking is higher when the cracking reaction temperature is higher, the coking can also cause the inactivation of a hydrogenation catalyst and the device can not stably run for a long period; 3) the hydrogenation product of the suspension bed enters the fixed bed reactor too early without reasonable separation, so that the hydrogenation load of the fixed bed is increased, the liquid yield and the oil product are influenced, and the energy conservation and emission reduction are not facilitated.

In view of this, there is an urgent need in the art to improve the existing suspension bed hydrogenation process to enhance the mixing effect of the catalyst and the feedstock oil, ensure the smooth progress of each reaction, and optimize the separation method, so as to improve the quality of the liquid and the light oil, and at the same time, achieve energy saving and emission reduction, and reduce the process cost to the utmost extent.

Disclosure of Invention

The invention aims to overcome the defects of nonuniform mixing of a catalyst and raw oil, insufficient reaction and unsatisfactory separation effect of hydrogenation products in the conventional suspension bed hydrogenation process, and further provides a suspension bed hydrogenation process for treating heavy oil, which has the advantages of uniform mixing of the catalyst and the raw oil, sufficient reaction, good separation effect, high yield and quality of light oil products, high yield and quality of asphalt, energy conservation and emission reduction.

Therefore, the technical scheme adopted by the invention for realizing the purpose is as follows:

a suspension bed hydrogenation process for treating heavy oil comprises the following steps:

(1) mixing part of raw oil with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carrying out primary shearing and secondary shearing on the mixture to obtain catalyst slurry;

(2) mixing the catalyst slurry with the rest raw oil and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 18-22.5 MPa, the temperature to be 390-460 ℃, and the volume ratio of hydrogen to oil to be 800-1500 so as to carry out hydrocracking reaction;

(3) carrying out thermal high-pressure separation on the suspension bed hydrogenation product obtained in the step (2), and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure separation gas is subjected to cold high-pressure separation and cold low-pressure separation in sequence to obtain cold low-pressure separation oil, the hot high-pressure separation oil is subjected to hot low-pressure separation to obtain hot low-pressure separation gas and hot low-pressure separation oil, the hot low-pressure separation gas and the cold low-pressure separation oil are subjected to steam stripping separation and then are converted into dry gas, naphtha and tower bottom oil, the hot low-pressure separation oil is subjected to reduced pressure distillation, and the first line oil and the second line oil are collected.

Preferably, in the catalyst slurry, the suspension bed hydrocracking catalyst is 0.1-10% by mass, and the particle size is 5-500 μm.

Preferably, the suspension bed hydrocracking catalyst comprises a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: (0.5-10), wherein:

the active metal is a metal of a VIII group and/or a VIB group;

the composite carrier comprises a semi-coke pore-enlarging material, a molecular sieve and a catalytic cracking waste catalyst, wherein the mass ratio of the semi-coke pore-enlarging material to the molecular sieve to the catalytic cracking waste catalyst is (1-5) to (2-4) to (0.5-5);

the specific surface area of the semi-coke reaming material is 150-300 m²(ii)/g, the average pore diameter is 70-80 nm;

the specific surface area of the molecular sieve is 200-300 m²(ii)/g, the average pore diameter is 5-10 nm;

the specific surface area of the catalytic cracking waste catalyst is 50-300 m²(ii)/g, the average pore diameter is 3 to 7 nm.

Preferably, the catalytic cracking spent catalyst comprises the following components in parts by weight:

15-55 parts of a Y-type molecular sieve;

15-55 parts of aluminum oxide;

0.5-1 part of at least one of nickel, vanadium or iron.

Preferably, the raw oil is an oil product subjected to purification treatment, and the purification treatment comprises the following steps:

contacting the raw oil with an adsorbent in a fluidized state to generate adsorption, and collecting a liquid phase after adsorption is finished; the adsorbent is semi-coke and/or kaolin.

Preferably, the adsorption is carried out at 50-100 ℃ and 0-1.0 MPa, and the mass ratio of the raw oil to the adsorbent is 1: (0.05-0.2), the specific surface area of the semi-carbon is 100-500m²The specific surface area of the kaolin is 50-200m²/g。

Preferably, the suspension bed hydrogenation reactor comprises two reactors connected in series, wherein one reactor is a suspension bed hydrocracking reactor, the other reactor is a suspension bed hydrogenation stabilizing reactor, and the operating temperature in the suspension bed hydrogenation stabilizing reactor is 20-50 ℃ lower than that in the suspension bed hydrocracking reactor.

Preferably, the catalyst slurry, the residual raw oil and hydrogen are mixed and then enter the suspension bed hydrocracking reactor to carry out hydrocracking reaction, so as to obtain a hydrocracking product; then sending the hydrocracking product into the suspension bed hydrogenation stabilization reactor, and carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst, thereby forming the suspension bed hydrogenation product;

the suspension bed hydrogenation stable catalyst is a supported catalyst which takes alumina as a carrier and is loaded with hydrogenation active metals, and the hydrogenation active metals are VIII group and/or VIB group metals.

Preferably, in the step (3), the hot low-molecular oil is distilled under normal pressure, and fractions at 150 to 250 ℃ and fractions at more than 250 ℃ are respectively collected; and heating the fraction at the temperature of more than 250 ℃, then carrying out reduced pressure distillation, and combining the fraction at the temperature of 150-250 ℃ with the naphtha.

Preferably, the reduced pressure distillation also obtains a third-line-reduced oil, 80-90 wt% of the third-line-reduced oil and 5-20 wt% of the third-line-reduced oil are combined to be used as a third-line-reduced washing liquid, the remaining 10-20 wt% of the third-line-reduced oil is used as a hot low-fraction washing liquid, the oil gas generated by the hot low-pressure separation is washed to obtain the hot low-fraction gas, meanwhile, a hot low-fraction washing recovery liquid is also obtained, and 30-90 wt% of the hot low-fraction washing recovery liquid is recycled to be used as the hot low-fraction washing liquid;

the distillation range of the minus wire oil is consistent with the operating temperature of the hot low-pressure separation.

Further, still include: and (3) feeding the first-line reducing oil, the second-line reducing oil and the tower bottom oil into a fixed bed hydrogenation reactor for carrying out hydrogenation treatment again, then separating a fixed bed hydrogenation product, and collecting a light oil product with the temperature of less than 350 ℃.

Preferably, the process parameters of the thermal high-pressure separation are as follows: the pressure is 18-22.5 MPa, and the temperature is 350-460 ℃;

the technological parameters of the cold high-pressure separation are as follows: the pressure is 18-22.5 MPa, and the temperature is 30-60 ℃;

the technological parameters of the cold low-pressure separation are as follows: the pressure is 0.5-1.5 MPa, and the temperature is 30-60 ℃;

the technological parameters of the thermal low-pressure separation are as follows: the pressure is 0.5-1.5 MPa, and the temperature is 350-430 ℃;

the temperature of the steam stripping separation is 80-90 ℃;

the first-line reduction operating temperature in the reduced pressure distillation is 110-210 ℃, and the second-line reduction operating temperature is 200-300 ℃;

controlling the operating pressure in the fixed bed hydrogenation reactor to be 18-22.5 MPa, the temperature to be 360-420 ℃, the hydrogen-oil volume ratio to be 500-1500 and the volume space velocity to be 0.5-1.5 h^-1。

Preferably, the cold high-pressure gas obtained by the cold high-pressure separation is used as circulating hydrogen, and the cold low-pressure gas obtained by the cold high-pressure separation is mixed with the dry gas to be used as fuel gas after the cold high-pressure oil is subjected to the cold low-pressure separation.

Preferably, a discharge system is connected with the suspension bed hydrogenation reactor and comprises a discharge pipeline, a cooling separation system, a torch system and a raw oil recycle system, wherein one end of the discharge pipeline is connected with the bottom of the suspension bed hydrogenation reactor, and the other end of the discharge pipeline is connected with the cooling separation system;

when the temperature of the suspension bed hydrogenation reactor rises to exceed the normal reaction temperature instantly, closing a feed valve of the suspension bed hydrogenation reactor, and opening a discharge valve group in the cooling separation system, so that the material in the suspension bed hydrogenation reactor is reduced to 0.6-1.0MPa through a pressure reduction pore plate on a discharge pipeline and then discharged into the cooling separation system for cooling separation treatment to obtain a gas phase material and a liquid-solid phase material, the gas phase material is discharged to the torch system, and the liquid-solid phase material is conveyed to the raw oil recycling system, thereby realizing the emergency discharge of the suspension bed hydrogenation reactor;

more preferably, the material in the suspension bed hydrogenation reactor firstly enters a discharge tank of the cooling separation system, and is mixed with the flushing oil in the discharge tank for cooling, and the cooled liquid-solid phase material is discharged into the raw oil recycling system through a discharge pipeline connected to the bottom of the discharge tank; the gas that obtains after the cooling process the gas leakage pipeline that the tank top of bleeding is connected gets into and cools off and divide liquid in the air cooler of the gas of promptly bleeding, and the gaseous material that obtains after dividing the liquid sends into torch system, and the liquid phase material that obtains after dividing the liquid returns in the tank of bleeding and finally discharge in the raw oil system of refining.

Compared with the prior art, the technical scheme of the invention has the following advantages:

1. according to the suspension bed hydrogenation process for treating heavy oil, part of raw oil and a suspension bed hydrocracking catalyst are mixed to form a mixture, and then primary shearing and secondary shearing are sequentially carried out on the mixture, so that high-dispersion mixing of the catalyst and the raw oil can be realized, and a uniformly mixed catalyst slurry is prepared, so that the hydrogenation catalytic activity of the catalyst can be better exerted, and the conversion rate of the raw oil and the yield of light oil are improved; and then mixing the catalyst slurry with the rest raw oil and hydrogen, feeding the mixture into a suspension bed hydrogenation reactor, controlling the operating pressure in the suspension bed hydrogenation reactor to be 18-22.5 MPa, the temperature to be 390-460 ℃ and the hydrogen-oil volume ratio to be 800-1500 to carry out hydrocracking reaction, carrying out thermal high-pressure separation on the obtained suspension bed hydrogenation product, respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil, sequentially carrying out cold high-pressure separation and cold low-pressure separation on the thermal high-pressure separation gas to obtain cold low-pressure separation oil, carrying out thermal low-pressure separation on the hot high-pressure separation oil to obtain thermal low-pressure separation gas and thermal low-pressure separation oil, carrying out steam stripping separation on the thermal low-pressure separation oil to convert the thermal low-pressure separation gas and the cold low-pressure separation oil into dry gas, naphtha and tower bottom oil, carrying out reduced pressure distillation on the thermal low-pressure separation oil, and collecting. The process adopts a reasonable separation process according to the composition and the property of the hydrogenation product of the suspension bed, separates low boiling point components such as hydrogen, dry gas, naphtha and the like in the hydrogenation product of the suspension bed in advance, separates heavy components such as reduced linear oil and the like in the hydrogenation product of the suspension bed, only sends medium components capable of being converted into light oil such as bottom oil of a stripping tower, hot low gas, reduced linear oil and the like into a subsequent fixed bed hydrogenation reactor for hydrocracking and hydrofining treatment again, greatly reduces the hydrogenation load of the fixed bed, more importantly improves the yield and the quality of the light oil to the maximum extent, can also effectively prolong the service life of a fixed bed catalyst, and is beneficial to energy conservation and emission reduction of the whole process.

2. The suspension bed hydrogenation process for treating heavy oil adopts a composite carrier formed by semi-coke hole expanding material with a specific structure, a molecular sieve and a catalytic cracking waste catalyst and an active metal oxide loaded on the composite carrier as a suspension bed hydrocracking catalyst, so that the characteristic that the pore size distribution is wide (large pores account for 50-60%, medium pores account for 20-30%, and the rest are micropores) is utilized, the catalytic activity of the catalyst is favorably exerted in the hydrogenation process, the cracking of macromolecular compounds in raw oil is promoted, asphaltene, colloid and the like are adsorbed, and the conversion rate of the raw oil and the yield of light oil can be improved.

3. According to the suspension bed hydrogenation process for treating the heavy oil, the raw oil is contacted with the fluidized adsorbent semi-coke and/or kaolin, so that the adsorption effect of the adsorbent is utilized to effectively remove colloids, asphaltenes and other solid impurities in the raw oil, and the substances are prevented from being coked in the subsequent hydrogenation process, and the conversion rate of the raw oil and the yield of the light oil are improved.

4. According to the suspension bed hydrogenation process for treating the heavy oil, two reactors connected in series are adopted, wherein one reactor is a suspension bed hydrocracking reactor, the other reactor is a suspension bed hydrogenation stabilizing reactor, and the operating temperature of the latter reactor is 20-50 ℃ lower than that of the former reactor, so that three reactions of cracking, hydrogenation and coke adsorption can be carried out under respective proper environmental conditions, and the conversion rate of raw oil and the yield of light oil are improved.

5. According to the suspension bed hydrogenation process for treating heavy oil, thermal low-temperature oil is distilled under normal pressure, fractions at the temperature of 150-250 ℃ and fractions at the temperature of more than 250 ℃ are respectively collected, then the fractions at the temperature of 150-250 ℃ (namely heavy naphtha) are combined with naphtha, and the fractions at the temperature of more than 250 ℃ are heated and then subjected to reduced pressure distillation, so that the heavy naphtha can be prevented from being greatly vaporized in a reduced pressure furnace, and the outlet temperature of the reduced pressure furnace cannot reach the designed feeding temperature of a reduced pressure tower; and secondly, heavy naphtha can be prevented from entering the vacuum tower to cause that oil products at each side line of the vacuum tower are too light and tower bottom residues can not meet the requirement of asphalt forming, so that light oil, wax oil and asphalt with excellent quality can be obtained, and the energy consumption of a downstream fixed bed reactor can be reduced.

6. According to the suspension bed hydrogenation process for treating the heavy oil, 80-90 wt% of the three-way reducing oil obtained by reduced pressure distillation and 5-20 wt% of the two-way reducing oil are combined to be used as a three-way reducing washing liquid, the remaining 10-20 wt% of the three-way reducing oil is used as a hot low-pressure washing liquid to wash oil gas generated by hot low-pressure separation to obtain hot low-pressure gas and hot low-pressure washing recovery liquid, and then 30-90 wt% of the hot low-pressure washing recovery liquid is recycled to be used as the hot low-pressure washing liquid, so that a closed circulating washing loop from the three-way reducing washing process to the hot low-pressure separation process and then returned to the reduced pressure distillation process is formed, and therefore the hot low-pressure gas, the two-way reducing oil, the one-way reducing oil and solid particles and other impurities in the top reducing gas can be effectively separated and removed, and the solid content of the light oil prepared by the suspension bed hydrogenation process is. Meanwhile, the process avoids discharging the three-line oil into the bottom of the vacuum tower because the three-line oil is recycled or used as hot low-component washing oil, so that the asphalt component at the bottom of the vacuum tower can be ensured to have a higher softening point, and the quality of the asphalt prepared by the suspension bed hydrogenation process is improved.

7. According to the suspension bed hydrogenation process for treating heavy oil, cold high-pressure gas obtained through cold high-pressure separation is used as circulating hydrogen, cold low-pressure gas obtained through cold high-pressure oil separation and dry gas obtained through cold low-pressure partial pressure separation are mixed to be used as fuel gas, and therefore energy consumption of the whole process can be further reduced.

8. According to the suspension bed hydrogenation process for treating heavy oil, the discharge system is connected and arranged at the bottom of the suspension bed hydrogenation reactor, so that when the temperature of the suspension bed hydrogenation reactor rises to exceed the normal reaction temperature instantly, the feed valve of the suspension bed hydrogenation reactor is closed, the discharge valve group is opened, the material in the suspension bed hydrogenation reactor is depressurized to 0.6-1.0MPa through the depressurization pore plate on the discharge pipeline and then discharged into the cooling separation system for cooling separation treatment, a gas phase material and a liquid-solid phase material are obtained, the gas phase material is discharged to the torch system, and the liquid-solid phase material is conveyed to the raw oil recycling system, so that the emergency discharge of the suspension bed hydrogenation reactor can be realized. When the emergency release is carried out, the liquid-solid phase in the suspension bed hydrogenation reactor is rapidly released in advance to avoid the contact of hydrogen and the liquid-solid phase, so that the hydrogenation reaction is not generated any more, the temperature runaway in the suspension bed hydrogenation reactor is effectively relieved and controlled, the liquid phase in the released material is uniformly wrapped with catalyst particles, the friction of the catalyst particles on a release pipeline is reduced to a certain extent, the safety release is facilitated, the energy consumption and the cost are reduced, meanwhile, the gas phase can be ensured to be reserved in the suspension bed hydrogenation reactor, the process that the suspension bed hydrogenation reactor needs to be re-pressurized when the next production recovery is carried out is avoided, and the equipment fatigue caused by frequent pressurization and depressurization of the equipment is avoided.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.

FIG. 1 is a flow diagram of a slurry bed hydrogenation process for treating heavy oil according to the present invention;

FIG. 2 is a structural diagram of a catalyst slurry preparation unit in example 4;

FIG. 3 is a block diagram of a feedstock oil pretreatment unit;

FIG. 4 is a block diagram of a hot low pressure separator and pressure reducing column;

FIG. 5 is a structural diagram of a catalyst slurry preparation unit in example 3;

wherein the reference numerals are as follows:

1-a primary shearing and mixing subunit, 2-a secondary shearing and mixing subunit, 3-a secondary shearing and mixing subunit, 4-a combustion furnace, 5-a suspension bed hydrocracking reactor, 6-a suspension bed hydrogenation and stabilization reactor, 7-a hot high-pressure separator, 8-a first heat exchanger, 9-a second heat exchanger, 10-a third heat exchanger, 11-an air condenser, 12-a cold high-pressure separator, 13-a cold low-pressure separator, 14-a hot low-pressure separator, 15-a stripping tower and 16-a pressure reducing tower; 20-a second catalyst feed system; 21-a catalyst preparation tank; 22-a catalyst transfer pot; 23-a stirrer; 24-first-grade powder-liquid shearing mixer; 25-second-level powder-liquid shearing mixer; 26-catalyst circulation pump; 27-secondary powder liquid shear mixer; 28-a first catalyst feed system; 29-catalyst mixing tank; 31-an oil pump; 32-an adsorption device; 33-sorbent addition means; 34-a solid-liquid separation device; 35-a fan; 36-a kneading device; 51-solvent buffer tank; 52-slurry preparation tank; 53-slurry mixing tank; 54-a stirring device; 55-a solid catalyst feed system; 56-venturi tube; 57-shear mixer; 58-solvent booster pump.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. 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.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. The terms "communicate," "connect," and the like are to be construed broadly and include, for example, fixed connections, removable connections, or integral connections unless expressly stated or limited otherwise; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.

The properties of the coal tar used in the following examples are shown in table 1 below:

TABLE 1 Properties of coal tar

The properties of the residues used in the following examples are shown in table 2:

TABLE 2 Properties of the residua

Density (20 deg.C), Kg/m³	0.9423
		Carbon residue in wt%	14.52
Sulfur, wt.%	4.51
		Gum, wt%	18.4
Asphaltenes, wt.%	13.2
		Fe，μg/g	14
Ni，μg/g	35
		V，μg/g	56

The properties of the semi-coke powder used in the following examples are shown in table 3:

TABLE 3 Properties of semi-coke

Test items	Unit of	Numerical value
			Moisture M_t	％	≤10
Ash content A_d	％	≤6
			Volatile component V_daf	％	5～7
Heating cartridge (Qb, ad)	MJ/kg	29～31
			Sulfur S_t,d	％	≤0.5
Fixed carbon FC_ad	％	80～85
			Range of particle size	mm	0.2～1

Example 1

As shown in fig. 1, the slurry bed hydrogenation process for treating heavy oil provided in this embodiment includes the following steps:

(1) selecting residual oil as raw oil of the process, mixing half amount of the residual oil with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carrying out primary shearing and secondary shearing on the mixture to obtain catalyst slurry;

(2) mixing the catalyst slurry with residual oil and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 18MPa, the temperature to be 425 ℃ and the hydrogen-oil volume ratio to be 1000 so as to carry out hydrocracking reaction;

(3) after the reaction in the step (2) is carried out for 1.5h, carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at the temperature of 400 ℃ under 18MPa, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 18MPa and 60 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1MPa and 60 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at 1MPa and 390 ℃ to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated with the cold low-fraction oil at 90 ℃ to obtain dry gas, naphtha and tower bottom oil;

and (2) carrying out reduced pressure distillation on the hot low-oil fraction, setting the operating temperatures of a first-line reduction oil, a second-line reduction oil and a third-line reduction oil to be 160 ℃, 230 ℃ and 300 ℃ respectively, and obtaining the first-line reduction oil (the main fractions are light wax oil and heavy diesel oil), the second-line reduction oil (the main fractions are wax oil), the third-line reduction oil (the main fractions are wax oil) and residues respectively, wherein the residues are used for producing asphalt, and the third-line reduction oil is used for self-washing oil circulation.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 0.1% and a particle size of 100 μm to 200 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: 1, the active metals are molybdenum, nickel, cobalt and iron; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 1:3:5, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:2, activating by water vapor at 900 ℃ for 0.5h, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying at 100 ℃ for 3h, wherein the average particle size of the semi-coke hole-expanding material is 60 mu m, and the specific surface area of the semi-coke hole-expanding material is 300m²G, average pore diameter of 70nm and average pore volume of 3cm³(ii)/g; the molecular sieve is a Y-type molecular sieve, the average particle size of the molecular sieve is 1mm, and the specific surface area of the molecular sieve is 300m²(ii)/g, average pore diameter 5 nm; the catalytic cracking waste catalyst comprises the following components in percentage by mass: 55: 0.5Y-type molecular sieve, alumina and metals (nickel, vanadium and iron) having an average particle diameter of 150 μm and a specific surface area of300m²In g, the mean pore diameter is 3 nm.

Example 2

(1) purification treatment of coal tar

Introducing air into the coal tar to make the particle diameter be 0.2mm and the specific surface area be 50m²The kaolin powder per gram and the coal tar are back-mixed and contacted according to the mass ratio of 0.1:1, and are adsorbed at the temperature of 50 ℃ and the pressure of 0.5MPa, and the flow of air required by every 1kg of the kaolin powder is 0.5m³S; after adsorption, settling and layering are carried out, upper-layer materials are collected, solid-liquid separation is carried out on the upper-layer materials, and the collected liquid phase is the purified coal tar;

compared with the coal tar before purification treatment, the carbon residue value in the purified coal tar is reduced to 0.1% and reduced by 79%; the asphaltene content is reduced by 76%; the colloid is reduced by 80%; the heavy metal impurities are reduced by 51 percent;

(2) mixing 30% of the purified coal tar with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carrying out primary shearing and secondary shearing on the mixture to obtain catalyst slurry;

(3) mixing the catalyst slurry with the residual purified coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 20MPa, the temperature to be 390 ℃ and the hydrogen-oil volume ratio to be 1200 so as to carry out hydrocracking reaction;

(4) after the reaction of the step (3) is carried out for 0.5h, carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at 19MPa and 350 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 18.5MPa and 50 ℃ to obtain cold high-pressure gas and cold high-pressure gas oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure gas oil is subjected to cold low-pressure separation at 1.2MPa and 40 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 350 ℃ under the pressure of 1.1MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated from the cold low-fraction oil at the temperature of 80 ℃ to obtain dry gas, naphtha and tower bottom oil;

and (2) carrying out reduced pressure distillation on the hot low-oil fraction, setting the operating temperatures of a first-line reduction oil, a second-line reduction oil and a third-line reduction oil to be 110 ℃, 250 ℃ and 330 ℃, and respectively obtaining the first-line reduction oil (the main fractions are light wax oil and heavy diesel oil), the second-line reduction oil (the main fractions are wax oil), the third-line reduction oil (the main fractions are wax oil) and residues, wherein the residues are used for producing asphalt, and the third-line reduction oil is used for self-washing oil circulation.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 5% and a particle size of 50 μm to 300 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: 0.5, the active metals are tungsten, nickel, cobalt and iron; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 5:2:2.75, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:6, activating for 0.5h by water vapor at 950 ℃, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying for 3h at 150 ℃, wherein the average particle size is 100 mu m, and the specific surface area is 150m²(ii)/g, average pore diameter of 80nm and average pore volume of 2cm³(ii)/g; the molecular sieve is a Y-type molecular sieve, the average particle size of the molecular sieve is 2mm, and the specific surface area of the molecular sieve is 200m²(ii)/g, average pore diameter 6 nm; the catalytic cracking waste catalyst comprises the following components in percentage by mass: 15: 1Y-type molecular sieve, alumina and metals (nickel, vanadium and iron) with an average particle size of 120 μm and a specific surface area of 200m²In terms of/g, the mean pore diameter is 5 nm.

Example 3

(1) preparing catalyst slurry

Selecting coal tar as raw oil of the process, referring to fig. 5, taking a half amount of coal tar, injecting the coal tar into a solvent buffer tank 51, buffering the coal tar by the solvent buffer tank 51 and pressurizing the coal tar by a solvent booster pump 58, then entering a venturi tube 56, meanwhile, enabling a suspension bed hydrocracking catalyst to enter the venturi tube 56 from a solid catalyst feeding system 55, preliminarily mixing the coal tar and the catalyst in the venturi tube 56, then entering a slurry preparation tank 52, forming a primary slurry under the stirring action of a stirring device 54 of the primary slurry preparation tank, wherein the temperature in the preparation tank is 90 ℃, and the pressure in the preparation tank is normal pressure; the latter slurry is sheared, stirred and mixed by a shearing mixer 57 and a slurry mixing tank 53 to finally obtain catalyst slurry;

(2) mixing the catalyst slurry with residual coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 21.5MPa, the temperature to be 440 ℃ and the hydrogen-oil volume ratio to be 800 so as to carry out hydrocracking reaction;

(3) after the reaction of the step (2) is carried out for 0.8h, carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at the temperature of 420 ℃ under the pressure of 20MPa, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 20MPa and 30 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 0.8MPa and 50 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-branch oil is subjected to hot low-pressure separation at the temperature of 420 ℃ under the pressure of 0.8MPa to obtain hot low-branch gas and hot low-branch oil, the hot low-branch gas enters a stripping tower and is separated from the cold low-branch oil at the temperature of 85 ℃ to obtain dry gas, naphtha and tower bottom oil, the hot low-branch oil is subjected to reduced pressure distillation, the operating temperatures of a first-line reduction oil, a second-line reduction oil and a third-line reduction oil are set to be 160 ℃, 250 ℃ and 330 ℃, respectively, and the first-line reduction oil (main fractions are light wax oil and heavy diesel oil), the second-line reduction oil (main fractions are wax oil), the third-line reduction oil (main fractions are wax oil) and residues are obtained, wherein the residues are used for producing asphalt, and the third-line reduction;

(4) after heat energy recovery, the first-line reduced oil and the bottom oil of the stripping tower are fed into a fixed bed hydrogenation reactor together for hydrocracking and refining again, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 21MPa, the temperature is controlled to be 350 ℃, the volume ratio of hydrogen to oil is controlled to be 900, and the volume space velocity is controlled to be 1.1h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 2% and a particle size of 5 μm to 100 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: 5, the active metals are tungsten, nickel, cobalt and iron; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 3:4:0.5, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:4, activating for 0.5h by water vapor at 920 ℃, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying for 3h at 120 ℃ to obtain the semi-coke hole-expanding material, wherein the average particle size of the semi-coke hole-expanding material is 80 mu m, and the specific surface area of the semi-coke hole-expanding material is 200m²G, average pore diameter of 75nm and average pore volume of 2.5cm³(ii)/g; the molecular sieve is a Y-type molecular sieve, the average particle size of the molecular sieve is 3mm, and the specific surface area of the molecular sieve is 250m²(ii)/g, average pore diameter 8 nm; the catalytic cracking waste catalyst comprises the following components in a mass ratio of 20: 55: 0.5Y-type molecular sieve, alumina, metal (nickel, vanadium and iron), with average particle diameter of 100 μm and specific surface area of 250m²In g, the mean pore diameter is 6 nm.

Example 4

(1) coal tar purification treatment

Selecting coal tar as raw oil, introducing air into coal tar to make the particle diameter be 0.3mm and specific surface area be 200m²High in/gBack-mixing and contacting the kaolin powder and the coal tar according to the mass ratio of 0.05:1, adsorbing at 75 ℃, wherein the flow of air required by every 1kg of kaolin powder is 0.9m³S; after adsorption is finished, settling and layering are carried out, an upper layer material and a lower layer precipitate are respectively collected, then solid-liquid separation is carried out on the upper layer material, a collected liquid phase is the purified coal tar, and a mixture obtained after the solid phase is combined with the lower layer precipitate is kneaded with coke powder according to the mass ratio of 0.8:1 to obtain the bonding asphalt;

compared with the coal tar before purification treatment, the carbon residue value of the purified coal tar is reduced by 80 percent in the embodiment; the asphaltene content is reduced by 76.8%; the colloid is reduced by 80.7%; the heavy metal impurities are reduced by 52.1%;

(2) preparing catalyst slurry

Referring to fig. 2, injecting a half amount of purified coal tar into a catalyst preparation tank, when the liquid level reaches a target liquid level, automatically cutting off a liquid inlet valve, starting a stirrer of the catalyst preparation tank, simultaneously starting a catalyst circulating pump and a primary powder-liquid shearing mixer, so that the coal tar in the catalyst preparation tank is pressurized by the catalyst circulating pump, mixed with a suspension bed hydrocracking catalyst from a catalyst feeding system, subjected to primary shearing mixing in the primary powder-liquid shearing mixer, and then returned to the catalyst preparation tank; the mixture output from the catalyst preparation tank is introduced into a secondary powder-liquid shearing mixer for secondary shearing and mixing, and then is conveyed into a catalyst mixing tank for secondary mixing to obtain catalyst slurry;

(3) mixing the catalyst slurry with the residual purified coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 22.5MPa, the temperature to be 405 ℃ and the hydrogen-oil volume ratio to be 1500 so as to carry out hydrocracking reaction;

(4) after reacting for 1h in the step (3), carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at the temperature of 380 ℃ under the pressure of 22.5MPa, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at the temperature of 20MPa and 40 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas is used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at the temperature of 0.5MPa and 45 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas is used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 370 ℃ under the pressure of 0.5MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated with the cold low-fraction oil at the temperature of 88 ℃ to obtain dry gas, naphtha and tower bottom oil;

(5) and (2) carrying out reduced pressure distillation on the hot low-distillate oil, setting the operating temperatures of a first-line reduction, a second-line reduction and a third-line reduction to be 130 ℃, 280 ℃ and 390 ℃ respectively, and obtaining first-line reduction oil (main fractions are light wax oil and heavy diesel oil), second-line reduction oil (main fractions are wax oil), third-line reduction oil (main fractions are wax oil) and residues respectively, wherein:

the residue is used for producing asphalt, the minus first-line oil is used for self oil washing circulation, the minus second-line oil, the minus first-line oil and the bottom oil of the stripping tower are conveyed into a fixed bed hydrogenation reactor together for hydrocracking and refining again after heat energy recovery, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 19MPa, the temperature is 360 ℃, the volume ratio of hydrogen to oil is 1200, and the volume space velocity is 1.3h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 7.5% and a particle size of 150 μm to 500 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: 7, the active metals are molybdenum, nickel, cobalt and iron; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 2:2.5:1, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:3, activating for 0.5h by water vapor at 910 ℃, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying for 3h at 130 ℃ to obtain the semi-coke hole-expanding materialTo have an average particle diameter of 90 μm and a specific surface area of 250m²(ii)/g, average pore diameter of 80nm and average pore volume of 3cm³(ii)/g; the molecular sieve is ZSM-5 molecular sieve, the average grain diameter of the molecular sieve is 4mm, and the specific surface area of the molecular sieve is 300m²(ii)/g, average pore diameter of 10nm, average pore volume of 0.23%; the catalytic cracking waste catalyst comprises the following components in a mass ratio of 20: 40: 1Y-type molecular sieve, alumina, metal (nickel, vanadium and iron), with an average particle size of 150 μm and a specific surface area of 300m²G, average pore diameter of 7 nm.

Example 5

(1) selecting coal tar as raw oil of the process, mixing 60% of the coal tar with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carrying out primary shearing and secondary shearing on the mixture to obtain catalyst slurry;

(2) mixing the catalyst slurry with residual coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrocracking reactor, controlling the operating pressure in the suspension bed hydrocracking reactor to be 19.5MPa, the temperature to be 460 ℃ and the hydrogen-oil volume ratio to be 1100 so as to carry out hydrocracking reaction, and obtaining a hydrocracking product after 2 hours;

feeding the hydrocracking product into the suspension bed hydrogenation stabilization reactor, controlling the operating pressure in the suspension bed hydrogenation stabilization reactor to be 19.5MPa, the temperature to be 440 ℃, the hydrogen-oil volume ratio to be 1100, and carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst for 1.5 hours to obtain a suspension bed hydrogenation product;

(3) carrying out thermal high-pressure separation on the obtained suspension bed hydrogenation product at 19MPa and 460 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 19MPa and 45 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.5MPa and 45 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 430 ℃ under the pressure of 1.5MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated with the cold low-fraction oil at the temperature of 82 ℃ to obtain dry gas, naphtha and tower bottom oil;

(4) and (2) carrying out reduced pressure distillation on the hot low-fraction oil, setting the operating temperatures of a first-line reduction, a second-line reduction and a third-line reduction to 210 ℃, 290 ℃ and 350 ℃, and respectively obtaining first-line reduction oil (main fractions are light wax oil and heavy diesel oil), second-line reduction oil (main fractions are wax oil), third-line reduction oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, the minus first-line oil is used for self oil washing circulation, the minus first-line oil and the bottom oil of the stripping tower are conveyed into a fixed bed hydrogenation reactor together for hydrocracking and refining again after heat energy recovery, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 22.5MPa, the temperature is 390 ℃, the volume ratio of hydrogen to oil is 500, and the volume space velocity is 1.2h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 10% and a particle size of 30 μm to 280 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 100: 2.5, the active metals are tungsten, nickel, cobalt and iron; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 4:3.5:4, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:4, activating for 0.5h by water vapor at 920 ℃, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying for 3h at 120 ℃ to obtain the semi-coke hole-expanding material, wherein the average particle size of the semi-coke hole-expanding material is 80 mu m, and the specific surface area of the semi-coke hole-expanding material is 200m²G, average pore diameter of 75nm and average pore volume of 2.5cm³The molecular sieve is β molecular sieve, the average particle diameter is 2.5mm, and the specific surface area is 280m²(ii)/g, average pore diameter 6 nm; the catalytic cracking waste catalyst comprises the following components in a mass ratio of 20: 55: 0.5Y-type molecular sieve, alumina, iron (nickel, vanadium and iron), with average particle diameter of 100 μm and specific surface area of 250m²In terms of/g, the mean pore diameter is 4 nm.

In this example, the suspension bed hydrogenation-stabilized catalyst is a supported catalyst loaded with cobalt, molybdenum and tungsten on alumina as a carrier.

Example 6

(2) mixing the catalyst slurry with residual oil and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 18.5MPa, the temperature to be 450 ℃ and the hydrogen-oil volume ratio to be 900 so as to carry out hydrocracking reaction;

(3) after reacting for 2 hours in the step (2), carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at the temperature of 440 ℃ under 18.5MPa, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 18MPa and 50 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.4MPa and 50 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 410 ℃ under the pressure of 1.3MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated from the cold low-fraction oil at the temperature of 86 ℃ to obtain dry gas, naphtha and tower bottom oil;

(4) distilling the hot low-temperature fraction oil under normal pressure, respectively collecting 150-250 ℃ fractions and fractions with the temperature higher than 250 ℃, combining the 150-250 ℃ fractions with the naphtha, heating the fractions with the temperature higher than 250 ℃, distilling under reduced pressure, setting the operating temperatures of a first reduction line, a second reduction line and a third reduction line to be 120 ℃, 200 ℃ and 370 ℃, respectively obtaining first reduction line oil (main fractions are light wax oil and heavy diesel oil), second reduction line oil (main fractions are wax oil), third reduction line oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, the minus first-line oil is used for self oil washing circulation, the minus second-line oil, the minus first-line oil and the bottom oil of the stripping tower are conveyed into a fixed bed hydrogenation reactor together for hydrocracking and refining again after heat energy recovery, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 18.5MPa, the temperature is 410 ℃, the volume ratio of hydrogen to oil is 1500, and the volume space velocity is 0.5h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 1% and a particle size of 200 μm to 500 μm; the suspension bed hydrocracking catalyst consists of a composite carrier and an active metal oxide loaded on the composite carrier, wherein the mass ratio of active metals in the composite carrier to the active metal oxide is 10: 1, the active metal is tungsten, nickel and cobalt; the composite carrier consists of a semi-coke pore-expanding material, a molecular sieve and a catalytic cracking waste catalyst in a mass ratio of 2.5:3.5:1.5, wherein: the semi-coke hole-expanding material is prepared by mixing semi-coke and sodium carbonate according to a mass ratio of 1:2, activating by water vapor at 900 ℃ for 0.5h, carrying out acid washing and water washing on a hole-expanded sample, carrying out centrifugal separation, and drying at 100 ℃ for 3h, wherein the average particle size of the semi-coke hole-expanding material is 60 mu m, and the specific surface area of the semi-coke hole-expanding material is 300m²G, average pore diameter of 70nm and average pore volume of 3cm³(ii)/g; the molecular sieve is a Y-type molecular sieve, the average particle size of the molecular sieve is 1mm, and the specific surface area of the molecular sieve is 300m²(ii)/g, average pore diameter 5 nm; the catalytic cracking waste catalyst comprises the following components in percentage by mass: 55: 0.5Y-type molecular sieve, alumina and metals (nickel, vanadium and iron) having an average particle diameter of 150 μm and a specific surface area of 300m²In g, the mean pore diameter is 3 nm.

Example 7

(1) selecting residual oil as raw oil of the process, mixing 40% of the residual oil with a suspension bed hydrocracking catalyst to form a mixture, and sequentially carrying out primary shearing and secondary shearing on the mixture to obtain catalyst slurry;

(2) mixing the catalyst slurry with residual oil and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 20.5MPa, the temperature to be 400 ℃ and the hydrogen-oil volume ratio to be 1200 so as to carry out hydrocracking reaction;

(3) after reacting for 1h in the step (2), carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at 19MPa and 350 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 18.5MPa and 50 ℃ to obtain cold high-pressure gas and cold high-pressure gas oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure gas oil is subjected to cold low-pressure separation at 1.2MPa and 40 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

(4) and (2) carrying out reduced pressure distillation on the hot low-distillate oil, setting the operating temperatures of a first-line reduction, a second-line reduction and a third-line reduction to be 150 ℃, 260 ℃ and 350 ℃, and respectively obtaining first-line reduction oil (main fractions are light wax oil and heavy diesel oil), second-line reduction oil (main fractions are wax oil), third-line reduction oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, 80 wt% of the three-way oil is combined with 10 wt% of the two-way oil to be used as a three-way reducing washing liquid, the remaining 20 wt% of the three-way oil is used as a hot low-pressure separating washing liquid to obtain hot low-pressure gas and hot low-pressure washing recovery liquid at the same time of washing oil gas generated by the hot low-pressure separation, and 30 wt% of the hot low-pressure washing recovery liquid is recycled to be used as the hot low-pressure separating washing liquid;

the rest 90 wt% of the second-line reduced oil is subjected to heat energy recovery and then is sent into a fixed bed hydrogenation reactor together with the first-line reduced oil and bottom oil of a stripping tower for hydrocracking and refining again, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 20MPa, the temperature is controlled to be 450 ℃, the volume ratio of hydrogen to oil is controlled to be 1000, and the volume space velocity is controlled to be 0.7h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 6.5% and a particle size of 350 μm to 500 μm; the composition of the suspension hydrocracking catalyst was the same as in example 2 of the present invention.

In this example, the solid contents and contents of the materials at the feed inlet of the thermal low-pressure separator, the outlet of the thermal low-pressure gas, the outlet of the thermal low-pressure scrubbing oil sump, the outlet of the thermal low-pressure oil, the outlet of the reduced-head gas, the outlet of the reduced-first-line oil, the outlet of the reduced-second-line oil, the outlet of the reduced-third-line oil, and the outlet of the bottom oil were measured, respectively, and the results are shown in table 4.

TABLE 4 solid content and content in the material at the inlet and outlet

As can be seen from table 4, in the case that the hot low-component feed contains 10% of the suspension bed hydrogenation catalyst, 20% of asphaltenes, 15% of colloids, 1% of metals and 1% of ash, the separation process in step (4) of this example can ensure that the materials at the hot low-component gas outlet, the reduced top gas outlet, the reduced first-line oil outlet and the reduced second-line oil outlet have a relatively low solid content, thereby demonstrating that the separation process described in the present invention can significantly improve the quality of the light oil product produced by the suspension bed hydrogenation process.

Example 8

(1) purification treatment of coal tar

Introducing air into the coal tar to make the particle diameter be 0.2mm and the specific surface area be 100m²The semi-coke powder and coal tar are back-mixed and contacted according to the mass ratio of 0.15:1, and are adsorbed at the temperature of 60 ℃ and the pressure of 0.8MPa, and the flow of air required by 1kg of the semi-coke powder is 0.6m³S; after adsorption is finished, settling and layering are carried out, an upper layer material and a lower layer precipitate are respectively collected, then solid-liquid separation is carried out on the upper layer material, a collected liquid phase is purified coal tar, and a mixture obtained after the solid phase is combined with the lower layer precipitate is kneaded with coke powder according to the mass ratio of 1:1 to obtain bonding asphalt;

compared with the coal tar before purification treatment, the carbon residue value in the purified coal tar is reduced to 0.11 percent and reduced by 80 percent; the asphaltene content is reduced by 78%; the colloid is reduced by 80%; the heavy metal impurities are reduced by 52 percent;

(2) preparing catalyst slurry

(3) hydrogenation in suspension bed

Mixing the catalyst slurry with the residual purified coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrocracking reactor, controlling the operating pressure in the suspension bed hydrocracking reactor to be 20.5MPa, the temperature to be 430 ℃ and the hydrogen-oil volume ratio to be 1000 so as to carry out hydrocracking reaction, and obtaining a hydrocracking product after 1 h;

feeding the hydrocracking product into the suspension bed hydrogenation stabilization reactor, controlling the operating pressure in the suspension bed hydrogenation stabilization reactor to be 20.5MPa, the temperature to be 380 ℃ and the hydrogen-oil volume ratio to be 1100, and carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst for 1h to obtain a suspension bed hydrogenation product;

(4) carrying out thermal high-pressure separation on the obtained suspension bed hydrogenation product at the temperature of 380 ℃ under the pressure of 20MPa, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 20MPa and 50 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.1MPa and 50 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 380 ℃ under the pressure of 1MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated from the cold low-fraction oil at the temperature of 85 ℃ to obtain dry gas, naphtha and tower bottom oil;

(5) and (2) carrying out reduced pressure distillation on the hot low-distillate oil, setting the operating temperatures of a first-line reduction, a second-line reduction and a third-line reduction to be 120 ℃, 260 ℃ and 350 ℃, and respectively obtaining first-line reduction oil (main fractions are light wax oil and heavy diesel oil), second-line reduction oil (main fractions are wax oil), third-line reduction oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, the minus first-line oil is used for washing oil circulation per se, the minus second-line oil, the minus first-line oil and the bottom oil of the stripping tower are conveyed into a fixed bed hydrogenation reactor together for hydrocracking and refining again after heat energy recovery, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 20MPa, the temperature is 350 ℃, the volume ratio of hydrogen to oil is 1100, and the volume space velocity is 1.1h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with temperature lower than 350 deg.c and tail oilCarrying out the back refining treatment.

In the catalyst slurry of this embodiment, the suspension hydrocracking catalyst has a mass percentage of 6.3% and a particle size of 80 to 440 μm; the compositions of the suspension bed hydrocracking catalyst and the suspension bed hydrogenation stabilizing catalyst are the same as those of the embodiment 5 of the invention.

Example 9

(2) mixing the catalyst slurry with residual oil and hydrogen, and then feeding the mixture into a suspension bed hydrogenation reactor, and controlling the operating pressure in the suspension bed hydrogenation reactor to be 19MPa, the temperature to be 460 ℃ and the hydrogen-oil volume ratio to be 1000 so as to carry out hydrocracking reaction;

(3) after reacting for 2 hours in the step (2), carrying out thermal high-pressure separation on the obtained hydrogenation product of the suspension bed at 18MPa and 450 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 18MPa and 40 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.3MPa and 40 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 410 ℃ under the pressure of 1.3MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated with the cold low-fraction oil at the temperature of 82 ℃ to obtain dry gas, naphtha and tower bottom oil;

(4) distilling the hot low-temperature fraction oil under normal pressure, respectively collecting 150-250 ℃ fractions and fractions with the temperature higher than 250 ℃, combining the 150-250 ℃ fractions with the naphtha, heating the fractions with the temperature higher than 250 ℃, distilling under reduced pressure, setting the operating temperatures of a first reduction line, a second reduction line and a third reduction line to be 130 ℃, 240 ℃ and 350 ℃, respectively obtaining first reduction line oil (main fractions are light wax oil and heavy diesel oil), second reduction line oil (main fractions are wax oil), third reduction line oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, 90 wt% of the three-way oil is combined with 5 wt% of the two-way oil to be used as a three-way reducing washing liquid, the remaining 10 wt% of the three-way oil is used as a hot low-pressure separating washing liquid to obtain hot low-pressure gas and hot low-pressure washing recovery liquid at the same time of washing oil gas generated by the hot low-pressure separation, and 60 wt% of the hot low-pressure washing recovery liquid is recycled to be used as the hot low-pressure separating washing liquid;

the rest 95 wt% of the second-line reduced oil is subjected to heat energy recovery and then is sent into a fixed bed hydrogenation reactor together with the first-line reduced oil and the bottom oil of the stripping tower for hydrocracking and refining again, the operating pressure in the fixed bed hydrogenation reactor is controlled to be 18.5MPa, the temperature is controlled to be 450 ℃, the volume ratio of hydrogen to oil is 1200, and the volume space velocity is controlled to be 1.3h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of this embodiment, the suspension hydrocracking catalyst has a mass percentage of 3.5% and a particle size of 300 μm to 480 μm; the composition of the suspension hydrocracking catalyst was the same as in example 3 of the present invention.

Example 10

(1) purification treatment of coal tar

Introducing air into the coal tar to make the particle diameter be 0.2mm and the specific surface area be 500m²The semi-coke powder and coal tar are back-mixed and contacted according to the mass ratio of 0.08:1, and are adsorbed at the temperature of 100 ℃ and the pressure of 0.2MPa, and the flow of air required by 1kg of the semi-coke powder is 0.7m³S; settling and layering after adsorption is finished, respectively collecting upper-layer material and lower-layer precipitate, then making solid-liquid separation on the upper-layer material, collecting liquid phase, namely after purificationThe solid phase and the lower layer precipitate are combined to obtain a mixture, and the mixture and the coke powder are kneaded according to the mass ratio of 0.8:1 to obtain the bonding asphalt;

compared with the coal tar before purification treatment, the carbon residue value of the purified coal tar is reduced to 0.1% and is reduced by 81%; the asphaltene content is reduced by 80%; the colloid is reduced by 79%; the heavy metal impurities are reduced by 51 percent;

(2) preparing catalyst slurry

Referring to fig. 2, injecting a half amount of purified coal tar into a catalyst preparation tank, when the liquid level reaches a target liquid level, automatically cutting off a liquid inlet valve, starting a stirrer of the catalyst preparation tank, simultaneously starting a catalyst circulating pump and a primary powder-liquid shearing mixer, so that the coal tar in the catalyst preparation tank is pressurized by the catalyst circulating pump, mixed with a suspension bed hydrocracking catalyst from a catalyst feeding system, subjected to primary shearing mixing in the primary powder-liquid shearing mixer, and then returned to the catalyst preparation tank; the mixture output from the catalyst preparation tank is sequentially introduced into a secondary liquid-separating shearing mixer and a catalyst conveying tank for secondary shearing mixing; finally, the mixture enters a secondary powder-liquid shearing mixer for secondary shearing mixing, and is conveyed into a catalyst mixing tank for secondary mixing to obtain catalyst slurry;

(3) hydrogenation in suspension bed

Mixing the catalyst slurry with the residual purified coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrocracking reactor, controlling the operating pressure in the suspension bed hydrocracking reactor to be 20MPa, the temperature to be 450 ℃ and the hydrogen-oil volume ratio to be 1200 so as to carry out hydrocracking reaction, and obtaining a hydrocracking product after 1.5 h;

feeding the hydrocracking product into the suspension bed hydrogenation stabilization reactor, controlling the operating pressure in the suspension bed hydrogenation stabilization reactor to be 20MPa, the temperature to be 410 ℃ and the hydrogen-oil volume ratio to be 1200, carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst, and obtaining a suspension bed hydrogenation product after 1.5 h;

(4) carrying out thermal high-pressure separation on the obtained suspension bed hydrogenation product at 20MPa and 400 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 20MPa and 60 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.4MPa and 50 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 380 ℃ under the pressure of 1.3MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated from the cold low-fraction oil at the temperature of 85 ℃ to obtain dry gas, naphtha and tower bottom oil;

(5) distilling the hot low-temperature fraction oil under normal pressure, respectively collecting fractions at 150-250 ℃ and fractions at more than 250 ℃, combining the fractions at 150-250 ℃ with the naphtha, heating the fractions at more than 250 ℃, distilling under reduced pressure, setting the operating temperatures of a first reduction line, a second reduction line and a third reduction line to be 120 ℃, 260 ℃ and 350 ℃, respectively obtaining first reduction line oil (main fractions are light wax oil and heavy diesel oil), second reduction line oil (main fractions are wax oil), third reduction line oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, 85 wt% of the three-way reducing oil and 20 wt% of the two-way reducing oil are combined to be used as three-way reducing washing liquid, the rest 15 wt% of the three-way reducing oil is used as hot low-pressure washing liquid to wash oil gas generated by the hot low-pressure separation to obtain hot low-pressure gas and hot low-pressure washing recovery liquid, and 90 wt% of the hot low-pressure washing recovery liquid is recycled to be used as hot low-pressure washing liquid;

recovering the heat energy of the rest 80 wt% of the first-line reduced oil, feeding the first-line reduced oil and the bottom oil of the stripping tower into a fixed bed hydrogenation reactor together for hydrocracking and refining again, and controlling the operating pressure in the fixed bed hydrogenation reactor to be 18.5MPa, the temperature to be 440 ℃, the hydrogen-oil volume ratio to be 1000 and the volume space velocity to be 1.5h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of this embodiment, the suspension hydrocracking catalyst has a mass percentage of 5.9% and a particle size of 250 μm to 500 μm; the compositions of the suspension bed hydrocracking catalyst and the suspension bed hydrogenation stabilizing catalyst are the same as those of the embodiment 5 of the invention.

Example 11

(1) purification treatment of coal tar

Introducing air into the coal tar to make the particle diameter be 0.2mm and the specific surface area be 300m²The semi-coke powder and coal tar are back-mixed and contacted according to the mass ratio of 0.2:1, and are adsorbed at the temperature of 80 ℃ and the pressure of 1MPa, and the flow of air required by each 1kg of the semi-coke powder is 0.8m³S; after adsorption is finished, settling and layering are carried out, an upper layer material and a lower layer precipitate are respectively collected, then solid-liquid separation is carried out on the upper layer material, a collected liquid phase is the purified coal tar, and a mixture obtained after the solid phase is combined with the lower layer precipitate is kneaded with coke powder according to the mass ratio of 0.9:1 to obtain the bonding asphalt;

compared with the coal tar before purification treatment, the carbon residue value of the purified coal tar is reduced to 0.12% and reduced by 83%; the asphaltene content is reduced by 81 percent; the colloid is reduced by 80%; the heavy metal impurities are reduced by 50%;

(2) preparing catalyst slurry

Injecting half amount of purified coal tar into a catalyst preparation tank, automatically cutting off a liquid inlet valve when the liquid level reaches a target liquid level, starting a stirrer of the catalyst preparation tank, simultaneously starting a catalyst circulating pump and a primary powder-liquid shearing mixer, mixing the coal tar in the catalyst preparation tank with a suspension bed hydrocracking catalyst from a catalyst feeding system after being boosted by the catalyst circulating pump, performing primary shearing mixing in the primary powder-liquid shearing mixer, and returning to the catalyst preparation tank; the mixture output from the catalyst preparation tank is introduced into a secondary powder-liquid shearing mixer for secondary shearing and mixing, and then is conveyed into a catalyst mixing tank for secondary mixing to obtain catalyst slurry;

(3) hydrogenation in suspension bed

Mixing the catalyst slurry with the residual purified coal tar and hydrogen, and then feeding the mixture into a suspension bed hydrocracking reactor, controlling the operating pressure in the suspension bed hydrocracking reactor to be 20.8MPa, the temperature to be 430 ℃ and the volume ratio of hydrogen to oil to be 1300 so as to carry out hydrocracking reaction, and obtaining a hydrocracking product after 1.5 hours;

feeding the hydrocracking product into the suspension bed hydrogenation stabilization reactor, controlling the operating pressure in the suspension bed hydrogenation stabilization reactor to be 20.8MPa, the temperature to be 400 ℃ and the hydrogen-oil volume ratio to be 1300, and carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst for 1h to obtain a suspension bed hydrogenation product;

(4) carrying out thermal high-pressure separation on the obtained suspension bed hydrogenation product at 20.5MPa and 400 ℃, and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure gas exchanges heat with raw oil, cold hydrogen, cold low-pressure gas and air in sequence, and then is subjected to cold high-pressure separation at 20MPa and 50 ℃ to obtain cold high-pressure gas and cold high-pressure oil, the cold high-pressure gas can be used as circulating hydrogen, the cold high-pressure oil is subjected to cold low-pressure separation at 1.5MPa and 50 ℃ to obtain cold low-pressure gas and cold low-pressure oil, the cold low-pressure gas can be used as fuel, and the cold low-pressure oil is sent into a stripping tower;

the hot high-fraction oil is subjected to hot low-pressure separation at the temperature of 380 ℃ under the pressure of 1.4MPa to obtain hot low-fraction gas and hot low-fraction oil, and the hot low-fraction gas enters a stripping tower to be separated from the cold low-fraction oil at the temperature of 90 ℃ to obtain dry gas, naphtha and tower bottom oil;

(5) distilling the hot low-temperature fraction oil under normal pressure, respectively collecting 150-250 ℃ fractions and fractions with the temperature higher than 250 ℃, combining the 150-250 ℃ fractions with the naphtha, heating the fractions with the temperature higher than 250 ℃, distilling under reduced pressure, setting the operating temperatures of a first reduction line, a second reduction line and a third reduction line to be 150 ℃, 270 ℃ and 370 ℃, respectively obtaining first reduction line oil (main fractions are light wax oil and heavy diesel oil), second reduction line oil (main fractions are wax oil), third reduction line oil (main fractions are wax oil) and residues, wherein:

the residue is used for producing asphalt, 88 wt% of the three-line-reduced oil and 15 wt% of the two-line-reduced oil are combined to be used as three-line-reduced washing liquid, the remaining 12 wt% of the three-line-reduced oil is used as hot low-pressure separation washing liquid to obtain hot low-pressure separation gas and hot low-pressure separation washing recovery liquid at the same time, and 70 wt% of the hot low-pressure separation washing recovery liquid is recycled to be used as hot low-pressure separation washing liquid;

recovering the heat energy of the rest 85 wt% of the first-line reduced oil, feeding the first-line reduced oil and the bottom oil of the stripping tower into a fixed bed hydrogenation reactor together for hydrocracking and refining again, and controlling the operating pressure in the fixed bed hydrogenation reactor to be 20.5MPa, the temperature to be 450 ℃, the hydrogen-oil volume ratio to be 1000 and the volume space velocity to be 1.3h^-1Then separating the hydrogenation product of the fixed bed to obtain light oil product with the temperature less than 350 ℃, and carrying out recycle treatment on the tail oil.

In the catalyst slurry of the embodiment, the suspension bed hydrocracking catalyst has a mass percentage of 8.1% and a particle size of 300 μm to 490 μm; the compositions of the suspension bed hydrocracking catalyst and the suspension bed hydrogenation stabilizing catalyst are the same as those of the embodiment 5 of the invention.

In this embodiment, the bottom of each of the two suspension bed hydrogenation reactors is connected with a discharge system, the discharge system comprises a discharge pipeline, a cooling separation system, a torch system and a raw oil recycle system, one end of the discharge pipeline is connected with the bottom of the suspension bed hydrogenation reactor, and the other end of the discharge pipeline is connected with the cooling separation system; in the process of hydrogenation of the suspension bed, when the temperature of a hydrogenation reactor of the suspension bed rises to exceed the normal reaction temperature instantly, closing a feed valve of the hydrogenation reactor of the suspension bed, opening a discharge valve group in the cooling and separating system, so that the material in the hydrogenation reactor of the suspension bed is reduced to 1.0MPa through a pressure reduction pore plate on a discharge pipeline and then discharged into a discharge tank of the cooling and separating system, is mixed with flushing oil in the discharge tank for cooling, and the cooled liquid-solid phase material is discharged into the raw oil recycling system through a discharge pipeline connected with the bottom of the discharge tank; the gas that obtains after the cooling process the gas release pipeline that the tank top of bleeding is connected gets into and cools off and divide liquid in the air cooler of the gas of promptly bleeding, and the gaseous phase material that obtains after dividing the liquid sends into torch system, and the liquid phase material that obtains after dividing the liquid returns in the tank of bleeding and finally discharge in the raw oil is made back to the system of making perfect still to can ensure the urgent of suspension bed hydrogenation ware and release.

Example 12

This embodiment provides a device for realizing heavy oil weight by using suspension bed hydrogenation technology, as shown in fig. 1, includes a raw oil pretreatment unit, a catalyst slurry preparation unit, a suspension bed hydrogenation unit, a separation unit, and a fixed bed hydrogenation unit, which are connected in sequence, wherein:

referring to fig. 3, the raw oil pretreatment unit includes at least one adsorption device 32, a fan 35, a solid-liquid separation device 34, and a kneading device 36, an oil inlet and an air inlet are provided at a lower portion of the adsorption device 32, an oil pump 31 is connected to the oil inlet of the adsorption device, an oil outlet, an air outlet, and an adsorbent inlet are provided at an upper portion of the adsorption device 32, and an adsorbent adding device 33, specifically an adsorbent adding tank, is connected to the adsorbent inlet; the fan 35 is provided with an air suction port and an air exhaust port, the air suction port is communicated with the air outlet of the adsorption device 32, and the air exhaust port is connected with the air inlet of the adsorption device 32; the solid-liquid separation device 34 is provided with an inlet, a solid-phase outlet and a liquid-phase outlet, the inlet is communicated with the oil outlet of the adsorption device 32, and the liquid-phase outlet is connected with the first solvent inlet and/or the second solvent inlet; the feed inlet of the kneading device 36 is respectively communicated with the slag discharge port arranged at the bottom of the adsorption device 32 and the solid phase outlet of the solid-liquid separation device 34. In this embodiment, as shown in fig. 3, the adsorption device 32 is an adsorption tower, the number of the adsorption towers is 2, after the previous adsorption tower reaches the adsorption saturation, the previous adsorption tower can be switched to the next adsorption tower for adsorption, and in the process of performing adsorption, the adsorbent is added into the previous adsorption tower, after the next adsorption tower reaches the adsorption saturation, the previous adsorption tower can be switched to perform adsorption, and the operation is repeated, so that the operation is simple and convenient. The solid-liquid separation device 34 in this embodiment is a centrifuge, but in other embodiments the solid-liquid separation device 34 may also be a filter, such as a plate and frame filter or an automatic back-flushing filter.

The catalyst slurry preparing unit comprises a primary shearing and mixing subunit 1, a secondary shearing and mixing subunit 2 and a secondary shearing and mixing subunit 3, please refer to fig. 2, in this embodiment, the primary shearing and mixing subunit 1 comprises a catalyst preparing tank 21, a catalyst circulating pump 26, a primary powder-liquid shearing and mixing machine 24 and a first catalyst feeding system 28, the sidewall of the catalyst preparing tank is respectively provided with a first solvent inlet and a first slurry inlet, the bottom of the catalyst preparing tank is provided with a first slurry outlet, the first slurry outlet is connected with the liquid inlet of the primary powder-liquid shearing and mixing machine 24 through the catalyst circulating pump 26, the solid material inlet of the primary powder-liquid shearing and mixing machine 24 is communicated with the first catalyst feeding system 28, and the slurry outlet of the primary powder-liquid shearing and mixing machine 24 is connected with the first slurry inlet; the secondary shearing and mixing sub-unit 2 comprises a catalyst conveying tank 22, a secondary powder-liquid shearing mixer 27, a second catalyst feeding system 20 and a catalyst circulating pump 26, wherein a second solvent inlet and a second slurry inlet are respectively formed in the side wall of the catalyst conveying tank 22, a second slurry outlet is formed in the bottom of the catalyst conveying tank, a liquid inlet of the secondary powder-liquid shearing mixer 27 is connected with the second slurry outlet or the first slurry outlet through the catalyst circulating pump 26, a solid material inlet of the secondary powder-liquid shearing mixer 27 is communicated with the second catalyst feeding system 20, a slurry outlet of the secondary powder-liquid shearing mixer 27 is connected with the second slurry inlet, and the second slurry outlet is further connected with the catalyst mixing tank 29 through the secondary powder-liquid shearing mixer 25; the secondary shearing and mixing subunit 3 comprises a secondary powder-liquid shearing mixer 25 and a catalyst mixing tank 29, and the first slurry outlet is connected with the catalyst mixing tank 29 through the secondary powder-liquid shearing mixer 25; stirrers 23 are arranged at the lower parts of the catalyst preparation tank 21, the catalyst conveying tank 22 and the catalyst mixing tank 9, and the stirrers 23 comprise two layers of spiral stirring paddles.

As shown in fig. 1, the suspension bed hydrogenation unit includes a suspension bed hydrocracking reactor 5 and a suspension bed hydrogenation stabilizing reactor 6 connected in series, a slurry inlet of the suspension bed hydrocracking reactor 5 is connected with a discharge port of the catalyst mixing tank 29, and a slurry outlet of the suspension bed hydrogenation stabilizing reactor 6 is communicated with a feed port of the thermal high-pressure separator 7.

The separation unit comprises a hot high-pressure separator 7, a hot low-pressure separator 14, a cold high-pressure separator 12, a cold low-pressure separator 13, a stripping tower 15, an atmospheric tower, a vacuum tower 16 and a heat exchange unit; wherein, the hot high-pressure gas outlet of the hot high-pressure separator 7 is connected with the feed inlet of the cold high-pressure separator 13, and the hot high-pressure oil outlet of the hot high-pressure separator 7 is connected with the feed inlet of the hot low-pressure separator 14; a cold high-pressure oil outlet of the cold high-pressure separator 12 is connected with a feed inlet of the cold low-pressure separator 13, and a cold low-pressure oil outlet of the cold low-pressure separator 13 is connected with a feed inlet of the stripping tower 15; a hot low-pressure gas outlet of the hot low-pressure separator 14 is communicated with a feed inlet of the stripping tower 15, a hot low-pressure oil outlet of the hot low-pressure separator 14 is connected with a feed inlet of the normal pressure tower, a normal slag outlet is arranged at the bottom of the normal pressure tower, the normal slag outlet is connected with a feed inlet of the decompression tower 16 through an adsorption tank, an exhaust port is also arranged at the top of the normal pressure tower, and the exhaust port is communicated with a heavy naphtha oil collecting tank; the heat exchange unit comprises a first heat exchanger 8, a second heat exchanger 9, a third heat exchanger 10 and an air cooler 11 which are sequentially connected in series, the hot high-pressure gas exchanges heat with raw oil in the first heat exchanger 8, the hot high-pressure gas exchanges heat with cold hydrogen in the second heat exchanger 9, and the hot high-pressure gas exchanges heat with the cold low-pressure gas in the third heat exchanger 10;

referring to fig. 4, a hot low-pressure separation washing section is arranged in the hot low-pressure separator 14, the hot low-pressure separation washing section is located between the feed inlet of the hot low-pressure separator 14 and the hot low-pressure separation gas outlet, the hot low-pressure separation washing section is provided with a hot low-pressure separation washing liquid inlet and a hot low-pressure separation washing oil outlet, and the hot low-pressure separation washing liquid outlet is respectively connected with the hot low-pressure separation washing liquid inlet and the hot low-pressure separation oil outlet; the top and the bottom of the decompression tower 16 are respectively provided with a top reducing gas outlet and a bottom reducing oil outlet, the side wall of the decompression tower 16 is also provided with a feeding port, and the feeding port is communicated with the hot low-temperature oil outlet through a combustion furnace 4; the pressure reducing tower is internally provided with a first line reducing washing section, a second line reducing washing section and a third line reducing washing section from top to bottom, wherein the top of the feeding port is sequentially provided with the following steps: the three-line-reduction washing section is provided with a three-line-reduction washing liquid inlet and a three-line-reduction oil outlet, and the three-line-reduction oil outlet is respectively communicated with the three-line-reduction washing liquid inlet, the hot low-concentration washing liquid inlet and a three-line-reduction oil collecting device; the second-line-reducing washing section is provided with a second-line-reducing washing liquid inlet and a second-line-reducing oil outlet, and the second-line-reducing oil outlet is respectively connected with the second-line-reducing washing liquid inlet, the third-line-reducing washing oil inlet and a second-line-reducing oil collecting device; the first-line-reducing washing section is provided with a first-line-reducing washing liquid inlet and a first-line-reducing oil outlet, and the first-line-reducing oil outlet is respectively connected with the first-line-reducing washing liquid inlet and the first-line-reducing oil collecting device; and an asphalt forming device is connected with the bottom reducing oil outlet. In this embodiment, the hot low branch washing section subtract a line washing section subtract the second line washing section with it all includes from last to down washing liquid distributor, filler and the washing oil header that sets gradually to reduce three way washing section the bottom of washing oil header is equipped with an inclined plane, the inclined plane is 5 ~ 30 with the contained angle of horizontal direction, the hot low branch washing oil export subtract a line oil export reduce the second line oil export with it all sets up in the inclined plane minimum of respective corresponding washing oil header to it can not deposit at washing oil header to guarantee solid particle.

The fixed bed hydrogenation unit comprises a fixed bed hydrogenation reactor and a separation tower, wherein a feed inlet of the fixed bed hydrogenation reactor is respectively connected with a tower bottom oil outlet of the stripping tower 15, a first reduction line oil outlet and a second reduction line oil outlet of the decompression tower 16, a discharge outlet of the fixed bed hydrogenation reactor is communicated with the separation tower, and the separation tower is provided with a light oil outlet and a tail oil outlet.

In another embodiment, as shown in fig. 5, the first stage shear mixing sub-unit 1 comprises a solvent booster pump 58, a venturi 56, a solid catalyst feed system 55, and a slurry make-up tank 52; one end of the venturi tube 56 is a solvent inlet, the other end is a slurry outlet, a catalyst inlet is arranged on the side wall of the venturi tube 56, the catalyst inlet is connected with the solid catalyst feeding system 55, the solvent inlet is communicated with the solvent booster pump 58, and a solvent buffer tank is further connected with the inlet of the solvent booster pump 58; the side wall of the slurry preparation tank 52 is respectively provided with a solvent inlet and a slurry inlet, the bottom of the slurry preparation tank is provided with a slurry outlet, and the slurry inlet is connected with the slurry outlet of the venturi tube 56; the secondary shearing and mixing subunit 2 comprises a shearing mixer 57 and a slurry mixing tank 53, and the slurry outlet of the slurry preparation tank 52 is connected with the slurry mixing tank 53 through the shearing mixer 57; stirring equipment 54 is arranged on the lower portions of the slurry preparation tank 52 and the slurry mixing tank 53, the stirring equipment 54 comprises two layers of spiral stirring paddles, and the rotating speed of a main shaft of the stirring equipment is 100-300 r/min.

Comparative example 1

This comparative example is a method for producing high-quality fuel oil by hydrocracking heavy oil disclosed in chinese patent document CN104388117A, and is described in the specification, paragraph 29.

Evaluation of Process Effect

The conversion of the raw oil, the yield of light oil and the coke formation in the processes of the above examples 3, 8, 9 and 10 and comparative example 1 of the present invention were calculated according to the following formulas to evaluate the effects of the processes, and the results are shown in Table 5.

The conversion rate of raw oil is less than 524 ℃ component mass (gas)/raw oil mass multiplied by 100 percent;

the yield of light oil is less than 350 ℃ and the mass of the fraction section/the mass of the raw oil is multiplied by 100 percent;

the coke rate is equal to toluene insoluble matter mass/raw oil mass multiplied by 100 percent;

the yield of wax oil is equal to the mass of the fraction segment at the temperature of more than 350 ℃ and less than 524 ℃ per the mass of the raw oil multiplied by 100 percent.

TABLE 5

	Conversion of raw oil/wt%	Yield of light oil/wt%	Yield of wax oil/wt%	Coke rate/wt%
					Example 3	94.8	60.2	34.2	1.53
Example 8	95.4	65.7	29.3	1.37
					Example 9	97.7	67.6	27.1	1.08
Example 10	98.8	70.8	25.1	1.67
					Comparative example 1	90.2	55.6	28.4	5.25

The quality of the light oil produced by the processes described in the above examples 8 to 10 and comparative example 1 of the present invention is shown in Table 6:

TABLE 6 quality of light oils

The yields and qualities of the asphalts produced by the processes of examples 8-10 and comparative example 1 are shown in Table 7:

TABLE 7 yield and quality of bitumen

	Penetration degree	Ductility (cm)	Softening Point (. degree. C.)	Yield (%)
					Example 8	92	49	44	3.1
Example 9	88	44	47	4.0
					Example 10	86	42	48	3.5
Comparative example 1	95	53	42	13.1

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims

1. A suspension bed hydrogenation process for treating heavy oil comprises the following steps:

(3) carrying out thermal high-pressure separation on the suspension bed hydrogenation product obtained in the step (2), and respectively collecting thermal high-pressure separation gas and thermal high-pressure separation oil; the hot high-pressure separation gas is subjected to cold high-pressure separation and cold low-pressure separation in sequence to obtain cold low-pressure separation oil, the hot high-pressure separation oil is subjected to hot low-pressure separation to obtain hot low-pressure separation gas and hot low-pressure separation oil, the hot low-pressure separation gas and the cold low-pressure separation oil are subjected to steam stripping separation and then are converted into dry gas, naphtha and tower bottom oil, the hot low-pressure separation oil is subjected to reduced pressure distillation, and first line oil and second line oil are collected;

feeding the first-line reducing oil, the second-line reducing oil and the tower bottom oil into a fixed bed hydrogenation reactor for carrying out hydrogenation treatment again, then separating a fixed bed hydrogenation product, and collecting a light oil product at the temperature of less than 350 ℃;

the technological parameters of the thermal high-pressure separation are as follows: the pressure is 18-22.5 MPa, and the temperature is 350-460 ℃;

the temperature of the steam stripping separation is 80-90 ℃;

the first-line reduction operating temperature in the reduced pressure distillation is 110-210 ℃, and the second-line reduction operating temperature is 200-300 ℃.

2. The slurry bed hydrogenation process for heavy oil treatment according to claim 1, wherein the slurry bed hydrocracking catalyst is contained in the catalyst slurry in an amount of 0.1 to 10% by mass and has a particle size of 5 to 500 μm.

3. The slurry hydrogenation process for treating heavy oil according to claim 1, wherein the slurry hydrocracking catalyst comprises a composite carrier and an active metal oxide supported on the composite carrier, and the mass ratio of active metals in the composite carrier to the active metal oxide is 100: (0.5-10), wherein:

the active metal is a metal of a VIII group and/or a VIB group;

4. The suspended bed hydrogenation process for heavy oil treatment according to claim 3, wherein the catalytic cracking spent catalyst comprises the following components in parts by weight:

15-55 parts of a Y-type molecular sieve;

15-55 parts of aluminum oxide;

0.5-1 part of at least one of nickel, vanadium or iron.

5. The slurry bed hydrogenation process for treating heavy oil according to any one of claims 1 to 4, wherein the feedstock is a purified oil, and the purification treatment comprises the following steps:

6. According to claim 5The suspension bed hydrogenation process for treating heavy oil is characterized in that the adsorption is carried out at 50-100 ℃ and 0-1.0 MPa, and the mass ratio of the raw oil to the adsorbent is 1: (0.05-0.2), the specific surface area of the semi-coke is 100-500m²The specific surface area of the kaolin is 50-200m²/g。

7. The suspension bed hydrogenation process for treating heavy oil according to claim 1, wherein the suspension bed hydrogenation reactor comprises two reactors connected in series, one of the reactors is a suspension bed hydrocracking reactor, the other reactor is a suspension bed hydrogenation stabilizing reactor, and the operating temperature in the suspension bed hydrogenation stabilizing reactor is 20-50 ℃ lower than the operating temperature in the suspension bed hydrocracking reactor.

8. The suspension bed hydrogenation process for treating heavy oil according to claim 7, wherein the catalyst slurry is mixed with the remaining raw oil and hydrogen and then enters the suspension bed hydrocracking reactor to undergo hydrocracking reaction, so as to obtain a hydrocracking product; then sending the hydrocracking product into the suspension bed hydrogenation stabilization reactor, and carrying out hydrofining in the presence of a suspension bed hydrogenation stabilization catalyst, thereby forming the suspension bed hydrogenation product;

9. The suspended bed hydrogenation process for treating heavy oil according to claim 1, wherein in step (3), the hot distillate oil is distilled under normal pressure, and fractions at 150-250 ℃ and above 250 ℃ are collected respectively; and heating the fraction at the temperature of more than 250 ℃, then carrying out reduced pressure distillation, and combining the fraction at the temperature of 150-250 ℃ with the naphtha.

10. The suspended bed hydrogenation process for treating heavy oil according to claim 1, wherein the vacuum distillation further obtains a third line-reducing oil, 80-90 wt% of the third line-reducing oil is combined with 5-20 wt% of the third line-reducing oil to be used as a third line-reducing washing liquid, the remaining 10-20 wt% of the third line-reducing oil is used as a hot low-temperature-component washing liquid to obtain the hot low-temperature-component washing liquid while washing oil gas generated by the hot low-pressure separation, and 30-90 wt% of the hot low-temperature-component washing liquid is recycled to be used as the hot low-temperature-component washing liquid;

11. The suspended bed hydrogenation process for heavy oil treatment according to claim 1, wherein:

12. The suspended bed hydrogenation process for heavy oil treatment according to claim 1, wherein the cold high partial gas obtained by cold high pressure separation is used as recycle hydrogen, and the cold low partial gas obtained by cold high partial oil separation is mixed with the dry gas to be used as fuel gas.

13. The suspended bed hydrogenation process for treating heavy oil according to claim 1 or 7, wherein:

a discharge system is connected with the suspension bed hydrogenation reactor and comprises a discharge pipeline, a cooling separation system, a torch system and a raw oil recycle system, wherein one end of the discharge pipeline is connected with the bottom of the suspension bed hydrogenation reactor, and the other end of the discharge pipeline is connected with the cooling separation system;

when the temperature of the suspension bed hydrogenation reactor rises to exceed the normal reaction temperature instantly, a feed valve of the suspension bed hydrogenation reactor is closed, a discharge valve group in the cooling separation system is opened, so that the material in the suspension bed hydrogenation reactor is reduced to 0.6-1.0MPa through a pressure reduction pore plate on a discharge pipeline and then is discharged into the cooling separation system for cooling separation treatment to obtain a gas phase material and a liquid-solid phase material, the gas phase material is discharged to the torch system, and the liquid-solid phase material is conveyed to the raw oil recycling system, so that the emergency discharge of the suspension bed hydrogenation reactor is realized.

14. The suspended bed hydrogenation process for heavy oil treatment according to claim 13, wherein: the material in the suspension bed hydrogenation reactor firstly enters a discharge tank of the cooling separation system, is mixed with the flushing oil in the discharge tank for cooling, and the cooled liquid-solid phase material is discharged into the raw oil recycling system through a discharge pipeline connected with the bottom of the discharge tank; the gas that obtains after the cooling warp the gas release pipeline that the tank top of bleeding is connected gets into and cools off and divide liquid in the air cooler of promptly bleeding, and the gaseous phase material that obtains after dividing the liquid sends into torch system, the liquid phase material that obtains after dividing the liquid returns in the tank of bleeding and finally discharge in the raw oil refining system, thereby can ensure suspension bed hydrogenation ware's urgent bleeding.