CN107502997A - Asphalt base carbon fiber material and preparation method thereof - Google Patents
Asphalt base carbon fiber material and preparation method thereof Download PDFInfo
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- CN107502997A CN107502997A CN201710721965.3A CN201710721965A CN107502997A CN 107502997 A CN107502997 A CN 107502997A CN 201710721965 A CN201710721965 A CN 201710721965A CN 107502997 A CN107502997 A CN 107502997A
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Classifications
-
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- 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)
- Manufacturing & Machinery (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Fibers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of asphalt base carbon fiber material and preparation method thereof, the preparation method includes：Coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, is stirred at 50 70 DEG C, mix asphalt raw material is made；Mix asphalt raw material, pitch viscosity reductant, fibrous material, phenolic resin, polyvinyl alcohol and polystyrene are mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Asphalt base carbon fiber material will be obtained after the heated charing of precursor；The thermal conductivity for solving existing asphalt base carbon fiber is higher so that and its insulating power is weaker, while the problem of its antistatic effect deficiency.
Description
Technical field
The present invention relates to field of heat insulating materials, in particular it relates to a kind of asphalt base carbon fiber material and preparation method thereof.
Background technology
Asphalt base carbon fiber be one kind using asphalt or coal tar pitch as raw material, refined, spinning, pre-oxidation through pitch,
Carbonization or phosphorus content is more than 92% special fibre prepared by graphitization.It is a kind of new material of excellent in mechanical performance, it
1/4 of proportion less than steel, carbon fiber resin composite material tensile strength is general all in more than 3500Mpa, is 7~9 times of steel, resists
Draw modulus of elasticity be 230~430Gpa be also higher than steel, be indispensable engineering material in aerospace industry, separately traffic,
Also be widely used in terms of machinery, sports and amusement, leisure goods, health care and civil construction, in this meaning predictive of
Broad prospect of application of the carbon fiber in engineering.But the thermal conductivity of existing asphalt base carbon fiber is higher so that its insulating power
It is weaker, while its antistatic effect deficiency.
Therefore it provides one kind on the premise of its mechanical property is ensured, further improves insulating power and antistatic effect
Asphalt base carbon fiber material and preparation method thereof the problem of being urgent need to resolve of the present invention.
The content of the invention
It is an object of the invention to provide a kind of asphalt base carbon fiber material and preparation method thereof, solves existing asphaltic base
The thermal conductivity of carbon fiber is higher so that and its insulating power is weaker, while the problem of its antistatic effect deficiency.
To achieve these goals, the invention provides a kind of preparation method of asphalt base carbon fiber material, the preparation
Method includes：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, in 50-70
It is stirred at DEG C, mix asphalt raw material is made；
(2) mix asphalt raw material, pitch viscosity reductant, fibrous material, phenolic resin, polyvinyl alcohol and polystyrene are mixed
Obtain mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20
DEG C/min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Add
The temperature of heat is 1-2h, and the time of heating is 220-240 DEG C.
Present invention also offers a kind of asphalt base carbon fiber material, wherein, the asphalt base carbon fiber material is by above-mentioned
Preparation method is made.
Pass through above-mentioned technical proposal, the invention provides a kind of asphalt base carbon fiber material and preparation method thereof, the system
Preparation Method includes：Coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, in 50-70
It is stirred at DEG C, mix asphalt raw material is made；By mix asphalt raw material, pitch viscosity reductant, fibrous material, phenolic resin, poly-
Vinyl alcohol and polystyrene are mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, in spinning processing
Elevated Temperature Conditions include：150-170 DEG C, then the programming rate liter with 5-10 DEG C/min are risen to 10-20 DEG C/min programming rate
To 190-210 DEG C；Asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Add
The temperature of heat is 1-2h, and the time of heating is 220-240 DEG C；Pass through the synergy between each raw material so that obtained pitch
Base carbon fibre material not only possesses excellent mechanical property, while also possesses excellent insulating power and antistatic effect, can
It is widely used in field of heat insulating materials, while the method for being used to prepare the asphalt base carbon fiber material is simple, raw material is easy to get.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The invention provides a kind of preparation method of asphalt base carbon fiber material, the preparation method includes：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, in 50-70
It is stirred at DEG C, mix asphalt raw material is made；
(2) mix asphalt raw material, pitch viscosity reductant, fibrous material, phenolic resin, polyvinyl alcohol and polystyrene are mixed
Obtain mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20
DEG C/min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Add
The temperature of heat is 1-2h, and the time of heating is 220-240 DEG C.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, relative to the mix asphalt raw material of 100 parts by weight, the dosage of pitch viscosity reductant is 5-15 weight
Part, the dosage of fibrous material is 20-40 parts by weight, and the dosage of phenolic resin is 10-30 parts by weight, and the dosage of polyvinyl alcohol is
25-55 parts by weight, the dosage of polystyrene is 25-60 parts by weight.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, relative to the mix asphalt raw material of 100 parts by weight, the dosage of pitch viscosity reductant is 8-12 weight
Part, the dosage of fibrous material is 25-35 parts by weight, and the dosage of phenolic resin is 15-25 parts by weight, and the dosage of polyvinyl alcohol is
35-45 parts by weight, the dosage of polystyrene is 40-50 parts by weight.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, one or more of the inert gas in nitrogen, helium and argon gas.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, the temperature of heating is 500-550 DEG C in step (1), and the time of heating is 0.5-1h.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, coal tar pitch and asphalt are 1 according to mass ratio：1-2 ratio is mixed.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, one or more of the fibrous material in glass fibre, boron fibre and ceramic fibre.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, the weight average molecular weight of phenolic resin is 5000-6000, and the weight average molecular weight of polyvinyl alcohol is
7000-9000, the weight average molecular weight of polystyrene is 7000-8000.
In a kind of preferred embodiment of the present invention, in order to further improve obtained asphalt base carbon fiber material
Insulating power and antistatic effect, pitch viscosity reductant in triethanolamine, polyacrylamide and ethylene bis stearamide one
Kind is a variety of.
Present invention also offers a kind of asphalt base carbon fiber material, wherein, the asphalt base carbon fiber material is by above-mentioned
Preparation method is made.
The present invention will be described in detail by way of examples below.In following examples, the Weight-average molecular of phenolic resin
Measure as 5000-6000, the weight average molecular weight of polyvinyl alcohol is 7000-9000, and the weight average molecular weight of polystyrene is 7000-
8000。
Embodiment 1
100g coal tar pitches and 100g asphalt are mixed, and (temperature of heating is 500 for heating under nitrogen protection
DEG C, the time of heating is 0.5h) to molten condition, it is stirred at 50 DEG C, mix asphalt raw material is made；100g is mixed and dripped
Blue or green raw material, 8g triethanolamines, 25g glass fibres, 15g phenolic resin, 35g polyvinyl alcohol and 40g polystyrene are mixed to get mixed
Compound M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10 DEG C/min's
Programming rate rises to 150 DEG C, then rises to 190 DEG C with 5 DEG C/min programming rate；Asphaltic base will be obtained after the heated charing of precursor
Carbon fibre material A1；Wherein, heating the condition of charing includes：The temperature of heating is 1h, and the time of heating is 220 DEG C.
Embodiment 2
100g coal tar pitches and 200g asphalt are mixed, and (temperature of heating is 550 for heating under helium protection
DEG C, the time of heating is 1h) to molten condition, it is stirred at 70 DEG C, mix asphalt raw material is made；By 100g mix asphalts
Raw material, 12g polyacrylamides, 35g boron fibres, 25g phenolic resin, 45g polyvinyl alcohol and 50g polystyrene are mixed to get mixing
Thing M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 20 DEG C/min liter
Warm speed rises to 170 DEG C, then rises to 210 DEG C with 10 DEG C/min programming rate；Asphaltic base will be obtained after the heated charing of precursor
Carbon fibre material A2；Wherein, heating the condition of charing includes：The temperature of heating is 2h, and the time of heating is 240 DEG C.
Embodiment 3
100g coal tar pitches and 150g asphalt are mixed, and (temperature of heating is 520 for heating under argon gas protection
DEG C, the time of heating is 0.8h) to molten condition, it is stirred at 60 DEG C, mix asphalt raw material is made；100g is mixed and dripped
Blue or green raw material, 10g ethylene bis stearamides, 30g ceramic fibres, 20g phenolic resin, 40g polyvinyl alcohol and the mixing of 45g polystyrene
Obtain mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 15 DEG C/
Min programming rate rises to 160 DEG C, then rises to 200 DEG C with 8 DEG C/min programming rate；It will be obtained after the heated charing of precursor
Asphalt base carbon fiber materials A 3；Wherein, heating the condition of charing includes：The temperature of heating is 1.5h, and the time of heating is 230
℃。
Embodiment 4
Carried out according to the method for embodiment 3, unlike, relative to 100g mix asphalt raw material, pitch viscosity reductant
Dosage is 5g, and the dosage of fibrous material is 20g, and the dosage of phenolic resin is 10g, and the dosage of polyvinyl alcohol is 25g, polystyrene
Dosage be 25g, obtain asphalt base carbon fiber materials A 4.
Embodiment 5
Carried out according to the method for embodiment 3, unlike, relative to 100g mix asphalt raw material, pitch viscosity reductant
Dosage is 15g, and the dosage of fibrous material is 40g, and the dosage of phenolic resin is 30g, and the dosage of polyvinyl alcohol is 55g, polyphenyl second
The dosage of alkene is 60g, obtains asphalt base carbon fiber materials A 5.
Comparative example 1
Carried out according to the method for embodiment 3, unlike, the Elevated Temperature Conditions in spinning processing include：With 5 DEG C/min liter
Warm speed rises to 140 DEG C, then rises to 170 DEG C with 3 DEG C/min programming rate, and heating the condition of charing includes：The temperature of heating
For 0.5h, the time of heating is 200 DEG C, obtains asphalt base carbon fiber material D1.
Comparative example 2
Carried out according to the method for embodiment 3, unlike, the Elevated Temperature Conditions in spinning processing include：With 25 DEG C/min's
Programming rate rises to 180 DEG C, then rises to 220 DEG C with 12 DEG C/min programming rate, and heating the condition of charing includes：The temperature of heating
Spend for 2.5h, the time of heating is 250 DEG C, obtains asphalt base carbon fiber material D2.
Comparative example 3
Carried out according to the method for embodiment 3, unlike, ceramic fibre is not included in raw material, obtains asphalt base carbon fiber
Material D3.
Comparative example 4
Carried out according to the method for embodiment 3, unlike, phenolic resin is not included in raw material, obtains asphalt base carbon fiber
Material D4.
Comparative example 5
Carried out according to the method for embodiment 3, unlike, polyvinyl alcohol is not included in raw material, obtains asphalt base carbon fiber
Material D5.
Table 1
It can be obtained by above table, asphalt base carbon fiber materials A 1-A5 produced within the scope of the present invention not only has
Standby excellent mechanical property, while have superior antistatic effect and insulating power, and drip produced outside the scope of the present invention
Blue or green base carbon fibre material D1-D, its mechanical property, antistatic effect and insulating power are relatively weak.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of asphalt base carbon fiber material, it is characterised in that the preparation method includes：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, at 50-70 DEG C
It is stirred, mix asphalt raw material is made；
(2) mix asphalt raw material, pitch viscosity reductant, fibrous material, phenolic resin, polyvinyl alcohol and polystyrene are mixed to get
Mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20 DEG C/
Min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Heating
Temperature is 1-2h, and the time of heating is 220-240 DEG C.
2. preparation method according to claim 1, wherein, relative to the mix asphalt raw material of 100 parts by weight, pitch visbreaking
The dosage of agent is 5-15 parts by weight, and the dosage of fibrous material is 20-40 parts by weight, and the dosage of phenolic resin is 10-30 parts by weight,
The dosage of polyvinyl alcohol is 25-55 parts by weight, and the dosage of polystyrene is 25-60 parts by weight.
3. preparation method according to claim 2, wherein, relative to the mix asphalt raw material of 100 parts by weight, pitch visbreaking
The dosage of agent is 8-12 parts by weight, and the dosage of fibrous material is 25-35 parts by weight, and the dosage of phenolic resin is 15-25 parts by weight,
The dosage of polyvinyl alcohol is 35-45 parts by weight, and the dosage of polystyrene is 40-50 parts by weight.
4. according to the preparation method described in any one in claim 1-3, wherein, inert gas is selected from nitrogen, helium and argon
One or more in gas.
5. according to the preparation method described in any one in claim 1-3, wherein, the temperature of heating is in step (1)
500-550 DEG C, the time of heating is 0.5-1h.
6. according to the preparation method described in any one in claim 1-3, wherein, coal tar pitch and asphalt are according to quality
Than for 1：1-2 ratio is mixed.
7. according to the preparation method described in any one in claim 1-3, wherein, it is fine that fibrous material is selected from glass fibre, boron
One or more in peacekeeping ceramic fibre.
8. according to the preparation method described in any one in claim 1-3, wherein, the weight average molecular weight of phenolic resin is
5000-6000, the weight average molecular weight of polyvinyl alcohol is 7000-9000, and the weight average molecular weight of polystyrene is 7000-8000.
9. according to the preparation method described in any one in claim 1-3, wherein, pitch viscosity reductant is selected from triethanolamine, gathered
One or more in acrylamide and ethylene bis stearamide.
10. a kind of asphalt base carbon fiber material, it is characterised in that the asphalt base carbon fiber material in claim 1-9 by appointing
Preparation method described in meaning one is made.
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| CN201710721965.3A CN107502997A (en) | 2017-08-22 | 2017-08-22 | Asphalt base carbon fiber material and preparation method thereof |
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| CN201710721965.3A CN107502997A (en) | 2017-08-22 | 2017-08-22 | Asphalt base carbon fiber material and preparation method thereof |
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Cited By (2)
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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 |
| CN111004641A (en) * | 2019-12-27 | 2020-04-14 | 西安郎格飞博科技有限公司 | Spinnable asphalt and preparation method thereof |
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| CN105217602A (en) * | 2015-11-09 | 2016-01-06 | 沈阳化工大学 | The brilliant material preparation method of a kind of pitch base carbon |
| CN105239207A (en) * | 2015-11-17 | 2016-01-13 | 安徽弘昌新材料有限公司 | Graphitized compound carbon fibers and preparation method thereof |
| CN105315426A (en) * | 2015-11-06 | 2016-02-10 | 沈阳化工大学 | Composite asphalt-based carbon crystal material preparation method and carbon crystal plate prepared from composite asphalt-based carbon crystal material |
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| CN105315426A (en) * | 2015-11-06 | 2016-02-10 | 沈阳化工大学 | Composite asphalt-based carbon crystal material preparation method and carbon crystal plate prepared from composite asphalt-based carbon crystal material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN111004641A (en) * | 2019-12-27 | 2020-04-14 | 西安郎格飞博科技有限公司 | Spinnable asphalt and preparation method thereof |
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Application publication date: 20171222 |