CN108914242A - A kind of graphene fiber material of high temperature resistant anti-dropping and preparation method thereof - Google Patents
A kind of graphene fiber material of high temperature resistant anti-dropping and preparation method thereof Download PDFInfo
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- CN108914242A CN108914242A CN201810526770.8A CN201810526770A CN108914242A CN 108914242 A CN108914242 A CN 108914242A CN 201810526770 A CN201810526770 A CN 201810526770A CN 108914242 A CN108914242 A CN 108914242A
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- graphene oxide
- high temperature
- dropping
- nylon
- temperature resistant
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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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- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses graphene fiber materials of a kind of high temperature resistant anti-dropping and preparation method thereof, it uses nylon 6 and modified graphene oxide composite spinning, and wherein modified graphene oxide uses and graphene oxide is dissolved in deionized water, ultrasound, obtain stable dispersions, it is heated to 80-95 DEG C, p-phenylenediamine is added dropwise, reacts 2-4h, filtering, cleaning, it is dry, it obtains.The preparation-obtained fibrous material of this method has excellent physical mechanical property, with only with graphene oxide, compared with the fiber that 6 composite spinning of nylon obtains, fibre strength, anti-dropping and high temperature resistance increase significantly.Fibrous material manufacturing process obtained by this method is simple, low in cost, has good high temperature resistant and anti-dropping performance, is used as high temperature resistant engineering part, flame retardant building material etc..
Description
Technical field
The present invention relates to graphene composite material field more particularly to a kind of graphene fiber materials of high temperature resistant anti-dropping
And preparation method thereof
Background technique
Fypro is commonly called as polyamide fibre, is a kind of industrialized synthetic fibers earliest in the world, has excellent intensity, resistance to
The advantages that mill property, elastic recovery rate, it is widely used in the industries such as various clothes, cable, silk screen.Traditional Fypro produces
For amount already close to saturation, product profit is relatively low, thus current Fypro future development trend be high performance, intelligence,
The directions such as multifunction.But polyamide fibre is inflammable, when a fire, molten drop, flame, the smog formed has aggravated fire significantly
Personal damage and substance damage.Nylon 6 fiber light fastness is bad simultaneously, easily turns yellow under daylight or ultraviolet light irradiation,
Mechanical properties decrease.Therefore there is the nylon fibre of flame retardant property, uvioresistant function to be of great importance for exploitation.It leads currently on the market
Will to add based on flame retardant, but a large amount of fire retardant addition can seriously affect fiber production efficiency and product other
Performance.
Graphene is a kind of two-dimensional single layer carbon material, and the conjugation carbon-carbon double bond structure of hydridization imparts its excellent property
Energy.Since graphene is had excellent performance, have been widely used in field of compound material tool, the mechanics that can be used to improve material is strong
Degree, and network structure can be formed in composite material, it generates blocking effect and improves the performances such as the flame-retardant and anti-dripping of material.Cause
This, graphene, which is added, in nylon 6 can not only improve the mechanical strength and applied at elevated temperature performance of nylon 6, while can also improve it
Anti-dropping performance, such multiple effect is and traditional modified nylon 6 agent is unable to reach.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of graphene fiber material of high temperature resistant anti-dropping and its systems
Preparation Method, this method is at low cost, is suitble to industrial mass production, has especially important meaning.The resistance to height that this method obtains
The intensity of the graphene fiber material of warm anti-dropping is up to 8-9 g deniers, and fiber oxygen index (OI) is more than 35%.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of graphene fiber material of high temperature resistant anti-dropping, which is characterized in that by the modified graphite oxide of 100 parts by weight
Alkene/nylon 6 nano-composite and the auxiliary agent of 0.1-5 parts by weight are obtained through melt spinning, and the fibre diameter is 5-50 μm.Its
In, the preparation method of the modified graphene oxide is：Graphene oxide GO is dissolved in deionized water, ultrasound, is obtained steady
Determine dispersion liquid, be heated to 80-95 DEG C, p-phenylenediamine is added dropwise, react 2-4h, filter, cleans, it is dry, obtain modified graphite oxide
Alkene；Wherein, the mass ratio of p-phenylenediamine and GO are 20-25：1.
Further, the ratio between the quality of modified graphene oxide and the gross mass of nylon 6 are 0.01-0.5：100.
Further, the auxiliary agent is by antioxidant, antistatic agent, filler, fire retardant, Antidrip agent master batch, phenols
One of antioxidant or a variety of compositions.
The present invention also provides a kind of preparation method of the graphene fiber material of high temperature resistant anti-dropping,
(1) graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersions, is heated to 80-95 DEG C, drop
Add p-phenylenediamine, react 2-4h, filter, cleans, it is dry, obtain modified graphene oxide；Wherein, p-phenylenediamine and graphite oxide
The mass ratio of alkene is 20-25：1；
(2) nylon 6 slice of 100 parts by weight is uniformly mixed with the modified graphene oxide of 5-8 parts by weight, is modified
Graphene oxide/nylon 6 nano-composite；
(3) auxiliary agent of modified graphene oxide/nylon 6 nano-composite of 100 parts by weight and 0.1-5 parts by weight is mixed
It closes, double screw extruder is added, shear at high temperature obtains molten state spinning solution；
(4) spinning solution obtained in step (3) is pressed into filament spinning component, obtains fiber through melt spinning.
Further, the condition of the melt spinning is：For melt temperature at 250-320 DEG C, continuous spinning speed is 3600-
6000 ms/min, drafting multiple is 1.5-4 times.
Excellent effect obtained by the present invention is, provides a kind of method of p-phenylenediamine modified graphene, is added to
In nylon 6, the graphene fiber material of high temperature resistant anti-dropping is then made by spinning, so that the intensity of fiber has greatly
It improves；The intensity of obtained fibrous material is up to 8-9 g deniers, and fiber oxygen index (OI) is more than 35%；Equipment letter in method of the invention
It is single, easy to operate, cheap.
Specific embodiment
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1
A kind of graphene fiber material of high temperature resistant anti-dropping, is prepared by following methods：
(1) graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersions, is heated to 80 DEG C, dropwise addition pair
Phenylenediamine reacts 2h, filters, and cleans, dry, obtains modified graphene oxide；Wherein, the matter of p-phenylenediamine and graphene oxide
Amount is than being 20：1；
(2) nylon 6 slice of 100 parts by weight is uniformly mixed with the modified graphene oxide of 5 parts by weight, obtains modified oxygen
Graphite alkene/nylon 6 nano-composite；
(3) auxiliary agent of modified graphene oxide/nylon 6 nano-composite of 100 parts by weight and 0.1 parts by weight is mixed
It closes, double screw extruder is added, shear at high temperature obtains molten state spinning solution；
(4) spinning solution obtained in step (3) is pressed into filament spinning component, obtains fiber through melt spinning.
Wherein the condition of the melt spinning is：For melt temperature at 250 DEG C, continuous spinning speed is 3600 ms/min, is led
Stretching multiple is 1.5 times.
After tested, obtaining fibre strength is 8 g deniers, limit oxygen index 40.5%, has good anti-dropping performance.
Embodiment 2
A kind of graphene fiber material of high temperature resistant anti-dropping, is prepared by following methods：
(1) graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersions, is heated to 95 DEG C, dropwise addition pair
Phenylenediamine reacts 4h, filters, and cleans, dry, obtains modified graphene oxide；Wherein, the matter of p-phenylenediamine and graphene oxide
Amount is than being 25：1；
(2) nylon 6 slice of 100 parts by weight is uniformly mixed with the modified graphene oxide of 8 parts by weight, obtains modified oxygen
Graphite alkene/nylon 6 nano-composite；
(3) modified graphene oxide/nylon 6 nano-composite of 100 parts by weight is mixed with the auxiliary agent of 5 parts by weight,
Double screw extruder is added, shear at high temperature obtains molten state spinning solution；
(4) spinning solution obtained in step (3) is pressed into filament spinning component, obtains fiber through melt spinning.
Further, the condition of the melt spinning is：For melt temperature at 320 DEG C, continuous spinning speed is 6000 ms/min
Clock, drafting multiple are 4 times.
After tested, obtaining fibre strength is 9 g deniers, limit oxygen index 42.6%, has good anti-dropping performance.
Embodiment 3
A kind of graphene fiber material of high temperature resistant anti-dropping, is prepared by following methods：
(1) graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersions, is heated to 90 DEG C, dropwise addition pair
Phenylenediamine reacts 3h, filters, and cleans, dry, obtains modified graphene oxide；Wherein, the matter of p-phenylenediamine and graphene oxide
Amount is than being 23：1；
(2) nylon 6 slice of 100 parts by weight is uniformly mixed with the modified graphene oxide of 6 parts by weight, obtains modified oxygen
Graphite alkene/nylon 6 nano-composite；
(3) modified graphene oxide/nylon 6 nano-composite of 100 parts by weight is mixed with the auxiliary agent of 4 parts by weight,
Double screw extruder is added, shear at high temperature obtains molten state spinning solution；
(4) spinning solution obtained in step (3) is pressed into filament spinning component, obtains fiber through melt spinning.
The condition of the melt spinning is：For melt temperature at 300 DEG C, continuous spinning speed is 5000m/minute, drawing-off times
Number is 3 times.
After tested, obtaining fibre strength is 9 g deniers, limit oxygen index 41.8%, has good anti-dropping performance.
Comparative example 1
A kind of graphene fiber material resistant to high temperature, is prepared by following methods：
(1) nylon 6 slice of 100 parts by weight is uniformly mixed with the graphene oxide of 6 parts by weight, obtains graphite oxide
Alkene/nylon 6 nano-composite；
(2) graphene oxide/nylon 6 nano-composite of 100 parts by weight is mixed with the auxiliary agent of 4 parts by weight, is added
Double screw extruder, shear at high temperature obtain molten state spinning solution；
(3) spinning solution obtained in step (2) is pressed into filament spinning component, obtains fiber through melt spinning.
The condition of the melt spinning is：For melt temperature at 300 DEG C, continuous spinning speed is 5000m/minute, drawing-off times
Number is 3 times.
After tested, obtaining fibre strength is 8 g deniers, limit oxygen index 33.3%.Anti-dropping performance is compared with embodiment 1-3 phase
It is poor.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (5)
1. a kind of graphene fiber material of high temperature resistant anti-dropping, which is characterized in that by the modified graphite oxide of 100 parts by weight
Alkene/nylon 6 nano-composite and the auxiliary agent of 0.1-5 parts by weight are obtained through melt spinning, and the fibre diameter is 5-50 μm, institute
The preparation method for stating modified graphene oxide is：Graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersion
Liquid is heated to 80-95 DEG C, and p-phenylenediamine is added dropwise, and reacts 2-4h, filters, and cleans, dry, obtains modified graphene oxide；Its
In, the mass ratio of p-phenylenediamine and graphene oxide is 20-25：1.
2. the graphene fiber material of high temperature resistant anti-dropping as described in claim 1, it is characterised in that：Modified graphene oxide
Quality and the ratio between the gross mass of nylon 6 be 0.01-0.5：100.
3. the graphene fiber material of high temperature resistant anti-dropping as described in claim 1, it is characterised in that：The auxiliary agent is by antioxygen
One of agent, antistatic agent, filler, fire retardant, Antidrip agent master batch, phenolic antioxidant or a variety of compositions.
4. a kind of preparation method of the graphene fiber material of high temperature resistant anti-dropping, it is characterised in that：
(1) graphene oxide is dissolved in deionized water, ultrasound obtains stable dispersions, is heated to 80-95 DEG C, dropwise addition pair
Phenylenediamine reacts 2-4h, filters, and cleans, dry, obtains modified graphene oxide；Wherein, p-phenylenediamine and graphene oxide
Mass ratio is 20-25：1；
(2) nylon 6 slice of 100 parts by weight is uniformly mixed with the modified graphene oxide of 5-8 parts by weight, is obtained modified oxidized
Graphene/nylon 6 nano-composite；
(3) modified graphene oxide/nylon 6 nano-composite of 100 parts by weight is mixed with the auxiliary agent of 0.1-5 parts by weight,
Double screw extruder is added, shear at high temperature obtains molten state spinning solution；
(4) spinning solution obtained in step (3) is pressed into filament spinning component, obtains fiber through melt spinning.
5. preparation method as claimed in claim 4, it is characterised in that：The condition of the melt spinning is：Melt temperature exists
250-320 DEG C, continuous spinning speed is 3600-6000 ms/min, and drafting multiple is 1.5-4 times.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810320021X | 2018-04-11 | ||
| CN201810320021 | 2018-04-11 |
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| CN108914242A true CN108914242A (en) | 2018-11-30 |
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| CN201810526770.8A Pending CN108914242A (en) | 2018-04-11 | 2018-05-29 | A kind of graphene fiber material of high temperature resistant anti-dropping and preparation method thereof |
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Cited By (3)
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| CN109796756A (en) * | 2019-01-04 | 2019-05-24 | 北京化工大学常州先进材料研究院 | A kind of difunctional graphite alkene synthesis and heat-conduction nylon material preparation method |
| CN110592778A (en) * | 2019-10-09 | 2019-12-20 | 刘国成 | Graphene-based composite fiber summer sleeping mat and preparation method thereof |
| CN111574136A (en) * | 2020-06-30 | 2020-08-25 | 郑州大学 | High-temperature-resistant geopolymer mortar and preparation method thereof |
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| CN111574136A (en) * | 2020-06-30 | 2020-08-25 | 郑州大学 | High-temperature-resistant geopolymer mortar and preparation method thereof |
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