CN114891527A - Preparation device and method of heavy oil-based coated asphalt - Google Patents
Preparation device and method of heavy oil-based coated asphalt Download PDFInfo
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- CN114891527A CN114891527A CN202210401885.0A CN202210401885A CN114891527A CN 114891527 A CN114891527 A CN 114891527A CN 202210401885 A CN202210401885 A CN 202210401885A CN 114891527 A CN114891527 A CN 114891527A
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- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
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Abstract
The application relates to the field of petrochemical industry, in particular to a preparation device and a preparation method of heavy oil-based coated asphalt. The preparation device comprises a crosslinking reactor, a gas-liquid separation device, an oxidized asphalt heater and a condensation reactor; the bottom of the crosslinking reactor is connected with an oxygen-containing mixed gas inlet pipe, the discharge port of the crosslinking reactor is connected with the feed port of a gas-liquid separation device, the liquid outlet of the gas-liquid separation device is connected with the feed port of an oxidized asphalt heater, the gas outlet of the gas-liquid separation device is connected with the purge gas inlet at the bottom of the condensation reactor, and the discharge port of the oxidized asphalt heater is connected with the feed port of the condensation reactor. The preparation method comprises the following steps: the coated asphalt is prepared by adopting the device. The device and the method provided by the application can realize continuous production of the coated asphalt, and the prepared coated asphalt has very low Quinoline Insoluble (QI) content.
Description
Technical Field
The invention relates to the field of petrochemical industry, in particular to a preparation device and a preparation method of heavy oil-based 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 poor compatibility of the graphite electrode and the organic electrolyte, excessive SEI films are generated on the surface of the negative electrode, lithium ions in the electrolyte are consumed, interfacial impedance is greatly increased, electrochemical dynamic barrier is generated, even dissociation and stripping of a graphite layer of the electrode occur, 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, the problems of low softening point, low coking value, high ash content, high quinoline insoluble substance and the like generally exist in common coating materials, so that the development of a coating asphalt material with ultrahigh softening point, low quinoline content and low ash content is particularly important for improving the electrochemical performance of a lithium battery cathode. Therefore, scholars at home and abroad carry out a great deal of research and put forward a plurality of production methods of the coated asphalt. Although the currently proposed method can prepare the high-softening-point coated asphalt, the problem of overlarge Quinoline Insoluble (QI) exists, so that the coated asphalt has poor fluidity at high temperature, cannot completely infiltrate the pore structure on the surface of graphite, and has poor coating modification effect on the surface of graphite, thereby affecting the electrochemical performance of the graphite electrode.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide a preparation device and a preparation method of heavy oil-based coated asphalt, which can realize continuous production and prepare the coated asphalt with very low Quinoline Insoluble (QI) content.
Embodiments of the invention may be implemented as follows:
in a first aspect, the invention provides a preparation device of heavy oil-based coated asphalt, which comprises a crosslinking reactor, a gas-liquid separation device, an oxidized asphalt heater and a condensation reactor;
the bottom of the crosslinking reactor is connected with an oxygen-containing mixed gas inlet pipe, the discharge port of the crosslinking reactor is connected with the feed port of a gas-liquid separation device, the liquid outlet of the gas-liquid separation device is connected with the feed port of an oxidized asphalt heater, the gas outlet of the gas-liquid separation device is connected with the purge gas inlet at the bottom of the condensation reactor, and the discharge port of the oxidized asphalt heater is connected with the feed port of the condensation reactor.
In an alternative embodiment, the number of crosslinking reactors is 2,2 crosslinking reactors are connected in parallel and 1 condensation reactor.
In an alternative embodiment, the apparatus for preparing heavy oil-based coated bitumen further comprises a heavy oil heater, and the discharge port of the heavy oil heater is connected with the feed port of the crosslinking reactor.
In an alternative embodiment, the gas-liquid separation device is a flash distillation device.
In a second aspect, the present invention provides a method for preparing a heavy oil-based coated asphalt, comprising:
introducing high-temperature heavy oil and oxygen-containing mixed gas into a cross-linking reactor for oxidation cross-linking reaction, wherein the temperature of the high-temperature heavy oil is 320-350 ℃, the oxygen-containing mixed gas is the mixed gas of oxygen and gas which does not react with the heavy oil at high temperature, and the heavy oil is at least one of ethylene tar, asphalt and vacuum residue;
introducing the product after the oxidation crosslinking reaction into a gas-liquid separation device for gas-liquid separation to obtain oxidized asphalt and oxygen-poor tail gas;
and (3) controlling the temperature of the oxidized asphalt to be 370-400 ℃, introducing the oxidized asphalt into a condensation reactor, introducing oxygen-deficient tail gas into the bottom of the condensation reactor to be used as purge gas, taking out light components generated by condensation reaction from the top of the condensation reactor by the purge gas, and discharging heavy component products of the condensation reaction from the bottom of the condensation reactor.
In an alternative embodiment, the oxidative crosslinking reaction parameters are: the reaction pressure is 0.05-0.6 Mpa, and the reaction time is 3-12 h;
preferably, the reaction pressure is 0.05-0.4 Mpa, and the reaction time is 3-8 h;
preferably, the temperature of the high-temperature heavy oil is 330-350 ℃.
In an alternative embodiment, the oxygen-containing mixture is air.
In an optional embodiment, the ratio of the air input of the oxygen-containing mixture to the heavy oil in the crosslinking reactor is 0.5-2L 3 min -1 kg -1 Preferably 0.5 to 1.5L 3 min -1 kg -1 。
In an alternative embodiment, the condensation reaction parameters are: the reaction pressure is 0.01-0.2 Mpa, and the reaction time is 0.5-4 h;
preferably, the reaction pressure is 0.01-0.1 Mpa, and the reaction time is 0.5-2 h;
preferably, the temperature of the oxidized asphalt is controlled to be 380-400 ℃, and the oxidized asphalt is introduced into the condensation reactor.
In an optional embodiment, a crosslinking reaction stirrer is arranged in the crosslinking reactor, and the rotating speed of the crosslinking reaction stirrer is 200-500 r/min;
preferably, a condensation reaction stirrer is arranged in the condensation reactor, and the rotating speed of the condensation reaction stirrer is 200-500 r/min.
The beneficial effects of the present invention include, for example:
1. the method provided by the application can realize continuous production of the coated asphalt, flexibly regulate and control production of series of coated asphalt products with different softening points by regulating and controlling reaction parameters according to market demands, greatly improve the economy of heavy oil, effectively overcome the problem that the existing coated asphalt preparation process needs stripping of inert gas or steam to remove light hydrocarbons by recycling reaction tail gas, greatly reduce the production cost, and expand and improve the utilization way and the additional value of the heavy oil.
2. The oxygen-poor tail gas generated by the gas-liquid separation device can be used as inert gas for stripping and removing light components from the coated asphalt. In the oxidation crosslinking process, oxygen in the air is consumed in a large amount as a crosslinking agent, the oxygen content in tail gas generated by a crosslinked product through a gas-liquid separation device is extremely low, and the tail gas can be used as inert gas for stripping and removing light components from the coated asphalt in a condensation reaction stage. Not only avoids the reintroduction of inert gas or steam for steam stripping operation, but also reduces the preheating treatment of the steam stripping raw material and the production cost.
3. The content of the prepared coated asphalt quinoline insoluble substance (QI) is very low and is less than 1%, the Softening Point (SP) is 150-250 ℃, and the coking value is more than 50%. Compared with the coated asphalt prepared by the prior art, the coated asphalt has good high-temperature fluidity, can completely infiltrate the pore structure on the surface of graphite, and has good coating modification effect on the surface of graphite.
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 a heavy oil-based coated asphalt production apparatus provided in an embodiment of the present application.
Icon: 1-a heavy oil heater; 2-a crosslinking reactor; 3-oxygen-containing mixed gas inlet pipe; 4-a first four-way valve; 5-a second four-way valve; 6-gas-liquid separation device; 7-an oxidized asphalt heater; 8-a condensation reactor; 9-heavy oil inlet pipe; 10-main oxygen-containing gas mixture; 11-a cross-linked product transport tube; 12-a bitumen oxide delivery pipe; 13-a lean oxygen tail gas conveying pipe; 14-a light component output pipe; 15-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 with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. indicate an orientation or a positional relationship based on that shown in the drawings or that the product of the present invention is used as it is, this is only for convenience of description and simplification of the description, and it does not indicate or imply that the device or the element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
Furthermore, the appearances of the terms "first," "second," and the like, if any, are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
Referring to fig. 1, a device for preparing heavy oil-based coated asphalt includes a crosslinking reactor 2, a gas-liquid separation device 6, an oxidized asphalt heater 7, and a condensation reactor 8;
the bottom of the crosslinking reactor 2 is connected with an oxygen-containing mixed gas inlet pipe 3, the discharge port of the crosslinking reactor 2 is connected with the feed inlet of a gas-liquid separation device 6, the liquid outlet of the gas-liquid separation device 6 is connected with the feed inlet of an oxidized asphalt heater 7, the gas outlet of the gas-liquid separation device 6 is connected with the purge gas inlet at the bottom of a condensation reactor 8, and the discharge port of the oxidized asphalt heater 7 is connected with the feed inlet of the condensation reactor 8.
The application provides a preparation facilities of heavy oil base cladding pitch, in letting in high temperature ethylene tar, pitch or heavy oil such as decompression slag oil in the device, carry out oxidation crosslinking reaction with oxygen in crosslinking reactor 2 after, get into gas-liquid separation device 6, obtain oxidation pitch and poor oxygen tail gas, oxidation pitch is heated through oxidation pitch heater 7 and is had to get into condensation reactor 8 and carry out condensation reaction, poor oxygen tail gas is also constantly let in condensation reactor 8 bottom from gas-liquid separation device 6 and is upwards swept condensation reaction product, the light component that condensation reaction produced is carried out by poor oxygen tail gas from condensation reaction upper portion, the heavy component that produces is discharged from condensation reactor 8 bottom, this heavy component is got heavy oil cladding pitch after shaping, cooling.
The preparation device for the heavy oil-based coated asphalt provided by the application is used for processing heavy oil, can be used for continuously preparing the series of coated asphalt with different softening points, effectively solves the problem that inert gas or steam is required for stripping and removing light hydrocarbon in the existing coated asphalt preparation process through recycling reaction tail gas, greatly reduces the production cost, and expands and improves the utilization approach and the added value of the heavy oil. The oxygen-poor tail gas generated by the gas-liquid separation device 6 can be used as inert gas for stripping and removing light components from the coated asphalt. In the oxidation crosslinking process, oxygen in the air is consumed as a crosslinking agent in a large amount, the oxygen content in tail gas generated by a crosslinked product through the gas-liquid separation device 6 is extremely low, and the tail gas can be used as inert gas for stripping and removing light components from the coated asphalt in a condensation reaction stage. Not only avoids the reintroduction of inert gas or steam for steam stripping operation, but also reduces the preheating treatment of the steam stripping raw material and the production cost.
Specifically, the crosslinking reactor 2 is connected with the gas-liquid separation device 6 through a crosslinked product conveying pipe 11, and an oxidized crosslinked product obtained by reaction in the crosslinking reactor 2 is conveyed into the gas-liquid separation device 6 through the crosslinked product conveying pipe 11 for gas-liquid separation; a liquid outlet of the gas-liquid separation device 6 is connected with the heavy oil heater 1 through an oxidized asphalt conveying pipe 12, the oxidized asphalt obtained after separation is conveyed into the heavy oil heater 1 by the oxidized asphalt conveying pipe 12 and is heated to the condensation temperature and then is conveyed into the condensation reactor 8, a gas outlet of the gas-liquid separation device 6 is connected with a bottom purge gas inlet of the condensation reactor 8 through an oxygen-deficient tail gas conveying pipe 13, and the separated oxygen-deficient tail gas is conveyed into the bottom of the condensation reactor 8 through the oxygen-deficient tail gas conveying pipe 13 to be used as a purge gas; the top of the condensation reactor 8 is connected with a light component output pipe 14, the purge gas discharges the light component generated by the condensation reaction from the light component output pipe 14, the bottom of the condensation reactor 8 is connected with a heavy component output pipe, and the heavy component obtained by the condensation reaction is discharged from the heavy component output pipe.
Preferably, the preparation device of the heavy oil-based coated asphalt further comprises a heavy oil heater, and the discharge port of the heavy oil heater is connected with the feed port of the crosslinking reactor 2.
The heavy oil heater is connected with a heavy oil inlet pipe 9, heavy oil enters the heavy oil heater from the heavy oil inlet pipe 9, and the heavy oil heater heats the heavy oil entering the device, so that the temperature of the heavy oil can be raised to meet the requirement of an oxidation crosslinking reaction.
Preferably, the number of crosslinking reactors 2 is 2,2 crosslinking reactors 2 are connected in parallel and 1 condensation reactor 8. Wherein, 2 crosslinking reactors 2 are in size, and the material injection time of the reactors is consistent with the oxidation crosslinking reaction time.
The two crosslinking reactors 2 are continuously switched for use in the material injection process and the oxidation crosslinking reaction process, and the condensation reactor 8 is matched for intermittent use. Compared with the oxidation crosslinking unit, the condensation reaction unit has shorter time, and the required time is only 1/4-1/2 of the oxidation crosslinking process, so that the whole process can be realized by one condensation reactor 8.
Further, the bottom of each crosslinking reactor 2 and the bottom of the condensation reactor 8 are provided with a gas distributor, the oxygen-containing mixed gas inlet pipe 3 is connected with the gas distributor at the bottom of the crosslinking reactor 2, and the oxygen-deficient tail gas conveying pipe 13 is connected with the gas distributor at the bottom of the condensation reactor 8. The gas distributor can make the gas uniformly distributed in the reaction device.
Further, a stirrer is provided in the bottom of each crosslinking reactor 2 and in the condensation reactor 8. When the reactor works, the stirrer also does not stop working, and the uniform and sufficient reaction can be ensured.
Preferably, the heavy oil heater is connected to the two crosslinking reactors 2 through a first four-way valve 4. If necessary, a crosslinking reactor 2 can be connected in parallel via this first four-way valve 4.
The preparation device of the heavy oil-based coated asphalt also comprises an oxygen-containing mixed gas main pipe 10, and two oxygen-containing mixed gas inlet pipes 3 respectively connected with the two crosslinking reactors 2 are connected with the oxygen-containing mixed gas main pipe 10 through a second four-way valve 5. If necessary, a further crosslinking reactor 2 is connected in parallel, the remaining connecting channel of the second four-way valve 5 being connected to the oxygen-containing gas mixture inlet 3 of the further parallel crosslinking reactor 2.
Further, the gas-liquid separation device 6 is a flash evaporation device.
The flash distillation device is a gas-liquid separation device 6 which is convenient to use in the field of petrochemical industry at present.
The embodiment of the application also provides a preparation method of the heavy oil-based coated asphalt, which comprises the following steps:
introducing high-temperature heavy oil and oxygen-containing mixed gas into a cross-linking reactor 2 for oxidation cross-linking reaction, wherein the temperature of the high-temperature heavy oil is 320-350 ℃, the oxygen-containing mixed gas is the mixed gas of oxygen and gas which does not react with the heavy oil at high temperature, and the heavy oil is at least one of ethylene tar, asphalt and vacuum residue;
introducing the product after the oxidation crosslinking reaction into a gas-liquid separation device 6 for gas-liquid separation to obtain oxidized asphalt and oxygen-poor tail gas;
and (3) controlling the temperature of the oxidized asphalt to be 370-400 ℃, introducing the oxidized asphalt into the condensation reactor 8, introducing the oxygen-deficient tail gas into the bottom of the condensation reactor 8 to be used as purge gas, taking out light components generated by condensation reaction from the top of the condensation reactor 8 by the purge gas, and discharging heavy component products of the condensation reaction from the bottom of the condensation reactor 8.
The method provided by the application has the following advantages:
the method can continuously prepare the series of coated asphalts with different softening points, effectively solves the problem that the prior coated asphalts need inert gas or steam for stripping to remove light hydrocarbons by recycling reaction tail gas, greatly reduces the production cost, and expands and improves the utilization approach and the added value of heavy oil.
The oxygen-poor tail gas generated by the gas-liquid separation device 6 can be used as inert gas for stripping and removing light components from the coated asphalt. In the oxidation crosslinking process, oxygen in the air is consumed as a crosslinking agent in a large amount, the oxygen content in tail gas generated by a crosslinked product through the gas-liquid separation device 6 is extremely low, and the tail gas can be used as inert gas for stripping and removing light components from the coated asphalt in a condensation reaction stage. Not only avoids the reintroduction of inert gas or steam for steam stripping operation, but also reduces the preheating treatment of the steam stripping raw material and the production cost.
The obtained coated asphalt has Quinoline Insoluble (QI) content lower than 1%, Softening Point (SP) higher than 150 deg.C, and coking value higher than 50%. Compared with the coated asphalt prepared by the prior art, the coated asphalt has good high-temperature fluidity, can completely infiltrate the pore structure on the surface of graphite, and has good coating modification effect on the surface of graphite.
The method provided by the application specifically comprises the following steps:
and S1, introducing the heavy oil into the heavy oil heater 1, raising the temperature to 320-350 ℃, and conveying the heavy oil from the top of the crosslinking reactor 2 to the crosslinking reactor 2 through the first four-way valve 4.
Preferably, the temperature is raised to 330-350 ℃ and then the mixture passes through the first four-way valve 4.
And S2, when the liquid level of the oxidation crosslinking reactor 2 reaches 50-80%, introducing oxygen-containing mixed gas into the crosslinking reactor 2 from a gas distributor at the bottom of the crosslinking reactor 2 through an oxygen-containing mixed gas inlet pipe 3, and starting oxidation crosslinking reaction, wherein a stirrer arranged in the crosslinking reactor 2 continuously stirs.
Preferably, the oxygen-containing gas is air.
Preferably, in order to ensure sufficient reaction, the ratio of the air input of the oxygen-containing mixture to the heavy oil in the crosslinking reactor 2 is 0.5-2L 3 ·min -1 ·kg -1 Preferably 0.5 to 1.5L 3 ·min -1 ·kg -1 。
Preferably, in order to make the oxidative crosslinking more sufficient, the parameters of the oxidative crosslinking reaction are: the reaction pressure is 0.05-0.6 Mpa, and the reaction time is 3-12 h. More preferably, the reaction pressure is 0.05-0.4 MPa, and the reaction time is 3-8 h.
Preferably, in order to ensure that the reaction is more efficient, the stirring speed of the stirrer is 200-500 r/min.
S3, conveying the reaction product of the oxidation crosslinking reactor 2 into a gas-liquid separation device 6 through a crosslinking product conveying pipe 11 for gas-liquid separation, and separating into oxidized asphalt and oxygen-poor tail gas.
And S4, conveying the oxidized asphalt into a heavy oil heater 1 through an oxidized asphalt conveying pipe 12, heating to 370-400 ℃ through the heavy oil heater 1, and then conveying into a condensation reactor 8.
Preferably, in order to ensure that the condensation reaction is more efficient, the oxidized asphalt is heated to 380-400 ℃ by a heavy oil heater and then is sent into the condensation reactor 8 for reaction.
And S5, conveying the oxygen-deficient tail gas into a gas distributor at the bottom of the condensation reactor 8 through the oxygen-deficient tail gas conveying pipe 13, and entering the condensation reactor 8 through the gas distributor.
S7, the asphalt oxide is subjected to condensation reaction in the condensation reactor 8, and the generated heavy component is discharged from a heavy component discharge pipe 15 at the bottom of the condensation reactor 8. The oxygen-deficient tail gas entering the condensation reactor 8 is used as a purge gas, and light components generated by the condensation reaction are upwards carried out from a light component output pipe 14.
Preferably, in order to ensure that the condensation reaction is carried out completely and efficiently, the condensation reaction parameters are: the reaction pressure is 0.01-0.2 Mpa, and the reaction time is 0.5-4 h. More preferably, the reaction pressure is 0.01 to 0.1MPa, and the reaction time is 0.5 to 2 hours.
Preferably, in order to ensure uniform and efficient condensation reaction, the stirring speed of the stirrer in the condensation reactor 8 is 200-500 r/min.
The present application will be described with reference to specific examples.
Ethylene tar and asphalt of a certain refinery in medium petrochemicals are used as heavy oil raw materials. Specific properties of each raw material are shown in table 1, and data of coated asphalt prepared in each example and comparative example are shown in table 2.
Table 1 raw material property data
Example 1
Heating asphalt as raw material to 330 deg.C, introducing into crosslinking reactor 2 under 0.1MPa, and the ratio of air amount to heavy oil in crosslinking reactor 2 is 0.6L 3 ·min -1 ·kg -1 After reacting for 3h, the temperature is raised to 380 ℃ again and the mixture enters a condensation reactor 8 to react for 1h under 0.05 Mpa.
Example 2
Heating asphalt as raw material to 330 deg.C, introducing into crosslinking reactor 2 under 0.1MPa, and the ratio of air amount to heavy oil in crosslinking reactor 2 is 0.8L 3 ·min -1 ·kg -1 After reacting for 4h, the temperature is raised to 380 ℃ again and the mixture enters a condensation reactor 8 to react for 1.2h under 0.05 Mpa.
Example 3
Heating asphalt as raw material to 340 deg.C, introducing into crosslinking reactor 2 under 0.06MPa, and the ratio of air amount to heavy oil in crosslinking reactor 2 is 1L 3 ·min -1 ·kg -1 After reacting for 4h, the temperature is raised to 390 ℃ again and then the mixture enters a condensation reactor 8 to react for 2h under 0.1 Mpa.
Example 4
Heating asphalt as raw material to 340 deg.C, introducing into a crosslinking reactor 2 under 0.04MPa, and the amount of air and heavy oil in the crosslinking reactor 2The ratio is 1.2L 3 ·min -1 ·kg -1 After reacting for 5h, the temperature is raised to 390 ℃ again and then the mixture enters a condensation reactor 8 to react for 1.5h under 0.1 Mpa.
Example 5
Heating asphalt as raw material to 350 deg.C, introducing into crosslinking reactor 2 under 0.04MPa, and the ratio of air amount to heavy oil in crosslinking reactor 2 is 1.5L 3 ·min -1 ·kg -1 After reacting for 4h, raising the temperature to 400 ℃ again, entering the condensation reactor 8, and reacting for 1.5h under 0.1 Mpa.
Example 6
Ethylene tar is used as raw material, heated to 340 ℃ and enters a crosslinking reactor 2, the reaction pressure is 0.2Mpa, and the ratio of the air quantity to the heavy oil quantity in the crosslinking reactor 2 is 1.5L 3 ·min -1 ·kg -1 After reacting for 4h, the temperature is raised to 380 ℃ again and the mixture enters a condensation reactor 8 to react for 2.5h under 0.1 Mpa.
Example 7
Ethylene tar is used as raw material, heated to 350 ℃ and enters a crosslinking reactor 2, the reaction pressure is 0.4Mpa, and the ratio of the air quantity to the heavy oil quantity in the crosslinking reactor 2 is 2L 3 ·min -1 ·kg -1 After reacting for 3.5h, the temperature is raised to 390 ℃ again and then the mixture enters a condensation reactor 8 to react for 1.5h under 0.1 Mpa.
Example 8
This embodiment is substantially the same as embodiment 1 except that: the crosslinking reaction temperature was 320 ℃.
Example 9
This example is substantially the same as example 7, except that: the crosslinking reaction pressure was 0.6 MPa.
Example 10
This embodiment is substantially the same as embodiment 2 except that: the condensation reaction pressure was 0.01 MPa.
Example 11
This example is substantially the same as example 7, except that: the condensation reaction pressure was 0.2 MPa.
Comparative example 1
This comparative example is essentially the same as example 1 except that: the crosslinking reaction temperature was 300 ℃.
Comparative example 2
This comparative example is essentially the same as example 7 except that: the crosslinking reaction temperature was 400 ℃.
Comparative example 3
This comparative example is essentially the same as example 2, except that: the condensation reaction temperature was 350 ℃.
Comparative example 4
This comparative example is essentially the same as example 7 except that: the crosslinking reaction temperature was 500 ℃.
Comparative example 5
This comparative example is essentially the same as example 7 except that: the crosslinking reaction temperature was 370 ℃.
Comparative example 6
This comparative example is essentially the same as example 1 except that: the crosslinking reaction temperature was 370 ℃.
Comparative example 7
This comparative example is essentially the same as example 5, except that: the crosslinking reaction temperature was 450 ℃.
Comparative example 8
This comparative example is essentially the same as example 5, except that: the crosslinking reaction pressure was 0.01 MPa.
TABLE 2 data for coated bitumens prepared in the examples and comparative examples
"-" in the table means that the softening point was too high and was not detected by the instrument and should be >380 deg.C
As can be seen from the above table, the coated asphalt prepared by the examples of the present application has a high softening point, particularly a very low Quinoline Insoluble (QI) content, which is less than 1%, and a coking value of more than 50%. Comparing each proportion with the corresponding examples, it can be seen that the quinoline insoluble content of the proportion is higher or the coking value is lower, which indicates that when preparing the coated asphalt, the reaction temperature needs to be within the range required by the application, and good-performance coated asphalt can not be obtained unless the reaction temperature is within the range required by the application.
In summary, the device and the method for preparing the heavy oil-based coated asphalt provided by the application have the following advantages:
1. the method provided by the application can realize continuous production of the coated asphalt, flexibly regulate and control production of series of coated asphalt products with different softening points by regulating and controlling reaction parameters according to market demands, greatly improve the economy of heavy oil, effectively overcome the problem that the existing coated asphalt needs inert gas or steam to strip and remove light hydrocarbon in the preparation process by recycling reaction tail gas, greatly reduce the production cost, and expand and improve the utilization approach and the added value of the heavy oil.
2. The oxygen-poor tail gas generated by the gas-liquid separation device can be used as inert gas for stripping and removing light components from the coated asphalt. In the oxidation crosslinking process, oxygen in the air is consumed in a large amount as a crosslinking agent, the oxygen content in tail gas generated by a crosslinked product through a gas-liquid separation device is extremely low, and the tail gas can be used as inert gas for stripping and removing light components from the coated asphalt in a condensation reaction stage. Not only avoids the reintroduction of inert gas or steam for steam stripping operation, but also reduces the preheating treatment of the steam stripping raw material and the production cost.
3. The content of the prepared coated asphalt quinoline insoluble substance (QI) is very low and is less than 1%, the Softening Point (SP) is 150-250 ℃, and the coking value is more than 50%. Compared with the coated asphalt prepared by the prior art, the coated asphalt has good high-temperature fluidity, can completely infiltrate the pore structure on the surface of graphite, and has good coating modification effect on the surface of graphite.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The preparation device of the heavy oil-based coated asphalt is characterized by comprising a crosslinking reactor, a gas-liquid separation device, an oxidized asphalt heater and a condensation reactor;
the bottom of the crosslinking reactor is connected with an oxygen-containing mixed gas inlet pipe, a discharge port of the crosslinking reactor is connected with a feed port of a gas-liquid separation device, a liquid outlet of the gas-liquid separation device is connected with a feed port of an oxidized asphalt heater, a gas outlet of the gas-liquid separation device is connected with a purge gas inlet at the bottom of the condensation reactor, and a discharge port of the oxidized asphalt heater is connected with a feed port of the condensation reactor.
2. The apparatus for producing heavy oil-based coated asphalt according to claim 1, wherein the number of the crosslinking reactors is 2,2 crosslinking reactors are connected in parallel, and the number of the condensation reactors is 1.
3. The apparatus for preparing heavy oil-based coated asphalt according to claim 1, wherein the apparatus further comprises a heavy oil heater, and the discharge port of the heavy oil heater is connected to the feed port of the crosslinking reactor.
4. The apparatus for producing heavy oil-based coated asphalt according to claim 1, wherein the gas-liquid separation device is a flash evaporation device.
5. The preparation method of the heavy oil-based coated asphalt is characterized by comprising the following steps:
introducing high-temperature heavy oil and oxygen-containing mixed gas into a cross-linking reactor for oxidation cross-linking reaction, wherein the temperature of the high-temperature heavy oil is 320-350 ℃, the oxygen-containing mixed gas is the mixed gas of oxygen and gas which does not react with the heavy oil at high temperature, and the heavy oil is at least one of ethylene tar, asphalt and vacuum residue;
introducing the product after the oxidation crosslinking reaction into a gas-liquid separation device for gas-liquid separation to obtain oxidized asphalt and oxygen-poor tail gas;
and controlling the temperature of the oxidized asphalt to be 370-400 ℃, introducing the oxidized asphalt into a condensation reactor, introducing the oxygen-deficient tail gas into the bottom of the condensation reactor to be used as a purge gas, taking out light components generated by condensation reaction from the top of the condensation reactor by the purge gas, and discharging heavy component products of the condensation reaction from the bottom of the condensation reactor.
6. The method of claim 5, wherein the oxidative crosslinking reaction parameters are: the reaction pressure is 0.05-0.6 Mpa, and the reaction time is 3-12 h;
preferably, the reaction pressure is 0.05-0.4 Mpa, and the reaction time is 3-8 h;
preferably, the temperature of the high-temperature heavy oil is 330-350 ℃.
7. The method of claim 5, wherein the oxygenated mixture is air.
8. The method for preparing heavy oil-based coated asphalt according to claim 5, wherein the ratio of the air input of the oxygen-containing mixed gas to the heavy oil in the crosslinking reactor is 0.5-2L 3 ·min -1 ·kg -1 Preferably 0.5 to 1.5L 3 ·min -1 ·kg -1 。
9. The method of claim 5, wherein the condensation reaction parameters are: the reaction pressure is 0.01-0.2 Mpa, and the reaction time is 0.5-4 h;
preferably, the reaction pressure is 0.01-0.1 Mpa, and the reaction time is 0.5-2 h;
preferably, the temperature of the oxidized asphalt is controlled to be 380-400 ℃, and the oxidized asphalt is introduced into the condensation reactor.
10. The method for preparing the heavy oil-based coated asphalt according to claim 5, wherein a crosslinking reaction stirrer is arranged in the crosslinking reactor, and the rotation speed of the crosslinking reaction stirrer is 200-500 r/min;
preferably, a condensation reaction stirrer is arranged in the condensation reactor, and the rotating speed of the condensation reaction stirrer ranges from 200 r/min to 500 r/min.
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