Road asphalt material and preparation method thereof
Through the fractionation of catalytic oil slurry and the reaction of solid strong acid catalyst, stable materials that meet the A-level requirements of road asphalt are generated, which solves the problem that catalytic oil slurry cannot meet the quality of high-level road asphalt, and achieves efficient utilization of resources and performance improvement.
Patent Information
- Application Number
- CN202410122993.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-30
- Publication Date
- 2025-08-01
AI Technical Summary
In the prior art, catalytic oil slurry cannot meet the quality requirements of advanced road asphalt, and the resource utilization efficiency is low, and the reaction instability leads to poor performance.
By fractionating the catalytic oil slurry into light, medium and heavy components, and reacting with solid strong acid catalysts, products I, II, and III are generated, and then mixed with the kettle residue, the reaction is controlled by the directional control of the catalyst to improve the reaction efficiency and stability.
The generated road asphalt material meets the A-level requirements of road petroleum asphalt in JTG F40, has stable performance, low temperature sensitivity, good high temperature strength, and high resource utilization value.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of road asphalt, and particularly to a road asphalt material and a preparation method thereof. Background Art
[0002] Catalytic slurry oil is the remaining aromatic-rich waste slurry discharged from a catalytic cracking unit during the petroleum refining process. Most catalytic cracking processes blend vacuum residue or atmospheric residue. With the continuous heavy and inferior quality of crude oil, the total amount of metal pollutants, high-molecular-weight asphalt and gum, and heteroatom compounds such as sulfur and nitrogen shows an obvious increasing trend. At the same time, the increase in the residue blending ratio of the raw material brings adverse effects such as poor product distribution and decreased unit throughput to the catalytic slurry oil. To address this problem, external discharging of the slurry oil is an often-used effective method. Currently, Chinese catalytic slurry oil is mainly used as a blending component for fuel oil or heavy fuel oil, with a small scope of use and low economic benefits.
[0003] Chinese catalytic slurry oil has characteristics such as high density, low hydrogen-to-carbon atom ratio, and high residue carbon value. In terms of composition, it has a high aromatic content, mostly above 55%, a low gum and asphaltene content, and a saturated hydrocarbon content mostly below 35%, making it an excellent component for improving the quality of asphalt. However, the catalytic slurry oil has a low boiling point and low degree of condensation, resulting in a series of problems such as poor temperature sensitivity and poor anti-aging performance after blending with asphalt, and it cannot meet the quality requirements of high-grade road asphalt.
[0004] CN115820289A discloses a method for preparing mesophase pitch. In this method, light aromatic oil, medium aromatic oil, and heavy aromatic oil in the catalytic slurry oil are respectively polymerized and distilled into low softening point mesophase pitch, medium softening point mesophase pitch, and high softening point mesophase pitch, and are mixed and modulated in different proportions to obtain mesophase pitch with different characteristics. The preparation process used in this method does not use any catalyst, the reaction randomness is relatively strong, the reaction conversion will vary greatly for catalytic slurry oils obtained from different raw materials, the softening point of the mesophase obtained after the reaction is too high, which is not suitable for road asphalt, and the still residue after distillation is not utilized.
[0005] CN108728147A discloses a method for preparing mesophase pitch and carbon fiber by rapid pyrolysis pretreatment of heavy oil - catalytic polycondensation. In this method, the raw material is pretreated by short-time high-temperature pyrolysis and then mixed with a catalyst to prepare mesophase pitch. The softening point of the mesophase pitch prepared by this method exceeds 230 °C and cannot be used as road asphalt. Summary of the Invention
[0006] To address the shortcomings of existing technologies, the present invention provides a road asphalt material and a method for preparing the same. The method is simple and easy to operate, resulting in a road asphalt material with outstanding comprehensive performance, meeting the technical requirements of existing Grade A road petroleum asphalt. Furthermore, while maintaining the performance of road asphalt, it also fully and rationally utilizes slurry resources, resulting in high resource utilization value.
[0007] A first aspect of the present invention provides a method for preparing a road asphalt material, comprising the following steps:
[0008] (1) Fractionating the catalytic oil slurry to obtain four components: light component, medium component, heavy component, and kettle residue;
[0009] (2) contacting the light component and the medium component separated in step (1) with a solid strong acid catalyst to react respectively to obtain product I and product II; and mixing the heavy component in step (1) with an oxygen-containing gas to react to obtain product III;
[0010] (3) Mixing the still residue in step (1) and product I, product II and product III obtained in step (2) to obtain the road asphalt material.
[0011] Furthermore, in step (1), the catalytic slurry is a catalytic slurry produced by a catalytic cracking unit of natural petroleum, and is a mixture rich in aromatics; the mass content of aromatics in the catalytic slurry is 50% to 90%, the mass content of paraffins in the catalytic slurry is less than 5%, and the mass content of cycloalkanes is less than 15%.
[0012] Furthermore, in step (1), the catalytic oil slurry fractionation method is preferably carried out by a reduced pressure distillation method with a vacuum degree of 2 to 5 mbar.
[0013] Furthermore, in step (1), the cutting point between the light component and the medium component is 340°C to 360°C, the cutting point between the medium component and the heavy component is 430°C to 450°C, and the cutting point between the heavy component and the still residue is 510°C to 530°C.
[0014] Furthermore, in step (1), the mass content of the light component in the catalytic oil slurry is 18-29%, the mass content of the medium component is 28-38%, the mass content of the heavy component is 30-40%, and the remainder is kettle residue.
[0015] Furthermore, in step (2), the solid strong acid catalyst is SO4 2- / ZrO2、SO4 2- / TiO2、SO4 2- / Fe2O3、SO4 2- / Fe2O3-Al2O3、SO4 2-At least one of / MoO3-TiO2, preferably SO4 2- / ZrO2; in the solid strong acid catalyst, the mass content of sulfur is 9.5% to 15%; the particle size of the solid strong acid catalyst is 120 to 300 mesh. The inventors found that using the solid strong acid catalyst of the present invention in the preparation method can obtain a road asphalt material with outstanding properties.
[0016] Further, in step (2), the light components in step (1) are reacted under the action of a catalyst, and the mass ratio of the light components to the catalyst is (10 to 20):(1 to 3).
[0017] Further, in step (2), the light components and the catalyst in step (1) are reacted. The reaction is carried out during stirring. The stirring speed is 100 r / min to 200 r / min, the reaction temperature is 170 °C to 190 °C, the reaction pressure is 1.3 MPa to 1.8 MPa, and the reaction time is 1 h to 5 h. When the 60 °C dynamic viscosity of the material reaches 80 to 120 Pa·s, the reaction is stopped to obtain product I.
[0018] Further, in step (2), the middle components in step (1) are reacted under the action of a catalyst, and the mass ratio of the middle components to the catalyst is (10 to 20):(1 to 3).
[0019] Further, in step (2), the middle components and the catalyst in step (1) are reacted. The reaction is carried out during stirring. The stirring speed is 100 r / min to 200 r / min, the reaction temperature is 180 °C to 200 °C, the reaction pressure is 1.5 MPa to 2.0 MPa, and the reaction time is 3 h to 5 h. When the 60 °C dynamic viscosity of the material reaches 130 to 170 Pa·s, the reaction is stopped to obtain product II.
[0020] Further, in step (2), the heavy components in step (1) are added to the reaction kettle, and an oxygen-containing gas is introduced during stirring. The air flow rate is 0.17 to 1.7 L / min, preferably 0.8 - 1.4 L / min; the stirring speed of the reaction kettle is 100 r / min to 200 r / min, the reaction temperature is 200 °C to 250 °C, the reaction pressure is 0.2 MPa to 0.5 MPa, and the reaction time is 1 h to 3 h. When the 60 °C dynamic viscosity of the material reaches 460 to 540 Pa·s, the reaction is stopped to obtain product III. The oxygen-containing gas is preferably air.
[0021] Further, the residue from step (1) is stirred and mixed with Product I, Product II, and Product III obtained in step (3). The mass ratio of Product I, Product II, Product III to the residue is (20 - 30):(30 - 40):(30 - 45):(5 - 10). The stirring speed is 200 r / min - 500 r / min, the stirring temperature is 170°C - 200°C, and the stirring time is 1 h - 2 h to obtain a road asphalt material.
[0022] In the second aspect of the present invention, there is provided a road asphalt material obtained by the above method for preparing a road asphalt material.
[0023] Further, the road asphalt material contains a catalytic slurry component and a catalyst.
[0024] Further, the mass content of the catalyst in the road asphalt material is 2 - 15%, preferably 4 - 13%.
[0025] Further, the catalytic slurry is a catalytic slurry produced by a catalytic cracking unit from natural petroleum, and is a mixture rich in aromatics. The mass content of aromatics in the catalytic slurry is 50% - 90%, the mass content of paraffins in the catalytic slurry is less than 5%, and the mass content of naphthenes is less than 15%.
[0026] Further, the catalytic slurry component includes a light component, a middle component, a heavy component, and a residue component.
[0027] Further, the catalyst is at least one of SO4 2- / ZrO2, SO4 2- / TiO2, SO4 2- / Fe2O3, SO4 2- / Fe2O3 - Al2O3, SO4 2- / MoO3 - TiO2, and is preferably SO4 2- / ZrO2.
[0028] Further, the road asphalt material meets the technical requirements of road petroleum asphalt in JTG F40. Among them, the penetration (0.1 mm) of the road asphalt material of the present invention at 25°C is 40 - 100, meeting the requirements of Grade A of No. 50, Grade A of No. 70, and Grade A of No. 90; the softening point is not lower than 45°C, meeting the requirements of Grade A of No. 50, Grade A of No. 70, and Grade A of No. 90; the ductility at 10°C is not lower than 45 cm, meeting the requirements of Grade A of No. 50, Grade A of No. 70, and Grade A of No. 90; the dynamic viscosity at �0°C is not less than 0 Pa·s, meeting the requirements of Grade A of No. 50, Grade A of No. 70, and Grade A of No. 90.
[0029] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0030] (1) In the method provided by the present invention, each component of the catalytic slurry is separated, and the directional control reaction is carried out by using the characteristics of each component of the catalytic slurry, so as to avoid the mutual interference of different components during the reaction, affect the reaction efficiency, and realize the molecular-level utilization of the slurry; in addition, the catalyst preparation method of the present invention is simple and has stable properties. Acting on the components of the catalytic slurry can increase the reaction rate of the oligomers in the catalytic slurry, has a good catalytic effect on the oligomerization reaction, and does not require a complex separation process to separate the catalyst remaining in the product. The saturated hydrocarbons contained in the light components and middle components separated from the catalytic slurry of the present invention have good chemical stability. In the polycondensation reaction of the light components, middle components and the catalyst, the dispersion degree of the reactants can be increased, ensuring that the condensation reaction proceeds slowly and stably, and avoiding the occurrence of violent polymerization reactions that affect the product quality. Each component of the catalytic slurry reacts with the catalyst, reducing the small-molecule substances and increasing the large-molecule substances in the catalytic slurry, and the thermal stability and chemical stability of the molecules are better, thereby improving the performance stability of the road asphalt material.
[0031] (2) Through the fractional reaction of each component of the catalytic slurry of the present invention, a road asphalt material with more suitable molecular weight and chemical components is generated, the colloidal structure stability of the material is better, the reaction stability is better, the temperature sensitivity is lower, and the high-temperature strength is better.
[0032] (3) Each component in the road asphalt material provided by the present invention cooperates with each other and acts together, making the material have outstanding stability, meeting the technical requirements of Class A road petroleum asphalt in JTG F40, and while taking into account the performance of the road asphalt, the slurry resources are fully and reasonably utilized, having a high resource utilization value. Detailed implementation mode
[0033] The technical solutions and effects of the present invention will be further described below through examples. The examples are implemented on the premise of the technical solutions of the present invention, and the detailed implementation methods and specific operation processes are given, but the protection scope of the present invention is not limited to the following examples.
[0034] [[ID=~15]]Example 1
[0035] Take 6 kg of catalytic slurry (the slurry is the catalytic slurry produced by the catalytic cracking unit of natural petroleum, and is a mixture rich in aromatics. The content of aromatics in the catalytic slurry is 78% (by mass). The mass content of paraffins in the catalytic slurry is 4.3%, and the mass content of naphthenes is 12.2%) and distill it through a vacuum distillation process. The vacuum degree is 3.2 mbar, and it is cut to obtain light components at room temperature to 350 °C, middle components at 350 °C to 440 °C, and heavy components at 440 °C to 520 °C respectively. The fraction remaining above 520 °C is used as the still residue, and the specific composition is shown in Table 1.
[0036] The catalyst is SO4 2- / Fe2O3. Among them, the mass content of sulfur is 10.6%. The particle size is 200 mesh.
[0037] Add the light components at room temperature to 350°C and the catalyst into the reaction kettle and stir to react. The mass ratio of the light components to the catalyst is 10:3, the stirring speed is 150 r / min, the reaction temperature is 170°C, the reaction pressure is 1.6 MPa, and the reaction time is 3 h. When the dynamic viscosity of the material at 60°C reaches 100 Pa·s, stop the reaction to obtain Product I.
[0038] Add the middle components at 350°C to 440°C and the catalyst into the reaction kettle and stir to react. The mass ratio of the middle components to the catalyst is 20:3, the stirring speed is 150 r / min, the reaction temperature is 180°C, the reaction pressure is 1.8 MPa, and the reaction time is 4 h. When the dynamic viscosity of the material at 60°C reaches 150 Pa·s, stop the reaction to obtain Product II.
[0039] Take the fraction at 440°C to 520°C as the heavy components and add them into the reaction kettle. During the stirring process, introduce air with an air flow rate of 0.85 L / min, the stirring speed is 150 r / min, the reaction temperature is 240°C, the reaction pressure is 0.5 MPa, and the reaction time is 2 h. When the dynamic viscosity of the material at 60°C reaches 500 Pa·s, stop the reaction to obtain Product III.
[0040] Stir and mix Product I, Product II, Product III and the kettle residue greater than 520°C according to a mass ratio of 22:31:38:9, with a stirring speed of 350 r / min, a stirring temperature of 175°C, and a stirring time of 1 h to obtain a road asphalt material with stable performance.
[0041] Example 2
[0042] Take 6 kg of catalytic slurry (the same as in Example 1), distill it through a vacuum distillation process with a vacuum degree of 3.2 mbar, and perform cutting to obtain light components at room temperature to 350°C, middle components at 350°C to 440°C, heavy components at 440°C to 520°C, and the remaining fraction greater than 520°C as the kettle residue. The specific components are shown in Table 1.
[0043] The catalyst is SO4 2- / Fe2O3 - Al2O3. Among them, the mass content of sulfur is 11.3%. The particle size is 200 mesh.
[0044] Add the light components at room temperature to 350 °C and the catalyst into the reaction kettle, stir and react. The mass ratio of the light components to the catalyst is 15:3, the stirring speed is 150 r / min, the reaction temperature is 180 °C, the reaction pressure is 1.6 MPa, and the reaction time is 4 h. When the dynamic viscosity of the material at 60 °C reaches 100 Pa·s, stop the reaction to obtain Product I.
[0045] Add the middle components at 350 °C to 440 °C and the catalyst into the reaction kettle, stir and react. The mass ratio of the middle components to the catalyst is 15:3, the stirring speed is 150 r / min, the reaction temperature is 190 °C, the reaction pressure is 1.8 MPa, and the reaction time is 3 h. When the dynamic viscosity of the material at 60 °C reaches 150 Pa·s, stop the reaction to obtain Product II.
[0046] Add the fraction at 440 °C to 520 °C as the heavy components into the reaction kettle, and introduce air during stirring. The air flow rate is 1.0 L / min, the stirring speed is 150 r / min, the reaction temperature is 230 °C, the reaction pressure is 0.5 MPa, and the reaction time is 2 h. When the dynamic viscosity of the material at 60 °C reaches 500 Pa·s, stop the reaction to obtain Product III.
[0047] Stir and mix Product I, Product II, Product III and the kettle residue above 520 °C according to the mass ratio of 24:35:32:8. The stirring speed is 350 r / min, the stirring temperature is 175 °C, and the stirring time is 1 h to obtain a road asphalt material with stable performance.
[0048] Example 3
[0049] Take 6 kg of catalytic slurry (the same as in Example 1), distill it through a vacuum distillation process, the vacuum degree is 3.2 mbar, and cut it to obtain the light components at room temperature to 350 °C, the middle components at 350 °C to 440 °C, and the heavy components at 440 °C to 520 °C. The remaining fraction above 520 °C is used as the kettle residue, and the specific components are shown in Table 1.
[0050] The catalyst is SO4 2- / ZrO2. Among them, the mass content of sulfur is 10.2%. The particle size is 200 mesh.
[0051] Add the light components at room temperature to 350 °C and the catalyst into the reaction kettle, stir and react. The mass ratio of the light components to the catalyst is 15:2, the stirring speed is 150 r / min, the reaction temperature is 190 °C, the reaction pressure is 1.6 MPa, and the reaction time is 5 h. When the dynamic viscosity of the material at 60 °C reaches 100 Pa·s, stop the reaction to obtain Product I.
[0052] Add the middle fraction at 350°C to 440°C and the catalyst into the reaction kettle, stir and react. The mass ratio of the middle fraction to the catalyst is 15:2, the stirring speed is 150 r / min, the reaction temperature is 200°C, the reaction pressure is 1.8 MPa, and the reaction time is 5 h. When the dynamic viscosity of the material at 60°C reaches 150 Pa·s, stop the reaction to obtain Product II.
[0053] Add the fraction at 440°C to 520°C as the heavy fraction into the reaction kettle, introduce air during stirring, the air flow rate is 1.3 L / min, the stirring speed is 150 r / min, the reaction temperature is 250°C, the reaction pressure is 0.5 MPa, and the reaction time is 3 h. When the dynamic viscosity of the material at 60°C reaches 500 Pa·s, stop the reaction to obtain Product III.
[0054] Stir and mix Product I, Product II, Product III and the kettle residue above 520°C according to the mass ratio of 27:36:31:6. The stirring speed is 350 r / min, the stirring temperature is 175°C, and the stirring time is 1 h to obtain a road asphalt material with stable performance.
[0055] Example 4
[0056] Take 6 kg of catalytic slurry (the same as in Example 1), distill it through a vacuum distillation process, the vacuum degree is 3.2 mbar, and perform cutting to obtain the light fraction at room temperature to 350°C, the middle fraction at 350°C to 440°C, the heavy fraction at 440°C to 520°C, and the remaining fraction above 520°C as the kettle residue. The specific components are shown in Table 1.
[0057] The catalyst is SO4 2- / TiO2. Among them, the mass content of sulfur is 11.6%. The particle size is 200 mesh.
[0058] Add the light fraction at room temperature to 350°C and the catalyst into the reaction kettle, stir and react. The mass ratio of the light fraction to the catalyst is 10:3, the stirring speed is 150 r / min, the reaction temperature is 170°C, the reaction pressure is 1.6 MPa, and the reaction time is 4 h. When the dynamic viscosity of the material at 60°C reaches 100 Pa·s, stop the reaction to obtain Product I.
[0059] Add the middle fraction at 350°C to 440°C and the catalyst into the reaction kettle, stir and react. The mass ratio of the middle fraction to the catalyst is 10:3, the stirring speed is 150 r / min, the reaction temperature is 180°C, the reaction pressure is 1.8 MPa, and the reaction time is 5 h. When the dynamic viscosity of the material at 60°C reaches 150 Pa·s, stop the reaction to obtain Product II.
[0060] The fraction of 440 °C to 520 °C is added as a heavy fraction to the reaction kettle, air is introduced during stirring, the air flow rate is 1.2 L / min, the stirring speed is 150 r / min, the reaction temperature is 240 °C, the reaction pressure is 0.5 MPa, and the reaction time is 4 h. When the kinematic viscosity of the material reaches 500 Pa·s at 60 °C, the reaction is stopped to obtain Product III.
[0061] Product I, Product II, Product III, and the kettle residue greater than 520 °C are stirred and mixed in a mass ratio of 19:30:39:12. The stirring speed is 350 r / min, the stirring temperature is 175 °C, and the stirring time is 1 h to obtain a road asphalt material with stable performance.
[0062] Comparative Example 1
[0063] Take 6 kg of catalytic slurry (the same as in Example 1), perform distillation through a vacuum distillation process with a vacuum degree of 3.2 mbar, and perform cutting to obtain light fractions from room temperature to 350 °C, middle fractions from 350 °C to 440 °C, and heavy fractions from 440 °C to 520 °C. The remaining fraction greater than 520 °C is used as the kettle residue, and the specific components are the same as in Example 1, as shown in Table 2 for details.
[0064] No catalyst is added to each component in this comparative example, and the stirring speed, reaction temperature, reaction pressure, and reaction time are the same as those in Example 1.
[0065] Add the light fraction from room temperature to 350 °C to the reaction kettle and stir for reaction. The stirring speed is 150 r / min, the reaction temperature is 170 °C, the reaction pressure is 1.6 MPa, and when the reaction time reaches 3 h, the reaction is stopped.
[0066] Add the middle fraction from 350 °C to 440 °C to the reaction kettle and stir for reaction. The stirring speed is 150 r / min, the reaction temperature is 180 °C, the reaction pressure is 1.8 MPa, and when the reaction time reaches 4 h, the reaction is stopped.
[0067] Add the fraction of 440 °C to 520 °C as a heavy fraction to the reaction kettle, introduce air during stirring, the air flow rate is 0.85 L / min, the stirring speed is 150 r / min, the reaction temperature is 240 °C, the reaction pressure is 0.5 MPa, the reaction time is 2 h, and then stop the reaction.
[0068] The reacted materials of the light fraction, middle fraction, and heavy fraction and the kettle residue greater than 520 °C are stirred and mixed in a mass ratio of 22:31:38:9. The stirring speed is 350 r / min, the stirring temperature is 175 °C, and the stirring time is 1 h to obtain a road asphalt material.
[0069] Comparative Example 2
[0070] Take 6 kg of catalytic slurry (same as in Example 1), distill it through a vacuum distillation process with a vacuum degree of 3.2 mbar, and perform cutting to obtain light components at room temperature to 350 °C, middle components at 350 °C to 440 °C, and heavy components at 440 °C to 520 °C respectively. The remaining fraction greater than 520 °C is used as the still residue, and the specific composition is the same as in Example 2, as shown in Table 2 specifically.
[0071] The catalyst is the same as in Example 2.
[0072] Add the light components at room temperature to 350 °C and the catalyst into the reaction kettle and stir for reaction. The mass ratio of the light components to the catalyst is 15:6, the stirring speed is 150 r / min, the reaction temperature is 180 °C, the reaction pressure is 1.6 MPa, and when the reaction time reaches 4 h, stop the reaction to obtain Product I.
[0073] Add the middle components at 350 °C to 440 °C and the catalyst into the reaction kettle and stir for reaction. The mass ratio of the middle components to the catalyst is 15:6, the stirring speed is 150 r / min, the reaction temperature is 190 °C, the reaction pressure is 1.8 MPa, and when the reaction time reaches 3 h, stop the reaction to obtain Product II.
[0074] Take the fraction at 440 °C to 520 °C as the heavy components and add them into the reaction kettle. During stirring, introduce air with an air flow rate of 1.0 L / min, the stirring speed is 150 r / min, the reaction temperature is 230 °C, the reaction pressure is 0.5 MPa, the reaction time is 2 h, and then stop the reaction to obtain Product III.
[0075] Stir and mix Product I, Product II, Product III, and the still residue greater than 520 °C in a mass ratio of 24:35:32:8. The stirring speed is 350 r / min, the stirring temperature is 175 °C, and the stirring time is 1 h to obtain the road asphalt material.
[0076] Comparative Example 3
[0077] Take 6 kg of catalytic slurry (same as in Example 1), distill it through a vacuum distillation process with a vacuum degree of 3.2 mbar, and perform cutting to obtain light components at room temperature to 350 °C, middle components at 350 °C to 440 °C, and heavy components at 440 °C to 520 °C respectively. The remaining fraction greater than 520 °C is used as the still residue, and the specific composition is the same as in Example 1, as shown in Table 2 specifically.
[0078] The catalyst is the same as in Example 1.
[0079] Add light components at room temperature to 350 °C and a catalyst into a reaction kettle, stir and react. The mass ratio of the light components to the catalyst is 10:3, the stirring speed is 150 r / min, the reaction temperature is 170 °C, the reaction pressure is 1.6 MPa, and the reaction time is 3 h. When the dynamic viscosity of the material at 60 °C reaches 100 Pa·s, stop the reaction to obtain Product I.
[0080] Add medium components at 350 °C to 440 °C and a catalyst into a reaction kettle, stir and react. The mass ratio of the medium components to the catalyst is 20:3, the stirring speed is 150 r / min, the reaction temperature is 180 °C, the reaction pressure is 1.8 MPa, and the reaction time is 4 h. When the dynamic viscosity of the material at 60 °C reaches 150 Pa·s, stop the reaction to obtain Product II.
[0081] Add fractions at 440 °C to 520 °C as heavy components into a reaction kettle, introduce nitrogen during stirring, the nitrogen flow rate is 0.85 L / min, the stirring speed is 150 r / min, the reaction temperature is 240 °C, the reaction pressure is 0.5 MPa, and the reaction time is 2 h. Stop the reaction to obtain Product III.
[0082] Stir and mix Product I, Product II, Product III and the kettle residue above 520 °C according to the mass ratio of 22:31:38:9, the stirring speed is 350 r / min, the stirring temperature is 175 °C, and the stirring time is 1 h to obtain a road asphalt material.
[0083] Comparative Example 4
[0084] Take 6 kg of catalytic slurry (same as in Example 1) without performing vacuum distillation process.
[0085] The catalyst is the same as in Example 1.
[0086] Add the catalytic slurry and the catalyst into a reaction kettle, stir and react. The mass ratio of the catalytic slurry to the catalyst is 10:3, the stirring speed is 150 r / min, the reaction temperature is 180 °C, the reaction pressure is 1.8 MPa, and the reaction time is 6 h. Stop the reaction to obtain a road asphalt material.
[0087] Table 1 Components and ratios after separation of catalytic slurry in each example
[0088] Material category Example 1 Example 2 Example 3 Example 4 Light component reactant / % 22 24 27 19 Medium component reactant / % 31 35 36 30 Heavy component reactant / % 38 32 31 39 Bottom residue / % 9 8 6 12
[0089] Table 2 Components and ratios after separation of catalytic slurry in each comparative example
[0090] Material category Comparative example 1 Comparative example 2 Comparative example 3 Light component reactant / % 22 24 22 Medium component reactant / % 31 35 31 Heavy component reactant / % 38 32 38 Bottom residue / % 9 8 9
[0091] The road asphalt materials prepared in Examples 1-4 and Comparative Examples 1-4 were tested with reference to some technical requirements of JTG F40-2004 "Technical Specifications for Construction of Highway Asphalt Pavements". The specific test methods and technical requirements are shown in Table 3, and the test results are shown in Tables 4 and 5.
[0092] Table 3 Technical Requirements
[0093]
[0094] Table 4 Properties of Road Asphalt Materials Obtained in Each Example
[0095]
[0096]
[0097] Table 5 Properties of Road Asphalt Materials Obtained in Each Comparative Example
[0098]
[0099] From the comparison results in Tables 4 and 5, the main indicators of Examples 1-4 all meet the requirements of Grade A of road petroleum asphalt, and are significantly better than the performance of Comparative Examples 1-4.
Claims
1. A preparation method of a road asphalt material, comprising the following steps: (1) Fractionating catalytic slurry oil to obtain four components: light fraction, middle fraction, heavy fraction, and still residue; (2) Contacting the light fraction and the middle fraction separated in step (1) with a solid strong acid catalyst respectively for reaction to obtain Product I and Product II; mixing the heavy fraction in step (1) with an oxygen-containing gas for reaction to obtain Product III; (3) Mixing the still residue component in step (1) with Product I, Product II, and Product III obtained in step (2) to obtain the road asphalt material.
2. The preparation method according to claim 1, characterized in that, In step (1), the catalytic slurry oil is the catalytic slurry oil produced by a catalytic cracking unit from natural petroleum, which is a mixture rich in aromatics; the mass content of aromatics in the catalytic slurry oil is 50% - 90%, the mass content of paraffins in the catalytic slurry oil is less than 5%, and the mass content of naphthenes is less than 15%.
3. The preparation method according to claim 1, characterized in that In step (1), the fractionation method of the catalytic slurry oil is carried out by vacuum distillation, and the vacuum degree is 2 - 5 mbar; And / or, in step (1), the cut-off point between the light fraction and the middle fraction is 340°C - 360°C, the cut-off point between the middle fraction and the heavy fraction is 430°C - 450°C, and the cut-off point between the heavy fraction and the still residue is 510°C - 530°C.
4. The preparation method according to claim 1, characterized in that In step (1), the mass content of the light fraction in the catalytic slurry oil is 18 - 29%, the mass content of the middle fraction is 28 - 38%, the mass content of the heavy fraction is 30 - 40%, and the rest is the still residue.
5. The preparation method according to claim 1, wherein In step (2), the solid strong acid catalyst is SO4 2- / ZrO2, SO4 2- / TiO2, SO4 2- / Fe2O3, SO4 2- / Fe2O3 - Al2O3, SO4 2- / MoO3 - TiO2, and is preferably SO4 2- / ZrO2.
6. The preparation method according to claim 1, wherein, In step (2), the particle size of the solid strong acid catalyst is 120 - 300 mesh.
7. The preparation method according to claim 1, characterized in that, In step (2), reacting the light fraction in step (1) under the action of the catalyst, and the mass ratio of the light fraction to the catalyst is (10 - 20):(1 - 3); And / or, in step (2), reacting the light fraction and the catalyst in step (1), the reaction is carried out during stirring, the stirring speed is 100 r / min - 200 r / min, the reaction temperature is 170°C - 190°C, the reaction pressure is 1.3 MPa - 1.8 MPa, the reaction time is 1 h - 5 h, and when the 60°C kinematic viscosity of the material reaches 80 - 120 Pa·s, the reaction is stopped to obtain Product I.
8. The preparation method according to claim 1, characterized in that, In step (2), reacting the middle fraction in step (1) under the action of the catalyst, and the mass ratio of the middle fraction to the catalyst is (10 - 20):(1 - 3); And / or, in step (2), reacting the middle fraction and the catalyst in step (1), the reaction is carried out during stirring, the stirring speed is 100 r / min - 200 r / min, the reaction temperature is 180°C - 200°C, the reaction pressure is 1.5 MPa - 2.0 MPa, the reaction time is 3 h - 5 h, and when the 60°C kinematic viscosity of the material reaches 130 - 170 Pa·s, the reaction is stopped to obtain Product II.
9. The preparation method according to claim 1, characterized in that, In step (2), the heavy components in step (1) are added to the reaction kettle, and an oxygen-containing gas is introduced during stirring. The air flow rate is 0.17 - 1.7 L / min; the stirring speed of the reaction kettle is 100 r / min - 200 r / min, the reaction temperature is 200°C - 250°C, the reaction pressure is 0.2 MPa - 0.5 MPa, and the reaction time is 1 h - 3 h. When the dynamic viscosity of the material at 60°C reaches 460 - 540 Pa·s, the reaction is stopped to obtain product III.
10. The preparation method according to claim 1, wherein, The kettle residue in step (1) is stirred and mixed with product I, product II, and product III obtained in step (3). The mass ratio of product I, product II, product III to the kettle residue is (20 - 30):(30 - 40):(30 - 45):(5 - 10). The stirring speed is 200 r / min - 500 r / min, the stirring temperature is 170°C - 200°C, and the stirring time is 1 h - 2 h to obtain the road asphalt material.
11. The road asphalt material obtained by the method for preparing a road asphalt material according to any one of claims 1 - 10.
Citation Information
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