CN108998851A - A kind of low cost halloysite nanotubes coordination plasticizing aramid fiber and preparation method - Google Patents
A kind of low cost halloysite nanotubes coordination plasticizing aramid fiber and preparation method Download PDFInfo
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- CN108998851A CN108998851A CN201810683902.8A CN201810683902A CN108998851A CN 108998851 A CN108998851 A CN 108998851A CN 201810683902 A CN201810683902 A CN 201810683902A CN 108998851 A CN108998851 A CN 108998851A
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- aramid fiber
- halloysite nanotubes
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- coordination plasticizing
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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
- 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
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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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)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of inexpensive halloysite nanotubes coordination plasticizing aramid fiber and preparation methods.The toughening aramid fiber is made by following steps: halloysite nanotubes a, are added in the polycaprolactam of melt shape, toughening material is made；B, toughening material and aramid fiber liquid are infiltrated, spinning solution is made；C, using liquid crystal dry-wet spinning liquid spinning moulding to get halloysite nanotubes coordination plasticizing aramid fiber.The present invention is sufficiently infiltrated by the way that halloysite nanotubes are added with aramid fiber liquid, is formed nanometer and is mixed masterbatch, effectively increases dispersibility of the halloysite nanotubes in resin, the impact resistance toughness of material is improved by coordination plasticizing, and cost is relatively low, application prospect is good.
Description
Technical field
The present invention relates to fibre modification fields, and in particular to the toughening modifying of aramid fiber, more particularly, to it is a kind of it is low at
This halloysite nanotubes coordination plasticizing aramid fiber and preparation method.
Background technique
Polyamide (PA6) also known as nylon 6 are translucent or opaque milky white colored particles, have thermoplasticity, lightweight, toughness
The characteristics such as good, chemicals-resistant and durability are good.Poly(p-phenylene terephthalamide) (PPTA) has molten cause due to molecule chain rigidity
Liquid crystal liquid crystal property easily forms anisotropy state texture under shearing force in the solution, have high-fire resistance, high-tensile and
Initial elastic modulus, high-insulativity and chemical corrosion resistance.PA6/PPTA is a kind of composite material of function admirable, is sent out in recent years
Exhibition and application attract attention.
PA6/PPTA composite material effectively combines the advantage of PPTA and PA6 respectively, and intensity and rigidity be not much higher than
Modified PA6 material, and creep is small, dimensional accuracy is good, thermal stability is high, damping and amortization is excellent and light weight.Its aerospace,
Defence and military, the fields of grade suffer from important purposes.But its disadvantages of there are poor toughness, thus be modified by adding filler
As main technique methods.Halloysite nanotubes are a kind of natural many walls nanotube shape material, excellent in mechanical performance, lamella
It is made of oxygen-octahedron and alumina octahedral, outer wall contains certain hydroxyl, has polarity, but mutual active force is not
By force, easily dispersion, it is cheap.Therefore, it is widely studied and applies as a kind of novel polymer reinforcing material.Its
Distinctive tubular structure can not only effectively improve the rigidity of resin material, moreover it is possible to big under few addition mass fraction
Width improves the impact flexibility of basis material, has broad application prospects in terms of filling-modified PA6/PPTA composite material.
Number of patent application 201610791306.2 discloses a kind of preparation method of anti-aging Fypro, by concave convex rod
Crystalline substance, aluminium borate whisker, white carbon black, wollastonite raphioid fiber, sodium bicarbonate aqueous solution, halloysite nanotubes are mixed, radiate
Afterwards, it is dipped in citric acid solution and heats, disperses, take suspended matter ultrasonication, upper layer suspended matter filtration washing is taken to dry, will
The enhancing age resister and magnesium borate crystal whisker, coupling agent, ultraviolet absorbing agent, light stabilizer, antioxidant stirring and drying arrived, then plus
Enter polyamide stirring, twin-screw melting is kneaded the anti-aging polyamide that extrusion obtains and conventional polyamide is separately dried, and melting is multiple
Conjunction is spun into anti-aging Fypro.The invention adds reinforcing material inorganic crystal whisker, anti-aging materials in polyamide
Wollastonite raphioid fiber, ultraviolet absorbing agent, light stabilizer, antioxidant are made anti-ageing with polyamide resin blends melting
Change the lasting anti-aging Fypro of core-skin type that polyamide is cortex.
Number of patent application 201110043478.9 discloses a kind of halloysite nanotubes enhancing flame retardant type anionic polymerisation Buddhist nun
The preparation method of dragon.The invention makes Ai Luo during caprolactam ring-opening polymerisation using the method for anionic in-situ polymerization
Stone nanotube is dispersed in polymeric matrix, is prepared into enhancing flame retardant type anionic polymerization nylon.Yin made from this method
Ionic polymerization nylon, mechanical property and flame retardant property are significantly improved.
Number of patent application 201710601174.7 discloses a kind of PA6 composite material and preparation method, PA6 composite material
Composed of the following components by weight: PA6 is 80 parts ~ 100 parts；PPTA fiber is 10 parts ~ 16 parts；Compatilizer is 0.1 part ~ 0.3
Part；Nanometer AZO is 4 parts ~ 6 parts；Antioxidant is 0.1 part ~ 0.5 part；Wherein PPTA fiber is the PPTA fiber after alkali process.
PPTA surface polarity key after alkali process increases, and is conducive to improve the compatibility between PPTA and PA6；The work of PPTA fiber
With mainly there is the following: (1) PPTA fiber itself has certain anti-flammability, its addition improves PA6 composite material
Flame retardant property；(2) addition of PPTA fiber improves the physical property of PA6 composite material.
Number of patent application 201610030453.8 discloses a kind of shock resistance scratch-resistant Heat conduction nylon composite material and its system
Preparation Method, using the nylon composite comprising copolymer nylon as resin matrix, with thermally conductive component, fire retardant, antioxidant, coupling agent
And shock resistance scratch-resistant Heat conduction nylon composite material is made by " two step melt-blending processes " in optional scratch resistance liniment.This is thermally conductive
Nylon composite materials toughness and low-temperature impact property are good, and surface hardness is low, scraping and wiping resistance performance is excellent, heating conduction, mechanical property
Can be good with flame retardant property, it can be widely applied to electric power tool shell, battery pack case, LED radiator, automobile-used LED bracket etc. and dissipate
The higher plastic items field of heat request.
It can be seen that PA6/PPTA composite material is there are preparation cost height in the prior art, the problems such as impact resistance is poor, and
Traditional filling-modified technical method, the bad dispersibility of filler in the base limit compound to affect reinforcing effect
The development and application of material.
Summary of the invention
Effectively to solve above-mentioned technical problem, the invention proposes a kind of inexpensive halloysite nanotubes coordination plasticizing aramid fibers
Fiber and preparation method, are remarkably improved the toughness of composite material, and reduce preparation cost.
The specific technical solution of the present invention is as follows:
A kind of preparation method of low cost halloysite nanotubes coordination plasticizing aramid fiber, the toughening aramid fiber is by an angstrom Lip river
The aramid fiber spinning solution of stone nanotube and polycaprolactam coordination plasticizing is made, specific preparation step through liquid crystal dry-wet spinning
Are as follows:
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, condensation, grinding point
It dissipates, toughening material is made；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
Preferably, in the step a, the melt flow rate (MFR) of polycaprolactam is 50 ~ 100g/10min.
Preferably, in the step a, the heating temperature of polycaprolactam is 260 ~ 270 DEG C.
Preferably, in the step a, 92 ~ 95 parts by weight of polycaprolactam, 5 ~ 8 parts by weight of halloysite nanotubes.
Preferably, in the step a, the ultrasonic frequency of ultrasonic disperse is 30 ~ 60kHz, and power is 150 ~ 180W, time
For 60 ~ 90min.
Preferably, in the step b, aramid fiber liquid is obtained by aramid fiber and n,N-dimethylacetamide with mass ratio 1:3 dispersion.
Preferably, in the step b, toughening material 20-30 parts by weight, aramid fiber liquid 70-80 parts by weight.
Preferably, in the step b, infiltrating time is 20 ~ 40min.
Preferably, in the step c, the tension pin angle of liquid crystal dry-wet spinning is 85 ~ 100 degree, spinning speed 200
~ 300m/min, spinning head aperture are 0.2 ~ 0.3mm.
Further provide for a kind of inexpensive halloysite nanotubes coordination plasticizing aramid fiber prepared by the above method.
Halloysite nanotubes are a kind of natural many walls nanotube shape materials, and excellent in mechanical performance, lamella is by silicon oxygen four
Face body and alumina octahedral form, and outer wall contains certain hydroxyl, have polarity, but active force is not strong each other, are easy to point
It dissipates.There is cheap advantage simultaneously, therefore HNTs is a kind of novel polymer filler with broad prospect of application.Its
Distinctive tubular structure can not only effectively improve the rigidity of resin material, moreover it is possible to big under few addition mass fraction
The impact flexibility of width raising basis material.And halloysite nanotubes and PA6 are used for toughening aramid fiber by the present invention simultaneously, are cooperateed with
Effect is obvious, is remarkably improved the impact of material.It can be increased between HNTs and PA6 resin, PPTA three by infiltration simultaneously
Compatibility, achieve the purpose that evenly dispersed.
The invention has the benefit that
Halloysite nanotubes association is made 1. proposing and forming after sufficiently infiltrating halloysite nanotubes using liquid crystal dry-wet spinning
With the method for toughening aramid fiber.
2. the present invention forms nanometer and mixes masterbatch, effectively improve by sufficiently infiltrating aramid fiber liquid and halloysite nanotubes
Dispersibilities of the halloysite nanotubes in resin, are uniformly distributed it, it is ensured that filling-modified effect.
3. the present invention acts synergistically by the way that halloysite nanotubes and polycaprolactam are added, make poly- paraphenylene terephthalamide to benzene two
Amine coordination plasticizing significantly improves the impact resistance of composite material, and effectively controls the preparation cost of composite material.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, and condensation is ground to
Toughening material is made less than 10 microns in partial size；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
The heating temperature of polycaprolactam is 260 DEG C.
In step a, 95 parts by weight of polycaprolactam, 5 parts by weight of halloysite nanotubes.The ultrasonic wave frequency of ultrasonic disperse
Rate is 60kHz, power 150W, time 90min.
In step b, 20 parts by weight of toughening material, 80 parts by weight of aramid fiber liquid；Aramid fiber liquid is by aramid fiber and DMAC N,N' dimethyl acetamide
It is obtained with mass ratio 1:3 dispersion.Infiltrating time is 40min.
The tension pin angle of liquid crystal dry-wet spinning is 85 degree, and spinning speed 300m/min, spinning head aperture is
0.3mm。
Embodiment 2
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, and condensation is ground to
Toughening material is made less than 10 microns in partial size；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
The heating temperature of polycaprolactam is 260 ~ 270 DEG C.
In step a, 92 parts by weight of polycaprolactam, 8 parts by weight of halloysite nanotubes.The ultrasonic wave frequency of ultrasonic disperse
Rate is 30kHz, power 180W, time 60min.
In step b, 30 parts by weight of toughening material, 70 parts by weight of aramid fiber liquid；Aramid fiber liquid is by aramid fiber and DMAC N,N' dimethyl acetamide
It is obtained with mass ratio 1:3 dispersion.Infiltrating time is 30min.
The tension pin angle of liquid crystal dry-wet spinning is 100 degree, and spinning speed 200m/min, spinning head aperture is
0.2mm。
Embodiment 3
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, and condensation is ground to
Toughening material is made less than 10 microns in partial size；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
The heating temperature of polycaprolactam is 265 DEG C.
In step a, 93 parts by weight of polycaprolactam, 7 parts by weight of halloysite nanotubes.The ultrasonic wave frequency of ultrasonic disperse
Rate is 40kHz, power 160W, time 70min.
In step b, 25 parts by weight of toughening material, 75 parts by weight of aramid fiber liquid；Aramid fiber liquid is by aramid fiber and DMAC N,N' dimethyl acetamide
It is obtained with mass ratio 1:3 dispersion.Infiltrating time is 30min.
The tension pin angle of liquid crystal dry-wet spinning is 90 degree, and spinning speed 250m/min, spinning head aperture is
0.25mm。
Embodiment 4
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, and condensation is ground to
Toughening material is made less than 10 microns in partial size；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
The heating temperature of polycaprolactam is 270 DEG C.
In step a, 92 parts by weight of polycaprolactam, 8 parts by weight of halloysite nanotubes.The ultrasonic wave frequency of ultrasonic disperse
Rate is 40kHz, power 170W, time 80min.
In step b, 20 parts by weight of toughening material, 80 parts by weight of aramid fiber liquid；Aramid fiber liquid is by aramid fiber and DMAC N,N' dimethyl acetamide
It is obtained with mass ratio 1:3 dispersion.Infiltrating time is 40min.
The tension pin angle of liquid crystal dry-wet spinning is 90 degree, and spinning speed 300m/min, spinning head aperture is
0.2mm。
Embodiment 5
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, and condensation is ground to
Toughening material is made less than 10 microns in partial size；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
The heating temperature of polycaprolactam is 260 DEG C.
In step a, 95 parts by weight of polycaprolactam, 5 parts by weight of halloysite nanotubes.The ultrasonic wave frequency of ultrasonic disperse
Rate is 50kHz, power 160W, time 70min.
In step b, 28 parts by weight of toughening material, 72 parts by weight of aramid fiber liquid；Aramid fiber liquid is by aramid fiber and DMAC N,N' dimethyl acetamide
It is obtained with mass ratio 1:3 dispersion.Infiltrating time is 25min.
The tension pin angle of liquid crystal dry-wet spinning is 95 degree, and spinning speed 250m/min, spinning head aperture is
0.25mm。
Comparative example 1
A, polycaprolactam is ground to partial size less than 10 microns, toughening material is made；
B, toughening material made from step a, halloysite nanotubes and aramid fiber liquid are sufficiently infiltrated, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
In step b, 25 parts by weight of toughening material, 3 parts by weight of halloysite nanotubes, 72 parts by weight of aramid fiber liquid；Aramid fiber liquid is by virtue
Synthetic fibre and DMAC N,N' dimethyl acetamide are obtained with mass ratio 1:3 dispersion.Infiltrating time is 25min.
The tension pin angle of liquid crystal dry-wet spinning is 95 degree, and spinning speed 250m/min, spinning head aperture is
0.25mm。
Toughening aramid fiber made from above-described embodiment 1 ~ 5 and comparative example 1, tests its tensile strength, stretch modulus and stretches
Long rate, the results are shown in Table 1.
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Unmodified aramid fiber |
| Tensile strength (MPa) | 2970 | 3066 | 2875 | 2900 | 2793 | 2620 | 2541 |
| Stretch modulus (MPa) | 97530 | 98200 | 95341 | 97885 | 90520 | 86510 | 71240 |
| Elongation (%) | 12.5 | 17.1 | 15.3 | 16.2 | 17.0 | 10.2 | 3.1 |
Claims (10)
1. a kind of preparation method of low cost halloysite nanotubes coordination plasticizing aramid fiber, it is characterised in that: the toughening virtue
Synthetic fibre fiber is to be made by the aramid fiber spinning solution of halloysite nanotubes and polycaprolactam coordination plasticizing through liquid crystal dry-wet spinning, tool
The preparation step of body are as follows:
A, polycaprolactam is heated to melt shape, halloysite nanotubes is added, ultrasonic disperse is uniform, condensation, grinding point
It dissipates, toughening material is made；
B, toughening material made from step a is sufficiently infiltrated with aramid fiber liquid, spinning solution is made；
C, the spinning solution spinning moulding of step b is made by halloysite nanotubes coordination plasticizing aramid fiber using liquid crystal wet-dry change.
2. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step a, the melt flow rate (MFR) of polycaprolactam is 50 ~ 100g/10min.
3. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step a, the heating temperature of polycaprolactam is 260 ~ 270 DEG C.
4. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step a, 92 ~ 95 parts by weight of polycaprolactam, 5 ~ 8 parts by weight of halloysite nanotubes.
5. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step a, the ultrasonic frequency of ultrasonic disperse is 30 ~ 60kHz, and power is 150 ~ 180W, the time is 60 ~
90min。
6. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step b, aramid fiber liquid is obtained by aramid fiber and n,N-dimethylacetamide with mass ratio 1:3 dispersion.
7. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step b, toughening material 20-30 parts by weight, aramid fiber liquid 70-80 parts by weight.
8. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step b, infiltrating time is 20 ~ 40min.
9. a kind of preparation method of inexpensive halloysite nanotubes coordination plasticizing aramid fiber according to claim 1, special
Sign is: in the step c, the tension pin angle of liquid crystal dry-wet spinning is 85 ~ 100 degree, and spinning speed is 200 ~ 300m/
Min, spinning head aperture are 0.2 ~ 0.3mm.
10. a kind of inexpensive halloysite nanotubes coordination plasticizing aramid fiber that any one of claim 1 ~ 9 the method is prepared
Fiber.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811423A (en) * | 2018-12-25 | 2019-05-28 | 中国纺织科学研究院有限公司 | The production method and the functional polyamide fiber of continuous polymerization fused mass directly spinning functional polyamide fiber |
| CN113777835A (en) * | 2021-08-19 | 2021-12-10 | 华南师范大学 | Electric response light modulation device and preparation method and application thereof |
| CN115364682A (en) * | 2022-08-19 | 2022-11-22 | 浙江工业大学 | Preparation method of nano heterostructure composite membrane and application of nano heterostructure composite membrane in dye desalination |
-
2018
- 2018-06-28 CN CN201810683902.8A patent/CN108998851A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811423A (en) * | 2018-12-25 | 2019-05-28 | 中国纺织科学研究院有限公司 | The production method and the functional polyamide fiber of continuous polymerization fused mass directly spinning functional polyamide fiber |
| CN109811423B (en) * | 2018-12-25 | 2021-10-26 | 中国纺织科学研究院有限公司 | Production method of continuous polymerization melt direct spinning functional polyamide fiber and functional polyamide fiber |
| CN113777835A (en) * | 2021-08-19 | 2021-12-10 | 华南师范大学 | Electric response light modulation device and preparation method and application thereof |
| CN113777835B (en) * | 2021-08-19 | 2024-04-30 | 华南师范大学 | Electric response dimming device and preparation method and application thereof |
| CN115364682A (en) * | 2022-08-19 | 2022-11-22 | 浙江工业大学 | Preparation method of nano heterostructure composite membrane and application of nano heterostructure composite membrane in dye desalination |
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Application publication date: 20181214 |