CN105463620B - A kind of graphene/PET composite fibre and preparation method thereof - Google Patents
A kind of graphene/PET composite fibre and preparation method thereof Download PDFInfo
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- CN105463620B CN105463620B CN201610027439.2A CN201610027439A CN105463620B CN 105463620 B CN105463620 B CN 105463620B CN 201610027439 A CN201610027439 A CN 201610027439A CN 105463620 B CN105463620 B CN 105463620B
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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
- D01F6/92—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 polyesters
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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
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
Abstract
The present invention relates to a kind of graphene/PET composite fibre and preparation method thereof, include in composite fibre by mass parts：5~20 parts of composite master batch, PET cut into slices 80~95 parts.Preparation method includes：Graphite oxidation is obtained into graphite oxide, then ultrasonic disperse in deionized water, obtain the graphite oxide aqueous solution, be dispersed in high boiling organic solvent, ultrasound, be heated to reflux, is evaporated under reduced pressure, washed, filtered, drying, obtain graphene；By graphene ultrasonic disperse in PET solvent, graphene dispersing solution is obtained, then adds PET, is stirred, oil bath heating backflow, cooling, ultrasound, washs, dries, obtain composite master batch；By composite master batch and PET section vacuum drying, then heat, extrude and be wound, drawing-off, produce.The present invention obtains fiber well dispersed and with some strength and function, has very big potential in functional fibre and fabric application.
Description
Technical field
The invention belongs to the preparation field of composite fibre, more particularly to a kind of graphene/PET is multiple
Condensating fiber and preparation method thereof.
Background technology
PET is widely used, technology maturation, but it is poor uvioresistant, antistatic property to be present, and dry-hot shrinkage is high to be waited not
Foot.Improve polymer performance at present mainly to carry out in terms of high-performance and functionalization, improve the master of mechanical performance and heat endurance
There are nanoclay, nano silicon, CNT etc.；Anti-ultraviolet function is by carbon black, silica, titanium dioxide etc.
Inorganic nanoparticles are completed；It is antistatic to complete functionalization using carbon materials such as expanded graphite, CNTs；In addition, magnetic, antibacterial
Its specific function is assigned etc. function doped magnetic metallic particles, Nano Silver etc..Application Number (patent) CN201010214235.2 profits
High-performance clothing is prepared with Nano titanium nitride uvioresistant polyester；Application Number (patent) CN201310410448.6 has made Nano Silver by oneself
It is antibacterial matrices, for preparing antibiotic odourproof fiber；Application Number (patent) CN201310239570.1 is simultaneously using organic and inorganic
Fire retardant, cooperate, prepare flame-retardant PET material.These nano-particles have that density is big, the less defect of specific surface area, lead
Cause inorganic particle addition high, spinnability reduces and the defects of damaged mechanical property, and needs a variety of nano-particles to cooperate
Reach multifunctional modification purpose.Because the specific surface area of graphene is very high, and with conduction, UV absorption, enhancing effect
The multi-functional characteristic such as good so that graphene, which is modified, turns into study hotspot.
The content of the invention
The technical problems to be solved by the invention be to provide a kind of graphene/PET composite fibre and
Its preparation method, this method raw material is cheap and easy to get, and the fiber dispersion obtained is good, and with multifunctionality；This method can
Obtain that nano-particle addition is few, the good nano-composite fiber of modified effect.
A kind of graphene/PET composite fibre of the present invention, mass parts are pressed in the composite fibre
Including：5~20 parts of composite master batch, PET cut into slices 80~95 parts；Wherein, in composite master batch graphene content for 1wt%~
20wt%.
A kind of preparation method of graphene/PET composite fibre of the present invention, including：
(1) graphite is obtained into graphite oxide by Hummers methods；By graphite oxide ultrasonic disperse in deionized water, obtain
To the 0.1wt%~1.0wt% graphite oxide aqueous solution；
(2) by the graphite oxide aqueous dispersion in step (1) 1~10 times (volume multiple of the aqueous solution) higher boiling
In organic solvent, ultrasound, 170~250 DEG C are flowed back 5 minutes~24 hours, steam most of high boiling organic solvent,
Washing of precipitate is filtered, high boiling organic solvent and byproduct of reaction is removed, drying, obtains graphene；
(3) the graphene ultrasonic disperse obtained in step (2) is obtained into graphene dispersing solution, then in PET solvent
PET sections or powder, stirring are added, 150-170 DEG C of backflow 1-5h of oil bath heating is cooled to room temperature, in frozen glue to being completely dissolved
Shape, ultrasound, wash, dry, the content for obtaining graphene is 1wt%~20wt% composite master batch；
(4) by the composite master batch in step (3) and PET section vacuum drying, be then fed into screw extruder 270~
300 DEG C carry out heating 30s~30min, extrude and are wound, and drawing-off, it is compound to obtain graphene/PET
Fiber；Wherein, the mass parts of composite master batch are 5~20 parts, and the mass parts of PET sections are 80~95 parts.
Graphite length and width dimensions are less than and (grow and width is respectively less than) 10 μm in the step (1).
Preferably, the graphite length and width dimensions are less than and (grow and width is respectively less than) 2 μm.
In the step (2) high boiling organic solvent be 1-METHYLPYRROLIDONE, ethylene glycol and diethylene glycol at least
It is a kind of.
PET solvent is 1-METHYLPYRROLIDONE, o-chlorphenol, phenol, tetrachloroethanes, three chloroethenes in the step (3)
At least one of acid and trifluoroacetic acid.
Preferably, the solvent of the PET is 1-METHYLPYRROLIDONE.
Washing is with low boiling point organic solvent or water washing in the step (3)；Wherein, low boiling point organic solvent is first
At least one of alcohol, ethanol, ether, acetone, tetrahydrofuran and propyl alcohol.
Graphene mass fraction is 1%~10% in composite master batch in the step (3).
Preferably, graphene mass fraction is 10% in the composite master batch.
Processing is dried for vacuum ＞ 0.85MPa vacuum drum drying machine in vacuum drying in the step (4),
80~160 DEG C of gradients dry 20~24h.
Drawing temperature is 120~200 DEG C in the step (4), and drafting multiple is 4~7 times.
The speed of winding is 200~5000m/min in the step (4).
It is characteristic of the invention that obtaining graphene using the method for heat-treating graphite oxide, carrying out solution blending with PET obtains
To master batch, finely dispersed composite fibre is obtained using masterbatch method melt drawing.The excellent mechanical performance of graphene itself, superelevation
Electrical conductivity, calorifics, uvioresistant performance will assign fiber multifunctional；And the specific surface area of graphene superelevation, and it is relatively low
Density so that obtained fibre density has relatively low density, relatively low nanometer compared with the composite fibre of other additives
Particle content is the improvement of availability.
It is excellent using graphene many-side it is an object of the invention to provide a kind of preparation method of graphene modified PET fiber
It is different in nature can, the characteristics of overcoming graphene easily to reunite, prepare finely dispersed graphene polymer nano-composite fiber.By graphene
It is compound with PET, so as to obtain the attention that the research of functional composite material causes scientific research personnel.
It is characteristic of the invention that preparing the method for graphene composite fibre, obtain well dispersed and there is some strength and work(
The fiber of energy.Because graphene has good mechanical performance, the electrical conductivity of superelevation and higher rate of absorbing UV so that this
The nano-composite fiber of invention has very big potential in functional fibre and fabric application.
Beneficial effect
(1) composite fibre density produced by the present invention has relatively low density compared with the composite fibre of other additives,
Relatively low nanoparticle content is the improvement of availability；
(2) raw material of the present invention is cheap and easy to get, and the fiber dispersion obtained is good, and uvioresistant performance is good and with multi-functional
Property.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of different graphene content composite master batch sections in embodiment 1, and wherein a-c corresponds to stone
Black alkene addition is 0.1wt.%, and it is 0.5wt.% that d-f, which corresponds to graphene addition, and g-i corresponds to graphene addition and is
It is 5.0wt.% that 1.0wt.%, j-l, which correspond to graphene addition, and it is 8.0wt.% that m-o, which corresponds to graphene addition,；
Fig. 2 is the optical microscope of the composite fibre of different graphene contents in embodiment 1, stone corresponding to wherein a-f
Black alkene addition is respectively 0%, 0.1wt.%, 0.2wt.%, 0.5wt.%, 0.8wt.% and 1.0wt.%；
Fig. 3 is the scanning electron microscope (SEM) photograph of the PET composite fibre sections that graphene content is 0.2wt.% in embodiment 1；Wherein,
A, b, c are different amplification；
Fig. 4 is the ultraviolet-visible absorption spectroscopy of the water slurry of different graphene content PET composite fibres in embodiment 1.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) preparation of graphite oxide：
30g sodium nitrate and concentrated sulfuric acid 675mL are added into three-necked flask, is slowly stirred under ice-water bath, adds 75g permanganic acid
Potassium, 15g graphite, ice-water bath 30min, mechanical agitation, heating water bath pour into 1300mL deionizations to 35 DEG C after keeping 5h at room temperature
In water, 98 DEG C are heated to, is kept stirring for, after about 30min plus hydrogen peroxide without gas to emerging, and reaction terminates.With 10% dilute salt
Acid elution product, to remove metal ion, graphite oxide is dried to obtain after the completion of washing.
(2) preparation of graphene：
1.0g graphite oxides are peeled off using Probe Ultrasonic Searching and are distributed in 100g water, power is about 40W, ultrasonic time 1.5
Hour, obtain dispersion liquid A.The aqueous solution of graphite oxide is added in 400g 1-METHYLPYRROLIDONEs (NMP), continues ultrasonic disperse,
Observation by light microscope is used after about 30min, it is scattered to reach good, obtain dispersion liquid B.Magnetic agitation and oil bath heating dispersion liquid B are extremely
100 DEG C, 5min is kept, adds condenser pipe to be heated to 200 DEG C of backflow 2h, completes thermal reduction.Evaporation removes NMP, and third is added in product
Ketone washs, and is filtered using the teflon membrane filter in 0.3 μm of aperture, and acetone washs colourless to washing lotion, and filter cake is dried to obtain heat
The graphene of reduction.
(3) preparation of compound resin master batch：
Heat-treat obtained graphene to be dispersed in NMP through probe sonication, observation by light microscope point is utilized after about 1.5h
Good rear addition PET powder, magnetic agitation are dissipated, 165 DEG C of oil bath heating flows back, is completely dissolved after about 3h, stops heating and stir,
Smashed to pieces after being cooled to room temperature, add a large amount of acetone ultrasounds.NMP is washed away, filtering and washing is colourless to filtrate.60 DEG C of bakings of convection oven
It is dry, 120 DEG C of baking 48h of vacuum drying oven.Prepare different graphene contents (0.1wt.%, 0.5wt.%, 1.0wt.%, 2.0wt.%,
5.0wt.%, 8.0wt.%) composite master batch, it is as shown in Figure 1 to obtain SEM figures；Wherein a-c corresponds to graphene addition
It is 0.5wt.% that 0.1wt.%, d-f, which correspond to graphene addition, and it is 1.0wt.% that g-i, which corresponds to graphene addition, and j-l is corresponding
Graphene addition is 5.0wt.%, and it is 8.0wt.% that m-o, which corresponds to graphene addition,.
(4) preparation of graphene modified composite fiber：
1) master batch and PET sections that graphene mass fraction is 2% are weighed by mass parts；
2) master batch and PET sections are sent into vacuum drum drying machine and processing is dried, drying process is vacuum
0.85MPa, dried using gradient, 80~160 DEG C (80 DEG C of 2h, 100 DEG C of 10h, 120 DEG C of 10h, 160 DEG C of 2h) dry 24h；
3) master batch and PET sections are sent into screw extruder to be melted, melting temperature is 290 DEG C, and the melting time is
30min；
4) melt sprays from spinneret, winding speed 500m/s；
5) drawing-off in air, drawing temperature are 180 DEG C, and drafting multiple is 4 times, obtains the graphite of different graphene contents
Alkene/PET composite fibre.
The optical microscope image of the composite fibre of different graphene contents is as shown in Figure 2.Wherein, graphene addition is
0.2wt.% (the final content of graphene in composite fibre, the mass parts of master batch 10 that graphene mass fraction is 2% during preparation,
PET cut into slices 90 mass parts) PET composite fibre sections stereoscan photograph it is as shown in Figure 3.The different compound fibres of graphene tret
Dimension uv-vis spectra of suspension in water is as shown in Figure 4, it is seen that addition is 0.2wt.%~1.0wt.% (composite fibres
The final content of middle graphene) composite fibre there is preferable uvioresistant performance.
Embodiment 2
The preparation of graphene oxide dispersion is the same as embodiment 1.
The preparation of compound resin master batch：
The graphene that 0.4g heat-treats to obtain is dispersed in o-chlorphenol through probe sonication, and optical microphotograph is utilized after about 1.5h
PET powder, magnetic agitation are added after sem observation is well dispersed, 165 DEG C of oil bath heating flows back, is completely dissolved after about 3h, stops adding
Heat and stirring, are smashed to pieces after being cooled to room temperature, add a large amount of acetone ultrasounds.O-chlorphenol is washed away, filtering and washing is colourless to filtrate.Drum
The 60 DEG C of drying of wind baking oven, 120 DEG C of baking 48h of vacuum drying oven.
The preparation of graphene modified composite fiber：
(1) mass parts of master batch 5, PET 95 mass parts of section are taken；
(2) master batch and PET sections are sent into vacuum drum drying machine and processing is dried, drying process is vacuum
0.85MPa, dried using gradient, 80~160 DEG C of dry 24h；
(3) master batch and PET sections are sent into screw extruder to be melted, melting temperature is 290 DEG C, and the melting time is
30min；
(4) melt sprays from spinneret, winding speed 500m/s.
(5) drawing-off in air, drawing temperature are 180 DEG C, and drafting multiple is 4 times, obtains graphene/poly terephthalic acid second
Diester composite fibre.
Claims (8)
1. a kind of preparation method of graphene/PET composite fibre, including：
(1) graphite is obtained into graphite oxide by Hummers methods；By graphite oxide ultrasonic disperse in deionized water, obtain
0.1wt%~1.0wt% graphite oxide the aqueous solution；
(2) by the graphite oxide aqueous dispersion in step (1) in the high boiling organic solvent of 1~10 times of aqueous solution volume,
Ultrasound, 170~250 DEG C are flowed back 5 minutes~24 hours, are evaporated under reduced pressure, and are washed, and are filtered, and drying, obtain graphene；
(3) the graphene sound obtained in step (2) is dispersed in PET solvent, obtains graphene dispersing solution, then add
PET, stirring, 150-170 DEG C of backflow 1-5h of oil bath heating, cooling, ultrasound, wash, dry, the content for obtaining graphene is
1wt%~20wt% composite master batch；
(4) by the composite master batch in step (3) and PET section vacuum drying, then carried out at 270~300 DEG C heating 30s~
30min, extrude and be wound, drawing-off, obtain graphene/PET composite fibre；Wherein, composite master batch
Mass parts be 5~20 parts, PET section mass parts be 80~95 parts.
2. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that graphite length and width dimensions are less than 10 μm in the step (1).
3. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that high boiling organic solvent is at least one in 1-METHYLPYRROLIDONE, ethylene glycol and diethylene glycol in the step (2)
Kind.
4. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that PET solvent is 1-METHYLPYRROLIDONE, o-chlorphenol, phenol, tetrachloroethanes, trichloroacetic acid in the step (3)
At least one of with trifluoroacetic acid.
5. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that washing is with low boiling point organic solvent or water washing in the step (3)；Wherein, low boiling point organic solvent be methanol,
At least one of ethanol, ether, acetone, tetrahydrofuran and propyl alcohol.
6. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that graphene mass fraction is 1%~10% in composite master batch in the step (3).
7. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that vacuum drying is that processing is dried in vacuum ＞ 0.85MPa vacuum drum drying machine in the step (4),
80~160 DEG C of gradients dry 20~24h.
8. a kind of preparation method of graphene/PET composite fibre according to claim 1, it is special
Sign is that drawing temperature is 120~200 DEG C in the step (4), and drafting multiple is 4~7 times；The speed of winding be 200~
5000m/min。
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| CN107501877A (en) * | 2017-06-13 | 2017-12-22 | 华烯新材料科技无锡有限公司 | A kind of compound PET master batch of graphene and preparation method thereof |
| CN107604462A (en) * | 2017-06-13 | 2018-01-19 | 绍兴标点纺织科技有限公司 | A kind of compound PBT fibers of graphene and preparation method |
| CN107488891A (en) * | 2017-08-21 | 2017-12-19 | 中国石油大学(北京) | A kind of new function graphite alkene composite fibre and preparation method and application |
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| CN109280991B (en) * | 2018-08-28 | 2021-07-20 | 中国科学院福建物质结构研究所 | Method for efficiently preparing graphene polyester |
| BR102019024477A2 (en) * | 2019-11-21 | 2021-06-01 | Dini Têxtil Indústria E Comércio Ltda. | PROCESS FOR OBTAINING TEXTILE FIBERS BASED ON GRAPHENE OXIDE AND POLYESTER |
| CN113718366A (en) * | 2021-09-18 | 2021-11-30 | 南通强生石墨烯科技有限公司 | Graphene super-strong flame-retardant fiber and preparation method thereof |
| CN113897699A (en) * | 2021-10-25 | 2022-01-07 | 南通强生石墨烯科技有限公司 | Graphene uvioresistant regenerated fiber and preparation method thereof |
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| CN102586952A (en) * | 2012-01-09 | 2012-07-18 | 东华大学 | Method for preparing graphene-reinforced polyacrylonitrile carbon fibers |
| CN104164707B (en) * | 2014-07-24 | 2016-07-06 | 桐乡市中辰化纤有限公司 | Graphene conductive polyester fiber and preparation method thereof |
| CN104357941B (en) * | 2014-11-04 | 2016-04-06 | 天津工业大学 | Graphene and multi-walled carbon nano-tubes work in coordination with enhanced polymer fiber and preparation method thereof |
| CN104894680B (en) * | 2015-06-15 | 2017-03-01 | 东华大学 | A kind of PPS/ Graphene hybridization compounding fiber and preparation method thereof |
| CN105200547B (en) * | 2015-10-19 | 2018-06-01 | 南通强生石墨烯科技有限公司 | A kind of preparation method of graphene-terylene nanometer composite fibre |
| CN105177753B (en) * | 2015-10-21 | 2017-06-06 | 东华大学 | A kind of preparation method of the antistatic high-strength fire-retarding terylene of military anti-dropping |
| CN105155024A (en) * | 2015-10-26 | 2015-12-16 | 太仓市双宇化纤有限公司 | Conductive composite fiber material and preparation method thereof |
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