System and process for co-producing petroleum purified asphalt and high-softening-point special asphalt
By using a combined production system and multi-step reaction, the problems of large fixed asset investment and unstable quality caused by different properties of asphalt products in existing technologies have been solved, and the stable preparation and large-scale production of high-quality asphalt have been achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- PETROCHINA CO LTD
- Filing Date
- 2024-10-29
- Publication Date
- 2026-05-01
AI Technical Summary
Existing technologies are insufficient for the simultaneous and efficient preparation of multiple asphalt products with different properties, resulting in large fixed asset investments, unstable product quality, and difficulty in achieving large-scale production.
A combined production system is adopted, including a first raw material tank, a second raw material tank, a modifier storage tank, a mixing tank, a heat exchanger, a distillation device, a heating device, multiple reactors and a vacuum device, to prepare high softening point homogeneous asphalt and mesophase asphalt through a multi-step reaction and separation process.
It has enabled the preparation of a variety of high-quality and stable asphalt products, meeting the material performance requirements in the fields of mechanics and electrochemistry, reducing production costs and improving the operability of large-scale production.
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Figure CN121950355A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a system and process for co-producing petroleum-purified bitumen and high-softening-point specialty bitumen, belonging to the field of carbon materials technology. Background Technology
[0002] Graphite electrodes, isostatic graphite, and various coarse and fine-structure graphite products all require pitch with low impurity content, sufficient carbon content, and suitable fluidity and molecular weight distribution as impregnating agents and binders. Generally, coal tar pitch and heavy petroleum oil are used as raw materials, and the inorganic and organic impurities are removed, and the degree of polymerization of aromatic molecules and the content of light components are controlled to obtain the pitch used as an impregnating agent and binder. The preparation of artificial graphite materials and special carbons also requires purified pitch with very low impurity content, especially pitch with a softening point above 150℃, to achieve high yields, structural strength, and electrochemical performance in subsequent carbonization and graphitization processes. High-performance pitch-based carbon fibers must be prepared using high-quality mesophase pitch as raw material. The mesophase content, aggregate morphology, molecular weight distribution, rheological properties, and impurity content in the pitch must all be controlled at very high levels and be highly stable. Although many research institutions and laboratories have conducted extensive work, it is still currently at the laboratory and pilot-scale levels. General-purpose pitch-based carbon fiber uses high-softening-point homopolymer pitch as raw material. This pitch can be formulated from coal-based or oil-based heavy oil. Unlike the regular arrangement of layered polycyclic aromatic hydrocarbon macromolecules in mesophase pitch, the polycyclic aromatic hydrocarbon molecules in homopolymer pitch retain more alkyl side chains or have poor planarity of the aromatic ring system. Therefore, the reaction processes and preparation technologies of mesophase pitch and homopolymer pitch differ significantly, and existing research and production facilities cannot simultaneously address both. Given the common requirements of various impregnating agent pitches, binder pitches, mesophase pitches, and homopolymer pitches for raw materials, the reaction process all involves dehydrogenation polymerization between aromatic molecules to increase molecular weight and size, while simultaneously requiring the removal of a certain amount of light components from intermediate products. Therefore, in principle, it is possible to design process technologies that meet the needs of multiple products, achieving co-production of multiple products, reducing production costs, and thus enabling the large-scale utilization of these currently high-priced products.
[0003] CN114410331A uses aromatic-rich heavy oil as feedstock. Preheated fresh feedstock is mixed with nitrogen and introduced from the top of a variable-temperature, variable-diameter tubular reactor, passing rapidly through the reactor to obtain an asphalt-like intermediate product with a softening point of 40-160℃. This product then enters a hot low-temperature separator, where nitrogen and some light components are separated from the top. The bottom product enters a scraped-film evaporator to remove and recover the light components, while the heavy components obtained at the bottom of the evaporator enter a mesophase storage tank, thus yielding high-quality spinnable mesophase asphalt. However, in this prior art, the asphalt-like intermediate product obtained from feedstock entering from the top of the reactor is prone to contain large-molecular-weight condensation polymers, affecting the optimal molecular weight distribution of the mesophase asphalt. When the degree of reaction in the tubular reactor is low, the product yield obtained through scraped-film evaporation is low.
[0004] CN115161054A describes a process where ethylene tar is distilled in two stages to obtain heavy components. These heavy components are then subjected to thermal polymerization in a two-stage reactor, during which the pH and sulfur content are adjusted. Short-path molecular distillation is then performed, followed by filtration and granulation to obtain high softening point asphalt. However, this existing technology uses ammonium phosphate in the reaction process, which is difficult to disperse in the oil-based molecular system, thus affecting the uniformity of the reaction products and increasing raw material costs.
[0005] CN113621397A first adds coumarone-indene resin to ethylene tar or petroleum-based pitch to obtain a formulation solution. Then, the formulation solution is mixed with coal tar pitch with a softening point of 30-90℃ to obtain a mixed pitch. The mixed pitch is then oxidized at 320-340℃ to obtain environmentally friendly high-softening-point pitch. However, this prior art uses a formulation solution with significantly different thermal reactivity of aromatic molecules from different sources, increasing the difficulty of reaction control. Furthermore, it cannot be used for the design and production of multiple product solutions.
[0006] CN114479895A uses catalytic or thermal cracked coal tar, FCC slurry clarified oil, reduced-pressure fourth fraction, deasphalted naphthenic vacuum residue, de-QI refined coal tar, and anthracene oil as raw materials. It utilizes a centrifugal reaction separation device, alternating between vertical and inclined rotation of the reaction sleeve 2-3 times to achieve uniform heating and polycondensation of the raw materials within the sleeve, and enrichment of the mesophase product in the lower part of the sleeve. By coordinating the opening and closing of valves at the bottom of the sleeve and the bottom of the device cavity, and by adjusting the molecular weight of the product using a flash evaporator, mesophase pitch and spinnable isotropic pitch can be obtained separately. However, in this prior art, because the density difference between mesophase pitch (softening point greater than 200℃) and isotropic pitch is small, high-speed centrifugation cannot completely separate these two different types of pitch. This operation is suitable for small-batch laboratory preparation, but industrial-scale production is extremely difficult.
[0007] Analysis of the existing technology information reveals two main problems: First, existing technologies and processes are all for single-product production. Different properties and structures of asphalt require different process equipment, resulting in large fixed asset investments. Furthermore, the complex composition of raw materials leads to poor controllability in the subsequent asphalt preparation process, resulting in inconsistent product quality and unstable quality during long-term operation. Second, these technologies are suitable for small-batch laboratory preparation, but their operability decreases and equipment limitations increase when scaling up. Therefore, developing technologies that achieve both low cost and high quality through reactor design and process flow optimization, based on the properties and market size differences of various asphalt products, is the most effective way to solve these industry problems. Summary of the Invention
[0008] To address the aforementioned shortcomings and deficiencies, the present invention aims to provide a system and process for the co-production of petroleum-purified bitumen and high-softening-point specialty bitumen. This invention utilizes a single system to prepare high-softening-point homogeneous bitumen and mesophase bitumen with excellent performance and stable quality, meeting the material performance requirements of various mechanical and electrochemical fields.
[0009] To achieve the above objectives, on the one hand, the present invention provides a system for co-producing petroleum purified asphalt and high softening point special asphalt, wherein the system for co-producing petroleum purified asphalt and high softening point special asphalt includes: a first raw material tank, a second raw material tank, a modifier storage tank, a mixing tank, a heat exchanger, a distillation device, a first gas source, a heating device, a first reactor, a second reactor, a third reactor, and a second gas source;
[0010] The second raw material tank and the conditioning agent storage tank are connected to the mixing tank through pipelines. The first outlet of the first raw material tank and the outlet of the mixing tank are connected to the inlet of the distillation unit through pipelines via a three-way valve or a mixing device. The outlet of the distillation unit for aromatic basic components is connected to the inlet of the first reactor through pipelines via a heating device. The first gas source is connected to the heating device through pipelines. The outlet of the first reactor is connected to the inlet of the second reactor through pipelines. The outlet of the second reactor and the outlet of the second gas source are connected to the inlet of the third reactor through pipelines.
[0011] The second outlet of the first raw material tank is connected to the inlet of the first reactor via a pipeline through a heating device. A first valve and a second valve are respectively installed on the pipeline between the first outlet of the first raw material tank and the three-way valve or the mixing device, and on the pipeline between the second outlet of the first raw material tank and the heating device.
[0012] In one specific embodiment of the system described above, the system further includes a third raw material tank and a first filter device, wherein the third raw material tank is connected to the inlet of the first raw material tank via a pipeline through the first filter device.
[0013] As a specific embodiment of the system described above in this invention, the system further includes a first vacuum device and a second vacuum device. The high-temperature oil and gas outlets of the distillation device and the first reactor are respectively connected to the first vacuum device via pipelines, and the high-temperature oil and gas outlets of the second reactor and the third reactor are respectively connected to the second vacuum device via pipelines. The first vacuum device includes a first oil and gas buffer tank, a first condenser, a first cryogenic cooler, and a first vacuum unit connected in sequence via pipelines. The second vacuum device includes a second oil and gas buffer tank, a second condenser, a second cryogenic cooler, and a second vacuum unit connected in sequence via pipelines.
[0014] In one specific embodiment of the system described above, the outlet of the mixing tank is also connected to the second vacuum device via a pipeline, so as to recover the naturally volatile petroleum components in the mixing tank through the second vacuum device and avoid safety problems such as explosions.
[0015] As a specific embodiment of the system described above in this invention, the system further includes a first asphalt buffer tank and a second asphalt buffer tank. The outlet of the first reactor is connected to the inlet of the second reactor via a pipeline through the first asphalt buffer tank, and the outlet of the second reactor is connected to the inlet of the third reactor via a pipeline through the second asphalt buffer tank.
[0016] As a specific embodiment of the system described above in this invention, the heating device may be, for example, a tubular furnace.
[0017] In one specific embodiment of the system described above in this invention, the second reactor is a heated reactor equipped with a turbine-type stirring paddle.
[0018] In one specific embodiment of the system described above, the bottom outlet of the second reactor is designed as a conical outlet. In some specific embodiments of the present invention, the taper can be, for example, 1:2.
[0019] In one specific embodiment of the system described above in this invention, the third reactor is provided with a wall-scraping frame agitator and a bottom agitator, and the outlet of the second gas source is also connected to the bottom agitator via a pipeline.
[0020] In one specific embodiment of the system described above, the outlet of the third reactor is connected to a cooling and collecting device via a heat tracing pipeline. An external magnetic strip is installed outside the heat tracing pipeline, and a second filter device is installed inside the heat tracing pipeline between the external magnetic strip and the cooling and collecting device. In some embodiments of the present invention, the second filter device may be, for example, a ceramic filter screen.
[0021] On the other hand, the present invention also provides a process for co-producing purified bitumen and homogeneous bitumen, wherein the process is implemented using the system described above and includes:
[0022] Step (1): Filter the first aromatic raw material to obtain aromatic raw material 1*, mix the second aromatic raw material and the modifier to obtain aromatic raw material 2*, mix aromatic raw material 1* and aromatic raw material 2* to obtain mixed aromatic oil, heat the mixed aromatic oil and then perform component adjustment and further impurity removal in a distillation device to obtain the basic aromatic components.
[0023] Step (2): The aromatic basic components and crosslinking gas are heated and then introduced into the first reactor to react, thereby obtaining purified basic asphalt;
[0024] Step (3): The purified base asphalt is introduced into the second reactor for reaction to obtain a high softening point homogeneous asphalt product;
[0025] Step (4): After mixing the high softening point homogeneous asphalt product with inert gas, the mixture is introduced into the third reactor. The high softening point homogeneous asphalt product undergoes deep reaction and molecular weight adjustment in the third reactor to obtain ultra-high softening point homogeneous asphalt.
[0026] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, the process further includes step (5): using a first vacuum device to sequentially heat and separate, condense and separate and cryogenically treat the high-temperature oil and gas generated by the distillation device in step (1) and the first reactor in step (2), and using a second vacuum device to sequentially heat and separate, condense and separate and cryogenically treat the high-temperature oil and gas generated by the second reactor in step (3) and the third reactor in step (4);
[0027] The temperatures of the heating separation, the condensation separation, and the cryogenic treatment are 190-220℃, 2-10℃, and -40 to -30℃, respectively; the pressure of the first vacuum system is 30-50KPa; and the pressure of the second vacuum device is 1-10Pa.
[0028] As a specific embodiment of the process described above in this invention, the first vacuum device includes a first oil-gas buffer tank, a first condenser, a first cryogenic device, and a first vacuum unit connected in sequence. During operation, the high-temperature oil and gas (medium-grade aromatic oil and light oil and gas) generated by the distillation device in step (1) and the first reactor in step (2) first enter the first oil-gas buffer tank to separate the medium-grade aromatic oil, and then pass through the first condenser to separate the light oil. The density (20°C) of the medium-grade aromatic oil is 0.79-0.82 g / cm³. 3 Non-condensable vapor enters the first cryogenic cooler for cooling.
[0029] In some embodiments of the present invention, the condensing medium in the first condenser may be cooling water, and the cooling medium in the first cryogenic reactor may be a mixture of water and ethylene glycol.
[0030] As a specific embodiment of the process described above in this invention, the second vacuum device includes a second oil-gas buffer tank, a second condenser, a second cryogenic reactor, and a second vacuum unit connected in sequence; during operation, the high-temperature oil and gas (heavy aromatic oil and oil and gas) generated by the second reactor in step (3) and the third reactor in step (4) first enter the second oil-gas buffer tank to separate the heavy aromatic oil, which has a density of 0.82-0.88 g / cm³. 3 The medium-grade aromatic oil is then separated in a second condenser, and the non-condensable vapor enters a second cryogenic cooler for further cooling. In some embodiments of the present invention, the condensing medium in the second condenser may be cooling water, and the cooling medium in the second cryogenic cooler may be a mixture of water and ethylene glycol.
[0031] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, the first aromatic feedstock includes one or a combination of several of the following: catalytic cracking slurry oil or its distillate oil, catalytic cycle oil or its distillate oil, solvent-de-oiled asphalt or its distillate oil, and thermal cracking residue oil or its distillate oil.
[0032] The second aromatic feedstock includes one or a combination of several of the following: ethylene tar or its distillate oil, hydrogenated ethylene tar wax oil or its distillate oil, coking wax oil or its distillate oil, furfural extract oil or its distillate oil, and deasphalted vacuum residue oil or its distillate oil.
[0033] In the process described above in this invention, the catalytic cracking slurry oil used as the first aromatic feedstock refers to the oil product obtained through a catalytic cracking unit. The feedstock processed by this catalytic cracking unit is heavy distillate oil obtained from processing naphthenic crude oil, or heavy distillate oil obtained from processing paraffinic and / or intermediate-based crude oil. The distillate oil used as the first or second aromatic feedstock refers to a portion (partial component) of the oil obtained through distillation from catalytic cracking slurry oil, catalytic cycle oil, solvent-de-oiled asphalt from residue oil, thermal cracking residue, ethylene tar, hydrogenated wax oil from ethylene tar, and de-asphalted oil from vacuum residue. For example, some catalytic cracking slurries contain lighter components; in actual operation, these lighter components are removed through processing, retaining only the heavier fractions.
[0034] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, the total aromatic hydrocarbon content in the second aromatic hydrocarbon feedstock is 70-90%, wherein, based on the total weight of the total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons, and aromatic hydrocarbons with more than five rings are 1-5%, 25-35%, 50-60%, and 10-20%, respectively.
[0035] The total aromatic hydrocarbon content in the aromatic raw material 1* is 60-80%, wherein, based on the total weight of the total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons, and aromatic hydrocarbons with more than five rings are 10-20%, 60-70%, 10-20%, and 5-10%, respectively.
[0036] In one specific embodiment of the process for co-producing purified bitumen and homogeneous bitumen described above in this invention, the ash content of the second aromatic feedstock is less than 10 ppm, and its density at 20°C is 1.10-1.25 g / cm³. 3 The total aromatic hydrocarbon content is 70-90%, of which, based on the total weight of total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings are 1-5%, 25-35%, 50-60% and 10-20%, respectively. The distillation range is 350-580℃, the sulfur content is 0.05-0.2% and the nitrogen content is 0.01-0.1%. The ash content, total aromatic hydrocarbon content, sulfur content and nitrogen content are all calculated based on the total weight of the second aromatic hydrocarbon feedstock.
[0037] The ash content of the aromatic feedstock 1* is less than 50 ppm, preferably less than 20 ppm, more preferably less than 5 ppm, and its density at 20°C is 1.01-1.12 g / cm³. 3The total aromatic hydrocarbon content is 60-80%, of which, based on the total weight of total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings are 10-20%, 60-70%, 10-20% and 5-10%, respectively. The distillation range of aromatic hydrocarbon feedstock 1* is 350-580℃, the sulfur content is 0.1-0.3% and the nitrogen content is 0.05-0.2%. The ash content, total aromatic hydrocarbon content, sulfur content and nitrogen content are all calculated based on the total weight of aromatic hydrocarbon feedstock 1*.
[0038] In step (1) of the process described above in this invention, the purpose of filtering the first aromatic raw material is to remove solid particles. The filtration process has virtually no effect on parameters such as the ash content, total aromatic content, and content of tricyclic aromatics, tetracyclic aromatics, pentacyclic aromatics, and aromatics with more than five rings in the first aromatic raw material. Therefore, it can be considered that the parameters of the first aromatic raw material and the aromatic raw material 1* are basically the same.
[0039] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), the second aromatic raw material and the modifier are mixed at a weight ratio of 1000:1-10, the mixing temperature is 30-40℃, the time is 0.5-1h, the mixing method is stirring, and the stirring speed is 800-900r / min.
[0040] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), the modifier is a quinone compound, including 9,10-anthraquinone and / or 1,4-naphthoquinone. This invention, by introducing a modifier, can better control the degree of reaction in the crosslinking process, the linkage mode of aromatic molecules, and the molecular spatial configuration, thereby being more conducive to the generation and quality control of high softening point homogeneous asphalt products.
[0041] In step (1) of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, the mixing ratio of aromatic feedstock 1* and aromatic feedstock 2* is adjusted according to the requirements of the target product properties. As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), aromatic feedstock 1* and aromatic feedstock 2* are mixed at a weight ratio of 1-3:10. The mixing method includes online mixing and / or stirring mixing, preferably online mixing. The mixing temperature is 100-150℃ and the linear velocity is 0.3-0.5m / s.
[0042] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), the mixed aromatic oil is heated and then subjected to component adjustment and further impurity removal in a distillation apparatus to obtain the basic aromatic components. The distillation apparatus has 1-5 side-stream outlets and an aromatic basic component outlet arranged sequentially from top to bottom on its sidewall. The first side-stream outlet yields light aromatic oil with a density (20°C) of 0.71-0.78 g / cm³. 3 Medium-quality aromatic oil was extracted from the second to the fifth side production line, with a density (20℃) of 0.79-0.82 g / cm³. 3 High-temperature oil and gas are extracted from the top of the distillation apparatus.
[0043] As a specific embodiment of the process for co-producing purified bitumen and homogeneous bitumen described above in this invention, in step (1), the distillation device may be, for example, a fractionation tower.
[0044] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), the heating equipment used to heat the mixed aromatic oil is a heat exchanger, and the medium is saturated steam, heat transfer oil or molten salt. It is preferred to use heat transfer oil for heating, and the temperature of the heat transfer oil is 250-350℃, more preferably 270-320℃, and more preferably 280-310℃. The temperature of the mixed aromatic oil after heating is 290-300℃.
[0045] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (1), the distillation device is operated under normal pressure or reduced pressure, preferably under reduced pressure, with a pressure of 30-50 kPa, an upper temperature of 120-150°C, a lower temperature of 360-380°C, and aromatic basic components are extracted from the lower part.
[0046] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (2), the crosslinking gas and aromatic basic components are mixed at a gas flow rate to aromatic basic component weight ratio of 1-5:100 and then heated to 310-350℃, wherein the gas flow rate is in L / min and the aromatic basic component weight is in kg.
[0047] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (2), the heating device used for heating is a tubular furnace. The specific operation steps of the mixing process include injecting crosslinking gas into the furnace tubes of the tubular furnace and mixing it with the passing aromatic basic components. The outlet temperature of the tubular furnace is 310-350℃. The purpose of injecting the crosslinking gas is to increase the linear velocity, and the crosslinking gas also participates in the chemical reaction carried out in the first reactor. During the reaction, the O element of the crosslinking gas connects the two aromatic components to form a linked structure. In the process described above in this invention, the crosslinking gas includes, but is not limited to, air and / or water vapor.
[0048] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (2), the internal temperature of the first reactor is 310-350℃ and the reaction residence time is 5-10h.
[0049] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (2), the properties of the purified base asphalt are: softening point 100-120℃, coking value 20-30%, quinoline insoluble content 0% and ash content 0.001-0.003%, wherein the contents are all weight percentages calculated based on the total weight of the purified base asphalt.
[0050] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (3), the internal temperature of the second reactor is 330-360℃ and the reaction residence time is 5-10h.
[0051] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (3), the reaction in the second reactor is carried out under stirring conditions, wherein the stirring speed is 100-150 r / min.
[0052] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (3), the properties of the obtained high softening point homogeneous asphalt product are: softening point 180-250℃, coking value 45-70%, quinoline insoluble content 0.1-0.5%, and ash content 0.001-0.004%, wherein the contents are all weight percentages calculated based on the total weight of the high softening point homogeneous asphalt product.
[0053] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), inert gas and high softening point homogeneous asphalt product are mixed at a gas flow rate to high softening point homogeneous asphalt product weight ratio of 1-5:100, wherein the gas flow rate is in L / min and the weight of high softening point homogeneous asphalt product is in kg. Preferably, the pipeline between the outlet of the second reactor and the inlet of the third reactor is an insulated conveying pipeline, and nitrogen is injected into the insulated conveying pipeline. In some embodiments of this invention, the inert gas includes nitrogen, etc. In step (4), the high softening point homogeneous asphalt product and inert gas are mixed and then introduced into the third reactor. The use of inert gas can promote the departure of small molecular weight components from the reaction system, concentrate the molecular weight and retain large molecular weight components, thereby obtaining a product with a narrow molecular weight distribution; in addition, inert gas can also promote the smooth entry of asphalt in the pipeline into the third reactor, so as to avoid the problem of blockage at the inlet of the third reactor due to slow flow rate.
[0054] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), the high softening point homogeneous asphalt product discharged from the outlet of the second reactor enters the second asphalt buffer tank at a temperature of 310-330°C, and the inert gas and the high softening point homogeneous asphalt product are mixed at a gas flow rate to high softening point homogeneous asphalt product weight ratio of 1-5:100.
[0055] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), the third reactor is a dual-stirring and heating reactor equipped with a scraper-frame agitator and a bottom agitator. The stirring speed of the scraper-frame agitator is 50-100 r / min, the stirring speed of the bottom agitator is 100-150 r / min, the ratio of the diameter of the bottom agitator to the diameter of the third reactor is 1-2:5, and nitrogen gas is introduced into the third reactor from the bottom of the bottom agitator. The ratio of the nitrogen flow rate to the asphalt in the third reactor is 1-5 L / min:100 kg. In this way, the introduction of inert gases such as nitrogen into the third reactor from the bottom of the bottom agitator allows for more thorough contact between the inert gases and the reactants, thereby carrying away the decomposed light components from the reactant system.
[0056] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), after the reaction is completed, the ultra-high softening point homogeneous asphalt formed by the deep reaction is discharged from the outlet of the third reactor. A heat tracing pipeline is connected to the outlet of the third reactor, with a heat tracing temperature of 330-350℃. An external magnetic strip installed outside the heat tracing pipeline can generate a magnetic field perpendicular to the heat tracing pipeline, with a magnetic field strength of 0.5-1T, which can be activated as needed. A second filter device is provided at the lower part of the heat tracing pipeline, preferably a ceramic filter screen (more preferably an insertable ceramic filter screen with a mesh size of 200-300 mesh, selected as needed). Finally, after cooling and collection, the ultra-high softening point homogeneous asphalt product is obtained. In some embodiments of this invention, the heat tracing of the heat tracing pipeline can be achieved by setting a heat tracing device at the outlet of the third reactor.
[0057] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), the internal temperature of the third reactor is 350-380℃ and the reaction residence time is 5-10h.
[0058] As a specific embodiment of the process for co-producing purified asphalt and homogeneous asphalt described above in this invention, in step (4), the properties of the obtained ultra-high softening point homogeneous asphalt are: softening point 275-285℃, coking value 72-80%, quinoline insoluble content 0.2-1%, ash content 0.002-0.005%, and yield 35-45% (calculated based on the total weight of the starting aromatic raw materials).
[0059] In the process of co-producing purified asphalt and homogeneous asphalt described above in this invention, the aromatic basic components are first cross-linked to obtain purified basic asphalt with suitable molecular weight and reasonable component distribution. Then, the purified basic asphalt is thermally polymerized a second time to obtain homogeneous asphalt with increased molecular weight. Finally, the homogeneous asphalt with high softening point is subjected to deep reaction and molecular weight adjustment to form homogeneous asphalt with ultra-high softening point.
[0060] In the process of co-producing purified bitumen and homogeneous bitumen described above in this invention, the high softening point homogeneous bitumen can be used as a binder for graphite electrodes or as a coating and granulating agent for lithium battery anode materials, and the ultra-high softening point homogeneous bitumen can be used for general-purpose carbon fibers.
[0061] In another aspect, the present invention also provides a process for co-producing base asphalt and mesophase asphalt, wherein the process is also implemented using the system described above, and includes:
[0062] Step 1): Filter the first aromatic raw material to obtain aromatic raw material 1*, heat the aromatic raw material 1* and let it enter the first reactor to react and obtain the base asphalt;
[0063] Step 2): The base asphalt is fed into the second reactor to react and generate mesophase components, resulting in mesophase asphalt with a low softening point.
[0064] Step 3): Mix the low-softening-point mesophase pitch with an inert gas and then introduce it into the third reactor. The low-softening-point mesophase pitch undergoes a deep reaction in the third reactor to obtain high-quality spinnable mesophase pitch.
[0065] As a specific embodiment of the process for co-producing basic asphalt and mesophase asphalt described above in this invention, in step 1), the first aromatic feedstock includes one or a combination of several of the following: catalytic cracking slurry oil or its distillate oil, catalytic cycle oil or its distillate oil, solvent-de-oiled asphalt or its distillate oil, and thermal cracking residue oil or its distillate oil.
[0066] The ash content of the aromatic feedstock 1* is less than 50 ppm, preferably less than 20 ppm, more preferably less than 5 ppm, and its density at 20°C is 1.01-1.12 g / cm³. 3 The total aromatic hydrocarbon content is 60-80%, of which the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings are 10-20%, 60-70%, 10-20% and 5-10% respectively, based on the total weight of the total aromatic hydrocarbons. The distillation range is 350-580℃, the sulfur content is 0.1-0.3% and the nitrogen content is 0.05-0.2%. The ash content, total aromatic hydrocarbon content, sulfur content and nitrogen content are all calculated based on the total weight of 1* of aromatic hydrocarbon raw material.
[0067] In step 1) of the process described above in this invention, the purpose of filtering the first aromatic raw material is to remove solid particles. The filtration process has virtually no effect on parameters such as the ash content, total aromatic content, and content of tricyclic aromatics, tetracyclic aromatics, pentacyclic aromatics, and aromatics with more than five rings in the first aromatic raw material. In other words, it can be considered that the parameters of the first aromatic raw material and the aromatic raw material 1* are basically the same.
[0068] As a specific embodiment of the process for co-producing basic asphalt and mesophase asphalt described above in this invention, in step 1), the internal temperature of the first reactor is 330-360℃ and the reaction residence time is 5-10h.
[0069] And / or, in step 2), the internal temperature of the second reactor is 410-430℃, the reaction residence time is 1-5h, and the reaction pressure is 3-5MPa;
[0070] And / or, in step 3), the internal temperature of the third reactor is 390-430℃, and the reaction residence time is 5-10h.
[0071] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the heating device used in step 1) can be, for example, a tubular heater with an outlet temperature of 330-350°C.
[0072] In one specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the discharge port (denoted as the first discharge port) of the first reactor used in step 1) is located at the bottom of the first reactor and has a conical discharge design. In this case, the heated aromatic feedstock 1* enters the first reactor from the first inlet located at the top or upper part of the first reactor. In some embodiments of this invention, the taper can be, for example, 1:1. Alternatively, the inlet (denoted as the second inlet) of the first reactor can also be located at its bottom or lower part, and the discharge port (denoted as the second discharge port) can be located at the upper part of the first reactor. In this case, the heated aromatic feedstock 1* enters the first reactor from the second inlet located at the bottom or lower part of the first reactor and exits from the second discharge port located at the upper part of the first reactor.
[0073] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the properties of the base asphalt obtained in step 1) are: softening point 100-120℃, coking value 30-40%, quinoline insoluble content 0.1-0.2% and ash content 0.001-0.005%, wherein the contents are all weight percentages calculated based on the total weight of the base asphalt.
[0074] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the properties of the low softening point mesophase asphalt obtained in step 2) are as follows: softening point 150-170℃, quinoline insoluble content 20-30%, toluene insoluble content 50-60%, and ash content 0.001-0.005%, wherein the contents are all weight percentages calculated based on the total weight of the low softening point mesophase asphalt.
[0075] In a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, in step 3), inert gas and low-softening-point mesophase asphalt are mixed at a gas flow rate to low-softening-point mesophase asphalt weight ratio of 1-5:100, where the gas flow rate is in L / min and the low-softening-point mesophase asphalt weight is in kg. Preferably, the pipeline between the outlet of the second reactor and the inlet of the third reactor is an insulated conveying pipeline, into which nitrogen gas is injected. In some embodiments of this invention, the inert gas includes nitrogen gas, etc. In step 3), the low-softening-point mesophase asphalt and inert gas are mixed and then introduced into the third reactor. The use of inert gas can promote the departure of low molecular weight components from the reaction system, concentrate the molecular weight while retaining high molecular weight components, thereby obtaining a product with a narrow molecular weight distribution. In addition, inert gas can also promote the smooth flow of asphalt in the pipeline into the third reactor, avoiding the problem of blockage at the inlet of the third reactor due to slow flow rate.
[0076] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, in step 3), the low softening point mesophase asphalt discharged from the outlet of the second reactor is introduced into the second asphalt buffer tank at a temperature of 310-330°C, and the inert gas and the low softening point mesophase asphalt are mixed at a gas flow rate to low softening point mesophase asphalt weight ratio of 1-5:100.
[0077] In a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, in step 3), the third reactor is a dual-stirring and heating reactor equipped with a wall-mounted agitator and a bottom agitator. The stirring speed of the wall-mounted agitator is 50-100 r / min, and the stirring speed of the bottom agitator is 100-150 r / min. The ratio of the bottom agitator diameter to the third reactor diameter is 1-2:5. Nitrogen gas is introduced into the third reactor from the bottom of the bottom agitator, with a nitrogen flow rate to asphalt ratio of 1-5 L / min:100 kg. Introducing inert gases such as nitrogen into the third reactor from the bottom of the bottom agitator allows for more thorough contact between the inert gas and the reactants, thereby carrying away the decomposed light components from the reactant system.
[0078] In a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, in step 3), after the reaction is completed, the high-quality spinnable mesophase asphalt formed through deep reaction is discharged from the outlet of the third reactor. A heat tracing pipeline is connected to the outlet of the third reactor, with a heat tracing temperature of 330-350℃. An external magnetic strip installed outside the heat tracing pipeline generates a magnetic field perpendicular to the heat tracing pipeline, with a magnetic field strength of 0.5-1T, which can be activated as needed. A second filter device is provided at the lower part of the heat tracing pipeline, preferably a ceramic filter (preferably an insertable ceramic filter with a mesh size of 100-200 mesh, selected as needed). Finally, after cooling and collection, high-quality spinnable mesophase asphalt is obtained. In some embodiments of this invention, the heat tracing of the heat tracing pipeline can be achieved by installing a heat tracing device at the outlet of the third reactor.
[0079] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the properties of the high-quality spinnable mesophase asphalt obtained in step 3) are as follows: softening point 275-285℃, quinoline insoluble content 40-50%, toluene insoluble content 70-80%, ash content 0.002-0.006%, mesophase content with wide-area streamline structure 100%, and yield 30-35% (calculated based on the total weight of the starting aromatic feedstock). The contents are all weight percentages calculated based on the total weight of the high-quality spinnable mesophase asphalt.
[0080] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the process further includes step 4): using a first vacuum device to sequentially heat and separate, condense and separate and cryogenically treat the high-temperature oil and gas generated in the first reactor in step 1), and using a second vacuum device to sequentially heat and separate, condense and separate and cryogenically treat the high-temperature oil and gas generated in the second reactor in step 2) and the third reactor in step 3).
[0081] The temperatures for heating separation, condensation separation, and cryogenic treatment are 190-220℃, 2-10℃, and -40 to -30℃, respectively. The pressure of the first vacuum system is 30-50 kPa. When the high-temperature oil and gas generated in the second reactor in step 2) is sequentially heated, condensed, and cryogenically treated using the second vacuum device, the vacuum of the second vacuum device is shut off, i.e., the second vacuum unit is shut down. When the high-temperature oil and gas generated in the third reactor in step 3) is sequentially heated, condensed, and cryogenically treated using the second vacuum device, the pressure of the second vacuum device is 80-90 kPa.
[0082] As a specific embodiment of the process for co-producing base asphalt and mesophase asphalt described above in this invention, the first vacuum device includes a first oil-gas buffer tank, a first condenser, a first cryogenic reactor, and a first vacuum unit connected in sequence. During operation, the high-temperature oil and gas (containing medium-grade aromatic oil and light oil and gas) extracted from the first reactor first enters the first oil-gas buffer tank for heating and separation to separate the medium-grade aromatic oil, wherein the density (20°C) of the separated medium-grade aromatic oil is 0.79-0.82 g / cm³. 3 The light oil is then separated in the first condenser, and the non-condensable vapor enters the first cryogenic cooler for cooling. In some embodiments of the present invention, the condensing medium in the first condenser may be cooling water, and the cooling medium in the second cryogenic cooler may be a mixture of water and ethylene glycol.
[0083] As a specific embodiment of the process described above in this invention, the second vacuum device includes a second oil-gas buffer tank, a second condenser, a second cryostat, and a second vacuum unit connected in sequence. During operation, the high-temperature oil-gas (heavy aromatic oil and light oil-gas) collected from the second reactor and the high-temperature oil-gas (heavy aromatic oil and light oil-gas) collected from the third reactor first enter the second oil-gas buffer tank for heating and separation to separate the heavy aromatic oil. Then, the medium aromatic oil is separated by the second condenser, and the non-condensable vapor enters the second cryostat for cooling.
[0084] The high-temperature oil and gas produced from the second reactor and the high-temperature oil and gas produced from the third reactor, after separation, yielded heavy aromatic oil with properties of 0.83-0.88 g / cm³. 3 .
[0085] In some embodiments of the present invention, the condensing medium in the second condenser may also be cooling water, and the cooling medium in the second cryogenic reactor may also be a mixture of water and ethylene glycol.
[0086] In the process of co-producing base asphalt and mesophase asphalt described above in this invention, the purified material is first pyrolyzed to obtain base asphalt, and then undergoes a high-temperature thermal polymerization reaction to generate mesophase asphalt with a low softening point. Finally, thermal polymerization is carried out to remove volatiles and obtain high-quality spinnable mesophase asphalt.
[0087] In the process of co-producing base asphalt and mesophase asphalt described above in this invention, the low softening point mesophase asphalt can be used as a binder for special fine-structured graphite, and the high-quality spinnable mesophase asphalt can be used for the preparation of high-modulus, high-thermal-conductivity, high-performance carbon fibers.
[0088] Compared with the prior art, the beneficial technical effects achieved by the present invention include:
[0089] The system and process provided by this invention are applicable to the production of high softening point homogeneous asphalt and mesophase asphalt products. By designing based on the differences in the properties of aromatic molecules in petroleum heavy oil feedstock, and by combining the overall process flow, feeding method, internal structure of the three-stage reactor, and process parameter adjustments, high softening point homogeneous asphalt and mesophase asphalt products with excellent performance and stable quality can be prepared. This achieves the goal of product diversification and flexible adjustment of product structure within the same system, which is beneficial for reducing production costs and improving equipment utilization.
[0090] In summary, this invention enables the production of asphalt products with different structures by using heavy petroleum oil feedstocks from different sources and designing differentiated heavy aromatic component polymerization technologies based on their compositional characteristics. The process flow meets the requirements for the preparation and production of stable and high-quality asphalt products. Compared with previous technologies, the entire process makes full use of equipment, minimizes investment, facilitates large-scale continuous production through equipment selection and design, results in low production costs, and ensures stable product quality. Attached Figure Description
[0091] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0092] Figure 1 This is a schematic diagram of the system for co-producing petroleum purified bitumen and high softening point special bitumen provided in Embodiment 1 of the present invention.
[0093] Explanation of main icon numbers:
[0094] 1. Third raw material tank; 2. Second raw material tank; 3. First raw material tank; 1-1. First filter; 1-2. Second filter; 1-3, 1-4, 1-5, 1-6, 1-7 and 1-8 are the first to sixth high-temperature gear pumps respectively; 1-9, 1-10, 1-11, 1-12 and 1-13 are the first to fifth valves respectively; 2-1. Adjusting agent storage tank; 2-2. Mixing tank; 4. Heat exchanger; 5. Fractionating tower; 6. Light oil tank; 7. Medium oil tank; 8-1 and 8-2 are the first and second oil-gas buffer tanks respectively; 9-1 and 9-2 are... 10-1 and 10-2 are respectively the first condenser and the second condenser; 11-1 and 11-2 are respectively the first vacuum unit and the second vacuum unit; 12, first gas source; 13, tubular heater; 14, first reactor; 15, first asphalt buffer tank; 16, second reactor; 16-1, stirrer; 17, second asphalt buffer tank; 18, third reactor; 18-1, frame stirrer; 18-2, bottom stirrer; 18-3, external magnetic strip; 18-4, ceramic filter screen; 18-5, cooling collector; 19, second gas source. Detailed Implementation
[0095] It should be noted that the term "comprising" and any variations thereof in the specification, claims, and accompanying drawings of this invention are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or devices.
[0096] The "range" disclosed in this invention is given in the form of a lower limit and an upper limit. It can be one or more lower limits and one or more upper limits, respectively. A given range is defined by selecting a lower limit and an upper limit. The selected lower and upper limits define the boundaries of the particular range. All ranges defined in this way are composable, meaning that any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for specific parameters, it is also expected that ranges of 60-110 and 80-120 are also expected. Furthermore, if the listed minimum range values are 1 and 2, and the listed maximum range values are 3, 4, and 5, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5.
[0097] In this invention, unless otherwise specified, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in this invention, and "0-5" is simply a shortened representation of these numerical combinations.
[0098] In this invention, unless otherwise specified, all embodiments and preferred embodiments mentioned in this invention can be combined with each other to form new technical solutions.
[0099] In this invention, unless otherwise specified, all technical features and preferred features mentioned in this invention can be combined with each other to form new technical solutions.
[0100] In this invention, unless otherwise specified, all steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially. For example, if the method includes steps (a) and (b), it means that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, if the method may also include step (c), it means that step (c) may be added to the method in any order. For example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc.
[0101] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying tables, drawings, and embodiments. The embodiments described below are some, but not all, embodiments of this invention, and are only used to illustrate the invention, and should not be considered as limiting the scope of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.
[0102] In this invention, the softening point of each asphalt product was tested according to the standard test method for softening point of asphalt (Miller's cup method) in ASTM D3461-97(2012). The ash content was tested according to the method for determining ash content in coking solids products in GB / T 2295-2008. The coking value was tested according to the method for determining coking value in coal tar pitch products in GB / T 8727-2008. The content of toluene-insoluble matter was tested according to the method for determining the content of toluene-insoluble matter in coking products in GB / T 2292-2018. The content of quinoline-insoluble matter was tested according to the method for testing quinoline-insoluble matter in coking solids products in GB / T 2293-1997. The content and structure of the mesophase were tested according to the method for determining the optical structure of mesophase coke in coal-series needle coke in YB / T 4822-2020.
[0103] Example 1
[0104] This embodiment provides a system for the co-production of petroleum-purified asphalt and high-softening-point specialty asphalt, the structural schematic diagram of which is shown below. Figure 1 As shown, from Figure 1 As can be seen from this, the system includes:
[0105] The reactor comprises a first raw material tank 3, a second raw material tank 2, a third raw material tank 1, a modifier storage tank 2-1, a mixing tank 2-2, a heat exchanger 4, a fractionation tower 5, a first gas source 12, a tubular heater 13, a first reactor 14, a second reactor 16, a third reactor 18, a second gas source 19, a first vacuum device, and a second vacuum device. The first reactor 14 has a first feed inlet at its top and a second feed inlet at its bottom, and correspondingly, a first discharge outlet at its bottom and a second discharge outlet at its top. The top of the first reactor 14 also has a high-temperature oil and gas extraction outlet. The second reactor 16 is a heated reactor with a turbine-type agitator. The discharge outlet of the second reactor 16 (located at its bottom) has a conical discharge design, with a taper of, for example, 1:2. The third reactor 18 is equipped with a wall-scraping frame agitator 18-1 and a bottom agitator 18-2, and the outlet of the second gas source 19 is connected to the bottom agitator 18-2 via a pipeline.
[0106] The third raw material tank 1 is connected to the inlet of the first raw material tank 3 via pipelines through the first filter 1-1, the second filter 1-2, and the first high-temperature gear pump 1-3. The second raw material tank 2 and the conditioning agent storage tank 2-1 are connected to the mixing tank 2-2 via pipelines. The first outlet of the first raw material tank 3 and the first outlet of the mixing tank 2-2 are connected to the inlet (located in the upper part) of the fractionation tower 5 via pipelines through a three-way valve and then through pipelines through the second high-temperature gear pump 1-4 and the heat exchanger 4. The side wall of the fractionation tower 5 is provided with 1-5 side-stream outlets and aromatic basic component outlets from top to bottom, and a high-temperature oil and gas outlet is provided at the top. The first side-stream outlet is connected to the light oil tank 6 via pipelines, and the second to fifth side-stream outlets are connected to the medium oil tank 7 via pipelines. The aromatic basic component outlet of the fractionation tower 5 is connected to the inlet of the first raw material tank 6 via pipelines through the second filter 1-1, the second filter 1-2, and the first high-temperature gear pump 1-3 via pipelines through the second filter 1-1, the second filter 1-2, and the first high-temperature gear pump 1-3. The third high-temperature gear pump 1-5 and the tubular heater 13 are connected to the second inlet of the first reactor 14. The first gas source 12 is connected to the tubular heater 13 through a pipeline. The second outlet of the first reactor 14 is connected to the inlet (located at its upper part) of the second reactor 16 through a pipeline via the first asphalt buffer tank 15. The outlet (located at its bottom) of the second reactor 16 is connected to the inlet (located at its top) of the third reactor 18 through a pipeline via the second asphalt buffer tank 17 and the fifth high-temperature gear pump 1-7, and then to the outlet pipeline of the second gas source 19 after converging at a three-way valve. The outlet of the third reactor 18 is connected to the cooling collector 18-5 through a heat tracing pipeline. An external magnetic strip 18-3 is installed outside the heat tracing pipeline. A ceramic filter screen 18-4 is installed inside the heat tracing pipeline between the external magnetic strip 18-3 and the cooling collector 18-5.
[0107] The second outlet of the first raw material tank 3 is connected to the first feed port or the second feed port of the first reactor 14 via a pipeline through the sixth high-temperature gear pump 1-8 and the tubular heater 13. Correspondingly, the first discharge port or the second discharge port of the first reactor 14 is connected to the inlet (located above it) of the second reactor 16 via a pipeline through the fourth high-temperature gear pump 1-6 and the first asphalt buffer tank 15. The first valve 1-9, the second valve 1-10 and the third valve 1-11 are respectively installed on the pipeline between the first outlet of the first raw material tank 3 and the three-way valve, the pipeline between the second outlet of the first raw material tank 3 and the sixth high-temperature gear pump 1-8 and the pipeline between the first gas source 12 and the tubular heater 13. The fourth valve 1-12 and the fifth valve 1-13 are respectively installed on the pipeline between the tubular heater 13 and the first feed port or the second feed port of the first reactor 14.
[0108] The first vacuum device includes a first oil-gas buffer tank 8-1, a first condenser 9-1, a first cryogenic unit 10-1 and a first vacuum unit 11-1 connected in sequence by pipelines; the second vacuum device includes a second oil-gas buffer tank 8-2, a second condenser 9-2, a second cryogenic unit 10-2 and a second vacuum unit 11-2 connected in sequence by pipelines.
[0109] The high-temperature oil and gas outlet at the top of the fractionation tower 5 and the high-temperature oil and gas outlet at the top of the first reactor 14 are respectively connected to the inlet of the first oil and gas buffer tank 8-1 in the first vacuum device through pipelines. The second outlet of the mixing tank 2-2, the high-temperature oil and gas outlet at the top of the second reactor 16 and the high-temperature oil and gas outlet at the top of the third reactor 18 are respectively connected to the second oil and gas buffer tank 8-2 in the second vacuum device through pipelines.
[0110] Example 2
[0111] This embodiment provides a process for co-producing purified asphalt and homogeneous asphalt, which is implemented using the system for co-producing petroleum purified asphalt and high softening point special asphalt provided in Example 1, and includes the following specific steps:
[0112] Step (a): Selection and pretreatment of raw materials:
[0113] Catalytic cracking slurry was selected as the first aromatic feedstock. The first aromatic feedstock was filtered using the first filter 1-1 and the second filter 1-2, respectively. After removing solid particles, aromatic feedstock 1* was obtained and stored in the first feedstock tank 3 for later use. Simultaneously, the second valve 1-10 on the pipeline between the second outlet of the first feedstock tank 3 and the sixth high-temperature gear pump 1-8 was closed. The ash content of aromatic feedstock 1* was 5 ppm, and its density (20℃) was 1.12 g / cm³. 3 The total aromatic hydrocarbon content is 75%, of which, by total weight, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings account for 13%, 62%, 20% and 5% respectively. The distillation range is 380-550℃, the sulfur content is 0.28%, and the nitrogen content is 0.15%.
[0114] Ethylene tar was selected as the second aromatic feedstock, with an ash content of 8 ppm and a density (20℃) of 1.17 g / cm³. 3The total aromatic hydrocarbon content is 90%, of which, by weight, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons, and aromatic hydrocarbons with more than five rings are 3%, 30%, 50%, and 17%, respectively. The distillation range is 350-580℃, the sulfur content is 0.1%, and the nitrogen content is 0.06%. In mixing tank 2-2, 9,10-anthraquinone is added to the second aromatic hydrocarbon feedstock as a reaction modifier. The weight ratio of the two is 1000:3, the mixing temperature is 35℃, the stirring speed is 900 r / min, and the mixing time is 0.5 hours, to obtain aromatic hydrocarbon feedstock 2*. Aromatic hydrocarbon feedstock 1 is then... * The aromatic raw material 2 was mixed with the aromatic raw material 2 at a weight ratio of 1:10 to obtain a mixture. The mixing method was online mixing, the mixing temperature was 150℃, and the linear velocity was 0.3m / s.
[0115] Step (b): Preparation of aromatic basic components:
[0116] The mixture enters heat exchanger 4, where it is heated to 300°C by the 340°C heat transfer oil. It then enters the upper part of fractionation tower 5 for the regulation of aromatic molecular structure and composition distribution. Fractionation tower 5 operates under reduced pressure (30-50 kPa). The upper part of fractionation tower 5 has a temperature of 120-150°C, and the lower part has a temperature of 290-310°C. The basic aromatic components are collected from the lower part, and high-temperature oil and gas are collected from the top of the tower and recovered through a first vacuum device. The recovery process includes: the oil and gas first enters the first oil and gas buffer tank 8-1; the separated gas phase is cooled by heat exchange in the first condenser 9-1; the pressure of the first vacuum device is 50 kPa; and the condensing medium in the first condenser 9-1 is cooling water. The first side stream outlet of fractionation tower 5 produces light aromatic oil with a density (20°C) of 0.76 g / cm³. 3 The oil extracted from the second to fifth side lines is medium-quality aromatic oil, with a density (20℃) of 0.81 g / cm³. 3 .
[0117] Step (c): Preparation of purified base bitumen:
[0118] The aromatic basic components are fed into a tubular heater 13, and steam is injected into its tubes. After heating in the tubular heater 13, the outlet temperature is 330℃. The gas flow rate to the mass ratio of aromatic basic components is 5L / min:100kg aromatic basic components. The heated aromatic basic components are then fed into the first reactor 14 through the second feed inlet at the bottom. The material resides in the first reactor 14 for 8 hours. The internal temperature of the first reactor 14 is 330℃, and the pressure is atmospheric pressure. After the molecular weight distribution of the aromatic basic components is initially adjusted in the first reactor 14, purified base asphalt and high-temperature oil and gas (medium aromatic oil and light aromatic oil) are obtained. (Oil and gas); Medium-quality aromatic oil and light oil and gas are recovered through the first vacuum device. The specific process is as follows: High-temperature oil and gas are extracted from the top of the first reactor 14 and first enter the first oil and gas buffer tank. The separated gas phase is then cooled by heat exchange in the first condenser to separate medium-quality aromatic oil. The non-condensable vapor enters the first cryogenic cooler for cooling. The temperature of the first oil and gas buffer tank is 200℃, the condensing medium used in the first condenser is cooling water at a temperature of 10℃, the cooling medium used in the first cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 50KPa. The density of the separated medium-quality aromatic oil (at 20℃) is 0.80 g / cm³. 3 ;
[0119] Tests showed that the purified base asphalt obtained in this step had the following properties: softening point 118℃, coking value 29%, quinoline insoluble content 0%, and ash content 0.001%.
[0120] Step (d): Preparation of high softening point homogeneous asphalt products:
[0121] The purified base asphalt overflows from the second outlet at the top of the first reactor 14 and enters the first asphalt buffer tank 15. Then, it enters the second reactor 16 by gravity for reaction. The internal temperature of the second reactor 16 is 360℃, the stirring speed is 150 r / min, the residence time of the purified base asphalt in the second reactor 16 is 5 hours, and the pressure is 10 Pa. After the reaction, the purified base asphalt produces a high softening point homogeneous asphalt product and high-temperature oil and gas, which contains heavy aromatic oil and light gas. The heavy aromatic oil and light oil and gas in the high-temperature oil and gas are recovered by a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the second reactor 16 and first enters the second oil and gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, which has a density (20℃) of 0.83 g / cm³. 3Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 200℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 10Pa.
[0122] Tests show that the high softening point homogeneous asphalt product obtained in this step has the following properties: softening point 220℃, coking value 65%, quinoline insoluble content 0.1%, and ash content 0.0015%.
[0123] Step (e): Preparation of ultra-high softening point isotropic asphalt products:
[0124] The high softening point homogeneous asphalt product obtained from the second reactor 16 is introduced into the second asphalt buffer tank 17 at a temperature of 310℃. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated transport pipeline carrying the high softening point homogeneous asphalt product, maintaining a mass-to-nitrogen flow rate ratio of 100 kg: 4 L / min. The stirring speed of the wall-scraping frame agitator 18-1 in the third reactor 18 is 50 r / min. The diameter ratio of the bottom agitator 18-2 to the diameter of the third reactor 18 is 1:5. Nitrogen gas is introduced into the bottom of the bottom agitator 18-2 in the third reactor 18. The temperature inside the third reactor 18 is 370℃, and the reaction residence time is 6 hours. After deep reaction, ultra-high softening point asphalt is formed. The softening point homogeneous asphalt product is discharged from the bottom through a heated pipeline (the heating device is located at the bottom outlet of the third reactor). The temperature of the heated pipeline is 330℃. During the discharge process, it first passes through a magnetic field with a magnetic field strength of 0.5T perpendicular to the heated pipeline, and then is filtered through a ceramic filter with a mesh size of 200 mesh. After cooling, it is collected to obtain the ultra-high softening point homogeneous asphalt product. At the same time, high-temperature oil and gas (heavy aromatic oil and light oil and gas) is extracted from the top of the third reactor 18. The high-temperature oil and gas is recovered using a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the third reactor and first enters the second oil and gas buffer tank. The separated gas phase is then separated into heavy aromatic oil by the second condenser. The density (20℃) of the heavy aromatic oil is 0.85 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 190℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 2Pa.
[0125] After testing, it was found that the ultra-high softening point homogeneous asphalt product obtained in this step has the following properties: softening point 283℃, coking value 79%, quinoline insoluble content 0.5%, ash content 0.002%, and yield 37% (calculated based on the total weight of the starting aromatic raw materials).
[0126] Example 3
[0127] This embodiment provides a process for co-producing base asphalt and mesophase asphalt, which is implemented using the system for co-producing petroleum purified asphalt and high softening point special asphalt provided in Example 1, and includes the following specific steps:
[0128] Step a): Selection and heat treatment of raw materials:
[0129] The aromatic raw material 1 in Example 2 * As a raw material alone, the aromatic raw material 1* is stored in the first raw material tank 3 for later use, and the second valve 1-10 on the pipeline between the second outlet of the first raw material tank 3 and the sixth high-temperature gear pump 1-8 and the fourth valve 1-12 on the pipeline between the tubular heater 13 and the first feed port of the first reactor 14 are opened, while the first valve 1-9, the third valve 1-11 and the fifth valve 1-13 are closed.
[0130] Step b): Preparation of base asphalt:
[0131] Aromatic feedstock 1* is fed into tubular furnace 13 for heating, with an outlet temperature of 350°C; the heated aromatic feedstock 1*... * The material enters the first reactor 14 through the first inlet, and the residence time in the first reactor 14 is 6 hours. The internal temperature of the first reactor 14 is 350℃. The reaction produces basic asphalt and high-temperature oil and gas, which contains medium aromatic oil and light oil and gas. After being discharged through the first outlet of the first reactor 14 (which is a conical discharge design with a taper of 1:1), the material is transported to the first asphalt buffer tank 15 by the fourth high-temperature gear pump 1-6. The basic asphalt is then added to the second reactor 16 by gravity. The high-temperature oil and gas containing medium aromatic oil and light oil and gas is recovered by the first vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the first reactor 14 and first enters the first oil and gas buffer tank 8-1. The separated gas phase is then separated into medium aromatic oil by the first condenser 9-1. The density (20℃) of the separated medium aromatic oil is 0.80 g / cm³. 3 Non-condensable vapors enter the first cryogenic cooler 10-1 for cooling; the temperature of the first oil-gas buffer tank 8-1 is 200℃, the condensing medium used in the first condenser 9-1 is cooling water at a temperature of 8℃, the cooling medium used in the first cryogenic cooler 10-1 is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 30KPa.
[0132] After testing, it was found that the properties of the base asphalt obtained in this step were: softening point 105℃, coking value 35%, quinoline insoluble content 0.2%, and ash content 0.002%.
[0133] Step c): Preparation of low softening point mesophase asphalt:
[0134] After discharge, the base asphalt is transported to the first asphalt buffer tank 15 via the fourth high-temperature gear pump 1-6. The base asphalt is then added to the second reactor 16 by gravity. The internal temperature of the second reactor 16 is 410℃, the residence time of the base asphalt in the second reactor 16 is 5 hours, the reaction pressure is 3MPa, and the stirring speed is 100r / min. After the reaction, the base asphalt generates low-softening-point mesophase asphalt and high-temperature oil gas, which contains heavy aromatic oil and light gas. After the reaction, the high-temperature oil gas containing heavy aromatic oil and light oil gas discharged from the top of the second reactor 16 is recovered by the second vacuum device. Specifically, the high-temperature oil gas is collected from the top of the second reactor 16 and first enters the second oil gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, the density of which (at 20℃) is 0.87g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler 10-2 for cooling; the temperature of the second oil-gas buffer tank 8-2 is 200℃, the condensing medium used in the second condenser 9-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler 10-2 is a mixture of water and ethylene glycol at a temperature of -40℃, and the vacuum of the second vacuum device is closed.
[0135] After testing, it was found that the properties of the low softening point mesophase asphalt obtained in this step were: softening point 162℃, quinoline insoluble content 22%, toluene insoluble content 53%, and ash content 0.0025%.
[0136] Step d): Preparation of high-quality spinnable mesophase pitch:
[0137] After being discharged from the second reactor 16, the low-softening-point mesophase asphalt enters the second asphalt buffer tank 17 at a temperature of 310℃. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated transport pipeline carrying the low-softening-point mesophase asphalt, ensuring a mass ratio of asphalt to nitrogen flow rate of 100 kg: 5 L / min. The stirring speed of the wall-scraping frame agitator 18-1 in the third reactor 18 is 100 r / min, and the stirring speed of the bottom agitator 18-2 is 120 r / min. The diameter ratio of the bottom agitator 18-2 to the diameter of the third reactor 18 is 1:5. Nitrogen gas is introduced into the bottom of the bottom agitator 18-2, with a nitrogen flow rate to asphalt mass ratio of 2 L / min: 100 kg in the third reactor 18. The temperature inside the third reactor 18... The reaction temperature is 390℃, and the residence time is 6 hours. After deep reaction, mesophase asphalt is formed and discharged from the bottom of the third reactor 18 through a heated pipeline (the heated pipeline is located at the bottom outlet of the third reactor). The temperature of the heated pipeline is 330℃. During the discharge process, it first passes through a magnetic field with a magnetic field strength of 1T perpendicular to the heated pipeline, and then is filtered through a ceramic filter with a mesh size of 100 mesh. After cooling, it is collected to obtain high-quality spinnable mesophase asphalt. High-temperature oil and gas containing heavy aromatic oil and light oil and gas are extracted from the top of the third reactor 18. These are recovered through the second vacuum device. Specifically, after the high-temperature oil and gas is extracted from the top of the third reactor 18, it first enters the second oil and gas buffer tank 8-2. The separated gas phase is then separated into heavy aromatic oil by the second condenser 9-2. The density of this heavy aromatic oil (at 20℃) is 0.85 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank 8-2 is 200℃, the condensing medium used in the second condenser 8-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -30℃, and the pressure of the second vacuum device is 80KPa.
[0138] After testing, it was found that the high-quality spinnable mesophase pitch obtained in this step had the following properties: softening point 283℃, quinoline insoluble content 50%, toluene insoluble content 75%, ash content 0.0027%, mesophase content with wide-area streamline structure 100%, and yield 32% (calculated based on the total weight of the starting aromatic feedstock).
[0139] Example 4
[0140] This embodiment provides a process for co-producing purified asphalt and homogeneous asphalt, which is implemented using the system for co-producing petroleum purified asphalt and high softening point special asphalt provided in Example 1, and includes the following specific steps:
[0141] Step (a): Selection and pretreatment of raw materials and step (b): Preparation of aromatic basic components are basically the same as in Example 2, except that: aromatic raw material 1 * The aromatic raw material 2 is mixed with the aromatic raw material 2 at a weight ratio of 3:10.
[0142] Step (c): Preparation of purified base bitumen:
[0143] The aromatic basic components are fed into a tubular heater 13, and steam is injected into its tubes. After heating in the tubular heater 13, the outlet temperature is 350℃. The gas flow rate to the mass ratio of aromatic basic components is 5L / min:100kg aromatic basic components. The heated aromatic basic components are then fed into the first reactor 14 through the second feed inlet at the bottom. The material resides in the first reactor 14 for 6 hours. The internal temperature of the first reactor 14 is 350℃, and the pressure is atmospheric pressure. After the molecular weight distribution of the aromatic basic components is initially adjusted in the first reactor 14, purified base asphalt and high-temperature oil and gas (medium aromatic oil and light aromatic oil) are obtained. (Oil and gas); medium-quality aromatic oil and light oil and gas are recovered through the first vacuum device. The specific process is as follows: high-temperature oil and gas are extracted from the top of the first reactor 14 and first enter the first oil and gas buffer tank. The separated gas phase is then cooled by heat exchange in the first condenser to separate the medium-quality aromatic oil. The non-condensable vapor enters the first cryogenic cooler for cooling. The temperature of the first oil and gas buffer tank is 200℃, the condensing medium used in the first condenser is cooling water at a temperature of 10℃, the cooling medium used in the first cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 50KPa. The density of the separated medium-quality aromatic oil (at 20℃) is 0.81g / cm³. 3 Tests showed that the purified base asphalt obtained in this step had the following properties: softening point 115℃, coking value 27%, quinoline insoluble content 0%, and ash content 0.0013%.
[0144] Step (d): Preparation of high softening point homogeneous asphalt products:
[0145] The purified base asphalt overflows from the second outlet at the top of the first reactor 14 and enters the first asphalt buffer tank 15. Then, it enters the second reactor 16 by gravity for reaction. The internal temperature of the second reactor 16 is 330℃, the stirring speed is 100 r / min, the residence time of the purified base asphalt in the second reactor 16 is 10 hours, and the pressure is 10 Pa. After the reaction, the purified base asphalt produces a high softening point homogeneous asphalt product and high-temperature oil and gas, which contains heavy aromatic oil and light gas. The heavy aromatic oil and light oil and gas in the high-temperature oil and gas are recovered by a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the second reactor 16 and first enters the second oil and gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, which has a density (20℃) of 0.82 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 200℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 10Pa.
[0146] Tests show that the high softening point homogeneous asphalt product obtained in this step has the following properties: softening point 210℃, coking value 62%, quinoline insoluble content 0.15%, and ash content 0.0015%.
[0147] Step (e): Preparation of ultra-high softening point isotropic asphalt products:
[0148] The high softening point homogeneous asphalt product obtained from the second reactor 16 is introduced into the second asphalt buffer tank 17 at a temperature of 310℃. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated transport pipeline carrying the high softening point homogeneous asphalt product, maintaining a mass-to-nitrogen flow rate ratio of 100 kg: 1 L / min. The stirring speed of the wall-scraping frame agitator 18-1 in the third reactor 18 is 50 r / min. The diameter ratio of the bottom agitator 18-2 to the diameter of the third reactor 18 is 2:5. Nitrogen gas is introduced into the bottom of the bottom agitator 18-2 in the third reactor 18. The temperature inside the third reactor 18 is 350℃, and the reaction residence time is 7 hours. After deep reaction, ultra-high softening point asphalt is formed. The softening point homogeneous asphalt product is discharged from the bottom through a heated pipeline (the heating device is located at the bottom outlet of the third reactor). The temperature of the heated pipeline is 330℃. During the discharge process, it first passes through a magnetic field with a magnetic field strength of 0.5T perpendicular to the heated pipeline, and then is filtered through a ceramic filter with a mesh size of 200 mesh. After cooling, it is collected to obtain the ultra-high softening point homogeneous asphalt product. At the same time, high-temperature oil and gas (heavy aromatic oil and light oil and gas) is extracted from the top of the third reactor 18. The high-temperature oil and gas is recovered using a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the third reactor and first enters the second oil and gas buffer tank. The separated gas phase is then separated into heavy aromatic oil by the second condenser. The density (20℃) of the heavy aromatic oil is 0.84 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 190℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 2Pa.
[0149] After testing, it was found that the ultra-high softening point homogeneous asphalt product obtained in this step has the following properties: softening point 279℃, coking value 76%, quinoline insoluble content 0.2%, ash content 0.002%, and yield 38% (calculated based on the total weight of the starting aromatic raw materials).
[0150] Example 5
[0151] This embodiment provides a process for co-producing base asphalt and mesophase asphalt, which is implemented using the system for co-producing petroleum purified asphalt and high softening point special asphalt provided in Example 1, and includes the following specific steps:
[0152] Step a): Selection and heat treatment of raw materials:
[0153] The aromatic raw material 1 in Example 2 *As a raw material alone, the aromatic raw material 1* is stored in the first raw material tank 3 for later use, and the second valve 1-10 on the pipeline between the second outlet of the first raw material tank 3 and the sixth high-temperature gear pump 1-8 and the fifth valve 1-13 on the pipeline between the tubular heater 13 and the second feed port of the first reactor 14 are opened, while the first valve 1-9, the third valve 1-11 and the fourth valve 1-12 are closed.
[0154] Step b): Preparation of base asphalt:
[0155] Aromatic feedstock 1* is fed into tubular furnace 13 for heating, with an outlet temperature of 330°C; the heated aromatic feedstock 1*... * The material enters the first reactor 14 through the second inlet, and the residence time in the first reactor 14 is 9 hours. The internal temperature of the first reactor 14 is 330℃. The reaction produces basic asphalt and high-temperature oil and gas, which contains medium aromatic oil and light oil and gas. After being discharged through the second outlet of the first reactor 14, the material overflows directly into the first asphalt buffer tank 15. The basic asphalt is then added to the second reactor 16 by gravity. The high-temperature oil and gas containing medium aromatic oil and light oil and gas is recovered by the first vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the first reactor 14 and first enters the first oil and gas buffer tank 8-1. The separated gas phase is then separated into medium aromatic oil by the first condenser 9-1. The density (20℃) of the separated medium aromatic oil is 0.80 g / cm³. 3 Non-condensable vapors enter the first cryogenic cooler 10-1 for cooling; the temperature of the first oil-gas buffer tank 8-1 is 200℃, the condensing medium used in the first condenser 9-1 is cooling water at a temperature of 8℃, the cooling medium used in the first cryogenic cooler 10-1 is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 30KPa.
[0156] After testing, it was found that the properties of the base asphalt obtained in this step were: softening point 112℃, coking value 38%, quinoline insoluble content 0.1%, and ash content 0.002%.
[0157] Step c): Preparation of low softening point mesophase asphalt:
[0158] After discharge, the base asphalt overflows directly into the first asphalt buffer tank 15. The base asphalt is then added to the second reactor 16 by gravity. The internal temperature of the second reactor 16 is 430℃, the residence time of the base asphalt in the second reactor 16 is 2 hours, the reaction pressure is 5MPa, and the stirring speed is 150r / min. After the reaction, the base asphalt generates low-softening-point mesophase asphalt and high-temperature oil gas, which contains heavy aromatic oil and light gas. After the reaction, the high-temperature oil gas containing heavy aromatic oil and light oil gas discharged from the top of the second reactor 16 is recovered through a second vacuum device. Specifically, the high-temperature oil gas is collected from the top of the second reactor 16 and first enters the second oil gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, whose density (at 20℃) is 0.85g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler 10-2 for cooling; the temperature of the second oil-gas buffer tank 8-2 is 200℃, the condensing medium used in the second condenser 9-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler 10-2 is a mixture of water and ethylene glycol at a temperature of -40℃, and the vacuum of the second vacuum device is closed.
[0159] After testing, it was found that the properties of the low softening point mesophase asphalt obtained in this step were: softening point 158℃, quinoline insoluble content 20%, toluene insoluble content 55%, and ash content 0.0025%.
[0160] Step d): Preparation of high-quality spinnable mesophase pitch:
[0161] After being discharged from the second reactor 16, the low-softening-point mesophase asphalt enters the second asphalt buffer tank 17 at a temperature of 310℃. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated conveying pipeline for transporting the low-softening-point mesophase asphalt, ensuring a mass ratio of asphalt to nitrogen flow rate of 100 kg: 5 L / min. The stirring speed of the wall-scraping frame agitator 18-1 in the third reactor 18 is 100 r / min, and the stirring speed of the bottom agitator 18-2 is 100 r / min. The diameter ratio of the bottom agitator 18-2 to the diameter of the third reactor 18 is 1:5. Nitrogen gas is introduced into the bottom of the bottom agitator 18-2, with a nitrogen flow rate to asphalt mass ratio of 2 L / min: 100 kg in the third reactor 18. The temperature inside the third reactor 18 is... The reaction temperature is 400℃, and the residence time is 5 hours. After deep reaction, mesophase asphalt is formed and discharged from the bottom of the third reactor 18 through a heated pipeline (the heated pipeline is located at the bottom outlet of the third reactor). The temperature of the heated pipeline is 330℃. During the discharge process, it first passes through a magnetic field with a magnetic field strength of 1T perpendicular to the heated pipeline, and then passes through a ceramic filter with a mesh size of 100 mesh. After cooling, it is collected to obtain high-quality spinnable mesophase asphalt. High-temperature oil and gas containing heavy aromatic oil and light oil and gas are extracted from the top of the third reactor 18. These are recovered through the second vacuum device. The specific process is as follows: after the high-temperature oil and gas is extracted from the top of the third reactor 18, it first enters the second oil and gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil. The density of the heavy aromatic oil (at 20℃) is 0.86 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank 8-2 is 220℃, the condensing medium used in the second condenser 8-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -30℃, and the pressure of the second vacuum device is 90KPa.
[0162] After testing, it was found that the high-quality spinnable mesophase pitch obtained in this step has the following properties: softening point 280℃, quinoline insoluble content 45%, toluene insoluble content 73%, ash content 0.0027%, mesophase content with wide-area streamline structure 100%, and yield 35% (calculated based on the total weight of the starting aromatic feedstock).
[0163] Example 6
[0164] This embodiment provides a process for co-producing base asphalt and mesophase asphalt. The main difference between this embodiment and Embodiment 5 is that the third reactor only has a wall-scraping frame agitator 18-1, without a bottom agitator 18-2, and also lacks external magnetic strips, ceramic filters, and a cooling collector. The process includes the following specific steps:
[0165] Step a): Selection and heat treatment of raw materials:
[0166] The aromatic raw material 1 in Example 2 * As a raw material alone, the aromatic raw material 1* is stored in the first raw material tank 3 for later use, and the second valve 1-10 on the pipeline between the second outlet of the first raw material tank 3 and the sixth high-temperature gear pump 1-8 and the fifth valve 1-13 on the pipeline between the tubular heater 13 and the second feed port of the first reactor 14 are opened, while the first valve 1-9, the third valve 1-11 and the fourth valve 1-12 are closed.
[0167] Step b): Preparation of base asphalt:
[0168] Aromatic feedstock 1* is fed into tubular furnace 13 for heating, with an outlet temperature of 330°C; the heated aromatic feedstock 1*... * The material enters the first reactor 14 through the second inlet, and the residence time in the first reactor 14 is 9 hours. The internal temperature of the first reactor 14 is 330℃. The reaction produces basic asphalt and high-temperature oil and gas, which contains medium aromatic oil and light oil and gas. After being discharged through the second outlet of the first reactor 14, the material overflows directly into the first asphalt buffer tank 15. The basic asphalt is then added to the second reactor 16 by gravity. The high-temperature oil and gas containing medium aromatic oil and light oil and gas is recovered by the first vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the first reactor 14 and first enters the first oil and gas buffer tank 8-1. The separated gas phase is then separated into medium aromatic oil by the first condenser 9-1. The density (20℃) of the separated medium aromatic oil is 0.80 g / cm³. 3 Non-condensable vapors enter the first cryogenic cooler 10-1 for cooling; the temperature of the first oil-gas buffer tank 8-1 is 200℃, the condensing medium used in the first condenser 9-1 is cooling water at a temperature of 8℃, the cooling medium used in the first cryogenic cooler 10-1 is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 30KPa.
[0169] After testing, it was found that the properties of the base asphalt obtained in this step were: softening point 112℃, coking value 38%, quinoline insoluble content 0.1%, and ash content 0.002%.
[0170] Step c): Preparation of low softening point mesophase asphalt:
[0171] After discharge, the base asphalt overflows directly into the first asphalt buffer tank 15. The base asphalt is then added to the second reactor 16 by gravity. The internal temperature of the second reactor 16 is 430℃, the residence time of the base asphalt in the second reactor 16 is 2 hours, the reaction pressure is 5MPa, and the stirring speed is 150r / min. After the reaction, the base asphalt generates low-softening-point mesophase asphalt and high-temperature oil gas, which contains heavy aromatic oil and light gas. After the reaction, the high-temperature oil gas containing heavy aromatic oil and light oil gas discharged from the top of the second reactor 16 is recovered through a second vacuum device. Specifically, the high-temperature oil gas is collected from the top of the second reactor 16 and first enters the second oil gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, whose density (at 20℃) is 0.85g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler 10-2 for cooling; the temperature of the second oil-gas buffer tank 8-2 is 200℃, the condensing medium used in the second condenser 9-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler 10-2 is a mixture of water and ethylene glycol at a temperature of -40℃, and the vacuum of the second vacuum device is closed.
[0172] After testing, it was found that the properties of the low softening point mesophase asphalt obtained in this step were: softening point 158℃, quinoline insoluble content 20%, toluene insoluble content 55%, and ash content 0.0025%.
[0173] Step d): Preparation of mesophase asphalt with a higher softening point:
[0174] After being discharged from the second reactor 16, the low-softening-point mesophase asphalt enters the second asphalt buffer tank 17 at a temperature of 310℃. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated transport pipeline carrying the low-softening-point mesophase asphalt, maintaining a mass ratio of 100 kg to 5 L / min. The stirring speed of the scraper-frame agitator 18-1 inside the third reactor 18 is 100 r / min. Nitrogen gas is introduced into the third reactor 18 from the bottom, with a nitrogen flow rate to asphalt mass ratio of 2 L / min to 100 kg. The temperature inside reactor 8 is 400℃, and the reaction residence time is 5 hours. After deep reaction, the mesophase asphalt formed is discharged from the bottom of the third reactor 18 through a heated pipeline (the heated pipeline is located at the bottom outlet of the third reactor), where the temperature of the heated pipeline is 330℃. High-temperature oil and gas containing heavy aromatic oil and light oil and gas are extracted from the top of the third reactor 18 and recovered through the second vacuum device. The specific process is as follows: after the high-temperature oil and gas is extracted from the top of the third reactor 18, it first enters the second oil and gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, the density of which (at 20℃) is 0.86 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank 8-2 is 200℃, the condensing medium used in the second condenser 8-2 is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -30℃, and the pressure of the second vacuum device is 85KPa.
[0175] After testing, it was found that the properties of the mesophase pitch with a higher softening point obtained in this step are as follows: softening point 245-263℃, quinoline insoluble content 32-45%, toluene insoluble content 54-62%, ash content 0.03%, mesophase content with a wide-area streamline structure 80-90%, and yield 15% (calculated based on the total weight of the starting aromatic feedstock).
[0176] Comparing Examples 5 and 6, it can be seen that, compared to Example 5, the third reactor used in Example 6 only has a scraper-frame agitator 18-1 installed inside, but not a bottom agitator 18-2, and no external magnetic strip, ceramic filter, or cooling collector is installed. Consequently, the softening point, quinoline insoluble content, toluene insoluble content, and mesophase content with a wide-area streamline structure of the mesophase obtained in step d) of Example 6 fluctuate somewhat compared to Example 5, and the ash content is higher. The reasons for this are: First, the scraper-frame agitator in the third reactor is difficult to reach the bottom of the reactor, resulting in a longer residence time for the material at the bottom and varying degrees of reaction; second, in cases of insufficient stirring, heavy components in the asphalt will settle to the bottom; finally, using existing stirring methods, such as using only a scraper-frame agitator, always leaves residue at the discharge port, easily clogging it. The addition of a bottom agitator in the third reactor in this invention can improve these problems, avoiding excessively long residence times and resulting in a more uniform quality of the final asphalt product, making continuous reaction more practical.
[0177] Comparative Example 1
[0178] This comparative example first uses the same ethylene tar as in Example 2 as the sole raw material. Following the same fractionation process as in Example 2, aromatic basic components are obtained. These components are then heated in a tubular furnace to an outlet temperature of 330°C. The heated aromatic basic components enter the first reactor through the second feed inlet at the bottom of the first reaction chamber. The residence time in the reactor is 8 hours. The internal temperature of the first reactor is 330°C, and the pressure is atmospheric pressure. This produces purified asphalt and high-temperature oil and gas, which contain medium-grade aromatic oil and light oil and gas. After the same separation process as in Example 2, the density (20°C) of the obtained medium-grade aromatic oil is 0.78 g / cm³. 3 The purified bitumen has the following properties: softening point 80℃, coking value 21%, quinoline insoluble content 0%, and ash content 0.0015%.
[0179] The purified asphalt from the first reactor is fed into a second reactor for reaction. The internal temperature of the second reactor is 360°C, the stirring speed is 150 r / min, the residence time of the purified asphalt in the second reactor is 5 hours, and the pressure is 10 Pa. After reaction, the purified asphalt produces a high-softening-point homogeneous asphalt product and high-temperature oil gas, which contains heavy aromatic oil and light gas. The high-temperature oil gas undergoes the same separation process as in Example 2, and the density (20°C) of the obtained heavy aromatic oil is 0.83 g / cm³. 3 The properties of high softening point homogeneous asphalt are: softening point 175℃, coking value 51%, quinoline insoluble content 0.1%, and ash content 0.0015%.
[0180] The high softening point isotropic asphalt obtained from the second reactor is directly transferred to the third reactor, where the internal temperature is 370°C and the reaction residence time is 6 hours. After deep reaction, ultra-high softening point isotropic asphalt is formed and discharged directly from the bottom. After cooling, the product is collected. The high-temperature oil and gas collection process is the same as in Example 2, and the density (20°C) of the obtained heavy aromatic oil is 0.87 g / cm³. 3 The properties of high softening point homogeneous bitumen are: softening point 245℃, coking value 63%, quinoline insoluble content 3%, ash content 0.002%, and yield 21% (calculated based on the total weight of the starting aromatic feedstock).
[0181] Comparative Example 2
[0182] This comparative example provides a process for co-producing purified bitumen and homogeneous bitumen, which is achieved using the system for co-producing petroleum purified bitumen and high softening point special bitumen provided in Example 1 (but this system does not include a modifier storage tank and a mixing tank), and includes the following specific steps:
[0183] Step (a): Selection and pretreatment of raw materials:
[0184] Catalytic cracking slurry was selected as the first aromatic feedstock. The first aromatic feedstock was filtered using the first filter 1-1 and the second filter 1-2, respectively. After removing solid particles, aromatic feedstock 1* was obtained and stored in the first feedstock tank 3 for later use. Simultaneously, the second valve 1-10 on the pipeline between the second outlet of the first feedstock tank 3 and the sixth high-temperature gear pump 1-8 was closed. The ash content of aromatic feedstock 1* was 5 ppm, and its density (20℃) was 1.12 g / cm³. 3 The total aromatic hydrocarbon content is 75%, of which, by total weight, tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings account for 13%, 62%, 20% and 5% respectively. The distillation range is 380-550℃, the sulfur content is 0.28% and the nitrogen content is 0.15%.
[0185] Step (b): Preparation of aromatic basic components:
[0186] Aromatic feedstock 1* is fed into heat exchanger 4, where it is heated to 300°C by heat transfer oil at 340°C. It then enters the upper part of fractionation tower 5 for the regulation of aromatic molecular structure and composition distribution. Fractionation tower 5 operates under reduced pressure (30-50 kPa), with the upper part at 120-150°C and the lower part at 290-310°C. The lower part yields the basic aromatic components, while the top yields high-temperature oil and gas, which is recovered through a first vacuum device. The recovery process includes: the oil and gas first enters the first oil and gas buffer tank 8-1; the separated gas phase is cooled by heat exchange in the first condenser 9-1; the pressure of the first vacuum device is 50 kPa; and the condensing medium in the first condenser 9-1 is cooling water. The first side stream from fractionation tower 5 yields light aromatic oil with a density (20°C) of 0.743 g / cm³. 3 The oil extracted from the second to fifth side streams is medium-quality aromatic oil, with a density (20℃) of 0.802 g / cm³. 3 .
[0187] Step (c): Preparation of purified base bitumen:
[0188] The aromatic basic components are fed into a tubular heater 13, and steam is injected into its tubes. After heating in the tubular heater 13, the outlet temperature is 330℃. The gas flow rate to the mass ratio of aromatic basic components is 5L / min:100kg aromatic basic components. The heated aromatic basic components are then fed into the first reactor 14 through the second feed inlet at the bottom. The material resides in the first reactor 14 for 8 hours. The internal temperature of the first reactor 14 is 330℃, and the pressure is atmospheric pressure. After the molecular weight distribution of the aromatic basic components is initially adjusted in the first reactor 14, purified base asphalt and high-temperature oil and gas (medium aromatic oil and light aromatic oil) are obtained. (Oil and gas); medium-quality aromatic oil and light oil and gas are recovered through the first vacuum device. The specific process is as follows: high-temperature oil and gas are extracted from the top of the first reactor 14 and first enter the first oil and gas buffer tank. The separated gas phase is then cooled by heat exchange in the first condenser to separate the medium-quality aromatic oil. The non-condensable vapor enters the first cryogenic cooler for cooling. The temperature of the first oil and gas buffer tank is 200℃, the condensing medium used in the first condenser is cooling water at a temperature of 10℃, the cooling medium used in the first cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the first vacuum device is 50KPa. The density of the separated medium-quality aromatic oil (at 20℃) is 0.801g / cm³. 3 ;
[0189] Tests showed that the purified base asphalt obtained in this step had the following properties: softening point 78℃, coking value 22%, quinoline insoluble content 0%, and ash content 0.001%.
[0190] Step (d): Preparation of homogeneous asphalt products:
[0191] The purified base asphalt overflows from the second outlet at the top of the first reactor 14 and enters the first asphalt buffer tank 15. Then, it enters the second reactor 16 by gravity for reaction. The internal temperature of the second reactor 16 is 360℃, the stirring speed is 150 r / min, the residence time of the purified base asphalt in the second reactor 16 is 5 hours, and the pressure is 10 Pa. After the reaction, the purified base asphalt produces a high softening point homogeneous asphalt product and high-temperature oil and gas, which contains heavy aromatic oil and light gas. The heavy aromatic oil and light oil and gas in the high-temperature oil and gas are recovered by a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the second reactor 16 and first enters the second oil and gas buffer tank 8-2. The separated gas phase then passes through the second condenser 9-2 to separate the heavy aromatic oil, which has a density (20℃) of 0.83 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 200℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 10Pa.
[0192] Tests showed that the homogeneous asphalt product obtained in this step had a softening point of 150℃, a coking value of 40%, a quinoline insoluble content of 0.03%, and an ash content of 0.0012%. Based on the properties of the homogeneous asphalt product obtained in step (d), it is clear that it no longer falls within the range of indicators for high softening point homogeneous asphalt.
[0193] Step (e): Preparation of homogeneous bitumen products:
[0194] The homogeneous asphalt product obtained from the second reactor 16 is fed into the second asphalt buffer tank 17 at a temperature of 310°C. It is then transported to the third reactor 18 via the fifth high-temperature gear pump 1-7. Nitrogen gas is injected into the insulated transport pipeline carrying the homogeneous asphalt product, maintaining a mass ratio of homogeneous asphalt product to nitrogen flow rate of 100 kg: 4 L / min. The stirring speed of the wall-scraping frame agitator 18-1 in the third reactor 18 is 50 r / min. The diameter ratio of the bottom agitator 18-2 to the diameter of the third reactor 18 is 1:5. Nitrogen gas is introduced into the bottom of the bottom agitator 18-2 in the third reactor 18. The temperature inside the third reactor 18 is 370°C, and the reaction residence time is 6 hours, resulting in a homogeneous asphalt product after deep reaction. The product is discharged from the bottom through a heated pipeline (the heated pipeline is located at the bottom outlet of the third reactor). The temperature of the heated pipeline is 330℃. During the discharge process, the product first passes through a magnetic field with a magnetic field strength of 0.5T perpendicular to the heated pipeline, and then is filtered through a ceramic filter with a mesh size of 200 mesh. After cooling, the product is collected to obtain an ultra-high softening point homogeneous asphalt product. At the same time, high-temperature oil and gas (heavy aromatic oil and light oil and gas) is extracted from the top of the third reactor 18. The high-temperature oil and gas is recovered using a second vacuum device. Specifically, the high-temperature oil and gas is extracted from the top of the third reactor and first enters the second oil and gas buffer tank. The separated gas phase is then separated into heavy aromatic oil by the second condenser. The density (20℃) of the heavy aromatic oil is 0.85 g / cm³. 3 Non-condensable vapors enter the second cryogenic cooler for cooling; the temperature of the second oil-gas buffer tank is 190℃, the condensing medium used in the second condenser is cooling water at a temperature of 8℃, the cooling medium used in the second cryogenic cooler is a mixture of water and ethylene glycol at a temperature of -40℃, and the pressure of the second vacuum device is 2Pa.
[0195] Testing revealed that the homogeneous asphalt product obtained in this step had the following properties: softening point 203℃, coking value 48%, quinoline insoluble content 0.1%, ash content 0.002%, and yield 35% (calculated based on the total weight of the starting aromatic raw materials). Based on the properties of the homogeneous asphalt product obtained in step (e), it is clear that it no longer falls within the range of indicators for ultra-high softening point homogeneous asphalt.
[0196] The difference between this comparative example and Example 2 is that aromatic raw material 2 was not used in step (a), and no reaction modifier was added. Comparing the property parameters of the products obtained in Example 2 and this comparative example, it can be seen that the degree of the first reaction is reduced in this comparative example. Although the softening point and coking value will continue to increase in the subsequent reactions, they cannot reach the index of high softening point asphalt, nor can they form ultra-high softening point asphalt products.
[0197] The above description is merely a specific embodiment of the present invention and should not be construed as limiting the scope of the invention. Therefore, any substitution of equivalent components or equivalent changes and modifications made within the scope of protection of this patent should still fall within the scope of this patent. Furthermore, the technical features, technical features and technical inventions, and technical inventions in this invention can be freely combined and used.
Claims
1. A system for co-producing petroleum-purified bitumen and high-softening-point specialty bitumen, characterized in that, The system for co-producing petroleum purified bitumen and high softening point special bitumen includes: a first raw material tank, a second raw material tank, a modifier storage tank, a mixing tank, a heat exchanger, a distillation unit, a first gas source, a heating unit, a first reactor, a second reactor, a third reactor, and a second gas source; The second raw material tank and the conditioning agent storage tank are connected to the mixing tank through pipelines. The first outlet of the first raw material tank and the outlet of the mixing tank are connected to the inlet of the distillation unit through pipelines via a three-way valve or a mixing device. The outlet of the distillation unit for aromatic basic components is connected to the inlet of the first reactor through pipelines via a heating device. The first gas source is connected to the heating device through pipelines. The outlet of the first reactor is connected to the inlet of the second reactor through pipelines. The outlet of the second reactor and the outlet of the second gas source are connected to the inlet of the third reactor through pipelines. The second outlet of the first raw material tank is connected to the inlet of the first reactor via a pipeline through a heating device. A first valve and a second valve are respectively installed on the pipeline between the first outlet of the first raw material tank and the three-way valve or the mixing device, and on the pipeline between the second outlet of the first raw material tank and the heating device.
2. The system according to claim 1, characterized in that, The system further includes a first vacuum device and a second vacuum device. The high-temperature oil and gas outlets of the distillation device and the first reactor are respectively connected to the first vacuum device via pipelines, and the high-temperature oil and gas outlets of the second reactor and the third reactor are respectively connected to the second vacuum device via pipelines. The first vacuum device includes a first oil and gas buffer tank, a first condenser, a first cryogenic cooler, and a first vacuum unit connected in sequence via pipelines. The second vacuum device includes a second oil and gas buffer tank, a second condenser, a second cryogenic cooler, and a second vacuum unit connected in sequence via pipelines.
3. The system according to claim 1, characterized in that, The third reactor is equipped with a wall-scraping frame agitator and a bottom agitator, and the outlet of the second gas source is also connected to the bottom agitator via a pipeline.
4. The system according to claim 1 or 3, characterized in that, The outlet of the third reactor is connected to the cooling and collecting device through a heat tracing pipeline. An external magnetic strip is installed outside the heat tracing pipeline, and a second filter device is installed inside the heat tracing pipeline between the external magnetic strip and the cooling and collecting device.
5. A process for co-producing purified bitumen and homogeneous bitumen, characterized in that, The process is implemented using the system described in any one of claims 1-4, and includes: Step (1): Filter the first aromatic raw material to obtain aromatic raw material 1*, mix the second aromatic raw material and the modifier to obtain aromatic raw material 2*, mix aromatic raw material 1* and aromatic raw material 2* to obtain mixed aromatic oil, heat the mixed aromatic oil and then perform component adjustment and further impurity removal in a distillation device to obtain the basic aromatic components. Step (2): The aromatic basic components and crosslinking gas are heated and then introduced into the first reactor to react, thereby obtaining purified basic asphalt; Step (3): The purified base asphalt is introduced into the second reactor for reaction to obtain a high softening point homogeneous asphalt product; Step (4): After mixing the high softening point homogeneous asphalt product with inert gas, the mixture is introduced into the third reactor. The high softening point homogeneous asphalt product undergoes deep reaction and molecular weight adjustment in the third reactor to obtain ultra-high softening point homogeneous asphalt.
6. The process according to claim 5, characterized in that, The process further includes step (5): using a first vacuum device to sequentially heat and separate, condense and separate, and cryogenically treat the high-temperature oil and gas generated by the distillation device in step (1) and the first reactor in step (2), and using a second vacuum device to sequentially heat and separate, condense and separate, and cryogenically treat the high-temperature oil and gas generated by the second reactor in step (3) and the third reactor in step (4); wherein the temperatures of the heating separation, the condensation separation, and the cryogenic treatment are 190-220℃, 2-10℃, and -40 to -30℃, respectively, the pressure of the first vacuum system is 30-50KPa, and the pressure of the second vacuum device is 1-10Pa.
7. The process according to claim 5 or 6, characterized in that, The first aromatic feedstock includes one or a combination of several of the following: catalytic cracking slurry oil or its distillate oil, catalytic cycle oil or its distillate oil, solvent-de-oiled asphalt or its distillate oil, and thermal cracking residue oil or its distillate oil. The second aromatic feedstock includes one or a combination of several of the following: ethylene tar or its distillate oil, hydrogenated ethylene tar wax oil or its distillate oil, coking wax oil or its distillate oil, furfural extract oil or its distillate oil, and deasphalted vacuum residue oil or its distillate oil.
8. The process according to claim 7, characterized in that, The total aromatic hydrocarbon content in the second aromatic hydrocarbon feedstock is 70-90%, of which, based on the total weight of total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons and aromatic hydrocarbons with more than five rings are 1-5%, 25-35%, 50-60% and 10-20%, respectively. The total aromatic hydrocarbon content in the aromatic raw material 1* is 60-80%, wherein, based on the total weight of the total aromatic hydrocarbons, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons, and aromatic hydrocarbons with more than five rings are 10-20%, 60-70%, 10-20%, and 5-10%, respectively.
9. The process according to claim 5, characterized in that, In step (1), the second aromatic raw material and the modifier are mixed at a weight ratio of 1000:1-10. The mixing temperature is 30-40℃, the time is 0.5-1h, and the stirring speed is 800-900r / min.
10. The process according to claim 5 or 9, characterized in that, In step (1), the modifier is a quinone compound, including 9,10-anthraquinone and / or 1,4-naphthoquinone.
11. The process according to claim 5 or 9, characterized in that, In step (1), aromatic raw material 1* and aromatic raw material 2* are mixed in a weight ratio of 1-3:10, the mixing temperature is 100-150℃, and the linear velocity is 0.3-0.5m / s.
12. The process according to claim 5 or 9, characterized in that, In step (1), the distillation apparatus is operated under normal or reduced pressure, with a pressure of 30-50 kPa. The upper part of the distillation apparatus has a temperature of 120-150°C, and the lower part has a temperature of 360-380°C. The lower part yields the basic aromatic components.
13. The process according to claim 5, characterized in that, In step (2), the crosslinking gas and the aromatic basic component are mixed at a gas flow rate to aromatic basic component weight ratio of 1-5:100 and then heated to 310-350℃. The gas flow rate is in L / min and the aromatic basic component weight is in kg.
14. The process according to claim 5 or 13, characterized in that, In step (2), the internal temperature of the first reactor is 310-350℃, and the reaction residence time is 5-10h.
15. The process according to claim 5 or 6, characterized in that, In step (3), the internal temperature of the second reactor is 330-360℃, and the reaction residence time is 5-10h.
16. The process according to claim 5, characterized in that, In step (4), inert gas and high softening point homogeneous asphalt product are mixed at a gas flow rate to high softening point homogeneous asphalt product weight ratio of 1-5:100, where the gas flow rate is in L / min and the high softening point homogeneous asphalt product weight is in kg.
17. The process according to claim 5 or 16, characterized in that, In step (4), the internal temperature of the third reactor is 350-380℃, and the reaction residence time is 5-10h.
18. A process for co-producing base asphalt and mesophase asphalt, characterized in that, The process is implemented using the system described in any one of claims 1-4, and includes: Step 1): Filter the first aromatic raw material to obtain aromatic raw material 1*, heat the aromatic raw material 1* and let it enter the first reactor to react and obtain the base asphalt; Step 2): The base asphalt is fed into the second reactor to react and generate mesophase components, resulting in mesophase asphalt with a low softening point. Step 3): Mix the low-softening-point mesophase pitch with an inert gas and then introduce it into the third reactor. The low-softening-point mesophase pitch undergoes a deep reaction in the third reactor to obtain high-quality spinnable mesophase pitch.
19. The process according to claim 18, characterized in that, In step 1), the first aromatic feedstock includes one or a combination of several of the following: catalytic cracking slurry or its distillate oil, catalytic cycle oil or its distillate oil, solvent-de-oiled residue asphalt or its distillate oil, and thermal cracking residue or its distillate oil. The ash content of the aromatic feedstock 1* is less than 50 ppm, and its density at 20°C is 1.01-1.12 g / cm³. 3 The total aromatic hydrocarbon content is 60-80%, of which, by total weight, the contents of tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, pentacyclic aromatic hydrocarbons, and aromatic hydrocarbons with more than five rings are 10-20%, 60-70%, 10-20%, and 5-10%, respectively. The distillation range is 350-580℃, the sulfur content is 0.1-0.3%, and the nitrogen content is 0.05-0.2%.
20. The process according to claim 18 or 19, characterized in that, In step 1), the internal temperature of the first reactor is 330-360℃, and the reaction residence time is 5-10h; And / or, in step 2), the internal temperature of the second reactor is 410-430℃, the reaction residence time is 1-5h, and the reaction pressure is 3-5MPa; And / or, in step 3), the internal temperature of the third reactor is 390-430℃, and the reaction residence time is 5-10h.
Citation Information
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