Method for preparing raw material for producing bright stock

Abstract

The invention provides a method for preparing a raw material for producing bright stock, which comprises the following steps: (1) feeding a residual oil raw material into a first fluidized bed hydrogenation reaction zone, and separating a reaction product to obtain a first liquid phase material flow; (2) the first liquid-phase material flow obtained in the step (1) enters a second fluidized bed hydrogenation reaction zone, and a reaction product is separated to obtain a second liquid-phase material flow; separating the second liquid-phase material flow to obtain hydrogenated heavy oil; (3) the hydrogenated heavy oil obtained in the step (2) enters a first extraction zone to be in contact with a solvent to obtain a first extraction phase and a first raffinate phase, and the first extraction phase enters a solvent recovery unit to obtain a bright oil material; and (4) feeding the first raffinate phase obtained in the step (3) into a second extraction zone, contacting with naphtha to obtain a second extraction phase and a second raffinate phase, and circulating the second extraction phase to the first separation zone and / or the second fluidized bed hydrogenation reaction zone. According to the method, the raw material source of the bright stock can be widened, and meanwhile the yield and quality of the bright stock are improved.

Description

Technical Field

[0001] This invention belongs to the field of petrochemical technology, and in particular relates to a method for preparing raw materials for the production of bright oil. Background Technology

[0002] In recent years, with the rapid growth of my country's construction machinery, power, automobile, steel, and shipbuilding industries, the demand for lubricating oil has been increasing. Among them, 150BS bright oil, as a high-end product in the heavy-duty lubricating oil series, is a basic raw material for the production of high-grade engine oil, high-quality air compressor oil, ball mill oil, marine oil, and synthetic heat transfer oil, and is widely used in many industries and fields.

[0003] The production process of bright oil mainly includes the traditional "three-step" production route (solvent refining, solvent dewaxing, and clay supplementary refining) and hydrotreating. However, the high viscosity index lubricating oil fractions used to produce high-end products such as aviation lubricants, rolling mill oils, and superheated cylinder oils are mainly found in vacuum residue. Vacuum residue contains a large amount of gums, asphaltenes, and heteroatom-containing compounds, making it difficult to obtain bright oil products directly using the traditional "three-step" or hydrotreating processes.

[0004] Currently, solvent deasphalting is mainly used to pretreat vacuum residue to remove gums, asphaltenes, and heteroatom-containing compounds. The deasphalted oil is then used as feedstock for producing bright oil. CN108473889A provides a method for forming lubricant base oils from feedstocks, such as vacuum residue or other feedstocks at 510°C+. The feedstock can be deasphalted, followed by catalytic and / or solvent processing to form lubricant base oils, including bright oils. This catalytic processing can be equivalent to processing in at least two stages. The conversion rates achieved in each stage can be varied to produce bright oils with various properties. However, this patented method has poor adaptability to feedstocks and is difficult to use directly from low-quality vacuum residue as feedstock to produce bright oil products. Summary of the Invention

[0005] In view of the shortcomings of the prior art, the main objective of this invention is to provide a method for preparing raw materials for the production of bright oil. The method can transform inferior residual oil into high-quality raw materials for the production of bright oil, thereby broadening the sources of raw materials for bright oil and improving the yield and quality of bright oil.

[0006] This invention provides a method for preparing raw materials for producing gloss oil, comprising the following steps:

[0007] (1) The residue oil feedstock enters the first fluidized bed hydrogenation reaction zone and reacts under the action of hydrogen and the first hydrogenation catalyst. The reaction products are separated by the first separation zone to obtain the first gas phase feed stream and the first liquid phase feed stream.

[0008] (2) The first liquid phase feed stream obtained in step (1) enters the second fluidized bed hydrogenation reaction zone and reacts under the action of hydrogen and the second hydrogenation catalyst. The reaction products are separated in the second separation zone to obtain the second gas phase feed stream and the second liquid phase feed stream. The second liquid phase feed stream is separated in the third separation zone to obtain naphtha, diesel, wax oil and hydrogenated heavy oil.

[0009] (3) The hydrotreated heavy oil obtained in step (2) enters the first extraction zone and, after contacting the solvent, obtains the first extract phase and the first raffinate phase. The first extract phase enters the solvent recovery unit to obtain bright oil and regenerated solvent.

[0010] (4) The first raffinate obtained in step (3) enters the second extraction zone and comes into contact with naphtha to obtain the second extract phase and the second raffinate phase. The second extract phase is recycled to the first separation zone and / or the second fluidized bed hydrogenation reaction zone, preferably to the first separation zone.

[0011] Furthermore, in the above method for preparing raw materials for producing bright oil, the properties of the residual oil raw material in step (1) are as follows: sulfur content 4.5wt%~6.0wt%, residual carbon 20wt%~26wt%, viscosity (150℃) 100mPa·s~200mPa·s.

[0012] Furthermore, in the above method for preparing raw materials for producing bright oil, in step (1), at least one fluidized bed reactor is set in the first fluidized bed hydrogenation reaction zone. The fluidized bed reactor can be at least one of the fluidized bed reactors in the prior art, preferably the STRONG fluidized bed reactor with built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd.

[0013] Furthermore, in the above method for preparing raw materials for producing bright oil, the first hydrogenation catalyst in step (1) is a catalyst with hydrocracking function, which is beneficial to the conversion of macromolecules in residue oil. The first hydrogenation catalyst can be prepared using a commercial catalyst or according to a preparation method disclosed in the prior art, such as using the fluidized bed hydrogenation catalyst with the commercial brand name FEM-10 developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. Generally, the first hydrogenation catalyst contains a support and an active metal component, wherein the support can be one or more of alumina, silica, alumina-silica, and titanium dioxide, and the active metal is a Group VIB and / or Group VIII metal, specifically one or more of nickel, cobalt, molybdenum, and tungsten.

[0014] Furthermore, in the above method for preparing raw materials for producing bright oil, the operating conditions of the first fluidized bed hydrogenation reaction zone in step (1) are as follows: reaction temperature is 350–450°C, preferably 380–430°C; reaction pressure is 10.0–25.0 MPa, preferably 15.0–19.0 ​​MPa; hydrogen-to-oil volume ratio is 300–1000, preferably 400–700; and liquid hourly space velocity is 0.1–2.0 h⁻¹. -1 Preferably, it is 0.2 to 1.0 h. -1 .

[0015] Furthermore, in the above method for preparing raw materials for producing bright oil, in step (2), at least one fluidized bed reactor is set in the second fluidized bed hydrogenation reaction zone, preferably one fluidized bed reactor; the fluidized bed reactor can be at least one of the fluidized bed reactors in the prior art, preferably the STRONG fluidized bed reactor with built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd.

[0016] Furthermore, in the above method for preparing raw materials for producing bright oil, the second hydrogenation catalyst in step (2) is a hydrogenation refining catalyst with hydrogenation and impurity removal function, which is beneficial for impurity removal and directional saturation of aromatics. The second hydrogenation catalyst can be prepared using a commercial catalyst or according to a preparation method disclosed in the prior art, such as using the fluidized bed hydrogenation catalyst with the commercial brand name FES-31 developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. Generally, the second hydrogenation catalyst contains a support and an active metal component, wherein the support can be one or more of alumina, silica, alumina-silica, and titanium dioxide, and the active metal is a Group VIB and / or Group VIII metal, specifically one or more of nickel, cobalt, molybdenum, and tungsten.

[0017] Furthermore, in the above method for preparing raw materials for producing bright oil, the operating conditions of the second fluidized bed hydrogenation reaction zone in step (2) are as follows: reaction temperature is 350–450°C, preferably 380–430°C; reaction pressure is 10.0–25.0 MPa, preferably 15.0–19.0 ​​MPa; hydrogen-to-oil volume ratio is 300–1000, preferably 400–700; and liquid hourly space velocity is 0.1–2.0 h⁻¹. -1 Preferably, it is 0.2 to 1.0 h. -1 .

[0018] Furthermore, in the above method for preparing raw materials for producing bright oil, the cutting point of naphtha and diesel in step (2) is 140-210°C, preferably 160-200°C; the cutting point of diesel and wax oil is 300-380°C, preferably 310-360°C; and the cutting point of wax oil and hydrotreated heavy oil is 450-570°C, preferably 470-540°C.

[0019] Furthermore, in the above method for preparing raw materials for producing bright oil, the solvent used in the first extraction zone in step (3) is at least one of C3 to C7 alkanes, preferably a C3 alkane.

[0020] Furthermore, in the above method for preparing raw materials for producing bright oil, at least one extraction tower is set in the first extraction zone in step (3). The extraction tower can be any of the existing technologies. Specifically, in this invention, a rotating disc tower and / or a packed tower can be used, preferably a packed tower. The packing material used in the packed tower can generally be selected from one or more of grids, Raschig rings, and Pall rings, preferably a grid.

[0021] Furthermore, in the above method for preparing raw materials for producing bright oil, the bright oil obtained in step (3) can be produced into bright oil products through a process of "furfural extraction-ketone benzene dewaxing-clay refining" or a process of "hydrogenation treatment-hydrogenation dewaxing-hydrogenation supplementary refining".

[0022] Furthermore, in the above method for preparing raw materials for producing bright oil, the operating conditions of the first extraction zone in step (3) are: temperature of 50-200℃, preferably 50-140℃, pressure of 2.0-6.0MPa, preferably 3.0-5.0MPa, and agent-to-oil mass ratio of 1.0-10.0, preferably 1.0-3.0.

[0023] Furthermore, in the above method for preparing raw materials for producing bright oil, the naphtha used in the second extraction zone in step (4) can be straight-run naphtha or naphtha from a secondary processing unit, such as naphtha from a wax oil hydrocracking unit, naphtha from a coal tar hydrocracking unit, or naphtha from a gasoline and diesel hydrocracking unit, or one or more of these; preferably, the naphtha used in the second extraction zone is the naphtha obtained in step (2).

[0024] Furthermore, in the above method for preparing raw materials for producing bright oil, the second extraction zone in step (4) can be any kind of extraction tower in the prior art, or a centrifugal extraction device, to achieve the separation of the extract phase and the raffinate phase by the difference in specific gravity.

[0025] Furthermore, in the above method for preparing raw materials for producing bright oil, the second raffinate phase in the second extraction zone in step (4) can be externally ejected from the device and can be used as a raw material for POX hydrogen production and / or coking.

[0026] Furthermore, in the above method for preparing raw materials for producing bright oil, the operating conditions of the second extraction zone in step (4) are: temperature of 50-200℃, preferably 80-150℃, pressure of 0.1-3.0MPa, preferably 1.0-2.0MPa, and agent-to-oil mass ratio of 0.4-1.5, preferably 0.5-1.0.

[0027] Furthermore, in the above method for preparing raw materials for producing bright oil, the first gaseous stream in step (1) and the second gaseous stream in step (2) enter the hydrogen recovery unit for processing, and after processing, recycled hydrogen and light hydrocarbons are obtained. The recycled hydrogen can be recycled back to the first fluidized bed reaction zone and / or the second fluidized bed reaction zone for use. The hydrogen recovery unit can be any of the existing hydrogen recovery devices in the art, and those skilled in the art can select one according to the actual situation. A hydrogen recovery device generally includes a hot high-pressure separator, a cold high-pressure separator, a hydrocarbon recovery unit, a recycled hydrogen desulfurization unit, and a membrane separation unit.

[0028] Furthermore, in the above method for preparing raw materials for producing bright oil, the equipment used in the first separation zone and the second separation zone in steps (1) and (2) is a high-temperature high-pressure separator, which can be a well-known hot high-pressure separator (hot high-pressure separator) in the art, preferably a vertical hot high-pressure separator; the equipment used in the third separation zone in step (2) is at least one of an atmospheric distillation tower and a vacuum distillation tower.

[0029] Compared with the prior art, the method for preparing raw materials for producing gloss oil provided by the present invention has the following advantages:

[0030] 1. In the method for preparing raw materials for producing bright oil in this invention, fluidized bed hydrogenation and solvent deasphalting technology are coupled, which can directly use inferior residue oil as raw material to obtain high-quality raw materials for producing bright oil, thus broadening the source of raw materials for bright oil and improving the yield of bright oil.

[0031] 2. In the method for preparing raw materials for producing bright oil according to the present invention, naphtha is used, preferably naphtha produced from the fluidized bed hydrogenation reaction zone to extract the first raffinate phase. The resulting second extract phase is recycled to the first separation zone and / or the second fluidized bed hydrogenation reaction zone, which can convert the potential bright oil components (saturated components, aromatic components, and some gum components) into bright oil components under the action of the catalyst in the second fluidized bed hydrogenation reaction zone. Through further deep hydrogenation, the content of unsaturated olefins and aromatics is further reduced, thereby improving its oxidation stability and viscosity index. Furthermore, the inventors found in their research that heavy components in bright oil are easily converted to heavy naphtha. If not properly controlled, the heavy components in bright oil will be converted into heavy naphtha. Based on the above findings, it is proposed to introduce the second extract phase into the second fluidized bed hydrogenation reaction zone. This increases the concentration of heavy naphtha in the reaction system of the second fluidized bed hydrogenation reaction zone, which can inhibit the conversion of bright oil to heavy naphtha, thereby improving the bright oil yield. In particular, the operation mode of circulating the second extraction phase to the first separation zone can separate the light naphtha fraction contained therein, increase the proportion of heavy naphtha in the material, thereby further inhibiting the conversion of bright oil to heavy naphtha and improving the yield of bright oil. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of a process flow diagram for preparing raw materials for producing gloss oil according to the present invention;

[0033] The components are as follows: 1-Residue feedstock; 2-First fluidized bed hydrogenation reaction zone; 3-First separation zone; 4-First liquid phase feed stream; 5-Second fluidized bed hydrogenation reaction zone; 6-First gas phase feed stream; 7-Second separation zone; 8-Second gas phase feed stream; 9-Hydrogen recovery unit; 10-Recycled hydrogen; 11-Liquid phase obtained from hydrogen recovery unit; 12-Second liquid phase feed stream; 13-Third separation zone; 14-Naphtha; 15-Diesel; 16-Wax oil; 17-Hydrogenated heavy oil; 18-First extraction zone; 19-First extract phase; 20-First raffinate phase; 21-Solvent recovery unit; 22-Regenerated solvent; 23-Bright oil; 24-Second extraction zone; 25-Second extract phase; 26-Second raffinate phase; 27-New hydrogen; 28-Fresh solvent. Detailed Implementation

[0034] The technical features of the present invention are further described below with reference to specific embodiments and accompanying drawings, but these embodiments are not intended to limit the present invention.

[0035] like Figure 1As shown, hydrogen obtained by mixing residual oil feedstock 1 with recycled hydrogen 10 and fresh hydrogen 27 enters the first fluidized bed hydrogenation reaction zone 2. After the reaction, the stream enters the first separation zone 3 and is separated to obtain a first gaseous stream 6 and a first liquid stream 4. The first liquid stream 4 is mixed with hydrogen and then enters the second fluidized bed hydrogenation reaction zone 5. The reaction products enter the second separation zone 7 and are separated to obtain a second gaseous stream 8 and a second liquid stream 12. The second gaseous stream 8 and the first gaseous stream 6 enter the hydrogen recovery unit 9, where they are processed to obtain recycled hydrogen 10. The second liquid stream 12 and the hydrogen recovery unit... The obtained liquid phase 11 is mixed and enters the third separation zone 13 for separation to obtain naphtha 14, diesel oil 15, wax oil 16 and hydrotreated heavy oil 17; the hydrotreated heavy oil 17, regenerated solvent 22 and fresh solvent 28 are mixed and enter the first extraction zone 18 to obtain the first extract phase 19 and the first raffinate phase 20. The first extract phase 19 enters the solvent recovery unit 21 to obtain the regenerated solvent 22 and bright oil 23; the first raffinate phase 20 and naphtha 14 are mixed and enter the second extraction zone 24 to obtain the second raffinate phase 26 and the second extract phase 25, wherein the second extract phase 25 is returned to the first separation zone 3.

[0036] In the embodiments and comparative examples of this invention, the oxidation stability of the lubricating oil was determined by the rotating bomb oxidation method, standard: SH / T 0193-2008.

[0037] The residue feedstock used in the embodiments and comparative examples of this invention is vacuum residue, the properties of which are shown in Table 1.

[0038] Table 1 Properties of Residue Oil Feedstock

[0039] project Residue oil feedstock <![CDATA[Density (20 °C), g / cm 3 > 1.018 Viscosity (150℃), mPa·s 160 Residual carbon, wt% 21.3 Sulfur content, wt% 5.0 Nitrogen content, wt% 0.35 Metal (Ni), mg / kg 67 Metal (V), mg / kg 132 C7 asphalt, wt% 10.2

[0040] Example 1

[0041] Example 1 uses Figure 1 The process flow shown is as follows.

[0042] The first fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The first hydrogenation catalyst is the FEM-10 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 410℃, reaction pressure 18.5MPa, hydrogen-to-oil volume ratio 400, and liquid hourly space velocity 0.28h⁻¹. -1 ;

[0043] The second fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The second hydrogenation catalyst is the FES-31 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 415℃, reaction pressure 17.5MPa, hydrogen-to-oil volume ratio 400, and liquid hourly space velocity 0.28h⁻¹. -1 ;

[0044] In the third separation zone, the cutting point for the distillation range of naphtha and diesel is 160℃, the cutting point for the distillation range of diesel and wax oil is 320℃, and the cutting point for the distillation range of wax oil and hydrotreated heavy oil is 480℃.

[0045] The first extraction zone uses a packed tower filled with corrugated plate structured packing; propane is selected as the solvent; the operating conditions are as follows: extraction temperature is 65℃, extraction pressure is 4.3MPa, and solvent-to-oil mass ratio is 1.5.

[0046] The second extraction zone uses a rotating disc extraction tower; the solvent is naphtha obtained in the third separation zone; the operating conditions are as follows: extraction temperature 110℃, extraction pressure 1.0MPa, and solvent-to-oil mass ratio 0.7.

[0047] The production of bright oil adopts the process of "furfural extraction - ketone-benzene dewaxing - clay refining", as detailed below:

[0048] Furfural extraction unit: Furfural solvent is selected, the top temperature of the extraction column is 120℃, the bottom temperature is 90℃, the solvent-to-oil volume ratio is 5, and the pressure is 0.5MPa.

[0049] Ketone-benzene dewaxing unit: The solvent used is a mixed solvent of methyl ethyl ketone (MEK) and toluene, with 60% toluene and the remainder being MEK; the temperature is -35℃, the pressure is 0.5MPa, and the solvent-to-oil volume ratio is 4.0.

[0050] White clay refining unit: White clay usage is 20wt%, refining temperature is 150℃, and refining time is 1h.

[0051] Example 2

[0052] Example 2 adopts Figure 1 The process flow shown is as follows.

[0053] The first fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The first hydrogenation catalyst is the FEM-10 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 424℃, reaction pressure 18.5MPa, hydrogen-to-oil volume ratio 500, and liquid hourly space velocity 0.32h⁻¹. -1 ;

[0054] The second fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The second hydrogenation catalyst is the FES-31 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 426℃, reaction pressure 17.5MPa, hydrogen-to-oil volume ratio 500, and liquid hourly space velocity 0.32h⁻¹. -1 ;

[0055] In the third separation zone, the cutting point for the distillation range of naphtha and diesel is 180℃, the cutting point for the distillation range of diesel and wax oil is 350℃, and the cutting point for the distillation range of wax oil and hydrotreated heavy oil is 500℃.

[0056] The first extraction zone uses a packed tower filled with corrugated plate structured packing; propane is selected as the solvent; the operating conditions are as follows: extraction temperature is 70℃, extraction pressure is 4.3MPa, and solvent-to-oil mass ratio is 2.0.

[0057] The second extraction zone uses a rotating disc extraction tower; the solvent is naphtha obtained in the third separation zone; the operating conditions are as follows: extraction temperature 130℃, extraction pressure 1.5MPa, and solvent-to-oil mass ratio 0.7.

[0058] The production of bright oil adopts the process of "furfural extraction - ketone-benzene dewaxing - clay refining", as detailed below:

[0059] Furfural extraction unit: Furfural solvent is selected, the top temperature of the extraction column is 120℃, the bottom temperature is 90℃, the solvent-to-oil volume ratio is 5, and the pressure is 0.5MPa.

[0060] Ketone-benzene dewaxing unit: The solvent used is a mixed solvent of methyl ethyl ketone (MEK) and toluene, with 60% toluene and the remainder being MEK; the temperature is -35℃, the pressure is 0.5MPa, and the solvent-to-oil volume ratio is 4.0.

[0061] White clay refining unit: White clay usage is 20wt%, refining temperature is 150℃, and refining time is 1h.

[0062] Example 3

[0063] Example 3 uses Figure 1 The process flow shown is as follows.

[0064] The first fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The first hydrogenation catalyst is the FEM-10 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 428℃, reaction pressure 16.5MPa, hydrogen-to-oil volume ratio 500, and liquid hourly space velocity 0.36h⁻¹. -1 ;

[0065] The second fluidized bed hydrogenation reaction zone is equipped with one fluidized bed hydrogenation reactor, which is the STRONG fluidized bed reactor with a built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The second hydrogenation catalyst is the FES-31 catalyst developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd. The operating conditions are as follows: reaction temperature 429℃, reaction pressure 15.5MPa, hydrogen-to-oil volume ratio 500, and liquid hourly space velocity 0.36h⁻¹. -1 ;

[0066] In the third separation zone, the cutting point for the distillation range of naphtha and diesel is 200℃, the cutting point for the distillation range of diesel and wax oil is 360℃, and the cutting point for the distillation range of wax oil and hydrotreated heavy oil is 535℃.

[0067] The first extraction zone uses a packed tower filled with corrugated plate structured packing; the solvent is a mixture of propane and n-butane (mass ratio 50% / 50%); the operating conditions are as follows: extraction temperature is 100℃, extraction pressure is 4.1MPa, and solvent-to-oil mass ratio is 2.0.

[0068] The second extraction zone uses a rotating disc extraction tower; the solvent is naphtha obtained in the third separation zone; the operating conditions are as follows: extraction temperature 150℃, extraction pressure 2.0MPa, and solvent-to-oil mass ratio 0.8.

[0069] The production of bright oil adopts the process of "furfural extraction - ketone-benzene dewaxing - clay refining", as detailed below:

[0070] Furfural extraction unit: Furfural solvent is selected, the top temperature of the extraction column is 120℃, the bottom temperature is 90℃, the solvent-to-oil volume ratio is 5, and the pressure is 0.5MPa.

[0071] Ketone-benzene dewaxing unit: The solvent used is a mixed solvent of methyl ethyl ketone (MEK) and toluene, with 60% toluene and the remainder being MEK; the temperature is -35℃, the pressure is 0.5MPa, and the solvent-to-oil volume ratio is 4.0.

[0072] White clay refining unit: White clay usage is 20wt%, refining temperature is 150℃, and refining time is 1h.

[0073] Example 4

[0074] The difference from Example 1 is that the second extract phase is not circulated to the first separation zone, but is circulated to the fluidized bed hydrogenation reactor set up in the second fluidized bed hydrogenation reaction zone. The rest is the same as in Example 1.

[0075] Example 5

[0076] The difference from Example 1 is that the naphtha used in the second extraction zone is straight-run naphtha, and the mass fractions of C5 and C6 components in the naphtha are 63% and 35%, respectively.

[0077] Comparative Example 1

[0078] The difference from Example 1 is that there is no second extraction zone in Comparative Example 1.

[0079] Comparative Example 2

[0080] The difference compared to Example 1 is that the second extract phase is recycled to the first fluidized bed hydrogenation reaction zone.

[0081] Comparative Example 3

[0082] The difference from Example 1 is that in the second extraction zone, the solvent used is n-heptane instead of naphtha.

[0083] The test results of Examples 1-5 and Comparative Examples 1-3 are shown in Table 2.

[0084] Table 2 Comparison of properties of gloss oils

[0085]

[0086]

Claims

1. A method for preparing raw materials for the production of bright varnishes, characterized in that: Includes the following steps: (1) The residue feedstock enters the first fluidized bed hydrogenation reaction zone and reacts under the action of hydrogen and the first hydrogenation catalyst. The reaction products are separated in the first separation zone to obtain the first gas phase feed stream and the first liquid phase feed stream. (2) The first liquid phase feed stream obtained in step (1) enters the second fluidized bed hydrogenation reaction zone and reacts under the action of hydrogen and the second hydrogenation catalyst. The reaction products are separated in the second separation zone to obtain the second gas phase feed stream and the second liquid phase feed stream. The second liquid phase feed stream is separated in the third separation zone to obtain naphtha, diesel, wax oil and hydrogenated heavy oil. (3) The hydrotreated heavy oil obtained in step (2) enters the first extraction zone, and after contacting the solvent, it is used to obtain the first extract phase and the first raffinate phase. The first extract phase enters the solvent recovery unit to obtain bright oil and regenerated solvent. (4) The first raffinate obtained in step (3) enters the second extraction zone and comes into contact with naphtha to obtain the second extract phase and the second raffinate phase. The second extract phase is recycled to the first separation zone and / or the second fluidized bed hydrogenation reaction zone, preferably to the first separation zone.

2. The method according to claim 1, characterized in that: The properties of the residual oil raw material mentioned in step (1) are as follows: sulfur content 4.5wt%~6.0wt%, carbon residue 20wt%~26wt%, viscosity (150℃) 100mPa·s~200mPa·s.

3. The method according to claim 1, characterized in that: In step (1), at least one fluidized bed reactor is set up in the first fluidized bed hydrogenation reaction zone. The fluidized bed reactor is the STRONG fluidized bed reactor with built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd.

4. The method according to claim 1, characterized in that: In step (1), the first hydrogenation catalyst comprises a support and an active metal component, wherein the support is one or more of alumina, silicon oxide, alumina-silicon oxide, and titanium oxide, and the active metal is a group VIB and / or group VIII metal, preferably one or more of nickel, cobalt, molybdenum, and tungsten.

5. The method according to claim 1, characterized in that: The operating conditions of the first fluidized bed hydrogenation reaction zone in step (1) are as follows: reaction temperature 350–450℃, preferably 380–430℃; reaction pressure 10.0–25.0 MPa, preferably 15.0–19.0 ​​MPa; hydrogen-to-oil volume ratio 300–1000, preferably 400–700; and liquid hourly space velocity 0.1–2.0 h⁻¹. -1 Preferably, it is 0.2 to 1.0 h. -1 .

6. The method according to claim 1, characterized in that: In step (2), at least one fluidized bed reactor is set in the second fluidized bed hydrogenation reaction zone, preferably one fluidized bed reactor; the fluidized bed reactor is the STRONG fluidized bed reactor with built-in three-phase separator developed by Sinopec (Dalian) Petrochemical Research Institute Co., Ltd.

7. The method according to claim 1, characterized in that: In step (2), the second hydrogenation catalyst comprises a support and an active metal component, wherein the support is one or more of alumina, silicon oxide, alumina-silicon oxide, and titanium oxide, and the active metal is a group VIB and / or group VIII metal, preferably one or more of nickel, cobalt, molybdenum, and tungsten.

8. The method according to claim 1, characterized in that: The operating conditions of the second fluidized bed hydrogenation reaction zone in step (2) are as follows: reaction temperature 350–450℃, preferably 380–430℃; reaction pressure 10.0–25.0 MPa, preferably 15.0–19.0 ​​MPa; hydrogen-to-oil volume ratio 300–1000, preferably 400–700; and liquid hourly space velocity 0.1–2.0 h⁻¹. -1 Preferably, it is 0.2 to 1.0 h. -1 .

9. The method according to claim 1, characterized in that: The cutting point between naphtha and diesel in step (2) is 140-210°C, preferably 160-200°C; the cutting point between diesel and wax oil is 300-380°C, preferably 310-360°C; and the cutting point between wax oil and hydrogenated heavy oil is 450-570°C, preferably 470-540°C.

10. The method according to claim 1, characterized in that: In step (3), the solvent used in the first extraction zone is at least one of C3 to C7 alkanes, preferably C3 alkanes.

11. The method according to claim 1, characterized in that: In step (3), at least one extraction tower is set in the first extraction zone. The extraction tower is a rotating disc tower and / or a packed tower, preferably a packed tower. The packing material used in the packed tower is selected from one or more of grids, Raschig rings and Pall rings, preferably a grid.

12. The method according to claim 1, characterized in that: The operating conditions of the first extraction zone in step (3) are: temperature of 50-200℃, preferably 50-140℃, pressure of 2.0-6.0MPa, preferably 3.0-5.0MPa, and agent-to-oil mass ratio of 1.0-10.0, preferably 1.0-3.

0.

13. The method according to claim 1, characterized in that: In step (4), the naphtha used in the second extraction zone is straight-run naphtha or naphtha from a secondary processing unit. The naphtha from the secondary processing unit is one or more of the following: naphtha from a wax oil hydrocracking unit, naphtha from a coal tar hydrocracking unit, and naphtha from a gasoline and diesel hydrocracking unit. Preferably, the naphtha used in the second extraction zone is the naphtha obtained in step (2).

14. The method according to claim 1, characterized in that: In step (4), the second extraction zone uses an extraction tower or a centrifugal extraction device.

15. The method according to claim 1, characterized in that: The operating conditions of the second extraction zone in step (4) are: temperature of 50-200℃, preferably 80-150℃, pressure of 0.1-3.0MPa, preferably 1.0-2.0MPa, and agent-to-oil mass ratio of 0.4-1.5, preferably 0.5-1.

0.

16. The method according to claim 1, characterized in that: In steps (1) and (2), the equipment used in the first and second separation zones is a high-temperature and high-pressure separator, which is a thermal high-pressure separator, preferably a vertical thermal high-pressure separator; in step (2), the equipment used in the third separation zone is at least one of an atmospheric distillation tower and a vacuum distillation tower.

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