CN114736705A - Method and device for preparing coated asphalt by adopting ethylene tar and coated asphalt - Google Patents
Method and device for preparing coated asphalt by adopting ethylene tar and coated asphalt Download PDFInfo
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- CN114736705A CN114736705A CN202210401709.7A CN202210401709A CN114736705A CN 114736705 A CN114736705 A CN 114736705A CN 202210401709 A CN202210401709 A CN 202210401709A CN 114736705 A CN114736705 A CN 114736705A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
- C10C1/16—Winning of pitch
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
- C10C1/08—Winning of aromatic fractions
- C10C1/12—Winning of aromatic fractions naphthalene fraction heavy fraction
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/20—Refining by chemical means inorganic or organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method and a device for preparing coated asphalt by adopting ethylene tar and the coated asphalt, and relates to the field of petrochemical industry. The method for preparing the coated asphalt by adopting the ethylene tar comprises the following steps: distilling the ethylene tar to obtain a tar light component and a tar heavy component with an end point of less than 220-250 ℃; preparing BTX by taking the tar light component as a raw material; introducing heavy tar components into an oxidation crosslinking reactor, and simultaneously introducing gas with oxidability into the oxidation crosslinking reactor to carry out oxidation crosslinking reaction; and (3) introducing stripping gas into the oxidation crosslinking reactor after the oxidation crosslinking reaction is finished, and taking out light components generated by oxidation crosslinking by the stripping gas. The device comprises: a distillation device and an oxidation crosslinking reactor which are connected with each other, and a gas inlet pipe connected with the reactor. The coated asphalt is prepared by adopting the device and the method. The device related to the application has a simple structure, can prepare the coated asphalt with better performance, and can additionally produce raw materials for preparing BTX.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a method and a device for preparing coated asphalt by adopting ethylene tar and the coated asphalt.
Background
Graphite materials are widely used as negative electrode materials of lithium ion batteries because of their characteristics of high specific capacity, long-life cycle, low lithium intercalation/deintercalation platform voltage, and the like. However, due to the poor compatibility of the graphite electrode and the organic electrolyte, excessive SEI films are generated on the surface of the negative electrode, which not only consumes lithium ions in the electrolyte, but also greatly increases interfacial impedance, generates electrochemical dynamic barrier, and even dissociates and peels off the graphite layer of the electrode, so that the cycle performance and energy density of the lithium ion battery are greatly reduced, and the service life of the lithium ion battery is greatly reduced. In order to avoid the problem, a great number of researches are carried out by broad scholars on modification and modification of graphite, wherein the graphite surface is subjected to coating treatment, so that the wide attention of the scholars is effectively paid to the simple process. The method mainly coats a layer of amorphous carbon on the surface of graphite, and due to the good compatibility of the amorphous carbon and an organic solvent, the low-voltage platform and the high capacity of a graphite electrode are reserved, the direct contact between the graphite electrode and an electrolyte is avoided, the electrochemical impedance is reduced, and the cycle performance and the rate performance of the lithium ion battery are further improved.
At present, batch reactors are generally adopted in the preparation process of the coated asphalt, the preparation process needs frequent loading and unloading and cleaning of the reactors, and the working procedures easily cause unstable product quality, so that the development of a continuous production process and a continuous production device with stable product quality is particularly important. Moreover, the devices involved in the current preparation processes have the problems of complex structure, inconvenient use, low comprehensive utilization rate of raw materials and the like.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a method and a device for preparing coated asphalt by using ethylene tar and the coated asphalt.
The invention is realized by the following steps:
in a first aspect, the present invention provides a process for preparing coated asphalt from ethylene tar, comprising:
distilling the ethylene tar to obtain a tar light component and a tar heavy component with an end point of less than 220-250 ℃;
preparing BTX by taking the tar light component as a raw material;
introducing heavy tar components into an oxidation crosslinking reactor, and introducing gas with oxidability into the oxidation crosslinking reactor to perform oxidation crosslinking reaction;
and (3) introducing stripping gas into the oxidation crosslinking reactor after the oxidation crosslinking reaction is finished, and taking out light components generated by oxidation crosslinking by the stripping gas.
In an alternative embodiment, before the preparation of BTX using the tar light component as a raw material, the method further comprises: and separating out naphthalene substances in the light tar component.
In an alternative embodiment, the temperature of the oxidative crosslinking reaction is 350-400 deg.C, the pressure is 0.1(2MPa, the ratio of the flow rate of the gas with oxidizing property to the mass of the heavy tar component in the oxidative crosslinking reactor is 0.5-5 m3(min-1(t-1；
Preferably, the oxidative crosslinking reaction temperature is 350-380 deg.C, and the pressure is 0.1(1MPa, gas with oxidizing property)The ratio of the flow rate to the mass of the tar heavy component in the oxidation crosslinking reactor is 1(2 m)3(min-1(t-1；
Preferably, the reaction time is 3-8 h, more preferably 3-7 h;
preferably, the stirring speed of a stirring device in the oxidation crosslinking reactor is 200-500 r/min;
preferably, the gas having oxidizing property is air.
In an optional embodiment, when the liquid level in the oxidation crosslinking reactor reaches 50-80%, gas with oxidability is introduced into the oxidation crosslinking reactor.
In an optional embodiment, the stripping gas is steam, the stripping pressure is 0.1-2 MPa, the steam temperature is 350-400 ℃, and the steam flow is 1-3 times of the oxidizing gas flow;
preferably, the flow rate of the water vapor is 1-2 times of the flow rate of the oxidizing gas;
preferably, the stripping time is 1-3 h; the stripping time is more preferably 1-2 h.
In a second aspect, the present invention provides an apparatus for preparing coated asphalt from ethylene tar, comprising:
a distillation device, an oxidation crosslinking reactor and a gas inlet pipe; the heavy component discharge port of the distillation device is connected with the feed inlet of the oxidation crosslinking reactor, and the gas inlet pipe is connected with the gas inlet at the bottom of the oxidation crosslinking reactor.
In an alternative embodiment, a heater is disposed between the distillation apparatus and the oxidative crosslinking reactor.
In an alternative embodiment, the apparatus for preparing coated asphalt from ethylene tar further comprises a naphthalene separation unit, and a feed inlet of the naphthalene separation unit is connected with a light component outlet of the distillation apparatus.
In an alternative embodiment, the number of oxidative crosslinking reactors is 2, and 2 oxidative crosslinking reactors are arranged in parallel.
In a third aspect, the present invention provides a coated asphalt prepared by the method or the apparatus of any of the preceding embodiments.
The invention has the following beneficial effects:
the device that this application scheme related to simple structure has overcome the shortcoming such as product quality unstability that present cauldron formula reaction frequently loaded and unloaded material, cleaning process lead to, and the accessible is to the distillation treatment of raw materials, and the by-product hydrocracking prepares BTX raw materials, can make softening point 220 ~ 310 ℃, quinoline insoluble is < 1.5%, and the coating pitch of coking value 60 ~ 80%. In a preferred embodiment, two reactors are connected in parallel, so that stable and continuous production of the product quality can be realized; in a preferred embodiment, the naphthalene separation unit is arranged, so that naphthalene and methylnaphthalene can be produced as byproducts, the capacities of naphthalene, methylnaphthalene and coated asphalt can be flexibly adjusted according to market demands, and the comprehensive utilization of ethylene tar can be greatly improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic structural diagram of an apparatus for preparing coated asphalt from ethylene tar according to an embodiment of the present disclosure.
Icon: 1-a distillation apparatus; a 2-naphthalene separation unit; 3-a heater; 4-a first oxidative crosslinking reactor; 5-a second oxidative crosslinking reactor; 6-a first four-way valve; 7-a second four-way valve; 8-stripping gas inlet pipe; 9-feeding pipe; 10-a light component delivery pipe; 11-BTX feedstock delivery pipe; a 12-naphthalene product delivery pipe; 13-a heavy ends transfer line; 14-a high-temperature heavy component conveying pipe; 15-light component discharge pipe; 16-an oxidation gas inlet pipe; 17-heavy ends discharge pipe.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following provides a detailed description of the method, apparatus and coated asphalt for preparing coated asphalt from ethylene tar.
The application provides an adopt device of ethylene tar preparation cladding pitch, includes:
a distillation device 1, an oxidation crosslinking reactor and a gas inlet pipe; the heavy component outlet of the distillation device 1 is connected with the feed inlet of the oxidation crosslinking reactor, and the gas inlet pipe is connected with the gas inlet at the bottom of the oxidation crosslinking reactor.
Introducing ethylene tar serving as a raw material into a distillation device 1, and separating a tar light component with an initial boiling point of less than 220-250 ℃ to obtain a tar heavy component; heating the heavy component, carrying out oxidation crosslinking reaction with gas with oxidability in an oxidation crosslinking reactor, introducing stripping gas into the oxidation crosslinking reactor to separate out light component, and molding and cooling the obtained heavy component to obtain coated asphalt; and the light component obtained by distillation can be used as a raw material for preparing BTX by hydrocracking. The light components of the tar with the final distillation point less than 250 ℃ are mainly 1 and 2 cyclic aromatic hydrocarbons and possibly a small part of 3 cyclic aromatic hydrocarbons; the light components of the tar with the final distillation point less than 220 ℃ are 1 and 2 cyclic aromatic hydrocarbons. And separating the light components of the tar with the final distillation point of less than 220-250 ℃, so that the light components can be used as a raw material for preparing BTX by hydrocracking.
Therefore, the device provided by the application has a simple structure, can prepare the conventional cheap ethylene tar into the coated asphalt with high added value, and can additionally prepare the raw material for preparing BTX by hydrocracking.
Preferably, the device for preparing the coated asphalt from the ethylene tar further comprises a naphthalene separation unit 2, and a feed inlet of the naphthalene separation unit 2 is connected with a light component outlet of the distillation device 1.
About half of naphthalene substances are contained in the tar light component with the final distillation point of less than 220-250 ℃, and the tar light component can be introduced into a naphthalene separation unit 2 to separate out the naphthalene substances. The processing operation of the light component of the ethylene tar is determined according to the market demand and price of naphthalene and methylnaphthalene. If the naphthalene and the methylnaphthalene are low in demand and low in price, the naphthalene separation unit 2 is not selected, the light components of the ethylene tar are all used as the raw materials for preparing the BTX through hydrocracking, and when the supply of the naphthalene and the methylnaphthalene is insufficient and the price is high, the naphthalene and the methylnaphthalene products are separated from the light components of the ethylene tar through the naphthalene separation unit 2 and then are used as the raw materials for preparing the BTX through hydrocracking.
Preferably, a heater 3 is provided between the distillation apparatus 1 and the oxidative crosslinking reactor.
The tar recombinant fraction is heated to the reaction temperature by a heater 3 and then is introduced into an oxidation crosslinking reactor for oxidation crosslinking reaction.
The number of the oxidation crosslinking reactors is 2, and 2 oxidation crosslinking reactors are arranged in parallel.
The 2 oxidation crosslinking reactors are respectively a first oxidation crosslinking reactor 4 and a second oxidation crosslinking reactor 5, when the first oxidation crosslinking reactor 4 carries out crosslinking reaction, the second oxidation crosslinking reactor 5 is switched to start working, ethylene tar heavy components start to be injected into the second oxidation crosslinking reactor 5, and the requirement that the material injection time of the two reactors is consistent with the time required by oxidation crosslinking reaction, steam stripping and discharging operation is met. Namely, when the cross-linking reaction, steam stripping and discharging of the first oxidation reactor are all completed, the material injection of the second oxidation cross-linking reactor 5 is just completed, and the processes are sequentially circulated, so that the continuous production is realized.
Preferably, each oxidation crosslinking reactor is also provided with a gas distributor, and after the gas (the gas with the oxidation property and the stripping gas) enters the device, the gas is uniformly distributed by the gas distributor and is sent into the reactor.
The specific structure of the device that this application embodiment relates to does:
a feed inlet of the distillation device 1 is connected with a feed pipe 9 for introducing ethylene tar, a light component outlet of the distillation device 1 is connected with the naphthalene separation unit 2 through a light component delivery pipe 10, the distillation device 1 is a flash column, and light components produced by distillation of the flash column are introduced into the naphthalene separation unit 2;
the naphthalene separation unit 2 is connected with a BTX raw material conveying pipe 11 and a naphthalene product conveying pipe 12, the monocyclic aromatic hydrocarbon separated by the naphthalene separation unit 2 is output from the BTX raw material conveying pipe 11, and the naphthalene and methylnaphthalene products separated by the naphthalene separation unit 2 are output from the naphthalene product conveying pipe 12;
a heavy component outlet of the distillation device 1 is connected with a heater 3 (such as a heating furnace) through a heavy component conveying pipe 13, and the heavy component of the tar is conveyed into the heater 3 through the heavy component conveying pipe 13 and heated to the oxidation crosslinking temperature;
the outlet of the heater 3 is connected with a high-temperature heavy component conveying pipe 14, the high-temperature heavy component conveying pipe 14 is connected with the two oxidation crosslinking reactors through a first four-way valve 6, and when the device works, the feeding of the two oxidation crosslinking reactors is switched through the first four-way valve 6;
the bottom of each oxidation crosslinking reactor is connected with a gas inlet pipe, the gas inlet pipe is connected with an oxidation gas inlet pipe 16 and a stripping gas inlet pipe 8 through a second four-way valve 7, the oxidation crosslinking reactor is connected with the gas inlet pipe through the second four-way valve 7 by switching the oxidation gas inlet pipe 16, and gas with oxidability is introduced into the oxidation crosslinking reactor, after the oxidation crosslinking reaction is finished, the stripping gas inlet pipe 8 is switched through the second four-way valve 7, stripping gas is introduced into the oxidation crosslinking reactor through the stripping gas inlet pipe 8, so that gas is carried out on oxidation crosslinking products, and light components are taken out;
the bottom of each oxidation crosslinking reactor is connected with a heavy component discharge pipe 17 for discharging heavy components generated by oxidation crosslinking;
the top of each oxidative crosslinking reactor is connected with a light component discharge pipe 15 for discharging stripping gas and light component gas generated by crosslinking.
The method for preparing the coated asphalt by adopting the ethylene tar comprises the following steps:
distilling the ethylene tar to obtain a tar light component and a tar heavy component with an end point of less than 220-250 ℃;
preparing BTX by taking the tar light component as a raw material;
introducing heavy tar components into an oxidation crosslinking reactor, and introducing gas with oxidability into the oxidation crosslinking reactor to perform oxidation crosslinking reaction;
after the oxidative crosslinking reaction is finished, introducing stripping gas into the oxidative crosslinking reactor, and taking out light components generated by oxidative crosslinking by the stripping gas.
The method for preparing the coated asphalt from the ethylene tar provided by the embodiment of the application can be implemented by the device provided by the embodiment of the application. The method provided by the embodiment of the application has a simple structure, can prepare the existing cheap ethylene tar into the coated asphalt with high added value, and can additionally prepare the raw material for preparing BTX by hydrocracking.
The preparation method specifically comprises the following steps:
s1, distilling the ethylene tar to obtain a tar light component and a tar heavy component with the final distillation point of less than 220-250 ℃.
And (3) introducing the ethylene tar into a distillation device 1 for distillation, and distilling the light tar component with the final distillation point of less than 220-250 ℃ and the heavy tar component with the initial distillation point of less than 220-250 ℃.
S2, preparing BTX by taking the tar light component as a raw material.
The data show that the monocyclic aromatic hydrocarbon accounts for about 41-45% and the bicyclic aromatic hydrocarbon accounts for about 55-57% in the light tar component with the final distillation point of less than 220-250 ℃, wherein the naphthalene accounts for about 45-55% and the tricyclic aromatic hydrocarbon accounts for about 0-1.2%; when the tar light component is directly used as the raw material for preparing BTX by hydrocracking, in the hydrogenation saturation and cracking process of the aromatic hydrocarbon, the polycyclic aromatic hydrocarbon is carried out by the way of hydrogenation of aromatic rings one by one, the first aromatic ring is most easily saturated, the subsequent aromatic hydrocarbon is more and more slowly hydrogenated, the last aromatic hydrocarbon is most difficult to hydrogenate, and the reaction rate constants are in the order of: tricyclic aromatics, bicyclic aromatics and monocyclic aromatics, so that all monocyclic aromatic products can be obtained by simply hydrocracking the light components of ethylene tar, thereby generating BTX (benzene, toluene and xylene). Therefore, the separated tar light component can be used as a raw material for preparing BTX by hydrocracking.
Preferably, as the tar light component contains about half of naphthalene products, if the naphthalene products have high scarce market value, the tar light component can be introduced into the naphthalene separation unit 2 to separate out naphthalene and methylnaphthalene products, and then the residual component is used as the raw material for preparing BTX by hydrocracking.
The light components of the ethylene tar firstly enter the naphthalene separation unit 2, when naphthalene and methylnaphthalene products are separated and then used as raw materials for preparing BTX by hydrocracking, after the naphthalene separation unit is used for processing, the remaining components mainly comprise monocyclic aromatic hydrocarbon and contain a small amount of tricyclic aromatic hydrocarbon, the reaction is more moderate, and only mild hydrocracking is needed to generate BTX.
And S3, introducing the heavy tar components into an oxidation crosslinking reactor, and introducing gas with oxidizing property into the oxidation crosslinking reactor to perform oxidation crosslinking reaction.
And (2) introducing the heavy tar component into the heater 3, raising the temperature of the heavy tar component to the oxidation crosslinking reaction temperature, introducing the high-temperature heavy tar component into the first oxidation crosslinking reactor 4, and introducing gas with oxidability into the first oxidation crosslinking reactor 4 when the liquid level in the first oxidation crosslinking reactor 4 reaches 50-80% of the reactor to perform oxidation crosslinking reaction liquid.
Preferably, the temperature of the oxidation crosslinking reaction is 350-400 ℃, the pressure is 0.1-2 Mpa, and the ratio of the flow rate of the gas with oxidability to the mass of the heavy components of the tar in the oxidation crosslinking reactor is 0.5-5 m3·min-1·t-1。
Further, in order to ensure the high efficiency and stability of production and obtain better performance of the coated asphalt, the temperature of the oxidation crosslinking reaction is 350-380 ℃, the pressure is 0.1-1 Mpa, and the ratio of the flow of the gas with oxidability to the mass of the heavy components of the tar in the oxidation crosslinking reactor is 1-2 m3·min-1·t-1。
Preferably, the reaction time is 3-8 h, more preferably 3-7 h. It should be noted that the reaction time can be adjusted according to specific working conditions.
Preferably, in order to ensure high efficiency and uniformity of the reaction, the stirring speed of the stirring device in the oxidation crosslinking reactor is 200-500 r/min.
Preferably, the gas having oxidizing properties is air, which is most readily available and does not require cost.
S4, introducing stripping gas into the oxidative crosslinking reactor after the oxidative crosslinking reaction is finished, and taking out light components generated by oxidative crosslinking by the stripping gas.
The method comprises the following steps: introducing heavy tar components into a heater 3, raising the temperature of the heavy tar components to the oxidation crosslinking reaction temperature, then controlling a first four-way valve 6, introducing high-temperature heavy tar components into a first oxidation crosslinking reactor 4, controlling a second four-way valve 7 when the liquid level in the first oxidation crosslinking reactor 4 reaches 50-80%, introducing gas with oxidability into the first oxidation crosslinking reactor 4, and switching the second four-way valve 7 to introduce stripping gas into the reactor after the reaction in the first oxidation crosslinking reactor 4 is finished; when the reaction in the first oxidation crosslinking reactor 4 is started, the first four-way valve 6 is switched to control the feeding of the second oxidation crosslinking reactor 5, after the feeding of the second oxidation crosslinking reactor 5 is finished, the discharging of the first oxidation crosslinking reactor 4 is finished, at this time, the first four-way valve 6 is controlled to switch the feeding of the first oxidation crosslinking reactor 4, the second four-way valve 7 is controlled to introduce the gas with the oxidizing property into the second oxidation crosslinking reactor 5, and the continuous production is realized by the circulation and alternate work.
And (3) taking out light components generated by the crosslinking reaction from the top of the reactor by stripping gas, discharging heavy components from the bottom of the reactor, and forming and cooling the discharged heavy components to obtain the coated asphalt. The softening point of the obtained coated asphalt is 220-310 ℃, the quinoline insoluble substance is less than 1.5%, and the coking value is 60-80%.
Preferably, the stripping gas is steam, the stripping process is stripping under pressure, and the stripping operation pressure is consistent with the oxidation crosslinking reaction pressure and is 0.1-2 MPa. The temperature of the water vapor is 350-400 ℃, and the flow rate of the water vapor is 1-3 times of that of the oxidizing gas. The process achieves the effect of reducing the partial pressure of light hydrocarbon in the reactor mainly by improving the flow of water vapor, thereby strengthening the process of removing the light hydrocarbon. Compared with the conventional pressure reduction light hydrocarbon removal, the method has low requirements on devices and is simple to operate. Meanwhile, the stripping gas passes through the oil-gas separation device, so that the separation of non-condensable gas, light oil and water can be realized, and the water can be recycled after being heated and vaporized.
Preferably, the flow rate of the water vapor is 1 to 2 times of the flow rate of the oxidizing gas.
Preferably, in order to ensure that the light component is fully separated from the heavy component, the stripping time is 1-3 h; more preferably 1-2 h.
The features and properties of the present invention are described in further detail below with reference to examples.
In the following examples, ethylene tar from a refinery of medium petrochemical origin is used as a raw material. Specific properties of the raw materials are shown in table 1, and data of coated asphalt prepared in each example are shown in table 2.
TABLE 1 raw material and intermediate reactant Property data
TABLE 2 ethylene tar light component Property data
Example 1
Separating ethylene tar into IBP-220 deg.C light component and more than 220 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 350 deg.C, introducing into oxidation crosslinking reactor with pressure of 1Mpa and air amount of 1m3·min-1·t-1The crosslinking reaction time is 8h, the steam flow is 1 time of air in the steam stripping process, and the steam stripping time is 1 h.
Example 2
Separating ethylene tar into IBP-220 deg.C light component and more than 220 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 350 deg.C, introducing into oxidation crosslinking reactor with pressure of 1Mpa and air amount of 2m3·min-1·t-1The crosslinking reaction time is 4.5h, the steam flow is 1 time of air in the steam stripping process, and the steam stripping time is 1 h.
Example 3
Separating ethylene tar into IBP-220 deg.C light component and more than 220 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 360 deg.C, introducing into oxidation crosslinking reactor with pressure of 1Mpa and air amount of 3m3·min-1·t-1Crosslinking reaction time of 3h, steam stripping processThe steam flow is 1 time of the air, and the stripping time is 1 h.
Example 4
Separating ethylene tar into IBP-220 deg.C light component and more than 220 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 360 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.9Mpa and air amount of 2m3·min-1·t-1The crosslinking reaction time is 3.5h, the steam flow is 1.5 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 5
Separating ethylene tar into IBP-220 deg.C light component and more than 220 deg.C heavy component by distillation device 1, heating the heavy component to 370 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.6Mpa and air amount of 1.4m3·min-1·t-1The crosslinking reaction time is 4h, the steam flow is 2 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 6
Separating ethylene tar into IBP-250 deg.C light component and more than 250 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 360 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.6Mpa and air amount of 1m3·min-1·t-1The crosslinking reaction time is 6h, the steam flow is 1 time of air in the steam stripping process, and the steam stripping time is 2 h.
Example 7
Separating ethylene tar into IBP-250 deg.C light component and more than 250 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 360 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.2Mpa and air amount of 1.2m3·min-1·t-1The crosslinking reaction time is 5h, the steam flow is 1.5 times of the air in the steam stripping process, and the steam stripping time is 2 h.
Example 8
Ethylene tar is separated into IBP-250 ℃ light components and more than 250 ℃ heavy components by a distillation device 1, the ethylene tar heavy components are heated to 370 ℃ and enter an oxidation crosslinking reactor for oxidation crosslinking reactionThe pressure of the device is 1Mpa, and the air quantity is 1.2m3·min-1·t-1The crosslinking reaction time is 5.5h, the steam flow is 2 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 9
Separating ethylene tar into IBP-250 deg.C light component and more than 250 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 380 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.1Mpa and air amount of 1.1m3·min-1·t-1The crosslinking reaction time is 5h, the steam flow is 2 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 10
Separating ethylene tar into IBP-250 deg.C light component and more than 250 deg.C heavy component by distillation device 1, heating the ethylene tar heavy component to 380 deg.C, introducing into oxidation crosslinking reactor with pressure of 0.1Mpa and air amount of 1m3·min-1·t-1The crosslinking reaction time is 6h, the steam flow is 2 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 11
Separating ethylene tar into IBP-250 deg.C light component and over 250 deg.C heavy component by distillation device 1, heating the heavy component to 400 deg.C, introducing into oxidation crosslinking reactor with pressure of 1.5Mpa and air amount of 1.5m3·min-1·t-1The crosslinking reaction time is 4.5h, the steam flow is 2 times of the air in the steam stripping process, and the steam stripping time is 1 h.
Example 12
This example is substantially the same as example 5, except that: the ethylene tar heavy component was heated to 380 ℃ and fed into the oxidative crosslinking reactor.
Example 13
This example is substantially the same as example 5, except that: the pressure in the oxidative crosslinking reactor was 0.4 MPa.
Example 14
This example is substantially the same as example 5, except that: air (a)The amount is 1m3·min-1·t-1。
Comparative example 1
This comparative example is essentially the same as example 5, except that the ethylene tar was separated by distillation apparatus 1 into an IBP-200 ℃ light fraction and a greater than 200 ℃ heavy fraction, and the coated asphalt was prepared with the greater than 200 ℃ heavy fraction.
Comparative example 2
This comparative example is essentially the same as example 5, except that the ethylene tar was separated by distillation apparatus 1 into an IBP-270 ℃ light fraction and a greater than 270 ℃ heavy fraction, and the coated asphalt was prepared with the greater than 270 ℃ heavy fraction.
Examples of the experiments
The coated asphalts produced in the examples and comparative examples were tested for their performance. The test data are recorded in table 3.
TABLE 3 data for coated bitumens prepared in the examples and comparative examples
| Item | Softening point, DEG C | Coking value,% of | Quinoline insoluble content% | Yield of coated asphalt% |
| Example 1 | 221 | 62.3 | 0.19 | 70.2 |
| Example 2 | 235 | 65.1 | 0.26 | 69.1 |
| Example 3 | 242 | 69.2 | 0.31 | 67.2 |
| Example 4 | 248 | 71.1 | 0.41 | 66.5 |
| Example 5 | 265 | 72.2 | 0.32 | 72.6 |
| Example 6 | 258 | 72.1 | 0.63 | 74.1 |
| Example 7 | 275 | 74.6 | 0.58 | 69.8 |
| Example 8 | 271 | 74.9 | 0.66 | 71.1 |
| Example 9 | 298 | 76.2 | 1.16 | 68.2 |
| Example 10 | 312 | 79.6 | 1.25 | 66.8 |
| Example 11 | 301 | 76.4 | 1.32 | 67.3 |
| Example 12 | 290 | 75.9 | 1.13 | 68.7 |
| Example 13 | 281 | 75.2 | 1.06 | 69.2 |
| Example 14 | 202 | 60.6 | 0.13 | 83.4 |
| Comparative example 1 | 277 | 72.8 | 0.89 | 48.9 |
| Comparative example 2 | 251 | 73.9 | 11.2 | 76.6 |
As can be seen from the above table, the coated pitches obtained in the examples of the present application have a higher softening point and a lower quinoline insoluble content, and when the distillation temperature of the heavy ends of the tar obtained by distillation is not in the range required in the present application to prepare the coated pitch, the yield of the coated pitch is low (comparative example 1) or the quinoline insoluble content is high (comparative example 2).
In conclusion, the device for preparing the coated asphalt by adopting the ethylene tar has a simple structure, overcomes the defects of unstable product quality and the like caused by frequent loading and unloading and cleaning procedures of the conventional kettle type reaction, can prepare the BTX raw material by carrying out distillation treatment on the raw material and by-product hydrocracking, and can prepare the coated asphalt with the softening point of 220-310 ℃, the quinoline insoluble content of less than 1.5 percent and the coking value of 60-80 percent. In a preferred embodiment, two reactors are connected in parallel, so that stable and continuous production of the product quality can be realized; in a preferred embodiment, the naphthalene separation unit is arranged, so that naphthalene and methylnaphthalene can be byproducts, the naphthalene, methylnaphthalene and coated asphalt production capacity can be flexibly adjusted according to market demands, and the comprehensive utilization of ethylene tar can be greatly improved.
The device that adopts ethylene tar preparation cladding pitch that this application provided, its device simple structure that involves has the same advantage with above-mentioned device.
The coated asphalt provided by the application has a softening point of 220-310 ℃, a quinoline insoluble substance of less than 1.5% and a coking value of 60-80%, and has good performance when being applied to coating of a lithium battery cathode.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The method for preparing the coated asphalt by adopting the ethylene tar is characterized by comprising the following steps:
distilling the ethylene tar to obtain a tar light component and a tar heavy component with an end point of less than 220-250 ℃;
preparing BTX by taking the tar light component as a raw material;
introducing the heavy tar component into an oxidation crosslinking reactor, and simultaneously introducing gas with oxidability into the oxidation crosslinking reactor to perform oxidation crosslinking reaction;
and after the oxidative crosslinking reaction is finished, introducing stripping gas into the oxidative crosslinking reactor, and taking out light components generated by oxidative crosslinking by the stripping gas.
2. The method for preparing coated asphalt from ethylene tar according to claim 1, wherein the step of preparing BTX from the light tar component as the raw material further comprises: and separating out naphthalene substances in the tar light component.
3. The method of claim 1, wherein the temperature of the oxidative crosslinking reaction is 350-400 ℃, the pressure is 0.1-2 MPa, and the ratio of the flow rate of the gas with oxidizability to the mass of the heavy tar component in the oxidative crosslinking reactor is 0.5-5 m3·min-1·t-1；
Preferably, the temperature of the oxidation crosslinking reaction is 350-380 ℃, the pressure is 0.1-1 Mpa, and the ratio of the flow rate of the gas with oxidability to the mass of the heavy components of the tar in the oxidation crosslinking reactor is 1-2 m3·min-1·t-1；
Preferably, the reaction time is 3-8 h, more preferably 3-7 h;
preferably, the stirring speed of a stirring device in the oxidation crosslinking reactor is 200-500 r/min;
preferably, the gas having an oxidizing property is air.
4. The method for preparing the coated asphalt from the ethylene tar according to claim 1, wherein an oxidizing gas is introduced into the oxidative crosslinking reactor when the liquid level in the reactor reaches 50-80%.
5. The method for preparing the coated asphalt by using the ethylene tar according to claim 1, wherein the stripping gas is steam, the stripping pressure is 0.1-2 MPa, the steam temperature is 350-400 ℃, and the steam flow is 1-3 times of the oxidizing gas flow;
preferably, the flow rate of the water vapor is 1-2 times of the flow rate of the oxidizing gas;
preferably, the stripping time is 1-3 h; the stripping time is more preferably 1-2 h.
6. Adopt ethylene tar preparation cladding pitch's device, its characterized in that includes:
a distillation device, an oxidation crosslinking reactor and a gas inlet pipe; and a heavy component discharge port of the distillation device is connected with a feed inlet of the oxidation crosslinking reactor, and the gas inlet pipe is connected with a bottom gas inlet of the oxidation crosslinking reactor.
7. The apparatus for preparing coated asphalt from ethylene tar according to claim 6, wherein a heater is disposed between the distillation apparatus and the oxidative crosslinking reactor.
8. The apparatus for preparing coated asphalt from ethylene tar according to claim 6, further comprising a naphthalene separation unit, wherein a feed inlet of the naphthalene separation unit is connected to the light component outlet of the distillation apparatus.
9. The apparatus of claim 6, wherein the number of the oxidative crosslinking reactors is 2, and 2 oxidative crosslinking reactors are arranged in parallel.
10. A coated asphalt, characterized in that it is prepared by the method according to any one of claims 1 to 5 or by the apparatus according to any one of claims 6 to 9.
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| CN115093874A (en) * | 2022-07-31 | 2022-09-23 | 中国石油化工股份有限公司 | Preparation method and system of low-quinoline insoluble matter high-softening-point petroleum-based coated asphalt |
| CN115594826A (en) * | 2022-11-25 | 2023-01-13 | 淄博鲁华泓锦新材料集团股份有限公司（Cn） | Low-energy-consumption synthesis method of efficient carbon negative electrode coating material |
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| CN115594826A (en) * | 2022-11-25 | 2023-01-13 | 淄博鲁华泓锦新材料集团股份有限公司（Cn） | Low-energy-consumption synthesis method of efficient carbon negative electrode coating material |
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