CN107868989A - A kind of preparation method of high resiliency fire-retardant polyamide fibre - Google Patents
A kind of preparation method of high resiliency fire-retardant polyamide fibre Download PDFInfo
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- CN107868989A CN107868989A CN201711200974.4A CN201711200974A CN107868989A CN 107868989 A CN107868989 A CN 107868989A CN 201711200974 A CN201711200974 A CN 201711200974A CN 107868989 A CN107868989 A CN 107868989A
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- graphene oxide
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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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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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Abstract
The invention discloses a kind of preparation method of high resiliency fire-retardant polyamide fibre, belong to nylon fibre production field, comprise the following steps：Take two-dimentional boron nitride to be placed in ball mill, add pentaerythrite or derivatives thereof, taken out after ball milling, dried in baking oven；Graphene oxide is disperseed to be ultrasonically treated in ethanol, obtains graphene oxide dispersion；Two-dimentional boron nitride composite is added in graphene oxide dispersion, mechanical agitation is evaporated to mixture after thick, to dry, and obtains graphene oxide and two-dimentional boron nitride blend composition；By slices of caprone and blend composition input screw extruder melting mixing extrusion, it is granulated；Master batch is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.The beneficial effects of the invention are as follows：Using the synergy of graphene oxide and boron nitride, the problems such as graphene oxide sp2 structures are destroyed, are difficult to combine between two-dimentional boron nitride and macromolecular fibre is successfully overcome, obtained nylon fibre has excellent elasticity and fire resistance.
Description
Technical field
The present invention relates to nylon fibre production field, more particularly to a kind of preparation method of high resiliency fire-retardant polyamide fibre.
Background technology
With the fast development of textile technology, the flame retardant textiles in China also obtain significant progress in recent years, and be in
Reveal different development trends.Current most fire resistance fibres or fabric only have anti-flaming function, can not meet the spy of some departments
It is different to require, as flame-retardant water-repellent, it is fire-retardant refuse oil, flame-retardant and anti-static, development flame-retardant multifunctional product is imperative.Graphene
(Graphene) be it is a kind of by carbon atom form hexagon be in honeycomb-patterned ordered arrangement two-dimensional material.Preferable single-layer graphene
Excellent properties mainly include：Up to 2630m2·g-1Theoretical specific surface area, 97.7% optical transmittance, up to 5300W/
(mK) thermal conductivity factor, more than 15000cm2/ (Vs) normal temperature electron mobility, as little as 10-6Ω cm resistivity.This
A little unique properties cause graphene to play great work in foregoing flame-retardant water-repellent, fire-retardant oil, flame-retardant and anti-static etc. refused
With.Graphene oxide to graphite by being aoxidized and stripping obtains graphene oxide.In the process, substantial amounts of oxidant and
Intercalator is used so that graphene sp2 structures are destroyed, and its intrinsic properties is also difficult to maintain.Fire-retardant and heat conduction is also largely lost
Lose, this causes effect of the graphene oxide in fire-retardant use to give a discount.But graphene oxide has on the top layer of graphene
Carboxyl, epoxy radicals, hydroxyl etc. reduce its surface energy, equal energy between energy and organic polymer and inorganic filler containing base group modification
There is good interfacial structure.So urgent need one kind effectively can keep graphene property and and can has very with organic polymer
The method of good adhesion.Two-dimentional boron nitride, it is commonly called as " white graphite alkene ".Compared to graphene, two-dimentional boron nitride has high heat
Lead and numerous excellent physical chemistry such as the mechanical property of high intensity, higher hot and chemical stability, deep-UV light-emitting performance
Property.
Such as a kind of Graphene fire retardant preparation methods with anti-static function of Chinese patent CN103275395A and its should
With the Graphene fire retardant component with anti-static function is：50~100 parts of graphene oxide, 100 parts of fire retardant, dispersant
10~20 parts, 0.1~0.2 part of process auxiliaries.The advantages of patent is that the Graphene fire retardant can play antistatic and flame-retardant
Composite effect, can be widely used for preparing thermoplastic polymer composite, process is simple, without dust pollution, product quality
It is stable, it is especially suitable for anlistatig occasion.
And for example Chinese patent CN102963046A discloses a kind of nanometer clothing material, is made up of trilaminate material, is respectively
Layer of nanomaterial, common material layer and articulamentum, common bed of cloth are located at nanometer clothing material superstructure：The nano material
Layer is connected with common bed of cloth by the articulamentum of centre.The advantages of patent, is healthy warming and has Water-proof and oil-proof, prevents
Dirty, mould proof effect, but be disadvantageous in that the harmful substance such as fine particle, bacterial virus in external environment can not be played very well
Protective action.
The content of the invention
To overcome, during oxidation and stripping, the use of oxidant and intercalator makes graphene oxide in the prior art
Obtain graphene sp2 structures to destroy, its intrinsic properties is also difficult to maintain, and fire-retardant and heat conduction is also largely lost, and graphene oxide exists
The problems such as effect during fire-retardant use is given a discount, the invention provides a kind of preparation method of high resiliency fire-retardant polyamide fibre, utilizes oxygen
The synergy of graphite alkene and two-dimentional boron nitride, obtained polyamide fibre have high resiliency and fire-retardant effect concurrently, comprised the following steps that：
Step 1：Take the two-dimentional boron nitride of 1~10 parts by weight to be placed in ball mill, add the pentaerythrite of 1~5 parts by weight
Or derivatives thereof, taken out after 4~8h of ball milling, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite；
Step 2：Graphene oxide is scattered in ethanol, 15~60min is ultrasonically treated, graphene oxide is obtained and disperses
Liquid；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is (10~1):1, the mechanical agitation at 80~90 DEG C
Mixture is evaporated to after thick, to be dried 12 hours at 50~60 DEG C, obtains graphene oxide and the blending of two-dimentional boron nitride
Material；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Graphene oxide and two-dimentional boron nitride are added in fire resistance fibre simultaneously, utilize the height point of graphene oxide
Property and the wearability and stability of two-dimentional boron nitride are dissipated, has reached and has improved flame retardant effect while also with wear-resisting, far infrared etc.
Characteristic so that the effect of obtained polyamide fibre has warming, health care, promotes people's body-internal-circulation and improve body immunity.Aoxidize stone
Black alkene has carboxyl, epoxy radicals on the top layer of graphene, and hydroxyl etc. contains base group modification, can there is preferable parent with macromolecular fibre
And power；Two-dimentional boron nitride, lubricant and fire proofing are often used as, but because its chemical inertness is difficult to add it to high score
In son.Graphene oxide and two-dimentional boron nitride are added in fire resistance fibre by the present invention simultaneously, and are made by reasonably arranging in pairs or groups
With the synergy using graphene oxide and two-dimentional boron nitride reaches excellent flame retardant effect.
Further, the two-dimentional boron nitride is six side's two dimension boron nitride, and piece footpath is 50nm~5 μm.
Further, the pentaerythrite and its derivative are pentaerythrite, the fatty acid ester of pentaerythrite, pentaerythrite ring
Oxygen derivative or dipentaerythritol.
Further, ball mill described in step 1 is tube mill, in bar type ball mill or horizontal ball mill.
Further, the rotating speed of ball mill described in step 1 is 200~400rpm, and ratio of grinding media to material is (60~80)：1.
Further, graphene oxide described in step 2 is with Brodie methods, Staudenmaier methods and Hummers legal systems
Standby graphene oxide.
Further, the concentration of graphene oxide is 5~20mg/ml in graphene oxide dispersion described in step 2.
Further, the percentage by weight that slices of caprone described in step 4 mixes with blend composition is (80~99)：(20~
1)。
Further, screw extruder described in step 4 is provided with seven melt regions from front to back, and each section of temperature control exists
160~200 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) using the synergy of graphene oxide and boron nitride, successfully overcome graphene oxide sp2 structures destroy,
The problems such as being difficult to combine between two-dimentional boron nitride and macromolecular fibre, reasonably matched by two kinds of components so that be made fire-retardant
Fiber has high resiliency and fire-retardant effect concurrently, and graphene and two-dimentional boron nitride all have excellent mechanical performance, and it adds
Entering makes fire resistance fibre more resistant；
(2) nylon fibre, work are prepared using ball mill ball milling, screw extruder extruding pelletization, melt spinning machine spinning etc.
Skill is simple to operation, and cost is cheap, high financial profit, is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the preferably scanning electron microscope (SEM) photograph of graphene oxide and two-dimentional boron nitride blend composition of the invention；
Fig. 2 is preferably fire-retardant polyamide fibre fiber scanning electron microscope (SEM) photograph of the invention.
Embodiment
With reference to embodiments and accompanying drawing, the present invention will be described in further detail.It is it should be appreciated that described herein
Specific embodiment only to explain the present invention, is not intended to limit the present invention.
Present embodiments provide for a kind of preparation method of high resiliency fire-retardant polyamide fibre, is nitrogenized using graphene oxide and two dimension
The synergy of boron, obtained polyamide fibre have high resiliency and fire-retardant effect concurrently, comprised the following steps that：
Step 1：Take the two-dimentional boron nitride of 1~10 parts by weight to be placed in ball mill, add the pentaerythrite of 1~5 parts by weight
Or derivatives thereof, taken out after 4~8h of ball milling, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite；
Step 2：Graphene oxide is scattered in ethanol, 15~60min is ultrasonically treated, graphene oxide is obtained and disperses
Liquid；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is (10~1):1, the mechanical agitation at 80~90 DEG C
Mixture is evaporated to after thick, to be dried 12 hours at 50~60 DEG C, obtains graphene oxide and the blending of two-dimentional boron nitride
Material, it is as shown in Figure 1 graphene oxide and the scanning electron microscope (SEM) photograph of two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning, such as
Fig. 2 show fire-retardant polyamide fibre fiber scanning electron microscope (SEM) photograph.
Graphene oxide and two-dimentional boron nitride are added in fire resistance fibre simultaneously, utilize the height point of graphene oxide
Property and the wearability and stability of two-dimentional boron nitride are dissipated, has reached and has improved flame retardant effect while also with wear-resisting, far infrared etc.
Characteristic so that the effect of obtained polyamide fibre has warming, health care, promotes people's body-internal-circulation and improve body immunity.Aoxidize stone
Black alkene has carboxyl, epoxy radicals on the top layer of graphene, and hydroxyl etc. contains base group modification, can there is preferable parent with macromolecular fibre
And power；Two-dimentional boron nitride, lubricant and fire proofing are often used as, but because its chemical inertness is difficult to add it to high score
In son.Graphene oxide and two-dimentional boron nitride are added in fire resistance fibre by the present invention simultaneously, and are made by reasonably arranging in pairs or groups
With the synergy using graphene oxide and two-dimentional boron nitride reaches excellent flame retardant effect.
As a preferred embodiment, the two-dimentional boron nitride is six side's two dimension boron nitride, piece footpath is the μ of 50nm~5
m。
As a preferred embodiment, the pentaerythrite and its derivative are pentaerythrite, the fat of pentaerythrite
Fat acid esters, pentaerythrite epoxides or dipentaerythritol.
As a preferred embodiment, ball mill described in step 1 is tube mill, bar type ball mill or sleeping
In formula ball mill.
As a preferred embodiment, the rotating speed of ball mill described in step 1 is 200~400rpm, ratio of grinding media to material is
(60~80)：1.
As a preferred embodiment, graphene oxide described in step 2 be with Brodie methods,
Graphene oxide prepared by Staudenmaier methods and Hummers methods.
As a preferred embodiment, described in step 2 in graphene oxide dispersion graphene oxide concentration
For 5~20mg/ml.
As a preferred embodiment, the percentage by weight that slices of caprone described in step 4 mixes with blend composition is
(80~99)：(20~1).
Below by several groups of embodiments and comparative example in present embodiment the preparation technology of high resiliency fire-retardant polyamide fibre it is excellent
Gesture and its effect are further elaborated.
Embodiment one：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Embodiment two：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 100g pieces footpath to be 200nm are placed in bar type ball mill, add 10g seasons penta
Tetrol, take out after ball milling 4h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed be 200rpm, ratio of grinding media to material 80：1；
Step 2：Graphene oxide is scattered in ethanol, 30min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 5mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 10:1, mechanical agitation is evaporated at 80~90 DEG C
After being thick to mixture, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 90：10；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Embodiment three：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 300nm are placed in bar type ball mill, add 50g seasons penta 4
Alcohol, take out after ball milling 4h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 400rpm, ratio of grinding media to material 80：1；
Step 2：Graphene oxide is scattered in ethanol, 60min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 10mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 2:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 99：1；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Example IV：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 500nm are placed in horizontal ball mill, add 20g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 100rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 30min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 15mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 8:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Embodiment five：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 50g pieces footpath to be 500nm are placed in horizontal ball mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 300rpm, ratio of grinding media to material 70：1；
Step 2：Graphene oxide is scattered in ethanol, 30min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 15mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 10:1, mechanical agitation is evaporated at 80~90 DEG C
After being thick to mixture, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 95：5；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Embodiment six：
The preparation method of high resiliency fire-retardant polyamide fibre, is comprised the following steps that in the present embodiment：
Step 1：The six side's two dimension boron nitride for taking 20g pieces footpath to be 500nm are placed in horizontal ball mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 400rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 30min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 10mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 10:1, mechanical agitation is evaporated at 80~90 DEG C
After being thick to mixture, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 90：10；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example one：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 60g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example two：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 110g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta
Tetrol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed be 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example three：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 3mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example four：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 25mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example five：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 0.5:1, mechanical agitation is evaporated at 80~90 DEG C
After being thick to mixture, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example six：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 12:1, mechanical agitation is evaporated at 80~90 DEG C
After being thick to mixture, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 80：20；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Comparative example seven：
The preparation method of polyamide fibre, is comprised the following steps that in this comparative example：
Step 1：The six side's two dimension boron nitride for taking 10g pieces footpath to be 100nm are placed in tube mill, add 10g seasons penta 4
Alcohol, take out after ball milling 8h, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite, wherein ball mill
Rotating speed is 350rpm, ratio of grinding media to material 60：1；
Step 2：Graphene oxide is scattered in ethanol, 15min is ultrasonically treated, obtains graphene oxide dispersion, its
The concentration of graphene oxide is 20mg/ml in middle graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added to the graphene oxide dispersion of step 2
In, wherein the weight of two-dimentional boron nitride composite and graphene oxide ratio is 5:1, mechanical agitation is evaporated at 80~90 DEG C
After mixture is thick, dried 12 hours at 50~60 DEG C, obtain graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated,
The percentage by weight that wherein slices of caprone mixes with blend composition is 70：30；
Step 5：The master batch that step 4 obtains is obtained into fire-retardant polyamide fibre through melt spinning machine spinning.
Above-mentioned six groups of embodiments and seven groups of comparative examples are subjected to combustibility, ultimate strength, elongation at break test, obtained
As a result it is as follows：
The obtained polyamide fibre that can be seen that from the test result of six groups of embodiments and seven groups of comparative examples in six groups of embodiments is fine
Dimension 60s vertical combustion length is respectively less than 60, and the Ds values in 4min are demonstrated by extraordinary fire resistance below 5；And
For its elongation at break more than 20%, fracture strength has good mechanical property and elasticity in 4cN.
The preferred embodiments of the present invention have shown and described in described above, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations, modification and
Environment, and can be changed in the scope of the invention is set forth herein by the technology or knowledge of above-mentioned teaching or association area
It is dynamic., then all should be appended by the present invention and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention
In scope of the claims.
Claims (8)
1. a kind of preparation method of high resiliency fire-retardant polyamide fibre, it is characterised in that comprise the following steps：
Step 1：Take the two-dimentional boron nitride of 1~10 parts by weight to be placed in ball mill, add 1~5 parts by weight pentaerythrite or its
Derivative, take out after 4~8h of ball milling, be placed in 60~80 DEG C of baking ovens and dry 12h, obtain two-dimentional boron nitride composite；
Step 2：Graphene oxide is scattered in ethanol, 15~60min is ultrasonically treated, obtains graphene oxide dispersion；
Step 3：The two-dimentional boron nitride composite that step 1 is obtained is added in the graphene oxide dispersion of step 2,
The weight ratio of wherein two-dimentional boron nitride composite and graphene oxide is (10~1):1, mechanical agitation is steamed at 80~90 DEG C
Mixture is sent to after thick, to be dried 12 hours at 50~60 DEG C, obtains graphene oxide and two-dimentional boron nitride blend composition；
Step 4：The blend composition input screw extruder melting mixing that slices of caprone and step 3 are obtained is extruded, is granulated；
Step 5：The master batch that step 4 obtains is obtained into required high resiliency fire-retardant polyamide fibre through melt spinning machine spinning.
A kind of 2. preparation method of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that the two dimension nitridation
Boron is six side's two dimension boron nitride, and piece footpath is 50nm~5 μm.
A kind of 3. preparation method of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that the pentaerythrite
And its derivative is pentaerythrite, the fatty acid ester of pentaerythrite, pentaerythrite epoxides or dipentaerythritol.
4. the preparation method of a kind of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that described in step 1
Ball mill is tube mill, in bar type ball mill or horizontal ball mill.
5. the preparation method of a kind of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that described in step 1
The rotating speed of ball mill is 200~400rpm, and ratio of grinding media to material is (60~80)：1.
6. the preparation method of a kind of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that described in step 2
Graphene oxide is the graphene oxide prepared with Brodie methods, Staudenmaier methods and Hummers methods.
7. the preparation method of a kind of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that described in step 2
The concentration of graphene oxide is 5~20mg/ml in graphene oxide dispersion.
8. the preparation method of a kind of high resiliency fire-retardant polyamide fibre according to claim 1, it is characterised in that described in step 4
The percentage by weight that slices of caprone mixes with blend composition is (80~99)：(20~1).
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