CN114763491B - Method for improving operation stability of ebullated bed hydrogenation device - Google Patents
Method for improving operation stability of ebullated bed hydrogenation device Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 66
- 238000006243 chemical reaction Methods 0.000 claims abstract description 74
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- 238000004517 catalytic hydrocracking Methods 0.000 claims abstract description 37
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- 239000001257 hydrogen Substances 0.000 claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 34
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- 238000000926 separation method Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 27
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- 239000002994 raw material Substances 0.000 claims abstract description 19
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- 239000012533 medium component Substances 0.000 claims abstract description 12
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- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 10
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- 230000000153 supplemental effect Effects 0.000 claims description 9
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
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- 239000010937 tungsten Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4012—Pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4018—Spatial velocity, e.g. LHSV, WHSV
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for improving the operation stability of a fluidized bed hydrogenation device, which comprises the following steps: firstly, carrying out hydrocracking reaction on an inferior hydrocarbonaceous raw material in a fluidized bed hydrogenation reaction zone, and separating reaction products to obtain a light component, a medium component and a heavy component; the obtained heavy component is treated with a treating agent and subjected to sedimentation separation to obtain a light fraction and a heavy fraction; the obtained heavy fraction enters a complementary hydrogenation reactor, hydrogenation reaction is carried out under the existence of hydrogen and a complementary hydrogenation catalyst, and the heavy fraction after hydrogenation obtained after the hydrogenation reaction is recycled to the ebullated bed hydrogenation reaction zone to be mixed with the inferior hydrocarbon-containing raw material for treatment. The method can greatly improve the stability of the hydrogenation system of the inferior hydrocarbonaceous material and improve the yield of light oil at the same time by adjusting the process flow, and realizes stable, high-efficiency and long-period operation of the device.
Description
Technical Field
The invention belongs to the field of oil refining chemical industry, and particularly relates to a fluidized bed hydrogenation method.
Background
Along with the continuous rapid development of world economy and the continuous enhancement of environmental awareness of people, the demands for clean fuel oil and chemical raw materials are rapidly increased, and most of the world major oil fields at present enter the middle and later stages of development, the proportion of the light crude oil which can be exploited is gradually reduced, and the crude oil bad trend is aggravated. In future refinery production, the proportion of heavy crude oil will be larger and larger, and it is important how to convert the heavy crude oil into light fuel or chemical raw material as much as possible, wherein the key is the lightening of residual oil with a larger specific gravity (40% -60%) in the crude oil. The existing residual oil lightening means comprise decarburization and hydrogenation, the decarburization process comprises coking, visbreaking, solvent deasphalting and the like, the delayed coking technology is mature, the flow is simple, the investment and operation cost is low, the raw material adaptability is strong, the method has certain advantages in the aspect of treating inferior residual oil such as high sulfur, high carbon residue and the like, and the method is an important means for treating the inferior residual oil in a refinery. However, the delayed coking process has obvious disadvantages such as low liquid yield, poor product quality, low added value coke generation and the like, and coking is not an optimal residual oil processing technology from the aspects of reasonable resource utilization and environmental protection. Visbreaking and solvent deasphalting also have problems such as low liquid recovery. The hydrogenation technology is mainly divided into four types of fixed bed, ebullated bed, suspended bed and moving bed heavy oil hydrogenation technology. The total processing capacity of global residuum is about 281 ten thousand barrels per day, accounting for 17% of the processing capacity of global residuum, wherein about 82% is fixed bed hydrotreating, 18% is ebullated bed hydrocracking, and the residuum suspension bed hydrocracking has no industrial application device yet. The residual oil hydrogenation process has high light oil yield, can produce low-sulfur fuel oil or provide raw materials for catalytic cracking and hydrocracking devices, has good economic benefit and is widely applied worldwide. In western developed countries such as united states, japan, germany, etc., the specific gravity of the residuum hydrotreating capacity is greater than 80% of the total residuum processing capacity, while the specific gravity of China is only 36.4%, which is far lower than the developed state level. The hydrogenation capability of China still has a great potential from the growing trend of the residual oil processing capability worldwide, from the reasonable utilization of resources and the clean requirement of products, the deep conversion of the residual oil hydrogenation is a target which is pursued for a long time by the oil refining industry of China, and the ebullated bed residual oil hydrogenation technology is a preferable technology of domestic oil refining technicians from the aspects of liquid recovery and technology maturity.
Disclosure of Invention
At present, in the process of hydro-conversion treatment of inferior hydrocarbonaceous materials by a boiling bed, particularly under the operation condition of high conversion rate (the high conversion rate generally means that the conversion depth is not less than 70 percent, preferably not less than 75 percent), the problems of unstable hydrogenation system, poor tail oil quality and the like exist.
In a first aspect, the present invention provides a method for improving the operational stability of a ebullated bed hydrogenation apparatus, said method comprising the steps of:
(1) Under the contact condition, the inferior hydrocarbonaceous raw material and hydrogen enter a fluidized bed hydrogenation reaction zone, and are subjected to hydrocracking reaction under the action of a fluidized bed hydrogenation catalyst, and a reaction product is separated to obtain a light component, a medium component and a heavy component;
(2) The heavy component obtained in the step (1) is contacted with a treating agent for treatment, a first oil phase material and a second oil phase material are obtained after treatment and separation, wherein the first oil phase material further enters a separation tower for sedimentation separation to obtain a light fraction and a heavy fraction;
(3) The heavy fraction obtained in the step (2) enters a complementary hydrogenation reactor, and hydrogenation reaction is carried out under the existence of hydrogen and a complementary hydrogenation catalyst;
(4) And (3) recycling the heavy fraction after hydrogenation obtained after the hydrogenation reaction in the step (3) to the ebullated bed hydrogenation reaction zone, and mixing with the inferior hydrocarbon-containing raw material for treatment.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, in the step (1), at least one ebullated bed hydrogenation reactor, preferably 1 or 2 ebullated bed hydrogenation reactors are provided, and when more than 2 ebullated bed hydrogenation reactors are provided, the plurality of ebullated bed hydrogenation reactors may be connected in series and/or parallel. The ebullated bed hydrogenation reactor preferably adopts an ebullated bed reactor with a built-in three-phase separator, and particularly can adopt an ebullated bed reactor with a built-in three-phase separator developed by China petrochemical industry Co., ltd.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the ebullated bed hydrogenation catalyst in step (1) may be any ebullated bed hydrogenation catalyst existing in the art, for example, one or more ebullated bed hydrogenation catalysts developed by the company of petrochemical Co., ltd, and specifically, may be a smooth stoneThe trade marks FES-30 and FEM-10 ebullated bed catalysts developed by the oil chemical industry institute can also be used for purchasing TEX2720 catalysts from the market. Typically, the ebullated bed hydrogenation catalyst comprises a support and an active metal, wherein the active metal may be one or more of nickel, cobalt, molybdenum or tungsten; the catalyst composition may comprise, in weight percent: nickel or cobalt is 0.5-10% (calculated by oxide), molybdenum or tungsten is 1-25% (calculated by oxide), and the carrier can be one or more of alumina, silica, alumina-silica or titania. The catalyst is in the shape of extrudate or sphere and has bulk density of 0.5-0.9 g/cm 3 The particle diameter (spherical diameter or bar-shaped diameter) is 0.04-1.0 mm, and the specific surface area is 80-300 m 2 /g。
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the poor hydrocarbon-containing raw material in the step (1) may be one or more of atmospheric residuum, vacuum residuum, oil sand asphalt, and may be one or more of partial wax oil and catalytic diesel oil.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the operation conditions of the ebullated bed hydrogenation reaction zone in step (1) are as follows: the reaction temperature is 380-450 ℃, the reaction pressure is 13-20.0 MPa, and the volume airspeed is 0.2-4.0 h -1 The preferred operating conditions of the hydrogen oil volume ratio of 300-1500 are as follows: the reaction temperature is 400-440 ℃, the reaction pressure is 14-18.0 MPa, and the volume airspeed is 0.3-1.5 h -1 The volume ratio of hydrogen to oil is 600-1000.
In the method for improving the operation stability of the ebullated bed hydrogenation apparatus, the final boiling point temperature of the light component in the step (1) is 160-190 ℃, and the final boiling point temperature of the medium component is 520-560 ℃. The separation of the light component, the medium component and the heavy component in the step (1) generally comprises an atmospheric fractionating tower and a vacuum fractionating tower. Wherein the light component and the fraction with the final distillation point temperature less than 370 ℃ in the middle component are separated in the normal pressure fractionating tower, and the fraction with the initial distillation point more than 370 ℃ in the middle component and the heavy component are respectively obtained at the side line and the bottom of the vacuum fractionating tower.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the light component in step (1) may be used as a naphtha blending component or may be further refined to be used as a product to be discharged from the apparatus.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the treating agent in the step (2) may be one or more of propane, n-butane, isobutane, n-pentane, isopentane, and naphtha, preferably one or more of n-butane, isopentane, and naphtha; further, the volume ratio of n-butane to isopentane is 4:1-1:4, preferably 2:1-1:2.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the treatment conditions in step (2) are as follows: the pressure is 4.0-8.0 MPa, the treatment temperature is 130-170 ℃, the volume ratio of the treating agent to the heavy component is 2:1-10:1, and the preferable treatment conditions are as follows: the pressure is 4.5-6.5 MPa, the treatment temperature is 135-160 ℃, and the volume ratio of the treating agent to the heavy components is 4:1-9:1.
In the method for improving the operation stability of the ebullated bed hydrogenation apparatus, in the step (2), the temperature of the separation column is controlled to be 160-190 ℃, preferably 150-170 ℃, the top of the separation column is used for obtaining light fraction, and the bottom of the separation column is used for obtaining heavy fraction.
Further, in the method for improving the operation stability of the ebullated bed hydrogenation apparatus, the second oil phase material obtained in the step (2) may be used as a material for producing petroleum coke products.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the operation conditions of the supplemental hydrogenation reactor in step (3) are as follows: the reaction temperature is 350-400 ℃, the reaction pressure is 10-15.0 MPa, and the volume airspeed is 0.8-3.0 h -1 Hydrogen oil volume ratio of 200-1000, preferred operation condition: the reaction temperature is 360-380 ℃, the reaction pressure is 11-14.0 MPa, and the volume space velocity is 1.0-2.0 h -1 The volume ratio of the hydrogen oil is 250-400.
In the method for improving the operation stability of the ebullated bed hydrogenation apparatus, the additional hydrogenation catalyst filled in the additional hydrogenation reactor in the step (3) may be one or more of the hydrofining catalysts existing in the art, may be commercially available products, or may be prepared according to the existing method.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the mass ratio of the heavy component after hydrogenation obtained in the step (3) to the poor hydrocarbon feedstock obtained in the step (4) may be generally controlled to be 1:25 to 1:10, preferably 1:20 to 1:12.
In a second aspect, the present invention provides a method for improving the operation stability of an ebullated-bed hydrogenation apparatus according to another embodiment, the method comprising the following steps:
(1) Under the contact condition, the inferior hydrocarbonaceous raw material and hydrogen enter a fluidized bed hydrogenation reaction zone, and are subjected to hydrocracking reaction under the action of a fluidized bed hydrogenation catalyst, and a reaction product is separated to obtain a light component, a medium component and a heavy component;
(2) The heavy component obtained in the step (1) is contacted with a treating agent for treatment, a first oil phase material and a second oil phase material are obtained after treatment and separation, wherein the first oil phase material further enters a separation tower for sedimentation separation to obtain a light fraction and a heavy fraction;
(3) The heavy fraction obtained in the step (2) enters a complementary hydrogenation reactor, and hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst;
(4) Recycling the heavy fraction after hydrogenation obtained after the hydrogenation reaction in the step (3) to the ebullated bed hydrogenation reaction zone, and mixing with the inferior hydrocarbon-containing raw material for treatment;
(5) And (3) feeding the middle component obtained in the step (1) and the light fraction obtained in the step (2) into a hydrocracking reaction zone, and carrying out hydrocracking reaction in the presence of hydrogen and a hydrocracking catalyst to obtain naphtha, aviation kerosene and tail oil after the reaction.
Furthermore, in the method for improving the operation stability of the ebullated bed hydrogenation apparatus, the naphtha obtained in the step (5) may be recycled as a treating agent to the step (2) for treatment with heavy components.
In the method for improving the operation stability of the ebullated bed hydrogenation apparatus, the tail oil obtained in the step (5) may be used as an ethylene cracking raw material, or may be partially or completely mixed with the first oil phase material and then enter the separation tower for treatment in the step (2).
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, at least one hydrocracking reactor is disposed in the hydrocracking reaction zone in step (5), and the hydrocracking reactor may be one or more of a fixed bed reactor, a fluidized bed reactor, an ebullated bed reactor, and a suspended bed reactor. The hydrocracking catalyst in the step (5) can be an existing hydrocracking catalyst in the field, can be commercially available products, can also be prepared according to a method disclosed in the field, for example, can be a multi-product chemical raw material hydrocracking catalyst developed by the China petrochemical Co., ltd, specifically can be an FF-66/FC-46 hydrocracking catalyst and the like.
Further, in the above method for improving the operation stability of the ebullated bed hydrogenation apparatus, the operation conditions of the hydrocracking reaction zone in step (5) are as follows: the reaction temperature is 350-400 ℃, the reaction pressure is 10-12.0 MPa, and the volume space velocity is 0.4-3.0 h -1 The preferred operating conditions of the hydrogen oil volume ratio of 300-1500 are as follows: the reaction temperature is 360-390 ℃, the reaction pressure is 11-13.0 MPa, and the volume airspeed is 0.5-1.5 h -1 The volume ratio of hydrogen to oil is 700-1200.
Compared with the prior art, the method for improving the operation stability of the ebullated bed hydrogenation device has the following technical advantages:
1. in the method for improving the operation stability of the ebullated bed hydrogenation device, the heavy fraction obtained after the ebullated bed hydrogenation reaction is firstly separated, and then the separated heavy fraction is hydrogenated and returned to the ebullated bed hydrogenation reaction zone, so that the applicant finds that the stability of a ebullated bed hydrogenation system can be greatly improved by returning the hydrogenated heavy fraction to the ebullated bed hydrogenation reaction zone in the research process, and the operation stability of the device is improved.
2. In the method for improving the operation stability of the fluidized bed hydrogenation device, the fluidized bed hydrogenation device is operated at a high conversion rate, so that the light oil yield can be greatly improved, the light oil extraction rate is more than 90%, and the main products are mainly naphtha and aviation kerosene high-added-value products.
Drawings
FIG. 1 is a schematic flow chart of a method for improving the operation stability of a ebullated bed hydrogenation apparatus according to the present invention.
Detailed Description
The invention is further described below with reference to the drawings and the detailed description, but does not limit the scope of the invention.
As shown in fig. 1, the present invention provides a method for improving the operation stability of a ebullated bed hydrogenation apparatus, the method comprising the following steps: the inferior hydrocarbonaceous feedstock 1 and hydrogen 2 enter a fluidized bed hydrogenation reaction zone 3, hydrogenation reaction is carried out in the presence of a fluidized bed hydrogenation catalyst, and a reaction effluent further enters a separation unit 4 to be separated to obtain a light component 5, a medium component 6 and a heavy component 7, wherein the light component 5 can be used as naphtha blending component or further refined to be used as naphtha product to be discharged out of the device; the heavy component 7 and the treating agent 8 enter a treating unit 9 to be treated to obtain a first oil phase material 10 and a second oil phase material 11, wherein the second oil phase material 11 can be used as a raw material for producing petroleum coke products, the first oil phase material 10 enters a separating tower 12 to be subjected to sedimentation separation to obtain a light fraction 13 and a heavy fraction 14, the heavy fraction 14 and hydrogen 2 enter a complementary hydrogenation reactor 15 to be subjected to hydrogenation treatment, and the heavy fraction 16 after hydrogenation obtained after the treatment enters a fluidized bed hydrogenation reaction zone to be mixed with a poor-quality hydrocarbon-containing raw material to be treated. The middle component 6, the light fraction 13 and the hydrogen enter a hydrocracking reaction zone 17 for hydrocracking reaction, the reaction effluent is separated by a hydrocracking separation unit 18 to obtain naphtha 19, aviation kerosene 20 and tail oil 21, and the tail oil 21 can be used as an ethylene cracking raw material or can be mixed with the first oil phase material 10 partially or completely to enter a separation tower 12 for treatment (not shown in the figure).
The fluidized bed hydrogenation reaction zone of the invention uses a fluidized bed reactor, in particular to a fluidized bed hydrogenation reactor which can use a built-in three-phase separator developed by China petrochemical industry Co. The fluidized bed hydrogenation catalyst adopts a commercial brand FES-30 microspherical fluidized bed hydrogenation catalyst developed by smooth petrochemical institute. The hydrocracking catalyst adopts the FF-66/FC-46 catalyst developed by the smooth petrochemical institute, the complementary hydrogenation reactor adopts the FF-66 hydrogenation catalyst developed by the smooth petrochemical institute, and the commercial catalyst with moderate aromatic saturation function can be purchased from the market.
The poor hydrocarbon-containing feedstock used in the examples and comparative examples of the present invention was vacuum residuum, and its specific properties are shown in table 1.
Example 1
The process flow described in fig. 1 was used, wherein the operating conditions of the ebullated-bed hydrogenation reactor were: reaction temperature: 430 ℃, 16.0MPa of reaction pressure and 0.4h of volume space velocity -1 Hydrogen oil volume ratio 800; the final distillation point of the light component is controlled to be 165 ℃, and the final distillation point of the medium component is controlled to be 538 ℃; the treating agent is n-butane and isopentane, the volume ratio of n-butane to isopentane is 1:1, the pressure is 5.0MPa, the treating temperature is 145 ℃, the solvent ratio is 5:1, and the operating temperature of the separation tower is 155 ℃. The operating conditions of the supplemental hydrogenation reactor: the reaction temperature is 370 ℃, the reaction pressure is 13.0MPa, and the volume space velocity is 1.5h -1 Hydrogen oil volume ratio 300. The heavy fraction after hydrogenation is recycled to the ebullated bed hydrogenation reactor, and the mass ratio of the heavy fraction after hydrogenation to the vacuum residue is 1:12. The operating conditions of the hydrocracking reactor were: the reaction temperature is 380 ℃, the reaction pressure is 11.5MPa, and the volume space velocity is 0.6h -1 The hydrogen-oil volume ratio is 900, and the cracked tail oil is recycled to the separation tower. The specific test results are shown in Table 2 and Table 3.
Example 2
The process flow described in fig. 1 was used, wherein the operating conditions of the ebullated-bed hydrogenation reactor were: reaction temperature: 425 ℃, 16.0MPa of reaction pressure and 0.4h of volume space velocity -1 Hydrogen oil volume ratio 800; the final distillation point of the light component is controlled to be 170 ℃, and the final distillation point of the medium component is controlled to be 545 ℃; the treating agent is naphtha obtained by a hydrocracking reactor, the pressure is 5.0MPa, the temperature is 145 ℃, the solvent ratio is 5:1, and the operating temperature of a separation tower is 155 ℃; the operating conditions of the supplemental hydrogenation reactor: reaction temperature 370 ℃, reaction pressure 13.0MPa and volume space velocity1.6h -1 Hydrogen oil volume ratio 300; the heavy fraction after hydrogenation is recycled to the ebullated bed hydrogenation reactor, and the mass ratio of the heavy fraction after hydrogenation to the vacuum residue is 1:15. The operating conditions of the hydrocracking reactor were: the reaction temperature is 370 ℃, the reaction pressure is 11.5MPa, and the volume space velocity is 0.6h -1 Hydrogen oil volume ratio 900, tail oil is circulated back to the separation tower. The specific test results are shown in Table 2 and Table 3.
Example 3
The process flow described in fig. 1 was used, wherein the operating conditions of the ebullated-bed hydrogenation reactor were: the reaction temperature is 435 ℃, the reaction pressure is 16.0MPa, and the volume space velocity is 0.4h -1 Hydrogen oil volume ratio 800; the light component end point was controlled at 180℃and the medium component end point was controlled at 550 ℃. The treating agent is naphtha obtained by a hydrocracking reactor, the pressure is 5.0MPa, the temperature is 145 ℃, the solvent ratio is 5:1, and the operating temperature of a separation tower is 165 ℃; the operating conditions of the supplemental hydrogenation reactor: the reaction temperature is 360 ℃, the reaction pressure is 13.0MPa, and the volume space velocity is 1.5h -1 Hydrogen oil volume ratio 300; the heavy fraction after hydrogenation is recycled to the ebullated bed hydrogenation reactor, and the mass ratio of the heavy fraction after hydrogenation to the vacuum residue is 1:15. The operating conditions of the hydrocracking reactor were: the reaction temperature is 380 ℃, the reaction pressure is 11.5MPa, and the volume space velocity is 0.8h -1 The hydrogen oil volume ratio is 900, and the cracked tail oil is directly taken as an ethylene cracking raw material. The specific test results are shown in Table 2 and Table 3.
Comparative example 1
Substantially the same as in example 1, except that the separation column and the supplemental hydrogenation reactor were not provided, the whole of the first oil phase obtained after the treatment was fed into the hydrocracking reaction zone. The specific test results are shown in Table 2 and Table 3.
Comparative example 2
Substantially the same as in example 1, except that no supplemental hydrogenation reactor was provided, the heavy fraction was returned directly to the ebullated bed hydrogenation reactor without being hydrogenated. The specific test results are shown in Table 2 and Table 3.
TABLE 1 feedstock vacuum residuum Properties
| Project | Vacuum residuum |
| Density/g.cm -3 | 1.023 |
| Carbon residue, wt% | 23.27 |
| C，wt% | 84.79 |
| H，wt% | 11.09 |
| S，wt% | 4.11 |
| N，wt% | 0.39 |
| Ni/μg·g -1 | 40.29 |
| V/μg·g -1 | 52.82 |
| Saturated fraction, wt% | 10.71 |
| Fragrance fraction, wt% | 52.04 |
| Colloid, wt% | 28.28 |
| Asphaltenes, wt% | 8.97 |
TABLE 2 reaction results
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Toluene insoluble matter content at bottom of atmospheric fractionating tower, wt% | 0.12 | 0.19 | 0.21 | 0.45 | 0.35 |
| Switching period and month of |
16 | 12 | 10 | 6 | 8 |
TABLE 3 Properties of the product
Note that: density of 20 DEG C
As can be seen from the above examples and comparative examples, the ebullated bed hydrogenation method of the present invention improves the stability of the hydrogenation system, reduces the toluene insoluble matter content in the produced oil, improves the light oil yield and improves the product quality.
Claims (18)
1. A method for improving the operational stability of a ebullated bed hydrogenation apparatus, said method comprising the steps of:
(1) Under the contact condition, the inferior hydrocarbonaceous raw material and hydrogen enter a fluidized bed hydrogenation reaction zone, and are subjected to hydrocracking reaction under the action of a fluidized bed hydrogenation catalyst, and a reaction product is separated to obtain a light component, a medium component and a heavy component; the operating conditions of the ebullated bed hydrogenation reaction zone are as follows: the reaction temperature is 380-450 ℃, the reaction pressure is 13-20.0 MPa, and the volume airspeed is 0.2-4.0 h -1 Hydrogen oil volume ratio is 300-1500;
(2) The heavy component obtained in the step (1) is contacted with a treating agent for treatment, a first oil phase material and a second oil phase material are obtained after treatment and separation, wherein the first oil phase material enters a separation tower for sedimentation separation to obtain a light fraction and a heavy fraction; the treating agent is one or more of propane, n-butane, isobutane, n-pentane, isopentane and naphtha; the treatment conditions were as follows: the pressure is 4.0-8.0 MPa, the treatment temperature is 130-170 ℃, and the volume ratio of the treating agent to the heavy component is 2:1-10:1; the temperature of the separation tower is controlled to be 150-170 ℃;
(3) The heavy fraction obtained in the step (2) enters a complementary hydrogenation reactor, and hydrogenation reaction is carried out under the existence of hydrogen and a complementary hydrogenation catalyst; supplemental hydrogenation reactor operationThe conditions are as follows: the reaction temperature is 350-400 ℃, the reaction pressure is 10-15.0 MPa, and the volume airspeed is 0.8-3.0 h -1 The volume ratio of hydrogen to oil is 200-1000;
(4) And (3) recycling the heavy fraction after hydrogenation obtained after the hydrogenation reaction in the step (3) to the ebullated bed hydrogenation reaction zone, and mixing with the inferior hydrocarbon-containing raw material for treatment.
2. A method for improving the operational stability of a ebullated bed hydrogenation apparatus, said method comprising the steps of:
(1) Under the contact condition, the inferior hydrocarbonaceous raw material and hydrogen enter a fluidized bed hydrogenation reaction zone, and are subjected to hydrocracking reaction under the action of a fluidized bed hydrogenation catalyst, and a reaction product is separated to obtain a light component, a medium component and a heavy component; the operating conditions of the ebullated bed hydrogenation reaction zone are as follows: the reaction temperature is 380-450 ℃, the reaction pressure is 13-20.0 MPa, and the volume airspeed is 0.2-4.0 h -1 Hydrogen oil volume ratio is 300-1500;
(2) The heavy component obtained in the step (1) is contacted with a treating agent for treatment, a first oil phase material and a second oil phase material are obtained after treatment and separation, wherein the first oil phase material enters a separation tower for sedimentation separation to obtain a light fraction and a heavy fraction; the treating agent is one or more of propane, n-butane, isobutane, n-pentane, isopentane and naphtha; the treatment conditions were as follows: the pressure is 4.0-8.0 MPa, the treatment temperature is 130-170 ℃, and the volume ratio of the treating agent to the heavy component is 2:1-10:1; the temperature of the separation tower is controlled to be 150-170 ℃;
(3) The heavy fraction obtained in the step (2) enters a complementary hydrogenation reactor, and hydrogenation reaction is carried out in the presence of hydrogen and a hydrogenation catalyst; the supplemental hydrogenation reactor operating conditions were as follows: the reaction temperature is 350-400 ℃, the reaction pressure is 10-15.0 MPa, and the volume airspeed is 0.8-3.0 h -1 The volume ratio of hydrogen to oil is 200-1000;
(4) Recycling the heavy fraction after hydrogenation obtained after the hydrogenation reaction in the step (3) to the ebullated bed hydrogenation reaction zone, and mixing with the inferior hydrocarbon-containing raw material for treatment;
(5) And (3) feeding the middle component obtained in the step (1) and the light fraction obtained in the step (2) into a hydrocracking reaction zone, and carrying out hydrocracking reaction in the presence of hydrogen and a hydrocracking catalyst to obtain naphtha, aviation kerosene and tail oil after the reaction.
3. The method for improving the operation stability of an ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein said poor hydrocarbon-containing material in step (1) is one or more of an atmospheric residue, a vacuum residue, and an oil sand pitch.
4. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 3, wherein said poor hydrocarbon-containing material in step (1) is blended with one or both of wax oil and catalytic diesel oil.
5. The method for improving the operational stability of a ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the operating conditions of the ebullated bed hydrogenation reaction zone in step (1) are as follows: the reaction temperature is 400-440 ℃, the reaction pressure is 14-18.0 MPa, and the volume airspeed is 0.3-1.5 h -1 The volume ratio of hydrogen to oil is 600-1000.
6. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the treating agent in the step (2) is one or more of n-butane, isopentane, and naphtha.
7. The method for improving the operational stability of a ebullated bed hydrogenation apparatus according to claim 6, wherein the volume ratio of n-butane to isopentane is from 4:1 to 1:4.
8. The method for improving the operational stability of a ebullated bed hydrogenation apparatus according to claim 6, wherein the volume ratio of n-butane to isopentane is from 2:1 to 1:2.
9. The method for improving the operational stability of an ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the process conditions in step (2) are as follows: the pressure is 4.5-6.5 MPa, the treatment temperature is 135-160 ℃, and the volume ratio of the treating agent to the heavy components is 4:1-9:1.
10. The method for improving the operational stability of an ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the supplemental hydrogenation reactor operating conditions in step (3) are as follows: the reaction temperature is 360-380 ℃, the reaction pressure is 11-14.0 MPa, and the volume space velocity is 1.0-2.0 h -1 The volume ratio of the hydrogen oil is 250-400.
11. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the light component in step (1) has a final boiling point temperature of 160 to 190℃and the medium component has a final boiling point temperature of 520 to 560 ℃.
12. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the mass ratio of the heavy fraction after hydrogenation to the poor hydrocarbon-containing material in the step (4) is 1:25 to 1:10.
13. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 1 or 2, wherein the mass ratio of the heavy fraction after hydrogenation to the poor hydrocarbon-containing material in the step (4) is 1:20 to 1:12.
14. The process for improving the operational stability of an ebullated bed hydrogenation apparatus according to claim 2, wherein the naphtha obtained in step (5) is recycled as a treating agent to the treatment with the heavy component in step (2).
15. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 2, wherein part or all of the tail oil obtained in step (5) is mixed with the first oil phase material and introduced into said separation column in step (2) for treatment.
16. The method for improving the operation stability of a ebullated bed hydrogenation apparatus according to claim 2, wherein said hydrocracking reaction zone in step (5) is provided with at least one hydrocracking reactor, and said hydrocracking reactor is one or more of a fixed bed reactor, a fluidized bed reactor, a ebullated bed reactor, and a suspended bed reactor.
17. The process for increasing the operational stability of an ebullated bed hydrogenation apparatus according to claim 2, wherein the operating conditions of the hydrocracking reaction zone in step (5) are as follows: the reaction temperature is 350-400 ℃, the reaction pressure is 10-12.0 MPa, and the volume space velocity is 0.4-3.0 h -1 Hydrogen oil volume ratio is 300-1500.
18. The process for increasing the operational stability of an ebullated bed hydrogenation apparatus according to claim 2 or 17, wherein the operating conditions of the hydrocracking reaction zone in step (5) are as follows: the reaction temperature is 360-390 ℃, the reaction pressure is 11-13.0 MPa, and the volume airspeed is 0.5-1.5 h -1 The volume ratio of hydrogen to oil is 700-1200.
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| CN102041084A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Heavy hydrocarbon hydrogenation combined process |
| CN103102944A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Combined process of hydrotreatment and light fraction-conversion for residual oil |
| CN103102982A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Combined process for conversion of residual oil |
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| CN102041084A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Heavy hydrocarbon hydrogenation combined process |
| CN103102944A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Combined process of hydrotreatment and light fraction-conversion for residual oil |
| CN103102982A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Combined process for conversion of residual oil |
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