CN114197111A - Preparation method of universal asphalt-based carbon fiber non-woven felt - Google Patents
Preparation method of universal asphalt-based carbon fiber non-woven felt Download PDFInfo
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- CN114197111A CN114197111A CN202010987588.XA CN202010987588A CN114197111A CN 114197111 A CN114197111 A CN 114197111A CN 202010987588 A CN202010987588 A CN 202010987588A CN 114197111 A CN114197111 A CN 114197111A
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- Prior art keywords
- based carbon
- carbon fiber
- asphalt
- woven felt
- oxidized
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 70
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 70
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000010426 asphalt Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 40
- 238000003763 carbonization Methods 0.000 claims abstract description 37
- 239000011261 inert gas Substances 0.000 claims abstract description 34
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000002074 melt spinning Methods 0.000 claims abstract description 12
- 239000003208 petroleum Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 239000010439 graphite Substances 0.000 claims description 26
- 229910002804 graphite Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 11
- 238000004939 coking Methods 0.000 abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 abstract 1
- 239000010935 stainless steel Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 15
- 230000003647 oxidation Effects 0.000 description 13
- 238000007254 oxidation reaction Methods 0.000 description 13
- 238000001816 cooling Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/04—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres
- D04H1/08—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres and hardened by felting; Felts or felted products
-
- 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 universal asphalt-based carbon fiber non-woven felt, which comprises the following steps: petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning; then pre-oxidizing the pitch-based carbon fiber protofilament to obtain pre-oxidized fiber; placing the pre-oxidized fiber on a high-temperature-resistant stainless steel grid plate which is suspended in a carbonization furnace, and carbonizing the pre-oxidized fiber in an inert gas atmosphere to obtain a general-grade pitch-based carbon fiber non-woven felt; wherein the inert gas is introduced from the bottom of the pre-oxidized fiber and exits from above the pre-oxidized fiber. According to the preparation method, the light components in the universal asphalt-based carbon fiber non-woven felt are taken away by the inert gas with the upward bottom, and the light component residues are avoided, so that the bottom of the universal asphalt-based carbon fiber non-woven felt is prevented from being hardened, coking and surface asphalt small particles are reduced, and the mechanical property of the universal asphalt-based carbon fiber non-woven felt is improved.
Description
Technical Field
The invention relates to the field of asphalt-based carbon fibers, in particular to a preparation method of a universal asphalt-based carbon fiber non-woven felt.
Background
The universal asphalt-based carbon fiber non-woven felt has the performances of low density, high resistance, incombustibility and high static resistance, and has excellent compression-resistant recovery, high safety, good construction performance and durable shock resistance, and the application fields of the universal asphalt-based carbon fiber non-woven felt include high-temperature heat-insulating materials, friction materials, cement reinforced materials and the like; the fiber is mainly prepared by using isotropic spinnable asphalt (such as petroleum asphalt) as a raw material through melt spinning, pre-oxidation and carbonization treatment; in the prior art, a carbonization furnace is adopted for carbonization treatment, inert gas is introduced into the carbonization furnace, and after the preoxidized fiber is put into the carbonization furnace for carbonization, the phenomenon of hardening at the bottom of the fiber, partial coking and small asphalt particles on the surface are found, so that the mechanical property of the non-woven felt is influenced finally.
In view of the above circumstances, it is desirable to develop a new method for preparing a general-purpose pitch-based carbon fiber non-woven felt, which can avoid the occurrence of a hardening phenomenon at the bottom of the fiber during carbonization, and reduce coking and pitch particles, thereby improving the mechanical properties of the general-purpose pitch-based carbon fiber non-woven felt.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a universal asphalt-based carbon fiber non-woven felt, which comprises the steps of placing pre-oxidized fibers on a high-temperature-resistant graphite porous plate, suspending the graphite porous plate in a carbonization furnace for carbonization treatment, taking away light components in the pre-oxidized fibers through inert gas with the bottom upward, and avoiding the light components from remaining at the bottom, so that the bottom of the universal asphalt-based carbon fiber non-woven felt is prevented from being hardened, coking and small asphalt particles on the surface are reduced, the mechanical property of the universal asphalt-based carbon fiber non-woven felt is improved, the tensile strength of the universal asphalt-based carbon fiber non-woven felt is 600-1000 MPa, and the tensile modulus is 30-50 GPa.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a universal asphalt-based carbon fiber non-woven felt comprises the following steps: the method comprises the following steps:
s1, carrying out melt spinning, namely obtaining asphalt-based carbon fiber precursor by taking petroleum asphalt as a raw material and carrying out melt spinning;
s2, pre-oxidizing, wherein the pitch-based carbon fiber protofilament is pre-oxidized to obtain pre-oxidized fiber;
s3, carbonizing, namely placing the pre-oxidized fibers on a graphite porous plate which is suspended in a carbonization furnace, and carbonizing in an inert gas atmosphere to obtain a universal pitch-based carbon fiber non-woven felt; and the inert gas is introduced from the bottom of the pre-oxidized fiber and is discharged from the upper part of the pre-oxidized fiber.
Preferably, in step S3, the inert gas enters from a plurality of transverse gas inlet pipes arranged on the porous graphite plate and exits from a plurality of longitudinal gas outlet holes arranged on the porous graphite plate.
Preferably, in the step S2, in the pre-oxidation process, the temperature of the pitch-based carbon fiber precursor is raised to 220 to 300 ℃ at a rate of 0.1 to 5 ℃/min in an air atmosphere, and the temperature is maintained for 1 to 6 hours.
Preferably, in the step S3, in the carbonization process, the pre-oxidized fiber is heated to 400 to 600 ℃ at a rate of 1 to 10 ℃/min in a carbonization furnace, and is kept warm for 0.5 to 5 hours, and then heated to 800 to 1200 ℃ at a rate of 0.5 to 5 ℃/min, and is kept warm for 0.5 to 3 hours.
Preferably, in step S3, the inert gas is also introduced from all directions of the carbonization furnace.
Preferably, the tensile strength of the universal asphalt-based carbon fiber non-woven felt is 600-1000 MPa, and the tensile modulus is 30-50 GPa.
The invention has the beneficial effects that:
the preparation method of the universal asphalt-based carbon fiber non-woven felt comprises the steps of placing pre-oxidized fibers on a graphite porous plate, suspending the graphite porous plate in a carbonization furnace for carbonization, taking away light components in the pre-oxidized fibers through inert gas with the bottom upward, and avoiding the light components from remaining, so that the bottom of the universal asphalt-based carbon fiber non-woven felt is prevented from being hardened, coking and small asphalt particles on the surface are reduced, the mechanical property of the universal asphalt-based carbon fiber non-woven felt is improved, the tensile strength of the universal asphalt-based carbon fiber non-woven felt reaches 600-1000 MPa, and the tensile modulus reaches 30-50 GPa.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram showing the distribution of a carbonization furnace and an inert gas pipeline in the preparation method of the general-purpose pitch-based carbon fiber non-woven felt;
fig. 2 is a schematic structural diagram of a graphite porous plate used in the method for preparing a general-purpose pitch-based carbon fiber non-woven felt according to the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way.
The invention provides a preparation method of a universal asphalt-based carbon fiber non-woven felt, which comprises the following steps:
s1, melt spinning
Petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning;
s2, pre-oxidation
The method comprises the following steps of (1) enabling pitch-based carbon fiber precursors to enter a pre-oxidation furnace, carrying out pre-oxidation in the air atmosphere, heating to 220-300 ℃ at a speed of 0.1-5 ℃/min, and carrying out heat preservation for 1-6 hours to obtain pre-oxidized fibers;
s3, charring
Placing the pre-oxidized fibers on a graphite porous plate 2 which is suspended in a carbonization furnace 1 (see figure 1), carbonizing in an inert gas atmosphere, heating to 400-600 ℃ at a speed of 1-10 ℃/min, preserving heat for 0.5-5 h, then heating to 800-1200 ℃ at a speed of 0.5-5 ℃/min, preserving heat for 0.5-3 h, and obtaining a general-grade pitch-based carbon fiber non-woven felt; wherein, inert gas is introduced from the bottom of the pre-oxidized fiber and is discharged from the upper part of the pre-oxidized fiber; specifically, the inert gas enters from a plurality of transverse gas inlet pipes 21 arranged on the graphite porous plate 2 and exits from a plurality of longitudinal gas outlet holes 22 arranged on the graphite porous plate 2; in addition, inert gas is also introduced from all directions into the carbonization furnace 1, wherein the inert gas line 3 is arranged in the carbonization furnace 1 in such a manner that, as shown in FIG. 1, the inert gas is introduced into the carbonization furnace 1 in the direction of the inert gas line 3 (the inert gas direction is indicated by an arrow K, L, M, N in FIG. 1).
A plurality of parallel transverse air inlet pipes 21 are arranged on the graphite porous plate 2 (see figure 2), and a plurality of longitudinal air outlet holes 22 are arranged on each transverse air inlet pipe 21; in the carbonization process, the pre-oxidized fiber is firstly placed on the graphite porous plate 2, and then the graphite porous plate 2 is placed in the air without contacting the bottom of the carbonization furnace 1; and then, the carbonization furnace 1 is vacuumized, inert gas is introduced, the furnace body is maintained at normal pressure, the inert gas is divided into two paths to perform the carbonization furnace 1, one path of the inert gas is introduced from each direction in the carbonization furnace 1 (see the inert gas trend in the figure 1), the other path of the inert gas enters from a plurality of transverse air inlet pipes 21 arranged on the graphite porous plate 2 and upwards moves from the bottom of the pre-oxidized fiber along a longitudinal air outlet hole 22 (see the figure 2), light components in the pre-oxidized fiber continuously escape along with the rise of the temperature, the upward inert gas at the bottom takes away the escaped light components, the light component residue is avoided, the hardening phenomenon in the carbonization process is prevented, and the prepared universal asphalt-based carbon fiber non-woven felt is coked and small asphalt particles appear, so that the mechanical property of the universal asphalt-based carbon fiber non-woven felt is influenced.
The general-purpose asphalt-based carbon fiber non-woven felt prepared by the preparation method has the tensile strength of 600-1000 MPa, the tensile modulus of 30-50 GPa and the tensile strength 200-300 MPa higher than that of general-purpose asphalt-based carbon fiber prepared by the existing method.
The following further describes the preparation method of the general-purpose pitch-based carbon fiber non-woven felt in combination with specific examples;
example 1
Petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning;
placing the pitch-based carbon fiber precursor in a pre-oxidation furnace, introducing air for pre-oxidation, slowly heating to 240 ℃ at the speed of 1 ℃/min, and preserving heat for 4 hours to obtain pre-oxidized fiber;
placing pre-oxidized fibers on a graphite porous plate 2, then suspending the graphite porous plate 2 in a carbonization furnace 1, introducing inert gas, heating to 400 ℃ at a speed of 5 ℃/min, preserving heat for 0.5h, then heating to 1000 ℃ at a speed of 3 ℃/min, preserving heat for 1h, cooling and taking out to obtain the universal asphalt-based carbon fiber non-woven felt without hardening and coking and small particles on the surface, and measuring the tensile strength of the universal asphalt-based carbon fiber non-woven felt to be 600-1000 MPa and the tensile modulus to be 30-50 GPa.
Example 2
Petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning;
placing the pitch-based carbon fiber precursor in a pre-oxidation furnace, introducing air for pre-oxidation, slowly heating to 260 ℃ at the speed of 1 ℃/min, and preserving heat for 3 hours to obtain pre-oxidized fiber;
placing pre-oxidized fibers on a porous graphite plate 2, then suspending the porous graphite plate 2 in a carbonization furnace 1, introducing inert gas, heating to 450 ℃ at a speed of 5 ℃/min, preserving heat for 0.5h, then heating to 1000 ℃ at a speed of 3 ℃/min, preserving heat for 0.5h, cooling and taking out to obtain the universal asphalt-based carbon fiber non-woven felt without hardening and coking and small particles on the surface, and measuring the tensile strength of the universal asphalt-based carbon fiber non-woven felt to be 600-1000 MPa and the tensile modulus to be 30-50 GPa.
Example 3
Petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning;
placing the pitch-based carbon fiber precursor in a pre-oxidation furnace, introducing air for pre-oxidation, slowly heating to 290 ℃ at the speed of 2 ℃/min, and preserving heat for 1.5h to obtain pre-oxidized fiber;
placing pre-oxidized fibers on a porous graphite plate 2, then suspending the porous graphite plate 2 in a carbonization furnace 1, introducing inert gas, heating to 450 ℃ at a speed of 5 ℃/min, preserving heat for 0.5h, then heating to 1000 ℃ at a speed of 2 ℃/min, preserving heat for 0.5h, cooling and taking out to obtain the universal asphalt-based carbon fiber non-woven felt without hardening and coking and small particles on the surface, and measuring the tensile strength of the universal asphalt-based carbon fiber non-woven felt to be 600-1000 MPa and the tensile modulus to be 30-50 GPa.
Comparative example
Petroleum asphalt is used as a raw material, and asphalt-based carbon fiber precursor is obtained after melt spinning;
placing the pitch-based carbon fiber precursor in a pre-oxidation furnace, introducing air for pre-oxidation, slowly heating to 290 ℃ at the speed of 2 ℃/min, and preserving heat for 1.5h to obtain pre-oxidized fiber;
placing the pre-oxidized fibers in a carbonization furnace 1, introducing inert gas, heating to 450 ℃ at a speed of 5 ℃/min, preserving heat for 0.5h, then heating to 1000 ℃ at a speed of 2 ℃/min, preserving heat for 0.5h, cooling and taking out to obtain the universal-grade asphalt-based carbon fiber non-woven felt, wherein the bottom of the universal-grade asphalt-based carbon fiber non-woven felt is hardened, part of the universal-grade asphalt-based carbon fiber non-woven felt is coked, asphalt small particles are generated on the surface of the universal-grade asphalt-based carbon fiber non-woven felt, the tensile strength of the universal-grade asphalt-based carbon fiber non-woven felt is 300-500 MPa, and the tensile modulus of the universal-grade asphalt-based carbon fiber non-woven felt is 20-40 GPa.
With the comprehensive implementation examples 1-3 and the comparative examples, the preparation method of the universal asphalt-based carbon fiber non-woven felt provided by the invention comprises the steps of placing pre-oxidized fibers on a graphite porous plate, suspending the graphite porous plate in a carbonization furnace for carbonization, taking away light components in the pre-oxidized fibers through inert gas with the bottom upward, and avoiding the light components from remaining, so that the bottom of the universal asphalt-based carbon fiber non-woven felt is prevented from being hardened, coking and small asphalt particles on the surface are reduced, the mechanical property of the universal asphalt-based carbon fiber non-woven felt is improved, the tensile strength of the universal asphalt-based carbon fiber non-woven felt reaches 600-1000 MPa, and the tensile modulus reaches 30-50 GPa.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A preparation method of a universal asphalt-based carbon fiber non-woven felt is characterized by comprising the following steps:
s1, carrying out melt spinning, namely obtaining asphalt-based carbon fiber precursor by taking petroleum asphalt as a raw material and carrying out melt spinning;
s2, pre-oxidizing, wherein the pitch-based carbon fiber protofilament is pre-oxidized to obtain pre-oxidized fiber;
s3, carbonizing, namely placing the pre-oxidized fibers on a graphite porous plate which is suspended in a carbonization furnace, and carbonizing in an inert gas atmosphere to obtain a universal pitch-based carbon fiber non-woven felt; and the inert gas is introduced from the bottom of the pre-oxidized fiber and is discharged from the upper part of the pre-oxidized fiber.
2. The method according to claim 1, wherein in step S3, the inert gas is introduced from a plurality of transverse gas inlet pipes provided on the porous graphite plate and is discharged from a plurality of longitudinal gas outlet holes provided on the porous graphite plate.
3. The method according to claim 1, wherein in the step S2, the temperature of the pitch-based carbon fiber precursor is raised to 220 to 300 ℃ at a rate of 0.1 to 5 ℃/min in an air atmosphere, and the temperature is maintained for 1 to 6 hours.
4. The preparation method according to claim 1, wherein in the step S3, in the carbonization process, the pre-oxidized fiber is heated to 400-600 ℃ at a rate of 1-10 ℃/min in a carbonization furnace, and is kept warm for 0.5-5 h, and then heated to 800-1200 ℃ at a rate of 0.5-5 ℃/min, and is kept warm for 0.5-3 h.
5. The method of claim 1, wherein in step S3, the inert gas is further introduced from all directions of the carbonization furnace.
6. The preparation method according to any one of claims 1 to 5, wherein the general-purpose pitch-based carbon fiber non-woven felt has a tensile strength of 500 to 1000MPa and a tensile modulus of 30 to 50 GPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115110206A (en) * | 2022-08-02 | 2022-09-27 | 清华大学 | Preparation method of superfine activated carbon fiber film and superfine activated carbon fiber film prepared by same |
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