CN108221090A - A kind of mesophase pitch-based carbon fibers and its precursor and preparation method with mixed type cross-sectional structure - Google Patents
A kind of mesophase pitch-based carbon fibers and its precursor and preparation method with mixed type cross-sectional structure Download PDFInfo
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- CN108221090A CN108221090A CN201810135885.4A CN201810135885A CN108221090A CN 108221090 A CN108221090 A CN 108221090A CN 201810135885 A CN201810135885 A CN 201810135885A CN 108221090 A CN108221090 A CN 108221090A
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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
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Abstract
The present invention provides a kind of mesophase pitch-based carbon fibers and its precursor and preparation method with mixed type cross-sectional structure, prepared mesophase pitch-based carbon fibers have the core radially external mixed type cross-sectional structure in cepaeform, not only higher tensile strength and stretch modulus had been maintained, but also with high thermal conductivity.Spinneret orifice draw ratio is used as (3 5):1 spinneret carries out spinning to mesophase pitch, obtains mesophase pitch precursor；Mesophase pitch precursor obtains the mesophase pitch-based carbon fibers with mixed type cross-sectional structure through pre-oxidizing, being carbonized and graphitization processing.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of mesophase pitch with mixed type cross-sectional structure
Base carbon fibre and its precursor and preparation method.
Background technology
Mesophase pitch-based carbon fibers have different cross-sectional structures, including cepaeform, radial and fold shape etc..This
A difference reflects the completely different crystallite dimension of mesophase pitch-based carbon fibers and degree of graphitization on microcosmic, macroscopically
Cause mesophase pitch-based carbon fibers mechanical property and thermal conductivity different.Cross-sectional structure is to mesophase pitch-based carbon fibers
Mechanical property especially tensile strength influence it is more apparent：Cepaeform cross-sectional structure crackle in fracture process connects
Continuous deflection can more be reasonably resistant to crack propagation, help to promote the tensile strength of mesophase pitch-based carbon fibers；And full spoke
Penetrating shape cross-sectional structure easily makes fracture crack be extended rapidly along fiber sheet direction, and mesophase pitch-based carbon fibers is caused " to collapse
Collapse formula " fracture, influence the tensile strengths of mesophase pitch-based carbon fibers；In addition, in carbonization and graphitizing process, radial radiation
Shape crystallite lamella easily generates big internal stress when shrinking, and fiber is caused to generate longitudinal splitting, fiber low-intensity is also resulted in and breaks
It splits.In terms of the influence of thermal conductivity：Radial or planar lamella is easier to be graphitized than accordion, and degree of graphitization is got over
Height, lattice defect is fewer, and lattice dimensions are bigger, and thermal conductivity is bigger.The higher random shape of degree of folding, cepaeform lamella are not easy stone
Mo Hua, thus thermal conductivity is also just low；The mesophase pitch-based carbon fibers of cepaeform easily stop oxygen to fibre during non-fusible
Tie up diffusion inside, core preoxidation degree is relatively low, in subsequent carbonisation because oxidation cross-linked degree not enough caused by core go out
The defects of existing molten condition and generation a large amount of hole, also causes thermal conductivity relatively low.
In summary it analyzes, the cross-sectional structure of cepaeform contributes to the promotion of tensile strength, radial cross section knot
Structure contributes to the promotion of thermal conductivity, and mesophase pitch-based carbon fibers of the prior art are single cross-sectional structures, causes
The problem of mechanical property cannot be taken into account with heat conductivility.Therefore, it is necessary to study a kind of comprising in both cross-sectional structures
Between asphalt phase base carbon fibre, to take into account mechanical property and heat conductivility.
Invention content
For problems of the prior art, the present invention provides a kind of interphase drip with mixed type cross-sectional structure
Green base carbon fibre and its precursor and preparation method, prepared mesophase pitch-based carbon fibers have core, and radially outside is in
The mixed type cross-sectional structure of cepaeform had not only maintained higher tensile strength and stretch modulus, but also with high thermal conductivity, solution
It has determined in the prior art because of mechanical property and heat conductivility caused by the single cross-sectional structure of mesophase pitch-based carbon fibers
The problem of cannot taking into account.
The present invention is to be achieved through the following technical solutions：
A kind of preparation method of the mesophase pitch-based carbon fibers with mixed type cross-sectional structure, includes the following steps,
Step 1 uses spinneret orifice draw ratio as (3-5):1 spinneret carries out spinning to mesophase pitch, obtains centre
Asphalt phase precursor；
Step 2, mesophase pitch precursor obtain tying with mixed type cross section through pre-oxidizing, being carbonized and graphitization processing
The mesophase pitch-based carbon fibers of structure.
Preferably, in step 1, mesophase pitch carries out spinning by twin screw extrusion process.
Preferably, in step 1, spinning temperature is 350-500 DEG C.
Preferably, in step 2, the detailed process of pre-oxidation is：By the mesophase pitch precursor that step 1 obtains in interval
Pre-oxidation treatment is carried out in formula pre-oxidation furnace, sets 25 DEG C of -200 DEG C of pre-oxidation heating rates as 5-10 DEG C/min, 200 DEG C -400
DEG C heating rate stablize 30-60min for 2-5 DEG C/min, and in 400 DEG C of constant temperature, whole preoxidation time is 90-300min.
Preferably, in step 2, using continous way carbonization and graphitization processing, carburizing temperature is 450-1800 DEG C, graphite
It is 2500-3000 DEG C to change temperature.
A kind of intermediate phase pitch-based carbon with mixed type cross-sectional structure obtained using any of the above-described preparation method is fine
Dimension, radially structure, outer layer are in cepaeform structure to core.
Preferably, the tensile strength of mesophase pitch-based carbon fibers is 2236-2800MPa, stretch modulus 659-
880GPa, thermal conductivity are 358-608W/ (m.K).
A kind of average diameter of mesophase pitch precursor that any of the above-described preparation method is used to obtain is 11-14 μm, fracture
Tension is more than 150CN.
Compared with prior art, the present invention has technique effect beneficial below：
It is (3-5) that the present invention, which selects spinneret orifice draw ratio,:1 big L/D ratio spinneret carries out spinning, and major diameter is bigger, spins
During silk, mesophase pitch melt passes through longer spinneret orifice so that mesophase pitch has more times to carry out molecular arrangement, shape
Into more regular orientation texture, so as to make that internal radiation is presented by the mesophase pitch-based carbon fibers that subsequent processing obtains
The mixed type cross-sectional structure of shape, external cepaeform.
Further, mesophase pitch precursor is subjected to intermittent pre-oxidation and continous way carbonization, graphitization processing.Precursor
Pre-oxidation treatment is carried out in intermittent pre-oxidation furnace, heating rate is set according to the thermal weight loss rule of raw material, 25 DEG C of setting-
200 DEG C of pre-oxidation heating rates are 5-10 DEG C/min, and 200 DEG C -400 DEG C of heating rate is 2-5 DEG C/min, and in 400 DEG C of perseverances
Temperature stablizes 30-60min, and whole preoxidation time is 90-300min.Carburizing temperature is 450-1800 DEG C, and graphitization temperature is
2500-3000℃。
The mesophase pitch-based carbon fibers that preparation method of the present invention obtains have mixed type cross-sectional structure, i.e. core is in spoke
Shape structure is penetrated, outer layer is in cepaeform structure.Its tensile strength be 2236-2800MPa, stretch modulus 659-880GPa, thermal conductivity
Rate is 358-608W/ (m.K).As it can be seen that the mesophase pitch-based carbon fibers of the mixed type cross-sectional structure both maintained it is higher
Mechanical property, and with high thermal conductivity.
The mesophase pitch precursor that the method for the present invention obtains has less diameter, the breaking tension of bigger, average diameter
It it is 11-14 μm, breaking tension is more than 150CN.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of mesophase pitch precursor cross section that the present invention is prepared.
Fig. 2 a are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 24000 times that the embodiment of the present invention 1 obtains
Retouch electron microscope.
Fig. 2 b are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 30000 times that the embodiment of the present invention 1 obtains
Retouch electron microscope.
Fig. 3 a are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 28000 times that the embodiment of the present invention 2 obtains
Retouch electron microscope.
Fig. 3 b are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 20000 times that the embodiment of the present invention 2 obtains
Retouch electron microscope.
Fig. 4 a are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 25000 times that the embodiment of the present invention 3 obtains
Retouch electron microscope.
Fig. 4 b are mesophase pitch-based carbon fibers cross section the sweeping in the case where amplifying 18000 times that the embodiment of the present invention 3 obtains
Retouch electron microscope.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The present invention is using the petroleum mesophase pitch that softening point is 310-330 DEG C, after twin-screw extrusion, through draw ratio
(3-5):1 big L/D ratio spinneret sprays, and the obtained average diameter of mesophase pitch precursor is 11-14 μm, breaking tension
More than 150CN；Mesophase pitch precursor through intermittent pre-oxidation and continuous carbonization and 2500-2800 DEG C of graphitization at
Reason, obtained mesophase pitch-based carbon fibers have it is internal radially, the external mixed type cross section in cepaeform structure ties
Structure.The mesophase pitch-based carbon fibers peak performance is tensile strength 2800MPa, stretch modulus 880GPa, thermal conductivity 608W/
(m.K).The mesophase pitch-based carbon fibers with mixed type cross-sectional structure had not only maintained higher mechanical property, but also have
High thermal conductivity.
The preparation method of mesophase pitch-based carbon fibers of the present invention with mixed type cross-sectional structure, specifically by with
Lower step is realized：
Step 1：Raw material spinning：
Be by softening point first 310-330 DEG C petroleum mesophase pitch pass through twin-screw extrusion carry out spinning, spinning
350-500 DEG C of temperature, the draw ratio of spinneret orifice is (3-5) on spinneret:1.Gained mesophase pitch precursor average diameter is 11-
14 μm, breaking tension is more than 150CN.
Step 2：The pre-oxidation treatment of mesophase pitch precursor：
The mesophase pitch precursor that step 1 obtains is subjected to pre-oxidation treatment, heating rate in intermittent pre-oxidation furnace
According to raw material thermal weight loss rule and set, by thermogravimetric curve understand the mesophase pitch increase weight since 200 DEG C, react with
It the raising of temperature and aggravates, and reacted most acutely at 350 DEG C, for the abundant progress of oxidation, 25 DEG C -200 of setting room temperature
DEG C pre-oxidation heating rate is 5-10 DEG C/min, and 200 DEG C -400 DEG C of heating rate is 2-5 DEG C/min, and steady in 400 DEG C of constant temperature
Determine 30-60min, whole preoxidation time is 90-300min.
Step 3：Continous way is carbonized and graphitization processing：
The pre-oxidized fibers that step 2 is obtained carry out continous way carbonization and graphitization processing, carburizing temperature 450-1800
DEG C, graphitization temperature is 2500-3000 DEG C；The continous way carbonization refers to pre-oxidized fibers being drawn through temperature step formula liter
High carbide furnace, obtained mesophase pitch-based carbon fibers have mixed type cross-sectional structure, i.e. core radial structure can be protected
The higher degree of graphitization of card and thermal conductivity, outer layer cepaeform structure can keep preferable mechanical property.Gained intermediate phase pitch-based
Carbon fiber tensile strength is 2236-2800MPa, stretch modulus 659-880GPa, thermal conductivity are 358-608W/ (m.K).
Specific embodiment is as follows.
Embodiment 1
Step 1：Raw material spinning：
Be by softening point first 310-330 DEG C petroleum mesophase pitch pass through twin-screw extrusion carry out spinning, spinning
Temperature is 350 DEG C, and the draw ratio of spinneret orifice is 3 on spinneret:1.Gained mesophase pitch precursor average diameter is 14 μm, fracture
Tension is more than 150CN, and the cross-sectional structure of mesophase pitch precursor is as shown in Figure 1.
Step 2：The pre-oxidation treatment of mesophase pitch precursor：
The mesophase pitch precursor that step 1 obtains is subjected to pre-oxidation treatment, heating rate in intermittent pre-oxidation furnace
It is set according to the thermal weight loss rule of raw material, understands that the petroleum mesophase pitch increases weight since 200 DEG C by thermogravimetric curve,
Reaction aggravates with the raising of temperature, and is reacted most acutely at 350 DEG C, for the abundant progress of oxidation, sets room temperature 25
DEG C of -200 DEG C pre-oxidation heating rates are 5 DEG C/min, and 200 DEG C -400 DEG C of heating rate is 2 DEG C/min, and in 400 DEG C of constant temperature
Stablize 60min, whole preoxidation time is 300min.
Step 3：Continous way is carbonized and graphitization processing：
The pre-oxidized fibers that step 2 is obtained carry out continous way carbonization and graphitization processing, carburizing temperature 450-1800
DEG C, graphitization temperature is 2500 DEG C.Obtained mesophase pitch-based carbon fibers have core radially, outer layer is in cepaeform
Mixed type cross-sectional structure, as shown in Figure 2 a and 2 b, i.e., core radial structure can ensure higher degree of graphitization and thermal conductivity
Rate, outer layer cepaeform structure can keep preferable mechanical property.Gained mesophase pitch-based carbon fibers tensile strength 2236MPa,
Stretch modulus 659GPa, thermal conductivity 358W/ (m.K).
Embodiment 2
Step 1：Raw material spinning：
Be by softening point first 310-330 DEG C petroleum mesophase pitch pass through twin-screw extrusion carry out spinning, spinning
Temperature is 470 DEG C, and the draw ratio of spinneret orifice is 4 on spinneret:1.Gained mesophase pitch precursor average diameter is 13 μm, fracture
Tension is more than 150CN.
Step 2：The pre-oxidation treatment of precursor：
The mesophase pitch precursor that step 1 obtains is subjected to pre-oxidation treatment, heating rate in intermittent pre-oxidation furnace
According to raw material thermal weight loss rule and set, by thermogravimetric curve understand the mesophase pitch increase weight since 200 DEG C, react with
It the raising of temperature and aggravates, and reacted most acutely at 350 DEG C, for the abundant progress of oxidation, 25 DEG C -200 of setting room temperature
DEG C pre-oxidation heating rate is 8 DEG C/min, and 200 DEG C -400 DEG C of heating rate is 4 DEG C/min, and stablizes in 400 DEG C of constant temperature
45min, whole preoxidation time are 120min.
Step 3：Continous way is carbonized and graphitization processing：
The pre-oxidized fibers that step 2 is obtained carry out continous way carbonization and graphitization processing, carburizing temperature 450-1800
DEG C, graphitization temperature is 2700 DEG C.Obtained mesophase pitch-based carbon fibers have core radially, outer layer is in cepaeform
Mixed type cross-sectional structure, as shown in Figure 3a and Figure 3b shows, i.e., core radial structure can ensure higher degree of graphitization and thermal conductivity
Rate, outer layer cepaeform structure can keep preferable mechanical property.Gained mesophase pitch-based carbon fibers tensile strength is
2487MPa, stretch modulus 721GPa, thermal conductivity are 456W/ (m.K).
Embodiment 3
Step 1：Raw material spinning：
Be by softening point first 310-330 DEG C petroleum mesophase pitch pass through twin-screw extrusion carry out spinning, spinning
Temperature is 500 DEG C, and the draw ratio of spinneret orifice is 5 on spinneret:1.Gained precursor average diameter is 11 μm, and breaking tension is more than
150CN。
Step 2：The pre-oxidation treatment of precursor：
The mesophase pitch precursor that step 1 obtains is subjected to pre-oxidation treatment, heating rate in intermittent pre-oxidation furnace
According to raw material thermal weight loss rule and set, by thermogravimetric curve understand the mesophase pitch increase weight since 200 DEG C, react with
It the raising of temperature and aggravates, and reacted most acutely at 350 DEG C, for the abundant progress of oxidation, 25 DEG C -200 of setting room temperature
DEG C pre-oxidation heating rate is 10 DEG C/min, and 200 DEG C -400 DEG C of heating rate is 5 DEG C/min, and stablizes in 400 DEG C of constant temperature
30min, whole preoxidation time are 90min.
Step 3：Continous way is carbonized and graphitization processing：
The pre-oxidized fibers that step 2 is obtained carry out continous way carbonization and graphitization processing, carburizing temperature 450-1800
DEG C, graphitization temperature is 3000 DEG C.Obtained mesophase pitch-based carbon fibers have core radially, outer layer is in cepaeform
Mixed type cross-sectional structure, as shown in figures 4 a and 4b, i.e., core radial structure can ensure higher degree of graphitization and thermal conductivity
Rate, outer layer cepaeform structure can keep preferable mechanical property.Gained mesophase pitch-based carbon fibers degree of graphitization reaches
94.1%, tensile strength reaches 2800MPa, stretch modulus reaches 880GPa, thermal conductivity reaches 608W/ (m.K).
Mesophase pitch-based carbon fibers degree of graphitization, thermal conductivity and the mechanical property that embodiment 1-3 is prepared such as 1 institute of table
Show.
1 mesophase pitch-based carbon fibers degree of graphitization of table, thermal conductivity and mechanical property list
To sum up, there is core in radiation using the mesophase pitch-based carbon fibers that the method for the invention is prepared
Shape, outer layer are in the mixed type cross-sectional structure of cepaeform, not only have higher degree of graphitization and thermal conductivity, but also with preferable power
Learn performance.
Claims (8)
1. a kind of preparation method of the mesophase pitch-based carbon fibers with mixed type cross-sectional structure, which is characterized in that including
Following steps,
Step 1 uses spinneret orifice draw ratio as (3-5):1 spinneret carries out spinning to mesophase pitch, obtains interphase drip
Green precursor；
Step 2, mesophase pitch precursor obtain having mixed type cross-sectional structure through pre-oxidizing, being carbonized and graphitization processing
Mesophase pitch-based carbon fibers.
2. the preparation method of the mesophase pitch-based carbon fibers according to claim 1 with mixed type cross-sectional structure,
It is characterized in that, in step 1, mesophase pitch carries out spinning by twin screw extrusion process.
3. the preparation method of the mesophase pitch-based carbon fibers according to claim 1 with mixed type cross-sectional structure,
It is characterized in that, in step 1, spinning temperature is 350-500 DEG C.
4. the preparation method of the mesophase pitch-based carbon fibers according to claim 1 with mixed type cross-sectional structure,
It is characterized in that, in step 2, the detailed process of pre-oxidation is：The mesophase pitch precursor that step 1 is obtained is intermittent pre-
Pre-oxidation treatment is carried out in oxidation furnace, sets 25 DEG C of -200 DEG C of pre-oxidation heating rates as 5-10 DEG C/min, 200 DEG C -400 DEG C
Heating rate is 2-5 DEG C/min, and stablizes 30-60min in 400 DEG C of constant temperature, and whole preoxidation time is 90-300min.
5. the preparation method of the mesophase pitch-based carbon fibers according to claim 1 with mixed type cross-sectional structure,
It is characterized in that, in step 2, using continous way carbonization and graphitization processing, carburizing temperature is 450-1800 DEG C, graphitization temperature
Spend is 2500-3000 DEG C.
6. a kind of interphase with mixed type cross-sectional structure obtained using any one of the claim 1-5 preparation methods
Asphalt base carbon fiber, which is characterized in that mesophase pitch-based carbon fibers have mixed type cross-sectional structure, and core is radially tied
Structure, outer layer are in cepaeform structure.
7. the mesophase pitch-based carbon fibers according to claim 6 with mixed type cross-sectional structure, which is characterized in that
The tensile strength of mesophase pitch-based carbon fibers is 2236-2800MPa, stretch modulus 659-880GPa, thermal conductivity 358-
608W/(m.K)。
8. it is a kind of use the average diameter of mesophase pitch precursor that any one of the claim 1-5 preparation methods obtain for
11-14 μm, breaking tension is more than 150CN.
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