Slurry reactor hydrocracking oil residue solid removal method
Through multi-stage homogenization and extraction treatment combined with different solvents, the solid-liquid separation problem of hydrocracked oil residue in slurry bed is solved, and efficient oil residue treatment and resource utilization are achieved.
Patent Information
- Application Number
- CN202410187153.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-02-20
- Publication Date
- 2025-08-22
AI Technical Summary
The prior art cannot effectively treat slurry bed hydrocracked oil residue, resulting in large amount of oil residue, low economic value, and poor solid-liquid separation effect.
Multi-stage homogeneity treatment and multi-stage extraction technology are adopted, combined with different types of organic solvents, and the solid-liquid separation effect of hydrocracked oil residue in slurry bed is improved through the circulation treatment of high-speed shear field and extraction solvents.
It significantly improves the solid-liquid separation effect of oil residue, reduces the residual carbon value and ash content, and enhances the economic value of oil residue.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of efficient conversion of oily waste residues, and relates to a method for efficiently removing solids from slurry-bed hydrocracking oil residues. Background Art
[0002] With the shrinking supply of light crude oil, the conversion and refining of inferior feedstocks, such as heavy crude oil and vacuum residue (VR), has attracted widespread attention, and research on related catalysts has become a hot topic. Compared to light crude oil, inferior feedstocks have lower API gravity (≤21°) and are inexpensive, offering promising prospects for refining and conversion. However, their high levels of sulfur, nitrogen, and metallic impurities, along with a significant proportion of high-boiling-point heavy hydrocarbons, present challenges in upgrading and converting these inferior feedstocks (viscosity reduction, boiling point reduction, desulfurization, demetallization, and increasing the H / C ratio). For example, VR contains 10% to 30% polycyclic aromatic hydrocarbons and heteroatom asphaltenes, with a boiling point exceeding 813K, making it highly susceptible to coking during processing.
[0003] Hydrocracking (HCK) is an important method for converting low-quality feedstocks into low-boiling-point distillates. Slurry-bed hydrocracking utilizes a homogeneous catalyst that mixes well with the feedstock, resulting in strong coke suppression and a conversion rate exceeding 95%. This technology offers significant advantages in adaptability and selectivity for low-quality feedstocks. Despite this, slurry-bed hydrocracking remains unable to fully utilize low-quality feedstocks. This is primarily due to the need to remove some of the coked residue to prevent the impact of coking on the hydrocracking process during the recycling process. This removed residue is characterized by low saturates, high colloidal asphaltene content, high residual carbon content, and metal enrichment. This amount typically accounts for over 3-10 wt% of the plant's processing capacity. For a 100-ton / year slurry-bed plant, for example, a conservative estimate suggests that over 30,000 tons of this residue is required annually. Currently, the main methods for disposing of this residue are gasification to produce hydrogen followed by incineration to recover a small amount of metals or as fuel for steelmaking. This generally has low economic value and results in significant carbon emissions. Therefore, the efficient and comprehensive utilization of the removed residue from the slurry bed has enormous economic potential.
[0004] There are currently few reports on the treatment and utilization of discarded oil residue. CN113736509 A reports a method for treating residual oil from residual oil slurry bed hydrogenation. The method mixes the residual oil with solvent oil and porous materials, removes the metals in the residual oil, and then separates the solvent oil for recycling. The residual oil can be further processed as a coking or hydrogenation raw material. CN111394122A discloses a hydrogenation tailings treatment process and its use and design method. The method utilizes the difference in mutual solubility of the components of heavy distillate oil in the solvent, uses a solvent to extract the light components from the heavy components, separates the light and heavy components, and then separates the light components from the solvent through distillation. The mass ratio of the extractant used as the tailings solvent to the tailings is 15 to 25:1. The solid-liquid separation effect after extraction in the above-mentioned extraction method still needs to be further improved, and the residual carbon value and ash content of the solid phase material need to be further improved. Summary of the Invention
[0005] In response to the deficiencies in the prior art, the present invention provides a method for desolidifying oil residue from slurry-bed hydrocracking, which can achieve efficient conversion of waste oil residue, and the deoiled ash residue after extraction has high carbon residue value and ash content, high degree of solid-liquid separation, and good separation effect.
[0006] The present invention provides a method for treating slurry bed hydrocracking oil residue, which comprises the following contents: subjecting the slurry bed hydrocracking oil residue to N-stage homogenization treatment and M-stage extraction treatment, and subjecting the material after any one of the homogenization treatments to extraction treatment, wherein N is an integer of at least 1, and M is an integer of at least 2, and N can be 1, 2, 3, or 4, and M can be 2, 3, 4, or 5.
[0007] In the method of the present invention, the solid phase material obtained after solid-liquid separation of the material after extraction treatment less than M levels can be homogenized or extracted again, and the material after M-th level extraction treatment can be further processed after solid-liquid separation, and the said again includes one or more times.
[0008] In the method of the present invention, the slurry bed hydrocracking oil residue has the following properties: residual carbon ≥ 36 wt%, ash ≥ 0.6 wt%, dynamic viscosity (135°C) ≥ 50 mPa·s, dynamic viscosity (250°C) ≥ 10 mPa·s, distillate volume at 350°C ≤ 2 wt%, and distillate volume at 540°C ≤ 55 wt%.
[0009] In the method of the present invention, the homogenization process can be any of ultrasonic homogenization, high-speed jet homogenization, high-speed shear field homogenization, and grinding field homogenization, preferably high-speed shear field homogenization. When the homogenization process is high-speed shear field homogenization, the linear speed of the shear rotor is 30 to 70 m / s.
[0010] In the method of the present invention, the extraction solvent can be aromatic hydrocarbons, diesel, or wax oil. When the solvent is an aromatic hydrocarbon, it can specifically be at least one of benzene, biphenyl, naphthalene, anthracene, toluene, p-xylene, o-xylene, m-xylene, diphenylmethane, triphenylmethane, p-diethylbenzene, m-diethylbenzene, n-propylbenzene, isopropylbenzene, butylbenzene, isobutylbenzene, pentylbenzene, dodecylbenzene, and hexadecylbenzene. When the solvent is diesel, it can specifically be light diesel of various grades, or it can be crude oil obtained by crude oil fractionation, hydrocracking, or catalytic cracking. When the diesel is crude oil, it should have the following properties: residual carbon ≤ 0.1wt%, ash ≤ 0.05wt%, dynamic viscosity (135°C) ≤ 8mPa·s, distillate at 350°C ≥ 85wt%, and distillate at 540°C ≥ 98wt%. When the solvent oil is wax oil, it can be atmospheric wax oil, coker wax oil, etc. The atmospheric wax oil and coker wax oil should have the following properties: residual carbon ≤ 1.0wt%, ash ≤ 0.08wt%, dynamic viscosity (135°C) ≤ 8mPa·s, and distillate volume at 540°C ≥ 98wt%.
[0011] In the method of the present invention, slurry bed hydrocracking oil residue is mixed with an appropriate amount of an organic solvent and then homogenized. The organic solvent includes one or more of benzene, biphenyl, naphthalene, anthracene, toluene, p-xylene, o-xylene, m-xylene, diphenylmethane, triphenylmethane, p-diethylbenzene, m-diethylbenzene, n-propylbenzene, isopropylbenzene, butylbenzene, isobutylbenzene, pentylbenzene, dodecylbenzene, hexadecylbenzene, diesel, and wax oil.
[0012] In the method of the present invention, preferably part or all of the extraction solvent is mixed as an organic solvent with the slurry bed hydrocracking oil residue and then homogenized. More preferably, all of the extraction solvent is mixed as an organic solvent with the slurry bed hydrocracking oil residue and then homogenized.
[0013] In the method of the present invention, the feed temperature of the slurry bed hydrocracking oil residue is 200-300°C, and the feed temperature of the organic solvent or the extraction solvent is 20-50°C.
[0014] In the method of the present invention, the mass ratio of the first-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is 1:1 to 1:5, preferably 1:2 to 1:4, the mass ratio of the H-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is higher than the mass ratio of the first-stage extraction slurry bed hydrocracking oil residue to the extraction solvent, and the mass ratio of the H-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is generally 1:1 to 5:1, where H is greater than 1 and less than or equal to M.
[0015] In the method of the present invention, the extraction solvents of any stage can be the same or different, and the extraction solvent of the first stage is preferably diesel or wax oil. When the first-stage extraction solvent is diesel, it can specifically be light diesel of various brands, or it can be crude oil obtained by crude oil fractionation, hydrocracking, or catalytic cracking. When the diesel is crude oil, it should have the following properties: residual carbon ≤ 0.1wt%, ash ≤ 0.05wt%, dynamic viscosity (135°C) ≤ 8mPa·s, 350°C distillate ≥ 85wt%, 540°C distillate ≥ 98wt%; when the first solvent oil is wax oil, it can be atmospheric wax oil, coker wax oil, etc., and the atmospheric wax oil and coker wax oil should have the following properties: residual carbon ≤ 1.0wt%, ash ≤ 0.08wt%, dynamic viscosity (135°C) ≤ 8mPa·s, 540°C distillate ≥ 98wt%.
[0016] In the method of the present invention, when the H-1 stage extraction solvent is diesel or wax oil, the H stage extraction solvent is aromatic hydrocarbons, and the H is greater than 1 and less than or equal to M. The aromatic hydrocarbons can specifically be at least one of benzene, biphenyl, naphthalene, anthracene, toluene, p-xylene, o-xylene, m-xylene, diphenylmethane, triphenylmethane, p-diethylbenzene, m-diethylbenzene, n-propylbenzene, isopropylbenzene, butylbenzene, isobutylbenzene, pentylbenzene, dodecylbenzene, and hexadecylbenzene. The diesel can specifically be light diesel of various grades, or it can be crude oil obtained by crude oil fractionation, hydrocracking, or catalytic cracking. When the diesel is crude oil, it should have the following properties: residual carbon ≤ 0.1wt%, ash ≤ 0.05wt%, dynamic viscosity (135°C) ≤ 8mPa·s, distillate at 350°C ≥ 85wt%, and distillate at 540°C ≥ 98wt%. The solvent is wax oil which may be atmospheric wax oil, coker wax oil, etc. The atmospheric wax oil and coker wax oil should have the following properties: residual carbon ≤ 1.0wt%, ash ≤ 0.08wt%, dynamic viscosity (135°C) ≤ 8mPa·s, and distillate at 540°C ≥ 98wt%.
[0017] In the method of the present invention, the extraction temperature at any stage is 50-200°C, preferably 80-150°C, the number of cyclic extractions is 1 to 5 times, preferably 2 to 4 times; and the time for each cyclic extraction is 15 to 60 minutes, preferably 25 to 45 minutes.
[0018] In a non-limiting embodiment of the present invention, the slurry bed hydrocracking oil residue is subjected to primary and secondary extraction treatments after a primary homogenization treatment, and the solid phase material after the extraction treatment is subjected to a secondary homogenization treatment and then to tertiary and quaternary homogenization treatments.
[0019] In the method of the present invention, the solid phase material can be further processed, or directly coked or compounded with slurry bed hydrocracking oil residue for gasification and hydrogen production; the liquid phase material is used for subsequent processing and refining.
[0020] Compared with the prior art, the present invention provides a method for treating slurry bed hydrocracking oil residue, which has the following advantages: the method adopts homogenization and multi-stage extraction to significantly improve the solid-liquid separation effect of inferior oil residue, and the residual carbon value and ash content of the de-oiled ash residue after extraction are high, especially the method adopts multi-stage homogenization and multi-stage extraction or controls the type of extraction solvent, which has a more obvious effect. DETAILED DESCRIPTION
[0021] The slurry bed hydrocracking oil residue desolidification method of the present invention is further described below through comparative examples and specific examples, but does not constitute a limitation of the present invention.
[0022] The raw materials described in the Examples and Comparative Examples of the present invention are all oil residues discarded from a slurry bed hydrocracking unit of a certain company. The main properties of the oil residues are shown in Table 1. It should be noted that the description of the raw material properties in Table 1 is only for the purpose of describing the basic properties of the slurry bed oil residues to facilitate the illustration of the desolidification effects and differences of the oil residues in the Examples and Comparative Examples, and does not constitute a limitation on the raw materials selected for the present invention.
[0023] As shown in the table, the ash content of the slurry bed oil residue is as high as 0.729wt%, the residual carbon is 46.16wt%, the distillation amount at 350℃ is 1.0wt%, the distillation amount at 540℃ is only 32.9wt%, and the dynamic viscosity at 135℃ is still as high as 71.6wt%. It has the characteristics of high metal content, high content of heavy components, high viscosity, and poor high-temperature fluidity. It is difficult to achieve effective separation of oil and solid phases using conventional methods.
[0024] Table 1 Properties of slurry bed oil residue raw materials
[0025]
[0026] Example 1 (Examples 1 to 5 second level, 1 to 3 versus 8 to 10)
[0027] 50 kg of 260°C oil residue and 20°C catalytic fuel wood were pumped into the primary homogenization system at a mass ratio of 1:4. The catalytic fuel wood had basic physical properties: residual carbon 0.053 wt%, ash 0.025 wt%, dynamic viscosity (135°C) <5 mPa·s, distillate yields of 92.9 wt% at 350°C, and 99.6 wt% at 540°C. After thorough homogenization by rotor shear at a linear speed of 35 m / s, the mixture entered the primary extraction tank at 150°C. The mixture in the primary extraction tank was subjected to three extraction cycles, each lasting 15 minutes. After the extraction, solid-liquid separation is carried out, and the separated solid material and catalytic firewood (the mass ratio of oil residue to catalytic firewood is 2:1, and the oil residue is calculated based on the initial introduction amount, the same below) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 45m / s, it enters the secondary extraction tank at 100°C, and the mixed material in the secondary extraction tank is subjected to two cycles of extraction, each extraction time is 40min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is determined to be 78.9%, and the ash value is 6.27%.
[0028] Example 2
[0029] 45 kg of 240°C oil residue and 40°C pulp wood were pumped into the primary homogenization system at a 1:1 mass ratio. The pulp wood had the following basic physical properties: residual carbon 0.074 wt%, ash 0.018 wt%, dynamic viscosity (135°C) <5 mPa·s, distillate yields of 87.2 wt% at 350°C, and 98.8 wt% at 540°C. After thorough homogenization by shearing with a rotor at a linear speed of 30 m / s, the mixture entered the primary extraction tank at 95°C. The mixture in the primary extraction tank was subjected to five extraction cycles, each lasting 22 minutes. After the extraction, solid-liquid separation is carried out, and the separated solid material and pulp wood (the mass ratio of oil residue to pulp wood is 4:1) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 70m / s, it enters the secondary extraction tank at 110°C. The mixed material in the secondary extraction tank is subjected to three cycles of extraction, with each extraction time of 38min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is determined to be 76.2%, and the ash value is 5.83%.
[0030] Example 3
[0031] 60 kg of 200°C oil residue and 50°C vacuum gas oil (VGO) were pumped into the primary homogenization system at a mass ratio of 1:5. The VGO's basic physical properties were: 0.37 wt% carbon residue, 0.023 wt% ash, a dynamic viscosity (135°C) of less than 5 mPa·s, and a distillate yield of 98.6 wt% at 540°C. After thorough homogenization using a rotor shearing process at a linear speed of 55 m / s, the mixture entered the primary extraction tank at 125°C. The mixture in the primary extraction tank was subjected to a single extraction cycle, with each extraction lasting 60 minutes. After the extraction, solid-liquid separation is carried out, and the separated solid material and VGO (oil residue: VGO = 5:1) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 65m / s, it enters the secondary extraction tank at 87°C. The mixed material in the secondary extraction tank is subjected to 5 cycles of extraction, each extraction time is 18min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is measured to be 74.9%, and the ash value is 5.87%.
[0032] Example 4
[0033] Fifty kilograms of 300°C oil residue and 45°C coker gas oil (CGO) were pumped into the primary homogenization system at a mass ratio of 1:4. The CGO's basic physical properties were: 0.54% carbon residue, 0.033% ash, a dynamic viscosity (135°C) of less than 5 mPa·s, and a 99.1% distillate at 540°C. After thorough homogenization using a rotor shearing system at a linear speed of 58 m / s, the mixture entered the primary extraction tank at 200°C. The mixture was then subjected to two 45-minute extraction cycles. After the extraction, solid-liquid separation is carried out, and the separated solid material and CGO (oil residue: CGO = 3:1) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 66m / s, it enters the secondary extraction tank at 160°C. The mixed material in the secondary extraction tank is subjected to 4 cycles of extraction, with each extraction time of 25min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is measured to be 76.4%, and the ash value is 5.25%.
[0034] Example 5
[0035] 50 kg of 255°C oil residue and 20°C meta-diethylbenzene were pumped into the primary homogenization system at a mass ratio of 1:2. After thorough homogenization by rotor shearing at a linear speed of 55 m / s, the mixture entered the primary extraction tank at 80°C. The mixture in the primary extraction tank was subjected to three extraction cycles, each lasting 20 minutes. After the extraction, solid-liquid separation was performed. The separated solid material and meta-diethylbenzene (oil residue: meta-diethylbenzene = 1:1) were pumped into the secondary homogenization system. After thorough homogenization by rotor shearing at a linear speed of 65 m / s, the mixture entered the secondary extraction tank at 50°C. The mixture in the secondary extraction tank was subjected to five extraction cycles, each lasting 28 minutes. After the extraction, solid-liquid separation was performed and the solid material was collected. The carbon residue in the solid phase was determined to be 77.2%, and the ash content was 5.66%.
[0036] Example 6 (6-7 are the third level, corresponding to the non-preferred conditions of 4-5)
[0037] Fifty kilograms of 300°C oil residue and 45°C coker gas oil (CGO) were pumped into the primary homogenization system at a 1:1 mass ratio. The CGO's basic physical properties were: 0.54% carbon residue, 0.033% ash, a dynamic viscosity (135°C) of less than 5 mPa·s, and a 99.1% distillate at 540°C. After thorough homogenization using a rotor shearing system at a linear speed of 58 m / s, the mixture entered the primary extraction tank at 210°C. The mixture was then subjected to two 10-minute extraction cycles. After the extraction, solid-liquid separation is carried out, and the separated solid material and CGO (oil residue: CGO = 1:3) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 66m / s, it enters the secondary extraction tank at 160°C. The mixed material in the secondary extraction tank is subjected to 4 cycles of extraction, and each extraction time is 10min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is measured to be 65.2%, and the ash value is 3.13.
[0038] Example 7
[0039] 50 kg of 255°C oil residue and 20°C meta-diethylbenzene were pumped into the primary homogenization system at a 1:1 mass ratio. The mixture was fully homogenized by shearing with a rotor at a linear speed of 55 m / s before entering the primary extraction tank at 80°C. The mixture in the primary extraction tank was subjected to three 10-minute extraction cycles. After the extraction, solid-liquid separation was performed. The separated solid material and meta-diethylbenzene (oil residue: meta-diethylbenzene = 1:2) were pumped into the secondary homogenization system. After fully homogenized by shearing with a rotor at a linear speed of 65 m / s, the mixture was entered into the secondary extraction tank at 50°C. The mixture in the secondary extraction tank was subjected to five 10-minute extraction cycles. After the extraction, solid-liquid separation was performed and the solid material was collected. The carbon residue in the solid phase was determined to be 66.8%, and the ash content was 3.42%.
[0040] Example 8 (Examples 8 to 10, first level, comparative examples 1 to 3, protection of different solvent extraction)
[0041] 50 kg of 260°C oil residue and 20°C catalytic fuel wood were pumped into the primary homogenization system at a mass ratio of 1:4. The catalytic fuel wood had basic physical properties: residual carbon 0.053 wt%, ash 0.025 wt%, dynamic viscosity (135°C) <5 mPa·s, distillate yields of 92.9 wt% at 350°C, and 99.6 wt% at 540°C. After thorough homogenization by rotor shear at a linear speed of 35 m / s, the mixture entered the primary extraction tank at 150°C. The mixture in the primary extraction tank was subjected to three extraction cycles, each lasting 15 minutes. After the extraction, solid-liquid separation is carried out, and the separated solid material and p-xylene (the mass ratio of oil residue to p-xylene is 2:1, and the oil residue is calculated based on the initial introduction amount, the same below) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 45m / s, it enters the secondary extraction tank at 100°C, and the mixed material in the secondary extraction tank is subjected to two cycles of extraction, each extraction time is 40min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is measured to be 83.8%, and the ash value is 7.65%.
[0042] Example 9
[0043] 45 kg of 240°C oil residue and 40°C pulp wood were pumped into the primary homogenization system at a 1:1 mass ratio. The pulp wood had the following basic physical properties: residual carbon 0.074 wt%, ash 0.018 wt%, dynamic viscosity (135°C) <5 mPa·s, distillate yields of 87.2 wt% at 350°C, and 98.8 wt% at 540°C. After thorough homogenization by shearing with a rotor at a linear speed of 30 m / s, the mixture entered the primary extraction tank at 95°C. The mixture in the primary extraction tank was subjected to five extraction cycles, each lasting 22 minutes. After the extraction, solid-liquid separation is carried out, and the separated solid material and isopropylbenzene (the mass ratio of oil residue to isopropylbenzene is 4:1) are pumped into the secondary homogenization system respectively. After the mixed material is fully homogenized by rotor shearing at a linear speed of 70m / s, it enters the secondary extraction tank at 110°C, and the mixed material in the secondary extraction tank is subjected to three cycles of extraction, each extraction time is 38min. After the extraction, solid-liquid separation is carried out, and the solid material is collected. The residual carbon value of the solid phase material is measured to be 85.2%, and the ash value is 7.79%.
[0044] Example 10
[0045] 60 kg of 200°C oil residue and 50°C vacuum gas oil (VGO) were pumped into the primary homogenization system at a mass ratio of 1:5. The VGO's basic physical properties were: 0.37 wt% carbon residue, 0.023 wt% ash, a dynamic viscosity (135°C) of less than 5 mPa·s, and a distillate yield of 98.6 wt% at 540°C. After thorough homogenization using a rotor shearing process at a linear speed of 55 m / s, the mixture entered the primary extraction tank at 125°C. The mixture in the primary extraction tank was subjected to a single extraction cycle, with each extraction lasting 60 minutes. After the extraction, solid-liquid separation was carried out, and the separated solid material and diethylbenzene (oil residue: diethylbenzene = 5:1) were pumped into the secondary homogenization system respectively. After the mixed material was fully homogenized by rotor shearing at a linear speed of 65m / s, it entered the secondary extraction tank at 87°C. The mixed material in the secondary extraction tank was subjected to 5 cycles of extraction, each extraction time was 18min. After the extraction, solid-liquid separation was carried out, and the solid material was collected. The residual carbon value of the solid phase material was measured to be 82.2%, and the ash value was 7.32.
Claims
1. A method for treating slurry bed hydrocracking oil residue, characterized in that: The method comprises the following contents: subjecting slurry bed hydrocracking oil residue to N-stage homogenization treatment and M-stage extraction treatment, and subjecting the material after any of the homogenization treatments to extraction treatment, wherein N is an integer of at least 1 and M is an integer of at least 2.
2. The method according to claim 1, wherein: The N is 1, 2, 3 or 4, and the M is 2, 3, 4 or 5.
3. The method according to claim 1, wherein: The solid phase material obtained after the solid-liquid separation of the material after the extraction treatment of less than M levels is homogenized or extracted again, and the material after the Mth level extraction treatment is further processed after solid-liquid separation.
4. The method according to claim 3, wherein: The again refers to one or more times.
5. The method according to claim 1, wherein: The slurry bed hydrocracking oil residue has the following properties: residual carbon ≥ 36 wt%, ash ≥ 0.6 wt%, dynamic viscosity (135°C) ≥ 50 mPa·s, dynamic viscosity (250°C) ≥ 10 mPa·s, distillation amount at 350°C ≤ 2 wt%, and distillation amount at 540°C ≤ 55 wt%.
6. The method according to claim 1, wherein: The homogenization treatment is any one of ultrasonic homogenization, high-speed jet homogenization, high-speed shear field homogenization, and grinding field homogenization, preferably high-speed shear field homogenization.
7. The method according to claim 6, characterized in that: When the homogenization method is high-speed shear field homogenization, the linear speed of the shear rotor is 30 to 70 m / s.
8. The method according to claim 1, wherein: The extraction solvent is aromatic hydrocarbon, diesel or wax oil.
9. The method according to claim 8, characterized in that: The aromatic hydrocarbon is at least one of benzene, biphenyl, naphthalene, anthracene, toluene, p-xylene, o-xylene, m-xylene, diphenylmethane, triphenylmethane, p-diethylbenzene, m-diethylbenzene, n-propylbenzene, isopropylbenzene, butylbenzene, isobutylbenzene, pentylbenzene, dodecylbenzene, and hexadecylbenzene.
10. The method according to claim 8, characterized in that: The diesel is crude diesel obtained by crude oil fractionation, hydrocracking, and catalytic cracking, and has the following properties: residual carbon ≤ 0.1 wt%, ash ≤ 0.05 wt%, dynamic viscosity (135° C.) ≤ 8 mPa·s, distillate volume at 350° C. ≥ 85 wt%, and distillate volume at 540° C. ≥ 98 wt%.
11. The method according to claim 8, wherein: The wax oil is atmospheric wax oil or coker wax oil, and has the following properties: residual carbon ≤1.0wt%, ash ≤0.08wt%, dynamic viscosity (135°C) ≤8mPa·s, and distillate amount at 540°C ≥98wt%.
12. The method according to claim 1, wherein: The slurry bed hydrocracking oil residue is mixed with an appropriate amount of organic solvent and then homogenized, with a mass ratio of 1:1 to 1:5, preferably 1:2 to 1:
4.
13. The method according to claim 1, wherein: The organic solvent includes one or more of benzene, biphenyl, naphthalene, anthracene, toluene, p-xylene, o-xylene, m-xylene, diphenylmethane, triphenylmethane, p-diethylbenzene, m-diethylbenzene, n-propylbenzene, isopropylbenzene, butylbenzene, isobutylbenzene, pentylbenzene, dodecylbenzene, hexadecylbenzene, diesel, and wax oil.
14. The method according to claim 1, wherein: Part or all of the extraction solvent is mixed as an organic solvent with the slurry bed hydrocracking oil residue and then subjected to homogenization treatment. More preferably, all of the extraction solvent is mixed as an organic solvent with the slurry bed hydrocracking oil residue and then subjected to homogenization treatment.
15. The method according to claim 1, wherein: The feed temperature of the slurry bed hydrocracking oil residue is 200°C to 300°C, and the feed temperature of the organic solvent or extraction solvent is 20°C to 50°C.
16. The method according to claim 1, wherein: The mass ratio of the first-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is 1:1 to 1:5, preferably 1:2 to 1:
4.
17. The method according to claim 1, wherein: The mass ratio of the H-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is higher than the mass ratio of the first-stage extraction slurry bed hydrocracking oil residue to the extraction solvent, and H is greater than 1 and less than or equal to M.
18. The method according to claim 17, wherein: The mass ratio of the H-stage extraction slurry bed hydrocracking oil residue to the extraction solvent is 1:1 to 5:
1.
19. The method according to claim 1, wherein: The extraction solvents of any stage are the same or different. Preferably, the extraction solvent of the first stage is diesel or wax oil.
20. The method according to claim 1, wherein: When the H-1 stage extraction solvent is diesel or wax oil, the H stage extraction solvent is aromatic hydrocarbons, and the H is greater than 1 and less than or equal to M.
21. The method according to claim 1, wherein: The extraction temperature at any stage is 50-200° C., preferably 80-150° C., the number of cyclic extractions is 1 to 5 times, preferably 2 to 4 times; and the time for each cyclic extraction is 15 to 60 minutes, preferably 25 to 45 minutes.
22. The method according to claim 1, wherein: The slurry bed hydrocracking oil residue is subjected to primary and secondary extraction treatments after the primary homogenization treatment, and the solid phase material after the extraction treatment is subjected to tertiary and quaternary homogenization treatments after the secondary homogenization treatment.
23. The method according to claim 1, wherein: The solid phase material is further processed, either directly subjected to coking treatment or compounded with slurry bed hydrocracking oil residue for gasification and hydrogen production; the liquid phase material is provided for subsequent processing and refining.
Citation Information
Patent Citations
Hydrogenation tailing treatment process as well as application and design method thereof
CN111394122A
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CN113736509A