CN108588899A - A kind of heat resistance graphene modified pitch fiber and preparation method - Google Patents
A kind of heat resistance graphene modified pitch fiber and preparation method Download PDFInfo
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- CN108588899A CN108588899A CN201810529399.0A CN201810529399A CN108588899A CN 108588899 A CN108588899 A CN 108588899A CN 201810529399 A CN201810529399 A CN 201810529399A CN 108588899 A CN108588899 A CN 108588899A
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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
- 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
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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
Abstract
The present invention provides a kind of heat resistance graphene modified pitch fiber and preparation methods.Graphene is cured with freezing after needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, graphene, trichorotrifluoroethane is set to be carried on needle-shaped micropore wollastonite, then it is mixed with spinning asphalt raw material, disperse under freezing conditions, remove, the heating stirring in spinning kettle, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.This method freezes solidification volume expansion by trichorotrifluoroethane, the stripping of screw rod disperses, using carrying for needle-shaped micropore wollastonite, pitch is dispersed graphene in, and along needle-shaped distribution, not only evenly dispersed modified pitch fiber, hence it is evident that improve the heat resistance and resistance type ability of pitch fibers.
Description
Technical field
The present invention relates to pitch fibers fields, and in particular to the preparation of high heat resistance fiber, more particularly to a kind of heat resistance
Graphene modified pitch fiber and preparation method.
Background technology
Pitch, which is generally considered as, a kind of to be wrapped in the asphalitine micelle with stable phase colloid and is dissolved or dispersed in grease tree
The boundary material formed in fat medium has colloid property.However, since the crude oil of extraction pitch is different, oil refining process and drip
It will appear aging during green military service, extremely complex and variable, domestic plain asphalt paraffin content is high, bonds force difference, ductility
The low, performance shortcomings such as temperature sensitivity is big.Pitch modified, temperature sensitivity reduce, and softening point increases, equivalent brittle point drop
It is low, so as to improve the pavement performance of pitch and asphalt.Pitch fibers play cracking resistance, absorption, dispersion and improvement pitch
High/low temperature stablizes the effect for reinforcing pitch, and application is widely noticed.
In modified pitch, the application of graphene increasingly attracts attention.Graphene is due to its unique structure and excellent
Physical and chemical performance make it become the hot spot in investigation of materials field, various composite materials and function material based on graphene
Material also emerges one after another.In previous report, people are often by various nano particles（Such as metal oxide, metal sulfide, your gold
Category, conductive polymer nanometer particle etc.）It is carried on larger-size graphene film（Radial dimension range is about 500 nm~5 μm)
Surface prepare graphene/nanometer particulate composite.Therefore, it when for asphalt modification, needs to carry out particular study
And application.
Chinese invention patent application number 201610990334.7 discloses a kind of compound carbon fiber of graphene/intermediate phase pitch-based
The preparation method of dimension.The compound carbon fiber of graphene/intermediate phase pitch-based that method described in the invention is prepared, compared to
Pure mesophase pitch, starting thermal weight loss temperature do not change, and rheological property is almost the same, and tensile strength and yield strength are equal
It is improved, conductive performance and modulus do not change substantially.
Chinese invention patent application number 201310212725.2 discloses a kind of intermediate phase pitch-based carbon of doped graphene
Fiber, including soluble mesophase pitch and graphene, carbon fiber is surpassed by soluble mesophase pitch and graphene oxide liquid phase
Sound is mixed with, graphene oxide content 0.1 ~ 5wt%, the 10 ~ 50um of carbon fiber diameter.The preparation method of carbon fiber is with low
Cost pitch is starting point, and doped graphene, the carbon fiber to preparing low cost, high-strength and high-modulus and good conductivity has preferable
Practical significance.
Chinese invention patent application number 201410067428.8 discloses a kind of graphene oxide modified pitch, by quality hundred
Point ratio consisting of：Graphene oxide 0.5% ~ 15% and matrix pitch 85% ~ 99.5%, the sum of above constituent mass percentage are
100%.Preparation method：Matrix pitch is heated and is melted, it is 120 ~ 200 DEG C to keep temperature, and graphene oxide is added, manually stirs
20 ~ 40min is mixed, cutter stirs 20 ~ 120min, is cooled to 100 ~ 150 DEG C, places 20 ~ 50min, it is made fully to be swollen；It will drip
Green mixture carries out 80~100min of shearing again on cutter, until graphene oxide is dispersed in pitch to obtain the final product.
Chinese invention patent application number 201510005123.9 discloses a kind of SBS modified pitch based on graphene oxide
And preparation method thereof.The SBS modified pitch based on graphene oxide described in the invention includes as the pitch of matrix, as adding
Graphene oxide, the linear SBS and sulfur containing promoter as modifying agent for adding agent；Graphene oxide quality accounts for matrix pitch quality
0.5 ~ 3%；The linear SBS mass accounts for the 3 ~ 5% of matrix pitch quality；The sulfur containing promoter accounts for matrix pitch quality
0.2 ~ 0.6%.Compared with prior art, the SBS modified pitch based on graphene oxide described in the invention gives full play to oxidation
The advantage of graphene has good high-temperature stability, high temperature Rut resistance, low-temperature cracking-resistance, fatigue resistance and water stability,
Preparation method is simple, and technique mitigates, at low cost.
According to above-mentioned, utilize graphene modified pitch, high-specific surface area that it is often made to reunite together in existing scheme,
It not only reduces the adsorption capacity of itself and influences the performance of graphene itself excellent properties, to affect graphene enhancing
The improvement of composite property, and it is irreversible to reunite, and unless applying external force, such as ultrasound and strong stirring make it uniformly
Dispersion, but the performance of pitch can be influenced.In consideration of it, the present invention propose a kind of heat resistance graphene modified pitch fiber and
Preparation method can effectively solve above-mentioned technical problem.
Invention content
When for the wider graphene modified pitch of current application, because of its high-specific surface area, easily reunites, not only drop
The low adsorption capacity of itself, and the performance of graphene itself excellent properties is influenced, it is compound to affect graphene enhancing
The improvement of material property, a kind of heat resistance graphene modified pitch fiber of present invention proposition and preparation method, to realize stone
Black alkene is evenly dispersed in pitch fibers, improves the heat resistance and resistance type ability of pitch fibers.
Specific technical solution of the present invention is as follows：
A kind of preparation method of heat resistance graphene modified pitch fiber, includes the following steps：
A kind of preparation method of heat resistance graphene modified pitch fiber, which is characterized in that include the following steps：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then by screw extruder cold
Disperse under the conditions of jelly, remove；
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane phase transformation
Gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers,
It is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.
Step（1）In the dispersion, 30 ~ 35 parts by weight of graphene, needle-shaped micropore wollastonite 60-80 parts by weight, three
65 ~ 70 parts by weight of chloro-trifluoro-ethane.
Phase-change material has the ability for changing its physical state in certain temperature range.By taking liquid-gas phase transformation as an example, adding
It when heat is to gasification temperature, just generates from liquid to gaseous phase transformation, during gasification, phase-change material is absorbed and stored a large amount of
Latent heat；When phase-change material cools down, the heat of storage will be dispersed into environment within the scope of certain temperature, be carried out from gaseous state
To the reverse transformation of liquid.When physical state changes, the temperature of material itself almost remains unchanged before phase transformation completion, is formed
One wide temperature platform absorbs although temperature-resistant or the latent heat of release is quite big.Phase-change material is being undergone phase transition
When, volume also changes.When becoming gaseous state from liquid, volume substantially expands, and generates powerful motive force.The present invention is exactly profit
The interlaminar action power for overcoming graphene is realized with this volume motive force, achievees the purpose that remove graphene.
Preferably, step（1）The supersonic frequency of the ultrasonic disperse is 100 ~ 150kHz, and power density is 0.6 ~ 0.8W/
cm2, processing time is 30 ~ 50min.
Preferably, step（1）The cured temperature of freezing is -10 ~ -30 DEG C.
Preferably, step（2）In the dispersion, 5 ~ 15 parts by weight of graphene composite material, spinning asphalt raw material 85 ~
95 parts by weight.
Preferably, step（2）The screw extruder is double screw extruder, three-screw extruder, four screw extruder
In one kind.
Preferably, step（2）The screw speed of the stripping is 40 ~ 60r/min.
Preferably, step（3）The heating temperature is 230 ~ 250 DEG C.
The present invention also provides a kind of heat resistance graphene modified pitch fibers that above-mentioned preparation method is prepared.By graphite
Alkene cures with freezing after needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, keeps graphene, trichorotrifluoroethane negative
It is loaded in needle-shaped micropore wollastonite, is then mixed with spinning asphalt raw material, disperses under freezing conditions, remove, add in spinning kettle
Thermal agitation is finally sprayed through conventional spinneret orifice, and graphene modified pitch fiber is made.This method is freezed by trichorotrifluoroethane
Cure volume expansion, the stripping of screw rod dispersion, using carrying for needle-shaped micropore wollastonite, disperses graphene in pitch, and edge
Needle-shaped distribution, not only evenly dispersed modified pitch fiber, hence it is evident that improve the heat resistance and resistance type ability of pitch fibers.
The present invention provides a kind of heat resistance graphene modified pitch fiber and preparation methods, compared with prior art,
Prominent feature and excellent effect are：
1, it proposes to cure graphene with freezing after needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, makes graphite
Alkene, trichorotrifluoroethane, which are carried on needle-shaped micropore wollastonite, makes graphene be easily dispersed.
2, this method freezes solidification volume expansion by trichorotrifluoroethane, the stripping of screw rod disperses, by graphene dispersion
In pitch, and along needle-shaped distribution, not only evenly dispersed modified pitch fiber, hence it is evident that improve the heat resistance and resistance of pitch fibers
Type ability.
3, modified pitch fiber produced by the present invention is heat-resist, and resistance type ability is strong, and application prospect is good.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；In dispersion, graphene 30
Parts by weight, needle-shaped 60 parts by weight of micropore wollastonite, 70 parts by weight of trichorotrifluoroethane.The supersonic frequency of ultrasonic disperse is
100kHz, power density 0.8W/cm2, processing time 30min.It is -30 DEG C to freeze cured temperature.
（2）By step（1）Obtained composite material is mixed with spinning asphalt raw material, is then being freezed by screw extruder
Under the conditions of dispersion, stripping；In dispersion, 5 parts by weight of graphene composite material, 95 parts by weight of spinning asphalt raw material.Screw rod squeezes
It is double screw extruder to go out machine.The screw speed of stripping is 40r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 250 DEG C.
Test method is：
Modified pitch fiber made from 10g embodiments 1 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g embodiments 1 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the embodiment 1 measured by the above method are lost
Weight percentage is as shown in table 1.
Embodiment 2
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；In dispersion, graphene 32
Parts by weight, needle-shaped 70 parts by weight of micropore wollastonite, 68 parts by weight of trichorotrifluoroethane.The supersonic frequency of ultrasonic disperse is
120kHz, power density 0.7W/cm2, processing time 35min.It is -20 DEG C to freeze cured temperature.
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, old 10 parts by weight of the compound ability of graphene, 90 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 50r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 240 DEG C.
Test method is：
Modified pitch fiber made from 10g embodiments 2 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g embodiments 2 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the embodiment 2 measured by the above method are lost
Weight percentage is as shown in table 1.
Embodiment 3
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；；In dispersion, graphene
34 parts by weight, needle-shaped 80 parts by weight of micropore wollastonite, 66 parts by weight of trichorotrifluoroethane.The supersonic frequency of ultrasonic disperse is
110kHz, power density 0.8W/cm2, processing time 30min.It is -10 DEG C to freeze cured temperature.
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, 15 parts by weight of graphene composite material, 85 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 60r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 230 DEG C.
Test method is：
Modified pitch fiber made from 10g embodiments 3 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g embodiments 3 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the embodiment 3 measured by the above method are lost
Weight percentage is as shown in table 1.
Embodiment 4
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；In dispersion, graphene 30
Parts by weight, needle-shaped 70 parts by weight of micropore wollastonite, 70 parts by weight of trichorotrifluoroethane.The supersonic frequency of ultrasonic disperse is
100kHz, power density 0.6W/cm2, processing time 50min.It is -15 DEG C to freeze cured temperature.
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, 5 parts by weight of graphene composite material, 95 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 55r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 235 DEG C.
Test method is：
Modified pitch fiber made from 10g embodiments 4 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g embodiments 4 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the embodiment 4 measured by the above method are lost
Weight percentage is as shown in table 1.
Embodiment 5
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；；In dispersion, graphene
30 parts by weight, needle-shaped 60 parts by weight of micropore wollastonite, 70 parts by weight of trichorotrifluoroethane.The supersonic frequency of ultrasonic disperse is
130kHz, power density 0.7W/cm2, processing time 45min.It is -20 DEG C to freeze cured temperature.
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, 10 parts by weight of graphene composite material, 90 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 50r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 240 DEG C.
Test method is：
Modified pitch fiber made from 10g embodiments 5 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g embodiments 5 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the embodiment 5 measured by the above method are lost
Weight percentage is as shown in table 1.
Comparative example 1
Preparation process is：
（1）By graphene and trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, makes graphene, trichlorine trifluoro
Ethane is compound to obtain graphene composite material；In dispersion, 30 parts by weight of graphene, 70 parts by weight of trichorotrifluoroethane.It is super
The supersonic frequency of sound dispersion is 130kHz, power density 0.7W/cm2, processing time 45min.Freeze cured temperature be-
20℃。
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, 10 parts by weight of graphene composite material, 90 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 50r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane
Phase transformation gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers
In, it is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.Heating temperature is 240 DEG C.
Test method is：
Modified pitch fiber made from 10g comparative examples 1 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10g comparative examples 1 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the comparative example 1 measured by the above method are lost
Weight percentage is as shown in table 1.
Comparative example 2
Preparation process is：
（1）By graphene and needle-shaped micropore wollastonite, ethyl alcohol mixing ultrasonic disperse, freezing solidification is then carried out, graphene, second are made
Alcohol is carried on needle-shaped micropore wollastonite and obtains graphene composite material；In dispersion, 30 parts by weight of graphene, needle-shaped microporous silicon
60 parts by weight of lime stone, 70 parts by weight of ethyl alcohol.The supersonic frequency of ultrasonic disperse is 130kHz, power density 0.7W/cm2, processing
Time is 45min.It is -20 DEG C to freeze cured temperature.
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then passes through screw extruder
Disperse under freezing conditions, remove；In dispersion, 10 parts by weight of graphene composite material, 90 parts by weight of spinning asphalt raw material.
Screw extruder is double screw extruder.The screw speed of stripping is 50r/min.
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, is most sprayed afterwards through spinneret orifice,
Graphene modified pitch fiber is made.Heating temperature is 240 DEG C.
Test method is：
Modified pitch fiber made from 10g comparative examples 2 is taken, under 25 DEG C, relative humidity 55%, is softened using SYD-2806- pitches
Point analyzer carries out softening point test, uses glycerol as medium, and initial heating temperature is 30 DEG C, and heating rate is 50 DEG C/
Min measures the softening point of pitch fibers；
Modified pitch fiber made from 10gUI ratios 2 is taken, after blasting air using oil-free air compressor and preheated, with
0.6m3/ h is passed through vertical cured furnace, is keen to 0 ~ 150 DEG C, 150 ~ 250 DEG C and 250 ~ 400 of analysis-e/or determining using ZRY-2P types
DEG C when evenly heat percent weight loss.
Graphene distribution characteristics, softening point and the heat of the modified pitch fiber of the comparative example 2 measured by the above method are lost
Weight percentage is as shown in table 1.
Table 1：
By experimental analysis, the present invention utilizes needle-shaped micropore wollastonite loadings graphene and trichorotrifluoroethane, effectively improves
Graphene is that pitch fibers heat resistance greatly improves in the dispersibility of pitch fibers.
Claims (9)
1. a kind of preparation method of heat resistance graphene modified pitch fiber, which is characterized in that include the following steps：
（1）By graphene and needle-shaped micropore wollastonite, trichorotrifluoroethane mixing ultrasonic disperse, freezing solidification is then carried out, is made
Graphene, trichorotrifluoroethane are carried on needle-shaped micropore wollastonite and obtain graphene composite material；
（2）By step（1）Obtained graphene composite material is mixed with spinning asphalt raw material, then by screw extruder cold
Disperse under the conditions of jelly, remove；
（3）By step（2）The material of extrusion heating stirring in spinning kettle, makes pitch melt, while trichorotrifluoroethane phase transformation
Gasification weakens graphene layer intermolecular forces, and graphene continues stripping and even single layer and is dispersed in pitch at several layers,
It is most sprayed afterwards through spinneret orifice, graphene modified pitch fiber is made.
2. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（1）In the dispersion, 30 ~ 35 parts by weight of graphene, needle-shaped micropore wollastonite 60-80 parts by weight, trichorotrifluoroethane 65 ~
70 parts by weight.
3. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（1）The supersonic frequency of the ultrasonic disperse is 100 ~ 150kHz, and power density is 0.6 ~ 0.8W/cm2, processing time be 30 ~
50min。
4. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（1）The cured temperature of freezing is -10 ~ -30 DEG C.
5. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（2）In the dispersion, 5 ~ 15 parts by weight of graphene composite material, 85 ~ 95 parts by weight of spinning asphalt raw material.
6. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（2）The screw extruder is one kind in double screw extruder, three-screw extruder, four screw extruder.
7. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（2）The screw speed of the stripping is 40 ~ 60r/min.
8. a kind of preparation method of heat resistance graphene modified pitch fiber according to claim 1, it is characterised in that：Step
（3）The heating temperature is 230 ~ 250 DEG C.
9. a kind of heat resistance graphene modified pitch fiber that any one of claim 1 ~ 8 preparation method is prepared.
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| CN201810529399.0A Withdrawn CN108588899A (en) | 2018-05-29 | 2018-05-29 | A kind of heat resistance graphene modified pitch fiber and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110629326A (en) * | 2019-10-29 | 2019-12-31 | 北京化工大学 | Preparation method of high-thermal-conductivity mesophase pitch-based carbon fiber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110629326A (en) * | 2019-10-29 | 2019-12-31 | 北京化工大学 | Preparation method of high-thermal-conductivity mesophase pitch-based carbon fiber |
| CN110629326B (en) * | 2019-10-29 | 2020-10-27 | 北京化工大学 | Preparation method of high-thermal-conductivity mesophase pitch-based carbon fiber |
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