CN109056098A - A kind of preparation method of high performance graphene aramid fiber and thus obtained high performance graphene aramid fiber - Google Patents
A kind of preparation method of high performance graphene aramid fiber and thus obtained high performance graphene aramid fiber Download PDFInfo
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- CN109056098A CN109056098A CN201810890616.9A CN201810890616A CN109056098A CN 109056098 A CN109056098 A CN 109056098A CN 201810890616 A CN201810890616 A CN 201810890616A CN 109056098 A CN109056098 A CN 109056098A
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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
- D01F6/905—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 of aromatic 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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Abstract
The present invention relates to a kind of preparation methods of high performance graphene aramid fiber, it includes the following steps: to provide flake graphite alkene, graphene is dissolved in formation graphene slurry in -2 pyrrolidones of 1- methyl and/or water, wherein, the mass percent of the flake graphite alkene in graphene slurry is 0.5-2wt.%；Phytic acid is added to be mixed in graphene slurry and forms mixed slurry；And Fanglun slurry cake is added in mixed slurry and is stirred, spinneret obtains high performance graphene aramid fiber, wherein flake graphite alkene: phytic acid: the mass ratio of Fanglun slurry cake is 1:1:18-98.The present invention also provides a kind of high performance graphene aramid fibers obtained by above-mentioned preparation method.Preparation method according to the present invention, by using graphene slurry, increase chance of the graphene in conjunction with aramid fiber, then the substance that centre connects using phytic acid as the two, graphene may be implemented and aramid fiber closely combines, solve the problems, such as that graphene is easy to fall off on aramid fiber.
Description
Technical field
The present invention relates to aramid fiber, relate more specifically to a kind of preparation method of high performance graphene aramid fiber with
And thus obtained high performance graphene aramid fiber.
Background technique
Aramid fiber full name is aromatic polyamide fibre, because of its low-density, the characteristics such as excellent corrosion-resistant, impact resistance, fire-retardant,
Frequently as the reinforced phase of polymer matrix composites, outer layer protection is carried out with the occasion easily impacted for easily rubbing, is such as used for aviation
Each field such as space flight, military affairs, machinery.Aramid fiber is broadly divided into two kinds: contraposition aramid fiber (PPTA) and meta position virtue amide
Fiber (PMIA).Aramid fiber is in apparent skin-core structure, and surface chemical property is stablized, and lacks active group, surface wettability
It is poor, it is lower with resin material interface bonding energy, the performance of its excellent properties is limited significantly.Since discovery aramid fiber in 1972
Since, aramid fiber relies on its excellent comprehensive performance, leads the development of numerous leading-edge fields always.Aramid fiber production neck
Domain, especially contraposition aramid fiber, development is very fast, such as the Kevlar fiber of Dupont, the Twaron of Japanese Di Ren company,
Technora fiber, Taparan (Tai Pulong) fiber of the calm and peaceful green wood in Yantai etc..Aramid fiber is modified, it appears it is particularly important,
Aramid fiber is modified, and surface macromolecular chain queueing discipline is deteriorated and in some active function groups of Surface Creation, such as C=
O ,-OH ,-COOH and NH2Deng.Chemical reaction can occur with basis material or generate hydrogen bond for these functional groups, so as to improve multiple
Condensation material interface performance.Surface grafting, bromine etching, chlorosulfonation, acetic anhydride processing and nitrification reduction, surface covering, high-energy ray
Irradiation, plasma modification, ultrasonic immersing etc., different processing methods can all improve the interface performance of composite material.Aramid fiber slurry
The dregs of rice are to carry out just obtaining after surface fibrillation processing to aramid fiber, and unique surface texture greatly improves mixing
The grasping force of object, therefore be highly suitable as a kind of reinforcing fiber and be applied in friction and sealed product.Fanglun l414 pulp, shallowly
Yellow wadding is flower-shaped, is in lint shape, and filoplume is abundant, and intensity is high, good stability of the dimension, no brittleness, high temperature resistant, it is corrosion-resistant, be commonly used for
Gasket reinforcing material, have preferable resilience performance and sealing performance, it is non-hazardous to human health and environment, can be used as in water,
The sealing of the media such as the soda acid of oil, hydro carbons and moderate strength, the gasket produced have excellent sealing performance and creep resistant relaxation
Performance
Graphene is a kind of new carbon haveing excellent performance, specific surface area with higher, high electrical and thermal conductivity, use
It can be very good the wear-resisting property of improvement fiber in fiber, intensity increases the conductive and heat-conductive ability of fiber and realizes resistant fiber
The abilities such as bacterium have had some patents to be reported, have mainly made aramid fiber with graphene in terms of graphene is for aramid fiber
Fiber is capped, preferably protects aramid fiber from the damage of ultraviolet radiation.Such as CN104047160A discloses one kind
The method of surface of graphene oxide graft modification aramid fiber, specific method are to coat dopamine in aramid fiber surface, then
Amidized graphene oxide is grafted on to the aramid fiber surface for having coated dopamine by schiff base reaction.The preparation method
The substance binding ability that the interface performance between aramid fiber and resin matrix dopamine can be improved, but be obtained by still compared with
Difference not can effectively improve the binding force between graphene and aramid fiber.Since stable company can not be formed between graphene and aramid fiber
It connects, graphene is easy to fall off.
Summary of the invention
In order to solve the problems, such as that above-mentioned graphene of the existing technology is easy to fall off, the present invention is intended to provide a kind of high property
The preparation method of the graphene aramid fiber of energy and thus obtained high performance graphene aramid fiber.
The present invention provides a kind of preparation method of high performance graphene aramid fiber comprising following steps: S1 is provided
Graphene is dissolved in formation graphene slurry in -2 pyrrolidones of 1- methyl and/or water, wherein graphene slurry by flake graphite alkene
The mass percent of flake graphite alkene in material is 0.5-2wt.%；Phytic acid is added in graphene slurry and is mixed by S2
Form mixed slurry；And S3, Fanglun slurry cake is added in mixed slurry and is stirred, spinneret obtains high performance graphene
Aramid fiber, wherein flake graphite alkene: phytic acid: the mass ratio of Fanglun slurry cake is 1:1:18-98.
In the present invention, phytic acid is attracted each other by the benzene ring structure with graphene and is connect, above phytic acid
Phosphate group and hydroxyl group and aramid fiber form hydrogen bond and chemical bond chelating connects, so that graphene be made to be wrapped in Fanglun slurry cake
On, the high performance graphene aramid fiber is formed finally by further spinning.In step s 2, graphene and phytic acid quilt
It is fused together well, in step s3, these types of substance is made by the π-π of graphene and aramid fiber and phytic acid interaction
It combines closely, through washing, rubs repeatedly, graphene will not fall off.Moreover, because the addition of graphene, the high performance stone
The mechanical strength and electrical and thermal conductivity performance of black alkene aramid fiber are all greatly improved, and realize superhigh intensity, highly conductive,
The preparation of the graphene coated aramid fiber of high thermal conductivity.
In the step S1, flake graphite alkene is provided by electrochemical stripping method or liquid phase stripping method.Preferred
In embodiment, which is the graphene of low defect or the graphene of high-quality.Preferably, the density of graphene slurry
For 5-20mg/ml.Preferably, the lamella transverse direction average-size of the flake graphite alkene in graphene slurry is 1-5 μm, the lamella number of plies
It is 3-6 layers.
In the step S2, phytic acid solid powder and/or phytic acid aqueous solution are added in graphene slurry.It is preferred that
Ground, the mass percent of the phytic acid in phytic acid aqueous solution are 60-80wt.%, more preferably 70wt.%.Preferably, it is mixed
0.5-3h。
In the step S3, Fanglun slurry cake is Fanglun l414 pulp.Preferably, the speed of spinneret is 2-5m/min, spray
The temperature of silk is 120-200 DEG C.Preferably, it is stirred and is carried out in high mixer.Preferably, it is stirred 2-5h.
The present invention also provides a kind of high performance graphene aramid fibers obtained by above-mentioned preparation method, wherein
The graphene aramid fiber is graphene coated aramid fiber.
The graphene coated aramid fiber that the present invention passes through, wherein graphene is the individual layer laminated structure being made of carbon atom
The two-dimentional carbon nanomaterial of flexibility, there is high electrical and thermal conductivity, high mechanical strength, high specific surface area and good soft
Property.Wherein aramid fiber is a kind of novel high-tech synthetic fibers, has superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, weight
It is light to wait excellent performances, it is widely used in the fields such as composite material, ballistic-resistant article, building materials, special type protection clothes, electronic equipment.It will
Graphene improves the electric conductivity of aramid fiber in conjunction with graphene and aramid fiber for wrapping up Fanglun slurry cake, enhances the intensity of aramid fiber and wear-resisting
Property, so that aramid fiber is had both conductive and higher intensity performance, it is mentioned in the present invention compared to other graphene aramid fiber composite materials
Graphene aramid fiber composite material has stronger composite junction resultant force, is repeatedly washing, is crumpling and not will lead to during folding
It falls off.
Preferably, the conductivity of the high performance graphene aramid fiber is 2500-4500S/m.It is fine with existing aramid fiber
Dimension is compared, and the tensile strength of high performance graphene aramid fiber provided by the invention improves 33-40%.
Preparation method according to the present invention increases chance of the graphene in conjunction with aramid fiber by using graphene slurry, then
The substance connected among using phytic acid as the two, may be implemented graphene and aramid fiber closely combines, and solves graphene and exists
The problem of being easy to fall off on aramid fiber.Moreover, combining the phytic acid of auxiliary bonding using relatively viscous graphene slurry, more uniformly
Graphene is bonded on aramid fiber.Wherein, graphene and aramid fiber are passed through π-π phase well by the phytic acid with adhesion
Stable connection function is realized in connection between interaction and functional group, and then improves aramid fiber poorly conductive, lacks activity
Group, the problem of surface infiltration difference.In addition, preparation method of the invention is simple and convenient, realized with existing fiber producing processes
Seamless interfacing, operating condition is mild, it can be achieved that graphene is to the industrialized production of aramid fiber, and economic effect is good.Thus it obtains
The high-performance aramid fiber of the graphene package obtained, has extraordinary electric conductivity and mechanical strength, is to be applied to a variety of intelligence
Equipment and dress ornament.
Specific embodiment
Presently preferred embodiments of the present invention is given below, and is described in detail.
Embodiment 1
Choose the slurry that the electrochemical stripping graphene that density is 5mg/ml low defect is dissolved in -2 pyrrolidones of 1- methyl (NMP)
Material, the mass percent of corresponding graphene content are 0.5wt.%, and wherein the size of graphene is 5 μm, and the number of plies is 6 layers, are pressed
Mass percentage, phytic acid is added in graphene slurry, is mixed evenly by each 5 parts by graphene and phytic acid solid
0.5h；
Then 90 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the mass ratio of Fanglun slurry cake
For 1:1:18, the lasting stirring 2h mixing in high mixer；It is to be mixed uniformly after with 2m/min speed, under the conditions of 200 DEG C of temperature
Routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber fibre
Dimension.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 3000S/m, and tensile strength improves
35%, solve the problems, such as that the aramid fiber of insulation is electrically conductive, graphene and aramid fiber bonding are close and high by graphene
Mechanical strength improves fiber tensile property.
Embodiment 2
The slurry that the graphene that the liquid phase that density is 20mg/ml low defect is removed is dissolved in NMP is chosen, corresponding graphene contains
The mass percent of amount is 2wt.%, and wherein the size of graphene is 1 μm, and the number of plies is 3 layers, by mass percentage, by graphite
Alkene and each 5 parts of phytic acid solid, phytic acid is added in graphene slurry, 0.5h is mixed evenly；
Then 90 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the mass ratio of Fanglun slurry cake
For 1:1:18, the lasting stirring 5h mixing in high mixer；It is to be mixed uniformly after with 5m/min speed, under the conditions of 120 DEG C of temperature
Routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber fibre
Dimension.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 4500S/m, and tensile strength improves
38%.Graphene slurry density is high, and additive amount is big, can wrap up aramid fiber slurry foil well, and a large amount of additions of phytic acid also promote
The conductivity of the connection of graphene and aramid fiber, composite fibre is significantly promoted, and tensile strength is obviously improved.
Embodiment 3
The graphene for choosing the electrochemical stripping that density is 20mg/ml low defect is dissolved in the slurry of NMP, corresponding graphene
The mass percent of content is 2wt.%, and wherein the size of graphene is 5 μm, and the number of plies is 6 layers, by mass percentage, by stone
Black alkene and each 1 part of phytic acid solid, phytic acid is added in graphene slurry, 3h is mixed evenly；
Then 98 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the mass ratio of Fanglun slurry cake
For 1:1:98, the lasting stirring 5h mixing in high mixer；It is to be mixed uniformly after with the speed of 5m/min, 150 DEG C of temperature conditions
Under routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber
Fiber.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 4000S/m, and tensile strength improves
40%.Graphene slurry density is big, and content is high, more for sticking aramid fiber material, finally compared to other ratios, significantly
Raising conductivity and tensile strength.
Embodiment 4
Choose the slurry that the graphene for the electrochemical stripping that density is 20mg/ml low defect is soluble in the aqueous phase, corresponding graphite
The mass percent of alkene content is 2wt.%, and wherein the size of graphene is 5 μm, and the number of plies is 6 layers, by mass percentage, is pressed
1 part of graphene and 1.43 parts of phytic acid aqueous solution (70wt.%), plant acid solution is added in the water phase slurry of graphene, is mixed
Stir evenly 0.5h；
Then 98 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the mass ratio of Fanglun slurry cake
For 1:1:98, the lasting stirring 2h mixing in high mixer；It is to be mixed uniformly after with 2m/min speed, under the conditions of 180 DEG C of temperature
Routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber fibre
Dimension.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 2500S/m, and tensile strength improves
33%.Graphene density is higher, although adding proportion is less, graphene solid content is integrally more, can wrap up virtue well
Synthetic fibre, but since in water phase, graphene dispersion is poor, therefore final conductivity improves seldom, tensile strength correspondinglys increase.
Comparative example 1
The slurry that the electrochemical stripping graphene that density is 3mg/ml low defect is dissolved in NMP is chosen, corresponding graphene contains
The mass percent of amount is 0.3wt.%, and wherein the size of graphene is 0.5 μm, and the number of plies is 8 layers, by mass percentage, is pressed
Graphene and each 0.5 part of phytic acid, phytic acid is added in graphene slurry, 0.5h is mixed evenly；
Then 50 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the mass ratio of Fanglun slurry cake
For 1:1:100, the lasting stirring 2h mixing in high mixer；It is to be mixed uniformly after with 2m/min speed, under the conditions of 200 DEG C of temperature
Routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber fibre
Dimension.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 60S/m, and tensile strength improves 3%,
But since the content of graphene is few, lamella size is small, and dosage is few, can not coat aramid fiber completely, leads to the material obtained
Conductivity is greatly lowered, and tensile strength improves unobvious.
Comparative example 2
The slurry that the electrochemical stripping graphene that density is 30mg/ml low defect is dissolved in NMP is chosen, corresponding graphene contains
The mass percent of amount is 3wt.%, and wherein the size of graphene is 10 μm, and the number of plies is 2 layers, by mass percentage, by graphite
Alkene and each 10 parts of phytic acid, phytic acid is added in graphene slurry, 0.5h is mixed evenly；
Then 100 parts of commercially available Fanglun slurry cake is added in mixed slurry, graphene: phytic acid: the quality of Fanglun slurry cake
Than for 1:1:10, the lasting stirring 2h mixing in high mixer；It is to be mixed uniformly after with 2m/min speed, 200 DEG C of temperature conditions
Under routinely preparation method spinneret, after sink is cooling, wire drawing finally obtains graphene and wraps up obtaining high performance graphene aramid fiber
Fiber.
The conductivity for the high performance graphene aramid fiber that the present embodiment obtains is 6000S/m, and tensile strength improves
2%, but since the content of graphene is too many, lamella size is big, and the number of plies is thin, and the specific surface area of graphene used is too big, and dosage
Greatly, lead to material is dispersed into very big problem, and graphene has disengaged from, and the material electric conductivity finally obtained is significantly promoted,
But since falling off for graphene makes tensile strength raising unobvious with uneven dispersion.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper
Stating embodiment can also make a variety of changes.Made by i.e. all claims applied according to the present invention and description
Simply, equivalent changes and modifications fall within the claims of the invention patent.The not detailed description of the present invention is
Routine techniques content.
Claims (9)
1. a kind of preparation method of high performance graphene aramid fiber, which comprises the steps of:
S1 provides flake graphite alkene, and graphene is dissolved in formation graphene slurry in -2 pyrrolidones of 1- methyl and/or water,
In, the mass percent of the flake graphite alkene in graphene slurry is 0.5-2wt.%；
Phytic acid is added to mixing in graphene slurry and forms mixed slurry by S2；And
Fanglun slurry cake is added in mixed slurry and is stirred by S3, and spinneret obtains high performance graphene aramid fiber,
In, flake graphite alkene: phytic acid: the mass ratio of Fanglun slurry cake is 1:1:18-98.
2. preparation method according to claim 1, which is characterized in that in the step S1, pass through electrochemical stripping method
Or liquid phase stripping method provides flake graphite alkene.
3. preparation method according to claim 2, which is characterized in that the density of graphene slurry is 5-20mg/ml.
4. preparation method according to claim 2, which is characterized in that the lamella of the flake graphite alkene in graphene slurry is horizontal
It is 1-5 μm to average-size, the lamella number of plies is 3-6 layers.
5. preparation method according to claim 1, which is characterized in that in the step S2, by phytic acid solid powder and/
Or phytic acid aqueous solution is added in graphene slurry.
6. preparation method according to claim 1, which is characterized in that in the step S3, Fanglun slurry cake is aramid fiber
1414 pulps.
7. preparation method according to claim 6, which is characterized in that the speed of spinneret is 2-5m/min, the temperature of spinneret
It is 120-200 DEG C.
8. a kind of high performance graphene aramid fiber that preparation method described in any one of -7 obtains according to claim 1,
Wherein, which is graphene coated aramid fiber.
9. high performance graphene aramid fiber according to claim 8, which is characterized in that the high performance graphene virtue
The conductivity of synthetic fibre fiber is 2500-4500S/m.
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| CN110477492A (en) * | 2019-08-15 | 2019-11-22 | 薄其军 | A kind of inherent flame retardant type aramid fabric |
| CN116791229A (en) * | 2022-03-14 | 2023-09-22 | 北京石墨烯研究院 | High-performance graphene modified aramid fiber and preparation method thereof |
| CN117385488A (en) * | 2023-12-12 | 2024-01-12 | 电子科技大学 | Flame-retardant and strength-enhanced graphene modified aramid fiber and preparation method thereof |
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| CN117385488B (en) * | 2023-12-12 | 2024-03-12 | 电子科技大学 | Flame-retardant and strength-enhanced graphene modified aramid fiber and preparation method thereof |
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