CN105603580A - Preparing method for oriented graphene oxide fibers - Google Patents
Preparing method for oriented graphene oxide fibers Download PDFInfo
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- CN105603580A CN105603580A CN201511030637.6A CN201511030637A CN105603580A CN 105603580 A CN105603580 A CN 105603580A CN 201511030637 A CN201511030637 A CN 201511030637A CN 105603580 A CN105603580 A CN 105603580A
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
Abstract
The invention belongs to the technical field of preparation of graphene fiber materials and particularly relates to a preparing method for oriented graphene oxide fibers. The preparing method comprises the following steps that graphene oxide is prepared with lamellar graphene as a raw material, and a graphene oxide spinning solution is prepared; with a wet spinning method, the graphene oxide spinning solution flows into a solidifying solution, and primary graphene oxide fibers are prepared; at a certain temperature, the graphene oxide fibers are subjected to radial stretching and drying, and the oriented graphene oxide fibers are obtained. The preparing method is easy to implement and low in cost, the stretching rate of the fibers can be precisely controlled, and a good stretching effect can be achieved. The oriented graphene oxide fibers prepared through the method are significantly improved on the aspect of tensile strength compared with the primary graphene oxide fibers, a simple and effective method is provided for preparing high-performance fiber materials based on graphene, and the application of the graphene fibers in practical production and living can be promoted.
Description
Technical field
The present invention relates to a kind of preparation method who is orientated graphene oxide fiber, belong to graphene fiber material preparation technology neckTerritory.
Background technology
Graphene since 2004 are found, has just obtained people's extensive concern as a kind of novel two-dimensional material. LogicalCross the single or multiple lift Graphene that CVD method or epitaxial growth method make and there is excellent mechanics, electricity, thermal property, makeIt all will have application very widely in fields such as structural material, energy storage device, electronic device, inductors.
Along with epoch development, various fibrous materials have become requisite element in people's productive life, how willGraphene sheet layer is assembled into macroscopical one dimension fibre material, realizes Graphene application in practice, is present stage people needsThe challenge facing. Based on this, the research work of the fibrous material of Graphene launches in succession. As CVD method or wet spinning legal systemStandby (CNT) fiber of the CNT based on graphene sheet layer and carbon fiber have mechanical performance and the electric property of superelevation.And these the two kinds experiment conditions of preparing fiber are all comparatively harsh. Adopt wet spinning process to make graphene sheet layer along axially-alignedThe fibrous material based on Graphene, compared with the preparation process of first two fiber, it is gentle many that experiment condition is wanted, Er QieqiPreparation method is easy to expanding production, is convenient to prepare a large amount of macroscopical one dimension fibre materials.
In order further to improve fibre property, much research is using the degree of orientation that improves fiber as a kind of approach, as spinning processMiddle rotation solidification liquid, thus the stretching action that makes fiber be subject to solution in forming process plays certain stretching effect to fiberReally, or adopt one step hydro thermal method to utilize template to prepare graphene oxide (GO) fiber of high orientation, but be all difficult to expandLarge to industrial level, limit its practical application.
Summary of the invention
Therefore, inventing technical problem to be solved is to overcome prior art and is difficult to provide effectively and can be used for expanding productionThe degree of orientation of raising graphene oxide fiber, thereby improve the mechanical performance of fiber and realize the method for practical application.
, the invention provides effectively and the preparation method of a kind of high-mechanical property orientation graphene oxide fiber that can expanding production for this reason,Comprise the following steps: prepare graphene oxide taking lamella graphite as raw material, and configure graphene oxide spinning solution; Pass through wet methodSpin processes graphene oxide spinning solution flows into solidification liquid, prepares primary graphene oxide fiber; At a certain temperature, to oxygenFunctionalized graphene fiber carries out radial drawing and dry, obtains product.
Further, described uniform temperature is 40 DEG C~70 DEG C, and be 5~48h described drying time.
Particularly, described graphite is inflatable crystalline flake graphite, and graphite is of a size of 300 μ m~500 μ m.
Particularly, the concentration of described graphene oxide spinning solution is 5mg/ml~20mg/ml.
Further, described graphene oxide concentration of dope is 5mg/ml~15mg/ml.
Further, the solvent of described graphene oxide spinning solution be polar organic solvent, the aqueous solution or polar organic solvent andThe mixed liquor of the aqueous solution.
Particularly, described polar organic solvent is any one in methyl alcohol, propyl alcohol, butanols, DMF, acetonitrile.
Further, described solidification liquid is for containing bivalent ions salts solution, the bases aqueous solution, containing positive charge moleculesThe aqueous solution or polymer, amine alcoholic solution or the amine aqueous solution in any one or multiple mixture.
Particularly, described solidification liquid is CaCl2The aqueous solution, CuSO4The aqueous solution, the NaOH aqueous solution, the KOH aqueous solution, CTAB,The mixture of any one or a few in shitosan.
As preferably, the speed of described wet spinning process is 0.3ml/min~0.8ml/min, selected spinning syringe needleInternal diameter is 0.25mm~1mm.
The preparation method of a kind of high-mechanical property orientation graphene oxide fiber of the present invention has the following advantages:
(1) a kind of preparation method who is orientated graphene oxide fiber of the present invention, by with the standby large lamella of lamella graphite-madeGraphene oxide, and prepare graphene oxide spinning solution, improve graphene oxide lamella size, make lamella in spinningIn journey, realize more effective stackingly, improve the mechanical performance of graphene oxide fiber.
(2) a kind of preparation method who is orientated graphene oxide fiber of the present invention, adopts wet spinning process, makes to be liquid crystalline phaseGraphene oxide spinning solution under the effect of shear stress and coagulating agent, self assembly forms primary graphene oxide fiber.
(3) a kind of preparation method who is orientated graphene oxide fiber of the present invention, by by the primary graphene oxide fibre makingDimension is arranged and is fixed on stretching device, and at a certain temperature fiber is done to stretch processing, and the breakthrough discovery of the present invention is executedAdd uniform temperature, energy is the effect between enhancement Layer further, is conducive to improve the mechanical performance of graphene oxide fiber; And logicalCross the speed of controlling wet spinning, restrained stretching speed, reaches optimum drawing effect, improves the machine of graphene oxide fiberTool performance.
(4) a kind of preparation method who is orientated graphene oxide fiber of the present invention, by researching condensed solid-liquid to graphene oxide fibreThe impact of the mechanical performance of dimension, finds can also promote coagulating agent and graphene oxide sheet in the time selecting amine as solidifying liqReaction on layer between group, improves the adhesion of graphene oxide sheet interlayer, is conducive to improve the machine of graphene oxide fiberTool performance.
(5) a kind of preparation method who is orientated graphene oxide fiber of the present invention, the graphene oxide fiber of preparing orientationWell, mechanical performance is high and preparation method simple and be easy to suitability for industrialized production, can be widely used in graphene fiber material systemStandby technical field.
Brief description of the drawings
Fig. 1 is primary graphene oxide fiber SEM figure in embodiment 1;
Fig. 2 is the SEM figure that is orientated graphene oxide fiber in embodiment 1.
Fig. 3 is the primary graphene oxide fiber in embodiment 1 and the mechanical property figure that is orientated graphene oxide fiber.
Detailed description of the invention
Embodiment 1
The preparation method of orientation graphene oxide fiber, comprises the following steps: prepare graphene oxide taking lamella graphite as raw material,And configure graphene oxide spinning solution; Flow into solidification liquid by wet spinning process graphene oxide spinning solution, prepare primary solidifyingGlue graphene oxide fiber; At a certain temperature, graphene oxide fiber is carried out to radial drawing and dry, obtain product.
The preparation of graphene oxide: take 5g, the inflatable natural flake graphite of 300 μ m, add the 200mL concentrated sulfuric acid and50mL fuming nitric aicd, slowly pours mixture in 2L deionized water after stirring at normal temperatures 24h, with diameter be 90mm,Aperture is the cellulose membrane suction filtration of 0.2um and washs twice by deionized water, after washing, at 60 DEG C, dries 24h. To doGraphite after the dry 30s that expands under 1000 DEG C of high temperature, obtains expanded graphite. Add the 200mL concentrated sulfuric acid, 13.2gK2S2O8And 16.2gP2O5Stir 5h at 80 DEG C of constant temperature, mixed liquor is poured in 2L deionized water, to be cooled to room temperature, with straightFootpath is 90mm, and the cellulose membrane suction filtration that aperture is 0.2um also washs twice by deionized water, is placed in drying 48h under room temperature.After dry, added in the 200mL concentrated sulfuric acid, under ice bath, slowly added 15g potassium permanganate, fully stirred, at 35 DEG CReaction 5h, slowly pours mixed liquor in 2L deionized water, waits solution to be cooled to 50 DEG C of peroxides that add 20mL30%Change hydrogen solution, become pale yellow solution to solution. Leave standstill 1 day, pour out supernatant liquid, with deionized water centrifuge washing 2Time, 1mol/L dilute hydrochloric acid solution centrifuge washing 2 times, then with deionized water centrifuge washing until the GO aqueous solution is neutral,To the graphene oxide solution of large lamella, make graphene oxide solution.
The preparation of spinning solution: get the graphene oxide solution 200ml making, be placed at 50 DEG C of oil bath pans, stir concentrated,The graphene oxide spinning solution that is 8mg/ml to concentration.
The preparation of aniline solidification liquid: the aniline alcoholic solution of preparation mass fraction 5% is as solidification liquid.
Primary graphene oxide fiber preparation: utilize mechanical syringe pump, selecting internal diameter is the spinning syringe needle of 0.43mm, passes throughSyringe pump is pushed syringe spinning solution is injected in solidification liquid with the speed of 0.3ml/min, forms primary graphene oxideFiber.
The preparation of orientation graphene oxide fiber: the primary gel graphene oxide fiber making is vertically arranged and is fixed on stretchingOn device, under the auxiliary baking of infrared lamp, wherein baking temperature is controlled at 60 DEG C of left and right, and slow stretching fiber, then by fibreDimension is placed in dry 5h under room temperature and obtains being orientated graphene oxide fiber.
As depicted in figs. 1 and 2, respectively primary graphene oxide fiber and orientation graphene oxide fiber are scannedElectron microscope (SEM) test, the primary graphene oxide fiber of Fig. 1, axially the fold of graphene oxide lamella is brighterAobvious, the degree of orientation is not high; And the graphene oxide fiber of the stretched processing of Fig. 2, graphene oxide lamella is axially presentingMore perfect orientations.
As shown in Figure 3, respectively primary graphene oxide fiber and orientation graphene oxide fiber are carried out to Mechanics Performance Testing,For the mechanical performance comparison diagram of fiber before and after stretching, can obviously find out, the pulling force characteristic of orientation graphene oxide fiber is 350Mpa, the pulling force characteristic of primary graphene oxide fiber, at 280MPa, illustrates that the mechanical performance of orientation graphene oxide fiber is brightAobvious higher than primary graphene oxide fiber.
Embodiment 2
The preparation method of orientation graphene oxide fiber and the difference of embodiment 1 of the present embodiment are: (1) oxidationGraphene preparation process, also comprises the graphene oxide solution making, and through freeze drying 5 days, prepares solid oxygen fossilChina ink alkene. (2) preparation of spinning solution: solid oxide Graphene is scattered in to DMF solution and does in solvent, ultrasonic 15min obtainsTo the graphene oxide solution of 10mg/ml, obtain the graphene oxide spinning solution that homogeneous disperses. All the other and embodiment 1Preparation method identical, do not repeat them here.
Embodiment 3
The preparation of graphene oxide: difference from Example 1 is: selecting lamella size is the inflatable sky of 500 μ mRight crystalline flake graphite is prepared graphene oxide as raw material, and all the other are identical with the preparation of the graphene oxide of embodiment 1.
Preparing of spinning solution: get the graphene oxide solution 200ml making, be placed at 50 DEG C of oil bath pans, stir concentrated,The graphene oxide spinning solution that is 5mg/ml to concentration.
The preparation of solidification liquid: the ethylenediamine solution of preparation mass fraction 5% is as solidification liquid.
Primary graphene oxide fiber preparation: utilize mechanical syringe pump, selecting internal diameter is the spinning syringe needle of 0.43mm, passes throughSyringe pump is pushed syringe spinning solution is injected in solidification liquid with the speed of 0.3ml/min, forms primary graphene oxideFiber.
The preparation of orientation graphene oxide fiber: the primary graphene oxide fiber making is vertically arranged and is fixed on stretching deviceUpper, under the auxiliary baking of infrared lamp, wherein baking temperature is controlled at 40 DEG C of left and right, and slow stretching fiber, then puts fiberIn vacuum drying chamber, dry 48h obtains being orientated graphene oxide fiber.
Embodiment 4
The preparation of graphene oxide: with embodiment 3.
Preparing of spinning solution: get the graphene oxide solution 200ml making, be placed at 50 DEG C of oil bath pans, stir concentrated,The graphene oxide spinning solution that is 15mg/ml to concentration.
The preparation of solidification liquid: the CuSO of preparation mass fraction 5%4The aqueous solution is as solidification liquid.
Primary graphene oxide fiber preparation: utilize mechanical syringe pump, selecting internal diameter is the spinning syringe needle of 1mm, by notePenetrate pump and push syringe spinning solution is injected in solidification liquid with the speed of 0.8ml/min, form primary graphene oxide fibreDimension.
The preparation of orientation graphene oxide fiber: the primary graphene oxide fiber making is vertically arranged and is fixed on stretching deviceUpper, under the auxiliary baking of infrared lamp, wherein baking temperature is controlled at 65 DEG C of left and right, and slow stretching fiber, then puts fiberIn vacuum drying chamber, dry 24h obtains being orientated graphene oxide fiber.
Embodiment 5
The preparation of graphene oxide: with embodiment 1.
Preparing of spinning solution: get the large lamella graphene oxide solution 200ml making, be placed at 55 DEG C of oil bath pans, stir denseContracting, obtaining concentration is the graphene oxide spinning solution of 8mg/ml.
The preparation of solidification liquid: the NaOH aqueous solution that preparation mass fraction is 10% is as solidification liquid.
Primary graphene oxide fiber preparation: utilize mechanical syringe pump, selecting internal diameter is the spinning syringe needle of 0.25mm, passes throughSyringe pump is pushed syringe spinning solution is injected in solidification liquid with the speed of 0.2ml/min, forms primary graphene oxideFiber.
The preparation of orientation graphene oxide fiber: the primary gel graphene oxide fiber making is vertically arranged and is fixed on stretchingOn device, under the auxiliary baking of infrared lamp, wherein baking temperature is controlled at 70 DEG C of left and right, and slow stretching fiber, then by fibreDimension is placed in the dry 36h of vacuum drying chamber and obtains being orientated graphene oxide fiber.
Embodiment 6
The preparation of graphene oxide: with embodiment 1.
Preparing of spinning solution: get the graphene oxide solution 200ml making, be placed at 50 DEG C of oil bath pans, stir concentrated,The graphene oxide spinning solution that is 15mg/ml to concentration.
The preparation of solidification liquid: the CTAB solution of preparation 0.5mg/ml is as solidification liquid.
Primary graphene oxide fiber preparation: utilize mechanical syringe pump, selecting internal diameter is the spinning syringe needle of 0.43mm, passes throughSyringe pump is pushed syringe spinning solution is injected in solidification liquid with the speed of 0.3ml/min, forms primary graphene oxideFiber.
The preparation of orientation graphene oxide fiber: the primary graphene oxide fiber making is vertically arranged and is fixed on stretching deviceUpper, under the auxiliary baking of infrared lamp, wherein baking temperature is controlled at 60 DEG C of left and right, and slow stretching fiber, then puts fiberIn vacuum drying chamber, dry 48h obtains being orientated graphene oxide fiber.
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment. ForThose of ordinary skill in the field, can also make other multi-form variation or change on the basis of the above descriptionMoving. Here without also giving exhaustive to all embodiments. And apparent variation or the change of being extended out thusAmong the moving still protection domain in the invention.
Claims (10)
1. a preparation method who is orientated graphene oxide fiber, is characterized in that, comprises the following steps:
Prepare graphene oxide taking lamella graphite as raw material, and configure graphene oxide spinning solution; Be oxidized by wet spinning processGraphene spinning solution flows into solidification liquid, prepares primary graphene oxide fiber; At a certain temperature, to graphite oxideAlkene fiber carries out radial drawing and dry, obtains product.
2. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described uniform temperatureBe 40 DEG C-70 DEG C, the described dry time is 5-48h.
3. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described graphite is canExpansion crystalline flake graphite, graphite is of a size of 300 μ m~500 μ m.
4. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described graphite oxideThe concentration of alkene spinning solution is 5mg/ml~20mg/ml.
5. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described graphite oxideAlkene concentration of dope is 5mg/ml~15mg/ml.
6. according to the preparation method of the orientation graphene oxide fiber described in claim 1 or 3, it is characterized in that: described oxidationThe solvent of Graphene spinning solution is the mixed liquor of polar organic solvent, the aqueous solution or polar organic solvent and the aqueous solution.
7. the preparation method of orientation graphene oxide fiber according to claim 5 in, is characterized in that: described polarity hasMachine solution is any one in methyl alcohol, propyl alcohol, butanols, DMF, acetonitrile.
8. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described solidification liquid isContain bivalent ions salts solution, the bases aqueous solution, the aqueous solution that contains positive charge molecules or polymer, amineAny one in alcoholic solution or the amine aqueous solution or multiple mixture.
9. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described solidification liquid isCaCl2The aqueous solution, CuS04Any one in the aqueous solution, the NaOH aqueous solution, the KOH aqueous solution, CTAB, shitosanOr several mixture.
10. the preparation method of orientation graphene oxide fiber according to claim 1, is characterized in that: described wet spinningThe speed of method is 0.2ml/min~0.8ml/min, and selected spinning syringe needle internal diameter is 0.25mm~1mm.
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Cited By (5)
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CN110512311A (en) * | 2019-09-09 | 2019-11-29 | 苏州大学 | A method of utilizing microflow control technique controllable preparation graphene fiber |
CN110655689A (en) * | 2019-10-22 | 2020-01-07 | 戴章 | Graphene nanocomposite with heat resistance |
CN110699779A (en) * | 2019-11-01 | 2020-01-17 | 常州富烯科技股份有限公司 | Graphene oxide fiber cloth and preparation method thereof, and graphene gas diffusion film and preparation method thereof |
CN111058107A (en) * | 2019-12-12 | 2020-04-24 | 杭州高烯科技有限公司 | Graphene oxide stretchable solution and preparation method and application thereof |
CN115341307A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | High-orientation-degree graphene oxide fiber and preparation method thereof |
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CN103741264A (en) * | 2013-11-14 | 2014-04-23 | 南京新月材料科技有限公司 | Method for preparing graphene fibers through self-assembly of large lamellar graphene oxide |
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CN103741264A (en) * | 2013-11-14 | 2014-04-23 | 南京新月材料科技有限公司 | Method for preparing graphene fibers through self-assembly of large lamellar graphene oxide |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110512311A (en) * | 2019-09-09 | 2019-11-29 | 苏州大学 | A method of utilizing microflow control technique controllable preparation graphene fiber |
CN110512311B (en) * | 2019-09-09 | 2022-12-30 | 苏州大学 | Method for controllably preparing graphene fibers by utilizing microfluidic technology |
CN110655689A (en) * | 2019-10-22 | 2020-01-07 | 戴章 | Graphene nanocomposite with heat resistance |
CN110699779A (en) * | 2019-11-01 | 2020-01-17 | 常州富烯科技股份有限公司 | Graphene oxide fiber cloth and preparation method thereof, and graphene gas diffusion film and preparation method thereof |
CN110699779B (en) * | 2019-11-01 | 2022-05-13 | 常州富烯科技股份有限公司 | Graphene oxide fiber cloth and preparation method thereof, and graphene gas diffusion film and preparation method thereof |
CN111058107A (en) * | 2019-12-12 | 2020-04-24 | 杭州高烯科技有限公司 | Graphene oxide stretchable solution and preparation method and application thereof |
CN111058107B (en) * | 2019-12-12 | 2024-03-05 | 杭州高烯科技有限公司 | Graphene oxide stretchable solution and preparation method and application thereof |
CN115341307A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | High-orientation-degree graphene oxide fiber and preparation method thereof |
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