CN108611705A - A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre - Google Patents
A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre Download PDFInfo
- Publication number
- CN108611705A CN108611705A CN201810363255.2A CN201810363255A CN108611705A CN 108611705 A CN108611705 A CN 108611705A CN 201810363255 A CN201810363255 A CN 201810363255A CN 108611705 A CN108611705 A CN 108611705A
- Authority
- CN
- China
- Prior art keywords
- polyacrylonitrile
- temperature
- carbon fibre
- preparation
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
- D01F9/20—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
-
- 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
Abstract
The invention discloses a kind of preparation methods of polyacrylonitrile-radical high-performance carbon fibre, are related to high-performance carbon fibre technical field, and a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre includes the following steps and is made：(1) polyacrylonitrile powder pre-processes；(2) prepared by polyacrylonitrile spinning solution；（3）It is prepared by polyacrylonitrile fibril；（4）Polyacrylonitrile-based carbon fibre；The tensile strength and stretch modulus that polyacrylonitrile-based carbon fibre can be greatly improved are significantly improved, and then expand the application field of polyacrylonitrile-based carbon fibre.
Description
Technical field
The invention belongs to high-performance carbon fibre technical fields, and in particular to a kind of system of polyacrylonitrile-radical high-performance carbon fibre
Preparation Method.
Background technology
Carbon fiber has high specific strength, and high ratio modulus, high temperature resistant is corrosion-resistant, creep resistant, conductive, heat transfer and heat
A series of excellent properties such as the coefficient of expansion is small.It both can be as the enhancing base bearing load of structural material, but also as function
Material is widely used in the fields such as aerospace, building, sport, automobile, medical treatment.What had both at present almost without other materials
So numerous characteristics, therefore, the development that carbon fiber is advanced by leaps and bounds in recent ten years.It is main in industrial production at present
Carbon fiber is produced for precursor using polyacrylonitrile (PAN) fiber, pitch fibers or viscose rayon.It can be made high by PAN precursor
Performance carbon fiber, and production technology is simple compared with other methods, thus rapidly developed.
The consistency of polyacrylonitrile-based carbon fibre prepared by existing method is relatively low, and elasticity modulus and tensile property are general, nothing
Method meets the increasing demand in market.
Invention content
The purpose of the present invention is for existing problem, provide a kind of preparation side of polyacrylonitrile-radical high-performance carbon fibre
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre, includes the following steps and is made：
(1) polyacrylonitrile powder pre-processes：Polyacrylonitrile powder is pressed into 60-80g：The ratio of 150mL is added to itaconic acid solution
In, it is 30-35 DEG C to keep the temperature of itaconic acid solution, while being handled using ultrasonic wave, is filtered after 10-15min, will
After polyacrylonitrile powder filtering, polyacrylonitrile powder is impregnated into 3-5min using deionized water, is then filtered, after the completion again by it
It is placed under conditions of temperature is 60-70 DEG C after being dried 20min, then polyacrylonitrile powder is put into silane coupling agent aqueous solution
Middle immersion treatment, it is 30-32 DEG C that heating, which keeps the temperature of silane coupling agent aqueous solution, is filtered after 40min, then poly- by what is filtered out
Acrylonitrile powder is handled using injecting type atmosphere low-temperature plasma surface treating machine, processing time 12-15s, processing
Distance is 35-38mm, processing power 800W；
(2) prepared by polyacrylonitrile spinning solution：Polyacrylonitrile powder is heated to 50 DEG C, 30-40min is kept the temperature, then heats up again
To 55 DEG C, 2-3 hours are kept the temperature, is sieved after 250-300 mesh, organic solvent temperature is adjusted to 1-3 DEG C, keeps the temperature 30min, then again
By 80-100g：Polyacrylonitrile powder is added in organic solvent by the ratio of 400-450mL, and continuation keeps the temperature 50- at 1-3 DEG C
60min, and stirred with 1500r/min rotating speeds, the activation nanometer sericite of polyacrylonitrile powder quality 5-8% is then added again, with
5 DEG C/10s is rapidly heated to 75.5-75.8 DEG C, keeps the temperature 80-90s, then proceedes to be warming up to 85-88 DEG C, constant temperature 3.5-4.5 is small
When, with 1800r/min rotating speeds stirring 40min to get；
（3）It is prepared by polyacrylonitrile fibril：By the technique of dry-wet spinning, polyacrylonitrile spinning solution is carried out by spinneret
It sprays, it is rear to enter solidification bathing solidification through fully exposing 10min under air, twice water-bath stretching is carried out after removing solvent,
Fixed length compacting by drying is carried out at 250 DEG C, finally carries out stretching sizing treatment under 120 DEG C of steam, polyacrylonitrile is obtained after dry
Base fiber precursor；
（4）Polyacrylonitrile-based carbon fibre：Under inert gas conditions by above-mentioned fiber precursor, it is carried out within the scope of 1200-1250 DEG C
Carbonization treatment 1.5-1.8min, total draft 0.1-1.5% obtain the polyacrylonitrile-based carbon fibre.
Further, the step（1）Underpants' health acid solutions are 1.5-2.5mol/L.
Further, the step（1）Middle ultrasonic frequency is 35-40kHz.
Further, the step（1）Middle silane coupling agent aqueous solution mass fraction is 12%.
Further, the step（2）Middle organic solvent is NN- dimethylformamides.
Further, the step（4）The activation nanometer sericite preparation method is：By nanometer sericite by uniform point
It is scattered in the ethanol solution that mass fraction is 30%, then adds the graphene oxide of nanometer quality of sericite 3-5%, then add oxygen
The crosslinking agent of graphite alkene quality 0.15%, is heated to 80-90 DEG C, is stirred 2 hours with 550r/min rotating speeds, is then filtered,
Drying to constant weight.
Further, the crosslinking agent is potassium manganate.
Further, the step（4）The process conditions of dry-wet spinning are that spinning temperature is 130-140 DEG C, and solidification is washed
Bath temperature is 50-70 DEG C, and first of water-bath draft temperature is 75-80 DEG C, and second water-bath draft temperature is 95-100 DEG C.
The present invention has the following advantages compared with prior art：The present invention is by pre-processing polyacrylonitrile powder, energy
The enough effective compactness for improving polyacrylonitrile-based carbon fiber structural, reduces the power that fault of construction is conducive to improve final carbon fiber
Learn performance.Polyacrylonitrile strand can be such that polyacrylonitrile fibre is formed finer and close in preprocessing process in conjunction with active group
Network structure, be conducive to the mechanical property for improving polyacrylonitrile fibril, the polyacrylonitrile fibril fibre structure of preparation uniformly causes
Close, the defect in the inside and outside portion of fiber is few, and the supramolecular structure of fiber is regular, and the degree of orientation is high, and crystallinity is high, the physical mechanical of fiber
It has excellent performance, fibre number is small, and diameter irregularity is low, is conducive to the pre-oxidation and carbonization of precursor, so that polyacrylonitrile is former
Silk fiber has high specific strength, high temperature resistant and a series of excellent properties such as anticorrosive, energy in carbonisation polyacrylonitrile carbon fiber
Enough it is widely used in national defence and civil field.It can by adding a certain amount of activation nanometer sericite in spinning solution
It is combined in the linear macromolecule chain of polyacrylonitrile fibril, keeps it not molten non-ignitable in subsequent carbonisation, keep thermodynamics
Stable state is the key that prepare high-performance carbon fibre, so as to which the stretching of polyacrylonitrile-based carbon fibre is greatly improved
Intensity is significantly improved with stretch modulus, and then expands the application field of polyacrylonitrile-based carbon fibre.
Specific implementation mode
Embodiment 1
A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre, includes the following steps and is made：
(1) polyacrylonitrile powder pre-processes：Polyacrylonitrile powder is pressed into 60g：The ratio of 150mL is added in itaconic acid solution,
It is 30 DEG C to keep the temperature of itaconic acid solution, while being handled using ultrasonic wave, is filtered after 10min, by polyacrylonitrile
After powder filter, polyacrylonitrile powder is impregnated into 3min using deionized water, is then filtered, placing it in temperature again after the completion is
After being dried 20min under conditions of 60 DEG C, then polyacrylonitrile powder is put into immersion treatment in silane coupling agent aqueous solution, added
It is 30 DEG C that heat, which keeps the temperature of silane coupling agent aqueous solution, is filtered after 40min, then by the polyacrylonitrile powder filtered out using spray
It penetrates formula atmosphere low-temperature plasma surface treating machine to be handled, processing time 12-15s, processing distance is 35-38mm, place
Reason power is 800W；
(2) prepared by polyacrylonitrile spinning solution：Polyacrylonitrile powder is heated to 50 DEG C, 30min is kept the temperature, is then warming up to 55 again
DEG C, 2 hours are kept the temperature, is sieved after 250 mesh, organic solvent temperature is adjusted to 1 DEG C, keeps the temperature 30min, then presses 80g again：400mL
Ratio polyacrylonitrile powder is added in organic solvent, continuation keeps the temperature 50min at 1 DEG C, and is stirred with 1500r/min rotating speeds
It mixes, then adds the activation nanometer sericite of polyacrylonitrile powder quality 5% again, be rapidly heated to 75.5 DEG C with 5 DEG C/10s, protected
Warm 80s, then proceedes to be warming up to 85 DEG C, constant temperature 3.5 hours, with 1800r/min rotating speeds stirring 40min to get；
（3）It is prepared by polyacrylonitrile fibril：By the technique of dry-wet spinning, polyacrylonitrile spinning solution is carried out by spinneret
It sprays, it is rear to enter solidification bathing solidification through fully exposing 10min under air, twice water-bath stretching is carried out after removing solvent,
Fixed length compacting by drying is carried out at 250 DEG C, finally carries out stretching sizing treatment under 120 DEG C of steam, polyacrylonitrile is obtained after dry
Base fiber precursor；
（4）Polyacrylonitrile-based carbon fibre：Under inert gas conditions by above-mentioned fiber precursor, it carries out at carbonization within the scope of 1200 DEG C
1.5min is managed, total draft 0.1% obtains the polyacrylonitrile-based carbon fibre.
Further, the step（1）Underpants' health acid solutions are 1.5mol/L.
Further, the step（1）Middle ultrasonic frequency is 35kHz.
Further, the step（1）Middle silane coupling agent aqueous solution mass fraction is 12%.
Further, the step（2）Middle organic solvent is NN- dimethylformamides.
Further, the step（4）The activation nanometer sericite preparation method is：By nanometer sericite by uniform point
It is scattered in the ethanol solution that mass fraction is 30%, then adds the graphene oxide of nanometer quality of sericite 3%, then add oxidation
The crosslinking agent of graphene quality 0.15% is heated to 80 DEG C, is stirred 2 hours with 550r/min rotating speeds, is then filtered, and dries
To constant weight.
Further, the crosslinking agent is potassium manganate.
Further, the step（4）The process conditions of dry-wet spinning are that spinning temperature is 130 DEG C, solidify bathing temperature
Degree is 50 DEG C, and first of water-bath draft temperature is 75 DEG C, and second water-bath draft temperature is 95 DEG C.
Embodiment 2
A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre, includes the following steps and is made：
(1) polyacrylonitrile powder pre-processes：Polyacrylonitrile powder is pressed into 80g：The ratio of 150mL is added in itaconic acid solution,
It is 35 DEG C to keep the temperature of itaconic acid solution, while being handled using ultrasonic wave, is filtered after 15min, by polyacrylonitrile
After powder filter, polyacrylonitrile powder is impregnated into 5min using deionized water, is then filtered, placing it in temperature again after the completion is
After being dried 20min under conditions of 70 DEG C, then polyacrylonitrile powder is put into immersion treatment in silane coupling agent aqueous solution, added
It is 32 DEG C that heat, which keeps the temperature of silane coupling agent aqueous solution, is filtered after 40min, then by the polyacrylonitrile powder filtered out using spray
It penetrates formula atmosphere low-temperature plasma surface treating machine to be handled, processing time 15s, processing distance is 38mm, processing power
For 800W；
(2) prepared by polyacrylonitrile spinning solution：Polyacrylonitrile powder is heated to 50 DEG C, 40min is kept the temperature, is then warming up to 55 again
DEG C, 3 hours are kept the temperature, is sieved after 300 mesh, organic solvent temperature is adjusted to 3 DEG C, keeps the temperature 30min, then presses 100g again：450mL
Ratio polyacrylonitrile powder is added in organic solvent, continuation keeps the temperature 60min at 3 DEG C, and is stirred with 1500r/min rotating speeds
It mixes, then adds the activation nanometer sericite of polyacrylonitrile powder quality 8% again, be rapidly heated to 75.8 DEG C with 5 DEG C/10s, protected
Warm 90s, then proceedes to be warming up to 88 DEG C, constant temperature 3.5-4.5 hours, with 1800r/min rotating speeds stirring 40min to get；
（3）It is prepared by polyacrylonitrile fibril：By the technique of dry-wet spinning, polyacrylonitrile spinning solution is carried out by spinneret
It sprays, it is rear to enter solidification bathing solidification through fully exposing 10min under air, twice water-bath stretching is carried out after removing solvent,
Fixed length compacting by drying is carried out at 250 DEG C, finally carries out stretching sizing treatment under 120 DEG C of steam, polyacrylonitrile is obtained after dry
Base fiber precursor；
（4）Polyacrylonitrile-based carbon fibre：Under inert gas conditions by above-mentioned fiber precursor, it carries out at carbonization within the scope of 1250 DEG C
1.8min is managed, total draft 1.5% obtains the polyacrylonitrile-based carbon fibre.
Further, the step（1）Underpants' health acid solutions are 2.5mol/L.
Further, the step（1）Middle ultrasonic frequency is 40kHz.
Further, the step（1）Middle silane coupling agent aqueous solution mass fraction is 12%.
Further, the step（2）Middle organic solvent is NN- dimethylformamides.
Further, the step（4）The activation nanometer sericite preparation method is：By nanometer sericite by uniform point
It is scattered in the ethanol solution that mass fraction is 30%, then adds the graphene oxide of nanometer quality of sericite 5%, then add oxidation
The crosslinking agent of graphene quality 0.15% is heated to 90 DEG C, is stirred 2 hours with 550r/min rotating speeds, is then filtered, and dries
To constant weight.
Further, the crosslinking agent is potassium manganate.
Further, the step（4）The process conditions of dry-wet spinning are that spinning temperature is 140 DEG C, solidify bathing temperature
Degree is 70 DEG C, and first of water-bath draft temperature is 80 DEG C, and second water-bath draft temperature is 100 DEG C.
Embodiment 3
A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre, includes the following steps and is made：
(1) polyacrylonitrile powder pre-processes：Polyacrylonitrile powder is pressed into 70g：The ratio of 150mL is added in itaconic acid solution,
It is 32 DEG C to keep the temperature of itaconic acid solution, while being handled using ultrasonic wave, is filtered after 12min, by polyacrylonitrile
After powder filter, polyacrylonitrile powder is impregnated into 4min using deionized water, is then filtered, placing it in temperature again after the completion is
After being dried 20min under conditions of 65 DEG C, then polyacrylonitrile powder is put into immersion treatment in silane coupling agent aqueous solution, added
It is 31 DEG C that heat, which keeps the temperature of silane coupling agent aqueous solution, is filtered after 40min, then by the polyacrylonitrile powder filtered out using spray
It penetrates formula atmosphere low-temperature plasma surface treating machine to be handled, processing time 13s, processing distance is 36mm, processing power
For 800W；
(2) prepared by polyacrylonitrile spinning solution：Polyacrylonitrile powder is heated to 50 DEG C, 35min is kept the temperature, is then warming up to 55 again
DEG C, 2.5 hours are kept the temperature, is sieved after 280 mesh, organic solvent temperature is adjusted to 2 DEG C, keeps the temperature 30min, then presses 90g again：
Polyacrylonitrile powder is added in organic solvent by the ratio of 420mL, and continuation keeps the temperature 55min at 2 DEG C, and with 1500r/min
Rotating speed stir, then add the activation nanometer sericite of polyacrylonitrile powder quality 5-8% again, with 5 DEG C/10s be rapidly heated to
75.6 DEG C, keep the temperature 88s, then proceed to be warming up to 86 DEG C, constant temperature 3.8 hours, with 1800r/min rotating speeds stirring 40min to get；
（3）It is prepared by polyacrylonitrile fibril：By the technique of dry-wet spinning, polyacrylonitrile spinning solution is carried out by spinneret
It sprays, it is rear to enter solidification bathing solidification through fully exposing 10min under air, twice water-bath stretching is carried out after removing solvent,
Fixed length compacting by drying is carried out at 250 DEG C, finally carries out stretching sizing treatment under 120 DEG C of steam, polyacrylonitrile is obtained after dry
Base fiber precursor；
（4）Polyacrylonitrile-based carbon fibre：Under inert gas conditions by above-mentioned fiber precursor, it carries out at carbonization within the scope of 1230 DEG C
1.6min is managed, total draft 0.8% obtains the polyacrylonitrile-based carbon fibre.
Further, the step（1）Underpants' health acid solutions are 1.8mol/L.
Further, the step（1）Middle ultrasonic frequency is 38kHz.
Further, the step（1）Middle silane coupling agent aqueous solution mass fraction is 12%.
Further, the step（2）Middle organic solvent is NN- dimethylformamides.
Further, the step（4）The activation nanometer sericite preparation method is：By nanometer sericite by uniform point
It is scattered in the ethanol solution that mass fraction is 30%, then adds the graphene oxide of nanometer quality of sericite 4%, then add oxidation
The crosslinking agent of graphene quality 0.15% is heated to 85 DEG C, is stirred 2 hours with 550r/min rotating speeds, is then filtered, and dries
To constant weight.
Further, the crosslinking agent is potassium manganate.
Further, the step（4）The process conditions of dry-wet spinning are that spinning temperature is 135 DEG C, solidify bathing temperature
Degree is 60 DEG C, and first of water-bath draft temperature is 78 DEG C, and second water-bath draft temperature is 96 DEG C.
Comparative example 1：It is differed only in step with embodiment 1（1）Underpants' health acid solution replaces with clear water.
Comparative example 2：It is differed only in without step with embodiment 1（1）Middle injecting type atmosphere low-temperature plasma surface
Processor processing.
Comparative example 3：It is differed only in step with embodiment 1（2）Middle activation nanometer sericite replaces with untreated receive
Rice sericite.
Comparative example 4：It is differed only in step with embodiment 1（2）Middle activation nanometer sericite replaces with nano mica powder.
Comparative example 5：Step is differed only in embodiment 1（1）For：Polyacrylonitrile powder is used into injecting type atmosphere low-temperature
Plasma surface treating machine is handled, processing time 13s, and processing distance is 36mm, processing power 800W, then will
Polyacrylonitrile powder presses 70g：The ratio of 150mL is added in itaconic acid solution, and it is 32 DEG C to keep the temperature of itaconic acid solution, together
Shi Caiyong ultrasonic waves are handled, and are filtered after 12min, and after polyacrylonitrile powder is filtered, polyacrylonitrile powder is used
Deionized water impregnates 4min, then filters, and places it in again after the completion under conditions of temperature is 65 DEG C after being dried 20min,
Polyacrylonitrile powder is put into immersion treatment in silane coupling agent aqueous solution again, heating keeps the temperature of silane coupling agent aqueous solution
It is 31 DEG C, is filtered after 40min.
Experiment
Commercial polypropylene itrile group fiber precursor performance, such as table 1；
Table 1
| Commercial polypropylene nitrile protofilament | |
| Precursor fiber number/dtex | 1.6 |
| Intensity/cNdtex-1 | 4.5 |
| Elongation/% | 12.1 |
| Modulus/cNdtex-1 | 705 |
| Boiling water shrinkage/% | 6.9 |
Embodiment and the pan based fibers precursor performance in comparative example are tested for the property：
Table 2
| Precursor fiber number/dtex | Intensity/cNdtex-1 | Elongation/% | Modulus/cNdtex-1 | Boiling water shrinkage/% | |
| Embodiment 1 | 1.0 | 6.8 | 16.3 | 892 | 2.4 |
| Embodiment 2 | 1.0 | 6.7 | 16.4 | 890 | 2.3 |
| Embodiment 3 | 1.0 | 6.6 | 16.5 | 891 | 2.5 |
| Comparative example 1 | 1.3 | 5.8 | 15.6 | 879 | 2.7 |
| Comparative example 2 | 1.1 | 6.3 | 13.5 | 823 | 3.8 |
| Comparative example 3 | 1.5 | 5.0 | 13.1 | 771 | 5.7 |
| Comparative example 4 | 1.5 | 4.9 | 12.8 | 765 | 6.0 |
| Comparative example 5 | 1.3 | 5.9 | 15.5 | 881 | 2.6 |
As can be seen from Table 2, the pan based fibers precursor comprehensive performance for preparing is more preferable in the present invention, by comparative example 1 with
Comparative example 5 is as can be seen that use injecting type atmosphere low-temperature plasma surface treating machine to handle polyacrylonitrile powder
Opportunity is different, has apparent influence to polypropylene-base protofilament performance.
Polyacrylonitrile-based carbon fibre performance test：
The measurement of the tensile strength, Young's modulus of polyacrylonitrile-based carbon fibre uses monofilament method, in electronic tensile machine (YGO02 types)
Enterprising to tell, standard testing span is ZOmm, and it is synnema intensity to take the average value of 20 monofilament：
Table 3
| Tensile strength GPa | Stretch modulus GPa | |
| Embodiment 1 | 5.12 | 295 |
| Embodiment 2 | 5.14 | 296 |
| Embodiment 3 | 5.11 | 294 |
| Comparative example 1 | 4.95 | 287 |
| Comparative example 2 | 4.90 | 283 |
| Comparative example 3 | 4.72 | 275 |
| Comparative example 4 | 4.60 | 271 |
As can be seen from Table 3, the polyacrylonitrile-based carbon fibre that prepared by the present invention has better tensile strength and stretch modulus, answers
Greatly expanded with field.
Claims (8)
1. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre, which is characterized in that include the following steps and be made：
(1) polyacrylonitrile powder pre-processes：Polyacrylonitrile powder is pressed into 60-80g：The ratio of 150mL is added to itaconic acid solution
In, it is 30-35 DEG C to keep the temperature of itaconic acid solution, while being handled using ultrasonic wave, is filtered after 10-15min, will
After polyacrylonitrile powder filtering, polyacrylonitrile powder is impregnated into 3-5min using deionized water, is then filtered, after the completion again by it
It is placed under conditions of temperature is 60-70 DEG C after being dried 20min, then polyacrylonitrile powder is put into silane coupling agent aqueous solution
Middle immersion treatment, it is 30-32 DEG C that heating, which keeps the temperature of silane coupling agent aqueous solution, is filtered after 40min, then poly- by what is filtered out
Acrylonitrile powder is handled using injecting type atmosphere low-temperature plasma surface treating machine, processing time 12-15s, processing
Distance is 35-38mm, processing power 800W；
(2) prepared by polyacrylonitrile spinning solution：Polyacrylonitrile powder is heated to 50 DEG C, 30-40min is kept the temperature, then heats up again
To 55 DEG C, 2-3 hours are kept the temperature, is sieved after 250-300 mesh, organic solvent temperature is adjusted to 1-3 DEG C, keeps the temperature 30min, then again
By 80-100g：Polyacrylonitrile powder is added in organic solvent by the ratio of 400-450mL, and continuation keeps the temperature 50- at 1-3 DEG C
60min, and stirred with 1500r/min rotating speeds, the activation nanometer sericite of polyacrylonitrile powder quality 5-8% is then added again, with
5 DEG C/10s is rapidly heated to 75.5-75.8 DEG C, keeps the temperature 80-90s, then proceedes to be warming up to 85-88 DEG C, constant temperature 3.5-4.5 is small
When, with 1800r/min rotating speeds stirring 40min to get；
（3）It is prepared by polyacrylonitrile fibril：By the technique of dry-wet spinning, polyacrylonitrile spinning solution is carried out by spinneret
It sprays, it is rear to enter solidification bathing solidification through fully exposing 10min under air, twice water-bath stretching is carried out after removing solvent,
Fixed length compacting by drying is carried out at 250 DEG C, finally carries out stretching sizing treatment under 120 DEG C of steam, polyacrylonitrile is obtained after dry
Base fiber precursor；
（4）Polyacrylonitrile-based carbon fibre：Under inert gas conditions by above-mentioned fiber precursor, it is carried out within the scope of 1200-1250 DEG C
Carbonization treatment 1.5-1.8min, total draft 0.1-1.5% obtain the polyacrylonitrile-based carbon fibre.
2. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（1）Underpants' health acid solutions are 1.5-2.5mol/L.
3. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（1）Middle ultrasonic frequency is 35-40kHz.
4. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（1）Middle silane coupling agent aqueous solution mass fraction is 12%.
5. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（2）Middle organic solvent is NN- dimethylformamides.
6. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（4）The activation nanometer sericite preparation method is：By nanometer sericite by evenly spread to mass fraction be 30% second
In alcoholic solution, the graphene oxide of nanometer quality of sericite 3-5% is then added, then adds the friendship of graphene oxide quality 0.15%
Join agent, be heated to 80-90 DEG C, is stirred 2 hours, be then filtered, drying to constant weight with 550r/min rotating speeds.
7. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 6, which is characterized in that described
Crosslinking agent is potassium manganate.
8. a kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre according to claim 1, which is characterized in that described
Step（4）The process conditions of dry-wet spinning are that spinning temperature is 130-140 DEG C, and solidification bathing temperature is 50-70 DEG C, first
Water-bath draft temperature is 75-80 DEG C, and second water-bath draft temperature is 95-100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810363255.2A CN108611705B (en) | 2018-04-21 | 2018-04-21 | Preparation method of polyacrylonitrile-based high-performance carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810363255.2A CN108611705B (en) | 2018-04-21 | 2018-04-21 | Preparation method of polyacrylonitrile-based high-performance carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108611705A true CN108611705A (en) | 2018-10-02 |
| CN108611705B CN108611705B (en) | 2020-11-20 |
Family
ID=63660910
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810363255.2A Active CN108611705B (en) | 2018-04-21 | 2018-04-21 | Preparation method of polyacrylonitrile-based high-performance carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108611705B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607578A (en) * | 2019-09-11 | 2019-12-24 | 大同新成新材料股份有限公司 | Production method of high-strength polyacrylonitrile-based carbon fiber |
| CN114990736A (en) * | 2022-06-13 | 2022-09-02 | 泰州市创新电子有限公司 | PAN-based carbon fiber for display bracket and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002004175A (en) * | 2000-06-20 | 2002-01-09 | Toray Ind Inc | Pan based precursor for carbon fiber and method of producing the same |
| CN101245500A (en) * | 2008-03-25 | 2008-08-20 | 东华大学 | Attapulgite nano-particle modified polyacrylonitrile-based carbon fiber protofilament and production method |
| CN101250770A (en) * | 2008-03-11 | 2008-08-27 | 东华大学 | Method for manufacturing polyacrylonitrile-based carbon fiber with enganced carbon nano-tube |
-
2018
- 2018-04-21 CN CN201810363255.2A patent/CN108611705B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002004175A (en) * | 2000-06-20 | 2002-01-09 | Toray Ind Inc | Pan based precursor for carbon fiber and method of producing the same |
| CN101250770A (en) * | 2008-03-11 | 2008-08-27 | 东华大学 | Method for manufacturing polyacrylonitrile-based carbon fiber with enganced carbon nano-tube |
| CN101245500A (en) * | 2008-03-25 | 2008-08-20 | 东华大学 | Attapulgite nano-particle modified polyacrylonitrile-based carbon fiber protofilament and production method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607578A (en) * | 2019-09-11 | 2019-12-24 | 大同新成新材料股份有限公司 | Production method of high-strength polyacrylonitrile-based carbon fiber |
| CN114990736A (en) * | 2022-06-13 | 2022-09-02 | 泰州市创新电子有限公司 | PAN-based carbon fiber for display bracket and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108611705B (en) | 2020-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110725024A (en) | Preparation method of fibrous photothermal conversion material | |
| CN104790067A (en) | Nano conductive polymer/graphene composite fiber, and preparation method and application thereof | |
| CN104695040A (en) | Preparation method of high-strength polyacrylonitrile nano-composite fiber | |
| CN108611705A (en) | A kind of preparation method of polyacrylonitrile-radical high-performance carbon fibre | |
| CN111793857A (en) | Carbon fiber surface treatment method | |
| CN113073395A (en) | Graphene modified high-water-absorption fiber and preparation method thereof | |
| JP2009197358A (en) | Flame resistant polymer fiber bundle and method for producing flame resistant fiber bundle | |
| CN109280997A (en) | The high-strength high-modules carbon fibre and preparation method thereof of low degree of graphitization | |
| CN102953151A (en) | Preparation method for polyacrylonitrile-based carbon fiber | |
| CN107653520A (en) | A kind of preparation method of cost degradation polyacrylonitrile-based carbon fibre | |
| CN115948862B (en) | Collagen cellulose fiber cloth and production method thereof | |
| CN109322010A (en) | Utilize the polyacrylonitrile carbon fiber and preparation method thereof of waste polypropylene nitrile fiber preparation | |
| CN110656391B (en) | Composite conductive fabric and manufacturing method thereof | |
| CN109679295B (en) | Method for enhancing composite performance of carbon fiber and resin matrix | |
| CN107287686A (en) | A kind of electrically conductive filament and preparation method thereof | |
| KR20110078306A (en) | Process for producing precursor fiber for acrylonitrile-based carbon fiber and carbon fiber obtained from the precursor fiber | |
| KR101098040B1 (en) | Carbon nanotube composite filament and manufacturing method thereof | |
| CN114941188B (en) | Method for continuously preparing carbon fiber from acrylic fiber | |
| CN108950730B (en) | Spinning method for preparing silicon carbide nanowire/alginic acid composite fiber | |
| CN114474787B (en) | Method for preparing umbrella rib from carbon fiber-based resin composite material | |
| JP2002004175A (en) | Pan based precursor for carbon fiber and method of producing the same | |
| CN109267317A (en) | A kind of high-quality modified silk fiber | |
| CN114395916B (en) | Antigen fibrillated cellulose fiber and preparation method thereof | |
| CN114232120B (en) | Antigen fibrillated cellulose fiber and preparation method thereof | |
| CN107557892A (en) | A kind of method that cyclisation PAN fiber is prepared after PAN spinning solutions are aromatic ring |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20201028 Address after: 236600 East District of Chengguan Town Industrial Park, Taihe County, Fuyang, Anhui Applicant after: ANHUI HAOHUA ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Address before: 236600, Anhui province Fuyang Taihe County double floating town, Shen Shen village committee, No. 14, Zhuang Village Applicant before: Guo Ping |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |