CN106245328A - A kind of aramid fiber surface particle modified method of irradiation grafting nanometer polymer - Google Patents
A kind of aramid fiber surface particle modified method of irradiation grafting nanometer polymer Download PDFInfo
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- CN106245328A CN106245328A CN201610610192.7A CN201610610192A CN106245328A CN 106245328 A CN106245328 A CN 106245328A CN 201610610192 A CN201610610192 A CN 201610610192A CN 106245328 A CN106245328 A CN 106245328A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/34—Polyamides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
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- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/02—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using organic solvents
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention discloses a kind of aramid fiber surface particle modified method of irradiation grafting nanometer polymer, described method includes that fiber surface cleans and is dried, fiber processes two steps with acrylonitrile monemer co-irradiation grafting.The present invention utilizes gamma-rays mutual radiation to process aramid fiber and acrylonitrile monemer, causes Raolical polymerizable by irradiation at fiber surface, at fiber surface graft polypropylene nitrile macromole.Under effect of irradiation, ionizing radiation and fiber molecule interact and energy transfer occur, and fiber molecule produces ion pair after absorbing energy and excites molecule, and fiber molecule can be through forming the process of free radical in this process.The acrylonitrile monemer generation Raolical polymerizable that the free radical capture formed is free, thus at fiber surface graft polypropylene nitrile macromole.Present invention process is simple, efficient, and reaction condition is gentle, and fiber treatment amount can control.
Description
Technical field
The present invention relates to a kind of aramid fiber method of modifying, particularly relate to a kind of aramid fiber surface irradiation grafting modification side
Method.
Background technology
High performance resin based composites has the advantages such as specific strength is high, specific modulus is big, high temperature resistant, corrosion-resistant, as weight
The defense strategy goods and materials wanted, are widely used in numerous national defense industry such as Aero-Space, weaponry field.Wherein aramid fiber is fine
Tie up little with its density, intensity is high, modulus is big, bigger than hardness, corrosion-resistant, wear-resistant, Heat stability is good, low conductance etc. are many excellent
Characteristic, the strategic continent in the various aircraft being widely used in space flight and aviation as high-performance reinforcing material, defence and military
On the guided missile of border.But aramid fiber construction unit Middle molecule chain link is that planar rigidity stretches shape, and intramolecular does not exist unformed area,
Make fiber have orientation and high-crystallinity, thus aramid fiber surface present bigger inertia, be unfavorable for aramid fiber with
Cohering of the matrix such as resin and rubber, causes being formed between aramid fiber and matrix boundary defect.Simultaneously because aramid fiber divides
There is a large amount of aromatic ring in minor structure, molecule interchain hydrogen bonded is weak, and the especially adhesion between cortex and sandwich layer is more weak,
Cause the 20% of fiber transverse strength only about longitudinal strength, limit the performance of composite property.Therefore, in order to improve
Aramid fiber and the bond strength of resin matrix, give full play to the excellent properties of aramid fiber, aramid fiber need to be carried out surface
Modification, introduces active group, improves surface activity, promotes fiber to form chemical bonds with resin matrix, makes stress energy
Enough uniformly transfer in composite inner.
Domestic aramid fiber F3 fiber quickly grows in application, has expanded to F3A fiber type, and its intensity level can reach
The level of Armos fiber, but its apparent condition is excessively poor, especially aramid fiber 3A fiber surface and the interface bonding energy of resin matrix
Power is well below Armos fiber, it is impossible to apply in corresponding engine model, therefore in the urgent need to it is carried out through engineering approaches
Surface modification, the interfacial combined function making housing is strong, and fibre strength coefficient can be not fully exerted, thus promotes China's weapon
The development of equipment.
At present aramid fiber modification processing method mainly has chemic modified method, Cement Composite Treated by Plasma, face coat method, ultrasonic
Ripple process and high-energy irradiation process etc..
Chemical modification is processed aramid fiber and is mainly etched or grafting at aramid fiber surface by chemical treatment method
Polar group or reactive active group, improve fiber surface activity so that occurs chemistry anti-between fiber and resin matrix
The interface interaction of covalent bond, reinforcing fiber and resin should be generated.At present frequently with method have fluorination treatment, chlorosulfonic acid process with
And friedel-craft reaction etc..Although the effectiveness comparison that chemical method processes aramid fiber is obvious, but response speed is fast, wayward,
Easily damage fiber, reduce the tensile property of material.
Plasma is the most well accepted fiber surface activity that is effectively improved, and improves composite material interface adhesive strength
Method, use this technology that the oxygen in air and nitrogen element oxide may be made to be incorporated into fiber surface, or in plasma
Introduce reactant gas etc., the polar group number of fiber surface can be increased, improve surface polarity, contribute to fiber hygroscopic
Improve, finally the cohesive of fiber with resin is had very great help.But modified aramid fiber strengthens the destruction of composite
Still destroying based on fiber core-skin, fibre strength mobilization factor is low.
Ultrasonic Treatment, mainly by ultrasonic air cavitation, forces resin and fiber to form good boundary moisture,
And ul-trasonic irradiation produces impact to fiber surface chemical composition.But ultrasonic Treatment is higher to producing equipment requirements,
And be not clearly to fiber surface activation effect.
Face coat method mainly grows nano wire at fiber surface, and deposition of rare-earth or absorption dopamine etc. reach surface
Modified purpose, but it is formed without effective chemical bond between graft and fiber, composite material interface performance improvement degree
It not the highest.
High-energy ray processes and utilizes high-energy gamma-rays photon to act on fiber surface and inside, makes surface active, produces and lives
Property group, thus the chemical bond strong with resin formation, improve two-phase interface bonding strength.Irradiation grafting skill can also be used simultaneously
Art increases the quantity of fiber surface polar group, improves the wettability of aramid fiber, adhesiveness, improves state of interface.The highest
Can have various features and advantage by irradiation technique, it has green, strong penetrance, it is adaptable to the process of whole group's fiber.
Summary of the invention
In order to solve that aramid fiber surface is smooth, chemism is low, fiber is weak with resin matrix Interaction Force asks
Topic, the invention provides a kind of aramid fiber surface particle modified method of irradiation grafting nanometer polymer.
It is an object of the invention to be achieved through the following technical solutions:
A kind of aramid fiber surface particle modified method of irradiation grafting nanometer polymer, cleans including fiber surface and dry, fine
Dimension processes two steps with acrylonitrile monemer co-irradiation grafting, is embodied as step as follows:
One, aramid fiber surface cleans and is dried:
(1) aramid fiber bundle is put in autoclave, seal, after evacuation, injected acetone by charging aperture wherein, make
Fiber submerges in acetone, closes charging aperture, reactor puts into baking oven, controls temperature at 60 ~ 80 DEG C, reacts 22 ~ 26 hours, instead
After having answered, take out fiber, with acetone rinsing 5 ~ 10 minutes；
(2) will take out through the aramid fiber that (1) step process is crossed, be placed in 70 ~ 80 DEG C of baking ovens and be dried 2 ~ 4h；
Two, fiber processes with acrylonitrile monemer co-irradiation grafting:
(1) dried aramid fiber is put in glass jar, inject acrylonitrile monemer and cyclohexane solvent, make fiber not have completely
Entering in solution, closed glass tank, the volume ratio of described acrylonitrile monemer and cyclohexane solvent is 1 ~ 4:50；
(2) glass jar that step (1) obtains is positioned over60Under Co irradiation bomb, under normal temperature and pressure conditions, carry out gamma-ray irradiation
Process, control irradiation dose in 200 ~ 1000kGy；
(3) fiber after step (2) being processed took out, with acetone rinsing 5 ~ 10 minutes；
(4) after step (3) being processed, fiber is positioned in ultrasonic cleaner, cleans 5 ~ 10 minutes；
(5) aramid fiber that step (4) processed takes out, and with deionized water rinsing 5 ~ 10 minutes, is placed in 70 ~ 80 DEG C of baking ovens
It is dried 2 ~ 4h.
Said method is applicable not only to domestic aramid fiber 3A, is also applied for other kinds of aramid fiber and organic synthesis is fine
Dimension.
Owing to gamma-rays has higher penetrance and energy, the present invention utilizes gamma-rays mutual radiation to process aramid fiber
(as a example by domestic fiber F-3A) and acrylonitrile monemer, cause Raolical polymerizable by irradiation at fiber surface, at fiber
Surface grafting polyacrylonitrile macromole.Under effect of irradiation, ionizing radiation and fiber molecule interact and energy transfer occur, fine
Producing ion pair after dimension molecule absorption energy and excite molecule, fiber molecule can be through forming the mistake of free radical in this process
Journey.The acrylonitrile monemer generation Raolical polymerizable that the free radical capture formed is free, thus it is grafted poly-third at fiber surface
Alkene nitrile macromole.Graft reaction schematic diagram is as shown in Figure 1.
Compared to prior art, present invention have the advantage that
1, due to maximum energy criterion, polyacrylonitrile macromolecular mass is polymerized to size and is grafted on fibre at the nano-particle of about 200nm
Dimension table face, forms the nano-particle of dimensionally stable.Polyacrylonitrile nano granule can improve fiber surface roughness, increases fiber
Specific surface area, therefore this processing method can effectively promote to form strong machinery riveted between fiber and resin matrix, improves
The interface performance of composite.
2, gamma-ray irradiation can improve " skin-core " structure of aramid fiber simultaneously, promotes fibrous inside molecule to cross-link, carries
High microsteping hot strength.
3, present invention process is simple, efficient, and reaction condition is gentle, and fiber treatment amount can control.
Accompanying drawing explanation
Fig. 1 is aramid fiber surface graft reaction schematic diagram；
Fig. 2 is SEM surface topography before and after aramid fiber grafting；
Fig. 3 is aramid fiber graft reaction infrared spectrogram；
Fig. 4 is composite material interface shear strength before and after aramid fiber grafting；
Fig. 5 is monofilament tensile strength before and after aramid fiber grafting.
Detailed description of the invention
Below in conjunction with the accompanying drawings technical scheme is further described, but is not limited thereto, every to this
Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should contain
In protection scope of the present invention.
Detailed description of the invention one: present embodiments provide for a kind of aramid fiber surface irradiation grafting nanometer polymer particle
Method of modifying, cleans including fiber surface and is dried, fiber and acrylonitrile monemer co-irradiation grafting process two steps, specifically real
Execute step as follows:
One, aramid fiber surface cleans and is dried:
(1) aramid fiber bundle is put in autoclave, seal, after evacuation, injected acetone by charging aperture wherein, make
Fiber submerges in acetone, closes charging aperture, reactor puts into baking oven, controls temperature at 60 ~ 80 DEG C, reacts 22 ~ 26 hours, instead
After having answered, take out fiber, with acetone rinsing 5 ~ 10 minutes；
(2) will take out through the aramid fiber that (1) step process is crossed, be placed in 70 ~ 80 DEG C of baking ovens and be dried 2 ~ 4h；
Two, fiber processes with acrylonitrile monemer co-irradiation grafting:
(1) dried aramid fiber is put in glass jar, inject acrylonitrile monemer and cyclohexane solvent, make fiber not have completely
Entering in solution, closed glass tank, the volume ratio of described acrylonitrile monemer and cyclohexane solvent is 1 ~ 4:50；
(2) glass jar that step (1) obtains is positioned over60Under Co irradiation bomb, under normal temperature and pressure conditions, carry out gamma-ray irradiation
Process, control irradiation dose in 200 ~ 1000kGy；
(3) fiber after step (2) being processed took out, with acetone rinsing 5 ~ 10 minutes；
(4) after step (3) being processed, fiber is positioned in ultrasonic cleaner, cleans 5 ~ 10 minutes；
(5) aramid fiber that step (4) processed takes out, and with deionized water rinsing 5 ~ 10 minutes, is placed in 70 ~ 80 DEG C of baking ovens
It is dried 2 ~ 4h.
Fig. 2 is fiber surface morphology change before and after grafting, can be seen that untreated aramid fiber surface light from Fig. 2 (a)
Sliding smooth, comprise only a small amount of groove.Through grafting process after from fiber surface uniform graft PAN granule (Fig. 2 b, c), and
Can be seen that PAN particle size size is about about 200nm from Fig. 2 (d).
Fig. 3 is the infrared spectrogram of aramid fiber before and after grafting.As can be seen from Figure 3, after grafting processes, aramid fiber is fine
Dimension is at 2925cm-1There is flexible (antisymmetry) vibration peak of methylene in place, at 2859cm-1There is the flexible (right of methylene in place
Claim) vibration peak.At 2240cm-1There is the stretching vibration peak of cyano group in place.This explanation fiber surface is successfully grafted PAN.
Table 1 is the change of fiber surface constituent content before and after grafting, and after grafting processes, fiber surface C, N element contain
Amount substantially increases, and O constituent content substantially reduces.
Table 2 is fabric contact angle and the change of surface energy before and after grafting, and after grafting processes, fiber is in water and diiodo-first
Contact angle in alkane substantially reduces, and surface can be improved to 56.25mN/m by 42.05mN/m, and the wetting property of fiber is improved.
Fig. 4 is fibre single thread hot strength change before and after grafting.Figure 4, it can be seen that the stretching of untreated aramid fiber
Intensity is 4.801GPa, and after grafting processes, fibre strength improves to 5.053GPa, improves 5.25%.
Fig. 5 is the change of fiber interface shear strength before and after grafting.As can be seen from Figure 5, untreated aramid fiber circle
Face shear strength is only 36.33MPa, and after grafting processes, fiber interface shear strength improves to 58.32MPa, improves
60.53%, fiber interface performance is obviously improved.
Before and after table 1 aramid fiber processes, constituent content (at.%) changes
Contact angle and surface energy before and after the process of table 2 aramid fiber
Detailed description of the invention two: present embodiments provide for a kind of aramid fiber surface irradiation grafting nanometer polymer particle modified
Method, cleans including fiber surface and is dried, fiber and acrylonitrile monemer co-irradiation grafting process two steps, are embodied as step
Rapid as follows:
One, aramid fiber surface cleans and is dried:
(1) aramid fiber bundle is put in autoclave, seal, after evacuation, injected acetone by charging aperture wherein, make
Fiber submerges in acetone, closes charging aperture, and reactor is put into baking oven, and control temperature, at 70 DEG C, is reacted 24 hours, reacted
After, take out fiber, with acetone rinsing 5 minutes；
(2) will take out through the aramid fiber that (1) step process is crossed, be placed in 75 DEG C of baking ovens and be dried 3h；
Two, fiber processes with acrylonitrile monemer co-irradiation grafting:
(1) dried aramid fiber is put in glass jar, inject acrylonitrile monemer and cyclohexane solvent, make fiber not have completely
Entering in solution, closed glass tank, the volume ratio of described acrylonitrile monemer and cyclohexane solvent is 1:50；
(2) glass jar that step (1) obtains is positioned over60Under Co irradiation bomb, under normal temperature and pressure conditions, carry out gamma-ray irradiation
Process, control irradiation dose at 500kGy；
(3) fiber after step (2) being processed took out, with acetone rinsing 5 minutes；
(4) after step (3) being processed, fiber is positioned in ultrasonic cleaner, cleans 5 minutes；
(5) aramid fiber that step (4) processed takes out, and with deionized water rinsing 5 minutes, is placed in 75 DEG C of baking ovens and is dried
3h。
Detailed description of the invention three: present embodiments provide for a kind of aramid fiber surface irradiation grafting nanometer polymer particle
Method of modifying, cleans including fiber surface and is dried, fiber and acrylonitrile monemer co-irradiation grafting process two steps, specifically real
Execute step as follows:
One, aramid fiber surface cleans and is dried:
(1) aramid fiber bundle is put in autoclave, seal, after evacuation, injected acetone by charging aperture wherein, make
Fiber submerges in acetone, closes charging aperture, and reactor is put into baking oven, and control temperature, at 80 DEG C, is reacted 24 hours, reacted
After, take out fiber, with acetone rinsing 10 minutes；
(2) will take out through the aramid fiber that (1) step process is crossed, be placed in 70 DEG C of baking ovens and be dried 4h；
Two, fiber processes with acrylonitrile monemer co-irradiation grafting:
(1) dried aramid fiber is put in glass jar, inject acrylonitrile monemer and cyclohexane solvent, make fiber not have completely
Entering in solution, closed glass tank, the volume ratio of described acrylonitrile monemer and cyclohexane solvent is 4:50；
(2) glass jar that step (1) obtains is positioned over60Under Co irradiation bomb, under normal temperature and pressure conditions, carry out gamma-ray irradiation
Process, control irradiation dose at 800kGy；
(3) fiber after step (2) being processed took out, with acetone rinsing 10 minutes；
(4) after step (3) being processed, fiber is positioned in ultrasonic cleaner, cleans 10 minutes；
(5) aramid fiber that step (4) processed takes out, and with deionized water rinsing 10 minutes, is placed in 80 DEG C of baking ovens and is dried
2h。
Claims (10)
1. the aramid fiber surface particle modified method of irradiation grafting nanometer polymer, it is characterised in that described method step is such as
Under:
One, aramid fiber surface cleans and is dried；
Two, fiber processes with acrylonitrile monemer co-irradiation grafting:
(1) dried aramid fiber is put in glass jar, inject acrylonitrile monemer and cyclohexane solvent, make fiber not have completely
Enter in solution, closed glass tank；
(2) glass jar that step (1) obtains is positioned over60Under Co irradiation bomb, under normal temperature and pressure conditions, carry out gamma-ray irradiation
Process；
(3) fiber after step (2) being processed takes out, and uses acetone rinsing；
(4) after step (3) being processed, fiber is positioned in ultrasonic cleaner cleaning；
(5) aramid fiber step (4) processed takes out, and with deionized water rinsing, is placed in baking oven and is dried.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In specifically comprising the following steps that of described step one
(1) aramid fiber bundle is put in autoclave, seal, after evacuation, injected acetone by charging aperture wherein, make
Fiber submerges in acetone, closes charging aperture, reactor is put into baking oven and reacts, and after having reacted, takes out fiber, rushes with acetone
Wash；
(2) will take out through the aramid fiber that (1) step process is crossed, be placed in baking oven and be dried.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 2, its feature exists
Being 60 ~ 80 DEG C in described reaction temperature, the time is 22 ~ 26 hours.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 2, its feature exists
Being 5 ~ 10 minutes in the described acetone rinsing time, baking temperature is 70 ~ 80 DEG C, and drying time is 2 ~ 4h.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, the volume ratio of acrylonitrile monemer and cyclohexane solvent is 1 ~ 4:50.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, control irradiation dose in 200 ~ 1000kGy.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, the acetone rinsing time is 5 ~ 10 minutes.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, the ultrasonic waves for cleaning time is 5 ~ 10 minutes.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, the deionized water rinsing time is 5 ~ 10 minutes.
The aramid fiber surface particle modified method of irradiation grafting nanometer polymer the most according to claim 1, its feature exists
In described step 2, baking temperature is 70 ~ 80 DEG C, and the time is 2 ~ 4h.
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Cited By (1)
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| CN107313242A (en) * | 2017-07-27 | 2017-11-03 | 贵州大学 | The application of the method for aramid fiber surface modification and products thereof |
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| CN107313242A (en) * | 2017-07-27 | 2017-11-03 | 贵州大学 | The application of the method for aramid fiber surface modification and products thereof |
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Application publication date: 20161221 |