CN109306552A - High-strength high-modules carbon fibre and preparation method thereof - Google Patents
High-strength high-modules carbon fibre and preparation method thereof Download PDFInfo
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- CN109306552A CN109306552A CN201710631180.7A CN201710631180A CN109306552A CN 109306552 A CN109306552 A CN 109306552A CN 201710631180 A CN201710631180 A CN 201710631180A CN 109306552 A CN109306552 A CN 109306552A
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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
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
Abstract
The invention discloses high-strength high-modules carbon fibre and preparation method thereof, this method is realized according to the following steps: (1) successively pre-oxidizing polyacrylonitrile fibril, low-temperature carbonization and high temperature cabonization, obtain carbon fiber；(2) carbon fiber is subjected to Infra Red laser radiations processing under an inert atmosphere, obtains radiation treatment carbon fiber；(3) the radiation treatment carbon fiber is subjected to gamma-ray irradiation processing, obtains high-strength high-modules carbon fibre.Polyacrylonitrile fibril is successively being pre-oxidized, is carrying out Infra Red laser radiations processing after low-temperature carbonization and high temperature cabonization again by this method, the random graphits structure of carbon fiber can be made to reset, form ordered structure, namely graphitization, and laser heating rate is fast, graphitization time can be shortened, improve throughput rate, then the carbon fiber further progress gamma-ray irradiation processing handled through Infra Red laser radiations can be made to crosslink between carbon fiber sheet layer, to further increase the intensity and modulus of carbon fiber.
Description
Technical field
The invention belongs to carbon fiber production field, especially a kind of high-strength high-modules carbon fibre and preparation method thereof.
Background technique
Polyacrylonitrile-based carbon fibre is widely used in composite material due to the features such as its high-strength and high-modulus.In 1500 DEG C of high temperature
The carbon fiber obtained under Carbonization Conditions has maximum intensity, and when temperature is more than 1500 DEG C, intensity is gradually reduced, and carbon fiber
Modulus be in monotone increasing trend as the temperature rises, therefore the high intensity of carbon fiber and the performance of high-modulus are difficult together
When take into account.The raising of modulus is since crystallite dimension becomes larger, and orientation is more preferable.And the reduction of intensity is due to stone under the high temperature conditions
Cross-linked structure between ink sheet layer is destroyed.
Therefore, the Carbon Fiber Technology that high-strength and high-modulus how is prepared needs further to be studied.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of high-strength high-modules carbon fibres and preparation method thereof, and this method exists
Polyacrylonitrile fibril is successively pre-oxidized, carries out Infra Red laser radiations processing after low-temperature carbonization and high temperature cabonization again, it can be with
The random graphits structure of carbon fiber is reset, forms ordered structure, namely graphitization, and laser heating rate is fast, energy
Enough shorten graphitization time, improve throughput rate, then the carbon fiber further progress γ handled through Infra Red laser radiations is penetrated
Line radiation treatment can make to crosslink between carbon fiber sheet layer, to further increase the intensity and modulus of carbon fiber.
In one aspect of the invention, the invention proposes a kind of methods for preparing high-strength high-modules carbon fibre.According to this hair
Bright embodiment, which comprises (1) polyacrylonitrile fibril is successively pre-oxidized, low-temperature carbonization and high temperature cabonization, obtained
To carbon fiber；(2) carbon fiber is subjected to Infra Red laser radiations processing under an inert atmosphere, obtains radiation treatment carbon fiber；
(3) the radiation treatment carbon fiber is subjected to gamma-ray irradiation processing, to obtain high-strength high-modules carbon fibre.
Preferably, in step (1), the content of acrylonitrile is not less than 90wt% in the polyacrylonitrile fibril.As a result, may be used
To guarantee the gained carbon fiber degree of orientation with higher, intensity and modulus.
Preferably, in step (1), acrylamide copolymer and methyl methacrylate are contained in the polyacrylonitrile fibril
At least one of ester copolymer.
Preferably, in step (1), the temperature of the pre-oxidation is 150~290 DEG C, and atmosphere is air atmosphere, and tension is
0~50MPa, time are 1~120min.
Preferably, in step (1), the pre-oxidation is carried out in continuous thermal reaction furnace.
Preferably, in step (1), the temperature of the low-temperature carbonization is 350~700 DEG C, and atmosphere is nitrogen atmosphere, tension
For 5~40MPa
Preferably, in step (1), 1000~1400 DEG C of the temperature of the high temperature cabonization, atmosphere is nitrogen atmosphere, tension
For 10~160MPa.
Preferably, in step (2), the wavelength of the laser light source of the Infra Red laser radiations is 760nm~1mm, power
For 4~10kW/cm2.Thus, it is possible to further increase the degree of orientation, the intensity and modulus of gained carbon fiber.
Preferably, in step (3), the gamma-ray irradiation processing is carried out in air, vacuum or inert atmosphere.
Preferably, in step (3), the radiation source of the gamma-ray irradiation processing is60Co gamma-rays, dose of radiation are
10-10000kGy, radiation dose rate 0.01-100kGy/h.Thus, it is possible to the degree of orientation of carbon fiber obtained by further increasing,
Intensity and modulus.
In another aspect of the invention, the invention proposes a kind of high-strength high-modules carbon fibres.Implementation according to the present invention
Example, the high-strength high-modules carbon fibre are prepared using method described above.Carbon fiber intensity with higher as a result,
And modulus.
Compared with prior art, the method for preparing high-strength high-modules carbon fibre of the invention by polyacrylonitrile fibril successively into
Infra Red laser radiations processing is carried out again after row pre-oxidation, low-temperature carbonization and high temperature cabonization, can make the turbostratic graphite knot of carbon fiber
Structure is reset, and forms ordered structure, namely graphitization, and laser heating rate is fast, can be shortened graphitization time, be improved
Then throughput rate can make carbon fiber to the carbon fiber further progress gamma-ray irradiation processing handled through Infra Red laser radiations
It is crosslinked between lamella, to further increase the intensity and modulus of carbon fiber, while the reaction involved in the present invention arrived is equal
It carries out under normal pressure, reaction condition is mild, and equipment is simple, and preparation cost is cheap, and implementation method is simple, is particularly suitable for quantization life
It produces.
Detailed description of the invention
Fig. 1 is the method flow schematic diagram according to an embodiment of the invention for preparing high-strength high-modules carbon fibre.
Specific embodiment
Below by conjunction with the embodiments and its Fig. 1 the invention will be further described, following embodiment be it is descriptive,
It is not restrictive, this does not limit the scope of protection of the present invention.
In one aspect of the invention, the invention proposes a kind of methods for preparing polyacrylonitrile carbon fiber.According to this hair
Bright embodiment, with reference to Fig. 1, this method comprises:
S100: polyacrylonitrile fibril is successively pre-oxidized, low-temperature carbonization and high temperature cabonization
In the step, polyacrylonitrile fibril is successively pre-oxidized, low-temperature carbonization and high temperature cabonization, obtains carbon fiber.
Specifically, polyacrylonitrile fibril is carried out pre-oxidation treatment during being somebody's turn to do, it is cyclized chain PAN molecule in polyacrylonitrile fibril
Dehydrogenation is converted into heat-resisting trapezoidal-structure, so that gained pre-oxidized fibers do not melt non-ignitable in high temperature cabonization, that is, guarantees it
Fibre morphology is kept in high temperature cabonization；During low-temperature carbonization, a series of small molecule (H in preoxidized fiber2、N2Deng) removing, and
Along with the recombination of cyclic structure；During high temperature cabonization, nitrogen is further removed in low-temperature carbonization fiber, while also adjoint
The further recombination of cyclic structure, ultimately form two-dimentional random graphits structure, i.e. carbon fiber structural.
According to one embodiment of present invention, the content of acrylonitrile can be not less than 90wt% in polyacrylonitrile fibril.Hair
Bright people's discovery, the polyacrylonitrile fibril of the acrylonitrile content advantageously form trapezoidal heat resistant structure, to improve final gained carbon
The quality of fiber.
Still another embodiment in accordance with the present invention contains acrylamide copolymer and methacrylic acid in polyacrylonitrile fibril
At least one of methyl terpolymer.It is avoided in preoxidation process specifically, both copolymers reduce the rigidity of precursor
Concentrate heat release.
According to still another embodiment of the invention, the temperature of pre-oxidation is 150~290 DEG C, and atmosphere is air atmosphere, tension
For 0~50MPa, the time is 1~120min, and pre-oxidizing is carried out in continuous thermal reaction furnace.Inventors have found that this is pre-
Other conditions can be significantly better than under oxidizing condition, and to promote in polyacrylonitrile fibril chain PAN molecule dehydrocyclization to be converted into heat-resisting
Trapezoidal-structure and then improve subsequent gained carbon fiber so that gained pre-oxidized fibers do not melt non-ignitable in high temperature cabonization
Quality.
According to still another embodiment of the invention, the temperature of low-temperature carbonization is 350~700 DEG C, and atmosphere is nitrogen atmosphere,
Power is 5~40MPa.Inventors have found that can be significantly better than other conditions under the conditions of the low-temperature carbonization promotes wire/fiber ring structure
Recombination, to further increase the quality of subsequent gained carbon fiber.
According to still another embodiment of the invention, 1000~1400 DEG C of the temperature of high temperature cabonization, atmosphere is nitrogen atmosphere,
Power is 10~160MPa.Inventors have found that can be significantly better than other conditions under the conditions of the high temperature cabonization improves subsequent gained carbon
The quality of fiber.
S200: carbon fiber is subjected to Infra Red laser radiations processing under an inert atmosphere
In the step, carbon fiber obtained above is subjected to Infra Red laser radiations processing under an inert atmosphere, to obtain
Radiation treatment carbon fiber.Inventors have found that by the way that polyacrylonitrile fibril is successively pre-oxidized, low-temperature carbonization and high temperature cabonization
It carries out Infra Red laser radiations processing again afterwards, carbon fiber can be made, ordered structure, namely graphitization are formed, to improve subsequent
The intensity and modulus of gained carbon fiber, and laser heating rate is fast, can shorten graphitization time, improve throughput rate.
According to still another embodiment of the invention, the wavelength of the laser light source of Infra Red laser radiations is 760nm~1mm, function
Rate is 4~10kW/cm2.Inventors have found that if power is too low so that carbon fiber and graphite degree is lower, and if power it is excessively high when
Fiber is easy to be blown；It is unfavorable for generating fuel factor if wavelength is too low, and wavelength is excessive will appear electric discharge phenomena.It uses as a result,
The laser light source of the wavelength and the Infra Red laser radiations of power bracket can guarantee final gained carbon fiber quality with higher.
S300: radiation treatment carbon fiber is subjected to gamma-ray irradiation processing
In the step, radiation treatment carbon fiber obtained above is subjected to gamma-ray irradiation processing, to obtain high-strength height
Modules carbon fibre.Inventors have found that can be with to the carbon fiber further progress gamma-ray irradiation processing handled through Infra Red laser radiations
Make to crosslink between carbon fiber lamella, to further increase the intensity and modulus of carbon fiber.
According to one embodiment of present invention, gamma-ray irradiation processing can be in air, vacuum or inert atmosphere into
Capable, and the radiation source of gamma-ray irradiation processing is60Co gamma-rays, dose of radiation 10-10000kGy, radiation dose rate are
0.01-100kGy/h.Inventors have found that radiation agent dose and the excessively high defect that can introduce of dosage rate make mechanical properties decrease, radiate
Dosage and the too low mechanical property of dosage rate improve unobvious.It as a result, can be significant using gamma-ray irradiation processing under this condition
Guarantee gained carbon fiber intensity and modulus with higher.
The method according to an embodiment of the present invention for preparing high-strength high-modules carbon fibre is successively carrying out polyacrylonitrile fibril in advance
Infra Red laser radiations processing is carried out again after oxidation, low-temperature carbonization and high temperature cabonization, and the random graphits structure of carbon fiber can be made to send out
It is raw to reset, ordered structure, namely graphitization are formed, and laser heating rate is fast, graphitization time can be shortened, improve production
Then rate can make carbon fiber sheet layer to the carbon fiber further progress gamma-ray irradiation processing handled through Infra Red laser radiations
Between crosslink, to further increase the intensity and modulus of carbon fiber, while the reaction involved in the present invention arrived is normal
Pressure carries out, and reaction condition is mild, and equipment is simple, and preparation cost is cheap, and implementation method is simple, is particularly suitable for quantization production.
It is of the invention in one aspect, the invention proposes a kind of high-strength high-modules carbon fibres.Implementation according to the present invention
Example, the high-strength high-modules carbon fibre is adopted to be prepared with the aforedescribed process.The carbon fiber is with higher as a result,
Intensity and modulus, specifically, the intensity of gained carbon fiber may be up to 3.6GPa, modulus may be up to 300GPa.It should be noted that
It is above-mentioned to be equally applicable to the high-strength high-modules carbon fibre for preparing feature and advantage described in high-strength high-modules carbon fibre, herein not
It repeats again.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment
Choosing the polyacrylonitrile fibril of 1K (i.e. 1000 number of monofilaments/beams) containing acrylamide copolymer, (acrylonitrile contains
Measure 92wt%), carry out 200 DEG C, 220 DEG C, 225 DEG C, 235 DEG C, 250 DEG C, 270 DEG C of five temperature ranges in air medium first
Thermostabilization processing, each temperature range residence time 10min, amount to 60min.Tension force is as follows: the first and second humidity province
Between tension force in 25MPa, third and fourth warm area tension force is 20MPa, the five, the six warm area tension forces be 25MPa to get
Pre-oxidized fibers, then under nitrogen protection by pre-oxidized fibers, 400 DEG C, 450 DEG C, 600 DEG C and 850 DEG C four humidity provinces
Carry out low-temperature carbonization, residence time 10min, tension force 15MPa；High temperature is carried out subsequently into 1400 DEG C of high temperature carbonization furnaces
Carbonization, residence time 3min, tension force obtains carbon fiber in 30MPa, then under protection of argon gas by carbon fiber, through infrared
Laser high-temperature heat treatment, irradiance power density 8kW/cm2, time 1min is handled, finally by the carbon fiber of laser treatment in argon
It is carried out under gas shielded60Co gamma-ray irradiation, radiation dose rate 2kGy/h, irradiation time 50h, total dose of radiation are 100kGy,
Obtain high-strength high-modules carbon fibre.
Comparative example
Fiber sample is handled the thermostabilization that polyacrylonitrile fibre is directly entered air atmosphere, humidity province with embodiment 1
Between be 200 DEG C, 220 DEG C, 225 DEG C, 235 DEG C, 250 DEG C and 270 DEG C, each warm area residence time be 10min, amount to 60min.?
Power control are as follows: the first and second temperature range tension force be 25MPa, third and fourth temperature range tension force be 20MPa, the 5th,
Six temperature range tension forces are 25MPa to get pre-oxidized fibers, then under nitrogen protection by pre-oxidized fibers, 400
DEG C, 450 DEG C, 600 DEG C and 850 DEG C of four humidity provinces carry out low-temperature carbonizations, residence time 10min, tension force 15MPa；
High temperature cabonization, residence time 3min are carried out subsequently into 1400 DEG C of high temperature carbonization furnaces, tension force obtains polypropylene in 30MPa
Nitrile carbon fiber.
Evaluation:
1, respectively to high-strength high-modules carbon fibre obtained by embodiment and the polyacrylonitrile carbon fiber volume density in comparative example, orientation
Degree, intensity and modulus are evaluated.
2, evaluation index and test method:
The test of volume density: the survey of carbon fiber density is carried out using the twin columns density gradient instrument of LLOYD company of Britain production
It is fixed.Density gradient method is placed in gradient liquid mixture in density gradient column by configuration rule using suspension theory, from top to
The density of lower part becomes larger and continuously distributed.Fiber sample is suspended in the identical gradient liquid of density therewith in gradient column,
The fluid density of levitation position is the density of fiber.The density of different location is marked with the accurate small ball of specific gravity in gradient column
Fixed (bead uses 23 ± 1 DEG C of temperature), draws out density-scale relation curve.Fiber is knotted and is put into density gradient column, 4
Fiber retention position scale is read after a hour, and scale is corresponded to by sample and density-scale relation curve calculates the body of fiber
Density, each sample test average value twice；
The test of the degree of orientation: respectively by high-strength high-modules carbon fibre obtained by embodiment and the polyacrylonitrile carbon fiber in comparative example
It shreds into powdered, its degree of orientation is analyzed using X-ray diffractometer (XRD)；
The test of intensity and modulus: by the carbon fiber Wesy epoxy resin liquid of preparation using fiber multifilament gluing machine solidification system
Standby carbon fiber multifilament sample strip carries out mechanical property (intensity and modulus) test to carbon fiber samples further according to G3362-82.
Test result is as shown in table 1:
High-strength high-modules carbon fibre obtained by 1 embodiment of table and the polyacrylonitrile carbon fiber the performance test results in comparative example
The above is only preferred embodiments of the invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as the protection scope that do not invent.
Claims (10)
1. a kind of method for preparing high-strength high-modules carbon fibre characterized by comprising
(1) polyacrylonitrile fibril is successively pre-oxidized, low-temperature carbonization and high temperature cabonization, obtains carbon fiber；
(2) carbon fiber is subjected to Infra Red laser radiations processing under an inert atmosphere, obtains radiation treatment carbon fiber；
(3) the radiation treatment carbon fiber is subjected to gamma-ray irradiation processing, obtains high-strength high-modules carbon fibre.
2. the method as described in claim 1, which is characterized in that in step (1), acrylonitrile in the polyacrylonitrile fibril
Content is not less than 90wt%.
3. the method as described in claim 1, which is characterized in that in step (1), contain propylene in the polyacrylonitrile fibril
At least one of amide copolymer and methylmethacrylate copolymer.
4. the method as described in claim 1, which is characterized in that in step (1), the temperature of the pre-oxidation is 150~290
DEG C, atmosphere is air atmosphere, and tension is 0~50MPa, and the time is 1~120min.
5. the method as described in claim 1, which is characterized in that in step (1), the pre-oxidation is in continuous thermal reaction furnace
Middle progress.
6. the method as described in claim 1, which is characterized in that in step (1), the temperature of the low-temperature carbonization is 350~
700 DEG C, atmosphere is nitrogen atmosphere, and tension is 5~40MPa.
7. the method as described in claim 1, which is characterized in that in step (1), the temperature 1000 of the high temperature cabonization~
1400 DEG C, atmosphere is nitrogen atmosphere, and tension is 10~160MPa.
8. the method as described in claim 1, which is characterized in that in step (2), the laser light source of the Infra Red laser radiations
Wavelength be 760nm~1mm, power be 4~10kW/cm2。
9. the method as described in claim 1, which is characterized in that in step (3), the gamma-ray irradiation processing is in sky
It is carried out in gas, vacuum or inert atmosphere；
Optional, in step (3), the radiation source of the gamma-ray irradiation processing is60Co gamma-rays, dose of radiation 10-
10000kGy, radiation dose rate 0.01-100kGy/h.
10. a kind of high-strength high-modules carbon fibre, which is characterized in that the high-strength high-modules carbon fibre is appointed using in claim 1-9
What one the method was prepared.
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Cited By (1)
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