CN108587571A - Graphene aerogel intelligence phase change fiber, preparation method and application - Google Patents
Graphene aerogel intelligence phase change fiber, preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of graphene aerogel intelligence phase change fiber, preparation method and applications.The graphene aerogel intelligence phase change fiber includes graphene aerogel fiber, phase-change material and hydrophobic coating, the graphene aerogel fiber, which has, is overlapped the continuous graphene three-dimensional porous network structure formed by graphene sheet layer, the phase-change material is wrapped on the graphene sheet layer and fills and is embedded in the three-dimensional porous network structure, and the hydrophobic coating is uniformly wrapped on the graphene aerogel fiber surface.The graphene aerogel intelligence phase change fiber of the present invention has excellent electricity, flexibility and hydrophobic performance, with adjustable phase-change material load capacity, heat enthalpy value and fusing point, there is good application in terms of phase-change accumulation energy and photothermal conversion and storage, electric heating conversion and storage, and preparation process is simple, reaction condition is mild, controllable, green non-pollution, suitable for large-scale production, application prospect is extensive.
Description
Technical field
The present invention relates to a kind of novel graphite alkene aeroge intelligence phase change fiber more particularly to a kind of graphene aerogel intelligence
Energy phase change fiber and the preparation method and application thereof, belongs to nano-porous materials and technical field of phase change energy storage.
Background technology
Phase change fiber has the function of intelligent thermoregulating, when change dramatically occurs for ambient temperature, the phase-change material meeting in fiber
Solid-liquid or solid-to-solid transition, influence of the buffering temperature change to human body occurs, and then comfortable micro climate ring is built for human body
Border.With the development of wearable/portable electronic product, flexible energy storage device is concerned by people.And with multi-functional, more
The intelligent fiber of response has great demand space as the basic component units of wearable device.How phase change fiber is assigned
Multiple stimulation response performance realizes the functions such as active temperature adjustment, energy storage and automatically cleaning, becomes a significant challenge.
The generation of aeroge originates from last century the '30s, by California, USA Pacific Ocean university chemistry man
A kind of substance that Sterven.S.Kistler is invented unintentionally is commonly called as " freezing smog ", the water in silica gel is extracted, so
Afterwards made of the method with the gas of such as carbon dioxide etc substitution water.By development in more than 80 years, aerogel material was
Commercialization is done step-by-step, there is important application in numerous areas.
The latent heat storage of phase-changing energy storage material is for waste heat produced by ambient enviroment, solar energy and locomotive or electronic device
It utilizes, is a kind of method the most feasible.Organic solid-liquid phase change material has wide transition temperature range, stabilization chemically
Matter, high latent heat, it is inexpensive the advantages that.However since the problems such as its low-heat/conductivity, leakage, limits its application.Find suitable branch
Frame material simultaneously assigns phase-changing energy storage material with high heat/conductivity, good shape stability and high enthalpy of phase change, is particularly heavy
It wants.Currently, the porous materials such as metal foam, carbon aerogels, graphene aerogel, carbon nanotube sponge and carbon nano pipe array
It is used in the research of organic phase change energy storage material, assigns its excellent electricity/thermal conductivity, and can light or electric drive progress thermal energy turn
It changes and stores.Therefore this material of aeroge is utilized to improve the predicament of phase-changing energy storage material, it is extremely feasible and has greatly
Application prospect.
Traditional phase-changing energy storage material is mostly applied to the timbering material of the closing of large scale equipment container or large scale, block
Phase-changing energy storage material.The introducing of wherein aeroge makes phase-change material show the thermal response of good electricity, light, realizes thermal energy
Conversion and Utilization.However this large scale can not be suitable for present flexible wearable equipment and more and more micro- in tradition application
In the electronic circuit of type, therefore the intelligent phase change fiber with good flexibility, electric conductivity will be important as the one of Future Development
Direction.
Demand in view of flexible wearable equipment and the intelligent device being increasingly miniaturized to new material, there is an urgent need to and carry
Go out a kind of structure and the novel intelligent phase-change material of performance and preparation method, it is simple for process, with short production cycle, at low cost to reach
Purpose, give full play to the advantage of phase-changing energy storage material, push the application of phase-change material to a new high degree, and then meet flexible
Wearable device and the growing demand of the intelligent device being increasingly miniaturized.
Invention content
The main purpose of the present invention is to provide a kind of graphene aerogel intelligence phase change fiber and preparation method thereof, with gram
Take deficiency in the prior art.
Another object of the present invention is to provide the application of foregoing graphites alkene aeroge intelligence phase change fiber.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes：
An embodiment of the present invention provides a kind of graphene aerogel intelligence phase change fibers comprising graphene aerogel is fine
Dimension, phase-change material and hydrophobic coating, the graphene aerogel fiber, which has, is overlapped the continuous stone formed by graphene sheet layer
Black alkene three-dimensional porous network structure, the phase-change material are wrapped on the graphene sheet layer and fill that be embedded in the three-dimensional more
In pore network structure, the hydrophobic coating is uniformly wrapped on the graphene aerogel fiber surface.
In some embodiments, the graphene aerogel fiber has by aperture in 2nm micropores below, aperture 2
The mesoporous and aperture of~50nm is the graphene three-dimensional porous network structure that the macro hole of 50nm~500 μm forms, the graphene
The porosity of three-dimensional porous network structure is 1~99%.
Further, in the graphene aerogel intelligence phase change fiber graphene aerogel fiber content be 10~
50wt%.
Further, a diameter of 10 μm~1mm of the graphene aerogel fiber, draw ratio are 10~107, specific surface
Product is 1~1200m20.1~3.5cm of/g, Kong Rongwei3/g。
In some embodiments, in the graphene aerogel intelligence phase change fiber phase-change material content be 1~
99wt%.
Further, the phase-change material include paraffin, polyalcohol, polyethylene glycol, erythrite, alkane, higher aliphatic,
Any one in higher fatty acids and polyolefin or two or more combinations.
In some embodiments, the thickness of the hydrophobic coating is adjustable between 10nm~50 μm, the hydrophobic coating
Material include in fluorocarbon resin, fluorine-carbon modified resin, organic siliconresin, organic-silicon-modified resin and cellulose any one or
Two or more combinations.
The embodiment of the present invention additionally provides the preparation method of foregoing graphites alkene aeroge intelligence phase change fiber comprising：
Graphene aerogel fiber and/or graphene aquagel fibre are provided；
By the way of melting filling and/or solution filling, with phase-change material to the graphene aerogel fiber and/or
Graphene aquagel fibre is filled, and obtains graphene/phase-change material composite fibre；
In the graphene/phase-change material composite fiber surface coated by hydrophobic coating, graphene aerogel intelligence phase is obtained
Become fiber.
In some embodiments, the preparation method includes：Graphene aquagel fibre is prepared by spining technology, later
Processing is dried, obtains graphene aerogel fiber.
Further, the spining technology includes arbitrary in wet spinning, confinement sol gel reaction or freezing dry-spinning
It is a kind of.
Further, the drying process includes freeze-drying and/or supercritical fluid drying.
In some embodiments, the preparation method includes：The leaching of graphene aerogel fiber is placed in molten state phase transformation material
1~12h in material, alternatively, graphene aerogel fiber and/or the leaching of graphene aquagel fibre are placed in phase-change material solution
5min~12h obtains graphene/phase-change material composite fibre later in 20~120 DEG C of dry 1~3h.
Further, the preparation method includes：The graphene/phase-change material composite fibre is impregnated in hydrophobic coating
5s~1h in solution, it is dry after taking-up, it impregnates repeatedly and dry, obtains graphene aerogel intelligence phase change fiber.
The embodiment of the present invention additionally provide foregoing graphites alkene aeroge intelligence phase change fiber in phase-change accumulation energy, intelligent response,
Photothermal conversion and storage, electric heating conversion and the application in storage or flexible wearable devices field.
Compared with prior art, advantages of the present invention includes：
1) graphene aerogel intelligence phase change fiber provided by the invention is mainly by graphene aerogel fiber, phase-change material
It is formed with hydrophobic coating, basis material of the graphene aerogel fiber as the intelligence phase change fiber, there is adjustable diameter, directly
Diameter is 10 μm of -1mm, big draw ratio, draw ratio 10-107, excellent electric heating, photo-thermal, energy storage and woven performance are provided,
And the intelligence phase change fiber has excellent electricity, flexibility and hydrophobic performance, has adjustable phase-change material load capacity, heat content
Value and fusing point；
2) graphene aerogel intelligence phase change fiber preparation process provided by the invention is simple, and reaction condition is mild, controllable,
Low energy consumption, green non-pollution are suitable for large-scale production, and application prospect is extensive；
3) graphene aerogel intelligence phase change fiber provided by the invention can be used for phase-change accumulation energy, photothermal conversion and storage,
In electric heating conversion and storage and flexible wearable device.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments described in invention, for those of ordinary skill in the art, without creative efforts,
Other drawings may also be obtained based on these drawings.
Fig. 1 is a kind of structural schematic diagram of graphene aerogel intelligence phase change fiber in a typical embodiments of the invention.
Fig. 2 a and Fig. 2 b are that the scanning electron of 1 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 3 a and Fig. 3 b are that the scanning electron of 2 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 4 a and Fig. 4 b are that the scanning electron of 3 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 5 a and Fig. 5 b are that the scanning electron of 4 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 6 a and Fig. 6 b are that the scanning electron of 5 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 7 a and Fig. 7 b are that the scanning electron of 6 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention is aobvious respectively
Micro mirror photo.
Fig. 8 a, Fig. 8 b, Fig. 9 a and Fig. 9 b are 7 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention respectively
Electron scanning micrograph.
Figure 10 is the TG curve graphs of 1 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention.
Figure 11 is the DSC curve figure of 1 obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention.
Figure 12 is the contact angle schematic diagram of 1 obtained graphene aerogel intelligence phase change fiber and water of the embodiment of the present invention.
Figure 13 is infrared photograph of 1 the obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention under electro photoluminescence.
Figure 14 is infrared photograph of 1 the obtained graphene aerogel intelligence phase change fiber of the embodiment of the present invention under light stimulus.
Specific implementation mode
In view of deficiency in the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
A kind of graphene aerogel intelligence phase change fiber that the one side of the embodiment of the present invention provides, structure are seen
Shown in Fig. 1, including graphene aerogel fiber, phase-change material and hydrophobic coating, the graphene aerogel fiber have by stone
Black alkene lamella overlaps the continuous graphene three-dimensional porous network structure to be formed, and the phase-change material is wrapped in the graphene film
It on layer and fills and is embedded in the three-dimensional porous network structure, the hydrophobic coating is uniformly wrapped on the graphene aerogel
Fiber surface.
In some embodiments, the graphene aerogel fiber has by aperture in 2nm micropores below, aperture 2
The mesoporous and aperture of~50nm is the continuous graphene three-dimensional porous network structure that the macro hole of 50nm~500 μm forms, and is had
The porosity of woven performance, the graphene three-dimensional porous network structure is 1~99%.
Further, in the graphene aerogel intelligence phase change fiber graphene aerogel fiber content be 10~
50wt%.
Further, basis material of the graphene aerogel fiber as the intelligence phase change fiber has adjustable
Diameter, a diameter of 10 μm~1mm, big draw ratio, draw ratio are 10~107, and excellent electric heating, photo-thermal energy storage and can are provided
Knitting property, specific surface area are 1~1200m20.1~3.5cm of/g, Kong Rongwei3/g。
In some embodiments, the content of phase-change material is adjustable in the graphene aerogel intelligence phase change fiber, be 1~
99wt%, preferably 25~95wt%, especially preferably 55~85wt%.
Further, the phase-change material includes but not limited to paraffin, polyalcohol, polyethylene glycol, erythrite, alkane, height
Any one in grade fatty alcohol, higher fatty acids and polyolefin etc. or two or more combinations.
Further, the latent heat of phase change of the graphene aerogel intelligence phase change fiber is adjustable, preferably 1~300J/g.
In some embodiments, the hydrophobic coating is fine and close, continuous film layer, and is uniformly wrapped on the graphene gas
Gelatinous fibre surface.
Further, the thickness of the hydrophobic coating is adjustable between 10nm~50 μm.
Further, the material of the hydrophobic coating includes but not limited to fluorocarbon resin, fluorine-carbon modified resin, organosilicon tree
Any one in fat, organic-silicon-modified resin and cellulose etc. or two or more combinations.
Further, the fluorocarbon resin includes Teflon series plastics, Kynoar series plastics, chlorotrifluoroethylene
Any one in copolymer series resin and polyvinyl chloride copolymer resin etc. or two or more combinations, but not limited to this.
Further, the organic siliconresin includes organochlorosilane resin, organoalkoxysilane resin, organic acyl-oxygen
Any one in base silane resin, Organosilicon Alcohol in Organic resin etc. or two or more combinations, alternatively, the organic siliconresin packet
It includes：In organochlorosilane, organoalkoxysilane, organic acyloxy silicone hydride, Organosilicon Alcohol in Organic etc. any one or it is two or more
The resin derived is combined, but not limited to this.
Further, the contact angle of the graphene aerogel intelligence phase change fiber is 90~175 °, the hydrophobic coating
Graphene aerogel intelligence phase change fiber is assigned with self-cleaning performance.
Graphene aerogel intelligence phase change fiber provided by the invention mainly by graphene aerogel fiber, phase-change material and
Hydrophobic coating forms, basis material of the graphene aerogel fiber as the intelligence phase change fiber, has adjustable diameter, diameter
For 10 μm of -1mm, big draw ratio, draw ratio 10-107, excellent electric heating, photo-thermal, energy storage and woven performance are provided, and
The intelligence phase change fiber has excellent electricity, flexibility and hydrophobic performance, has adjustable phase-change material load capacity, heat enthalpy value
And fusing point.
The other side of the embodiment of the present invention additionally provides the preparation side of foregoing graphites alkene aeroge intelligence phase change fiber
Method comprising：
Graphene aerogel fiber and/or graphene aquagel fibre are provided；
By the way of melting filling and/or solution filling, with phase-change material to the graphene aerogel fiber and/or
Graphene aquagel fibre is filled, and obtains graphene/phase-change material composite fibre；
In the graphene/phase-change material composite fiber surface coated by hydrophobic coating, graphene aerogel intelligence phase is obtained
Become fiber.
Further, the preparation method may include：
1) prepared by the spinning of graphene aerogel fiber；
2) the melting filling of phase-change material and/or solution filling；
3) hydrophobic coating coats.
In some embodiments, the preparation method includes：Graphene aquagel fibre is prepared by spining technology, later
Processing is dried, obtains graphene aerogel fiber.It simply says, the preparation of the graphene aerogel fiber includes graphite
The spinning and drying of alkene aquagel fibre.
Further, the spining technology includes arbitrary in wet spinning, confinement sol gel reaction or freezing dry-spinning
It is a kind of.
Further, the drying process includes freeze-drying and/or supercritical fluid drying.
Further, the wet spinning includes：Graphene oxide liquid crystal is set to be coagulated to selected by selected needle injection
Gu bath in, after through roller collect, reduction treatment, obtain graphene aquagel fibre.
Especially further, the content of graphene oxide is 0.01~10wt% in the graphene oxide liquid crystal.
Especially further, the internal diameter of the syringe needle be 30 μm~5mm, preferably 50 μm~1500 μm, further preferably
It is 100 μm~500 μm.
Especially further, the coagulating bath includes CaCl2It is solution (aq), anilinechloride solution (aq), dilute hydrochloric acid, dilute
Any one in sulfuric acid, the water of NaOH and alcohol mixed solution, the water of NaOH and tert-butyl alcohol mixed solution, reducing agent solution etc.
Or two or more combinations, but not limited to this.
Especially further, the reducing agent includes HI, ascorbic acid, sodium ascorbate, hydrazine hydrate, ethylenediamine, contains Fe2+
Any one in compound and dopamine etc. or two or more combinations, but not limited to this.
Further, the confinement sol gel reaction includes：Graphene oxide water solution is set to be placed in closed container such as hair
In thin glass tube, and in 100~180 DEG C of hot environments reaction 12~for 24 hours, obtain graphene aquagel fibre, alternatively, making packet
Mixed aqueous solution containing graphene oxide and reducing agent is placed in closed container such as glass capillary, and in 30~95 DEG C of environment
1~12h is reacted, graphene aquagel fibre is obtained.
Wherein, the mass ratio of the graphene oxide and reducing agent is 1：20~20：1.
Especially further, a concentration of 1~10mg/mL of the graphene oxide water solution.
Especially further, the reducing agent includes HI, ascorbic acid, sodium ascorbate, dopamine, ethylenediamine, hydration
Hydrazine, sodium borohydride and contain Fe2+Any one in compound etc. or two or more combinations, but not limited to this.
In some embodiments, the preparation method includes：The leaching of graphene aerogel fiber is placed in molten state phase transformation material
1~12h in material, alternatively, graphene aerogel fiber and/or the leaching of graphene aquagel fibre are placed in phase-change material solution
5min~12h obtains graphene/phase-change material composite fibre later in 20~120 DEG C of dry 1~3h.
Specifically, the method for the melting filling may include：Graphene aerogel fiber is soaked in molten state phase transformation
1~12h in material, then by fabric suspension, 1~3h, cooling acquisition graphene/phase-change material are compound in 20~120 DEG C of environment
Fiber.
Specifically, the method for the solution filling may include：By graphene aerogel fiber and/or graphene hydrogel
Fiber bubble in phase-change material solution 5min~12h, phase-change material solution concentration be 0.01~99wt%, then by fiber in
Suspension is stood with drying under 120 DEG C of atmospheric pressure environments, obtains graphene/phase-change material composite fibre.
Further, the preparation method includes：The graphene/phase-change material composite fibre is impregnated in hydrophobic coating
5s~1h in solution, preferably 3s~1h, it is dry after taking-up, it impregnates repeatedly and dry, obtains graphene aerogel intelligence phase transformation
Fiber.
Especially further, the content of lyophobic dust is 0.01~20wt% in the hydrophobic coating solution.Wherein, institute
It includes but not limited to fluorocarbon resin, fluorine-carbon modified resin, organosilicon to state the material that lyophobic dust is hydrophobic coating above-mentioned
Resin, organic-silicon-modified resin and cellulose etc., specific details are not described herein again.
Especially further, the environment of the drying is normal temperature and pressure or 30~150 DEG C of vacuum.
Especially further, the dipping and dry number are 1~100 time repeatedly.
Graphene aerogel intelligence phase change fiber preparation process provided by the invention is simple, and reaction condition is mild, controllable, low
Energy consumption, green non-pollution are suitable for large-scale production, and application prospect is extensive.
The other side of the embodiment of the present invention additionally provides foregoing graphites alkene aeroge intelligence phase change fiber and is stored up in phase transformation
Energy, intelligent response, photothermal conversion and storage, electric heating conversion and the application in storage or flexible wearable devices field.
Further, the graphene aerogel intelligence phase change fiber is fine when applying external voltage and/or by illumination
It ties up own temperature to increase, and stores heat, realize electric-thermal and/or light- heat transfer and storage.
For example, a kind of phase-changing energy storage material can also be provided in the embodiment of the present invention comprising graphene aerogel intelligence above-mentioned
It can phase change fiber.
In another example a kind of flexible wearable device can also be provided in the embodiment of the present invention, before at least part of component uses
The graphene aerogel intelligence phase change fiber stated.
To sum up, by above-mentioned technical proposal, intelligence phase change fiber provided by the invention mainly by graphene aerogel fiber,
Phase-change material and hydrophobic coating composition, the graphene aerogel fiber have continuous three-dimensional porous network structure, and having can
The diameter of tune, big draw ratio, and the phase-change material be wrapped on graphene sheet layer and be present in graphene sheet layer overlap joint and
At porous structure in, the intelligence phase change fiber surface has fine and close, continuous hydrophobic coating.The intelligence phase change fiber is available
In phase-change accumulation energy, electric heating conversion and storage and photothermal conversion and storage, flexible wearable device.
Below by way of several embodiments and the technical solution that present invention be described in more detail in conjunction with attached drawing.However, selected
Embodiment be merely to illustrate the present invention, and do not limit the scope of the invention.
Embodiment 1
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is spun into HCl/VC by wet spinning to mix
In aqueous solution, graphene aquagel fibre is obtained, subsequent aquagel fibre obtains graphene aerogel fiber through supercritical drying.
(2) preparation of graphene/phase-change material composite fibre：Graphene aerogel fiber is soaked in molten state paraffin
In, and be statically placed in 10h in 100 DEG C of vacuum environments, by the fabric suspension containing paraffin in 80 DEG C of baking ovens 1h to remove fiber table
The residual paraffin in face, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 5s, then
Room temperature is dried, and graphene aerogel intelligence phase change fiber is obtained, wherein hydrophobic coating thickness is 100nm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment is as shown in Figure 2 a and 2 b, TG and
DSC curve is as shown in Figure 10, Figure 11, sees Figure 12 with the contact angle of water, and the electric heating conversion under electro photoluminescence is shown in figure with memory response
13, the photothermal conversion under light stimulus is shown in that Figure 14, structure chart can refer to Fig. 1 with memory response, and related property parameter is shown in Table 1.
Embodiment 2
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is spun into HCl/HI by wet spinning to mix
In aqueous solution, graphene aquagel fibre, the subsequent freeze-dried acquisition graphene aerogel of graphene aquagel fibre are obtained
Fiber.
(2) preparation of graphene/phase-change material composite fibre：Graphene aerogel fiber is soaked in molten state PEG,
And be statically placed in 1h in 80 DEG C of vacuum environments, by the fabric suspension containing paraffin in 80 DEG C of baking ovens 1h to remove the residual of fiber surface
Remaining paraffin, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 10nm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment is as shown in Figure 3a and Figure 3b shows, related property
Parameter is shown in Table 1.
Embodiment 3
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is spun into 10wt%HCl water by wet spinning
It in solution, is then soaked in HI aqueous solutions, obtains graphene aquagel fibre, subsequent freeze-dried acquisition graphene airsetting
Glue fiber.
(2) preparation of graphene/phase-change material composite fibre：Graphene aerogel fiber is soaked in 10wt%PEG
(aq) in, and be statically placed in 1h in 80 DEG C of environment, by the fabric suspension containing paraffin in 80 DEG C of baking ovens 1h to remove fiber surface
Residual paraffin, the cooling of subsequent room temperature obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 50nm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment as shown in figures 4 a and 4b, related property
Parameter is shown in Table 1.
Embodiment 4
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is injected into 5wt%NaOH by wet spinning
In water/ethanol solution, wet gel fiber is obtained, graphite oxide aerogel fiber is then obtained by supercritical drying.Then
Through hydrazine hydrate steam reduction, graphene aerogel fiber is obtained.
(2) preparation of graphene/phase-change material composite fibre：Graphene aerogel fiber is soaked in 20wt%PEG
(aq) in, and be statically placed in 5min in 80 DEG C of environment, by the fabric suspension containing paraffin in 80 DEG C of baking ovens 3h to remove fiber table
The residual paraffin in face, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 200nm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment as shown in figure 5 a and 5b, related property
Parameter is shown in Table 1.
Embodiment 5
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is spun into t-butanol solution by wet spinning
In, subsequent 35 DEG C are soaked in HI aqueous solutions, and water-bath stands 12h, obtains graphene aquagel fibre, subsequent aquagel fibre is through cold
Dry acquisition graphene aerogel fiber is lyophilized.
(2) preparation of graphene/phase-change material composite fibre：It is hard that above-mentioned graphene aerogel fiber is soaked in molten state
In resin acid, and be statically placed in 12h in 60 DEG C of vacuum environments, by the fabric suspension containing paraffin in 120 DEG C of baking ovens 1h to remove fibre
The residual paraffin in dimension table face, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 1 μm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment as shown in figures 6 a and 6b, related property
Parameter is shown in Table 1.
Embodiment 6
(1) preparation of graphene aerogel fiber：By graphene oxide liquid crystal, it is mixed that acetone/water is spun by wet spinning
It closes in solution, is then soaked in HI aqueous solutions, 55 DEG C of water-baths stand 12h, obtain graphene aquagel fibre, and subsequent hydrogel is fine
Dimension obtains graphene aerogel fiber through supercritical drying.
(2) preparation of graphene/phase-change material composite fibre：Above-mentioned airsetting glue fiber is soaked in polyvinyl alcohol water solution
In (30wt%), and be statically placed in 3h in 90 DEG C, by the fabric suspension containing paraffin in 80 DEG C of baking ovens 1h to remove fiber surface
Remaining polyethylene glycol, the cooling of subsequent room temperature obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 10 μm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment as shown in figs. 7 a and 7b, related property
Parameter is shown in Table 1.
Embodiment 7
(1) preparation of graphene aerogel fiber：Graphene oxide liquid crystal is spun into HCl/ ethylenediamines by wet spinning
In mixed aqueous solution, subsequent 75 DEG C of water-baths stand 12h, obtain graphene aquagel fibre, subsequent aquagel fibre is through overcritical
It is dry to obtain graphene aerogel fiber.
(2) preparation of graphene/phase-change material composite fibre：Graphene aerogel fiber is soaked in 35wt%PEG
(aq) in, and be statically placed in 12h in 30 DEG C of atmospheric pressure environments, by the fabric suspension containing paraffin in 120 DEG C of baking ovens 1h to remove fibre
The residual paraffin in dimension table face, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in fluorocarbon resin solution 3-5s, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 20 μm.
The Scanning Electron microscope photo of intelligent phase change fiber obtained by the present embodiment is as shown in Fig. 8 a-9b, related property ginseng
Number is shown in Table 1.
The structure and performance parameter of the graphene aerogel intelligence phase change fiber prepared in 1 embodiment 1-7 of table
Embodiment 8
(1) preparation of graphene aerogel fiber：Using confinement sol gel reaction method, by graphene oxide water solution
It is placed in closed glass capillary, is placed in 100 DEG C of hot environments for 24 hours, a concentration of 1mg/mL of graphene oxide solution is obtained
Graphene aquagel fibre, the subsequent freeze-dried acquisition graphene aerogel fiber of aquagel fibre, a diameter of 10 μm.
(2) preparation of graphene/phase-change material composite fibre：Above-mentioned graphene aerogel fiber is soaked in molten state to gather
In ethylene, and be statically placed in 12h in 60 DEG C of vacuum environments, by the fabric suspension containing polyethylene in 100 DEG C of baking ovens 2h to remove
The residual polyethylene of fiber surface, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in organic siliconresin solution 1h, with
Room temperature is dried afterwards, obtains graphene aerogel intelligence phase change fiber, wherein hydrophobic coating thickness is 15 μm.
Embodiment 9
(1) preparation of graphene aerogel fiber：Using confinement sol gel reaction method, by graphene oxide water solution
It is placed in closed glass capillary, is placed in 12h in 180 DEG C of hot environments, a concentration of 10mg/mL of graphene oxide solution,
Obtain graphene aquagel fibre, the subsequent freeze-dried acquisition graphene aerogel fiber of aquagel fibre, a diameter of 100 μ
m。
(2) preparation of graphene/phase-change material composite fibre：It is red that above-mentioned graphene aerogel fiber is soaked in molten state
In moss alcohol, and be statically placed in 12h in 60 DEG C of vacuum environments, by the fabric suspension containing erythrite in 20 DEG C of baking ovens 3h to remove fibre
The remaining erythrite in dimension table face, subsequent room temperature cooling, obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in organic-silicon-modified resin solution
0.5h, subsequent room temperature are dried, and graphene aerogel intelligence phase change fiber is obtained, wherein hydrophobic coating thickness is 30 μm.
Embodiment 10
(1) preparation of graphene aerogel fiber：Using confinement sol gel reaction method, by graphene oxide water solution
It is placed in closed glass capillary, is placed in 18h in 150 DEG C of hot environments, a concentration of 8mg/mL of graphene oxide solution is obtained
Obtain graphene aquagel fibre, the subsequent freeze-dried acquisition graphene aerogel fiber of aquagel fibre, a diameter of 1mm.
(2) preparation of graphene/phase-change material composite fibre：Above-mentioned graphene aerogel fiber is soaked in higher aliphatic
5min in alcoholic solution, and it is statically placed in 12h in 60 DEG C of vacuum environments, by the fabric suspension containing higher aliphatic in 120 DEG C of baking ovens
For middle 1h to remove the remaining higher aliphatic of fiber surface, subsequent room temperature cooling obtains graphene/phase-change material composite fibre.
(3) preparation of hydrophobic coating：Graphene/phase-change material composite fibre is soaked in cellulose solution 0.5h, then
Room temperature is dried, and graphene aerogel intelligence phase change fiber is obtained, wherein hydrophobic coating thickness is 50 μm.
Pass through embodiment 1-10, it is found that the graphene aerogel intelligence obtained by the above-mentioned technical proposal of the present invention
Energy phase change fiber has excellent electricity, flexibility and hydrophobic performance, has adjustable phase-change material load capacity, heat enthalpy value and melts
Point has good application, and preparation process letter in terms of phase-change accumulation energy and photothermal conversion and storage, electric heating conversion and storage
Mildly, controllably, low energy consumption, green non-pollution is suitable for large-scale production to single, reaction condition, has huge application prospect.
In addition, mode of the inventor referring also to embodiment 1-10, with the other raw materials and item listed in this specification
Part etc. is tested, and has equally been made and has been realized thermal energy storage and release with flexible, super-hydrophobic, heat/optical electrical multiple response
The graphene aerogel intelligence phase change fiber of function.
It should be appreciated that above-described is only some embodiments of the present invention, it is noted that for the common of this field
For technical staff, under the premise of not departing from the concept of the present invention, other modification and improvement can also be made, these are all
It belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of graphene aerogel intelligence phase change fiber, it is characterised in that including graphene aerogel fiber, phase-change material and
Hydrophobic coating, the graphene aerogel fiber, which has, is overlapped the three-dimensional porous net of continuous graphene formed by graphene sheet layer
Network structure, the phase-change material are wrapped on the graphene sheet layer and fill and be embedded in the three-dimensional porous network structure,
The hydrophobic coating is uniformly wrapped on the graphene aerogel fiber surface.
2. graphene aerogel intelligence phase change fiber according to claim 1, it is characterised in that：The graphene aerogel
The content of graphene aerogel fiber is 10~50wt% in intelligent phase change fiber；Preferably, the graphene aerogel fiber
It is formed with the macro hole that the mesoporous and aperture for being 2~50nm in 2nm micropores below, aperture by aperture is 50nm~500 μm
Graphene three-dimensional porous network structure；Preferably, the porosity of the graphene three-dimensional porous network structure is 1~99%；It is excellent
Choosing, a diameter of 10 μm~1mm of the graphene aerogel fiber, draw ratio is 10~107, specific surface area be 1~
1200m20.1~3.5cm of/g, Kong Rongwei3/g。
3. graphene aerogel intelligence phase change fiber according to claim 1, it is characterised in that：The graphene aerogel
In intelligent phase change fiber the content of phase-change material be 1~99wt%, preferably 25~95wt%, especially preferably 55~
85wt%；Preferably, the phase-change material includes paraffin, polyalcohol, polyethylene glycol, erythrite, alkane, higher aliphatic, height
Any one in grade aliphatic acid and polyolefin or two or more combinations；Preferably, the graphene aerogel intelligence phase transformation
The latent heat of phase change of fiber is 1~300J/g.
4. graphene aerogel intelligence phase change fiber according to claim 1, it is characterised in that：The hydrophobic coating is to cause
Close, continuous film layer, and it is uniformly wrapped on the graphene aerogel fiber surface；Preferably, the thickness of the hydrophobic coating
For 10nm~50 μm；Preferably, the material of the hydrophobic coating includes fluorocarbon resin, fluorine-carbon modified resin, organic siliconresin, has
Any one in machine Si modification resin and cellulose or two or more combinations；Especially preferred, the fluorocarbon resin includes
Teflon series plastics, Kynoar series plastics, chlorotrifluoroethylene series plastics and polyvinyl chloride copolymer tree
Any one in fat or two or more combinations；Especially preferred, the organic siliconresin includes organochlorosilane resin, has
Any one in machine alkoxy silane resin, organic acyloxy silicone hydride resin and Organosilicon Alcohol in Organic resin or two or more groups
It closes；Preferably, the contact angle of the graphene aerogel intelligence phase change fiber and water is 90~175 °.
5. the preparation method of the graphene aerogel intelligence phase change fiber as described in any one of claim 1-4, feature exist
In including：
Graphene aerogel fiber and/or graphene aquagel fibre are provided；
By the way of melting filling and/or solution filling, with phase-change material to the graphene aerogel fiber and/or graphite
Alkene aquagel fibre is filled, and obtains graphene/phase-change material composite fibre；
In the graphene/phase-change material composite fiber surface coated by hydrophobic coating, it is fine to obtain the phase transformation of graphene aerogel intelligence
Dimension.
6. preparation method according to claim 5, it is characterised in that including：Graphene hydrogel is prepared by spining technology
Processing is dried in fiber later, obtains graphene aerogel fiber；Preferably, the spining technology includes wet spinning, limit
Domain sol gel reaction or freezing dry-spinning in any one；Preferably, the drying process includes freeze-drying and/or surpasses
Supercritical fluid drying；
Especially preferred, the wet spinning includes：Graphene oxide liquid crystal is set to pass through selected needle injection to selected coagulating bath
In, after through collect, reduction treatment, obtain graphene aquagel fibre；It is especially preferred, oxygen in the graphene oxide liquid crystal
The content of graphite alkene is 0.01~10wt%；Especially preferred, the internal diameter of the syringe needle is 30 μm~5mm, preferably 50 μm
~1500 μm, further preferably 100 μm~500 μm；Especially preferred, the coagulating bath includes CaCl2Solution, aniline hydrochloric acid
Salting liquid, dilute hydrochloric acid, dilute sulfuric acid, the water of NaOH and alcohol mixed solution, the water of NaOH and tert-butyl alcohol mixed solution, reducing agent are molten
Any one in liquid or two or more combinations；It is especially preferred, the reducing agent include HI, ascorbic acid, sodium ascorbate,
Hydrazine hydrate, contains Fe at ethylenediamine2+Any one in compound and dopamine or two or more combinations；
Especially preferred, the confinement sol gel reaction includes：Graphene oxide water solution is set to be placed in closed container, and
React 12 in 100~180 DEG C~for 24 hours, graphene aquagel fibre is obtained, alternatively, making comprising graphene oxide and reducing agent
Mixed aqueous solution is placed in closed container, and reacts 1~12h in 30~95 DEG C, obtains graphene aquagel fibre；Particularly preferably
, the mass ratio of the graphene oxide and reducing agent is 1：20~20：1；It is especially preferred, the graphene oxide water solution
A concentration of 1~10mg/mL；Especially preferred, the reducing agent includes HI, ascorbic acid, sodium ascorbate, dopamine, second
Diamines, hydrazine hydrate, sodium borohydride and contain Fe2+Any one in compound or two or more combinations.
7. preparation method according to claim 5, it is characterised in that including：The leaching of graphene aerogel fiber is placed in melting
1~12h in state phase-change material, alternatively, graphene aerogel fiber and/or the leaching of graphene aquagel fibre are placed in phase-change material
5min~12h in solution obtains graphene/phase-change material composite fibre later in 20~120 DEG C of dry 1~3h；Preferably,
A concentration of 0.01~99wt% of the phase-change material solution.
8. preparation method according to claim 5, it is characterised in that including：By the compound fibre of graphene/phase-change material
Dimension is impregnated in 5s~1h in hydrophobic coating solution, dry after taking-up, impregnates repeatedly and dry, obtains graphene aerogel intelligence phase
Become fiber；Preferably, the content of lyophobic dust is 0.01~20wt% in the hydrophobic coating solution；Preferably, the leaching
The time of stain is 3s~1h；Preferably, the environment of the drying is normal temperature and pressure or 30~150 DEG C of vacuum；Preferably, institute repeatedly
The number for stating dipping and drying is 1~100 time.
9. claim 1-4 any one of them graphene aerogel intelligence phase change fibers are in phase-change accumulation energy, intelligent response, photo-thermal
Conversion and storage, electric heating conversion and the application in storage or flexible wearable devices field.
10. application according to claim 9, it is characterised in that including：To claim 1-4 any one of them graphenes
Aeroge intelligence phase change fiber applies external voltage and/or illumination, the temperature liter of the graphene aerogel intelligence phase change fiber
Height, and heat is stored, realize photothermal conversion and storage and/or electric heating conversion and storage.
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