CN114479906A - Method for preparing high-quality petroleum coke - Google Patents
Method for preparing high-quality petroleum coke Download PDFInfo
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- CN114479906A CN114479906A CN202011165518.2A CN202011165518A CN114479906A CN 114479906 A CN114479906 A CN 114479906A CN 202011165518 A CN202011165518 A CN 202011165518A CN 114479906 A CN114479906 A CN 114479906A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
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Abstract
The invention relates to the field of petroleum coke preparation, and discloses a method for preparing petroleum coke, which is characterized by comprising the following steps: (1) mixing raw oil containing high aromatic hydrocarbon components with light mixed liquid phase components rich in tricyclic aromatic hydrocarbon and tetracyclic aromatic hydrocarbon, heating the mixed feed by a green coke heating unit, and then feeding the heated mixed feed into a coke tower to generate oil gas and a wide-area intermediate phase; (2) and the coke tower enters an air flow coke pulling stage to react to generate oil gas and needle coke, and the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons, which is heated by a coke pulling heating unit, is independently introduced into the coke tower in the air flow coke pulling stage of the coke tower. The method of the invention is beneficial to the formation of a large-area intermediate phase and the production of high-quality needle coke.
Description
Technical Field
The invention relates to the field of petroleum coke preparation, in particular to a method for preparing high-quality petroleum coke-needle coke.
Background
The high-quality petroleum coke-needle coke is a main raw material for producing high-power and ultrahigh-power graphite electrodes, has higher price, and can be widely applied as ultrahigh-power graphite electrodes for electric furnace steelmaking, super capacitors for electric vehicles and lithium ion electrodes for communication batteries. The most critical influencing factor in needle coke production is the feedstock properties, the better the feedstock properties the higher the grade of needle coke product obtained.
CN106635149B discloses a method for preparing needle coke, in which the middle distillate oil and catalytic cracking slurry oil obtained by catalytic cracking process enter a coke tower, the top oil-gas of the coke tower is separated to obtain gas, light oil and circulating oil, the middle distillate oil and the circulating oil are mixed and enter the coking tower in the temperature raising process of a coking heating furnace, and the method can prepare a large-area wide-area mesophase.
Disclosure of Invention
The invention aims to provide a method for preparing petroleum coke, which can effectively utilize raw materials such as catalytic cracking slurry oil to prepare the petroleum coke with high quality.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing petroleum coke, the method comprising:
(1) mixing raw oil containing high-aromatic hydrocarbon components with light mixed liquid phase components rich in tricyclic aromatic hydrocarbon and tetracyclic aromatic hydrocarbon, heating the mixed feed by a green coke heating unit, and then feeding the heated mixed feed into a coke tower to generate a wide-area intermediate phase;
(2) and the coke tower enters an air flow coke pulling stage to react to generate oil gas and needle coke, and the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons, which is heated by a coke pulling heating unit, is independently introduced into the coke tower in the air flow coke pulling stage of the coke tower.
The method can effectively utilize raw materials such as catalytic cracking slurry oil to prepare high-quality needle coke.
According to the preferred embodiment of the invention, raw oil containing high aromatic hydrocarbon components is mixed with light mixed liquid phase components obtained by separating, condensing and mixing light distillate oil, and the mixed feed is heated by a green coke heating furnace and enters a coke tower to generate a wide-area intermediate phase; in the air flow coke-pulling stage, the light mixed liquid phase component enters a coke tower through a coke-pulling heating furnace to carry out the air flow coke-pulling process, and finally needle coke is generated; separating the high-temperature oil gas in a fractionating tower to obtain fractions such as rich gas, coker gasoline, coker diesel oil, coker wax oil and fractionating tower bottom oil; when the coke tower is used for feeding, multiple feeding ports are adopted for feeding, the proportion of light fraction mixed with the raw material oil containing high aromatic hydrocarbon components is adjusted according to different outlet temperature intervals of the heating furnace, and the switching between the green coke heating furnace and the coke-drawing heating furnace is realized; when the raw coke heating furnace heats the raw material, the operation is carried out in a multi-stage temperature rise and multi-stage constant temperature mode. Thereby, the quality of the needle coke can be further improved.
Additional features of the invention will be described in the detailed description which follows.
Drawings
Fig. 1 is a schematic flow diagram of a process for producing needle coke in accordance with a preferred embodiment of the present invention.
Description of the reference numerals
1 is catalytic cracking slurry oil 2 is an outlet material flow of a radiation section of a raw coke heating furnace;
3. 6 is the material entering the coke tower and 4 is the total material of the coke tower;
5. 7 are all coke drum feed 8 is the coke drum;
9, oil gas and 10 are fractionating towers;
11 is coking rich gas 12 is coking gasoline;
13 is coker diesel oil and 14 is coker gas oil;
15 coking heavy wax oil reflux 16 fractionating tower bottom oil;
17 is a coke-drawing heating furnace and 18 is a coke-producing heating furnace;
a stripping tower 19 and a condensation reactor 20;
21 is the light component with vapor 22 being the light fraction;
23 heavy component 24, which is a light fraction, is a branched stream of light mixed liquid phase components;
a branch stream 26 which is a light mixed liquid phase component is an outlet material flow of the coke-drawing heating furnace;
27. 28 is a branch stream of the coke oven exit stream to the coke drum.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a method for preparing petroleum coke, which comprises the following steps:
(1) mixing raw oil containing high-aromatic hydrocarbon components with light mixed liquid phase components rich in tricyclic aromatic hydrocarbon and tetracyclic aromatic hydrocarbon, heating the mixed feed by a green coke heating unit, and then feeding the heated mixed feed into a coke tower to generate a wide-area intermediate phase;
(2) and the coke tower enters an air flow coke pulling stage to react to generate oil gas and needle coke, and the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons, which is heated by a coke pulling heating unit, is independently introduced into the coke tower in the air flow coke pulling stage of the coke tower.
In the invention, the gas velocity in the coke tower can be increased by independently introducing the light mixed liquid phase component rich in tricyclic and tetracyclic aromatics heated by the coke-pulling heating unit into the coke tower in the gas flow coke-pulling stage of the coke tower, so that the mesophase forms a more obvious needle-shaped structure under the action of a larger shearing force, the mesophase has better anisotropy, and the finally generated needle-shaped coke has better quality.
According to the preferred embodiment of the invention, when the outlet temperature of the green coke heating furnace is higher than 488-495 ℃, preferably higher than 488-491 ℃, the coke tower enters the gas flow coking stage, so that when the temperature is higher than 488-495 ℃, preferably higher than 488-491 ℃, only the light mixed liquid phase component rich in the tricyclic and tetracyclic aromatic hydrocarbons heated by the coking heating unit is separately introduced into the coke tower. Thereby realizing the coke drawing process of the intermediate phase in the coke tower.
According to a preferred embodiment of the invention, the method comprises: and (3): and (3) fractionating the oil gas obtained in the step (2) to obtain coking rich gas, coking gasoline, coking diesel oil, coking wax oil and fractionating tower bottom oil.
According to a preferred embodiment of the present invention, more preferably, the coker gas oil and/or fractionator bottoms are separated to obtain a heavy fraction rich in tricyclic and tetracyclic aromatics and a light fraction rich in monocyclic and bicyclic aromatics; carrying out condensation reaction on the light component rich in the monocyclic and bicyclic aromatic hydrocarbons to obtain a liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons; and taking the liquid phase component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon and/or the heavy component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon as the raw material of the light mixed liquid phase component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon.
In the invention, the light component rich in the monocyclic and bicyclic aromatic hydrocarbons contains a large amount of monocyclic aromatic hydrocarbons and bicyclic aromatic hydrocarbons, a small amount of tricyclic aromatic hydrocarbons and tetracyclic aromatic hydrocarbons and trace amounts of aromatic hydrocarbons larger than tetracyclic aromatic hydrocarbons, but the monocyclic aromatic hydrocarbons and bicyclic aromatic hydrocarbons are main components, so that the light component is the light component rich in the monocyclic and bicyclic aromatic hydrocarbons; the heavy component rich in the tricyclic and tetracyclic aromatics contains a small amount of monocyclic aromatics and bicyclic aromatics, a large amount of tricyclic aromatics and tetracyclic aromatics and a small amount of aromatics larger than tetracyclic aromatics, but the tricyclic aromatics and the tetracyclic aromatics are main components, so that the heavy component is a component rich in the tricyclic and tetracyclic aromatics.
According to a preferred embodiment of the present invention, more preferably, the separation of the coker wax oil and/or the fractionator bottoms is by extractive separation or by stripping separation.
The present invention has no particular requirement on the manner of separation nor on the conditions of separation, and according to a preferred embodiment of the present invention, more preferably, the conditions of stripping separation comprise: the pressure is 0.1-0.15MPa, and/or the temperature is 300-330 ℃, and/or the weight ratio of the injected steam quantity to the separated raw material component is 0.05-0.1: 1.
The present invention has no particular requirement on the condensation reaction conditions, and according to a preferred embodiment of the present invention, more preferably, the condensation reaction conditions include: the temperature is 350-600 ℃, preferably 400-490 ℃; and/or a pressure of 0.12 to 6MPa, preferably 1.5 to 4 MPa.
In the process of the present invention, preferably, the condensation reaction is carried out in a condensation reactor in the presence of a catalyst comprising an active component containing at least one of iron, copper and nickel (e.g., an active component such as iron, copper, nickel, iron-copper, iron-nickel, copper-nickel or iron-copper-nickel) and a carrier containing at least one of alumina and a molecular sieve (e.g., an alumina support, a molecular sieve or an alumina-molecular sieve), and the content of the active component in terms of element is 5 to 35% by weight and the content of the carrier is 65 to 95% by weight, based on the weight of the catalyst. When the active ingredient contains a plurality of components, the ratio between the aforementioned plurality of components is not particularly required, and may be any ratio as long as it can satisfy the total content of the active ingredient in terms of elements of 5 to 35% by weight; when the carrier contains a plurality of components, the ratio between the plurality of components is not particularly limited, and may be any ratio as long as the content of the carrier is from 65 to 95% by weight. The foregoing catalysts may be commercially available or prepared by themselves. The method for preparing the catalyst is not particularly limited, and various methods commonly used in the art may be used, and examples thereof include: the carrier is soaked in the solution of soluble salt of active component in the same volume, and the mixture is stoved and roasted.
In the invention, when the outlet temperature of the green coke heating unit is lower than 450-470 ℃, preferably lower than 450-460 ℃, the mixing ratio of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatics to the raw oil containing high aromatic hydrocarbon component is 0.1: 1-0.6: 1, preferably 0.3: 1-0.6: 1. Therefore, the concentration of the effective components of tricyclic and tetracyclic aromatics in the raw materials can be improved, and the high aromatic hydrocarbon components are utilized to the maximum extent.
In the invention, when the outlet temperature of the green coke heating unit is higher than 450-470 ℃, preferably higher than 450-460 ℃, the flow of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons is increased to 1.01-3 times, preferably 1.1-2.5 times. When the outlet temperature of the green coke heating unit is higher than 450-470 ℃, preferably higher than 450-460 ℃, the mixing ratio of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatics to the raw oil containing high aromatic hydrocarbon component is 0.4: 1-1: 1, and more preferably 0.4: 1-0.8: 1. Therefore, the viscosity of the liquid phase in the tower can be reduced at relatively high temperature, the continuous growth of the intermediate phase is facilitated, the generated intermediate phase can gradually start to be directionally arranged, and finally the wide-area intermediate phase with large range and good anisotropy is obtained.
In the invention, the coke tower comprises a plurality of coke towers, preferably each coke tower comprises the coke forming stage, the coke drawing stage and the coke removing stage, the coke towers can be operated simultaneously or alternately, and preferably each coke tower coke forming stage is supplied with a mixed feed of raw oil containing high aromatic hydrocarbon components and light mixed liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons by a coke forming heating unit, and the coke drawing stage is supplied with the heated light mixed liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons by a coke drawing heating unit. Therefore, the gas velocity in the coke tower can be increased, the intermediate phase forms a more obvious needle-shaped structure under the action of larger shearing force, the intermediate phase has better anisotropy, and although the coke-drawing time is shorter and the temperature is higher, the coke generated by the light mixed liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons also has certain anisotropy, and the influence on the quality of the needle-shaped coke in the whole tower is smaller.
According to the present invention, it is preferred to feed with 2 to 10 feed ports at the bottom of the coke drum, and it is preferred to feed with 3 to 5 feed ports at the bottom of the coke drum. Therefore, the materials at the lower part of the coke tower can be mixed more uniformly, so that the concentration difference along the radial direction and/or the vertical direction of the coke tower can be reduced or reduced, and the quality of the intermediate phase and the needle coke is improved.
According to the invention, preferably, the raw coke heating unit adopts a programmed heating operation mode of first-stage heating, second-stage constant temperature, third-stage heating and fourth-stage constant temperature when heating; more preferably, the first-stage heating is gradually heated to 400-460 ℃ at the speed of 1-10 ℃/h, the second-stage constant temperature is constant temperature for 1-10 h at the first-stage heating temperature, the third-stage heating is increased to 495 ℃ at the speed of 0.5-6 ℃/h, and the fourth-stage constant temperature is constant temperature for 1-10 h at the third-stage heating temperature. The liquid phase can be warmed up gently, and the generation of a large amount of isotropic coke due to rapid warming can be reduced and avoided. According to the invention, a one-section heating-two-section constant temperature programmed heating operation mode is preferably adopted when the green coke heating unit is used for heating; preferably, the first-stage heating is gradually heated to 400-495 ℃ at the speed of 1-10 ℃/h, and the second-stage constant temperature is 400-495 ℃ for 1-20 h. According to the invention, the green coke heating unit can adopt a programmed heating operation mode of first-stage heating, second-stage constant temperature, third-stage heating and fourth-stage constant temperature; or a one-stage heating-two-stage constant temperature programmed heating operation mode can be adopted; preferably, a programmed heating operation mode of first-stage heating, second-stage constant temperature, third-stage heating and fourth-stage constant temperature is adopted.
According to the invention, a temperature control mode of first-stage temperature rise and second-stage constant temperature is adopted when the coke-drawing heating unit heats; preferably, the temperature of the first section is raised to 490-510 ℃ at the speed of 0.5-6 ℃/h, and the constant temperature of the second section is 490-510 ℃ for 1-5 h. Therefore, the gas velocity in the coke tower can be gradually increased, the intermediate phase forms a more obvious needle-shaped structure under the action of larger shearing force, the intermediate phase has better anisotropy, and the quality of the finally generated needle-shaped coke is better.
According to the present invention, the aromatic content of the feedstock oil containing a high aromatic content is preferably 20 wt% or more, and more preferably 50 to 90 wt%.
According to the present invention, it is preferable that the ash content in the feedstock oil containing a high aromatic hydrocarbon component is not higher than 0.1 wt%.
According to the present invention, preferably, the content of asphaltenes in the feedstock oil containing a high aromatic hydrocarbon component is not higher than 0.5 wt%.
According to the present invention, preferably, the raw oil containing high aromatic hydrocarbon components is selected from one or more of catalytic oil slurry, ethylene tar, furfural extract oil and coal tar, and is preferably selected from catalytic oil slurry.
According to the invention, preferably, the distillation range, the density, the ash content and the asphaltene content of the light mixed liquid phase rich in the tricyclic and tetracyclic aromatic hydrocarbons are lower than those of the raw oil containing high aromatic hydrocarbon components.
According to the present invention, preferably, the composition and properties of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatics comprise: the sum of the content of tricyclic aromatic hydrocarbon and tetracyclic aromatic hydrocarbon is 40-85 wt%, the content of ash is not higher than 0.05 wt%, the content of asphaltene is not higher than 0.025 wt%, and the density is 0.8-1.01 kg/m3。
According to the present invention, the conditions for the fractionation can be selected in a wide range, and for the present invention, preferred conditions for the fractionation include: the temperature of the top of the fractionating tower is 100-145 ℃; and/or the tower top pressure of the fractionating tower is 0.1-0.17 MPa; and/or the temperature of the bottom of the fractionating tower is 310-360 ℃. Through the fractionation, the oil-gas mixture at the top of the coke tower generated by the delayed coking reaction can be separated into coking rich gas, coking gasoline, coking diesel oil, coking wax oil (namely a wax oil component) and coking heavy wax oil.
While a wide range of operating conditions for the coke drums is possible in accordance with the present invention, for purposes of the present invention, preferred operating conditions for the coke drum include: the pressure of the coke tower is 0.3-2.5MPa, preferably 0.5-1.0 MPa; and/or the coking period is 24-72h, preferably 48-64 h.
According to the present invention, in order to effectively utilize heat, it is preferable that the method further comprises: and (3) exchanging heat between raw oil containing high-aromatic hydrocarbon components and one or more of the coking rich gas, the coking gasoline, the coking diesel oil, the coking wax oil and the bottom oil of the fractionating tower, and then mixing the raw oil with the light mixed liquid phase components rich in the tricyclic and tetracyclic aromatic hydrocarbons.
According to a preferred embodiment of the present invention, there is provided a process for the preparation of petroleum coke, the process comprising:
(1) mixing raw oil containing high aromatic hydrocarbon components with light distillate oil such as the coker gas oil and/or bottom oil of a fractionating tower to obtain light mixed liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons, heating the mixed feed by a green coke heating furnace, and then feeding the heated mixed feed into a coke tower to generate a wide-area intermediate phase;
(2) in the air flow coke-pulling stage, the light mixed liquid phase component enters a coke tower through a coke-pulling heating furnace to carry out the air flow coke-pulling process, and finally needle coke is generated;
(3) when the coke tower is used for feeding, the coke tower adopts bottom feeding, wherein the bottom of the coke tower adopts a plurality of feeding holes for feeding;
(4) separating high-temperature oil gas generated at the top of the coke tower in a fractionating tower to obtain fractions such as rich gas, coking gasoline, coking diesel oil, coking wax oil and fractionating tower bottom oil;
(5) and adjusting the mixing proportion of the phase components of the light mixed liquid mixed with the raw material oil containing the high aromatic hydrocarbon component at different temperature raising stages of the green coke heating furnace and realizing the switching between the green coke heating furnace and the coke-drawing heating furnace.
In the method, the heating method of the heating furnace in the step (1) is particularly limited, when the raw material is heated in the raw coke heating furnace, a programmed heating operation mode of first-stage heating, second-stage constant temperature, third-stage heating and fourth-stage constant temperature can be adopted, when the outlet temperature of the raw coke heating furnace reaches a certain range, the raw coke heating furnace is redirected to another coke tower for feeding, and simultaneously the coke-drawing heating furnace starts to feed to the original coke tower; or the raw materials can also adopt a one-stage heating-two-stage constant temperature programmed heating operation mode when the heating furnace heats the raw materials, when the outlet temperature of the raw coke heating furnace reaches a certain range, the raw coke heating furnace is changed to another coke tower for feeding, and meanwhile, the coke-drawing heating furnace starts to feed to the original coke tower.
In a preferred embodiment of the present invention, the coking reaction conditions further comprise: the coke tower pressure is 0.3-2.5MPa, and more preferably 0.5-1.0 MPa; the coking cycle is 24-72h, more preferably 48-64 h.
In the present invention, the pressure means an absolute pressure.
In a preferred embodiment of the present invention, the coke drum may have 2 or 3 feed ports at the bottom, optionally one or more of which may be fed simultaneously, preferably two feed ports are fed simultaneously.
In the present invention, the bottom feed position is a feed position commonly used in the art, and may be, for example, at the lower cone of a coke drum.
In a preferred embodiment of the invention, when the outlet temperature of the green coke heating furnace is lower than 450-470 ℃, preferably lower than 450-460 ℃, the mixing ratio of the light oil and the high aromatic oil is 0.1: 1-0.6: 1, preferably 0.3: 1-0.6: 1, and when the outlet temperature of the green coke heating furnace is higher than 450-470 ℃, preferably higher than 450-460 ℃, the mixing ratio of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons and the raw oil containing the high aromatic hydrocarbon component is 0.4: 1-1: 1, preferably 0.4: 1-0.8: 1;
in the preferred embodiment of the invention, when the outlet temperature of the green coke heating furnace reaches the temperature range of 488-495 ℃, preferably 488-491 ℃, the green coke heating furnace starts to feed to another coke tower, and the original coke tower starts to feed from the coke-drawing heating furnace; when the coke-pulling heating furnace is supplied by a coke tower, only the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons is introduced.
In the method, the raw oil containing high aromatic hydrocarbon components is selected from one or more of catalytic slurry oil, ethylene tar, furfural extract oil, coal tar and other distillate oil with higher aromatic hydrocarbon content, and the catalytic slurry oil is preferred. According to the invention, the aromatic hydrocarbon content of the high aromatic hydrocarbon raw oil is preferably required to be more than 20 weight percent, and preferably 50-90 weight percent; and the ash content in the high aromatic hydrocarbon raw oil is required to be not higher than 0.1 wt% and the asphaltene content in the high aromatic hydrocarbon raw oil is required to be not higher than 0.5 wt%.
In the method of the invention, the light fraction is selected from distillate oil with distillation range, density, ash content and asphaltene content lower than or less than that of the high aromatic hydrocarbon raw material, preferably the light fraction separated from a fractionating tower in the device is selected from one or two of coker gas oil and bottom oil of the fractionating tower.
In the process of the present invention, the conditions of the coker fractionator include: the temperature of the top of the fractionating tower is 100-145 ℃, the pressure of the top of the fractionating tower is 0.1-0.17MPa, and the temperature of the bottom of the fractionating tower is 310-360 ℃. Through the fractionation, the oil-gas mixture at the top of the coke tower generated by the delayed coking reaction can be separated into coking rich gas, coking gasoline, coking diesel oil, coking wax oil (namely a wax oil component) and coking heavy wax oil.
In the method of the present invention, the separation method is not particularly limited as long as the separation raw material can be separated into the light component of the wax oil rich in the monocyclic and bicyclic aromatic hydrocarbons and the heavy component of the wax oil rich in the tricyclic and tetracyclic aromatic hydrocarbons. Preferably, the separation is by extraction or stripping.
Preferably, the stripping separation is carried out in a stripping column, the conditions of the stripping separation comprising: the pressure is 0.1-0.15MPa, the temperature is 300-330 ℃, and the weight ratio of the injected steam quantity to the wax oil component entering the stripping tower is (0.05-0.1): 1.
In the method of the present invention, the conditions for the condensation reaction preferably include: the temperature is 350-600 ℃, and the more preferable temperature is 400-490 ℃; the pressure is 0.12 to 6MPa, more preferably 1.2 to 6MPa, and still more preferably 1.5 to 4 MPa.
In the process of the present invention, preferably, the condensation reaction is carried out in a condensation reactor in the presence of a catalyst comprising an active component containing at least one of iron, copper and nickel (e.g., an active component such as iron, copper, nickel, iron-copper, iron-nickel, copper-nickel or iron-copper-nickel) and a carrier containing at least one of alumina and a molecular sieve (e.g., an alumina support, a molecular sieve or an alumina-molecular sieve), and the content of the active component in terms of element is 5 to 35% by weight and the content of the carrier is 65 to 95% by weight, based on the weight of the catalyst. When the active ingredient contains a plurality of components, the ratio between the aforementioned plurality of components is not particularly required, and may be any ratio as long as it can satisfy the total content of the active ingredient in terms of elements of 5 to 35% by weight; when the carrier contains a plurality of components, the ratio between the plurality of components is not particularly limited, and may be any ratio as long as the content of the carrier is from 65 to 95% by weight. The foregoing catalysts may be commercially available or prepared by themselves. The method for preparing the catalyst is not particularly limited, and various methods commonly used in the art may be used, and examples thereof include: the carrier is soaked in the solution of soluble salt of active component in the same volume, and the mixture is stoved and roasted.
In the method of the present invention, it is preferable that the heavy fraction obtained as described above and the light fraction obtained after condensation are mixed, and the mixed stream is fed to a heating unit, whereby the quality of the needle coke raw material can be improved.
The process of the present invention may be carried out using an apparatus for producing needle coke feedstock, preferably comprising a heating unit, a coke forming unit, a fractionation unit and a condensation unit,
the heating unit is used for heating a mixture obtained by mixing raw oil containing high aromatic hydrocarbon components and a light mixed liquid phase component obtained by separating, condensing and mixing light distillate oil so as to provide heat;
the coke-producing unit is used for generating an intermediate phase in a coke tower by using raw materials and forming needle coke by coke drawing through airflow;
the fractionating unit is used for fractionating the oil-gas mixture from the green coke unit to obtain various light components, and separating light distillate oil to form light distillate oil components rich in monocyclic and bicyclic aromatics and light distillate oil heavy components rich in tricyclic and tetracyclic aromatics;
the condensation unit is used for carrying out condensation reaction on light components of light distillate oil from the light distillate oil passing through the separation unit to obtain liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons.
According to one embodiment of the present invention, as shown in FIG. 1, the process for producing needle coke is carried out using an apparatus consisting essentially of: a coke tower 8, a fractionating tower 10, a condensation reactor 20, a stripping tower 19, a green coke heating furnace 17 and a coke-drawing heating furnace 18. Specifically, the method for producing needle coke may include: selectively exchanging heat between catalytic cracking slurry oil 1 and coker gasoline 12, coker diesel oil 13, coker gas oil 14 and coker heavy wax oil 15 (not shown in figure 1), pumping out bottom oil 16 of a fractionating tower, then feeding the bottom oil into a stripping tower 19 for stripping (steam injection 21), obtaining a light component 22 of a light fraction rich in one-ring and two-ring aromatics at the top of the stripping tower 19, obtaining a heavy component 23 of the light fraction at the bottom of the stripping tower 19, namely a heavy component of the bottom oil of the fractionating tower rich in three-ring and four-ring aromatics, feeding the light component 22 of the light fraction into a condensation reactor 20 for condensation reaction, obtaining a pumped material flow of the condensation reactor, namely a liquid phase component rich in three-ring and four-ring aromatics, and mixing the heavy component 23 of the bottom oil of the fractionating tower with the pumped material flow of the condensation reactor to obtain a light mixed liquid phase component; the phase component of the light mixed liquid is divided into two paths of feeding materials 24 and 25, wherein the feeding materials 24 and 25 are sent to a coke-drawing heating furnace, and the feeding materials 25 are sent to a green coke heating furnace to be mixed with the catalytic slurry oil 1 after heat exchange; then the mixture flow enters a convection section of a heating furnace 17 in sequence, a radiation section is heated, and the heating furnace adopts a 4-section temperature rise control mode; the material flow 2 at the outlet of the radiation section is taken as the total material 4 fed by the coke tower, the material flow 4 is taken as the material flow 3 or 6 fed by the coke tower, and the material flow 3 or 6 is divided into two material flows 5 and 7 fed by the coke tower 8; when the coke-producing furnace reaches a certain temperature range, the coke drum is switched to another coke drum to start feeding, and the outlet stream 26 of the coke-pulling furnace 18 starts feeding the original coke drum through a pipeline through the stream 27 or 28. High-temperature oil gas 9 at the top of the coke tower enters the lower part of a fractionating tower 10, liquid-phase material flow formed after the high-temperature oil gas 9 at the lower part of the fractionating tower 10 exchanges heat with coking heavy wax oil 15 and fractionating tower bottom return tower oil in a backflow mode forms fractionating tower bottom oil 16 at the bottom of the fractionating tower 10, and the fractionating tower bottom oil 16 enters a stripping tower after being extracted; the generated needle coke is left in a coke tower 8, and a coking rich gas 11, a coking gasoline 12, a coking diesel oil 13 and a coking wax oil 14 are obtained at the side line of a fractionating tower.
The present invention will be described in detail below by way of examples, but the present invention is not limited thereto. In each of examples and comparative examples, unless otherwise specified, all methods used are conventional in the art.
Example 1
This example illustrates the process of the present invention for producing a needle coke feedstock.
The operation was carried out according to the procedure described above with reference to FIG. 1.
Selectively exchanging heat between the catalytic slurry oil 1 and the coking gasoline 12, the coking diesel oil 13, the coking wax oil 14 and the coking heavy wax oil 15 (not shown in figure 1), pumping out bottom oil 16 of the fractionating tower, then feeding the bottom oil into a stripping tower 19 for stripping (injecting steam 21), obtaining a light component 22 of the bottom oil of the fractionating tower which is rich in one ring and two rings of aromatic hydrocarbons at the top of the stripping tower 19, obtaining a heavy component 23 of the bottom oil of the fractionating tower which is rich in three rings and four rings of aromatic hydrocarbons at the bottom of the stripping tower 19, feeding the light component 22 of the bottom oil of the fractionating tower into a condensation reactor 20 for condensation reaction, obtaining a pumped material flow of the condensation reactor, namely a liquid component which is rich in three rings and four rings of aromatic hydrocarbons, and mixing the heavy component 23 of the bottom oil of the fractionating tower with the pumped material flow of the condensation reactor to obtain a light mixed liquid phase component; the phase component of the light mixed liquid is divided into two paths of feeding materials 24, 25, wherein 24 is sent to a coke-drawing heating furnace, and 25 is sent to a green coke heating furnace to be mixed with the catalytic slurry oil 1 after heat exchange; then the mixture flow sequentially enters a convection section of a heating furnace 17, a radiation section is used for heating, the heating furnace adopts a first-stage heating-second-stage constant temperature-third-stage heating-four-stage constant temperature heating control mode, the first-stage heating is to gradually heat to 450 ℃ at the speed of 5 ℃/h, the second-stage constant temperature is to keep the temperature of 450 ℃ for 15h, the third-stage heating is to raise to 490 ℃ at the speed of 2 ℃/h, and the four-stage constant temperature is to keep the temperature of 490 ℃ for 5 h; the material flow 2 at the outlet of the radiation section is used as a total material flow 4 fed into a coke tower, then the total material flow 4 is used as a material flow 3 fed into the coke tower, the material flow 3 is divided into two material flows 5 and 7 which are used as the feed of the coke tower 8, and the mass ratio of the material flow 5 to the material flow 7 is 1: 1; in the process, the circulation ratio, namely the weight of the bottom oil 16 of the fractionating tower to the catalytic cracking slurry oil 1 is 0.4:1, when the first-stage heating-second-stage constant temperature-third-stage heating-four-stage constant temperature process of the green coke heating furnace is completed, the green coke heating furnace 17 is switched to another coke tower to start feeding, the coke-pulling heating furnace 18 starts feeding to the original coke tower through a pipeline 28, the outlet temperature of the coke-pulling heating furnace is 505 ℃, the feeding time is 8 hours, and the circulation ratio, namely the weight of the bottom oil 16 of the fractionating tower to the catalytic cracking slurry oil 1 is 0.7: 1. High-temperature oil gas 9 at the top of the coke tower enters the lower part of a fractionating tower 10, liquid-phase material flow formed after the high-temperature oil gas 9 at the lower part of the fractionating tower 10 exchanges heat with coking heavy wax oil 15 and fractionating tower bottom return tower oil in a backflow mode forms fractionating tower bottom oil 16 at the bottom of the fractionating tower 10, and the fractionating tower bottom oil 16 enters a stripping tower after being extracted; the generated needle coke is left in a coke tower 8, and a coking rich gas 11, a coking gasoline 12, a coking diesel oil 13 and a coking wax oil 14 are obtained at the side line of a fractionating tower.
The pressure at the top of the coke tower is 0.5MPa, and the coking period is 48 h; the generated coke is left in a delayed coking coke tower 8, the generated high-temperature oil gas 9 enters a delayed coking fractionating tower 10 for separation (the separation conditions are that the pressure of the top of the fractionating tower is 0.12MPa, the temperature of the bottom of the fractionating tower is 332 ℃, and the temperature of the top of the fractionating tower is 126 ℃), and the coking rich gas 11, the coking gasoline 12, the coking diesel oil 13 and the coking wax oil 14 are obtained. Stripping is carried out under the conditions that the weight ratio of the steam 21 injected into the stripping tower 19 to the bottom oil of the fractionating tower entering the stripping tower is 0.05, the temperature is 300 ℃, and the pressure is 0.12 MPa; the condensation reactor 20 is operated in the presence of a catalyst (based on the weight of the catalyst, the catalyst comprises 10 wt% copper and 90 wt% alumina and is prepared by impregnating alumina with equal volume of copper nitrate solution, drying the mixture at 120 deg.C for 5h, and calcining at 500 deg.C for 2h) to perform condensation reaction at 450 deg.C and 2 MPa.
The distribution of the final product and the properties of the resulting needle coke after forging are shown in Table 2, wherein the temperature after forging is 2700 ℃ and the test temperature of the thermal expansion coefficient is from room temperature to 600 ℃.
Example 2
This example illustrates the process of the present invention for producing a needle coke feedstock.
The process of example 1 was used except that the conditions for the delayed coking reaction included: the pressure of a coke tower is 0.9MPa, the coking period is 36h, a green coke heating furnace adopts a four-section heating mode, the first-section heating mode is that the temperature is gradually heated to 460 ℃ at the speed of 5 ℃/h, the second-section constant temperature is that the temperature is kept at 460 ℃ for 13h, the third-section heating mode is that the temperature is increased to 495 ℃ at the speed of 3 ℃/h, and the temperature is kept at 495 ℃ for 4h in the fourth-section constant temperature; the outlet temperature of the coke-drawing heating furnace is 505 ℃, and the feeding time is 5 hours; the conditions of the fractionation include: the top temperature of the fractionating tower is 115 ℃, the top pressure of the fractionating tower is 0.13MPa, and the bottom temperature of the fractionating tower is 320 ℃;
the distribution of the final product and the properties of the resulting needle coke after forging are shown in Table 2, wherein the temperature after forging is 2700 ℃ and the test temperature of the thermal expansion coefficient is from room temperature to 600 ℃.
Example 3
This example illustrates the process of the present invention for producing needle coke feedstock. The method of example 1 is adopted, except that when the green coke heating furnace is used for four-stage temperature rise, the first stage temperature rise and the second stage constant temperature circulation ratio, namely the weight of the bottom oil 16 of the fractionating tower and the catalytic cracking slurry oil 1 is 0.3:1, and the third stage temperature rise and the fourth stage constant temperature circulation ratio is 0.5: 1; the distribution of the final product and the properties of the resulting needle coke after forging are shown in Table 2, wherein the temperature after forging is 2700 ℃ and the test temperature of the thermal expansion coefficient is from room temperature to 600 ℃.
Example 4
This example illustrates the process of the present invention for producing a needle coke feedstock. The method of example 1 is adopted, except that when the green coke heating furnace is used for four-stage temperature rise, the first stage temperature rise and the second stage constant temperature circulation ratio, namely the weight of the bottom oil 16 of the fractionating tower and the catalytic cracking slurry oil 1 is 0.5:1, and the third stage temperature rise and the fourth stage constant temperature circulation ratio is 0.8: 1; the distribution of the final product and the properties of the resulting needle coke after forging are shown in Table 2, wherein the temperature after forging is 2700 ℃ and the test temperature of the thermal expansion coefficient is from room temperature to 600 ℃.
TABLE 1 Properties of the raw materials
TABLE 2 product distribution and needle coke quality
As can be seen from the data in Table 2, the needle coke produced by the method of the invention according to GB/T37308-2019 meets the standard of high-quality needle coke, so that the method of the invention can effectively utilize catalytic cracking slurry oil to prepare high-quality needle coke.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (14)
1. A process for producing petroleum coke, the process comprising:
(1) mixing raw oil containing high aromatic hydrocarbon components with light mixed liquid phase components rich in tricyclic and tetracyclic aromatic hydrocarbons, heating the mixed feed by a green coke heating unit, and then feeding the heated mixed feed into a coke tower to generate oil gas and a wide area intermediate phase;
(2) and the coke tower enters an air flow coke pulling stage to react to generate oil gas and needle coke, and the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons, which is heated by a coke pulling heating unit, is independently introduced into the coke tower in the air flow coke pulling stage of the coke tower.
2. The process according to claim 1, wherein the coke drum enters the gas stream decoking stage when the green coke oven exit temperature is above 488-495 ℃, preferably above 488-491 ℃.
3. The method of claim 1 or 2, wherein the method comprises:
and (3): fractionating the oil gas obtained in the step (2) to obtain coking rich gas, coking gasoline, coking diesel oil, coking wax oil and fractionating tower bottom oil;
preferably, the first and second electrodes are formed of a metal,
separating the coker gas oil and/or the bottom oil of the fractionating tower to obtain a heavy component rich in tricyclic and tetracyclic aromatic hydrocarbons and a light component rich in monocyclic and bicyclic aromatic hydrocarbons;
carrying out condensation reaction on the light component rich in the monocyclic and bicyclic aromatic hydrocarbons to obtain a liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons;
and taking the liquid phase component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon and/or the heavy component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon as the raw material of the light mixed liquid phase component rich in the tricyclic aromatic hydrocarbon and the tetracyclic aromatic hydrocarbon.
4. A process according to claim 3, wherein the coker wax oil and/or fractionator bottoms are separated by extraction or stripping, preferably,
the conditions for the stripping separation include: the pressure is 0.1-0.15MPa, the temperature is 300-330 ℃, and the weight ratio of the injected steam quantity to the separated raw material components is 0.05-0.1: 1; and/or
The conditions of the condensation reaction include: the temperature is 350-600 ℃, preferably 400-490 ℃; the pressure is 0.12-6MPa, preferably 1.5-4 MPa;
preferably, the condensation reaction is carried out in the presence of a catalyst comprising an active component containing at least one of iron, copper and nickel and a support containing at least one of alumina and a molecular sieve, and the content of the active component on an elemental basis is from 5 to 35% by weight and the content of the support is from 65 to 95% by weight, based on the weight of the catalyst.
5. The method of any one of claims 1-4,
when the outlet temperature of the green coke heating unit is lower than 450-470 ℃, preferably lower than 450-460 ℃, the mixing ratio of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons to the raw oil containing high aromatic hydrocarbon component is 0.1: 1-0.6: 1, preferably 0.3: 1-0.6: 1; and/or
When the outlet temperature of the green coke heating unit is higher than 450-470 ℃, preferably higher than 450-460 ℃, increasing the flow of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons to 1.01-3 times, preferably 1.1-2.5 times;
more preferably, when the outlet temperature of the green coke heating unit is higher than 450-470 ℃, preferably higher than 450-460 ℃, the mixing ratio of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatic hydrocarbons to the raw oil containing high aromatic hydrocarbon component is 0.4: 1-1: 1, and more preferably 0.4: 1-0.8: 1.
6. The method of any of claims 1-5, wherein the coke drum comprises a plurality of coke drums, each coke drum comprising the green stage, the coke pulling stage, and the decoking stage, the plurality of coke drums being operable simultaneously or in a rotating motion, and each of the coke drum green stages being supplied with a heated mixed feed of a feedstock oil containing a high aromatic hydrocarbon component and a light mixed liquid phase component rich in tricyclic and tetracyclic aromatics from a green coke heating unit, and the coke pulling stage being supplied with the heated light mixed liquid phase component rich in tricyclic and tetracyclic aromatics from a coke pulling heating unit.
7. Process according to any one of claims 1 to 6, wherein the feed is applied with 2 to 10 feed openings in the bottom of the coke drum, preferably with 3 to 5 feed openings in the bottom of the coke drum.
8. The method according to any one of claims 1 to 7, wherein the green coke heating unit is heated by a one-stage heating-two-stage constant temperature-three-stage heating-four-stage constant temperature programmed heating operation mode;
the first-stage heating is gradually heated to 400-460 ℃ at the rate of 1-10 ℃/h, the second-stage constant temperature is constant temperature for 1-30 h at the first-stage heating temperature, the third-stage heating is increased to 495 ℃ at the rate of 0.5-6 ℃/h, and the fourth-stage constant temperature is constant temperature for 1-10 h at the third-stage heating temperature; or
The raw coke heating unit adopts a one-section heating-two-section constant temperature programmed heating operation mode during heating; preferably, the first-stage heating is gradually heated to 400-495 ℃ at the speed of 1-10 ℃/h, and the second-stage constant temperature is 400-495 ℃ for 1-20 h.
9. The method of any one of claims 1-7,
when the coke-drawing heating unit is used for heating, a temperature control mode of first-stage temperature rise and second-stage constant temperature is adopted; preferably, the temperature of the first section is raised to 490-510 ℃ at the speed of 0.5-6 ℃/h, and the constant temperature of the second section is 490-510 ℃ for 1-5 h.
10. The method of any one of claims 1-9,
the aromatic hydrocarbon content of the raw oil containing high aromatic hydrocarbon components is more than 20 weight percent, preferably 50 to 90 weight percent; and/or
The ash content in the raw oil containing the high aromatic hydrocarbon component is not higher than 0.1 wt%; and/or
The content of asphaltene in the raw oil containing the high aromatic hydrocarbon component is not higher than 0.5 wt%;
preferably, the raw oil containing high aromatic hydrocarbon components is selected from one or more of catalytic oil slurry, ethylene tar, furfural extract oil and coal tar, and is preferably selected from catalytic oil slurry.
11. The process of any one of claims 1-10, wherein the light mixed liquid phase fraction enriched in tricyclic and tetracyclic aromatics, density, ash content, asphaltene content are lower than a feedstock oil containing a high aromatic fraction;
preferably, the composition and properties of the light mixed liquid phase component rich in tricyclic and tetracyclic aromatics comprise: the sum of the content of tricyclic aromatic hydrocarbon and tetracyclic aromatic hydrocarbon is 40-85 wt%, the content of ash is not higher than 0.05 wt%, the content of asphaltene is not higher than 0.025 wt%, and the density is 0.8-1.01 kg/m3。
12. The method of any one of claims 1-11, wherein the conditions of fractionation comprise: the temperature of the top of the fractionating tower is 100-145 ℃; and/or
The tower top pressure of the fractionating tower is 0.1-0.17 MPa; and/or
The bottom temperature of the fractionating tower is 310-360 ℃.
13. The method of any of claims 1-12, wherein the operating conditions of the coke drum comprise:
the pressure of the coke tower is 0.3-2.5MPa, preferably 0.5-1.0 MPa; and/or
The coke-forming period is 24-72h, preferably 48-64 h.
14. The method of any one of claims 1-13, wherein the method further comprises: and (3) exchanging heat between raw oil containing high-aromatic hydrocarbon components and one or more of the coking rich gas, the coking gasoline, the coking diesel oil, the coking wax oil and the bottom oil of the fractionating tower, and then mixing the raw oil with the light mixed liquid phase components rich in the tricyclic and tetracyclic aromatic hydrocarbons.
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| CN101302443A (en) * | 2008-06-20 | 2008-11-12 | 中国石油大学(华东) | Combined process for cogeneration of needle coke and light oil |
| CN106635143A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Needle-like coke preparation method |
| CN107987880A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of method and apparatus for preparing needle-shape coke raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101302443A (en) * | 2008-06-20 | 2008-11-12 | 中国石油大学(华东) | Combined process for cogeneration of needle coke and light oil |
| CN106635143A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Needle-like coke preparation method |
| CN107987880A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of method and apparatus for preparing needle-shape coke raw material |
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| WO2024060685A1 (en) * | 2022-09-20 | 2024-03-28 | 中国石油化工股份有限公司 | Method and apparatus for batch-fed manufacture of needle coke |
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