CN108486689B - Preparation method of high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filament - Google Patents
Preparation method of high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filament Download PDFInfo
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- CN108486689B CN108486689B CN201810189047.5A CN201810189047A CN108486689B CN 108486689 B CN108486689 B CN 108486689B CN 201810189047 A CN201810189047 A CN 201810189047A CN 108486689 B CN108486689 B CN 108486689B
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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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- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/14—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with organic compounds, e.g. macromolecular compounds
-
- 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
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
Abstract
The invention discloses a preparation method of a high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament, which comprises the steps of firstly, unwinding a primary-spun asphalt fiber continuous filament bundle to an oxidation carbonization mesh belt furnace through a filament returning mechanism for continuous oxidation carbonization treatment, realizing regulation and control of a molecular structure of the primary-spun asphalt fiber continuous filament bundle by regulating oxygen concentrations of different temperature areas in an oxidation process, and rewinding after the fiber obtains certain strength; and then, the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament product is prepared through the processes of uncoiling, high-temperature carbonization, graphitization, sizing, drying, rolling and the like, wherein the tensile modulus is 900-950 GPa, the heat conductivity is 900-1100W/m.K, the tensile strength is 2-3.5 GPa, and the continuous length can reach more than 20000 m. On the premise of realizing the continuous preparation of the asphalt fibers, the modulus and the heat conductivity of the asphalt fibers are greatly improved by adjusting the pre-oxidation process, the production efficiency is high, and the industrial production is easy to realize.
Description
Technical Field
The invention belongs to the technical field of high-performance asphalt-based carbon fiber preparation processes, and particularly relates to a method for preparing high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filaments.
Background
The high-modulus and high-heat-conductivity asphalt-based carbon fiber has the advantages of incomparable high modulus and high heat conductivity of Polyacrylonitrile (PAN) -based carbon fiber, is called as 'pearl on crown' in the field of carbon fiber, is used as a structural material for bearing load while realizing light weight on aerospace equipment, top-end industrial equipment, electronic products and the like, is used as a functional material for heat prevention and heat conduction, has no replaceability, and is a high-end carbon fiber variety with great development prospect.
The preparation process of the high-modulus high-thermal-conductivity asphalt-based carbon fiber has long technological process, generally comprises the processes of modulation of high-purity spinnable mesophase asphalt, melt spinning, pre-oxidation, carbonization, graphitization, surface treatment, washing, drying, sizing, drying, rolling and the like, and the continuous preparation difficulty is particularly high due to low strength and high brittleness of the primary spun asphalt fiber, so that the industrial preparation of the high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filament is still blank in China at present.
The Chinese invention patent (CN105088420A) directly uncoils an asphalt fiber protofilament, enters a roller type pre-oxidation furnace at the speed of 0.1m/min under the drive of a roller to perform continuous pre-oxidation treatment for 50-60 min, and then performs continuous carbonization and graphitization treatment to obtain an asphalt-based carbon fiber sample with the tensile strength of 2521MPa, the tensile modulus of 508GPa and the thermal conductivity of 603W/mK. Because the asphalt fiber has low strength and large brittleness, the continuous pre-oxidation is directly carried out under the traction of a roller, the yarn breaking and fluffing of the asphalt fiber are easily caused, and the operation difficulty is large; in addition, the whole wire adopts the wire moving speed of 0.1m/min, so that the production efficiency is extremely low, and the industrial production is difficult to realize.
The united states invention patent (USP4351816) pre-oxidizes the continuous filament bundle of the as-spun pitch fiber together with a roller, and although the problem of drafting, uncoiling and pre-oxidation of the pitch fiber precursor is avoided, the winding and oxidation of the pitch fiber are easy to cause uneven internal and external oxidation, and the preparation of high-performance pitch-based carbon fiber continuous filament samples with the performance of kilometers or even kilometers in the typical long axis direction is difficult. The Chinese invention patent (CN103046165A) integrally soaks the as-spun asphalt fiber bundle and the winding drum in a liquid phase solution for preliminary non-melting, then washes the fiber bundle with deionized water, then partially soaks the fiber bundle in high temperature resistant silicon oil for low speed filament rewinding, then enters a continuous pre-oxidation furnace for continuous pre-oxidation, and then carries out low temperature carbonization, high temperature carbonization and graphitization. The process route has the disadvantages of complicated pre-oxidation process, more factors influencing the quality consistency, low production efficiency and difficult realization of continuous and industrial preparation.
Therefore, aiming at the existing preparation method of the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament, no method which is particularly suitable for industrial production is found, and the development of the preparation technology of the high-performance asphalt-based carbon fiber continuous filament in China is seriously hindered.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filament aiming at the defects in the prior art. The method is mainly characterized in that the continuous filament bundle of the primary spinning asphalt fiber is directly unwound to an oxidation carbonization mesh belt furnace for continuous oxidation and carbonization treatment, and the fiber is wound after obtaining certain strength, so that the problems of easy breakage and fluffing of the primary spinning asphalt fiber due to direct drafting preoxidation are avoided; meanwhile, the concentration of oxygen in different chambers in the pre-oxidation furnace is changed, so that the asphalt fiber obtains sufficient stress relaxation, the regulation and control of the molecular structure of the asphalt fiber are completed, and further, a high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament sample with a thick graphite sheet structure and good orientation is obtained. The process is simple and controllable, the production efficiency is high, the industrial production is easy to realize, and the modulus and the heat conductivity of the prepared asphalt-based carbon fiber are high.
In order to solve the technical problems, the invention adopts the technical scheme that:
step (1): carrying out melt spinning on an asphalt raw material with the mesophase content of 100%, the ash content of less than 40ppm, the S content of less than 1000ppm, the N content of less than 1000ppm and the softening point of 250-270 ℃ to obtain an asphalt fiber continuous filament bundle with the continuous length of more than 20000 m;
step (2): unwinding the continuous asphalt fiber filament bundle to an oxidation carbonization mesh belt furnace through a filament returning mechanism, firstly carrying out heat treatment for 5-10 min at the temperature of 180-200 ℃ under the condition of nitrogen atmosphere, carrying out continuous dehydration, deoiling agent and devolatilization treatment, and simultaneously enabling the continuous asphalt fiber filament bundle to obtain stress relaxation; carrying out continuous oxidation treatment at the temperature of 200-260 ℃ in the air condition for 60-90 min; then carrying out continuous oxidation treatment at the temperature of 260-290 ℃ under the condition of mixing air and nitrogen for 30-60 min, and controlling the oxidation weight gain within the range of 4-6%, wherein the concentration of oxygen in the mixed gas of air and nitrogen is 5-15%; finally, carrying out continuous carbonization treatment at the temperature of 350-900 ℃ under the protection of high-purity nitrogen for 10-15 min to obtain a low-temperature carbonized fiber continuous filament bundle with the tensile strength of 1.0-1.5 GPa, and then winding again;
and (3): uncoiling a low-temperature carbonized fiber continuous filament bundle, and then carrying out high-temperature carbonization treatment at the temperature of 1000-1400 ℃ under the protection of high-purity nitrogen for 1-2 min under the tension of 600cN to obtain a high-temperature carbonized fiber continuous filament bundle;
and (4): carrying out continuous ultrahigh-temperature graphitization treatment on the high-temperature carbonized fiber continuous filament bundle at the temperature of 2600-2800 ℃ under the protection of high-purity argon for 1-2 min, wherein the tension is 200cN, and thus obtaining a graphitized fiber continuous filament bundle;
and (5): carrying out surface sizing treatment on the graphitized fiber continuous filament bundle, wherein the sizing liquid is water-based epoxy resin, the solid content is 2-2.5%, and the sizing time is 10-30 s;
and (6): and drying the sized continuous graphite fiber bundle by a hot air circulation drying furnace at the drying temperature of 110-120 ℃ for 3-5 min, and then winding and rolling to obtain the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament finished product, wherein the tensile modulus is 900-950 GPa, the heat conductivity is 900-1100W/m.K, the tensile strength is 2-3.5 GPa, and the continuous length is more than 20000 m.
The spinning asphalt is coal-based mesophase asphalt or oil-based mesophase asphalt.
The aperture of the micropores of the spinneret plate used in the asphalt melt spinning is 0.2mm, the length of the micropores is 1mm, the spinning viscosity is 10-20 Pa.s, the diameter of the asphalt fiber is 14 +/-1 mu m, and the number of the tows is 0.5K, 1K or 2K.
The heating mode of the oxidation carbonization mesh belt furnace is divided into two types: heating at the temperature below 300 ℃ in a hot air circulation mode, and controlling the temperature uniformity to be +/-1 ℃; heating is carried out at 300-900 ℃ in a ceramic heating plate mode, and the temperature uniformity is controlled to be +/-3 ℃.
Compared with the prior art, the invention has the following advantages:
1. the continuous filament bundle of the primary spun asphalt fiber is directly unwound to an oxidation carbonization mesh belt furnace for continuous oxidation and carbonization treatment, and the fiber is wound after obtaining certain strength, so that the problems of easy breakage and fluffing of the primary spun asphalt fiber due to the direct drafting and preoxidation are solved.
2. The method has the advantages that the asphalt fiber obtains sufficient stress relaxation by changing the oxygen concentration of different chambers in the pre-oxidation furnace, the regulation and control of the molecular structure of the asphalt fiber are completed, and then the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament sample with a thick graphite sheet structure and good orientation is obtained.
3. The process is relatively simple and controllable, has high production efficiency, is easy to realize industrial production, and the prepared asphalt-based carbon fiber has high modulus and thermal conductivity, and is particularly suitable for preparing asphalt-based carbon fiber continuous filament products with larger tows.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Description of the drawings:
FIG. 1 is a micro-topography of a high modulus, high thermal conductivity pitch-based carbon fiber prepared in example 1;
fig. 2 is a micro-topography of the high modulus high thermal conductivity pitch-based carbon fiber prepared in example 2.
Detailed Description
Example 1
This embodiment is a specific implementation manner of the present invention, and specifically includes the following steps:
step 1: melt-spinning oil-based mesophase pitch with the mesophase content of 100%, the ash content of 30ppm, the S content of 900ppm, the N content of 800ppm and the softening point of 270 ℃ to obtain a continuous filament bundle of pitch fibers with the continuous length of 25000 m;
step 2: unwinding a continuous filament bundle of the primary-spun asphalt fiber to an oxidation carbonization mesh belt furnace through a filament returning mechanism, and firstly treating for 10min at the temperature of 200 ℃ under the condition of nitrogen atmosphere; then carrying out continuous oxidation treatment at the temperature of 200-260 ℃ in the air condition for 60 min; then, carrying out continuous oxidation treatment at the continuous temperature range of 260-290 ℃ under the condition of mixing air and nitrogen (oxygen concentration is 6%), wherein the treatment time is 30 min; finally, continuous carbonization treatment is carried out within the temperature gradient range of 350-900 ℃ under the protection of high-purity nitrogen for 10min, and then winding is carried out again;
and step 3: uncoiling a continuous filament bundle of low-temperature carbonized fiber, and then carrying out continuous high-temperature carbonization treatment at the temperature gradient range of 1000-1400 ℃ under the protection of high-purity nitrogen for 2min, wherein the tension is 600 cN;
and 4, step 4: continuously graphitizing the high-temperature carbonized fiber continuous filament bundle at 2800 ℃ for 2min under the protection of high-purity argon, wherein the tension is 200 cN;
and 5: carrying out surface sizing treatment on the continuous graphitized fiber bundle, wherein the sizing liquid is water-based epoxy resin, the solid content is 2%, and the sizing time is 20 s;
step 6: and (3) drying the sized continuous graphite fiber bundle by a vertical hot air circulation drying furnace at the drying temperature of 120 ℃ for 4min, and then winding and rolling to obtain the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament finished product, wherein the tensile modulus of the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament finished product is 950GPa, the heat conductivity of the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament finished product is 1100W/m.K, the tensile strength of the high-modulus high-heat-conductivity asphalt-based.
The microstructure of the high-modulus high-thermal-conductivity asphalt-based carbon fiber prepared by the process is shown in figure 1, and the graphite sheet layer is coarse and has high orientation degree.
Example 2
This embodiment is a specific implementation manner of the present invention, and specifically includes the following steps:
the heat treatment process in step 2 of example 1 was adjusted as follows: firstly, treating for 10min at 190 ℃ under the condition of nitrogen atmosphere; then carrying out continuous oxidation treatment at the temperature of 200-260 ℃ in the air condition for 90 min; and then carrying out continuous oxidation treatment at the continuous temperature range of 260-290 ℃ under the condition of mixing air and nitrogen (oxygen concentration is 15%), wherein the treatment time is 60 min. The tensile modulus was 900GPa, the thermal conductivity was 920W/m.K, and the tensile strength was 3.2 GPa.
The microstructure of the high modulus and high thermal conductivity asphalt-based carbon fiber prepared by the process is shown in figure 2, and the graphite sheet layer and the orientation of the high modulus and high thermal conductivity asphalt-based carbon fiber are slightly smaller than those of figure 1.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (4)
1. A preparation method of a high-modulus high-thermal-conductivity asphalt-based carbon fiber continuous filament is characterized by comprising the following steps:
step (1): carrying out melt spinning on an asphalt raw material with the mesophase content of 100%, the ash content of less than 40ppm, the S content of less than 1000ppm, the N content of less than 1000ppm and the softening point of 250-270 ℃ to obtain an asphalt fiber continuous filament bundle with the continuous length of more than 20000 m;
step (2): unwinding the continuous asphalt fiber filament bundle to an oxidation carbonization mesh belt furnace through a filament returning mechanism, firstly carrying out heat treatment for 5-10 min at the temperature of 180-200 ℃ under the condition of nitrogen atmosphere, carrying out continuous dehydration, deoiling agent and devolatilization treatment, and simultaneously enabling the continuous asphalt fiber filament bundle to obtain stress relaxation; carrying out continuous oxidation treatment at the temperature of 200-260 ℃ in the air condition for 60-90 min; then carrying out continuous oxidation treatment at the temperature of 260-290 ℃ under the condition of mixing air and nitrogen for 30-60 min, and controlling the oxidation weight gain within the range of 4-6%, wherein the concentration of oxygen in the mixed gas of air and nitrogen is 5-15%; finally, carrying out continuous carbonization treatment at the temperature of 350-900 ℃ under the protection of high-purity nitrogen for 10-15 min to obtain a low-temperature carbonized fiber continuous filament bundle with the tensile strength of 1.0-1.5 GPa, and then winding again;
and (3): uncoiling a low-temperature carbonized fiber continuous filament bundle, and then carrying out high-temperature carbonization treatment at the temperature of 1000-1400 ℃ under the protection of high-purity nitrogen for 1-2 min under the tension of 600cN to obtain a high-temperature carbonized fiber continuous filament bundle;
and (4): carrying out continuous ultrahigh-temperature graphitization treatment on the high-temperature carbonized fiber continuous filament bundle at the temperature of 2600-2800 ℃ under the protection of high-purity argon for 1-2 min, wherein the tension is 200cN, and thus obtaining a graphitized fiber continuous filament bundle;
and (5): carrying out surface sizing treatment on the graphitized fiber continuous filament bundle, wherein the sizing liquid is water-based epoxy resin, the solid content is 2-2.5%, and the sizing time is 10-30 s;
and (6): and drying the sized continuous graphite fiber bundle by a hot air circulation drying furnace at the drying temperature of 110-120 ℃ for 3-5 min, and then winding and rolling to obtain the high-modulus high-heat-conductivity asphalt-based carbon fiber continuous filament finished product, wherein the tensile modulus is 900-950 GPa, the heat conductivity is 900-1100W/m.K, the tensile strength is 2-3.5 GPa, and the continuous length is more than 20000 m.
2. The method for preparing the high modulus high thermal conductivity asphalt-based carbon fiber continuous filament as claimed in claim 1, wherein: the spinning pitch in the step (1) is coal-based mesophase pitch or oil-based mesophase pitch.
3. The method for preparing the high modulus high thermal conductivity asphalt-based carbon fiber continuous filament as claimed in claim 1, wherein: the aperture of the micropores of the spinneret plate used in the asphalt melt spinning in the step (1) is 0.2mm, the length of the micropores is 1mm, the spinning viscosity is 10-20 Pa s, the diameter of the asphalt fiber is 14 +/-1 mu m, and the number of the tows is 0.5K, 1K or 2K.
4. The method for preparing the high modulus high thermal conductivity asphalt-based carbon fiber continuous filament as claimed in claim 1, wherein: the heating modes of the oxidation carbonization mesh belt furnace in the step (2) are divided into two types: heating at the temperature below 300 ℃ in a hot air circulation mode, and controlling the temperature uniformity to be +/-1 ℃; heating is carried out at 300-900 ℃ in a ceramic heating plate mode, and the temperature uniformity is controlled to be +/-3 ℃.
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| CN111101241B (en) * | 2018-10-25 | 2023-11-10 | 中国石油化工股份有限公司 | Manufacturing method for improving strength of carbon fiber |
| CN109610048B (en) * | 2018-12-20 | 2021-06-15 | 湖南东映碳材料科技有限公司 | Preparation method of asphalt-based carbon fiber with hollow cross-section structure |
| CN110128160B (en) * | 2019-04-22 | 2021-05-11 | 湖南东映碳材料科技有限公司 | Method for preparing high-thermal-conductivity carbon-carbon composite material from two-dimensional network of pitch fiber precursors |
| CN110592727A (en) * | 2019-09-24 | 2019-12-20 | 陕西天策新材料科技有限公司 | Preparation method of high-thermal-conductivity mesophase pitch-based graphite fiber filament |
| CN115029816A (en) * | 2022-06-17 | 2022-09-09 | 武汉科技大学 | Ultrahigh-thermal-conductivity mesophase pitch-based carbon fiber, composite material and preparation method thereof |
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