CN117701303A - Heavy oil processing technology and processing system - Google Patents
Heavy oil processing technology and processing system Download PDFInfo
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a heavy oil processing technology and a processing system, wherein the heavy oil processing technology comprises the following contents: the heavy oil raw material enters a first ebullated bed reaction zone for reaction, and a first gas phase material flow and a first liquid phase material flow are obtained after reaction products are separated; the obtained first liquid phase material flow enters a second ebullated bed reaction zone for reaction, and a second gas phase material flow and a second liquid phase material flow are obtained after reaction products are separated; separating the second liquid phase material flow to obtain light fraction and heavy fraction; the obtained heavy fraction enters a first extraction zone and contacts with an extraction solvent to obtain a first extraction phase material flow and a first raffinate phase material flow; the first extract phase material flow enters a second extraction zone and contacts with an extraction solvent to obtain a second extract phase material flow and a second raffinate phase material flow; the second extract phase material flow enters a separation unit, and an oil phase material flow is obtained after the extraction solvent is recovered. The heavy oil processing system adopting the processing technology is also provided. The heavy oil processing technology and the processing system provided by the invention can realize operation of boiling bed heavy oil hydrogenation under high conversion rate, and ensure long-period stable operation of the device.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a heavy oil ebullated bed processing technology and a processing system.
Background
In recent years, the deep processing of inferior heavy oil has become an important point for the technical development of the oil refining industry, and mainly comprises a hydrogenation technology and a decarburization technology. The boiling bed heavy oil hydrogenation technology has the remarkable advantages in the aspect of heavy oil lightening, has the advantages of capability of on-line replacement of a catalyst, high utilization rate, long operation period, flexible operation of the device and the like, can meet the requirements of large-scale and long-period operation of the device, and has the important role in the existing refining and transformation process.
The current worldwide ebullated bed hydrocracking technology mainly includes H-Oil process and T-Star process of Axens, france, LC-finishing process of CLG, USA, and the global total ebullated bed hydrocracking device is nearly 30 sets. At present, 3 sets of H-Oil fluidized bed hydrocracking devices are introduced in China and are respectively built in constant force petrochemical and medium petrochemical sea-level refining, and the total residual Oil processing amount reaches 900 ten thousand tons/year. With the heavy weight of processed crude oil, the boiling bed hydrocracking technology increasingly stands out the advantages of the heavy oil processing unit which is a vital link of a refinery.
CN 106947523A the invention discloses a hydrocracking method for ebullated-bed residuum. The method comprises two boiling bed reactors connected in series, wherein a residual oil hydrotreating catalyst is adopted in the first boiling bed reactor, and a residual oil hydrocracking catalyst is adopted in the second boiling bed reactor. The high conversion of the sediment in this catalyst configuration makes it difficult to ensure a stable long-term operation of the device.
USP3809644 discloses a multi-stage ebullated bed hydrogenation process for producing low sulfur fuel oils from petroleum residuum of high sulfur and high metal content. The process comprises three reactors, wherein the first reactor is filled with demetallization catalyst, the second reactor is filled with demetallization and desulfurization catalyst, and the third reactor is filled with desulfurization catalyst. The method adopts a conventional residuum hydrotreating catalyst, has lower conversion rate on residuum, and increases the formation of sediment in the generated oil if the conversion rate is increased, thereby influencing the running period of the device.
CN103102944a discloses an integrated process for hydrocracking residuum and solvent deasphalting, wherein a residuum hydrocarbon fraction and hydrogen are reacted in a first ebullated bed hydroconversion reactor system and then enter a fractionation system, vacuum residuum is fed into a solvent deasphalting system to obtain deasphalted asphalt and deasphalted oil, wherein the deasphalted asphalt and the deasphalted oil are respectively hydrotreated, the resultant oil is fed into the fractionation system, and a vacuum fractionation unit is disposed in the fractionation system in the process, so that coking risk still exists.
CN108102706a discloses a heavy oil hydrotreating method, heavy oil raw materials are fractionated to obtain light fraction and heavy fraction, the heavy fraction enters a solvent deasphalting device, and deasphalted oil and deasphalted asphalt are obtained after treatment; the deasphalted oil is treated by adopting a fixed bed, the generated oil obtained by the fixed bed hydrotreatment enters a fluidized bed hydrocracking reaction zone, and the reaction effluent of the fluidized bed hydrocracking reaction zone is separated to obtain gas, gasoline, diesel oil, wax oil and unconverted oil. The coking tendency of a follow-up fractionating system of the ebullated bed of the heavy oil treatment method is very low, and the coking tendency is mainly the reason for high quality of processed raw materials, the conversion rate of heavy fraction in the process flow is low, meanwhile, the characteristic of strong adaptability to poor raw materials is not exerted by ebullated bed hydrogenation, and the high-efficiency conversion of heavy raw materials is difficult to realize.
Disclosure of Invention
The applicant finds that the core factor restricting the long-period stable operation of the boiling bed heavy oil hydrogenation device is the problem of coking of a fractionation system at present in the research process, especially the coking of a vacuum fractionation tower in the fractionation system seriously affects the long-period stable operation of the whole device, the vacuum fractionation tower needs to be subjected to decoking treatment regularly, meanwhile, a heat exchanger (usually adopting a spiral plate structure heat exchanger) of bottom oil of the vacuum fractionation tower is easy to be blocked, and a standby heat exchanger needs to be cleaned regularly and arranged for switching use, so that the investment cost and the operation cost of the device are greatly increased. Research shows that the stable colloid structure in petroleum is destroyed during hydroconversion, the petroleum colloid stability depends on the hydrocarbon composition and content of petroleum, the stability is in dynamic balance, and the system can exist stably only when the four component content and composition in the oil phase are matched, the stability of the hydrogenated residual oil colloid is reduced, and the stability coefficient is reduced. Compared with the fixed bed residuum hydrogenation process, the ebullated bed residuum hydrogenation process is generally operated at a higher residuum conversion rate, which tends to cause easier damage to the residuum system, and the content of sediment in the hydrogenated oil exhibiting stability parameters is higher. However, the boiling bed hydrogenation technology can convert more heavy components in residual oil into light oil products and chemical raw materials, can realize online addition and discharge of catalysts, ensures long-period operation of the device, and is a hydrogenation technology with great advantages in the current transformation process of oil refining structures.
Aiming at the defects in the prior art, the main purpose of the invention is to provide a heavy oil processing technology and a processing system, which can realize that the heavy oil hydrogenation of a boiling bed is operated under high conversion rate and ensure the long-period stable operation of the device.
The first aspect of the present invention provides a heavy oil processing process, comprising the steps of:
(1) The heavy oil raw material enters a first ebullated bed reaction zone, and reacts under the action of hydrogen and a first hydrogenation catalyst, and a reaction product is separated to obtain a first gas phase material flow and a first liquid phase material flow;
(2) The first liquid phase material flow obtained in the step (1) enters a second ebullated bed reaction zone, and reacts under the action of hydrogen and a second hydrogenation catalyst, and a reaction product is separated to obtain a second gas phase material flow and a second liquid phase material flow;
(3) Separating the second liquid phase material flow obtained in the step (2) to obtain a light fraction and a heavy fraction;
(4) The heavy fraction obtained in the step (3) enters a first extraction zone and contacts with an extraction solvent to obtain a first extraction phase material flow and a first raffinate phase material flow;
(5) The first extract phase material flow obtained in the step (4) enters a second extraction zone and contacts with an extraction solvent to obtain a second extract phase material flow and a second raffinate phase material flow;
(6) And (3) feeding the second extract phase material flow obtained in the step (5) into a separation unit, and recovering the extraction solvent to obtain an oil phase material flow.
Further, in the heavy oil processing technology, the heavy oil raw material in the step (1) may be one or more selected from atmospheric residuum, vacuum residuum, oilfield thick oil, heavy fuel oil, oil sand, coal tar, ethylene tar and the like, and optionally one or more selected from catalytic slurry oil, vacuum wax oil and furfural extract oil.
Further, in the heavy oil processing technology, the first ebullated bed reaction zone is provided with at least one ebullated bed hydrogenation reactor, and the ebullated bed reactor can adopt at least one of the existing ebullated bed reactors, specifically can adopt a ebullated bed reactor with a circulating cup and a STRONG ebullated bed reactor with a built-in three-phase separator developed by China petrochemical and large-connection petrochemical industry institute, and preferably adopts a STRONG ebullated bed reactor with a built-in three-phase separator developed by China petrochemical industry institute. When the ebullated bed reactor with the circulating cup is adopted, a unit with a gas-liquid separation function is required to be arranged between the first ebullated bed reaction zone and the second ebullated bed reaction zone, for example, a high-pressure separation unit is adopted, and the main purpose of the unit is to separate hydrogen and light hydrocarbon components from heavy fractions in the reaction product of the first ebullated bed reactor; when the STRONG ebullated bed reactor with the built-in three-phase separator developed by China petrochemical industry institute is adopted, the gas phase and the liquid phase can be directly separated in the reactor without arranging a unit with a gas-liquid separation function because the STRONG ebullated bed reactor is internally provided with the three-phase separator.
Further, in the heavy oil processing technology, the operating conditions of the first ebullated-bed reaction zone are as follows: the reaction temperature is 350-450 ℃, preferably 380-430 ℃, the reaction pressure is 10.0-20.0 MPa, preferably 15.0-18.0 MPa, the hydrogen-oil volume ratio is 400-2000, preferably 500-1500, and the liquid hourly space velocity is 0.1-5.0 h -1 Preferably 0.2 to 2.0h -1 。
Further, in the heavy oil processing technology, the second ebullated bed reaction zone is provided with at least one ebullated bed hydrogenation reactor, and the ebullated bed reactor can adopt at least one of the existing ebullated bed reactors, specifically can adopt a ebullated bed reactor with a circulating cup and a STRONG ebullated bed reactor with a built-in three-phase separator developed by China petrochemical and large-connection petrochemical industry institute, and preferably adopts a STRONG ebullated bed reactor with a built-in three-phase separator developed by China petrochemical industry institute.
Further, in the heavy oil processing technology, the first hydrogenation catalyst filled in the first ebullated bed reaction zone can be prepared by adopting a commercial catalyst or a preparation method disclosed by the prior art, such as a series of ebullated bed hydrodemetallization catalysts developed by Dalian petrochemical institute of China petrochemical Co., ltd. Typically, the first catalyst comprises a support and an active metal component, wherein the active metal is a group VIB and/or VIII metal, and may specifically be one or more of nickel, cobalt, molybdenum or tungsten; the carrier can be one or more of alumina, silica, alumina-silica and titania.
Further, in the heavy oil processing technology, the second hydrogenation catalyst filled in the second ebullated bed reaction zone can be prepared by adopting a commercial catalyst or a preparation method disclosed by the prior art, such as a series of ebullated bed hydrogenation catalysts developed by Dalian petrochemical institute of China petrochemical Co., ltd. Typically, the first catalyst comprises a support and an active metal component, wherein the active metal is a group VIB and/or VIII metal, and may specifically be one or more of nickel, cobalt, molybdenum or tungsten; the carrier can be one or more of alumina, silica, alumina-silica and titania.
Further, in the heavy oil processing technology, the operating conditions of the second ebullated-bed reaction zone are as follows: the reaction temperature is 350-450 ℃, preferably 380-430 ℃, the reaction pressure is 10.0-20.0 MPa, preferably 15.0-18.0 MPa, the hydrogen-oil volume ratio is 400-2000, preferably 500-1500, and the liquid hourly space velocity is 0.1-5.0 h -1 Preferably 0.2 to 2.0h -1 。
Further, in the heavy oil processing process, the cutting point of the light fraction and the heavy fraction is 180 to 450 ℃, preferably 260 to 400 ℃.
Further, in the heavy oil processing technology, the first gas phase material flow and the second gas phase material flow enter a hydrogen recovery unit for treatment, and the hydrogen recovery unit adopts any one of the existing hydrogen recovery devices in the field, and can be selected by a person skilled in the art according to practical situations. Generally comprises a hot high-pressure separator, a cold high-pressure separator, a hydrocarbon recovery unit, a circulating hydrogen desulfurization unit and a membrane separation unit, and the circulating hydrogen and the light hydrocarbon are obtained after treatment, wherein the circulating hydrogen can be recycled to the first ebullated bed reaction zone and/or the second ebullated bed reaction zone.
Further, in the heavy oil processing technology, the light fraction obtained after the separation of the second liquid phase stream is mainly naphtha fraction and diesel fraction, wherein the naphtha fraction can be used as a raw material for producing olefin by a steam cracking device or used as a raw material for producing aromatic hydrocarbon by a reforming device according to the hydrocarbon composition difference of the naphtha fraction. The diesel fraction can enter a hydrofining unit to produce clean diesel products, and can also be used as a raw material of a hydrocracking unit to produce light chemical product raw materials.
Further, in the heavy oil processing technology, the extraction solvent used in the first extraction zone may be at least one of alkane and naphtha, wherein the alkane is at least one of C3-C7.
Further, in the heavy oil processing technology, the operation conditions of the first extraction zone are as follows: the temperature is 80-200 ℃, preferably 100-160 ℃, the pressure is 2.0-6.0 MPa, preferably 3.0-5.0 MPa, and the volume ratio of the solvent is 1.0-10.0, preferably 3.0-8.0. The yield of the first raffinate stream is controlled between 20wt% and 70wt%, preferably between 30wt% and 55wt%.
Further, in the heavy oil processing technology, the first raffinate phase material flow can be completely or partially returned to the first ebullated bed reaction zone for treatment, and if part of the first raffinate phase material flow is returned to the first ebullated bed reaction zone, the rest material flow can be used as a coking raw material for producing low-sulfur petroleum coke or used as a hydrogen production raw material; alternatively, the first raffinate stream may be used directly as a coker for producing low sulfur petroleum coke, or as a hydrogen production feedstock, without being returned to the first ebullated bed reaction zone for treatment.
Further, in the heavy oil processing process described above, the first raffinate stream is preferably mixed with the oil-soluble catalyst and returned to the first ebullated-bed reaction zone. The oil soluble catalyst is added in an amount of 0.05wt% to 5wt%, preferably 0.5wt% to 2wt% based on the weight of the first raffinate stream. The oil soluble catalyst may be a slurry bed residuum hydrogenation catalyst.
Further, in the heavy oil processing technology, the extraction solvent used in the second extraction zone may be at least one of alkane and naphtha, wherein the alkane is at least one of C3-C7.
Further, in the heavy oil processing technology, the operating conditions of the second extraction zone are as follows: the temperature is 80-200 ℃, preferably 120-160 ℃, the pressure is 2.0-6.0 MPa, preferably 3.0-5.0 MPa, and the volume ratio of the solvent is 1.0-10.0, preferably 3.0-8.0. The yield of the second raffinate stream is controlled between 10wt% and 50wt%, preferably between 10wt% and 30wt%.
Further, in the heavy oil processing process, the second raffinate stream may be returned to the first ebullated bed reaction zone and/or the second ebullated bed reaction zone in whole or in part, and when partially returned, the remaining portion may be used as a feedstock or pitch for catalytic cracking, hydrocracking, delayed coking, etc., and a low sulfur ship-fuel blending component.
Furthermore, in the heavy oil processing technology, the second raffinate phase material flow can be directly used as the feed or asphalt of catalytic cracking, hydrocracking, delayed coking and other devices and the low-sulfur ship combustion blending component without returning to the first ebullated bed reaction zone and/or the second ebullated bed reaction zone.
In the heavy oil processing technology, the separation unit adopts supercritical solvent separation, the extraction solvent obtained after separation is returned to the first extraction zone and/or the second extraction zone for use, the oil phase material flow is directly discharged out of the device as a product, and the oil phase material flow can be used as a feeding material of a hydrocracking device or a feeding material of a catalytic cracking device and can also be used as conveying oil or quenching oil during online replacement of a hydrogenation catalyst used in the ebullated bed reaction zone.
A second aspect of the present invention provides a heavy oil processing system comprising:
the first ebullated bed reaction zone is used for receiving heavy oil raw materials, and reacting under the action of hydrogen and a first hydrogenation catalyst to obtain a reaction product after the reaction;
a first separation unit for receiving the reaction product of the first ebullated-bed reaction zone, after separation, to obtain a first vapor phase stream and a first liquid phase stream;
a second ebullated-bed reaction zone for receiving the first liquid phase stream from the first separation unit and reacting with hydrogen and a second hydrogenation catalyst to obtain a reaction product;
a second separation unit for receiving the reaction product of the second ebullated-bed reaction zone, after separation, to obtain a second vapor phase stream and a second liquid phase stream;
a third separation unit for receiving the second liquid phase stream from the second separation unit, after separation, to obtain a light fraction and a heavy fraction;
a first extraction zone for receiving the heavy fraction from the third separation unit and contacting with an extraction solvent to produce a first extract phase stream and a first raffinate phase stream;
a second extraction zone for receiving the first extract phase stream from the first extraction zone, contacting with an extraction solvent to produce a second extract phase stream and a second raffinate phase stream;
a fourth separation unit for receiving the second extract phase stream from the second extraction zone, and separating to obtain an extraction solvent and an oil phase stream.
Further, in the heavy oil processing system, the first raffinate stream is returned to the first ebullated-bed reaction zone via a pipeline.
Further, in the heavy oil processing system, the second raffinate stream is returned to the first ebullated-bed reaction zone and/or the second ebullated-bed reaction zone via a pipeline.
Further, in the heavy oil processing system, the first ebullated bed reaction zone is provided with at least one ebullated bed hydrogenation reactor, and the ebullated bed reactor can adopt at least one of the existing ebullated bed reactors, specifically can adopt a ebullated bed reactor with a circulating cup and a STRONG ebullated bed reactor with a built-in three-phase separator developed by the institute of petrochemical industry and petrochemical industry, and preferably adopts a STRONG ebullated bed reactor with a built-in three-phase separator developed by the institute of petrochemical industry and petrochemical industry.
Furthermore, in the heavy oil processing system, the first separation unit is equipment with a gas-liquid separation function, such as a gas-liquid separator, when the STRONG ebullated bed reactor of the built-in three-phase separator developed by China petrochemical industry institute is adopted, the first separation unit can be omitted, and the three-phase separator in the reactor can realize gas-liquid two-phase separation.
Further, in the heavy oil processing system, the second ebullated bed reaction zone is provided with at least one ebullated bed hydrogenation reactor, and the ebullated bed reactor can adopt at least one of the existing ebullated bed reactors, specifically can adopt a ebullated bed reactor with a circulating cup and a STRONG ebullated bed reactor with a built-in three-phase separator developed by the institute of petrochemical industry and petrochemical industry, and preferably adopts a STRONG ebullated bed reactor with a built-in three-phase separator developed by the institute of petrochemical industry and petrochemical industry.
Furthermore, in the heavy oil processing system, the second separation unit is equipment with a gas-liquid separation function, such as a gas-liquid separator, when the STRONG ebullated bed reactor of the built-in three-phase separator developed by China petrochemical industry institute is adopted, the first separation unit can be omitted, and the three-phase separator in the reactor can realize gas-liquid two-phase separation.
Further, in the heavy oil processing system, the third separation unit may be any one of an atmospheric fractionating tower, a flash tank, and the like.
Furthermore, in the heavy oil processing system, the first extraction zone may be an existing extraction tower, and a turntable tower or a packing tower, preferably a packing tower, may be selected according to the internal structure of the extraction tower; the filler can be selected from one or more of a grid, a Raschig ring and a pall ring, and is preferably a grid.
Furthermore, in the heavy oil processing system, the second extraction zone may be an existing extraction tower, and a turntable tower or a packing tower, preferably a packing tower, may be selected according to the internal structure of the extraction tower; the filler can be selected from one or more of a grid, a Raschig ring and a pall ring, and is preferably a grid.
Further, in the heavy oil processing system, the fourth separation unit comprises an existing conventional solvent recovery tower, and an inner member can be arranged in the tower, wherein the inner member can be a tower plate or a filler, and is preferably a filler; the filler is generally selected from one or more of a grid, a Raschig ring and a pall ring, and is preferably a grid.
Compared with the prior art, the heavy oil processing technology and the heavy oil processing system provided by the invention have the following advantages:
1. the heavy oil processing system of the invention eliminates a subsequent decompression fractionation device for ebullated bed conversion, adopts a solvent deasphalting device to realize a fraction separation function, and further avoids the coking problem of the decompression fractionation device caused by poor stability of oil generated by the ebullated bed; meanwhile, the characteristic of poor stability of the oil generated by the boiling bed is skillfully utilized, and the fraction separation can be promoted by adopting a solvent extraction mode, so that the separation efficiency is greatly improved.
2. In the heavy oil processing technology, the heavy oil is skillfully returned to different reaction units of the boiling bed for processing according to the property characteristics of different fractions separated from the oil solvent generated by the hydrogenation of the boiling bed. The first raffinate phase material flow obtained in the first extraction zone is mainly enriched with colloid and asphaltene molecules with larger structures, contains more aromatic components, and has higher sulfur content, but compared with residual oil molecules, the molecular structure size is greatly reduced, the molecular structure size is returned to the first ebullated bed reaction zone, the pore channel structure and hydrogenation performance of the catalyst in the first ebullated bed reaction zone are fully utilized, and the efficient conversion of the fraction molecules can be realized. Meanwhile, the second raffinate phase material flow obtained from the second extraction zone containing more aromatic components and colloid components enters the second ebullated bed reaction zone, so that the stability of a reaction system can be further improved, and meanwhile, the aromatic components with relatively smaller molecular weight can be dissociated among macromolecules, so that the hydrogenation reaction of the macromolecules can be promoted, and the residual oil conversion rate is further improved. In addition, the second extract phase material flow can also enter the first ebullated bed reaction zone, so that the viscosity of the feeding residual oil can be reduced, and the impurity removal rate can be improved.
3. The heavy oil processing process flow is more flexible, the product structure is flexible and variable, the first raffinate phase material flow and the second raffinate phase material of the extraction unit can be returned to the ebullated bed hydrogenation unit for direct processing, and can also be used as the feed of a subsequent processing unit, for example, the first raffinate phase material flow is used as a hydrogen production raw material, and the second raffinate phase material can be used as a low-sulfur ship combustion blending component or a low-sulfur petroleum coke raw material; the oil phase stream of the extraction unit may be used as a feedstock for hydrocracking or catalytic cracking (cracking). In the process that the first raffinate phase material flow of the extraction unit returns to the first reaction zone of ebullated bed hydrogenation, a dispersive oil-soluble catalyst is selected, so that the conversion of heavy components can be further promoted.
Drawings
FIG. 1 is a schematic diagram of a heavy oil processing process and processing system of the present invention;
wherein, 1-raw oil; 2-a first ebullated bed reaction zone; 3-a first separation unit; 4-a first liquid phase stream; a 5-second ebullated bed reaction zone; 6-a first gas phase stream; 7-a second separation unit; 8-a second liquid phase stream; 9-a third separation unit; 10-a second gas phase stream; 11-a hydrogen recovery unit; 12-circulating hydrogen; 13-heavy fraction; 14-a first extraction zone; 15-a first extract phase stream; 16-a second extraction zone; 17-a second extract phase stream; 18-a fourth separation unit; 19-regenerating the extraction solvent; 20-a first raffinate stream; 21-a second raffinate stream; 22-an oil phase stream; 23-light hydrocarbon component; 24-light fraction.
FIG. 2 is a process flow diagram employed in comparative example 1 of the present invention;
1-raw oil; 2-a first ebullated bed reaction zone; 3-a first separation unit; 4-a first liquid phase stream; a 5-second ebullated bed reaction zone; 6-a first gas phase stream; 7-a second separation unit; 8-a second gas phase stream; 9-a hydrogen recovery unit; 10-circulating hydrogen; 11-light hydrocarbon component; 12-a second liquid phase stream; 13-an atmospheric fractionation unit; 14-hydrogenated naphtha fraction; 15-a hydrogenated diesel fraction; 16-hydrogenation of atmospheric residuum fraction; 17-a reduced pressure fractionation unit; 18-a hydrogenated wax oil fraction; 19-hydrogenated vacuum residuum.
FIG. 3 is a process flow diagram for comparative example 2 of the present invention;
1-raw oil; 2-a first ebullated bed reaction zone; 3-a first separation unit; 4-a first liquid phase stream; a 5-second ebullated bed reaction zone; 6-a first gas phase stream; 7-a second separation unit; 8-a second gas phase stream; 9-a hydrogen recovery unit; 10-circulating hydrogen; 11-light hydrocarbon component; 12-a second liquid phase stream; 13-an atmospheric fractionation unit; 14-hydrogenated naphtha fraction; 15-a hydrogenated diesel fraction; 16-hydrogenation of atmospheric residuum fraction; 17-a reduced pressure fractionation unit; 18-a hydrogenated wax oil fraction; 19-hydrogenated vacuum residuum; 20-an extraction zone; 21-raffinate stream; 22-extract stream; 23-a solvent recovery unit; 24-an oil phase stream; 25-regenerating the solvent.
Detailed Description
The technical features of the present invention will be further described below by way of specific examples in conjunction with the accompanying drawings, but these examples are not intended to limit the present invention.
As shown in fig. 1, the heavy oil processing technology provided by the invention comprises the following contents: raw oil 1 and hydrogen 12 are mixed and enter a first ebullated-bed reaction zone 2, a reacted material flow enters a first separation zone 3 and is separated into a first gas-phase material flow 6 and a first liquid-phase material flow 4, wherein the first liquid-phase material flow 4 is mixed with the hydrogen 12 and enters a second ebullated-bed reaction zone 5, a reaction product enters a second gas-phase material flow 10 and a second liquid-phase material flow 8 which are obtained after separation in a second separation zone 7, and the second gas-phase material flow 10 and the first gas-phase material flow 6 enter a hydrogen recovery unit 11 and are treated to obtain circulating hydrogen 12 and a light hydrocarbon component 23; the second liquid phase stream 8 enters a third separation unit 9 for separation to obtain a light fraction 24 and a heavy fraction 13; the heavy fraction 13 enters a first extraction zone 14, and is contacted with an extraction solvent to obtain a first extraction phase stream 15 and a first raffinate phase stream 20, wherein the first extraction phase stream 15 enters a second extraction zone 16, is contacted with the extraction solvent to obtain a second extraction phase stream 17 and a second raffinate phase stream 21, the second extraction phase stream 17 enters a fourth separation unit 18, a regenerated extraction solvent 19 and an oil phase stream 22 are obtained through separation, and the regenerated extraction solvent 19 is returned to the first extraction zone 14 and the second extraction zone 16 for recycling.
The vacuum residuum obtained in the examples and comparative examples of the present invention using the current atmospheric and vacuum apparatus had a density (20 ℃ C.) of 1.105g/cm 3 Sulfur contentThe amount of the catalyst is 4.3wt%, the nitrogen content is 5200mg/kg, the carbon residue is 26.4wt%, the metal (nickel and vanadium) is 293.5 mg/kg, the asphaltene content is 8.6%, and the catalyst is a high-nitrogen high-metal difficult-to-process residual oil which is difficult to process by a conventional ebullated bed process route. Table 1 shows the operation of the different examples and comparative examples.
Example 1
Example 1 employs the process flow shown in fig. 1, wherein the first raffinate stream 20 is all returned to the first ebullated-bed reaction zone 2 and the second raffinate stream 21 is all returned to the second ebullated-bed reaction zone 5. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second boiling bed reaction zone adopts FEM-31 catalyst developed by Dalian petrochemical institute; the third separation unit adopts an atmospheric distillation device, wherein the temperature cutting point of the light fraction and the heavy fraction is controlled to be 300 ℃; the solvent in the first extraction zone and the second extraction zone is butane solvent; the temperatures of the first boiling bed reaction zone and the second reaction zone are 425 ℃ and 430 ℃ respectively, the reaction pressure is 17MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.25h -1 . The temperature of the first extraction zone and the second extraction zone are 110 ℃ and 125 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Example 2
Example 1 the process flow shown in fig. 1 was used, essentially the same as example 1, except that the first raffinate stream 20 was returned to the first ebullated-bed reaction zone 2 in part at 10wt% relative to the fresh feed. The second raffinate stream 21 is not returned to the second ebullated-bed reaction zone 5. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second boiling bed reaction zone adopts FEM-31 catalyst developed by Dalian petrochemical institute; the third separation unit adopts an atmospheric distillation device, wherein the temperature cutting point of the light fraction and the heavy fraction is controlled to be 300 ℃; the solvent in the first extraction zone and the second extraction zone is butane solvent; the temperatures of the first boiling bed reaction zone and the second reaction zone are 425 ℃ and 430 ℃ respectively, the reaction pressure is 17MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.25h -1 . The temperature of the first extraction zone and the second extraction zone are 110 ℃ and 125 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Example 3
Example 2 the process flow shown in figure 1 was used essentially the same as example 1 except that the first raffinate stream 20 was not returned to the first ebullated-bed reaction zone 2 and the second raffinate stream 21 was partially returned to the second ebullated-bed reaction zone 5 at 10wt% relative to fresh feed. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second boiling bed reaction zone adopts FEM-31 catalyst developed by Dalian petrochemical institute; the third separation unit adopts an atmospheric distillation device, wherein the temperature cutting point of the light fraction and the heavy fraction is controlled to be 300 ℃; the solvent in the first extraction zone and the second extraction zone is butane solvent; the temperatures of the first boiling bed reaction zone and the second reaction zone are 415 ℃ and 420 ℃ respectively, the reaction pressure is 15MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.18h -1 . The temperature of the first extraction zone and the second extraction zone are respectively 113 ℃ and 130 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Example 4
Example 3 the process flow shown in fig. 1 was used essentially the same as example 1, except that neither the first raffinate stream 20 nor the second raffinate stream 21 was returned to the ebullated-bed reaction zone, but was processed as a feedstock for other subsequent units. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second boiling bed reaction zone adopts FEM-31 catalyst developed by Dalian petrochemical institute; the third separation unit adopts an atmospheric distillation device, wherein the temperature cutting point of the light fraction and the heavy fraction is controlled to be 300 ℃; the solvent in the first extraction zone and the second extraction zone is butane solvent; the temperatures of the first boiling bed reaction zone and the second reaction zone are 420 ℃ and 425 ℃ respectively, the reaction pressure is 17MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.2h -1 . The temperature of the first extraction zone and the second extraction zone are 110 ℃ and 125 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Example 5
Example 2 the process flow shown in FIG. 1 was used, essentially the same as example 1, except that the first raffinate stream 20 was not returned to the first ebullated-bed reaction zone 2, but instead was used as it wasThe raw materials are processed by other subsequent devices. The second raffinate stream 21 was partially returned to the first ebullated-bed reaction zone 2 at 10wt% relative to fresh feed. The temperatures of the first boiling bed reaction zone and the second boiling bed reaction zone are 415 ℃ and 420 ℃ respectively, the reaction pressure is 15MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.18h -1 . The temperatures of the first extraction zone and the second extraction zone are 113 ℃ and 130 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Comparative example 1
Comparative example 1 adopts the process flow shown in fig. 2, as shown in fig. 2, raw oil 1 and hydrogen 10 are mixed and enter a first ebullated bed reaction zone 2, the reacted material flow enters a first separation zone 3 and is separated into a first gas phase material flow 6 and a first liquid phase material flow 4, wherein the first liquid phase material flow 4 is mixed with the hydrogen 10 and enters a second ebullated bed reaction zone, the reaction product enters a second separation zone 7 and is separated to obtain a second gas phase material flow 8 and a second liquid phase material flow 12, the second gas phase material flow 8 and the first gas phase material flow 6 enter a hydrogen recovery unit 9, and the recycled hydrogen 10 and a light hydrocarbon component 11 are obtained after treatment; the second liquid phase stream 12 and the light hydrocarbon component 11 are mixed and enter an atmospheric fractionation unit 13 for separation to obtain a hydrogenated naphtha fraction 14, a hydrogenated diesel fraction 15 and a hydrogenated atmospheric residuum fraction 16, wherein the hydrogenated atmospheric residuum fraction 16 enters a vacuum fractionation unit 17 for separation to obtain a hydrogenated wax oil fraction 18 and a hydrogenated vacuum residuum fraction 19. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second ebullated bed reaction zone employs FEM-31 catalyst developed by Dalian petrochemical institute. The temperatures of the first boiling bed reaction zone and the second reaction zone are 415 ℃ and 420 ℃ respectively, the reaction pressure is 15MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.18h -1 。
Comparative example 2
Comparative example 2 Using the process flow shown in FIG. 3, as shown in FIG. 3, raw oil 1 and hydrogen 10 were mixed and fed into first ebullated bed reaction zone 2, and the reacted stream was fed into first separation zone 3 and separated to obtain first gas phase stream 6 and first liquid phase stream 4, wherein first liquid phase stream 4 was mixed with hydrogen 10 and fed into second ebullated bed reaction zone 5, and the reaction product was fed into second separation zone 7 to obtain second gas phase streamStream 8 and a second liquid phase stream 12, wherein the second gas phase stream 8 and the first gas phase stream 6 enter a hydrogen recovery unit 9 to yield hydrogen 10 and a light hydrocarbon component 11; the second liquid phase stream 12 and the light hydrocarbon component 11 are mixed into an atmospheric fractionation unit 13 to obtain a hydrogenated naphtha fraction 14, a hydrogenated diesel fraction 15 and a hydrogenated atmospheric residuum fraction 16, wherein the hydrogenated atmospheric residuum fraction 16 is fed into a vacuum fractionation unit 17 to obtain a hydrogenated wax oil fraction 18 and a hydrogenated vacuum residuum fraction 19. The hydrogenated vacuum residuum fraction 19 and the extraction solvent are passed into an extraction zone 20 to produce a raffinate stream 21 and an extract stream 22, wherein the extract stream 22 is passed into a solvent recovery unit 23 for separation to produce an oil phase stream 24 and a regenerated solvent 25. The first boiling bed reaction zone adopts FEM-10 catalyst developed by Dalian petrochemical institute; the second boiling bed reaction zone adopts FEM-31 catalyst developed by Dalian petrochemical institute; the temperatures of the first boiling bed reaction zone and the second reaction zone are 415 ℃ and 420 ℃ respectively, the reaction pressure is 15MPa, the hydrogen-oil volume ratio is 500, and the liquid volume space velocity is 0.18h -1 . The temperature of the extraction area is 110 ℃, the extraction pressure is 4.2MPa, and the volume ratio of the catalyst to the oil is 5.0.
Table 1 example reaction results
Note that: the light oil product yield is mainly the liquid phase yield after the first raffinate phase material flow, the hydrogenated vacuum residuum or the raffinate material flow is removed
Table 2 comparative reaction results
Claims (18)
1. A heavy oil processing process comprising the steps of:
(1) The heavy oil raw material enters a first ebullated bed reaction zone, and reacts under the action of hydrogen and a first hydrogenation catalyst, and a reaction product is separated to obtain a first gas phase material flow and a first liquid phase material flow;
(2) The first liquid phase material flow obtained in the step (1) enters a second ebullated bed reaction zone, and reacts under the action of hydrogen and a second hydrogenation catalyst, and a reaction product is separated to obtain a second gas phase material flow and a second liquid phase material flow;
(3) Separating the second liquid phase material flow obtained in the step (2) to obtain a light fraction and a heavy fraction;
(4) The heavy fraction obtained in the step (3) enters a first extraction zone and contacts with an extraction solvent to obtain a first extraction phase material flow and a first raffinate phase material flow;
(5) The first extract phase material flow obtained in the step (4) enters a second extraction zone and contacts with an extraction solvent to obtain a second extract phase material flow and a second raffinate phase material flow;
(6) And (3) feeding the second extract phase material flow obtained in the step (5) into a separation unit, and recovering the extraction solvent to obtain an oil phase material flow.
2. The heavy oil processing process according to claim 1, characterized in that: the heavy oil raw material in the step (1) is selected from one or more of atmospheric residuum, vacuum residuum, oilfield thick oil, heavy fuel oil, oil sand, coal tar, ethylene tar and the like, and one or more of catalytic slurry oil, vacuum wax oil and furfural extract oil are optionally blended.
3. The heavy oil processing process according to claim 1, characterized in that: the operating conditions of the first ebullated-bed reaction zone were: the reaction temperature is 350-450 ℃, preferably 380-430 ℃, the reaction pressure is 10.0-20.0 MPa, preferably 15.0-18.0 MPa, the hydrogen-oil volume ratio is 400-2000, preferably 500-1500, and the liquid hourly space velocity is 0.1-5.0 h -1 Preferably 0.2 to 2.0h -1 。
4. The heavy oil processing process according to claim 1, characterized in that: the operating conditions of the second ebullated-bed reaction zone were: the reaction temperature is 350-450 ℃, preferably 380-430 ℃, the reaction pressure is 10.0-20.0 MPa, preferably 15.0-18.0 MPa, and the hydrogen-oil volume ratio is 400-2000, preferably500-1500, and the liquid hourly space velocity is 0.1-5.0 h -1 Preferably 0.2 to 2.0h -1 。
5. The heavy oil processing process according to claim 1, characterized in that: the cutting point of the light fraction and the heavy fraction is 180-450 ℃, preferably 260-400 ℃.
6. The heavy oil processing process according to claim 1, characterized in that: the extraction solvent used in the first extraction zone is at least one of alkane and naphtha, wherein the alkane is at least one of C3-C7 alkane.
7. The heavy oil processing process according to claim 1, characterized in that: the operating conditions of the first extraction zone were: the temperature is 80-200 ℃, preferably 100-160 ℃, the pressure is 2.0-6.0 MPa, preferably 3.0-5.0 MPa, and the volume ratio of the solvent is 1.0-10.0, preferably 3.0-8.0.
8. The heavy oil processing process according to claim 1, characterized in that: the yield of the first raffinate stream is 20wt% to 70wt%, preferably 30wt% to 55wt%.
9. The heavy oil processing process according to claim 1, characterized in that: the first raffinate stream is returned to the first ebullated bed reaction zone in whole or in part for treatment, and if the first raffinate stream is returned to the first ebullated bed reaction zone in part, the remaining portion of the first raffinate stream is used as a coking feedstock for producing low sulfur petroleum coke or is used as a hydrogen production feedstock.
10. The heavy oil processing process according to claim 1, characterized in that: the first raffinate stream is mixed with the oil-soluble catalyst and returned to the first ebullated bed reaction zone, the oil-soluble catalyst being added in an amount of 0.05wt% to 5wt%, preferably 0.5wt% to 2wt% based on the weight of the first raffinate stream.
11. The heavy oil processing process according to claim 1, characterized in that: the extraction solvent used in the second extraction zone is at least one of alkane and naphtha, wherein the alkane is at least one of C3-C7 alkane.
12. The heavy oil processing process according to claim 1, characterized in that: the operating conditions of the second extraction zone were: the temperature is 80-200 ℃, preferably 120-160 ℃, the pressure is 2.0-6.0 MPa, preferably 3.0-5.0 MPa, and the volume ratio of the solvent is 1.0-10.0, preferably 3.0-8.0.
13. The heavy oil processing process according to claim 1, characterized in that: the yield of the second raffinate stream is from 10wt% to 50wt%, preferably from 10wt% to 30wt%.
14. The heavy oil processing process according to claim 1, characterized in that: the second raffinate stream is returned in whole or in part to the first ebullated-bed reaction zone and/or the second ebullated-bed reaction zone, with the remainder being fed as catalytic cracking, hydrocracking, delayed coking, or as pitch and low sulfur ship-fuel blending components when partially returned.
15. The heavy oil processing process according to claim 1, characterized in that: the separation unit adopts supercritical solvent separation, and the extraction solvent obtained after separation is returned to the first extraction zone and/or the second extraction zone for use.
16. A heavy oil processing system comprising:
the first ebullated bed reaction zone is used for receiving heavy oil raw materials, and reacting under the action of hydrogen and a first hydrogenation catalyst to obtain a reaction product after the reaction;
a first separation unit for receiving the reaction product of the first ebullated-bed reaction zone, after separation, to obtain a first vapor phase stream and a first liquid phase stream;
a second ebullated-bed reaction zone for receiving the first liquid phase stream from the first separation unit and reacting with hydrogen and a second hydrogenation catalyst to obtain a reaction product;
a second separation unit for receiving the reaction product of the second ebullated-bed reaction zone, after separation, to obtain a second vapor phase stream and a second liquid phase stream;
a third separation unit for receiving the second liquid phase stream from the second separation unit, after separation, to obtain a light fraction and a heavy fraction;
a first extraction zone for receiving the heavy fraction from the third separation unit and contacting with an extraction solvent to produce a first extract phase stream and a first raffinate phase stream;
a second extraction zone for receiving the first extract phase stream from the first extraction zone, contacting with an extraction solvent to produce a second extract phase stream and a second raffinate phase stream;
a fourth separation unit for receiving the second extract phase stream from the second extraction zone, and separating to obtain an extraction solvent and an oil phase stream.
17. The heavy oil processing system of claim 16, wherein: the first raffinate stream is returned to the first ebullated bed reaction zone via line.
18. The heavy oil processing system of claim 16, wherein: the second raffinate stream is returned to the first ebullated bed reaction zone and/or the second ebullated bed reaction zone via a line.
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