Method for preparing mesophase pitch by reformed C9 aromatic hydrocarbon dissolved asphaltene mixed with FCC (Fluid Catalytic Cracking) oil slurry
By reforming C9 aromatics and asphaltenes through π–π conjugation and high-temperature dehydrogenation polycondensation, the dissolution and dispersion problems of asphaltenes in the preparation of mesophase asphalt were solved, resulting in the preparation of mesophase asphalt with high softening point and low quinoline insolubles, thus improving product performance.
Patent Information
- Application Number
- CN202511876019.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-12
- Publication Date
- 2026-02-06
AI Technical Summary
In the existing technology, asphaltene is difficult to fully dissolve and disperse in the preparation of mesophase asphalt, resulting in problems such as poor optical anisotropy of the product, high content of quinoline insolubles, and low softening point. In addition, traditional aromatic solvents have limited solubility and cannot achieve homogeneous reaction and dense mesophase structure.
The process involves mixing reformed C9 aromatics with asphaltene, disrupting the aggregated structure of asphaltene through π–π conjugation to form a stable homogeneous solution, which is then mixed with FCC slurry and subjected to dehydrogenation polycondensation and aromatization reactions at high temperatures to form a continuous mesophase asphalt.
It significantly improves the solubility and dispersion stability of asphalt, enhances the softening point and purity of mesophase asphalt, and reduces the content of quinoline insolubles, thus achieving efficient preparation of mesophase asphalt.
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Figure CN121471937A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of special mesophase pitch, and particularly relates to a method for preparing mesophase pitch by dissolving pitch and mixed FCC oil slurry of C9 aromatic hydrocarbons. BACKGROUND
[0002] In recent years, with the continuous increase in the production capacity of large ethylene and aromatic hydrocarbon combined devices, the production of heavy reforming C9 heavy aromatic hydrocarbons has increased significantly. There are mainly three ways for the development and utilization of heavy reforming C9 heavy aromatic hydrocarbons at home and abroad. First, the heavy aromatic hydrocarbon components are directly utilized without separation, usually sold at a low price or mixed into fuel oil. However, this method not only causes resource waste, but also pollutes the environment, and with the improvement of fuel oil emission standards, its utilization gradually decreases. Second, different components in heavy aromatic hydrocarbons are separated to extract high-value chemical products such as mesitylene, cymene, indane, methyl indane, tetramethyl benzene, diethyl benzene and naphthalene, which are then further processed into fine chemical products. Finally, the heavy aromatic hydrocarbons are subjected to lightening treatment to generate benzene, toluene, xylene and other basic petrochemical products by dealkylation, and the unconvertible by-products such as tetramethyl benzene and naphthalene are separated. The non-active components in the heavy reforming C9 heavy aromatic hydrocarbons can also be used to produce aromatic solvent oil. The aromatic solvent oil has a high boiling point and a slow evaporation speed at room temperature, and thus becomes an ideal solvent and is widely used in laboratory research, paint and coating, printing and ink and other fields.
[0003] Xinjiang crude oil is one of the important energy resources in China, with unique geological characteristics and chemical composition. Typical Xinjiang crude oil has medium to high density, medium viscosity, and contains a high proportion of asphaltene, with an average relative molecular weight usually between 1200 and 2400. Its asphaltene content is generally between 20% and 30%, which is crucial for its practical application in road construction and other building applications, because the asphaltene content directly affects the adhesion, flexibility and durability of asphalt products. These characteristics make Xinjiang crude oil have unique advantages in processing and utilization.
[0004] In the refining and chemical industry, FCC oil slurry is widely used in the preparation of mesophase pitch due to its unique chemical composition. Its gum and asphaltene components perform well in thermal processing, effectively forming a durable and excellent adhesive carbon mesophase. In addition, the high content of aromatic hydrocarbons improves the flexibility and weather resistance of the pitch, significantly improving its performance under complex environmental conditions, especially for road construction and waterproof engineering. Therefore, FCC oil slurry not only has significant characteristics in chemical composition, but also has superior performance in industrial applications, making it an important object in research and application fields.
[0005] However, the utilization effect of asphaltene in the preparation process of mesophase pitch in the prior art is not ideal. Asphaltene has high molecular weight, polycyclic aromatic structure and strong self-aggregation tendency, which is easy to form uneven structure or even coking in the heating or polycondensation process, resulting in problems such as poor optical anisotropy, high quinoline insoluble content and low softening point of the product. Due to the difficulty of fully dissolving and dispersing asphaltene, the homogeneous reaction of asphaltene and FCC oil slurry cannot be realized in the traditional process, and a dense and continuous mesophase structure is formed. Although the existing method attempts to add aromatic solvents or adjust the reaction conditions to improve the system, the solubility of the aromatic solvent is limited, and the asphaltene still has the problems of phase separation and aggregation, which restricts the further improvement of the product performance. SUMMARY
[0006] The purpose of the present application is to provide a method for preparing mesophase pitch by dissolving asphaltene in reforming C9 aromatic hydrocarbon and mixing with FCC oil slurry, which fully utilizes the solubility of reforming C9 aromatic hydrocarbon to dissolve asphaltene and prepare mesophase pitch by mixing with FCC oil slurry.
[0007] In one aspect of the present application, a method for preparing mesophase pitch by dissolving asphaltene in reforming C9 aromatic hydrocarbon and mixing with FCC oil slurry is provided. According to an embodiment of the present application, the method comprises the following steps:
[0008] (1) mixing reforming C9 aromatic hydrocarbon and asphaltene at a mass ratio of 1-10:1, and obtaining a mixed oil sample I by constant temperature mechanical stirring;
[0009] This step is the asphaltene dissolving and dispersing stage. Reforming C9 aromatic hydrocarbon has high aromaticity, and the multi-ring aromatic rings in the molecule interact with the asphaltene molecules through π-π conjugation, which destroys the original asphaltene colloidal aggregation structure, changes the asphaltene from the aggregated state to the molecular state, and forms a stable homogeneous solution, providing a good dispersion basis for the subsequent reaction.
[0010] (2) mixing the mixed oil sample I and FCC oil slurry at a mass ratio of 1-2:10, and obtaining a mixed oil sample II by constant temperature mechanical stirring and volatilizing light components;
[0011] This step is the system homogenization and light component volatilization stage. The asphaltene dissolved by reforming C9 aromatic hydrocarbon is fully mixed with the condensed ring aromatic hydrocarbon and alkyl-substituted aromatic hydrocarbon in the FCC oil slurry, and the molecular rearrangement is promoted under heating and stirring. The moderate volatilization of light aromatic components increases the viscosity and aromaticity of the system, thereby enhancing the molecular stacking and interaction, and creating a high aromaticity and high reactivity reaction environment for the formation of mesophase.
[0012] (3) heating and warming the mixed oil sample II to constant temperature mechanical stirring to obtain mesophase pitch.
[0013] This step is the polycondensation and mesophase generation stage. Under the heat treatment condition of 370-430℃, the polycyclic aromatic structure of asphaltene and FCC oil slurry in the mixed system undergoes dehydrogenation polycondensation and aromatization reaction, and larger aromatic layers are formed through C-C bond or C-H-C bridging between molecules. Continuous stirring promotes the ordered orientation of molecules and the accumulation of layers, and finally forms mesophase pitch with obvious optical anisotropy.
[0014] In addition, the method for preparing mesophase pitch by dissolving asphaltene mixed FCC oil slurry according to the above-mentioned embodiments of the present application can also have the following additional technical features:
[0015] In some embodiments of the present application, the asphaltene is extracted from Xinjiang crude oil. Xinjiang crude oil has high asphaltene content (usually up to 20-30%), high aromaticity of molecules, short alkyl side chains, and moderate content of heteroatoms (S, N, O), which makes the asphaltene have strong aromatic stacking ability and good thermal stability. Compared with crude oils in other regions, the proportion of polycyclic aromatic hydrocarbons in the structure of Xinjiang crude oil asphaltene is higher, the molecular polarity is weaker, and it is more easily depolymerized and dispersed by the reforming C9 aromatic hydrocarbon solvent, thereby significantly improving the solubility and reactivity of asphaltene in the aromatic hydrocarbon system.
[0016] In some embodiments of the present application, in step (1), the temperature of the constant-temperature mechanical stirring is 120-170℃, the stirring rate is 300-500 r / min, and the treatment time is 2-10 h. In this temperature range, the aromatic ring of the reforming C9 aromatic hydrocarbon solvent is in an activated state, can significantly interact with asphaltene molecules, and thus effectively destroy the aggregation structure of asphaltene. Below 120℃, the dissolution rate is slow and the system is not fully dispersed. Above 170℃, slight thermal cracking may be induced, resulting in structural damage. Controlling the stirring rate at 300-500 r / min can ensure that the system is fully mixed and mass transfer is uniform, preventing local deposition. A treatment time of 2-10 h can ensure that the asphaltene is fully depolymerized and dispersed, and also avoids increasing energy consumption or causing light polymerization due to long-term heating.
[0017] In some embodiments of the present application, in step (2), the temperature of the constant-temperature mechanical stirring and volatilization is 200-320℃, the stirring rate is 300-500 r / min, and the treatment time is 4-12 h. This temperature range corresponds to the boiling range of light aromatic hydrocarbons and part of alkyl aromatic hydrocarbons in the FCC oil slurry, and can effectively promote the volatilization and concentration of light components in the system. Below 200℃, the solvent volatilization rate is slow, and there is more light component remaining in the system, which can easily lead to phase separation in the subsequent reaction; above 320℃, part of the aromatic components may undergo thermal cracking or coking, affecting the stability of the product.
[0018] In this temperature range, the asphaltene molecules and the polycyclic aromatic hydrocarbons in the FCC oil slurry have enhanced π-π stacking and intermolecular attraction, and the system gradually forms a uniform high-aromaticity reaction matrix. The stirring rate is kept at 300-500 r / min to prevent local overheating and stratification and ensure uniform mass transfer; and the treatment time is 4-12 h to ensure that the light solvent completely escapes, so that the system has moderate viscosity and uniform molecular distribution.
[0019] The process realizes the transformation of asphaltene from a dissolved state to a semi-concentrated homogeneous system, providing necessary molecular structure conditions for subsequent ordered orientation and mesophase formation.
[0020] In some embodiments of the present application, in step (3), the temperature of the constant-temperature mechanical stirring is 370-430°C, the stirring rate is 300-500 r / min, and the treatment time is 8-16 h. This temperature range is in the main reaction interval of the thermal polycondensation reaction of the FCC oil slurry and asphaltene, which can promote the dehydrogenation condensation and aromatization reaction of polycyclic aromatic molecules. When the temperature is lower than 370°C, the molecular energy is insufficient, the polycondensation rate is slow, and a continuous ordered mesophase structure cannot be formed. When the temperature exceeds 430°C, the system is prone to excessive carbonization and coking, which destroys the molecular orientation. The stirring rate is maintained at 300-500 r / min to prevent local overheating and adhesion deposition, ensure uniform heating of the system, and promote the growth of aromatic lamellae. The treatment time of 8-16 h can ensure that the aromatic lamellae are fully developed and reach thermal equilibrium, so that a continuous phase of optically anisotropic regions is formed in the product. This temperature and time control causes the ordered accumulation of asphaltene and the copolymerization components of the FCC oil slurry in the system, and finally a mesophase pitch with a high softening point, a low quinoline insoluble content, and an excellent microstructure is obtained.
[0021] In another aspect of the present application, the present application proposes a mesophase pitch prepared by the method.
[0022] Compared with the prior art, the present application has the following beneficial effects:
[0023] (1) The present application extracts asphaltene from crude oil by n-heptane dissolution extraction and drying, uses reforming C9 aromatic hydrocarbons to dissolve asphaltene components, evaporates and removes reforming C9 aromatic hydrocarbons for recycling, and uses mixed FCC oil slurry to prepare mesophase pitch by thermal polycondensation. The mesophase pitch prepared by the method of the present application has the characteristics of a wide optical structure.
[0024] (2) The present application can increase the incorporation ratio of asphaltene to more than 10%, which is higher than the ≤4% of the traditional process, and significantly improves the utilization rate of asphaltene.
[0025] (3) The present application finds that reforming C9 aromatic hydrocarbons not only can be used as a solvent in the system, but also can significantly improve the solubility and dispersion stability of asphaltene, and give reforming C9 aromatic hydrocarbons a new reactive application approach.
[0026] (4) The whole process of the application is simple, efficient, low in energy consumption, small in equipment requirement, low in investment cost, and beneficial to industrialized production. BRIEF DESCRIPTION OF DRAWINGS
[0027] Figure 1 are polarizing microscope pictures of the method for preparing the mesophase pitch of Examples 1-3 and Comparative Examples 1-2 of the application, and the pictures are, in order from left to right and from top to bottom, Comparative Example 1, Comparative Example 2, Example 1, Example 2, and Example 3. DETAILED DESCRIPTION
[0028] The technical solutions in the embodiments of the application will be apparently and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all the other embodiments obtained by a person of ordinary skill in the art without creative labor fall within the protection scope of the application.
[0029] The raw oil samples used in the following examples are as follows: the reforming C9 aromatic hydrocarbons and the FCC oil slurry are by-products from an Anqing petrochemical device, and the asphaltene is extracted from Xinjiang crude oil.
[0030] The reforming C9 aromatic hydrocarbons are heavy aromatic hydrocarbon fractions separated from an Anqing petrochemical aromatic hydrocarbon combined device, the distillation range of which is 160-250 ℃, and the main components include trimethylbenzene, indane, methylindane, naphthalene and its derivatives, and the like high aromaticity components, which are dried by anhydrous sodium sulfate to remove trace amounts of water before use. The FCC oil slurry is taken from the bottom product of a catalytic cracking device of the Anqing petrochemical device. The asphaltene is extracted from Xinjiang crude oil by a n-heptane extraction method: the crude oil and n-heptane are mixed at a mass ratio of 1:20, stirred at 70 ℃ for 1 h, and then layered after standing, and the insoluble phase is obtained after suction filtration, washing, and drying to obtain the asphaltene sample.
[0031] The basic properties of the reforming C9 aromatic hydrocarbons are as follows:
[0032] Table 1 Basic properties of reforming C9 aromatic hydrocarbons
[0033]
[0034] Example 1
[0035] A method for preparing mesophase pitch by dissolving asphaltene in FCC oil slurry mixed with reforming C9 aromatic hydrocarbons, comprising the following steps:
[0036] (1) Extracting asphaltene and dissolving with reforming C9 aromatic hydrocarbons
[0037] Xinjiang crude oil and n-heptane were dissolved at a mass ratio of 1:20, stirred at a constant temperature of 70°C for 1 h. After cooling to room temperature, the upper layer residue was filtered and dried to obtain the desired asphaltene. The reforming C9 aromatic hydrocarbon was mixed with the asphaltene at a mass ratio of 4:1, the temperature was increased to 150°C, the stirring rate was 500 r / min, and constant temperature stirring was performed for 6 h to obtain a mixed oil sample one.
[0038] (2) Preparation of mesophase pitch by mixing FCC oil slurry
[0039] The mixed oil sample one was mixed with the FCC oil slurry, the temperature was increased to 300°C, the stirring rate was 500 r / min, and constant temperature stirring was performed for 4 h to obtain a mixed oil sample two.
[0040] (3) 50 g of the mixed oil sample two was placed in a high-temperature and high-pressure reaction kettle, N2 was purged for 20 min, heated to 420°C, and reacted for 600 min, the pressure in the kettle was controlled at 2 MPa, and the stirring rate was 400 r / min to obtain a mesophase pitch. As shown in FIG. 1, the proportion of reforming C9 aromatic hydrocarbon in this embodiment is higher, the depolymerization and dispersion of asphaltene are more sufficient, the uniformity of the system is better, and in the subsequent polycondensation stage, the aromatic lamellae are oriented and stacked in one direction along the heat flow and shear direction, so that the mesophase pitch formed is a fine streamline. Figure 1
[0041] Example 2
[0042] A method for preparing mesophase pitch by dissolving asphaltene and mixing FCC oil slurry with reforming C9 aromatic hydrocarbon, comprising the following steps:
[0043] (1) Extraction of asphaltene and dissolution with reforming C9 aromatic hydrocarbon
[0044] Xinjiang crude oil and n-heptane were dissolved at a mass ratio of 1:20, stirred at a constant temperature of 70°C for 1 h. After cooling to room temperature, the upper layer residue was filtered and dried to obtain the desired asphaltene. The reforming C9 aromatic hydrocarbon was mixed with the asphaltene at a mass ratio of 6:1, the temperature was increased to 150°C, the stirring rate was 500 r / min, and constant temperature stirring was performed for 6 h to obtain a mixed oil sample one.
[0045] (2) Preparation of mesophase pitch by mixing FCC oil slurry
[0046] The mixed oil sample one was mixed with the FCC oil slurry, the temperature was increased to 300°C, the stirring rate was 500 r / min, and constant temperature stirring was performed for 4 h to obtain a mixed oil sample two.
[0047] (3) 50 g of the mixed oil sample two was placed in a high-temperature and high-pressure reaction kettle, N2 was purged for 20 min, heated to 420°C, and reacted for 600 min, the pressure in the kettle was controlled at 2 MPa, and the stirring rate was 400 r / min to obtain a mesophase pitch. As shown in FIG. 1, the proportion of reforming C9 aromatic hydrocarbon in this embodiment is higher, the depolymerization and dispersion of asphaltene are more sufficient, the uniformity of the system is better, and in the subsequent polycondensation stage, the aromatic lamellae are oriented and stacked in one direction along the heat flow and shear direction, so that the mesophase pitch formed is a fine streamline. Figure 1 As shown, this is because the ratio of reformed C9 aromatics to asphaltenes in this embodiment is at the optimal level, and the solubility and viscosity of the system are in the equilibrium range, resulting in multiple competing orientation domains growing in parallel during the polycondensation orientation process, ultimately forming an anisotropic phase structure with a larger scale and wider region, and the resulting mesophase asphalt is of the wide watershed type.
[0048] Example 3
[0049] A method for preparing mesophase asphalt from reformed C9 aromatic dissolved asphalt mixtures using FCC slurry includes the following steps:
[0050] (1) Extracting asphalt and dissolving it using reformed C9 aromatics
[0051] Xinjiang crude oil was dissolved with n-heptane at a mass ratio of 1:20 and stirred at a constant temperature of 70℃ for 1 hour. After cooling to room temperature, the mixture was filtered, and the upper residue was dried to obtain the desired asphaltene. Reformed C9 aromatics were mixed with asphaltene at a mass ratio of 8:1, heated to 150℃, stirred at a stirring rate of 500 r / min, and stirred at a constant temperature for 6 hours to obtain mixed oil sample one.
[0052] (2) Preparation of mesophase asphalt by mixing FCC slurry
[0053] Mixed oil sample one with FCC oil slurry, heated to 300℃, stirred at a speed of 500r / min, and stirred at a constant temperature for 4h to obtain mixed oil sample two.
[0054] (3) Place 50g of mixed oil sample 2 into a high-temperature and high-pressure reactor, purge with N2 for 20 minutes, then heat to 420℃ and react for 600 minutes. Control the pressure inside the reactor to 2 MPa and the stirring rate to 400 r / min to obtain mesophase asphalt. Figure 1 As shown, because the proportion of reformed C9 aromatics is further increased in this embodiment, the system already has extremely high homogeneity and low initial viscosity before polycondensation, which enables the aromatic sheets to obtain higher orientation driving force and spatial constraint during the polycondensation stage, thereby preferentially forming fine streamlined mesophase pitch.
[0055] Comparative Example 1
[0056] A method for preparing mesophase asphalt from asphalt-based FCC slurry includes the following steps:
[0057] (1) Extraction of asphalt
[0058] Xinjiang crude oil was dissolved in n-heptane at a mass ratio of 1:20, and stirred at a constant temperature of 70℃ for 1 hour. After cooling to room temperature, the mixture was filtered, and the upper residue was dried to obtain the desired asphaltene.
[0059] (2) Preparation of mesophase asphalt by mixing FCC slurry
[0060] The asphalt obtained in step (1) was mixed with FCC slurry at a mass ratio of 1:19, heated to 300℃, stirred at a stirring rate of 500r / min, and stirred at a constant temperature for 4h to obtain a mixed oil sample.
[0061] (3) Place 50g of the mixed oil sample in a high-temperature and high-pressure reactor, purge with N2 for 20min, then heat to 420℃ and react for 360min. Control the pressure inside the reactor to 2MPa and the stirring rate to 400r / min to obtain mesophase asphalt. Figure 1 As shown, since reformed C9 aromatics were not used to pre-dissolve and disperse the asphaltene in this comparative example, the asphaltene could not form a homogeneous system in the FCC slurry. During thermal polycondensation, early local coking and non-uniform orientation occurred, and only isolated and dispersed anisotropic small phase domains could be generated, which ultimately showed a mosaic-like structure, accompanied by some unreacted oil sample residue.
[0062] Comparative Example 2
[0063] A method for preparing mesophase bitumen from FCC slurry includes the following steps:
[0064] 50g of FCC slurry was placed in a high-temperature, high-pressure reactor. After purging with N2 for 20 minutes, the mixture was heated to 420℃ and reacted for 360 minutes. The pressure inside the reactor was controlled at 2 MPa, and the stirring rate was 400 r / min to obtain mesophase asphalt. Figure 1 As shown, since the system in this comparative example is composed only of FCC oil slurry, it lacks the participation of aromatic solvents that can uniformly depolymerize and disperse asphaltenes. The condensation reaction only occurs in the locally enriched active aromatic ring regions. The anisotropic phase grows in an isolated nucleation manner rather than co-expanding, eventually forming a dispersed spherical mesophase structure, which cannot develop into a continuous strip-shaped or wide-area structure.
[0065] The softening point, quinoline insolubles, and elemental analysis of the mesophase pitches prepared in each embodiment and comparative example were performed using the following methods:
[0066] (1) Softening point (SP): Determined by ring and ball method according to Chinese national standard GB / T4507-2014. The heating medium used is glycerol, which can test the softening point of 30~150 ℃. The sample is first ground and then melted. Two copper sample rings are preheated and placed on a metal plate coated with glycerol. Sufficient molten sample is filled into the sample rings with a little excess. The excess is then scraped off with a hot scraper until it is flush with the surface of the metal ring. The sample rings and metal balls are then placed on a softening point tester that has been preheated to 32 ℃ in an oil bath beaker. Stirring is then turned on and the temperature is gradually increased, with the temperature rising by about 5 ℃ every 3 min. The temperature of the softened metal ball when it falls to the bottom plate is recorded. The difference between two parallel tests is considered successful if it is within 2 ℃. The average value is taken as the softening point of the sample.
[0067] (2) Quinoline insolubles (QI): The content of quinoline insolubles of the product is detected according to the Chinese national standard GB / T 2293-2019. The whole operation process is performed according to the specification, and about 0.5 g of sample is placed into a filter containing diatomite, and the sample is filtered and washed with hot quinoline, hot toluene and acetone in sequence for multiple times. After drying, the overall weight change is compared, and the mass percentage of quinoline insolubles is calculated by the following formula:
[0068]
[0069] In the formula, G2 is the total mass of quinoline insolubles, diatomite and filter, G1 is the mass of diatomite and filter, and G is the mass of sample.
[0070] (3) Elemental analysis: The content of C, H, S, N and O elements of the raw material is determined by using a VARIO EL CUBE type elemental analyzer produced by Germany ELEMENTAR.
[0071] The specific results are shown in Table 2.
[0072] Table 2 Performance table of mesophase pitch prepared in Examples 1-3 and Comparative Examples 1-2
[0073]
[0074] Comparative analysis of Examples 1-3 and Comparative Examples 1 and 2 shows that the mesophase pitch prepared by the method of the present application has significant advantages in softening point, quinoline insoluble (QI) content and impurity level. Specifically, the softening points of the samples of Examples 1-3 are 117℃, 133℃ and 159℃, respectively, which are significantly higher than those of Comparative Example 1 (98℃) and Comparative Example 2 (141℃), indicating that the molecular polycondensation degree of the mesophase pitch obtained by the method of the present application is higher, and the aromatic lamellar structure is more ordered. At the same time, the QI content of the examples is significantly reduced (1.04%-2.57%), compared with 5.84% of Comparative Example 1 and 2.69% of Comparative Example 2, and the impurity content is reduced by more than 60%, indicating that the asphaltene in the system is fully dispersed and homogeneously reacted.
[0075] From the elemental analysis results, the S and N contents of the sample of the example are significantly lower than those of the comparative example, indicating that the present application effectively reduces the retention rate of heteroatoms in the thermal reaction through the synergistic process of C9⁺ aromatic hydrocarbon dissolution-mixing-polycondensation, and improves the product purity.
[0076] In summary, the present application realizes uniform dispersion and ordered polymerization of asphaltene molecules by the three-step method of reforming C9 aromatic hydrocarbon to dissolve asphaltene and synergistically reacting with FCC oil slurry, and the obtained mesophase pitch has higher softening point, lower QI content and better element composition, which is significantly better than the prior art.
[0077] The above merely illustrates and explains the present application, and those skilled in the art can make various modifications or supplements to the described specific embodiments or use similar ways to replace, as long as the modifications or supplements do not deviate from the structure of the present application or exceed the scope defined by the present claims, and should belong to the protection scope of the present application.
Claims
1. A method for preparing mesophase asphalt from reformed C9 aromatics-dissolved asphalt mixtures using FCC slurry, characterized in that, Includes the following steps: (1) Mix reformed C9 aromatics and asphalt at a mass ratio of 10:1 to 1 and mechanically stir at a constant temperature to obtain mixed oil sample one; (2) Mix the mixed oil sample one with the FCC oil slurry at a mass ratio of 1 to 2:10, stir mechanically at a constant temperature and volatilize the light components to obtain the mixed oil sample two; (3) Heat the mixed oil sample two to a constant temperature and mechanically stir to obtain mesophase asphalt.
2. The method for preparing mesophase asphalt from reformed C9 aromatics dissolved asphalt mixed with FCC slurry according to claim 1, characterized in that: The asphaltene was extracted from crude oil in Xinjiang.
3. The method for preparing mesophase asphalt from reformed C9 aromatics-dissolved asphalt mixtures using FCC slurry, as described in claim 1, is characterized in that: In step (1), the temperature of the constant temperature mechanical stirring is 120-170℃, the stirring rate is 300-500r / min, and the processing time is 2-10h.
4. The method for preparing mesophase asphalt from reformed C9 aromatics dissolved asphalt mixed with FCC slurry according to claim 1, characterized in that: In step (2), the temperature for constant temperature mechanical stirring and volatilization is 200-320℃, the stirring rate is 300-500r / min, and the treatment time is 4-12h.
5. The method for preparing mesophase asphalt from reformed C9 aromatics dissolved asphalt mixed with FCC slurry according to claim 1, characterized in that: In step (3), the temperature of the constant temperature mechanical stirring is 370-430℃, the stirring rate is 300-500 r / min, and the processing time is 8-16h.
6. An mesophase pitch prepared by the method of any one of claims 1-5.