CN111363577A - Spinnable asphalt for coal-based general-grade asphalt carbon fibers and preparation method thereof - Google Patents
Spinnable asphalt for coal-based general-grade asphalt carbon fibers and preparation method thereof Download PDFInfo
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- CN111363577A CN111363577A CN202010171531.2A CN202010171531A CN111363577A CN 111363577 A CN111363577 A CN 111363577A CN 202010171531 A CN202010171531 A CN 202010171531A CN 111363577 A CN111363577 A CN 111363577A
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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
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
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- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Working-Up Tar And Pitch (AREA)
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Abstract
The invention discloses spinnable asphalt for coal-based general-grade asphalt carbon fibers and a preparation method thereof, belonging to the field of coal chemical industry. The spinnable asphalt for the coal-based general-grade asphalt carbon fiber provided by the invention has the softening point of 224-237 ℃ and the quinoline insoluble content of 10-15%. The preparation method comprises (1) mixing high temperature coal tar pitch with solvent, and discharging insoluble solvent after dissolving; (2) recovering the solvent from the solvent soluble matter and the solvent at 250-300 deg.c, settling and discharging the settled components; (3) vacuum distilling the settled asphalt, and discharging light components; (4) and (3) performing air purging thermal polycondensation on the material subjected to reduced pressure distillation to obtain the spinnable asphalt. The invention has the advantages that: (1) the process equipment is less, no catalyst is needed, and the industrial production can be realized; (2) the raw materials are low in price and low in cost; (3) no waste liquid is discharged, and the environment is protected.
Description
Technical Field
The invention relates to the field of coal chemical industry, in particular to spinnable asphalt for coal-based general-grade asphalt carbon fibers and a preparation method thereof.
Background
The raw material for preparing coal-based general-grade asphalt carbon fibers is spinnable asphalt which is a main product in a coal coking process and is a complex organic mixture. Has high aromaticity and carbon content, and is easy to polymerize or crosslink. Is an important raw material for preparing active carbon for capacitors, graphite cathodes, high-temperature binders and pitch carbon fibers. The pitch carbon fiber is an indispensable material for advanced technologies of aerospace, aviation, war industry and the like, and is also a high-end basic raw material of a plurality of important civil industries.
CN201910737735.5, CN201910737734.0 and CN201811160012.5 respectively disclose methods for preparing general-grade pitch carbon fiber spinnable pitch by modifying medium and low temperature coal pitch with pyromellitic dianhydride and polystyrene, pyromellitic dianhydride, maleic anhydride and petrolatum as modifiers;
CN201811158411.8, CN103014919A, CN101135074A and CN105219414A respectively disclose methods for preparing spinnable asphalt and general-grade asphalt carbon fibers from coal tar, coal tar maltha and ethylene tar, and the methods have complex extraction processes and various solvent varieties.
CN201810866701.1, CN201810622405.7 and CN102733008A disclose methods for preparing mesophase spinnable pitch using coal pitch, coal liquefaction residue and coal tar as raw materials, respectively.
CN201610574118.4 and CN102477595A respectively disclose spinnable asphalt prepared from coal liquefaction residues, a preparation method thereof and carbon fibers, wherein solvents used comprise highly toxic solvents such as toluene, quinoline, tetrahydroquinoline and the like.
CN201511008731.1 discloses a method for preparing petroleum-based isotropic carbon fiber spinnable pitch, which comprises purifying ethylene cracking tar, flashing at 280-320 ℃ under normal pressure, then carrying out reduced pressure flash evaporation, and proportionally mixing the material subjected to reduced pressure flash evaporation with coumarone or other raw materials to produce medium-temperature pitch for polycondensation reaction.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a spinnable asphalt for coal-based general-grade asphalt carbon fibers, a preparation method and application thereof by taking high-temperature coal tar pitch as a raw material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the spinnable asphalt for the coal-based general-grade asphalt carbon fibers has the softening point of 224-237 ℃, quinoline insoluble substances of 10-15 percent, the single-hole melt spinning length of more than or equal to 8km and the diameter mean square error non-uniformity rate CVd of less than 10 percent.
A preparation method of spinnable asphalt for coal-based general-grade asphalt carbon fibers comprises the following steps:
(1) mixing high-temperature coal tar pitch and a solvent in proportion, placing the mixture in a reactor, stirring the mixture at normal temperature, standing the mixture, and discharging insoluble substances of the solvent; then heating and recovering the solvent to obtain refined asphalt;
(2) settling the refined asphalt, and separating out heavy components;
(3) stirring the residual refined asphalt in the step (2), and carrying out reduced pressure distillation to discharge light components;
(4) heating the material after reduced pressure distillation to a reaction temperature, and introducing normal pressure air for reaction;
(5) and filtering the reacted asphalt by a filter plate to obtain the spinnable asphalt for the universal-grade asphalt carbon fiber.
The method accurately separates the high-temperature coal tar pitch, selects proper components to prepare the spinnable pitch, is easy to realize the operation of each step in the preparation method, is easy to control the reaction process, and has the advantages of uniform composition of the prepared product, good spinning performance and excellent uniformity of the pitch fiber structure.
Further, the weight ratio of the high-temperature coal tar pitch to the solvent in the step (1) is 1:4-10, so that effective components in the high-temperature coal tar pitch are extracted as much as possible, and the yield of the high-temperature coal tar pitch is improved; wherein the solvent is tetrahydrofuran, and the softening point of the high-temperature coal tar pitch is 95-120 ℃.
Further, the stirring time in the step (1) is 20min to ensure that the effective components are fully dissolved, and the standing time is 10min to ensure that the insoluble substances in the solvent are completely settled; the temperature rise is 250-300 ℃, not only can the solvent be completely recovered, but also the temperature can be raised to the sedimentation temperature in one step, the operation process is simplified, and the energy loss is reduced; the height-diameter ratio of the reactor is 1-5:1, so that the settling separation of heavy components is facilitated.
Furthermore, the temperature of the sedimentation in the step (2) is 250-300 ℃, the sedimentation time is 30-40 hours, and the full sedimentation of heavy components in the refined asphalt under low viscosity is realized while the sedimentation time is shortened; the weight of the separated heavy components accounts for 10-20% of the weight of the refined asphalt.
Further, in the step (3), the temperature is kept between 250 ℃ and 300 ℃ during stirring; the vacuum degree of the reduced pressure distillation is 10-50Kpa, and the distillation time is 1-2 hours. The light components which are not beneficial to the reaction are removed in the lowest possible vacuum degree and short distillation time, and the energy consumption is reduced.
Furthermore, the reaction temperature in the step (4) is 350-420 ℃, and the coking reaction can be reduced at the reaction temperature; the flow of the introduced air is 200-800L/min-t, which not only can provide oxygen required by the reaction, but also entrains low molecular compounds generated by the reaction out of the reaction system, thereby improving the softening point of the spinnable asphalt; the reaction time is 3-5 hours, and the refined asphalt can be completely converted into spinnable asphalt with high softening point.
Further, in the step (5), the pore diameter of a stainless steel filter plate used for the pitch after the reaction is 2.6-13 μm, so as to remove large particle components (secondary quinoline insoluble substances) generated after the reaction as much as possible and reduce the size of colloidal particles in the spinnable pitch.
The spinnability of the spinnable asphalt is evaluated by adopting the evaluation standard of a single-hole melt spinning method, which comprises the following steps:
the feeding amount of each time is 5-30g of spinnable asphalt, the spinning temperature is 71-75 ℃ higher than the softening point temperature, the spinning pressure is 0.8-1.2MPa, the diameter of a spinning nozzle is 0.3mm, and the winding speed is 300 m/min. The length of the single-hole melt spinning of the spinnable asphalt is more than or equal to 8 km.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the invention does not use catalyst and is easy for industrialized production;
(2) the raw materials adopted by the invention are low in price and low in cost;
(3) the preparation process of the invention has no waste liquid discharge, and is environment-friendly;
(4) the spinnable asphalt provided by the invention has the characteristics of high softening point (224-237 ℃) and good spinnability (the length of single-hole melt spinning is more than or equal to 8 km).
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1:
the spinnable asphalt for the coal-based general-grade asphalt carbon fibers is characterized in that the spinnable asphalt has a softening point of 224 ℃, quinoline insoluble substances of 10 percent and a single-hole melt spinning length of 12 km.
The method for preparing the spinnable asphalt for the coal-based general-grade asphalt carbon fiber comprises the following steps:
(1) mixing 1 ton of high-temperature coal tar pitch with a softening point of 95 ℃ and tetrahydrofuran in a ratio of 1:4, placing the mixture in a reactor (the height-diameter ratio of the reactor is 1:1), stirring the mixture at normal temperature at a rotating speed of 100rmp for 20min, standing the mixture for 10min, and discharging 0.1 ton of insoluble solvent from a discharge outlet; then setting the temperature to 260 ℃, starting heating, and recovering the solvent to obtain refined asphalt;
(2) after the temperature of the reactor rises to 260 ℃, stopping stirring and settling for 30 hours; discharging 0.09 ton of heavy component from a discharge hole at the lower end;
(3) opening stirring, wherein the stirring speed is 200r/min, and carrying out reduced pressure distillation on the residual asphalt in the step (2) for 1 hour at the temperature of 260 ℃ and the vacuum degree of 50 KPa;
(4) heating the material subjected to reduced pressure distillation in the step (3) to 350 ℃, and introducing air to perform thermal polycondensation for 3 hours, wherein the gas flow is 200L/min.t;
(5) filtering the material subjected to thermal polycondensation in the step (4) by using a stainless steel filter screen with the diameter of 2.6 mu m to obtain 0.45 ton of spinnable asphalt, wherein the softening point is 224 ℃, and the quinoline insoluble substance is 10 percent;
(6) spinning the spinnable asphalt obtained in the step (5) at 295 ℃, 1.0MPa and a filament winding speed of 300m/min to obtain asphalt fiber precursor with the length of 12km and the diameter of 18 mu m;
(7) stabilizing the pitch fiber precursor in air, heating the pitch fiber precursor from room temperature to 215 ℃ at the speed of 5 ℃/min, then heating the pitch fiber precursor to 290 ℃ at the speed of 1 ℃/min, keeping the temperature for 1 hour, and then continuing heating the pitch fiber precursor to 320 ℃ at the speed of 1 ℃/min, keeping the temperature for 2 hours; the mass flow of air relative to each gram of asphalt fiber is 0.1L/min g;
(8) and (4) carbonizing the stabilized asphalt fiber obtained in the step (7) under the protection of nitrogen, wherein the carbonization temperature is 900-1000 ℃, the temperature rise speed is 20 ℃/min, the carbonization time is 10 minutes, the tensile strength of the obtained asphalt carbon fiber is 748MPa, and the tensile modulus is 51 GPa.
Example 2:
the spinnable asphalt for the coal-based general-grade asphalt carbon fibers is characterized in that the spinnable asphalt has a softening point of 230 ℃, quinoline insoluble substances of 12 percent and a single-hole melt spinning length of 10 km.
The method for preparing the spinnable asphalt for the coal-based general-grade asphalt carbon fiber comprises the following steps:
(1) mixing 1 ton of high-temperature coal tar pitch with a softening point of 120 ℃ and tetrahydrofuran in a ratio of 1:10, placing the mixture in a reactor (the height-diameter ratio of the reactor is 3:1), stirring the mixture at normal temperature at a rotating speed of 100rmp for 20min, standing the mixture for 10min, and discharging 0.12 ton of insoluble solvent from a discharge outlet; then setting the temperature to 290 ℃, starting heating, and recovering the solvent to obtain refined asphalt;
(2) after the temperature of the reactor is raised to 290 ℃, stopping stirring and settling for 40 hours; discharging 0.13 ton of heavy component from a discharge hole at the lower end;
(3) opening stirring, wherein the stirring speed is 200r/min, and carrying out reduced pressure distillation on the residual asphalt in the step (2) for 1 hour at the temperature of 280 ℃ and the vacuum degree of 30 KPa;
(4) heating the material obtained after the reduced pressure distillation in the step (3) to 380 ℃, and introducing air to carry out thermal polycondensation for 5 hours, wherein the gas flow is 500L/min.t;
(5) filtering the material subjected to thermal polycondensation in the step (4) by a stainless steel filter screen with the diameter of 13 mu m to obtain 0.43 ton of spinnable asphalt, wherein the softening point is 230 ℃, and the quinoline insoluble substance is 12%;
(6) spinning the spinnable asphalt obtained in the step (5) at 305 ℃, 0.8MPa and a filament-receiving speed of 300m/min to obtain asphalt fiber precursor with the length of 10km and the diameter of 15 mu m;
(7) stabilizing the pitch fiber precursor in air, heating the pitch fiber precursor from room temperature to 220 ℃ at a speed of 5 ℃/min, then heating the pitch fiber precursor to 300 ℃ at a speed of 1 ℃/min, keeping the temperature for 2 hours, and then continuing heating the pitch fiber precursor to 320 ℃ at a speed of 1 ℃/min, keeping the temperature for 1 hour; the mass flow of air relative to each gram of asphalt fiber is 0.1L/min g;
(8) and (4) carbonizing the stabilized asphalt fiber obtained in the step (7) under the protection of nitrogen, wherein the carbonization temperature is 900-1000 ℃, the temperature rise speed is 20 ℃/min, the carbonization time is 10 minutes, the tensile strength of the obtained asphalt carbon fiber is 851MPa, and the tensile modulus is 60 GPa.
Example 3:
the spinnable asphalt for the coal-based general-grade asphalt carbon fibers is characterized in that the spinnable asphalt has a softening point of 234 ℃, quinoline insoluble substances of 14% and a single-hole melt spinning length of 9 km.
The method for preparing the spinnable asphalt for the coal-based general-grade asphalt carbon fiber comprises the following steps:
(1) mixing 1 ton of high-temperature coal tar pitch with a softening point of 105 ℃ and tetrahydrofuran in a ratio of 1:6, placing the mixture in a reactor (the height-diameter ratio of the reactor is 4:1), stirring the mixture at normal temperature at a rotating speed of 100rmp for 20min, standing the mixture for 10min, and discharging 0.11 ton of insoluble solvent from a discharge outlet; then setting the temperature to 300 ℃, starting heating, and recovering the solvent to obtain refined asphalt;
(2) after the temperature of the reactor is raised to 300 ℃, stopping stirring and settling for 35 hours; discharging 0.18 ton of heavy component from a discharge hole at the lower end;
(3) opening stirring, wherein the stirring speed is 200r/min, and carrying out reduced pressure distillation on the residual asphalt in the step (2) for 1.5 hours at the temperature of 300 ℃ and the vacuum degree of 20 KPa;
(4) heating the material subjected to reduced pressure distillation in the step (3) to 400 ℃, and introducing air to perform thermal polycondensation for 4 hours, wherein the gas flow is 800L/min.t;
(5) filtering the material subjected to thermal polycondensation in the step (4) by a stainless steel filter screen with the diameter of 6.5 mu m to obtain 0.42 ton of spinnable asphalt, wherein the softening point is 234 ℃, and the quinoline insoluble substance is 14 percent;
(6) spinning the spinnable asphalt obtained in the step (5) at 306 ℃, 1.2MPa and a filament-receiving speed of 300m/min to obtain asphalt fiber precursor filaments with the length of 9km and the diameter of 16 mu m;
(7) stabilizing the pitch fiber precursor in air, heating the pitch fiber precursor from room temperature to 225 ℃ at a speed of 5 ℃/min, then heating the pitch fiber precursor to 300 ℃ at a speed of 1 ℃/min, keeping the temperature for 3 hours, and then continuing heating the pitch fiber precursor to 330 ℃ at a speed of 1 ℃/min, keeping the temperature for 1 hour; the mass flow of air relative to each gram of asphalt fiber is 0.1L/min g;
(8) and (4) carbonizing the stabilized asphalt fiber obtained in the step (7) under the protection of nitrogen, wherein the carbonization temperature is 900-1000 ℃, the temperature rising speed is 20 ℃/min, the carbonization time is 10 minutes, the tensile strength of the obtained asphalt carbon fiber is 952MPa, and the tensile modulus is 78 GPa.
Example 4:
the spinnable asphalt for the coal-based general-grade asphalt carbon fibers is characterized in that the spinnable asphalt has a softening point of 237 ℃, quinoline insoluble substances of 15% and a single-hole melt spinning length of 8 km.
The method for preparing the spinnable asphalt for the coal-based general-grade asphalt carbon fiber comprises the following steps:
(1) mixing 1 ton of high-temperature coal tar pitch with a softening point of 110 ℃ and tetrahydrofuran in a ratio of 1:8, placing the mixture in a reactor (the height-diameter ratio of the reactor is 5:1), stirring the mixture for 20min at normal temperature at a rotating speed of 100rmp, standing the mixture for 10min, and discharging 0.11 ton of insoluble solvent from a discharge outlet; then setting the temperature to be 250 ℃, starting to heat up, and recovering the solvent to obtain refined asphalt;
(2) after the temperature of the reactor is raised to 250 ℃, stopping stirring and settling for 38 hours; discharging 0.16 ton of heavy component from a discharge hole at the lower end;
(3) opening stirring, wherein the stirring speed is 200r/min, and carrying out reduced pressure distillation on the residual asphalt in the step (2) for 1.7 hours at 250 ℃ and the vacuum degree of 10 KPa;
(4) heating the material obtained after the reduced pressure distillation in the step (3) to 420 ℃, and introducing air to carry out thermal polycondensation for 4 hours, wherein the gas flow is 400L/min.t;
(5) filtering the material subjected to thermal polycondensation in the step (4) by a stainless steel filter screen with the diameter of 10 mu m to obtain 0.43 ton of spinnable asphalt, wherein the softening point is 237 ℃, and the quinoline insoluble substance is 15%;
(6) spinning the spinnable asphalt obtained in the step (5) at the temperature of 310 ℃, the pressure of 1.0MPa and the filament collecting speed of 300m/min to obtain asphalt fiber precursor with the length of 8km and the diameter of 16 mu m;
(7) stabilizing the pitch fiber precursor in air, heating the pitch fiber precursor from room temperature to 225 ℃ at a speed of 5 ℃/min, then heating the pitch fiber precursor to 280 ℃ at a speed of 1 ℃/min, keeping the temperature for 1 hour, then heating the pitch fiber precursor to 300 ℃, and keeping the temperature for 2 hours; finally, the temperature is raised to 330 ℃, the temperature is kept for 1 hour, and the mass flow of air relative to each gram of asphalt fiber is 0.1L/min g;
(8) and (4) carbonizing the stabilized asphalt fiber obtained in the step (7) under the protection of nitrogen, wherein the carbonization temperature is 900-1000 ℃, the temperature rise speed is 20 ℃/min, the carbonization time is 10 minutes, the tensile strength of the obtained asphalt carbon fiber is 921MPa, and the tensile modulus is 65 GPa.
Claims (8)
1. The spinnable asphalt for the coal-based general-grade asphalt carbon fiber is characterized by comprising the following components in parts by weight: the softening point of the spinnable asphalt is 224-237 ℃, the quinoline insoluble substance is 10-15%, and the length of the single-hole melt spinning is more than or equal to 8 km.
2. A method for preparing the spinnable pitch for coal-based general-grade pitch carbon fiber according to claim 1, which comprises the following steps: the method comprises the following steps:
(1) mixing high-temperature coal tar pitch and a solvent in proportion, placing the mixture in a reactor, stirring the mixture at normal temperature, standing the mixture, and discharging insoluble substances of the solvent; then heating and recovering the solvent to obtain refined asphalt;
(2) settling the refined asphalt, and separating out heavy components;
(3) stirring the residual refined asphalt in the step (2), and carrying out reduced pressure distillation to discharge light components;
(4) heating the material after reduced pressure distillation to a reaction temperature, and introducing normal pressure air for reaction;
(5) and filtering the reacted asphalt by a filter plate to obtain the spinnable asphalt for the universal-grade asphalt carbon fiber.
3. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: the weight ratio of the high-temperature coal tar pitch to the solvent in the step (1) is 1:4-10, wherein the solvent is tetrahydrofuran, and the softening point of the high-temperature coal tar pitch is 95-120 ℃.
4. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: the stirring time in the step (1) is 20min, and the standing time is 10 min; the temperature rise is 250-300 ℃; the ratio of height to diameter of the reactor used is 1-5: 1.
5. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: the temperature of the sedimentation in the step (2) is 250-300 ℃, and the sedimentation time is 30-40 hours; the weight of the separated heavy components accounts for 10-20% of the weight of the refined asphalt.
6. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: in the step (3), the temperature is kept between 250 and 300 ℃ during stirring; the vacuum degree of the reduced pressure distillation is 10-50Kpa, and the distillation time is 1-2 hours.
7. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: the reaction temperature in the step (4) is 350-420 ℃, the flow rate of the introduced air is 200-800L/min-t, and the reaction time is 3-5 hours.
8. The method for preparing the spinnable pitch for coal-based universal-grade pitch carbon fibers according to claim 2, wherein the method comprises the following steps: the aperture of the filter plate used for filtering the reacted asphalt in the step (5) is 2.6-13 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149819A (en) * | 2021-12-01 | 2022-03-08 | 中国矿业大学(北京) | Method for increasing softening point temperature of asphalt and asphalt obtained by method |
| CN114540065A (en) * | 2022-02-18 | 2022-05-27 | 山东大学 | Method for extracting asphalt soluble substance by adopting o-xylene and water |
| CN115434038A (en) * | 2022-10-12 | 2022-12-06 | 中国矿业大学(北京) | High-softening-point asphalt-based microporous activated carbon fiber and preparation method thereof |
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