CN111826187B - Special high-performance asphalt for carbon material and preparation method thereof - Google Patents
Special high-performance asphalt for carbon material and preparation method thereof Download PDFInfo
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- CN111826187B CN111826187B CN202010646825.6A CN202010646825A CN111826187B CN 111826187 B CN111826187 B CN 111826187B CN 202010646825 A CN202010646825 A CN 202010646825A CN 111826187 B CN111826187 B CN 111826187B
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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
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
Abstract
The invention relates to a preparation method of special high-performance asphalt for carbon materials, which comprises the steps of carrying out preliminary thermal polycondensation on raw material coal asphalt to form a microcrystal unit, respectively carrying out component cutting by adopting two solvents, and then carrying out treatments such as asphaltization, thermal separation, filter pressing, distillation, hydrogenation and the like to simultaneously obtain novel special high-performance asphalt for carbon materials, which keeps good plasticity and fluidity, stable thermal reactivity and uniformity in a wider temperature range under two heat treatments; one of the raw materials can be used as impregnant asphalt, binder asphalt, special asphalt, general-grade spinnable asphalt for carbon fiber, lithium ion battery cathode material, ultrahigh-power graphite electrode, spherical active carbon and the like; the other can be used as the raw material of coal-series mesophase pitch, high-performance carbon fiber spinnable pitch, high-heat-conductivity foam carbon and the like. The performance index of the product prepared by the invention is flexible and adjustable, and the product can better adapt to market change and reduce enterprise operation risk.
Description
Technical Field
The invention relates to the technical field of efficient utilization of coal pitch, in particular to high-performance pitch special for a carbon material and a preparation method thereof.
Background
Coal tar pitch is a bulk product separated in the coal tar processing process, accounts for about 50-60% of the coal tar, and the processing and utilization level of the coal tar pitch is very important for the whole coal tar processing and carbon material development and preparation. The coal tar pitch is a complex mixture composed of polycyclic aromatic hydrocarbons, has the characteristics of high molecular weight, high aromaticity, high condensation degree, high carbon content, relatively low content of heteroatoms and metals and the like, and is a high-quality precursor for preparing functional carbon materials. The chemical composition and the molecular structure of the coal pitch are reasonably designed, and the construction of the functional carbon material by taking coal pitch molecules as basic structural units is expected to become one of important ways for high added value utilization of the coal pitch, such as impregnant pitch, binder pitch, special pitch, spinnable pitch for general-grade carbon fiber, lithium ion battery cathode material, ultrahigh power graphite electrode, spherical active carbon, coal-series mesophase pitch, high-performance carbon fiber spinnable pitch, high-heat-conductivity foam carbon and other fields.
The high-performance asphalt special for the novel carbon material has the characteristics of high content (over 60 percent) of aromatic compounds, narrow molecular weight distribution, alkyl side chains and naphthenic groups, few and short side chains, low content of impurity elements and ash, and the like.
The asphalt prepared by direct polycondensation of coal tar pitch cannot meet the requirements, and the coal tar pitch needs to be pretreated or modified to adjust the chemical composition and molecular structure of the coal tar pitch, control the structure and molecular weight distribution of raw materials and remove ash and heteroatoms.
Chinese patent application publication No. CN 102690672A discloses a method for preparing coal tar refined pitch, which comprises performing mild thermal polycondensation reaction on coal tar medium temperature pitch serving as a raw material to obtain a polycondensation product, adding the polycondensation product into an aromatic hydrocarbon solvent to perform solvent washing and filtering, filtering to remove filter residue to obtain a filtrate of refined pitch, performing reduced pressure distillation on the obtained filtrate, and removing the solvent to obtain the refined pitch. The method has the advantages that the viscosity of the polymerized asphalt is high, the filter residue removing process is difficult to realize, and the performance of the prepared refined asphalt is unstable.
The method comprises the steps of carrying out preliminary thermal polycondensation on raw material coal pitch to form a microcrystal unit, respectively carrying out component cutting by adopting two solvents, and then carrying out treatments such as asphaltization, thermal separation, filter pressing, distillation, hydrogenation and the like to simultaneously obtain two types of special high-performance pitch for novel carbon materials, which can keep good plasticity and fluidity, stable thermal reactivity and uniformity in a wider temperature range under thermal treatment, wherein the special high-performance pitch can be used as impregnant pitch, binder pitch, special pitch, spinnable pitch for general-grade carbon fibers, lithium ion battery cathode materials, ultrahigh-power graphite electrodes, spherical active carbon and the like; the other can be used as coal-series mesophase pitch, high-performance carbon fiber spinnable pitch, high-thermal conductivity foam carbon and the like. The performance index of the product is flexible and adjustable, the product can better adapt to market change, and the operation risk of enterprises is reduced.
Disclosure of Invention
The invention provides a preparation method of special high-performance asphalt for carbon materials, which can simultaneously obtain two types of novel special high-performance asphalt for carbon materials, which can keep good plasticity and fluidity, stable thermal reaction and uniformity in a wider temperature range under heat treatment, not only solves the problem of high-efficiency high-added-value utilization of coal asphalt, but also further optimizes the product structure, extends the industrial chain and reduces the production cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of special high-performance asphalt for carbon materials comprises the following steps of preparing novel special high-performance asphalt for carbon materials, wherein the novel special high-performance asphalt for carbon materials comprises rectified asphalt B and refined hydrogenated asphalt D; the preparation process comprises the following steps:
firstly, under inert atmosphere, according to the activation energy of high-reactivity components contained in raw material asphalt, carrying out primary thermal polycondensation on the raw material asphalt by controlling the thermal reaction temperature to form a microcrystal unit, wherein the prepared intermediate is called pre-polymerized asphalt;
step two, mixing the pre-polymerized asphalt obtained in the step one with a solvent I according to a set agent oil ratio, fully stirring, standing, settling and separating to obtain light phase oil and heavy phase oil according to a set separation ratio; the solvent-oil ratio of the pre-polymerized asphalt to the solvent I is (0.5-5): 1; the set separation ratio is light phase oil according to the mass ratio: heavy phase oil = (5-9.5): (5-0.5);
step three, distilling the light phase oil obtained in the step two to recover a solvent I, and then performing asphaltization treatment under the protection of inert gas to obtain rectified asphalt A;
step four, the heavy phase oil obtained in the step two is returned to the solvent I with a certain proportion, and a soluble component and an insoluble component are obtained after thermal separation treatment; the heavy phase oil and the first solvent which is recycled are heavy phase oil according to the mass ratio: solvent i = 1: (0.2-10); mixing the insoluble component with a solvent II according to a set solvent-oil ratio, and performing filter pressing treatment to obtain a filter cake and a filtrate, wherein the filter cake is inorganic impurities and other insoluble solid particles; the solvent-oil ratio of the insoluble component to the solvent II is 1: (0.5 to 10); mixing the filtrate with soluble components, and distilling to recover solvent I and solvent II to obtain rectified asphalt B;
step five, mixing the rectified asphalt A obtained in the step three with a hydrogen supply reagent according to a set proportion, and performing high-temperature and high-pressure heat treatment to obtain hydrogenated asphalt C; the mixing proportion of the rectified asphalt A to the hydrogen donor reagent is 1: (1-8); distilling the hydrogenated asphalt C to recover an unreacted hydrogen donor reagent, mixing the hydrogen donor reagent with the solvent I according to a set solvent-oil ratio, removing residues through hot filtration, and distilling to recover the solvent I to obtain refined hydrogenated asphalt D; the solvent-oil ratio of the hydrogenated asphalt C to the solvent I is (0.5-5): 1.
in the first step, the raw material asphalt is coal asphalt obtained by high-temperature dry distillation of coal, the softening point is 20-150 ℃, and the mass content of quinoline insoluble substances is 1-20%.
In the first step, the inert atmosphere is a high-purity nitrogen atmosphere or a high-purity argon atmosphere.
In the first step, the high-reactivity components are solid particles such as heavy components insoluble in quinoline and inorganic impurities in the raw material asphalt.
In the first step, the temperature of the preliminary thermal polycondensation is 350-400 ℃, the constant temperature time is 0.5-8 h, and the heating rate is 0.5-5 ℃/min.
In the first step, the density of the pre-polymerized asphalt is 1.1-1.6 g/cm3The size of the microcrystal unit is controlled to be 2-15 μm.
In the second step, the first solvent is any one or a mixture of more than two of fractions at 200-350 ℃ in the separation process of coal tar, coal directly liquefied light oil, wash oil, first anthracene oil, second anthracene oil, coking heavy oil, coking light oil, naphthalene oil, kerosene, petroleum ether, gasoline, diesel oil, lubricating oil and paraffin oil.
In the second step, the standing, settling and separating are performed in a way that the length-diameter ratio is (1-20): 1, the settling temperature is 80-200 ℃, and the settling time is 0.5-5 h.
In the second step, the density of the light phase oil is 0.85-1.1 g/cm3The density of the heavy phase oil is 1.0-1.35 g/cm3。
In the third step, the distillation comprises atmospheric distillation and reduced pressure distillation; wherein, the atmospheric distillation conditions are as follows: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the third step, the temperature of the asphaltization treatment is 330-420 ℃, the heating rate is 0.5-5 ℃/min, and the final temperature retention time is 0.5-10 h.
In the third step, the rectified asphalt A is micromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-1800 and the centralized molecular weight of 600-1200, the softening point is 35-95 ℃, the mass content of quinoline insoluble substances is 0-0.05%, and the atomic ratio of H to C is (0.45-0.6): 1.
in the fourth step, the thermal separation treatment adopts centrifugal separation, and the treatment conditions are as follows: the separation temperature is 60-150 ℃, the separation time is 0.5-3 h, the centrifugal rotation speed is 800-2000 rad/min, and the separation solid phase density is 0.9-1.3 g/cm3The mesh number of the screen is 300-1200 meshes.
In the fourth step, the solvent II is any one or a mixture of more than two of toluene, xylene, pyridine, heptane, pentane and tetrahydrofuran.
In the fourth step, the filter pressing treatment conditions are as follows: the filter pressing temperature is 80-150 ℃, the filter pressing time is 0.5-3 h, and the mesh number of the screen is 300-1200 meshes.
In the fourth step, the mass content of quinoline insoluble substances in the filtrate is less than 0.1%.
In the fourth step, the distillation comprises atmospheric distillation or reduced pressure distillation; the atmospheric distillation conditions were: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the fourth step, the rectified asphalt B is macromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-2000 and the concentrated molecular polycyclic aromatic hydrocarbon of 800-1400, the softening point is 30-80 ℃, the mass content of quinoline insoluble substances is 0-0.2%, and the atomic ratio of H to C is (0.45-0.55): 1.
in the fifth step, the hydrogen donor reagent is any one or a mixture of more than two of tetrahydronaphthalene, octahydronaphthalene, tetrahydroquinoline and decahydroquinoline.
In the fifth step, the hydrogenation conditions of the high-temperature high-pressure heat treatment are as follows: and filling nitrogen into the reaction kettle, wherein the initial pressure is 0.5-3 MPa, the heating rate is 1-10 ℃/min, the final temperature is 380-440 ℃, the heat preservation time is 1-6 h, and the final pressure in the kettle is 4-6 MPa.
In the fifth step, the distillation comprises atmospheric distillation or reduced pressure distillation; the atmospheric distillation conditions were: the gas phase temperature is 210-300 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 150-240 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the fifth step, the hot filtration adopts a suction filtration mode, and the conditions are as follows: the filtering temperature is 100-250 ℃, the vacuum degree is 0.01-0.09 MPa, and the mesh number of the screen is 300-1200 meshes.
In the fifth step, the refined hydrogenated asphalt D has a softening point of 30-80 ℃, a quinoline insoluble matter content of 0-0.05%, and an H/C atomic ratio of (0.55-0.75): 1.
compared with the prior art, the invention has the beneficial effects that:
1) two kinds of special high-performance asphalt for the novel carbon material, namely refined hydrogenated asphalt D and refined asphalt B, which can keep good plasticity and fluidity and stable and uniform thermal reactivity in a wider temperature range under heat treatment can be obtained simultaneously;
2) the coal tar pitch has high processing degree, multiple varieties and high added value of products, optimizes the product structure, extends the industrial chain and reduces the production cost;
3) the performance index of the product is flexible and adjustable, the product can better adapt to market change, and the enterprise operation risk is reduced;
4) the rectified asphalt B can be used as impregnant asphalt, binder asphalt, special asphalt, spinnable asphalt for general-grade carbon fiber, lithium ion battery cathode material, ultrahigh-power graphite electrode, spherical active carbon and the like; the refined hydrogenated pitch D can be used as coal-based mesophase pitch, high-performance carbon fiber spinnable pitch, high-thermal conductivity foam carbon and the like.
Drawings
FIG. 1 is a process flow chart of the preparation method of the high-performance asphalt special for carbon materials.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
as shown in figure 1, the preparation method of the special high-performance asphalt for carbon materials comprises the steps of preparing a novel special high-performance asphalt for carbon materials, wherein the novel special high-performance asphalt for carbon materials comprises rectified asphalt B and refined hydrogenated asphalt D; the preparation process comprises the following steps:
firstly, under inert atmosphere, according to the activation energy of high-reactivity components contained in raw material asphalt, carrying out primary thermal polycondensation on the raw material asphalt by controlling the thermal reaction temperature to form a microcrystal unit, wherein the prepared intermediate is called pre-polymerized asphalt;
step two, mixing the pre-polymerized asphalt obtained in the step one with a solvent I according to a set agent oil ratio, fully stirring, standing, settling and separating to obtain light phase oil and heavy phase oil according to a set separation ratio; the solvent-oil ratio of the pre-polymerized asphalt to the solvent I is (0.5-5): 1; the set separation ratio is light phase oil according to the mass ratio: heavy phase oil = (5-9.5): (5-0.5);
step three, distilling the light phase oil obtained in the step two to recover a solvent I, and then performing asphaltization treatment under the protection of inert gas to obtain rectified asphalt A;
step four, the heavy phase oil obtained in the step two is returned to the solvent I with a certain proportion, and a soluble component and an insoluble component are obtained after thermal separation treatment; the heavy phase oil and the first solvent which is recycled are heavy phase oil according to the mass ratio: solvent i = 1: (0.2-10); mixing the insoluble component with a solvent II according to a set solvent-oil ratio, and performing filter pressing treatment to obtain a filter cake and a filtrate, wherein the filter cake is inorganic impurities and other insoluble solid particles; the solvent-oil ratio of the insoluble component to the solvent II is 1: (0.5 to 10); mixing the filtrate with soluble components, and distilling to recover solvent I and solvent II to obtain rectified asphalt B;
step five, mixing the rectified asphalt A obtained in the step three with a hydrogen supply reagent according to a set proportion, and performing high-temperature and high-pressure heat treatment to obtain hydrogenated asphalt C; the mixing proportion of the rectified asphalt A to the hydrogen donor reagent is 1: (1-8); distilling the hydrogenated asphalt C to recover an unreacted hydrogen donor reagent, mixing the hydrogen donor reagent with the solvent I according to a set solvent-oil ratio, removing residues through hot filtration, and distilling to recover the solvent I to obtain refined hydrogenated asphalt D; the solvent-oil ratio of the hydrogenated asphalt C to the solvent I is (0.5-5): 1.
in the first step, the raw material asphalt is coal asphalt obtained by high-temperature dry distillation of coal, the softening point is 20-150 ℃, and the mass content of quinoline insoluble substances is 1-20%.
In the first step, the inert atmosphere is a high-purity nitrogen atmosphere or a high-purity argon atmosphere.
In the first step, the high-reactivity components are solid particles such as heavy components insoluble in quinoline and inorganic impurities in the raw material asphalt.
In the first step, the temperature of the preliminary thermal polycondensation is 350-400 ℃, the constant temperature time is 0.5-8 h, and the heating rate is 0.5-5 ℃/min.
In the first step, the density of the pre-polymerized asphalt is 1.1-1.6 g/cm3The size of the microcrystal unit is controlled to be 2-15 μm.
In the second step, the first solvent is any one or a mixture of more than two of fractions at 200-350 ℃ in the separation process of coal tar, coal directly liquefied light oil, wash oil, first anthracene oil, second anthracene oil, coking heavy oil, coking light oil, naphthalene oil, kerosene, petroleum ether, gasoline, diesel oil, lubricating oil and paraffin oil.
In the second step, the standing, settling and separating are performed in a way that the length-diameter ratio is (1-20): 1, the settling temperature is 80-200 ℃, and the settling time is 0.5-5 h.
In the second step, the density of the light phase oil is 0.85-1.1 g/cm3The density of the heavy phase oil is 1.0-1.35 g/cm3。
In the third step, the distillation comprises atmospheric distillation and reduced pressure distillation; wherein, the atmospheric distillation conditions are as follows: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the third step, the temperature of the asphaltization treatment is 330-420 ℃, the heating rate is 0.5-5 ℃/min, and the final temperature retention time is 0.5-10 h.
In the third step, the rectified asphalt A is micromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-1800 and the centralized molecular weight of 600-1200, the softening point is 35-95 ℃, the mass content of quinoline insoluble substances is 0-0.05%, and the atomic ratio of H to C is (0.45-0.6): 1.
in the fourth step, the thermal separation treatment adopts centrifugal separation, and the treatment conditions are as follows: the separation temperature is 60-150 ℃, the separation time is 0.5-3 h, the centrifugal rotation speed is 800-2000 rad/min, and the separation solid phase density is 0.9-1.3 g/cm3The mesh number of the screen is 300-1200 meshes.
In the fourth step, the solvent II is any one or a mixture of more than two of toluene, xylene, pyridine, heptane, pentane and tetrahydrofuran.
In the fourth step, the filter pressing treatment conditions are as follows: the filter pressing temperature is 80-150 ℃, the filter pressing time is 0.5-3 h, and the mesh number of the screen is 300-1200 meshes.
In the fourth step, the mass content of quinoline insoluble substances in the filtrate is less than 0.1%.
In the fourth step, the distillation comprises atmospheric distillation or reduced pressure distillation; the atmospheric distillation conditions were: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the fourth step, the rectified asphalt B is macromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-2000 and the concentrated molecular polycyclic aromatic hydrocarbon of 800-1400, the softening point is 30-80 ℃, the mass content of quinoline insoluble substances is 0-0.2%, and the atomic ratio of H to C is (0.45-0.55): 1.
in the fifth step, the hydrogen donor reagent is any one or a mixture of more than two of tetrahydronaphthalene, octahydronaphthalene, tetrahydroquinoline and decahydroquinoline.
In the fifth step, the hydrogenation conditions of the high-temperature high-pressure heat treatment are as follows: and filling nitrogen into the reaction kettle, wherein the initial pressure is 0.5-3 MPa, the heating rate is 1-10 ℃/min, the final temperature is 380-440 ℃, the heat preservation time is 1-6 h, and the final pressure in the kettle is 4-6 MPa.
In the fifth step, the distillation comprises atmospheric distillation or reduced pressure distillation; the atmospheric distillation conditions were: the gas phase temperature is 210-300 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 150-240 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
In the fifth step, the hot filtration adopts a suction filtration mode, and the conditions are as follows: the filtering temperature is 100-250 ℃, the vacuum degree is 0.01-0.09 MPa, and the mesh number of the screen is 300-1200 meshes.
In the fifth step, the refined hydrogenated asphalt D has a softening point of 30-80 ℃, a quinoline insoluble matter content of 0-0.05%, and an H/C atomic ratio of (0.55-0.75): 1.
the following examples are carried out on the premise of the technical scheme of the invention, and detailed embodiments and specific operation processes are given, but the scope of the invention is not limited to the following examples. The methods used in the following examples are conventional methods unless otherwise specified.
[ example 1 ]
In the embodiment, the raw material asphalt is coal-series soft asphalt with a softening point of 30 ℃, and according to the quinoline insoluble content of 1.83%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is raised to 400 ℃ from the normal temperature at the speed of 3 ℃/min, the mixture is kept at the constant temperature for 4 hours, a microcrystal unit is formed, and the pre-polymerization asphalt is prepared.
Mixing the pre-polymerized asphalt and the wash oil according to the mass ratio of 3: 1, fully stirring at the temperature of 120 ℃, and pouring the mixture with the length-diameter ratio of 8: 1, carrying out standing sedimentation separation in a standing sedimentation device, wherein the sedimentation temperature is 130 ℃, the sedimentation time is 3h, and then mixing the raw materials in a mass ratio of 8: 2 separating light phase oil and heavy phase oil, and determining the density of the light phase oil to be 1.0g/cm3The density of the heavy phase oil is 1.3g/cm3。
Pouring light-phase oil into a distillation kettle, keeping the gas-phase final temperature at 320 ℃ for 1.5H, recovering washing oil by atmospheric distillation, heating to 380 ℃ at the speed of 3 ℃/min, keeping the temperature for 5H, and carrying out asphaltization treatment to obtain the rectified asphalt A, wherein the softening point of the rectified asphalt A is 60 ℃, the mass content of quinoline insoluble substances is 0.01%, and the atomic ratio of H to C is 0.5: 1.
according to the weight phase oil: the mass ratio of the washing oil is 1: 3 mixing, heating to 70 ℃, fully stirring for 2h, centrifuging at the rotating speed of 800rad/min, and separating the solid phase with the density of 0.9g/cm3And the mesh number of the screen is 400 meshes, and the soluble component and the insoluble component are obtained by centrifugal separation. Mixing insoluble components and toluene according to a mass ratio of 1: 3, heating to 80 ℃, fully stirring for 1.5h, and performing pressure filtration under the vacuum degree of 0.08MPa and the mesh number of a screen of 400 meshes to obtain a filter cake and a filtrate, wherein the QI mass content in the filtrate is 0.02%. Mixing the filtrate with the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 320 ℃ for 1.5 hours, distilling and recovering toluene and wash oil under normal pressure to obtain the rectified asphalt B, wherein the softening point of the rectified asphalt B is 30 ℃, the mass content of quinoline insoluble substances is 0.05 percent, and the H/C atomic ratio is 0.55: 1.
mixing the rectified asphalt A and tetrahydronaphthalene according to the mass ratio of 1: 3, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, filling nitrogen into the reaction kettle, raising the initial pressure to 420 ℃ at the heating rate of 4 ℃/min, preserving the heat for 4 hours, and finally keeping the pressure in the reaction kettle at 4MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase temperature at 230 ℃ for 1h, distilling at normal pressure to recover unreacted tetrahydronaphthalene, and when the temperature in the reaction kettle is reduced to about 200 ℃, adding the hydrogenated asphalt C and the solvent I in a mass ratio of 1: 3, pouring washing oil, mixing, and filtering to remove residues with a 600-mesh screen under the vacuum degree of 0.09 MPa. Pouring the mixed solution into a distillation kettle, keeping the gas phase temperature at 280 ℃ for 1H, and recovering the wash oil by atmospheric distillation to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 30 ℃, the mass content of quinoline insoluble substances is 0.01 percent, and the atomic ratio of H to C is 0.65: 1.
[ example 2 ]
In the embodiment, the raw material asphalt is coal-series medium-temperature asphalt with a softening point of 70 ℃, and according to the mass content of quinoline insoluble matters of 3.85%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is raised to 390 ℃ from the normal temperature at the speed of 2 ℃/min, and the raw material asphalt stays for 5 hours at the constant temperature to form a microcrystal unit, so that the pre-polymerization asphalt is prepared.
Mixing the pre-polymerized asphalt and the dianthracene oil according to a mass ratio of 2: 1, fully stirring at 150 ℃, and pouring the mixture with the length-diameter ratio of 9: 1 in a standing settling deviceAnd (3) performing precipitation separation, wherein the precipitation temperature is 140 ℃, the precipitation time is 3h, and the mass ratio of the components is 7: 3 separating out light phase oil and heavy phase oil, and determining the density of the light phase oil to be 0.9g/cm3The density of the heavy phase oil is 1.2g/cm3。
Pouring the light-phase oil into a distillation kettle, distilling and recovering anthracene oil under the conditions that the final temperature of a gas phase is 260 ℃ and the vacuum degree is 0.08MPa for 1 hour, heating to 400 ℃ at the speed of 2 ℃/min, and standing for 4 hours at constant temperature to perform asphaltization treatment to obtain the rectified asphalt A, wherein the softening point of the rectified asphalt A is 40 ℃, the mass content of quinoline insoluble substances is 0.02%, and the atomic ratio of H to C is 0.55: 1.
the heavy phase oil and the anthracene oil are mixed according to the mass ratio of 1: 4 mixing, heating to 80 ℃, fully stirring for 2h, centrifuging at 1000rad/min, separating the solid phase density to 1.1g/cm3And centrifuging with a screen mesh of 500 meshes to obtain soluble components and insoluble components. Mixing insoluble components and xylene according to a mass ratio of 1: 4, heating to 90 ℃, fully stirring for 2h, and performing pressure filtration under the vacuum degree of 0.09MPa and the mesh number of a screen of 500 meshes to obtain a filter cake and a filtrate, wherein the QI mass content in the filtrate is 0.01%. Mixing the filtrate with the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 260 ℃ for 1H, and recovering xylene and dianthracene oil by reduced pressure distillation under the vacuum degree of 0.08MPa to obtain the rectified asphalt B, wherein the softening point of the rectified asphalt B is 50 ℃, the mass content of quinoline insoluble substances is 0.1%, and the atomic ratio of H to C is 0.5: 1.
mixing the rectified asphalt A and tetrahydronaphthalene according to the mass ratio of 1: and 4, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, introducing nitrogen into the high-temperature high-pressure reaction kettle, raising the initial pressure to 430 ℃ at the heating rate of 5 ℃/min, preserving the heat for 5 hours, and finally keeping the pressure in the kettle at 5MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase at 180 ℃ for 1h, carrying out reduced pressure distillation under the vacuum degree of 0.09MPa to recover unreacted tetrahydronaphthalene, and when the temperature in the reaction kettle reaches about 200 ℃, adding the hydrogenated asphalt C into the distillation kettle according to the mass ratio of 2: 1, pouring anthracene oil into the reactor, mixing, carrying out suction filtration under the conditions that the vacuum degree is 0.08MPa and the mesh number of a screen is 600 meshes to remove residues, pouring the mixed solution into a distillation kettle, keeping the gas phase temperature at 280 ℃ for 1H, and carrying out atmospheric distillation to recover the anthracene oil to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 50 ℃, the mass content of quinoline insoluble substances is 0.02%, and the atomic ratio of H to C is 0.6: 1.
[ example 3 ]
In the embodiment, the raw material asphalt is coal-series medium-temperature asphalt with a softening point of 95 ℃, and according to the mass content of quinoline insoluble substances of 6.82%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is raised to 380 ℃ from the normal temperature at a speed of 2 ℃/min, and the mixture stays for 6 hours at the constant temperature to form a microcrystal unit, so that the pre-polymerization asphalt is prepared.
Mixing pre-polymerized asphalt and anthracene oil according to a mass ratio of 1: 1, fully stirring at 160 ℃, and pouring the mixture with the length-diameter ratio of 10: 1, settling and separating in a standing and settling device, wherein the settling temperature is 140 ℃, the settling time is 3h, and then the mass ratio of the components is 8: 2 separating out light phase oil and heavy phase oil, and determining the density of the light phase oil to be 1.06g/cm3The density of the heavy phase oil is 1.34g/cm3。
Pouring the light-phase oil into a distillation kettle, keeping the gas-phase final temperature at 330 ℃ for 1H, distilling under normal pressure to recover anthracene oil, heating to 390 ℃ at the speed of 2 ℃/min, keeping the temperature for 5H to carry out asphaltization treatment to obtain the rectified asphalt A, wherein the softening point of the rectified asphalt A is 50 ℃, the mass content of quinoline insoluble substances is 0.01%, and the atomic ratio of H to C is 0.52: 1.
according to the weight phase oil: the mass ratio of anthracene oil is 1: 5 mixing, heating to 100 deg.C, stirring for 1.5h, centrifuging at 1200rad/min, and separating to obtain solid phase with density of 1.2g/cm3And centrifuging under 600 meshes to obtain soluble component and insoluble component. Mixing insoluble components with pyridine according to a mass ratio of 1: 5, mixing, heating to 100 ℃, fully stirring for 2h, and performing pressure filtration under the vacuum degree of 0.08MPa and the mesh number of a screen of 600 meshes to obtain a filter cake and a filtrate, wherein the QI mass content in the filtrate is 0.04%. Mixing the filtrate with the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 330 ℃ for 1H, distilling and recovering pyridine and anthracene oil under normal pressure to obtain the rectified asphalt B, wherein the softening point of the rectified asphalt B is 60 ℃, the mass content of quinoline insoluble substances is 0.09%, and the H/C atomic ratio is 0.48: 1.
mixing the rectified asphalt A and tetrahydronaphthalene according to the mass ratio of 1: 5, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, introducing nitrogen into the high-temperature high-pressure reaction kettle, raising the initial pressure to 410 ℃ at the heating rate of 6 ℃/min, preserving the heat for 6 hours, and finally keeping the pressure in the kettle at 4MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase temperature at 240 ℃ for 1h, distilling at normal pressure to recover unreacted tetrahydronaphthalene, and when the temperature in the reaction kettle is reduced to about 200 ℃, adding the hydrogenated asphalt C into the distillation kettle according to the mass ratio of 1: 1 pouring anthracene oil into the reactor, mixing, carrying out suction filtration under the conditions that the vacuum degree is 0.07MPa and the mesh number of a screen is 800 meshes to remove residues, pouring the mixed solution into a distillation kettle, keeping the gas phase temperature at 280 ℃ for 1H, and carrying out atmospheric distillation to recover anthracene oil to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 60 ℃, the mass content of quinoline insoluble substances is 0.02%, and the atomic ratio of H to C is 0.58: 1.
[ example 4 ]
In the embodiment, the raw material asphalt is coal-series modified asphalt with a softening point of 120 ℃, and according to the mass content of quinoline insoluble matters of 8.52%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is raised to 380 ℃ from the normal temperature at a speed of 1.5 ℃/min, and the mixture stays for 7 hours at the constant temperature to form a microcrystal unit, so that the pre-polymerized asphalt is prepared.
And (2) mixing the pre-polymerized asphalt with the coking light oil according to the mass ratio of 2: 1, fully stirring at 180 ℃, and pouring the mixture into a mixer with the length-diameter ratio of 12: 1, settling and separating in a standing and settling device, wherein the settling temperature is 150 ℃, the settling time is 2h, and the mass ratio of the materials is 6: 4 separating light phase oil and heavy phase oil, and determining the density of the light phase oil to be 0.85g/cm3The density of the heavy phase oil is 1.18g/cm3。
Pouring light-phase oil into a distillation kettle, distilling and recovering coking light oil under the conditions that the final temperature of a gas phase is 280 ℃, the gas phase stays for 1H and the vacuum degree is 0.09MPa, heating to 410 ℃ at the speed of 3 ℃/min, staying for 4H at constant temperature, and carrying out asphaltization treatment on the coking light oil to obtain rectified asphalt A, wherein the softening point of the rectified asphalt A is 70 ℃, the mass content of quinoline insoluble substances is 0.02%, and the atomic ratio of H to C is 0.48: 1.
according to the weight phase oil: the mass ratio of the coking light oil is 1: 6 mixing, heating to 120 ℃, fully stirring for 1.5h, centrifuging at the rotation speed of 1200rad/min, and separating the solid phase with the density of 1.2g/cm3And centrifuging under 600 meshes to obtain soluble component and insoluble component. Mixing insoluble components with heptane in a mass ratio of 1: 6, mixing, heating to 110 ℃, fully stirring for 2h, and carrying out pressure filtration under the vacuum degree of 0.09MPa and the mesh number of a screen of 600 meshes to obtain a filter cake and a filtrate, wherein the QI mass content in the filtrate is 0.06%. Will filterMixing the solution and the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 280 ℃ for 1H, and recovering heptane and coking light oil by vacuum distillation under the vacuum degree of 0.09MPa to obtain the rectified asphalt B, wherein the softening point of the rectified asphalt B is 70 ℃, the mass content of quinoline insoluble substances is 0.12%, and the atomic ratio of H to C is 0.46: 1.
mixing the rectified asphalt A and tetrahydronaphthalene according to the mass ratio of 1: 6, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, filling nitrogen into the reaction kettle, raising the initial pressure to 420 ℃ at the heating rate of 5 ℃/min, preserving the heat for 5 hours, and finally keeping the pressure in the reaction kettle at 6MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase at 200 ℃ for 1h, carrying out reduced pressure distillation under the vacuum degree of 0.08MPa to recover unreacted tetrahydronaphthalene, and when the temperature in the reaction kettle reaches about 200 ℃, adding the hydrogenated asphalt C into the distillation kettle according to the mass ratio of 2: 1, pouring coking light oil, mixing, carrying out suction filtration under the conditions that the vacuum degree is 0.08MPa and the mesh number of a screen is 800 meshes to remove residues, pouring the mixed solution into a distillation kettle, keeping the mixed solution at the gas phase temperature of 280 ℃ for 1H, and carrying out atmospheric distillation to recover the coking light oil to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 80 ℃, the mass content of quinoline insoluble substances is 0.03%, and the H/C atomic ratio is 0.55: 1.
[ example 5 ]
In the embodiment, the raw material asphalt is coal-series soft asphalt with a softening point of 45 ℃, and according to the mass content of quinoline insoluble matters of 2.54%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is increased to 400 ℃ from the normal temperature at a speed of 4 ℃/min, and the mixture stays for 4 hours at the constant temperature to form a microcrystal unit, so that the pre-polymerization asphalt is prepared.
And (3) mixing the pre-polymerized asphalt with the coking heavy oil according to the mass ratio of 3: 1, fully stirring at 150 ℃, and pouring the mixture with the length-diameter ratio of 8: 1, settling and separating in a standing and settling device, wherein the settling temperature is 130 ℃, the settling time is 4h, and then the mass ratio of the components is 7: 3 separating out light phase oil and heavy phase oil, and determining the density of the light phase oil to be 0.94g/cm3The density of the heavy phase oil is 1.19g/cm3。
Pouring light-phase oil into a distillation kettle, keeping the gas-phase final temperature at 330 ℃ for 1H, recovering the coking heavy oil by atmospheric distillation, heating to 400 ℃ at the speed of 2 ℃/min, keeping the temperature for 6H, and carrying out asphaltization treatment to obtain the rectified asphalt A, wherein the softening point of the rectified asphalt A is 35 ℃, the mass content of quinoline insoluble substances is 0.01%, and the atomic ratio of H to C is 0.58: 1.
the heavy phase oil and the coking heavy oil are mixed according to the mass ratio of 1: 3 mixing, heating to 150 ℃, fully stirring for 2h, centrifuging at 1500rad/min, separating the solid phase density to 1.0g/cm3And centrifuging under the mesh number of 400 meshes to obtain soluble components and insoluble components. Mixing insoluble components with pentane according to a mass ratio of 1: 3, heating to 85 ℃, fully stirring for 1.5h, and performing pressure filtration under the vacuum degree of 0.08MPa and the mesh number of a screen of 400 meshes to obtain a filter cake and a filtrate, wherein the QI mass content in the filtrate is 0.05%. Mixing the filtrate with the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 330 ℃ for 1H, distilling under normal pressure to recover pentane and coking heavy oil to obtain rectified asphalt B, wherein the softening point of the rectified asphalt B is 40 ℃, the mass content of quinoline insoluble substances is 0.06%, and the atomic ratio of H to C is 0.52: 1.
mixing the rectified asphalt A and tetrahydronaphthalene according to the mass ratio of 1: 4, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, introducing nitrogen into the high-temperature high-pressure reaction kettle, raising the initial pressure to 400 ℃ at the heating rate of 4 ℃/min, preserving the heat for 6 hours, and finally keeping the pressure in the kettle at 6MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase temperature at 260 ℃ for 0.5h, distilling at normal pressure to recover unreacted tetrahydronaphthalene, and cooling the temperature in the reaction kettle to about 200 ℃ according to a mass ratio of 3: 1, pouring coking heavy oil, mixing, carrying out suction filtration under the conditions that the vacuum degree is 0.08MPa and the mesh number of a screen is 600 meshes to remove residues, pouring the mixed solution into a distillation kettle, keeping the mixed solution at the gas phase temperature of 280 ℃ for 1H, and carrying out atmospheric distillation to recover the coking heavy oil to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 40 ℃, the mass content of quinoline insoluble substances is 0.01 percent, and the atomic ratio of H to C is 0.62: 1.
[ example 6 ]
In the embodiment, the raw material asphalt is coal-series modified asphalt with a softening point of 142 ℃, and according to the mass content of quinoline insoluble substances of 10.08%, the raw material asphalt is added into a stainless steel reaction kettle under the protection of high-purity nitrogen, the temperature is raised to 370 ℃ from the normal temperature at the speed of 2 ℃/min, and the mixture stays for 6 hours at the constant temperature, so that a microcrystal unit is formed, and the pre-polymerized asphalt is prepared.
Mixing the pre-polymerized asphalt and the naphthalene oil according to a mass ratio of 1: 1, fully stirring at 170 ℃, and pouring the mixture into a mixer with the length-diameter ratio of 14: 1 is a solution ofAnd (3) settling and separating in a settling device, wherein the settling temperature is 150 ℃, the settling time is 3h, and the mass ratio of the components is 8: 2 separating light phase oil and heavy phase oil, and determining the density of the light phase oil to be 1.09g/cm3The density of the heavy phase oil is 1.33g/cm3。
Pouring the light-phase oil into a distillation kettle, distilling under reduced pressure at the gas phase final temperature of 290 ℃ for 0.5H and the vacuum degree of 0.09MPa to recover naphthalene oil, heating to 410 ℃ at the speed of 3 ℃/min, standing for 5H at constant temperature, and carrying out asphaltization treatment to obtain the rectified asphalt A, wherein the softening point of the rectified asphalt A is 90 ℃, the mass content of quinoline insoluble substances is 0.02%, and the atomic ratio of H to C is 0.45: 1.
the heavy phase oil and the naphthalene oil are mixed according to the mass ratio of 1: 6 mixing, heating to 130 deg.C, stirring thoroughly for 2h, centrifuging at 1400rad/min, separating solid phase density of 1.1g/cm3, and centrifuging with 600 mesh sieve to obtain soluble component and insoluble component. Mixing insoluble components with tetrahydrofuran according to a mass ratio of 1: 5, mixing, heating to 110 ℃, fully stirring for 2h, and performing pressure filtration under the vacuum degree of 0.09MPa and the mesh number of a screen of 600 meshes to obtain a filter cake and a filtrate, wherein the QI content in the filtrate is 0.08%. Mixing the filtrate with the soluble components, pouring the mixture into a distillation kettle, keeping the gas phase at the final temperature of 290 ℃ for 0.5H, performing reduced pressure distillation under the vacuum degree of 0.09MPa to recover tetrahydrofuran and naphthalene oil, and obtaining the rectified asphalt B, wherein the softening point of the rectified asphalt B is 80 ℃, the mass content of quinoline insoluble substances is 0.08%, and the atomic ratio of H to C is 0.45: 1. and then mixing the rectified asphalt A and the tetrahydronaphthalene according to the mass ratio of 1: 6, mixing and adding the mixture into a high-temperature high-pressure reaction kettle, introducing nitrogen into the high-temperature high-pressure reaction kettle, raising the initial pressure to 440 ℃ at the heating rate of 6 ℃/min, preserving the heat for 4 hours, and finally keeping the pressure in the kettle at 5MPa to obtain the hydrogenated asphalt C. Pouring the hydrogenated asphalt C into a distillation kettle, keeping the gas phase at 210 ℃ for 1h, carrying out reduced pressure distillation under the vacuum degree of 0.09MPa to recover unreacted tetrahydronaphthalene, and cooling the reaction kettle to 200 ℃ or so according to the mass ratio of 1: pouring naphthalene oil into the reactor 1, mixing, carrying out suction filtration under the conditions that the vacuum degree is 0.09MPa and the mesh number of a screen is 800 meshes to remove residues, pouring the mixed solution into a distillation kettle, keeping the gas phase temperature at 280 ℃ for 1H, and carrying out atmospheric distillation to recover the naphthalene oil to obtain refined hydrogenated asphalt D, wherein the softening point of the refined hydrogenated asphalt D is 70 ℃, the mass content of quinoline insoluble substances is 0.025%, and the H/C atomic ratio is 0.56: 1.
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (19)
1. A preparation method of special high-performance asphalt for carbon materials is characterized in that the special high-performance asphalt for carbon materials comprises rectified asphalt B and refined hydrogenated asphalt D; the preparation process comprises the following steps:
firstly, under inert atmosphere, according to the activation energy of high-reactivity components contained in raw material asphalt, carrying out primary thermal polycondensation on the raw material asphalt by controlling the thermal reaction temperature to form a microcrystal unit, wherein the prepared intermediate is called pre-polymerized asphalt; the high-reactivity components are heavy components which are insoluble in quinoline in the raw material asphalt and inorganic impurity solid particles;
step two, mixing the pre-polymerized asphalt obtained in the step one with a solvent I according to a set agent oil ratio, fully stirring, standing, settling and separating to obtain light phase oil and heavy phase oil according to a set separation ratio; the solvent-oil ratio of the pre-polymerized asphalt to the solvent I is (0.5-5): 1; the set separation ratio is light phase oil according to the mass ratio: heavy phase oil = (5-9.5): (5-0.5);
step three, distilling the light phase oil obtained in the step two to recover a solvent I, and then performing asphaltization treatment under the protection of inert gas to obtain rectified asphalt A; the rectified asphalt A is micromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-1800 and the centralized molecular weight of 600-1200, the softening point is 35-95 ℃, the mass content of quinoline insoluble substances is 0-0.05%, and the atomic ratio of H to C is (0.45-0.6): 1;
step four, the heavy phase oil obtained in the step two is returned to the solvent I with a certain proportion, and a soluble component and an insoluble component are obtained after thermal separation treatment; the heavy phase oil and the first solvent which is recycled are heavy phase oil according to the mass ratio: solvent i = 1: (0.2-10); mixing the insoluble component with a solvent II according to a set solvent-oil ratio, and performing filter pressing treatment to obtain a filter cake and a filtrate, wherein the filter cake is inorganic impurities and other insoluble solid particles; the solvent-oil ratio of the insoluble component to the solvent II is 1: (0.5 to 10); mixing the filtrate with soluble components, and distilling to recover solvent I and solvent II to obtain rectified asphalt B; the rectified asphalt B is macromolecular polycyclic aromatic hydrocarbon with the molecular weight of 400-2000 and the concentrated molecular polycyclic aromatic hydrocarbon of 800-1400, the softening point is 30-80 ℃, the mass content of quinoline insoluble substances is 0-0.2%, and the atomic ratio of H to C is (0.45-0.55): 1;
step five, mixing the rectified asphalt A obtained in the step three with a hydrogen supply reagent according to a set proportion, and performing high-temperature and high-pressure heat treatment to obtain hydrogenated asphalt C; the mixing proportion of the rectified asphalt A to the hydrogen donor reagent is 1: (1-8); distilling the hydrogenated asphalt C to recover an unreacted hydrogen donor reagent, mixing the hydrogen donor reagent with the solvent I according to a set solvent-oil ratio, removing residues through hot filtration, and distilling to recover the solvent I to obtain refined hydrogenated asphalt D; the solvent-oil ratio of the hydrogenated asphalt C to the solvent I is (0.5-5): 1; the refined hydrogenated asphalt D has a softening point of 30-80 ℃, a quinoline insoluble matter content of 0-0.05%, and an H/C atomic ratio of (0.55-0.75): 1.
2. the method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the first step, the raw material asphalt is coal asphalt obtained by high-temperature dry distillation of coal, the softening point is 20-150 ℃, and the mass content of quinoline insoluble substances is 1-20%.
3. The method for preparing the special high-performance asphalt for carbon materials according to claim 1, wherein in the first step, the inert atmosphere is a high-purity nitrogen atmosphere or a high-purity argon atmosphere.
4. The method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the first step, the temperature of the preliminary thermal polycondensation is 350-400 ℃, the constant temperature time is 0.5-8 h, and the temperature rise rate is 0.5-5 ℃/min.
5. The method for preparing the special high-performance asphalt for carbon materials according to claim 1, wherein in the step one, the density of the pre-polymerized asphalt is 1.1-1.6 g/cm3The size of the microcrystal unit is controlled to be 2-15 μm.
6. The method for preparing the high-performance asphalt special for carbon materials according to claim 1, wherein in the second step, the first solvent is any one or a mixture of more than two of 200-350 ℃ fractions, coal directly liquefied light oil, wash oil, mono-anthracene oil, di-anthracene oil, coking heavy oil, coking light oil, naphthalene oil, kerosene, petroleum ether, gasoline, diesel oil, lubricating oil and paraffin oil in the separation process of coal tar.
7. The preparation method of the special high-performance asphalt for carbon materials according to claim 1, wherein in the second step, the standing, settling and separating are performed in a way that the length-diameter ratio is (1-20): 1, the settling temperature is 80-200 ℃, and the settling time is 0.5-5 h.
8. The method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the second step, the density of the light-phase oil is 0.85-1.1 g/cm3The density of the heavy phase oil is 1.0-1.35 g/cm3。
9. The method for preparing the high-performance asphalt specially used for carbon materials according to claim 1, wherein in the third step, the distillation comprises atmospheric distillation and vacuum distillation; wherein, the atmospheric distillation conditions are as follows: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
10. The method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the third step, the temperature of the asphalting treatment is 330-420 ℃, the heating rate is 0.5-5 ℃/min, and the final temperature retention time is 0.5-10 h.
11. The method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the fourth step, the thermal separation treatment adopts centrifugal separation, and the treatment conditions are as follows: the separation temperature is 60-150 ℃, the separation time is 0.5-3 h, the centrifugal rotation speed is 800-2000 rad/min, and the separation solid phase density is 0.9-1.3 g/cm3The mesh number of the screen is 300-1200 meshes.
12. The method for preparing the special high-performance asphalt for carbon materials according to claim 1, wherein in the fourth step, the solvent II is any one or a mixture of more than two of toluene, xylene, pyridine, heptane, pentane and tetrahydrofuran.
13. The method for preparing the high-performance asphalt special for carbon materials according to claim 1, wherein in the fourth step, the conditions of the pressure filtration treatment are as follows: the filter pressing temperature is 80-150 ℃, the filter pressing time is 0.5-3 h, and the mesh number of the screen is 300-1200 meshes.
14. The method for preparing the high-performance asphalt special for carbon materials according to claim 1, wherein in the fourth step, the mass content of quinoline insoluble substances in the filtrate is less than 0.1%.
15. The method for preparing the high-performance asphalt specially used for carbon materials according to claim 1, wherein in the fourth step, the distillation comprises atmospheric distillation or vacuum distillation; the atmospheric distillation conditions were: the gas phase temperature is 280-350 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 200-300 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
16. The method for preparing the special high-performance asphalt for carbon materials according to claim 1, wherein in the fifth step, the hydrogen donor is any one or a mixture of more than two of tetrahydronaphthalene, octahydronaphthalene, tetrahydroquinoline and decahydroquinoline.
17. The method for preparing the special high-performance asphalt for carbon materials according to claim 1, wherein in the fifth step, the hydrogenation conditions of the high-temperature high-pressure heat treatment are as follows: and filling nitrogen into the reaction kettle, wherein the initial pressure is 0.5-3 MPa, the heating rate is 1-10 ℃/min, the final temperature is 380-440 ℃, the heat preservation time is 1-6 h, and the final pressure in the kettle is 4-6 MPa.
18. The method for preparing the high-performance asphalt specially used for carbon materials according to claim 1, wherein in the fifth step, the distillation comprises atmospheric distillation or vacuum distillation; the atmospheric distillation conditions were: the gas phase temperature is 210-300 ℃, and the final temperature retention time is 0.5-2 h; the reduced pressure distillation conditions were: the gas phase temperature is 150-240 ℃, the vacuum degree is 0.01-0.09 MPa, and the final temperature retention time is 0.5-2 h.
19. The method for preparing the high-performance asphalt special for the carbon material according to claim 1, wherein in the fifth step, the hot filtration is performed in a suction filtration mode under the conditions that: the filtering temperature is 100-250 ℃, the vacuum degree is 0.01-0.09 MPa, and the mesh number of the screen is 300-1200 meshes.
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