CN112744804A - Method for preparing carbon material from heavy oil slurry - Google Patents
Method for preparing carbon material from heavy oil slurry Download PDFInfo
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- CN112744804A CN112744804A CN201911039785.2A CN201911039785A CN112744804A CN 112744804 A CN112744804 A CN 112744804A CN 201911039785 A CN201911039785 A CN 201911039785A CN 112744804 A CN112744804 A CN 112744804A
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Abstract
The invention relates to the field of heavy oil slurry treatment, and discloses a method for preparing a carbon material from heavy oil slurry, which comprises the following steps: a. carbonizing a mixture of heavy oil slurry and ferric salt in an inert atmosphere to obtain pyrolysis gas and a porous carbon material; b. condensing the cracked gas; c. carrying out catalytic cracking on the oil gas component with the boiling point of below 50 ℃ obtained by condensation to obtain a carbon nano material; wherein the distillation range of the heavy oil slurry is more than 500 ℃, the colloid content of the heavy oil slurry is 10-40 wt%, the asphaltene content of the heavy oil slurry is 5-20 wt%, and the solid content of the heavy oil slurry is 2-7g solid/L oil slurry. The method provides a two-stage cracking technology, so that non-ideal heavy components contained in heavy oil slurry can be utilized, and various nano carbon materials with higher values can be produced.
Description
Technical Field
The invention relates to the field of heavy oil slurry treatment, in particular to a method for preparing a carbon material from heavy oil slurry.
Background
In the process of fluidized catalytic cracking in petroleum refining, a fluidized catalytic cracking unit is usually required to throw out a part of slurry oil in order to control the coke rate and the solid content of the slurry oil, and ensure the safe and stable operation of the unit and the distribution and quality of products. The distillation range of the external throwing slurry is generally higher than 350 ℃, the solid content and the content of polycyclic aromatic hydrocarbon are higher, coke is easy to generate, and the cracking performance is poor. Therefore, the treatment and the comprehensive utilization of the external throwing slurry are the problems to be solved by refineries. The oil slurry can be directly used as a fuel oil blending component, and can also be fed into a delayed coking device together with residual oil, and the utilization value is low although the operation is convenient. And with the improvement of the environmental protection requirement, fuel oil and coke with high sulfur content can not be sold. In addition, higher slurry solids can cause fuel line plugging and higher coke ash content. According to the composition characteristics, the oil slurry can be used for other purposes after pretreatment and separation. The key point of the oil slurry solid removal is the removal of catalyst powder, and the method mainly comprises a settling method, an electrostatic separation method and a filtering method.
In order to improve the added value of the product, the external throwing slurry oil can also be used for producing needle coke through coking. The needle coke is a high-quality petroleum coke with metallic luster and a fibrous texture structure, has the characteristics of easy graphitization, low thermal expansion, high conductivity, low ash content and low sulfur content, and is a main raw material for preparing High Power (HP) and Ultra High Power (UHP) graphite electrodes. With the development of electric vehicles, needle coke is also used as a negative electrode raw material of lithium ion batteries. However, the preparation of needle coke has more severe requirements on raw materials and process, so the oil slurry must be separated, the separated rich saturated components and light aromatic hydrocarbon components can be mixed into the catalytic cracking raw materials, the rich aromatic hydrocarbon components can be used as raw materials for producing the needle coke, and the rich colloid components and asphaltene components can be used for blending road asphalt. Depending on the use of the slurry, there are different methods for separating components or removing bitumen, such as solvent extraction, residue hydrogenation, vacuum distillation, ionic liquid supercritical extraction, etc.
CN1872963A discloses a two-step method of vacuum distillation and hydrogenation for pretreating needle coke raw materials, which can remove non-ideal components in raw oil, and simultaneously keep the content of short side chain less cyclic aromatic hydrocarbon of the ideal components from decreasing. The non-ideal components comprise light saturated hydrocarbon, colloid and asphaltene, and most of the colloid and the asphaltene are in the heavy oil slurry component with the distillation range of more than 500 ℃.
CN106883871A discloses a method for producing needle coke raw material by a combined process of visbreaking treatment and solvent deasphalting treatment. The raw material mixed with the catalyst is heated by a heating furnace and enters a viscosity reduction reactor, then enters a fractionating tower to fractionate dry gas, gasoline fraction and viscosity reduction heavy components, the viscosity reduction heavy components are subjected to solvent deasphalting, deasphalted oil is used for producing needle coke, and the deasphalted asphalt is used as an asphalt blending component.
CN103013567A discloses a method for setting a protection zone before hydrogenation to filter out most of catalytic cracking catalyst powder carried in catalytic cracking slurry oil, so as to realize long-period operation and produce qualified needle coke raw materials.
CN1382761A discloses a method for extracting catalytic cracking clarified oil from lubricant oil extract, in which the extract oil containing catalyst powder and residual oil raw material are used together to produce ordinary petroleum coke or used as fuel oil, and the aromatic hydrocarbon component in the lubricant oil extract, which is beneficial to producing needle coke, is recovered.
However, all of the above patents presuppose that the needle coke feedstock is preferred. There is no good way to handle the non-ideal components, which are only used for asphalt blending, etc.
Disclosure of Invention
The invention aims to solve the problem of how to realize high value-added processing of non-ideal components in the external throwing slurry oil generated by catalytic cracking, and provides a method for preparing a carbon material from heavy slurry oil, which can realize high value-added utilization of the non-ideal components in the heavy slurry oil.
In order to achieve the above object, the present invention provides a method for preparing a carbon material from a heavy oil slurry, comprising:
a. carbonizing a mixture of heavy oil slurry and ferric salt in an inert atmosphere to obtain pyrolysis gas and a porous carbon material;
b. condensing the cracked gas;
c. carrying out catalytic cracking on the oil gas component with the boiling point temperature of below 50 ℃ obtained by condensation to obtain a carbon nano material;
wherein the distillation range of the heavy oil slurry is more than 500 ℃, the colloid content of the heavy oil slurry is 10-40 wt%, the asphaltene content of the heavy oil slurry is 5-20 wt%, and the solid content of the heavy oil slurry is 2-7g solid/L oil slurry.
Preferably, the weight ratio of the heavy oil slurry to the iron salt is 2-5: 1.
preferably, the carbonization temperature is 600-900 ℃, the carbonization pressure is 0.05-0.15MPa, and the carbonization time is 10-120 min.
Preferably, the iron salt is selected from at least one of ferric trichloride, ferric hydroxide, ferric oxide, ferric nitrate, ferric sulfate and ferrocene.
Preferably, the temperature of the catalytic cracking is 600-1200 ℃, and the time of the catalytic cracking is 10-180 min.
Through the technical scheme, the method provided by the invention can utilize the non-ideal heavy components contained in the heavy oil slurry and convert the non-ideal heavy components into the carbon material with higher value. Provides two-stage cracking technology to make full use of non-ideal heavy components.
Drawings
FIG. 1 is a scanning electron micrograph of a porous carbon material obtained in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a cracked carbon obtained in example 1 of the present invention;
fig. 3 is a scanning electron micrograph of the multilayer graphene-like obtained in example 2 of the present invention;
fig. 4 is a scanning electron micrograph of the filamentous nanocarbon obtained in example 3 of the present invention.
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 invention provides a method for preparing a carbon material from heavy oil slurry, which comprises the following steps:
a. carbonizing a mixture of heavy oil slurry and ferric salt in an inert atmosphere to obtain pyrolysis gas and a porous carbon material;
b. condensing the cracked gas;
c. carrying out catalytic cracking on the oil gas component with the boiling point temperature of below 50 ℃ obtained by condensation to obtain a carbon nano material;
wherein the distillation range of the heavy oil slurry is more than 500 ℃, the colloid content of the heavy oil slurry is 10-40 wt%, the asphaltene content of the heavy oil slurry is 5-20 wt%, and the solid content of the heavy oil slurry is 2-7g solid/L oil slurry.
The external throwing oil slurry obtained in the catalytic cracking process is used for preparing heavy oil slurry containing non-ideal components separated in the needle coke preparation process, the components in the heavy oil slurry are used as sources of carbon materials, the carbon materials are converted into carbon materials with higher values, and the utilization rate of the heavy oil slurry is improved. The method provided by the invention provides two-stage cracking, firstly, the porous carbon material is obtained by carbonizing in the step a, and then the obtained pyrolysis gas is further catalytically cracked to produce the carbon nano material. The porous carbon material obtained in the step a can be observed to have a porous structure through a scanning electron microscope, as shown in fig. 1. The conditions of the step a can realize the obtaining of the porous carbon material.
In step a of the method provided by the invention, the heavy slurry oil is treated by carbonization for the first stage of cracking. And in the carbonization process, iron salt is also added into the heavy oil slurry for playing a role in catalyzing and carbonizing to obtain the porous carbon material. Preferably, the weight ratio of the heavy oil slurry to the iron salt is 2-5: 1.
in the present invention, the iron salt may be a powder having an average particle diameter of 10 to 100. mu.m. Preferably, the iron salt is selected from at least one of ferric trichloride, ferric hydroxide, ferric oxide, ferric nitrate, ferric sulfate and ferrocene.
In the step a of the method provided by the invention, preferably, the carbonization temperature is 600-900 ℃, the carbonization pressure is 0.05-0.15MPa, and the carbonization time is 10-120 min. The carbonization condition is favorable for cracking and carbonizing heavy oil slurry with non-ideal components at high temperature, and further, catalytic carbonization is carried out under the participation of ferric salt.
In the invention, the inert atmosphere in the step a can be a gas which does not influence or participate in the reaction process of carbonization, and does not influence the performance of the obtained pyrolysis gas and the porous carbon material. Such as argon, nitrogen, or a mixture of both. The inert atmosphere may be introduced in an amount of 100-500 mL/min.
In the method provided by the invention, preferably, in the step a, the mixture is obtained by the following method: and dissolving the heavy oil slurry in an organic solvent, uniformly mixing the heavy oil slurry with the ferric salt, and then distilling the solvent to remove the organic solvent to obtain the mixture. The use of the organic solvent facilitates uniform mixing of the heavy oil slurry with the iron salt. And the organic solvent is removed through distillation, so that the interference on the reaction process of carbonization is avoided, and the influence on the cracking gas and the porous carbon material of the product is avoided. Preferably, the organic solvent may be selected from Nitrogen Methyl Pyrrolidone (NMP) or toluene.
In the present invention, preferably, the heavy oil slurry: organic solvent: the weight ratio of the ferric salt is 2-5: 5-12: 1.
in the invention, the carbonization in the step a can be carried out in a heating furnace, and the components in the heavy oil slurry are thermally condensed and carbonized to form the porous carbon material. Preferably, the parameters of the porous carbon material include: the average pore diameter is 2-300nm, the specific surface area is 200-1600m2/g。
In the present invention, preferably, the method further includes contacting the porous carbon material with an acid solution to perform cleaning, specifically including: mixing the porous carbon material with acid liquor, and then heating and distilling to clean and remove the residual metal salt compound. The acid solution is at least one of hydrochloric acid solution, nitric acid solution and sulfuric acid solution, and the mass concentration of the acid solution can be 10-30 wt%. The metal salt compound is mainly ferric salt compound.
In the invention, the heavy oil slurry is converted to provide the pyrolysis gas in the step a, and the pyrolysis gas can be suitable for further processing to produce carbon nano materials. B, further separating components in the pyrolysis gas, and separating out liquid components with the boiling point temperature of more than 50 ℃ from the pyrolysis gas through condensation, wherein the liquid components can be left in a condenser; and separating oil gas components with the boiling point temperature of below 50 ℃ and further carrying out step c treatment. The invention selects the cracking gas obtained in the step a, and selects oil gas components with the boiling point temperature of below 50 ℃ to further prepare the carbon nano material.
The step c provided by the invention is used for obtaining the carbon nano material by the oil gas component through the catalytic cracking reaction. Preferably, the temperature of the catalytic cracking is 600-1200 ℃, and the time of the catalytic cracking is 10-180 min.
In the method provided by the invention, preferably, in step c, the catalytic cracking catalyst comprises a carrier and a supported active component, the active component is selected from at least one of copper, cobalt, iron, nickel, copper oxide, cobalt oxide, iron oxide, nickel oxide, copper salt, iron salt, cobalt salt and nickel salt, and the carrier is MgO and Al2O3、Mg(OH)2、Al(OH)3And hydrotalcite.
Further, some embodiments of the present invention provide that, preferably, the active component is contained in an amount of 0.5 to 2 wt% and the carrier is contained in an amount of 98 to 99.5 wt%, based on the total amount of the catalyst.
Further, the method of the invention can use different catalysts to obtain different carbon nanomaterials. Preferably, the carbon nanomaterial is a cracked carbon, a carbon nanofiber, or a graphene-like.
In the present invention, preferably, in step c, the relationship between the amount of the oil gas component and the catalyst is 100-300mL of oil gas component/g of catalyst. So that the oil and gas components are converted into the carbon nano material in the step c.
The present invention will be described in detail below by way of examples. In the following examples of the present invention,
the distillation range of the heavy slurry oil was >500 ℃, the gum content was 28.7 wt%, the asphaltene content was 17.6 wt%, and the solids content was 2.3g solids/L slurry oil. And others: 0.55 wt% of sulfur, 0.63 wt% of ash, 26 wt% of carbon residue (micro method), 15.5 wt% of saturated hydrocarbon and 38.2 wt% of aromatic hydrocarbon.
The pore size and specific surface area of the porous carbon material were measured by the BET nitrogen adsorption method.
The morphology of the porous carbon material and various nano carbon materials prepared in the examples is observed by a scanning electron microscope (Hitachi SU8010, 3 kV).
Example 1
(1) Dissolving the heavy oil slurry in N-methyl pyrrolidone (NMP), and adding ferric chloride, wherein the weight ratio of the heavy oil slurry: NMP: the mass ratio of the ferric chloride is 2:10: 1; after stirring uniformly, distilling the solvent to recover NMP to obtain a solid mixture in which the heavy oil slurry and ferric chloride are mixed uniformly;
placing the mixture into a horizontal cracking furnace, introducing nitrogen as protective gas with flow rate of 200mL/min, performing heating carbonization reaction at 900 deg.C and pressure of 0.15MPa for 30min to obtain cracked gas and porous carbon material (average pore diameter of about 200nm, specific surface area of about 682 m)2The shape observed by a scanning electron microscope is shown in figure 1); further, the prepared porous carbon material is washed by hydrochloric acid, and residual metal salts in the porous carbon material are washed away.
(2) Condensing and separating the pyrolysis gas generated in the step (1) into a liquid component with a boiling point higher than 50 ℃ and an oil-gas component with a boiling point lower than 50 ℃;
(3) carrying out catalytic cracking reaction on an oil gas component and a catalytic cracking catalyst (the composition comprises 0.15g of iron loaded on 10g of hydrotalcite) at 900 ℃ for 60min, wherein the dosage relationship of the oil gas component and the catalyst is 300mL of the oil gas component per 1g of the catalyst, so as to generate cracking carbon, and the appearance is observed by a scanning electron microscope and is shown in figure 2.
Example 2
(1) Dissolving the heavy oil slurry in toluene, and then adding ferric chloride, wherein the weight ratio of the heavy oil slurry: NMP: the mass ratio of the ferric chloride is 4:12: 1; after stirring uniformly, distilling the solvent to recover toluene to obtain a solid mixture in which the heavy oil slurry and ferric chloride are uniformly mixed;
placing the mixture into a horizontal cracking furnace, introducing nitrogen as protective gas with flow rate of 300mL/min, performing heating carbonization reaction at 800 deg.C and pressure of 0.05MPa for 30min to obtain cracked gas and porous carbon material (average pore diameter is about 184nm, specific surface area is about 902 m)2(iv)/g, morphology similar to figure 1); further, the prepared porous carbon material is washed by hydrochloric acid, and residual metal salts in the porous carbon material are washed away.
(2) Condensing and separating the pyrolysis gas generated in the step (1) into a liquid component with a boiling point higher than 50 ℃ and an oil-gas component with a boiling point lower than 50 ℃;
(3) carrying out catalytic cracking reaction on an oil gas component and a catalytic cracking catalyst (the composition comprises 0.2g of Cu loaded on 10g of hydrotalcite) at 1200 ℃ for 60min, wherein the dosage relationship of the oil gas component and the catalyst is 100mL of the oil gas component per 1g of the catalyst, generating multilayer graphene, and observing the morphology by a scanning electron microscope is shown in figure 3.
Example 3
(1) Dissolving the heavy slurry oil in N-methyl pyrrolidone (NMP), and adding ferric nitrate, the heavy slurry oil: NMP: the mass ratio of the ferric nitrate is 5:5: 1; after stirring uniformly, distilling the solvent to recover NMP to obtain a solid mixture of the heavy oil slurry and ferric nitrate which are uniformly mixed;
placing the mixture into a horizontal cracking furnace, introducing nitrogen as protective gas with flow rate of 200mL/min, performing heating carbonization reaction at 900 deg.C and pressure of 0.1MPa for 30min to obtain cracked gas and porous carbon material (average pore diameter of 261nm, specific surface area of 843 m)2The shape is shown in figure 1); further, it is prepared by using hydrochloric acidThe porous carbon material is cleaned, and the residual metal salts are cleaned.
(2) Condensing and separating the pyrolysis gas generated in the step (1) into a liquid component with a boiling point higher than 50 ℃ and an oil-gas component with a boiling point lower than 50 ℃;
(3) the oil gas component and a catalytic cracking catalyst (the composition comprises 0.06g of Co loaded on 10g of hydrotalcite) are subjected to catalytic cracking reaction for 60min at the temperature of 600 ℃, the dosage relationship of the oil gas component and the catalyst is 100mL of oil gas component/1 g of catalyst, so that carbon nanofibers are generated, and the appearance is observed by a scanning electron microscope and is shown in figure 4.
The embodiment of the method provided by the invention can be used for utilizing non-ideal components in heavy oil slurry to prepare various carbon nano materials.
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.
Claims (10)
1. A method for preparing carbon material from heavy oil slurry comprises the following steps:
a. carbonizing a mixture of heavy oil slurry and ferric salt in an inert atmosphere to obtain pyrolysis gas and a porous carbon material;
b. condensing the cracked gas;
c. carrying out catalytic cracking on the oil gas component with the boiling point temperature of below 50 ℃ obtained by condensation to obtain a carbon nano material;
wherein the distillation range of the heavy oil slurry is more than 500 ℃, the colloid content of the heavy oil slurry is 10-40 wt%, the asphaltene content of the heavy oil slurry is 5-20 wt%, and the solid content of the heavy oil slurry is 2-7g solid/L oil slurry.
2. The method of claim 1, wherein in the step a, the weight ratio of the heavy oil slurry to the iron salt is 2-5: 1.
3. the method as claimed in claim 1 or 2, wherein in step a, the temperature of the carbonization is 600-900 ℃, the pressure of the carbonization is 0.05-0.15MPa, and the time of the carbonization is 10-120 min.
4. The process according to claim 1, wherein in step a, the mixture is obtained by: dissolving the heavy oil slurry in an organic solvent, uniformly mixing the heavy oil slurry with the ferric salt, and then distilling the solvent to remove the organic solvent to obtain the mixture;
preferably, the heavy oil slurry: organic solvent: the weight ratio of the ferric salt is 2-5: 5-12: 1.
5. the method of any one of claims 1-4, wherein the iron salt is selected from at least one of iron trichloride, iron hydroxide, iron nitrate, iron sulfate, and ferrocene.
6. The method of claim 1 further comprising contacting the porous carbon material with an acid solution to clean and remove residual metal salt compounds.
7. The method as claimed in claim 1, wherein in step c, the temperature of the catalytic cracking is 600-1200 ℃, and the time of the catalytic cracking is 10-180 min.
8. The method of claim 1, wherein in step c, the catalytic cracking catalyst comprises a carrier and a supported active component, the active component is selected from at least one of copper, cobalt, iron, nickel, copper oxide, cobalt oxide, iron oxide, nickel oxide, copper salt, iron salt, cobalt salt and nickel salt, and the carrier is MgO, Al2O3、Mg(OH)2、Al(OH)3And hydrotalcite;
preferably, the active component is contained in an amount of 0.5 to 2 wt% and the carrier is contained in an amount of 98 to 99.5 wt%, based on the total amount of the catalyst.
9. The method as claimed in claim 8, wherein in step c, the relationship between the amount of the hydrocarbon component and the amount of the catalyst is 100-300mL of the hydrocarbon component/g of the catalyst.
10. The method of claim 1, wherein the carbon nanomaterial is a cracked carbon, a carbon nanofiber, or a graphene-like.
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| CN113604241A (en) * | 2021-08-26 | 2021-11-05 | 西北大学 | Method for preparing needle coke by medium-low temperature coal tar pitch composite extraction modification |
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| CN113604241A (en) * | 2021-08-26 | 2021-11-05 | 西北大学 | Method for preparing needle coke by medium-low temperature coal tar pitch composite extraction modification |
| CN113604241B (en) * | 2021-08-26 | 2022-08-30 | 西北大学 | Method for preparing needle coke by medium-low temperature coal tar pitch composite extraction modification |
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