A process and system for co-production of impregnating pitch and coating pitch
By fractionating and controlling the polymerization reaction of ethylene tar and catalytic slurry, the problems of complex production processes and low raw material utilization of impregnated and coated asphalt have been solved, enabling the large-scale production of high-performance asphalt, which is suitable for high-performance graphite electrodes and lithium-ion battery anode materials.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHINA PETROLEUM & CHEMICAL CORP
- Filing Date
- 2024-12-06
- Publication Date
- 2026-06-09
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Figure CN122168316A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of petrochemicals and relates to methods and systems for producing asphalt, particularly to a method and system for producing impregnated asphalt and coated asphalt. Background Technology
[0002] Impregnating bitumen is a common densifying and reinforcing agent in carbon material production, mainly used to generate high-power and ultra-high-power graphite electrodes and high-tech carbon products. Impregnating bitumen generally needs to possess good rheological properties, penetration performance, and a good coking value. To improve the quality of electrodes and electrode joints and reduce electrode energy consumption, it is crucial to increase the bulk density and strength of the electrodes and electrode joints. Currently, most industries in China use ordinary medium-temperature bitumen as a substitute for impregnating bitumen, resulting in unstable product quality, high energy consumption, and difficulty in meeting high-level application requirements. This seriously hinders product upgrading and replacement in the graphite industry. Therefore, a method for large-scale production of high-quality impregnating bitumen is needed.
[0003] Coated bitumen is mainly used for surface coating of graphite materials, which can improve the cycle stability and coulombic efficiency of lithium-ion battery anode materials. Currently, coated bitumen is expensive and suffers from poor product performance and low yield. Softening point is an important indicator reflecting the high-temperature stability of bitumen; the higher the value, the better the high-temperature stability of the bitumen. Softening point is mainly affected by factors such as composition, structure, and temperature.
[0004] Patent CN105271168A discloses a method for the continuous preparation of mesophase carbon microspheres and the co-production of impregnating agent pitch and coated pitch. The method uses medium-temperature coal tar pitch as raw material, adds a stabilizer for mixing, first heats at a low temperature, then performs a short-term high-temperature polymerization reaction, cools down, mixes with an extractant for extraction, centrifuges, and then feeds into a reactor for a modification reaction. This process requires both stabilizers and extractants, involves an extractant recovery process, and is complex.
[0005] Patent CN110540855 A discloses a petroleum-based impregnated bitumen and its preparation method. The method involves solvent deasphalting of catalytic cracking slurry, mixing purified reduced-triple-line furfural extract oil or reduced-quadruple-line furfural extract oil with the purified catalytic cracking slurry in a specific ratio, and then performing a thermal polymerization reaction. The resulting product is distilled to remove light components, thus obtaining the impregnated bitumen. This process requires solvent deasphalting experiments, involves solvent use and recovery processes, and is complex in its production process. Summary of the Invention
[0006] To address the shortcomings of existing technologies, the main objective of this invention is to provide a method and system for the co-production of impregnated bitumen and coated bitumen. The provided production method utilizes the oxidizing light components generated during the oxidation process of coated bitumen production as the oxidant for producing impregnated bitumen. The resulting impregnated bitumen has advantages such as high coking value, low quinoline insoluble content, and low ash content. Graphite electrodes prepared using this asphalt exhibit high bulk density and can be used as ultra-high power graphite electrodes. The resulting coated bitumen has advantages such as low quinoline insoluble content and low ash content. The provided production method offers advantages such as readily available raw materials, high raw material utilization, controllable product softening point, and easy large-scale production of high-quality impregnated bitumen and coated bitumen, solving the problems of complex production processes, low raw material utilization, difficulty in controlling the softening point of coated bitumen, and high quinoline insoluble content in existing technologies.
[0007] The technical solution of this invention includes the following aspects:
[0008] A first aspect of the present invention provides a method for co-producing impregnated bitumen and coated bitumen, the method comprising the following steps:
[0009] (1) The first raw material is separated to obtain a first light fraction and a first heavy fraction;
[0010] (2) The second raw material is separated to obtain a second light fraction, a middle fraction and a second heavy fraction;
[0011] (3) The first light fraction obtained in step (1) and the second light fraction obtained in step (2) enter the first reaction unit for the first heat treatment to obtain the first feed stream;
[0012] (4) The first heavy fraction obtained in step (1) enters the second reaction unit for a second heat treatment to obtain the second feed stream;
[0013] (5) The second heavy fraction obtained in step (2) enters the third reaction unit for third heat treatment to obtain the third feed stream;
[0014] (6) Under the presence of an oxygen-containing atmosphere, the second material stream obtained in step (4) and the third material stream obtained in step (5) enter the fourth reaction unit for the fourth heat treatment. After the treatment is completed, light components and coated asphalt are obtained.
[0015] (7) The intermediate fraction obtained in step (2), the first feed stream obtained in step (3) and the light component obtained in step (6) enter the fifth reaction unit for the fifth heat treatment, and after treatment, the gaseous feed stream and impregnated asphalt are obtained.
[0016] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the first raw material is ethylene tar, and the total content of saturated and aromatic components in the ethylene tar is not less than 70%, preferably 71% to 85%; furthermore, the ash content in the ethylene tar is not higher than 0.01 wt%.
[0017] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the second raw material is catalytic oil slurry, and the total content of saturated and aromatic components in the catalytic oil slurry is not less than 80%, preferably 85% to 94%; furthermore, the ash content in the catalytic oil slurry is not higher than 0.04 wt%.
[0018] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the cutting temperature of the first light fraction and the first heavy fraction in step (1) is 250-270°C, preferably 258-265°C.
[0019] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the cutting temperatures of the second light fraction and the middle fraction in step (2) are 250℃~280℃, preferably 260℃~275℃; the cutting temperatures of the middle fraction and the second heavy fraction are 350℃~480℃, preferably 350~460℃.
[0020] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the first reaction unit in step (3) is carried out under the following operating conditions: the first heat treatment temperature is 350-480°C, preferably 360-420°C, and the material residence time is 1-9h, preferably 0.5-8h.
[0021] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the second reaction unit is carried out under the following operating conditions: the second heat treatment temperature is 360-420°C, preferably 365-385°C, and the material residence time is 0.5-12h, preferably 2-4.5h.
[0022] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the second heat treatment in step (4) is carried out under an inert atmosphere protection condition, wherein the inert atmosphere can be nitrogen and / or an inert gas, and the inert gas can be at least one of helium, neon, argon, krypton, and xenon.
[0023] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the third reaction unit is carried out under the following operating conditions: the third heat treatment temperature is 360-420°C, preferably 380-410°C, and the material residence time is 0.5-12h, preferably 4-8h.
[0024] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the third heat treatment in step (5) is carried out under an inert atmosphere protection condition, wherein the inert atmosphere can be nitrogen and / or an inert gas, and the inert gas can be at least one of helium, neon, argon, krypton, and xenon.
[0025] In the above-mentioned method for co-producing impregnated asphalt and coated asphalt, as a preferred embodiment, the oxygen volume concentration in the oxygen-containing atmosphere in step (6) is 18% to 100%, preferably 20% to 28%; the oxygen-containing atmosphere can be a mixture of oxygen, air, oxygen and an inert atmosphere, and the inert atmosphere can be nitrogen and / or an inert gas.
[0026] In the above-described method for co-producing impregnated asphalt and coated asphalt, as a preferred embodiment, the oxygen-containing atmosphere in step (6) is preferably in countercurrent contact with the feed (the mixed feed stream of the second and third feed streams), and the flow rate of the oxygen-containing atmosphere can be controlled to be 0.1–1.5 m³ / s. 3 / min.
[0027] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the light component obtained in step (6) can enter the fifth reaction unit and undergo a fifth heat treatment together with the intermediate fraction obtained in step (2) and the first feed stream obtained in step (3).
[0028] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the fourth reaction unit is carried out under the following operating conditions: the fourth heat treatment temperature is 350-420°C, preferably 360-410°C, and the reaction time is 0.5-8 hours, preferably 1-6 hours.
[0029] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the softening point of the second material flow obtained in step (4) is generally controlled to be 90-195℃, preferably 105-160℃.
[0030] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the softening point of the third material flow obtained in step (5) is generally controlled at 120-280℃, preferably 135-245℃.
[0031] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the mass ratio of the second material stream and the third material stream in step (6) is generally controlled to be 1:(0.1-1).
[0032] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the fifth reaction unit is carried out under the following operating conditions: the reaction temperature is 260-450℃, preferably 300-360℃; the reaction time is 0.5-8h, preferably 3-6h.
[0033] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the fifth heat treatment in the fifth reaction unit in step (7) can be carried out in the presence of an oxygen-containing atmosphere, wherein the oxygen concentration in the oxygen-containing atmosphere is 18%-100%; the oxygen-containing atmosphere can be a mixture of oxygen, air, oxygen and an inert atmosphere, and the inert atmosphere can be nitrogen and / or an inert gas.
[0034] In the above-mentioned method for co-producing impregnated asphalt and coated asphalt, as a preferred embodiment, the gaseous material stream obtained after treatment in step (7) is preferably processed in the third reaction unit.
[0035] In the above-mentioned method for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the obtained impregnated bitumen has a softening point greater than or equal to 90℃; quinoline insoluble matter greater than 0.2wt%; coking value greater than or equal to 45wt%; volatile matter content less than or equal to 60wt%; and ash content less than 0.1wt%. Furthermore, the graphite electrode prepared using this impregnated bitumen exhibits a weight gain of not less than 11wt% after the impregnation process, and a bulk density of not less than 1.72 g / cm³. 3 .
[0036] A second aspect of the present invention provides a system for co-producing impregnated bitumen and coated bitumen, the system comprising:
[0037] The first separation unit is used to receive and separate the first raw material, and obtain a first light fraction and a first heavy fraction after separation.
[0038] The second separation unit is used to receive and separate the second feedstock oil, and after separation, a second light fraction, a middle fraction and a second heavy fraction are obtained.
[0039] The first reaction unit is used to receive the first light fraction from the first separation unit and the second light fraction from the second separation unit, and obtains the first feed stream after the heat treatment reaction is completed;
[0040] The second reaction unit is used to receive the first heavy fraction from the first separation unit and react it to obtain the second feed stream.
[0041] The third reaction unit is used to receive the second heavy fraction from the second separation unit and react it to obtain the third feed stream.
[0042] The fourth reaction unit is used to receive the second feed stream from the second reaction unit and the third feed stream from the third reaction unit, and after the reaction, light components and coated asphalt are obtained;
[0043] The fifth reaction unit is used to receive the first material stream obtained from the first reaction unit and the intermediate fraction from the second separation unit, and after the reaction, obtains a gaseous material stream and impregnated bitumen.
[0044] In the aforementioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the first separation unit includes at least one device capable of cutting materials according to their distillation range, specifically a fractionating tower, and particularly preferably a vacuum distillation tower.
[0045] In the aforementioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the second separation unit includes at least one device capable of cutting materials according to the distillation range, specifically at least one of a vacuum distillation tower and a flash distillation tower.
[0046] In the aforementioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the light component generated by the fourth reaction unit is connected to the fifth reaction unit via a pipeline, and the light component enters the fifth reaction unit for processing together with the first material stream and the intermediate fraction of the second separation unit.
[0047] In the above-mentioned system for co-producing impregnated asphalt and coated asphalt, as a preferred embodiment, the gaseous material flow obtained after the reaction in the fifth reaction unit is connected to the third reaction unit via a pipeline, and the gaseous material flow enters the third reaction unit for processing.
[0048] In the above-mentioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the first reaction unit may be a batch reactor or a tank reactor.
[0049] In the above-mentioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the second reaction unit, the third reaction unit and the fourth reaction unit can each adopt at least one of the following: tower reactor, tank reactor and batch reactor.
[0050] In the above-mentioned system for co-producing impregnated bitumen and coated bitumen, as a preferred embodiment, the fifth reaction unit can be at least one of a tower reactor, a tank reactor, and a batch reactor.
[0051] Compared with the prior art, the method and system for co-producing impregnated bitumen and coated bitumen provided by the present invention have one or more of the following beneficial effects:
[0052] 1. The method for co-producing impregnated asphalt and coated asphalt provided by this invention, based on the perspective of molecular petroleum processing, involves the processing of two raw materials. Specifically, the first raw material is separated into two different fractions, and the second raw material oil is separated into three different fractions. First, the two light fractions are processed, and then the middle fraction of the second raw material is mixed with the processed light fractions to produce impregnated asphalt. The two heavy fractions are introduced into the second and third reaction units for processing, respectively. By controlling the reaction temperature and other conditions of materials with different polymerization capacities, two asphalts with different degrees of polymerization are generated. The mixed asphalt obtained by blending the two asphalts is then used to prepare coated asphalt. This effectively controls the softening point and quinoline insoluble content of the coated asphalt. The light components obtained from the reaction are recycled back to the fifth reaction unit as an oxidant in the impregnated asphalt reaction. This process allows for flexible adjustment of the production of impregnated and coated asphalt, control of the asphalt oxidation depth, and the use of the light components produced from the coated asphalt as an oxidant in the production of impregnated asphalt. The production method for co-producing impregnated bitumen and coated bitumen provided by this invention can maximize the utilization of raw materials, control the production volume of impregnated bitumen and coated bitumen, and flexibly adjust the production process according to the market demand for different types of bitumen to maximize profits.
[0053] 2. This invention provides a method and system for producing coated asphalt from impregnated asphalt for high-bulk-density graphite electrodes. It avoids introducing highly corrosive liquid or gaseous catalysts and utilizes the gaseous material stream generated in the fifth reaction unit to return to the third reaction unit, improving material utilization and providing raw materials with oxidizing functions. This facilitates the synthesis of coated asphalt at lower reaction temperatures, effectively increasing the softening point of the asphalt while maintaining a low quinoline insoluble content. Furthermore, it helps reduce production costs and promotes large-scale industrialization. Moreover, graphite electrodes prepared from impregnated asphalt produced using this process are beneficial for producing high-power graphite electrodes. Attached Figure Description
[0054] Figure 1 This is a schematic diagram of the method for co-producing impregnated bitumen and coated bitumen provided by the present invention.
[0055] Wherein: 1-First raw material, 2-Second raw material, 3-First separation unit, 4-Second separation unit, 5-First light fraction, 6-First heavy fraction, 7-Second light fraction, 8-Middle fraction, 9-Second heavy fraction, 10-First heating furnace, 11-Second heating furnace, 12-Heated first heavy fraction, 13-Heated second heavy fraction, 14-First reaction unit, 15-First feed stream, 16-Second reaction unit, 17-Third reaction unit, 18-Fifth reaction unit, 19-Gas phase feed stream, 20-Impregnated asphalt, 21-First carrier gas, 22-Second carrier gas, 23-Second feed stream, 24-Third feed stream, 25-Mixed feed stream, 26-Fourth reaction unit, 27-Oxygen-containing atmosphere, 28-Light component, 29-Coated asphalt. Detailed Implementation
[0056] The specific embodiments of the present invention will be described in detail below. However, it should be noted that the scope of protection of the present invention is not limited to these specific embodiments, but is determined by the claims in the appendix.
[0057] All publications, patent applications, patents, and other references mentioned in this specification are incorporated herein by reference. Unless otherwise defined, all technical and scientific terms used in this specification have the meanings commonly understood by those skilled in the art. In case of conflict, the definitions in this specification shall prevail.
[0058] When this specification uses the prefixes “known to those skilled in the art,” “prior art,” or similar terms to derive materials, substances, methods, steps, apparatus, or components, the objects derived from such prefixes cover those commonly used in the art at the time of this application, but also include those that are not currently commonly used but will become generally recognized in the art as suitable for similar purposes.
[0059] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.
[0060] In the context of this specification, for ease of description, spatial relative terms such as “below,” “under,” “down,” “above,” “over,” “upper,” etc., may be used to describe the relationship of one element or feature to another element or feature in the accompanying drawings. It should be understood that spatial relative terms are intended to encompass different orientations of an object in use or operation, other than those depicted in the figures. For example, if an object in the figure is flipped, an element described as “below” or “under” another element or feature would be oriented “above” said element or feature. Thus, the exemplary term “below” can encompass both the downward and upward orientations. An object may also have other orientations (e.g., rotated 90 degrees or other orientations), and the spatial relative terms used herein should be interpreted accordingly.
[0061] In the context of this specification, the terms "first," "second," etc., are used to distinguish two different elements or parts, and are not used to define a specific position or relative relationship. In other words, in some embodiments, the terms "first," "second," etc., can also be used interchangeably.
[0062] In the context of this specification, all numeric values of parameters (e.g., quantities or conditions) should be understood to be modified by the term “about” in all cases, regardless of whether “about” actually appears before the numeric value.
[0063] In the context of this specification, the ash content of the raw materials is determined by method GB / T 508, and the sulfur content is determined by method SH / T0689.
[0064] Unless otherwise specified, all percentages, parts, ratios, etc. mentioned in this instruction manual are based on weight, and the pressure is gauge pressure.
[0065] In the context of this specification, softening point is determined using GB / T 4507-2014 and ASTM D3461-18 methods. Due to the wide range of softening points in the product asphalt, testing is conducted according to the national standard for Asphalt Softening Point Determination – Ring and Ball Method. A Mettler (DP90) high-temperature asphalt dropping point softening point tester is used for the determination of high softening point asphalt. Low softening point asphalt is determined according to national standards using water bath or oil bath methods.
[0066] In the context of this specification, coking value is determined using the method of GB / T 8727-2008.
[0067] In the context of this specification, the content of quinoline insolubles is determined by the method of GB / T 2293-2019.
[0068] In the context of this specification, any two or more embodiments of the present invention can be arbitrarily combined, and the resulting technical solutions are part of the original disclosure of this specification and also fall within the protection scope of the present invention.
[0069] like Figure 1 The present invention provides a method for co-producing impregnated bitumen and coated bitumen, the specific process flow of which is as follows: First raw material 1 enters first separation unit 3, and after separation, a first light fraction 5 and a first heavy fraction 6 are obtained; second raw material 2 enters second separation unit 4, and after separation, a second light fraction 7, an intermediate fraction 8, and a second heavy fraction 9 are obtained; wherein the first light fraction 5 obtained from first separation unit 3 and the second light fraction 7 obtained from second separation unit 4 enter first reaction unit 14, and after reaction, a first feed stream 15 is obtained; the first heavy fraction 6 obtained from first separation unit 3 is heated by first heating furnace 10 to obtain a heated first heavy fraction 12. The first heavy fraction 12 enters the second reaction unit 16 and reacts in the presence of the first carrier gas 21, resulting in a second feed stream 23. The second heavy fraction 9 obtained from the second separation unit 4 is heated by the second heater 11 to obtain a heated second heavy fraction 13. The heated second heavy fraction 13 enters the third reaction unit 17 and reacts in the presence of the second carrier gas 22, resulting in a third feed stream 24. The second feed stream 23 and the third feed stream 24 are mixed to obtain a mixed feed stream 25, which enters the fourth reaction unit 26 and reacts in the presence of an oxygen-containing atmosphere 27, resulting in a light component 28 and coated asphalt 29. The intermediate fraction 8 obtained from the second separation unit 4, the first feed stream 15, and the light component 28 obtained from the fourth reaction unit enter the fifth reaction unit 18, resulting in a gaseous feed stream 19 and impregnated asphalt 20. The gaseous feed stream 19 can be returned to the third reaction unit 17 for further processing.
[0070] In the context of this specification, the raw materials used include four types: raw material A (ethylene tar 1), raw material B (ethylene tar 2), raw material C (catalytic oil slurry 1), and raw material D (catalytic oil slurry 2), the specific properties of which are shown in Table 1.
[0071] Table 1 Analysis of Raw Material Properties
[0072]
[0073]
[0074] Example 1
[0075] In Example 1, the first raw material is raw material A from Table 1, and the second raw material is raw material C. Figure 1The process flow describes a gaseous material stream entering a third reaction unit. The cutting point temperature of the first separation unit is 250℃, and the first cutting point temperature of the second separation unit is 280℃, while the second cutting point temperature is 350℃. The reaction temperature of the first reaction unit is 355℃, with a material residence time of 2 hours; the reaction temperature of the second reaction unit is 366℃, with a material residence time of 4 hours; the reaction temperature of the third reaction unit is 380℃, with a material residence time of 3 hours; the reaction temperature of the fourth reaction unit is 363℃, with a material residence time of 3 hours; the mass ratio of the second to the third material stream is 1:0.1; and the reaction temperature of the fifth reaction unit is 306℃, with a material residence time of 3.5 hours. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 90.1℃, a quinoline insoluble content of 0.02%, and a coking value of 46.1%. The properties of the coated asphalt are shown in Table 4, with a softening point of 181.3℃ and a quinoline insoluble content of 0.06%.
[0076] Example 2
[0077] In Example 2, the first raw material is raw material A from Table 1, and the second raw material is raw material D. Figure 1 The process flow described above includes a gaseous material stream entering the third reaction unit. The cutting point temperature of the first separation unit is 258℃, the first cutting point temperature of the second separation unit is 273℃, and the second cutting point temperature is 368℃. The reaction temperature of the first reaction unit is 391℃, and the material residence time is 4 hours; the reaction temperature of the second reaction unit is 371℃, and the material residence time is 2.5 hours; the reaction temperature of the third reaction unit is 394℃, and the material residence time is 5 hours; the reaction temperature of the fourth reaction unit is 368℃, and the material residence time is 3 hours; the mass ratio of the second and third material streams is 1:0.4; and the reaction temperature of the fifth reaction unit is 314℃, and the material residence time is 3 hours. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 92.4℃, a quinoline insoluble content of 0.03%, and a coking value of 46.9%. The properties of the coated asphalt are shown in Table 4, with a softening point of 211.4℃ and a quinoline insoluble content of 0.22%.
[0078] Example 3
[0079] In Example 3, the first raw material is raw material B from Table 1, and the second raw material is raw material C. Figure 1The process flow is as follows: the gaseous material stream enters the third reaction unit; the cutting point temperature of the first separation unit is 270℃; the first cutting point temperature of the second separation unit is 260℃; and the second cutting point temperature is 420℃. The reaction temperature of the first reaction unit is 443℃, and the material residence time is 5.5 hours; the reaction temperature of the second reaction unit is 377℃, and the material residence time is 3.5 hours; the reaction temperature of the third reaction unit is 403℃, and the material residence time is 4 hours; the reaction temperature of the fourth reaction unit is 399℃, and the material residence time is 4 hours; the mass ratio of the second and third material streams is 1:0.5; and the reaction temperature of the fifth reaction unit is 345℃, and the material residence time is 6 hours. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 93.4℃, a quinoline insoluble content of 0.03%, and a coking value of 48.5%. The properties of the coated asphalt are shown in Table 4, with a softening point of 235.9℃ and a quinoline insoluble content of 0.34%.
[0080] Example 4
[0081] In Example 4, the first raw material is raw material B from Table 1, and the second raw material is raw material D. Figure 1 The process flow is as follows: the gaseous material stream enters the third reaction unit; the cutting point temperature of the first separation unit is 255℃; the first cutting point temperature of the second separation unit is 270℃; and the second cutting point temperature is 465℃. The reaction temperature of the first reaction unit is 467℃, and the material residence time is 6 hours; the reaction temperature of the second reaction unit is 384℃, and the material residence time is 4.5 hours; the reaction temperature of the third reaction unit is 408℃, and the material residence time is 6 hours; the reaction temperature of the fourth reaction unit is 418℃, and the material residence time is 6 hours; the mass ratio of the second and third material streams is 1:1; and the reaction temperature of the fifth reaction unit is 357℃, and the material residence time is 5 hours. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 96.5℃, a quinoline insoluble content of 0.05%, and a coking value of 50.6%. The properties of the coated asphalt are shown in Table 4, with a softening point of 278.6℃ and a quinoline insoluble content of 0.46%.
[0082] Example 5
[0083] Similar to Example 2, except that the fumed feedstock does not enter the third reaction unit for processing. The properties of the impregnated bitumen product are shown in Table 3, with a softening point of 91.4℃, a quinoline-insoluble content of 0.04%, and a coking value of 44.8%. The properties of the coated bitumen are shown in Table 4, with a softening point of 201.3℃ and a quinoline-insoluble content of 0.32%.
[0084] Comparative Example 1
[0085] Comparative Example 1 is essentially the same as Example 1, except that a third reaction unit is not included. The first and second heavy fractions after heating are simultaneously processed in the second reaction unit. The gaseous stream 19 goes to the second reaction unit. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 96.7℃, a quinoline-insoluble content of 0.13%, and a coking value of 50.6%. The properties of the coated asphalt are shown in Table 4, with a softening point of 194.7℃ and a quinoline-insoluble content of 3.97%.
[0086] Comparative Example 2
[0087] Comparative Example 2 is essentially the same as Example 1, except that a second reaction unit is not provided; the first and second heavy fractions after heating are simultaneously processed in the third reaction unit. The properties of the impregnated bitumen product are shown in Table 3, with a softening point of 95.1℃, a quinoline-insoluble content of 0.12%, and a coking value of 56.4%. The properties of the coated bitumen are shown in Table 5, with a softening point of 186.8℃ and a quinoline-insoluble content of 3.45%.
[0088] Comparative Example 3
[0089] Comparative Example 3 is essentially the same as Example 1, except that the light component 28 was not processed in the fifth reaction unit. The properties of the impregnated bitumen product are shown in Table 3, with a softening point of 79.4°C, a quinoline-insoluble content of 0.13%, and a coking value of 38.9%. The properties of the coated bitumen are shown in Table 4, with a softening point of 190.1°C and a quinoline-insoluble content of 3.23%.
[0090] Comparative Example 4
[0091] Comparative Example 4 is essentially the same as Example 1, except that the middle fraction obtained after separating the second raw material is first mixed with the first and second light fractions and then processed in the first reaction unit to obtain the first feed stream, which then enters the fifth reaction unit for further processing. The properties of the impregnated asphalt product are shown in Table 3, with a softening point of 98.3℃, a quinoline-insoluble content of 0.22%, and a coking value of 59.6%. The properties of the coated asphalt are shown in Table 4, with a softening point of 194.3℃ and a quinoline-insoluble content of 3.86%.
[0092] Table 2 Process Conditions
[0093]
[0094]
[0095] Table 3 Properties of Impregnated Asphalt Products
[0096]
[0097] Table 4 Properties of Coated Asphalt Products
[0098]
Claims
1. A method for co-producing impregnated bitumen and coated bitumen, the method comprising the following steps: (1) The first raw material is separated to obtain a first light fraction and a first heavy fraction; (2) The second raw material is separated to obtain a second light fraction, a middle fraction, and a second heavy fraction; (3) The first light fraction obtained in step (1) and the second light fraction obtained in step (2) enter the first reaction unit for first heat treatment to obtain the first feed stream; (4) The first heavy fraction obtained in step (1) enters the second reaction unit for a second heat treatment to obtain the second feed stream; (5) The second heavy fraction obtained in step (2) enters the third reaction unit for third heat treatment to obtain the third feed stream; (6) Under the presence of an oxygen-containing atmosphere, the second material stream obtained in step (5) and the third material stream obtained in step (6) enter the fourth reaction unit for the fourth heat treatment. After the treatment is completed, light components and coated asphalt are obtained. (7) The intermediate fraction obtained in step (2), the first feed stream obtained in step (3) and the light component obtained in step (6) enter the fifth reaction unit for the fifth heat treatment. After treatment, the gaseous feed stream and impregnated asphalt are obtained; the gaseous feed stream is returned to the third reaction unit for use.
2. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The first raw material is ethylene tar, and the total content of saturated and aromatic components in the ethylene tar is not less than 70%, preferably 71% to 85%.
3. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The second raw material is catalytic oil slurry, and the total content of saturated and aromatic components in the catalytic oil slurry is not less than 80%, preferably 85% to 94%.
4. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The cutting temperature of the first light fraction and the first heavy fraction in step (1) is 250-270°C, preferably 258-265°C.
5. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The cutting temperatures of the second light fraction and the middle fraction in step (2) are 250℃~280℃, preferably 260℃~275℃; the cutting temperatures of the middle fraction and the second heavy fraction are 350℃~480℃, preferably 350~460℃.
6. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The first heat treatment temperature in step (3) is 350-480℃, preferably 360-420℃, and the material residence time is 1-9h, preferably 0.5-8h.
7. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The operating conditions of the second reaction unit are as follows: the second heat treatment temperature is 360-420℃, preferably 365-385℃, and the material residence time is 0.5-12h, preferably 2-4.5h.
8. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The second heat treatment in step (4) is carried out under an inert atmosphere, wherein the inert atmosphere is nitrogen and / or an inert gas, and the inert gas is at least one of helium, neon, argon, krypton, and xenon.
9. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The operating conditions for the third reaction unit are as follows: the third heat treatment temperature is 360–420℃, preferably 380–410℃, and the material residence time is 0.5–12h, preferably 4–8h.
10. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The third heat treatment in step (5) is carried out under an inert atmosphere, wherein the inert atmosphere is nitrogen and / or an inert gas, and the inert gas is at least one of helium, neon, argon, krypton, and xenon.
11. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The oxygen volume concentration in the oxygen-containing atmosphere in step (6) is 18-100%, preferably 20-28%; the oxygen-containing atmosphere is a mixture of oxygen, air, oxygen and an inert atmosphere, and the inert atmosphere is nitrogen and / or an inert gas.
12. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The operating conditions for the fourth reaction unit are as follows: the fourth heat treatment temperature is 350-420℃, preferably 360-410℃, and the reaction time is 0.5-8 hours, preferably 1-6 hours.
13. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The softening point of the second material flow obtained in step (4) is 90-195°C, preferably 105-160°C.
14. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The softening point of the third material flow obtained in step (5) is 120-280℃, preferably 135-245℃.
15. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, In step (6), the mass ratio of the second and third material flows is 1:(0.1-1).
16. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The operating conditions for the fifth reaction unit are as follows: the reaction temperature is 260-450℃, preferably 300-360℃; the reaction time is 0.5-8h, preferably 3-6h.
17. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, In step (7), the fifth heat treatment in the fifth reaction unit is carried out in the presence of an oxygen-containing atmosphere, wherein the oxygen volume concentration in the oxygen-containing atmosphere is 18%-100%; the oxygen-containing atmosphere is a mixture of oxygen, air, oxygen and an inert atmosphere, wherein the inert atmosphere is nitrogen and / or an inert gas.
18. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The obtained impregnated bitumen has a softening point greater than or equal to 90℃; quinoline insoluble matter greater than 0.2wt%; coking value greater than or equal to 45wt%; volatile matter content less than or equal to 60wt%; and ash content less than 0.1wt%.
19. The method for co-producing impregnated bitumen and coated bitumen according to claim 1, wherein, The gaseous material stream obtained after processing in step (7) enters the third reaction unit for further processing.
20. A system for co-producing impregnated bitumen and coated bitumen, the system comprising: The first separation unit is used to receive and separate the first raw material, and obtain a first light fraction and a first heavy fraction after separation. The second separation unit is used to receive and separate the second feedstock oil, and after separation, a second light fraction, a middle fraction and a second heavy fraction are obtained. The first reaction unit is used to receive the first light fraction from the first separation unit and the second light fraction from the second separation unit, and obtains the first feed stream after the heat treatment reaction is completed; The second reaction unit is used to receive the first heavy fraction from the first separation unit and react it to obtain the second feed stream. The third reaction unit is used to receive the second heavy fraction from the second separation unit and react it to obtain the third feed stream. The fourth reaction unit is used to receive the second feed stream from the second reaction unit and the third feed stream from the third reaction unit, and after the reaction, light components and coated asphalt are obtained; The fifth reaction unit is used to receive the first material stream obtained from the first reaction unit, the intermediate fraction from the second separation unit, and the light component from the fourth reaction unit, and after the reaction, obtains a gaseous material stream and impregnated bitumen.
21. The system for co-producing impregnated bitumen and coated bitumen according to claim 20, wherein, The first separation unit includes at least one device capable of cutting materials according to their distillation range, which is a fractionating column, particularly preferably a vacuum distillation column.
22. The system for co-producing impregnated bitumen and coated bitumen according to claim 20, wherein, The second separation unit includes at least one device capable of cutting materials according to the distillation range, selected from at least one of a vacuum distillation column and a flash distillation column.
23. The system for co-producing impregnated bitumen and coated bitumen according to claim 20, wherein, The first reaction unit employs at least one of a batch reactor or a tank reactor.
24. The system for co-producing impregnated bitumen and coated bitumen according to claim 20, wherein, The second, third, fourth, and fifth reaction units each employ at least one of the following: a tower reactor, a tank reactor, and a batch reactor.
25. The system for co-producing impregnated bitumen and coated bitumen according to claim 20, wherein, After the fifth reaction unit reacts, the resulting gaseous material flow is connected to the third reaction unit via a pipeline, and the gaseous material flow enters the third reaction unit for processing.