CN113528175B - Method for preparing needle coke raw material asphalt by coal tar through one-step solvent method - Google Patents
Method for preparing needle coke raw material asphalt by coal tar through one-step solvent method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/007—Working-up pitch, asphalt, bitumen winning and separation of asphalt from mixtures with aggregates, fillers and other products, e.g. winning from natural asphalt and regeneration of waste asphalt
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method comprises the following steps: 1) Desalting and dehydrating coal tar, and removing light oil at 230 ℃ by reduced pressure distillation to obtain heavy oil; 2) Fully mixing heavy oil with aromatic hydrocarbon extractant, and extracting and separating to obtain soluble phase; 3) Recovering aromatic hydrocarbon extractant from the soluble phase by reduced pressure distillation, and simultaneously cutting off 330 ℃ front cut fraction to obtain polycyclic aromatic hydrocarbon oil; 4) And (3) stripping the polycyclic aromatic hydrocarbon oil by inert gas to obtain the raw material asphalt for the needle coke. The invention can obtain the raw material asphalt for the needle coke, which has uniform group composition components, uniform asphalt component reactivity, uniform asphalt thermal reaction and easier control of the liquid phase carbonization process, not only breaks through the technical difficulties of impurity removal and purification of the raw material asphalt, but also solves the problems of complex pretreatment process and higher production cost of the raw material of the needle coke, and lays a foundation for producing high-quality needle coke products.
Description
Technical Field
The invention relates to the technical field of needle coke preparation, in particular to a method for preparing high-quality raw material asphalt for needle coke by using coal tar through a one-step solvent method.
Background
The needle coke is a high-quality carbon material, and the particles are slender needles after being crushed. The needle coke has metallic luster and lamellar structure inside, and has good orientation, electric conductivity and heat conductivity, so that the needle coke is the main raw material for manufacturing the ultra-high power graphite electrode for steelmaking.
Needle coke can be produced by using heavy distillate oil from petroleum processing and coal tar processing, such as thermal cracking residual oil, catalytic cracking clarified oil, coal pitch, etc., and polycyclic (3-4 rings) aromatic hydrocarbon rich in short side chains and linear connection is a high-quality raw material for producing needle coke. Needle coke is classified into coal-based needle coke and oil-based needle coke by raw materials. The requirements of the industrial production on needle coke raw materials are high aromatic hydrocarbon content (about 30-50% by weight ratio) and low colloid asphaltene content (generally controlling heptane insoluble matters)<2.0%), ash (in general<0.05%) and low sulfur content (not more than 0.5%), and vanadium and nickel contents of not more than 50ppm. In addition, the density requirement for the raw material is more than 1.0g/cm 3 To ensure needle coke yield. The narrow molecular weight distribution range, proper distillation range, low viscosity and the like are all necessary conditions for ensuring the quality of coke.
The production technology of pretreatment of coal needle coke raw materials mainly comprises the following 4 types: (1) vacuum distillation method: in 1971, the us LCI company first proposed a vacuum separation method for separating needle coke from coal tar pitch, and applied for us patent, and the core technology is to cut a raw material suitable for producing needle coke by vacuum distillation, the process is simpler, and the yield of needle coke is low. (2) solvent extraction method: in 1981, the company LCI applied for us patent for a method of removing Quinoline Insoluble (QI) components from asphalt by solvent treatment. The treatment technology is similar to an industrial device for producing needle coke from coal tar pitch by Japanese new daily chemical company. The needle coke obtained by the solvent treatment technology has high yield and good quality, but the process is more complex and the investment is higher. (3) M-L method: in 1985, the M-L process of LCI company and Mardzen petrochemical company applied for U.S. patent, which combines special raw material pretreatment technology with a unique two-stage delayed coking system, is the first set of needle coke production equipment using coal tar pitch as raw material. The quality of the produced needle coke is best, but the problems of lower yield, complex process and high investment are also existed. (4) flash-polycondensation process: in 1985, the flash evaporation-polycondensation process was developed together by Anshan coke-resistant Coke, anshan iron and Steel university and Shijia coking plant, and Chinese patent was filed. The method is that the mixed raw oil is sent into a specific flash tower, flash oil is distilled out under a certain temperature and vacuum, and the flash oil enters a polycondensation kettle to be polymerized, thus obtaining the polycondensation asphalt. The process has moderate yield and simple process.
The method is characterized in that a 2 ten thousand t/year coal needle coke production device is built by adopting a Anshan coke hospital-resistant technology in 8 months in 1994 by adopting a flash evaporation and narrow fraction polymerization process, and 4000 tons of products are intermittently produced in 1998 through 4 years of production test run, device transformation and technical improvement, so that the method is used for manufacturing high-power graphite electrodes. However, the utilization rate of the asphalt is very low after flash evaporation and polymerization, the process is difficult to run smoothly, the economic benefit is poor, and the device stops running at the end of 1998. The Jinzhou petrochemical company adopts Beijing stone department technology to build a 4 ten thousand t/a petroleum needle coke production device in 1995, the sulfur content, ash content, true density and the like of the product are close to the level of foreign high-quality needle coke (which can be proportioned to produce ultra-high power graphite electrodes) after device transformation in 2005, but the product is inferior to the foreign high-quality needle coke in terms of strength, granularity distribution and the like, but a few domestic large carbon factories are in use. The Shandong Jining mining blue coalification company adopts the technology of a medium steel heat energy institute, a 2 ten thousand t/a coal needle coke production device is built in 1999, no production is put into operation for various reasons, the existing raw material pretreatment system is used for producing impregnant asphalt and binder asphalt, and the delayed coking system is changed into coal tar processing. The steel has a set of delayed coking unit with the capacity of 5 ten thousand t/a, is used for producing asphalt coke, and a set of pilot plant for needle coke is built in 2002, and no qualified needle coke product is produced. 5 ten thousand tons/year coal needle coke production device is built in Shanxi Hongte 2005, flash evaporation and narrow fraction (polymerization) process are adopted, and product quality indexes (such as granularity, true density, CTE and the like) do not reach the imported needle coke level yet.
Disclosure of Invention
The invention aims to provide a method for preparing high-quality raw material asphalt for needle coke by using coal tar through a one-step solvent method, wherein the preparation method provided by the invention can obtain raw material asphalt for needle coke, which has uniform group composition components (the group composition refers to toluene and quinoline extraction on the coal asphalt, and the obtained alpha component, beta component and gamma component), uniform asphalt component reaction activity, uniform asphalt thermal reactivity and easier control of a liquid-phase carbonization process, thereby breaking through the technical difficulties of impurity removal and purification of the raw material asphalt, solving the problems of complex pretreatment process and higher production cost of the needle coke raw material, and laying a foundation for producing high-quality needle coke products.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method comprises the following steps:
1) Desalting and dehydrating coal tar, and removing light oil at 230 ℃ by reduced pressure distillation to obtain heavy oil;
2) Fully mixing heavy oil with aromatic hydrocarbon extractant, and extracting and separating to obtain soluble phase;
3) Recovering aromatic hydrocarbon extractant from the soluble phase by reduced pressure distillation, and simultaneously cutting off 330 ℃ front cut fraction to obtain polycyclic aromatic hydrocarbon oil;
4) And (3) stripping the polycyclic aromatic hydrocarbon oil by inert gas to obtain the raw material asphalt for the needle coke.
The coal tar in the step 1) is medium-low temperature coal tar or high-temperature carbonization coal tar, wherein the saturated content of the medium-low temperature coal tar is less than or equal to 35wt%, the aromatic content is more than or equal to 45wt%, the colloid and asphaltene content is less than or equal to 20wt%, and the toluene insoluble content is less than or equal to 5wt%; the content of phenol in the high-temperature carbonization coal tar is less than or equal to 3wt percent, and the content of toluene insoluble matters is less than or equal to 10wt percent.
The light oil in the step 1) comprises light oil, phenol oil, naphthalene oil, saturated fraction, wax oil and 230 ℃ front-end distillate.
The distillate amount of the heavy oil in the step 1) is more than or equal to 50 percent by volume, the content of heptane insoluble matters is more than or equal to 70 percent by mass, the content of toluene soluble matters is more than or equal to 50 percent by mass, and the content of toluene insoluble matters is more than or equal to 5 percent by mass.
The aromatic hydrocarbon extractant in the step 2) is one or a mixture of a plurality of crude benzene, light benzene, toluene, xylene or pyridine.
The oil-to-liquid ratio of the heavy oil and the aromatic hydrocarbon extractant in the step 2) is the mass ratio, and the ratio is the heavy oil: aromatic hydrocarbon extractant= (0.25-10): 1.
the temperature of the mixing of the heavy oil and the aromatic hydrocarbon extractant in the step 2) is 20-80 ℃, the mixing time is 0.5-3 h, and the stirring rotating speed is 20-200 rad/min.
The extraction and separation in the step 2) is extraction or supercritical extraction, the extraction condition is that the bottom temperature of the kettle is 80-160 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature residence time is 0.5-6 h; the supercritical extraction condition is that the reaction temperature is 40-100 ℃, the pressure is 0.5-4 Mpa, and the time is 0.5-4 h. .
The distillate of the soluble phase in the step 2) at 380 ℃ is more than or equal to 70 percent by volume, the content of heptane insoluble matters is more than or equal to 85 percent by mass, the content of toluene soluble matters is more than or equal to 70 percent by mass, and the content of toluene insoluble matters is less than or equal to 1 percent by mass.
The heptane solubles of the polycyclic aromatic hydrocarbon oil in the step 3) is less than or equal to 20 weight percent, the heptane insoluble matters are more than or equal to 75 weight percent, and the toluene insoluble matters are less than or equal to 8 weight percent.
The inert gas in the stripping reaction in the step 4) is nitrogen or argon, the temperature is 230-320 ℃, and the flow is 0.5-5L/min.
The raw material asphalt for needle coke in the step 4) has a softening point of 15-40 ℃, toluene insoluble component content of 0.1-1 wt%, quinoline insoluble component content of 0-0.1 wt%, ash content less than 0.1wt%, sulfur content less than or equal to 0.55wt% and nitrogen content less than or equal to 0.5wt%.
Compared with the prior art, the invention has the beneficial effects that:
1) Compared with the conventional solvent method which is used for preparing the recycled soft asphalt, the method directly takes the coal tar as the raw material, and reduces the raw material cost in the production process of the needle coke for preparing the needle coke in the tar processing field;
2) The traditional solvent method is that the raw material asphalt for the needle coke is obtained after the soft asphalt is subjected to the processes of wash oil dissolution, kerosene flocculation and sedimentation, the ideal treatment effect can be obtained by only using one solvent, the treatment temperature is low, the treatment condition is mild, the yield of the obtained raw material asphalt for the needle coke is high, and the production cost in the preparation process of the needle coke is reduced;
3) The raw material asphalt for needle coke obtained by the traditional solvent method contains 0.01-1% of quinoline insoluble component and 4-10% of toluene insoluble component, and the raw material asphalt for needle coke contains 0.0-0.1% of quinoline insoluble component and 0.01-4% of toluene insoluble component. The invention not only breaks through the technical difficulties of raw material asphalt impurity removal and purification, but also solves the problems of complex pretreatment process and higher production cost of needle coke raw materials, and lays a foundation for producing high-quality needle coke products.
Drawings
FIG. 1 is a graph of the macroscopic morphology of needle coke produced by the process of the present invention;
FIG. 2 is a view showing the polarizing microstructure of needle coke produced by the method of the present invention.
Detailed Description
The present invention will be described in more detail by way of examples, which are merely illustrative of the best modes of carrying out the invention, and do not limit the scope of the invention in any way.
Example 1:
after desalting and dehydrating the high-temperature carbonization coal tar, distilling the coal tar by a distillation tower under the conditions that the tower bottom temperature is 380 ℃, the tower top temperature is 240 ℃, the vacuum degree is 0.05MPa, cutting off the front cut at the gas phase temperature of 230 ℃, and obtaining heavy oil at the tower bottom according to the oil agent ratio of 0.25:1, fully mixing heavy oil and crude benzene in an oil mixing kettle at the temperature of 40 ℃ for 1h at the stirring rotation speed of 60rad/min, treating the mixed solution by an extraction reactor, wherein the kettle bottom temperature is 100 ℃, the vacuum degree is 0.05MPa, the final temperature residence time is 2h, obtaining a soluble phase at the bottom of the kettle after extraction, distilling the soluble phase by a distillation tower under the conditions of the bottom temperature of 410 ℃, the top temperature of 280 ℃, the vacuum degree of 0.08MPa, recovering crude benzene at the side line of the tower, cutting off a front fraction at the gas phase temperature of 330 ℃, obtaining condensed ring aromatic oil at the bottom of the distillation tower, wherein the heptane soluble substance is 12%, the heptane insoluble substance is 88%, and the toluene insoluble substance is 3%. The polycyclic aromatic hydrocarbon oil is subjected to gas stripping in nitrogen atmosphere at 270 ℃, the nitrogen flow is 3L/min, and the raw material asphalt for needle coke is obtained, wherein the softening point is 30 ℃, the toluene insoluble matter component content is 0.3wt% and the quinoline insoluble matter component content is 0.01wt%.
Example 2:
after desalting and dehydrating the high-temperature carbonization coal tar, distilling the coal tar by a distillation tower under the conditions that the tower bottom temperature is 400 ℃, the tower top temperature is 260 ℃, the vacuum degree is 0.03MPa, cutting off the front cut at the gas phase temperature of 230 ℃, and obtaining heavy oil at the tower bottom according to the oil agent ratio of 1: and 1, fully mixing heavy oil and light benzene in an oil mixing kettle at the temperature of 60 ℃ for 1.5h at the stirring rotation speed of 45rad/min, treating the mixed solution by an extraction reactor after uniform mixing, wherein the bottom temperature of the kettle is 90 ℃, the vacuum degree is 0.08MPa, the final temperature residence time is 1.5h, obtaining a soluble phase at the bottom of the kettle after extraction, distilling the soluble phase by a distillation tower under the conditions of the bottom temperature of 430 ℃, the top temperature of 300 ℃ and the vacuum degree of 0.06MPa, recovering crude benzene at the side line of the tower, cutting off a front fraction at the gas phase temperature of 260 ℃, and obtaining polycyclic aromatic hydrocarbon oil at the bottom of the distillation tower, wherein the heptane soluble substance is 14%, the heptane insoluble substance is 86% and the toluene insoluble substance is 4%. The polycyclic aromatic hydrocarbon oil is stripped in nitrogen atmosphere at 280 ℃, the nitrogen flow is 3.5L/min, and the raw material asphalt for needle coke is obtained, wherein the softening point is 35 ℃, the toluene insoluble matter component content is 0.5wt%, the quinoline insoluble matter component content is 0.01wt%, the ash content is 0.06wt%, the sulfur content is 0.45wt%, and the nitrogen content is 0.40wt%.
Example 3:
desalting and dehydrating the low-temperature coal tar, and distilling the low-temperature coal tar by a distillation tower under the conditions that the bottom temperature is 390 ℃, the top temperature is 255 ℃, the vacuum degree is 0.04MPa, cutting off the front cut at the gas phase temperature of 230 ℃, and obtaining heavy oil at the bottom of the distillation tower according to the oil agent ratio of 6:1, fully mixing heavy oil and toluene in an oil mixing kettle, wherein the mixing temperature is 20 ℃, the time is 3h, the stirring rotating speed is 150rad/min, after uniform mixing, carrying out supercritical extraction on the mixed solution, the reaction temperature is 60 ℃, the pressure is 0.3MPa, the time is 3h, obtaining a soluble phase at the bottom of the kettle after extraction, distilling the soluble phase by a distillation tower, the distillation condition is that the tower bottom temperature is 380 ℃, the tower top temperature is 260 ℃, the vacuum degree is 0.09MPa, crude benzene is recovered from the side line of the tower, the front fraction of the gas phase temperature is 340 ℃, and obtaining polycyclic aromatic hydrocarbon oil at the bottom of the distillation tower, wherein the heptane soluble substance is 18%, the heptane insoluble substance is 82%, and the toluene insoluble substance is 2%. The polycyclic aromatic hydrocarbon oil is stripped in nitrogen atmosphere at 300 ℃, the nitrogen flow is 2.5L/min, and the raw material asphalt for needle coke is obtained, wherein the softening point is 20 ℃, the content of toluene insoluble matters is 0.1wt%, the content of quinoline insoluble matters is 0.005wt%, the ash content is 0.03wt%, the sulfur content is 0.35wt% and the nitrogen content is 0.32wt%.
Example 4:
desalting and dehydrating the low-temperature coal tar, and distilling the low-temperature coal tar by a distillation tower under the conditions that the bottom temperature is 410 ℃, the top temperature is 265 ℃, the vacuum degree is 0.05MPa, cutting off the front cut at the gas phase temperature of 230 ℃, and obtaining heavy oil at the bottom of the distillation tower according to the oil agent ratio of 9:1, fully mixing heavy oil and dimethylbenzene in an oil mixing kettle at the temperature of 75 ℃ for 0.5h at the stirring speed of 100rad/min, carrying out supercritical extraction on the mixed solution after uniform mixing, wherein the reaction temperature is 90 ℃, the pressure is 0.15MPa, the time is 2h, obtaining a soluble phase at the bottom of the kettle after extraction, distilling the soluble phase in a distillation tower under the conditions of the bottom temperature of 400 ℃ and the top temperature of 280 ℃ and the vacuum degree of 0.07MPa, recovering crude benzene at the side line of the tower, cutting off a front fraction at the gas phase temperature of 320 ℃, and obtaining condensed ring aromatic oil at the bottom of the distillation tower, wherein the heptane soluble substance is 9%, the heptane insoluble substance is 91% and the toluene insoluble substance is 5%. The polycyclic aromatic hydrocarbon oil is stripped in nitrogen atmosphere at the temperature of 250 ℃, the nitrogen flow is 4L/min, and the raw material asphalt for needle coke is obtained, wherein the softening point is 40 ℃, the content of toluene insoluble matters is 0.8wt%, the content of quinoline insoluble matters is 0.01wt%, the ash content is 0.02wt%, the sulfur content is 0.25wt%, and the nitrogen content is 0.30wt%.
Claims (6)
1. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method is characterized by comprising the following steps of:
1) Desalting and dehydrating coal tar, and removing light oil at 230 ℃ by reduced pressure distillation to obtain heavy oil;
2) Fully mixing heavy oil with aromatic hydrocarbon extractant, and extracting and separating to obtain soluble phase;
3) Recovering aromatic hydrocarbon extractant from the soluble phase by reduced pressure distillation, and simultaneously cutting off 330 ℃ front cut fraction to obtain polycyclic aromatic hydrocarbon oil;
4) The polycyclic aromatic hydrocarbon oil is subjected to gas stripping by inert gas to obtain raw material asphalt for needle coke;
the coal tar in the step 1) is medium-low temperature coal tar or high-temperature carbonization coal tar, wherein the saturated content of the medium-low temperature coal tar is less than or equal to 35wt%, the aromatic content is more than or equal to 45wt%, the colloid and asphaltene content is less than or equal to 20wt%, and the toluene insoluble content is less than or equal to 5wt%; the phenol content of the high-temperature carbonization coal tar is less than or equal to 3wt percent, and the toluene insoluble matter content is less than or equal to 10wt percent;
the aromatic hydrocarbon extractant in the step 2) is one or a mixture of a plurality of crude benzene, light benzene, toluene, xylene or pyridine.
The oil-to-liquid ratio of the heavy oil and the aromatic hydrocarbon extractant in the step 2) is the mass ratio, and the ratio is the heavy oil: aromatic hydrocarbon extractant= (0.25-10): 1, a step of;
the temperature for mixing the heavy oil and the aromatic hydrocarbon extractant is 20-80 ℃, the mixing time is 0.5-3 h, and the stirring rotating speed is 20-200 rad/min;
the extraction and separation in the step 2) is extraction or supercritical extraction, the extraction condition is that the bottom temperature of the kettle is 80-160 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature residence time is 0.5-6 h; the supercritical extraction condition is that the reaction temperature is 40-100 ℃, the pressure is 0.5-4 Mpa, and the time is 0.5-4 h;
the distillate of the soluble phase in the step 2) at 380 ℃ is more than or equal to 70 percent by volume, the content of heptane insoluble matters is more than or equal to 85 percent by mass, the content of toluene soluble matters is more than or equal to 70 percent by mass, and the content of toluene insoluble matters is less than or equal to 1 percent by mass.
2. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method according to claim 1, wherein the light oil in the step 1) comprises light oil, phenol oil, naphthalene oil, saturated fraction, wax oil and 230 ℃ front cut oil.
3. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method according to claim 1, wherein the amount of the heavy oil distilled out in the step 1) at 380 ℃ is more than or equal to 50% by volume fraction, the content of heptane insoluble matters is more than or equal to 70% by mass fraction, the content of toluene soluble matters is more than or equal to 50% by mass fraction, and the content of toluene insoluble matters is more than or equal to 5% by mass fraction.
4. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method according to claim 1, wherein the heptane solubles of the polycyclic aromatic hydrocarbon oil in the step 3) is less than or equal to 20wt%, the heptane insoluble matter is less than or equal to 75wt%, and the toluene insoluble matter is less than or equal to 8wt%.
5. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method according to claim 1, wherein the inert gas in the stripping reaction in the step 4) is nitrogen or argon, the condition is that the temperature is 230-320 ℃, and the flow is 0.5-5L/min.
6. The method for preparing needle coke raw material asphalt by using coal tar through a one-step solvent method according to claim 1, wherein the raw material asphalt for needle coke in the step 4) has a softening point of 15-40 ℃, toluene insoluble component content of 0.1-1 wt%, quinoline insoluble component content of 0-0.1 wt%, ash content of less than 0.1wt%, sulfur content of less than or equal to 0.55wt%, and nitrogen content of less than or equal to 0.5wt%.
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