CN108385208A - A kind of B-Si doping pitch based carbon fiber and preparation method thereof - Google Patents

A kind of B-Si doping pitch based carbon fiber and preparation method thereof Download PDF

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CN108385208A
CN108385208A CN201810224870.5A CN201810224870A CN108385208A CN 108385208 A CN108385208 A CN 108385208A CN 201810224870 A CN201810224870 A CN 201810224870A CN 108385208 A CN108385208 A CN 108385208A
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carbon fiber
based carbon
pitch
doping
pitch based
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CN108385208B (en
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董志军
杜力
李轩科
袁观明
丛野
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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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
    • 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
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Fibers (AREA)

Abstract

The present invention relates to a kind of B Si to adulterate pitch based carbon fiber and preparation method thereof.Its technical solution is：By boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（1~5）∶（14~18）Dispensing, then the asphalt mixture obtained after mixing is dissolved in organic solvent, it stirs, is warming up to 200 ~ 400 °C in reaction kettle under inert atmosphere and stirring condition, keep the temperature, natural cooling；It is subsequently placed in the molten cylinder of melt spinning device, is kept the temperature under the conditions of inert atmosphere and 280 ~ 380 °C, the spinning under the conditions of 260 ~ 360 °C and 0.2 ~ 0.8MPa, be placed in pre-oxidation furnace and kept the temperature under the conditions of 180 ~ 280 °C；500 ~ 1600 °C are finally warming up under inert atmosphere in retort, keeps the temperature 1 ~ 2h, B Si are made and adulterate pitch based carbon fiber.The present invention have the characteristics that it is simple for process, at low cost, without special installation and be easy to industrialized production, prepared B Si doping pitch based carbon fiber high temperature resistants and antioxygenic property are good.

Description

A kind of B-Si doping pitch based carbon fiber and preparation method thereof
Technical field
The invention belongs to pitch based carbon fiber technical fields.More particularly to a kind of B-Si adulterates pitch based carbon fiber and its system Preparation Method.
Background technology
General purpose grade pitch based carbon fiber because it is simple for process, derive from a wealth of sources industrially play the part of with advantage at low cost it is important Role is commonly used for high temperature insulating material, brake system, the reinforcement of cement, capacitor, water body purification etc., has very extensive Application prospect (He Fu carbon fibers and its application technology [M] Chemical Industry Press, 2004.).But Carbon fibe higher than It begins to aoxidize in 400 °C of aerobic environment, continued oxidation can cause mechanical property to be remarkably decreased, and limit its service life and answer Use environment.Therefore, the problem of anti-oxidant research of Carbon fibe is urgent need to resolve.
Currently, surface changes performance enhancement carbon fiber surface performance, so as in extreme environment (high temperature, high ionization radiation etc.) Middle application.Oxidation-resistant ceramic coating is a key technology of modified carbon fiber surface performance.However, since most of ceramics apply Coefficient of thermal expansion between layer and Carbon fibe matrix mismatches, and coating cracking is caused to peel off, and cannot effectively inhibit oxidation to make Coating failure (Tkachenko L A, Shaulov A Y, Berlin A A. High-temperature protective coatings for carbon fibers[J]. Inorganic Materials, 2012, 48(3):213-221.)。
Using the method for matrix modification, i.e., ceramic forerunner is introduced in asphalt stock, prepare and adulterate by melt spinning Pitch based carbon fiber, which is avoided that, there is this problem.S.Lu etc., which is reacted using asphalt with polydimethylsiloxane, to be prepared Si and contains 26%wt% spinning presomas are measured, C-Si alloy fibers are prepared through melt spinning, non-fusible and 1200 °C of heat treatments, at 1200 °C Exposure a period of time in aerobic environment, the SiO that fiber surface is formed2Glass-film can effectively improve fiber antioxygenic property (Lu S, Rand B, Bartle K D, et al. NOVEL OXIDATION RESISTANT CARBON SILICON ALLOY FIBRES[J]. Carbon, 1997, 35(10–11):1485-1493.).Kaikai Ge etc. pass through SiCN and SiBCN ceramics Presoma is mixed with polyacrylonitrile, prepares dopen Nano Carbon fibe by electrostatic spinning, SiBCN doping improves Carbon fibe and exists Antioxygenic property (Ge K, Ye L, Han W, et al. Si (B) CN-doped carbon in 500 °C of air environments nanofibers with excellent oxidation resistance[J]. Materials Letters, 2013, 112(1):124-128.)。
Though the prior art has respective advantage, there is of high cost, complex process, needs the problems such as special installation.
Invention content
It is the present invention is directed to overcome the deficiencies in the prior art, and it is an object of the present invention to provide a kind of simple for process, at low cost and be not required to spy The preparation method of the B-Si doping pitch based carbon fibers of different equipment, the resistance to height of pitch based carbon fiber is adulterated with B-Si prepared by this method Mild antioxygenic property is good.
To achieve the above object, the technical solution adopted by the present invention is：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（1~5）∶（14~18）, by institute Boracic organic precursor, the siliceous organic precursor and pitch mixing are stated, asphalt mixture is obtained.
The B content of the boracic organic precursor is 0.5 ~ 5wt%, and boracic organic precursor is polyborazine and poly- borosilicate One kind in azane；The Si contents of the siliceous organic precursor are 10 ~ 40wt%, and siliceous organic precursor is Polycarbosilane, gathers One kind in dimethylsilane and PVDF hollow fiber membrane.
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（1~3）, the asphalt mixture is molten In organic solvent, 2 ~ 3h is stirred, pitch organic solvent mixed liquor is obtained.
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with The rate of 2 ~ 10 °C/min is warming up to 200 ~ 400 °C, keeps the temperature 2 ~ 6h；Then stop stirring, it is naturally cold under inert atmosphere conditions But, B-Si doping pitches are obtained.
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, inert atmosphere and 280 ~ 1 ~ 3h is kept the temperature under the conditions of 380 °C to obtain with 70 ~ 300m/min speed spinning under the conditions of 260 ~ 360 °C and 0.2 ~ 0.8MPa B-Si adulterates pitch based carbon fiber precursor.
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 °C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers.
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, with the rate liter of 2 ~ 10 °C/min Temperature keeps the temperature 1 ~ 2h to 500 ~ 1600 °C, and B-Si is made and adulterates pitch based carbon fiber.
The pitch is asphalt or is coal tar pitch.
The organic solvent is toluene or is dimethylbenzene.
The rotating speed of the stirring is 200 ~ 500r/min.
The inert atmosphere is argon gas or is nitrogen, purity >=99.999vol% of inert atmosphere.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
(1) present invention utilizes pitch, boracic organic precursor and siliceous organosilane precursor body hypothermia copyrolysis, and B-Si doping drips are made Blueness, then by melt spinning, pre-oxidation treatment and high temperature firing, B-Si is made and adulterates pitch based carbon fiber, with existing asphaltic base The oxidation protection technology of Carbon fibe is compared, present invention process is simple, it is at low cost, without special installation and be easily industrialized.
(2) B-Si prepared by the present invention adulterates pitch based carbon fiber even thickness, simultaneously silk and bridge joint phenomenon does not occur； Made product contains BN and SiC ceramic phase, and BN and SiC ceramic mutually react the B generated with oxygen in an oxidizing environment2O3And SiO2 Product antioxygenic property can be effectively improved.
(3) the B-Si doping pitch based carbon fibers that prepared by the present invention aoxidize 4h weightlessness 25wt% in 600 °C of air, and not Doping pitch based carbon fiber aoxidizes 4h weightlessness 33wt% in 600 °C of air, therefore B-Si doping significantly improves pitch based carbon fiber High temperature resistant and antioxygenic property, improve the performance of fibre reinforced composites.
Therefore, the present invention have the characteristics that it is simple for process, at low cost, without special installation and be easy to industrialized production, institute The B-Si doping pitch based carbon fiber high temperature resistants and antioxygenic property of preparation are good.
Description of the drawings
Fig. 1 is a kind of SEM photograph of B-Si doping pitch based carbon fibers prepared by the present invention；
Fig. 2 is the XRD spectra of the doping pitch based carbon fibers of B-Si shown in Fig. 1.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments, invention is further described in detail, not to its protection domain Limitation.
In present embodiment：
The rotating speed of the stirring is 200 ~ 500r/min.
Purity >=99.999vol% of the inert atmosphere.
It is repeated no more in embodiment.
Embodiment 1
A kind of B-Si doping pitch based carbon fiber and preparation method thereof.It is the step of preparation method described in the present embodiment：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（1~2）∶（16.5~18）, will The boracic organic precursor, the siliceous organic precursor and pitch mixing, obtain asphalt mixture.
The B content of the boracic organic precursor is 0.5 ~ 2wt%, and boracic organic precursor is polyborazine；It is described siliceous The Si contents of organic precursor are 10 ~ 18wt%, and siliceous organic precursor is Polycarbosilane.
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（1~1.5）, by the asphalt mixture It is dissolved in organic solvent, stirs 2 ~ 3h, obtain pitch organic solvent mixed liquor.
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with The rate of 2 ~ 10 °C/min is warming up to 200 ~ 250 °C, keeps the temperature 2 ~ 6h；Then stop stirring, it is naturally cold under inert atmosphere conditions But, B-Si doping pitches are obtained.
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, inert atmosphere and 280 ~ 1 ~ 3h is kept the temperature under the conditions of 380 °C to obtain with 70 ~ 300m/min speed spinning under the conditions of 260 ~ 300 °C and 0.2 ~ 0.35MPa Pitch based carbon fiber precursor is adulterated to B-Si.
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 °C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers.
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, with the rate liter of 2 ~ 10 °C/min Temperature keeps the temperature 1 ~ 2h to 500 ~ 900 °C, and B-Si is made and adulterates pitch based carbon fiber.
The pitch is asphalt.
The organic solvent is toluene.
The inert atmosphere is argon gas.
Embodiment 2
A kind of B-Si doping pitch based carbon fiber and preparation method thereof.It is the step of preparation method described in the present embodiment：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（1.5~3）∶（15.5~17）, The boracic organic precursor, the siliceous organic precursor and the pitch are mixed, asphalt mixture is obtained.
The B content of the boracic organic precursor is 1.5 ~ 3wt%, and boracic organic precursor is PVDF hollow fiber membrane；It is described to contain The Si contents of silicon organic precursor are 18 ~ 25wt%, and siliceous organic precursor is polydimethylsiloxane.
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（1.5~2）, by the asphalt mixture It is dissolved in organic solvent, stirs 2 ~ 3h, obtain pitch organic solvent mixed liquor.
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with The rate of 2 ~ 10 °C/min is warming up to 250 ~ 300 °C, keeps the temperature 2 ~ 6h；Then stop stirring, it is naturally cold under inert atmosphere conditions But, B-Si doping pitches are obtained.
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, inert atmosphere and 280 ~ 1 ~ 3h is kept the temperature under the conditions of 380 °C to obtain with 70 ~ 300m/min speed spinning under the conditions of 280 ~ 320 °C and 0.35 ~ 0.5MPa Pitch based carbon fiber precursor is adulterated to B-Si.
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 °C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers.
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, with the rate liter of 2 ~ 10 °C/min Temperature keeps the temperature 1 ~ 2h to 800 ~ 1200 °C, and B-Si is made and adulterates pitch based carbon fiber.
The pitch is coal tar pitch.
The organic solvent is dimethylbenzene.
The inert atmosphere is nitrogen.
Embodiment 3
A kind of B-Si doping pitch based carbon fiber and preparation method thereof.It is the step of preparation method described in the present embodiment：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（2.5~4）∶（14.5~16）, The boracic organic precursor, the siliceous organic precursor and the pitch are mixed, asphalt mixture is obtained.
The B content of the boracic organic precursor is 2.5 ~ 4wt%, and boracic organic precursor is polyborazine；It is described siliceous The Si contents of organic precursor are 25 ~ 32wt%, and siliceous organic precursor is PVDF hollow fiber membrane.
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（2~2.5）, by the asphalt mixture It is dissolved in organic solvent, stirs 2 ~ 3h, obtain pitch organic solvent mixed liquor.
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with The rate of 2 ~ 10 °C/min is warming up to 300 ~ 350 °C, keeps the temperature 2 ~ 6h；Then stop stirring, it is naturally cold under inert atmosphere conditions But, B-Si doping pitches are obtained.
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, inert atmosphere and 280 ~ 1 ~ 3h is kept the temperature under the conditions of 380 °C to obtain with 70 ~ 300m/min speed spinning under the conditions of 300 ~ 340 °C and 0.5 ~ 0.65MPa Pitch based carbon fiber precursor is adulterated to B-Si.
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 °C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers.
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, with the rate liter of 2 ~ 10 °C/min Temperature keeps the temperature 1 ~ 2h to 1000 ~ 1400 °C, and B-Si is made and adulterates pitch based carbon fiber.
The pitch is asphalt.
The organic solvent is toluene.
The inert atmosphere is nitrogen.
Embodiment 4
A kind of B-Si doping pitch based carbon fiber and preparation method thereof.It is the step of preparation method described in the present embodiment：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（3.5~5）∶（14~15）, will The boracic organic precursor, the siliceous organic precursor and pitch mixing, obtain asphalt mixture.
The B content of the boracic organic precursor is 3.5 ~ 5wt%, and boracic organic precursor is PVDF hollow fiber membrane；It is described to contain The Si contents of silicon organic precursor are 32 ~ 40wt%, and siliceous organic precursor is Polycarbosilane, polydimethylsiloxane and poly- borosilicate Any one of azane.
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（2.5~3）, by the asphalt mixture It is dissolved in organic solvent, stirs 2 ~ 3h, obtain pitch organic solvent mixed liquor.
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with The rate of 2 ~ 10 °C/min is warming up to 350 ~ 400 °C, keeps the temperature 2 ~ 6h；Then stop stirring, it is naturally cold under inert atmosphere conditions But, B-Si doping pitches are obtained.
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, inert atmosphere and 280 ~ 1 ~ 3h is kept the temperature under the conditions of 380 °C to obtain with 70 ~ 300m/min speed spinning under the conditions of 320 ~ 360 °C and 0.65 ~ 0.8MPa Pitch based carbon fiber precursor is adulterated to B-Si.
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 °C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers.
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, with the rate liter of 2 ~ 10 °C/min Temperature keeps the temperature 1 ~ 2h to 1200 ~ 1600 °C, and B-Si is made and adulterates pitch based carbon fiber.
The pitch is coal tar pitch.
The organic solvent is toluene.
The inert atmosphere is nitrogen.
Present embodiment has following good effect compared with prior art：
(1) present embodiment utilizes pitch, boracic organic precursor and siliceous organosilane precursor body hypothermia copyrolysis, and B- is made Si adulterates pitch, then by melt spinning, pre-oxidation treatment and high temperature firing, and B-Si is made and adulterates pitch based carbon fiber, and existing There is the oxidation protection technology of pitch based carbon fiber to compare, present embodiment is simple for process, it is at low cost, without special installation and It is easily industrialized.
(2) the B-Si doping pitch based carbon fibers prepared by present embodiment are as shown in the picture, and Fig. 1 is embodiment 2 A kind of SEM photograph of B-Si doping pitch based carbon fibers prepared；Fig. 2 is the XRD of the doping pitch based carbon fibers of B-Si shown in Fig. 1 Spectrogram.It will be seen from figure 1 that, there is not simultaneously silk and bridge joint phenomenon in made product even thickness；Figure it is seen that made Product contains BN and SiC ceramic phase, and BN and SiC ceramic mutually react the B generated with oxygen in an oxidizing environment2O3And SiO2Can have Effect improves product antioxygenic property.
(3) the B-Si doping pitch based carbon fibers that prepared by present embodiment aoxidize 4h weightlessness in 600 °C of air 25wt%, and 4h weightlessness 33wt% are aoxidized in 600 °C of air undoped with pitch based carbon fiber, therefore B-Si doping significantly improves drip The high temperature resistant and antioxygenic property of green based carbon fiber, improve the performance of fibre reinforced composites.
Therefore, present embodiment have it is simple for process, at low cost, without special installation and be easy to industrialized production Feature, prepared B-Si adulterates pitch based carbon fiber high temperature resistant and antioxygenic property is good.

Claims (6)

1. a kind of preparation method of B-Si doping pitch based carbon fiber, it is characterised in that the preparation method comprises the concrete steps that：
Step 1: pressing boracic organic precursor: siliceous organic precursor: the mass ratio of pitch is 1:（1~5）∶（14~18）, by institute Boracic organic precursor, the siliceous organic precursor and pitch mixing are stated, asphalt mixture is obtained；
The B content of the boracic organic precursor is 0.5 ~ 5wt%, and boracic organic precursor is polyborazine and PVDF hollow fiber membrane In one kind；The Si contents of the siliceous organic precursor are 10 ~ 40wt%, and siliceous organic precursor is Polycarbosilane, poly- diformazan One kind in base silane and PVDF hollow fiber membrane；
Step 2: pressing the asphalt mixture: the mass ratio of organic solvent is 1:（1~3）, the asphalt mixture, which is dissolved in, to be had In solvent, 2 ~ 3h is stirred, pitch organic solvent mixed liquor is obtained；
Step 3: the pitch organic solvent mixed liquor is moved in reaction kettle, under inert atmosphere and stirring condition, with 2 ~ The rate of 10 °C/min is warming up to 200 ~ 400 °C, keeps the temperature 2 ~ 6h；Then stop stirring, under inert atmosphere conditions natural cooling, Obtain B-Si doping pitches；
Step 4: B-Si doping pitches are placed in the molten cylinder of melt spinning device, in inert atmosphere and 280 ~ 380 °C of items 1 ~ 3h is kept the temperature under part to obtain B-Si with 70 ~ 300m/min speed spinning under the conditions of 260 ~ 360 °C and 0.2 ~ 0.8MPa and mix Miscellaneous pitch based carbon fiber precursor；
Step 5: B-Si doping pitch based carbon fiber precursor is placed in pre-oxidation furnace, in air atmosphere, with 1 ~ 10 ° C/min rates are warming up to 180 ~ 280 °C, keep the temperature 12 ~ 48h, obtain pre-oxidized fibers；
Step 6: the pre-oxidized fibers are placed in retort, under an inert atmosphere, it is warming up to the rate of 2 ~ 10 °C/min 500 ~ 1600 °C, 1 ~ 2h is kept the temperature, B-Si is made and adulterates pitch based carbon fiber.
2. the preparation method of B-Si according to claim 1 doping pitch based carbon fiber, it is characterised in that the pitch is Asphalt is coal tar pitch.
3. the preparation method of B-Si doping pitch based carbon fiber according to claim 1, it is characterised in that described organic molten Agent is toluene or is dimethylbenzene.
4. the preparation method of B-Si doping pitch based carbon fiber according to claim 1, it is characterised in that the stirring Rotating speed is 200 ~ 500r/min.
5. the preparation method of B-Si doping pitch based carbon fiber according to claim 1, it is characterised in that the indifferent gas Atmosphere is argon gas or is nitrogen, purity >=99.999vol% of inert atmosphere.
6. a kind of B-Si adulterates pitch based carbon fiber, it is characterised in that the B-Si doping pitch based carbon fiber is wanted according to right Seek the B-Si doping asphaltic base Carbon fibers prepared by the preparation method of any one of 1 ~ 5 B-Si doping pitch based carbon fiber Dimension.
CN201810224870.5A 2018-03-19 2018-03-19 B-Si doped asphalt-based carbon fiber and preparation method thereof Active CN108385208B (en)

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CN109763209A (en) * 2019-01-31 2019-05-17 山东瑞城宇航碳材料有限公司 A method of manufacture high thermal conductivity asphalt base carbon fiber
CN109762351A (en) * 2018-12-24 2019-05-17 湖南鑫长胜材料科技有限公司 A kind of modified pitch and preparation method thereof
CN113388961A (en) * 2021-05-18 2021-09-14 武汉科技大学 Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109762351A (en) * 2018-12-24 2019-05-17 湖南鑫长胜材料科技有限公司 A kind of modified pitch and preparation method thereof
CN109763209A (en) * 2019-01-31 2019-05-17 山东瑞城宇航碳材料有限公司 A method of manufacture high thermal conductivity asphalt base carbon fiber
CN113388961A (en) * 2021-05-18 2021-09-14 武汉科技大学 Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film

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