CN107488892A - 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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- CN107488892A CN107488892A CN201710721995.4A CN201710721995A CN107488892A CN 107488892 A CN107488892 A CN 107488892A CN 201710721995 A CN201710721995 A CN 201710721995A CN 107488892 A CN107488892 A CN 107488892A
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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)
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, polyvinyl resin, acrylic resin and methacrylonitrile 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) by mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, acrylic resin and metering system
Nitrile is 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：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, polyvinyl resin,
Acrylic resin and methacrylonitrile are mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, at spinning
Elevated Temperature Conditions in reason include：150-170 DEG C, then the heating with 5-10 DEG C/min are risen to 10-20 DEG C/min programming rate
Speed rises to 190-210 DEG C；Asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, the condition of charing is heated
Including：The temperature of heating is 1-2h, and the time of heating is 220-240 DEG C；Pass through the synergy between each raw material so that be made
Asphalt base carbon fiber material not only possess excellent mechanical property, while also possess excellent insulating power and antistatic energy
Power, field of heat insulating materials is can be widely applied for, while the method for the asphalt base carbon fiber material is simple, raw material is easy for preparing
.
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) by mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, acrylic resin and metering system
Nitrile is 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：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 polyvinyl resin is 10-30 parts by weight, the dosage of acrylic resin
For 25-55 parts by weight, the dosage of methacrylonitrile 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 polyvinyl resin is 15-25 parts by weight, the dosage of acrylic resin
For 35-45 parts by weight, the dosage of methacrylonitrile 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 polyvinyl resin are 5000-6000, the weight average molecular weight of acrylic resin
For 7000-9000.
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 is in acrylic resin, polyacrylamide and ethylene bis stearamide
It is one or more.
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, polyvinyl resin is divided equally again
Son amount is 5000-6000, and the weight average molecular weight of acrylic resin is 7000-9000.
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 acrylic resins, 25g glass fibres, 15g polyvinyl resins, 35g acrylic resins and 40g methacrylonitriles mix
Conjunction obtains mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10
DEG C/min programming rate rises to 150 DEG C, then rises to 190 DEG C with 5 DEG C/min programming rate；It will be obtained after the heated charing of precursor
To asphalt base carbon fiber materials A 1；Wherein, heating the condition of charing includes：The temperature of heating is 1h, and the time of heating is 220
℃。
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 polyvinyl resins, 45g acrylic resins and 50g methacrylonitriles mix
To mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 20 DEG C/
Min programming rate rises to 170 DEG C, then rises to 210 DEG C with 10 DEG C/min programming rate；It will be obtained after the heated charing of precursor
Asphalt base carbon fiber materials A 2；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 polyvinyl resins, 40g acrylic resins and 45g metering systems
Nitrile is mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：
160 DEG C are risen to 15 DEG C/min programming rate, then 200 DEG C are risen to 8 DEG C/min programming rate；By the heated charing of precursor
After obtain asphalt base carbon fiber materials A 3；Wherein, heating the condition of charing includes：The temperature of heating is 1.5h, the time of heating
For 230 DEG C.
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 polyvinyl resin is 10g, and the dosage of acrylic resin is 25g, methyl
The dosage of acrylonitrile is 25g, obtains 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 polyvinyl resin is 30g, and the dosage of acrylic resin is 55g, first
The dosage of base acrylonitrile 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, methacrylonitrile is not included in raw material, obtains pitch base carbon fibre
Tie up material D3.
Comparative example 4
Carried out according to the method for embodiment 3, unlike, polyvinyl resin is not included in raw material, obtains pitch base carbon fibre
Tie up material D4.
Comparative example 5
Carried out according to the method for embodiment 3, unlike, acrylic resin is not included in raw material, obtains pitch base carbon fibre
Tie up 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, polyvinyl resin, acrylic resin and methacrylonitrile are mixed
Conjunction obtains 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 polyvinyl resin is 10-30 weight
Part, the dosage of acrylic resin is 25-55 parts by weight, and the dosage of methacrylonitrile 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 polyvinyl resin is 15-25 weight
Part, the dosage of acrylic resin is 35-45 parts by weight, and the dosage of methacrylonitrile 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 polyvinyl resin is
5000-6000, the weight average molecular weight of acrylic resin is 7000-9000.
9. according to the preparation method described in any one in claim 1-3, wherein, pitch viscosity reductant be selected from acrylic resin,
One or more in polyacrylamide 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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| CN201710721995.4A CN107488892A (en) | 2017-08-22 | 2017-08-22 | Asphalt base carbon fiber material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710721995.4A CN107488892A (en) | 2017-08-22 | 2017-08-22 | Asphalt base carbon fiber material and preparation method thereof |
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| CN201710721995.4A Pending CN107488892A (en) | 2017-08-22 | 2017-08-22 | Asphalt base carbon fiber material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108070268A (en) * | 2017-12-26 | 2018-05-25 | 宜兴市天宇世纪高新科技有限公司 | A kind of preparation method of asphalt base carbon fiber pitch |
| CN108411407A (en) * | 2018-03-21 | 2018-08-17 | 青岛美卡新型材料有限公司 | A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology |
| CN109943919A (en) * | 2017-12-21 | 2019-06-28 | 宜兴市宜泰碳纤维织造有限公司 | A kind of asphalt base carbon fiber manufacture craft |
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| CN109943919A (en) * | 2017-12-21 | 2019-06-28 | 宜兴市宜泰碳纤维织造有限公司 | A kind of asphalt base carbon fiber manufacture craft |
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| CN108411407A (en) * | 2018-03-21 | 2018-08-17 | 青岛美卡新型材料有限公司 | A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology |
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Application publication date: 20171219 |