CN109320286A - The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure - Google Patents
The magnetic graphite alkenyl aerogel material and preparation method thereof for having ordered structure Download PDFInfo
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Abstract
The invention discloses a kind of magnetic graphite alkenyl aerogel materials and preparation method thereof for having ordered structure, belong to new material technology field.The preparation method is using magnetic polymer nanofiber as regulatory factor, pass through ice template method and be orderly crosslinked the three-dimensional net structure of simultaneously orientations by magnetic field orientating technology and orientation Refrigeration Technique formation magnetic polymer nanofiber and graphene sheet layer, so that the structure for realizing the orderly magnetic graphite alkenyl aerogel material of microstructure is constructed.The ordered structure graphene aerogel material is expected to be applied to the device under the field of force, electric field, magnetic field or complicated field with functions such as sensing, drivings.
Description
Technical field
The present invention relates to graphene aerogel materials, belong to new material technology field, have orderly more particularly to one kind
Magnetic graphite alkenyl aerogel material of structure and preparation method thereof.
Background technique
Graphene is by sp2Two with honeycomb structure and only single atomic layer level thickness of hydbridized carbon atoms composition
Tie up thin slice.Aerogel material is using special process the liquid gas displacement in wet gel, and does not significantly change gel
The structure and volume of network, with the three-dimensional porous material of low-density and high-specific surface area obtained from.Existing graphene
Aeroge is mainly used in the fields such as catalysis, absorption, heat-insulated, energy conversion, and what is made full use of is the excellent electrical property of graphene
And the characteristics of aeroge high-specific surface area.But due in graphene hydrogel backbone in the preparation process of graphene aerogel
There are surface tension for portion's solvent, can occur under drying skeleton collapse and structure is destroyed, cause three inside graphene aerogel
Dimension space structure is unable to get effective control, while the graphene aerogel functional limitation prepared is in chemical property and suction
Attached performance limits the application of graphene aerogel.Therefore, real simultaneously in the preparation process of graphene-based aeroge
Now become the bottleneck for restricting graphene-based aerogel material development to the regulation of structure and functionalization.Such as: Chinese invention patent
It is natural that application (application publication number: CN106006615A applies for publication date: 2016-10-12) discloses a kind of graphene aerogel
Dry preparation method.After graphene oxide solution and borax are mixed as reducing agent using ethylenediamine the invention provides one kind again
The preparation method of graphene aerogel is prepared using natural drying.The invention promotes the rigid of aeroge using borate crosslinks effect
It spends and reduces the capillary force in drying process.This method preparation process is simply easily controllable, obtains graphene aerogel mechanical property
Can be excellent, production cost is low, is easy to produce in batches.But this method is larger by extraneous effect of natural conditions, needs external environment
In a kind of relatively stable and suitable condition, it is difficult to effectively be promoted and applied in the whole nation or global range.Simultaneously should
Aeroge does not show good electric property, has limitation in application aspect.
Chinese invention patent application (application publication number: CN106044752A applies for publication date: 2016-10-26) discloses
A kind of preparation method of highly oriented graphene aerogel: graphene or graphene oxide dispersion are placed in electroded container
In, the method being orientated by extra electric field obtains highly oriented graphene or graphene oxide dispersion, continues that electric field is kept to make
With the cryocoagulation in liquid nitrogen, by obtaining highly oriented graphene aerogel after freeze-drying or supercritical drying.The method is
Induce graphene sheet layer that orientations occur by electric field action, graphene sheet layer quality requirement is higher to preparing, while to not
Conductive or poor electric conductivity material is unable to get effective application.
Chinese invention patent application (application publication number CN103977748A applies for publication date: 2015-10-28) is open
A kind of magnetic graphite alkenyl aerogel material and preparation method thereof: with graphene oxide for carrier loaded Fe 3 O 4 magnetic
Nanoparticle acts on its morphological stability of enhancing using carbon nanotube as skeleton or by calcium ion crosslinking, freeze-dried to obtain
The magnetic graphite alkenyl airsetting that graphene oxide magnetism aeroge obtains graphene magnetic graphite alkenyl aeroge, but obtains
Irregular distribution is presented in glue internal structure, causes its properties bad.
Chinese invention patent application (application publication number CN107140620A applies for publication date: 2017-09-08) is open
A kind of preparation method of magnetic graphite alkenyl aeroge: after the amine-modified graphene oxide of DOPA and iron ion crosslinking, pass through
Heating reduction, is self-assembled into three-dimensional grapheme hydrogel structure, and by being freeze-dried and being heat-treated, reduction obtains magnetic graphene
Base aerogel material.This method preparation process is complicated and magnetic because subcategory is single, and can not reach for the different magnetic factors has
Application effect is imitated, the magnetic graphite alkenyl aerogel material function being prepared is more single.
Since graphene aerogel possesses the high feature of bigger serface, porosity, effect has been obtained in adsorbing domain
With as Chinese invention patent application (application publication number CN106006616A applies for publication date: 2016-10-12) discloses one
The preparation method of kind high absorption property graphene aerogel.The invention cooperates reduction-oxidation graphite using ammonia borine and ferrous sulfate
Alkene prepares graphene aerogel.The invention accelerates the reduction rate that incubation water heating reacts with ferrous sulfate using ammonia borine, and
And it is easy to operate, preparation method is simple, and to the adsorption effect of fuel rhodamine B height.Although the invention is directed to dyestuff (Luo Dan
Bright B) there is a preferable adsorptivity, but for the absorption property of the pollutants such as other kinds of dyes, pigment how there are no verifying,
It not can guarantee with good absorption property.
Chinese invention patent application (application publication number is CN 106006620A, applies for publication date: 2016-10-12) is open
A kind of preparation method of graphene oxide and graphene aerogel.The invention synthesizes graphite oxide using Hummer method is improved
Alkene solution and synthesizing graphite alkene aeroge, and can effectively be applied in terms of environment.Graphene aerogel prepared by the invention
All there is preferable characterization of adsorption to hydrophily pollutant (rhodamine B) and hydrophobic contaminant.But the preparation of this method
Journey is relatively complicated, and condition requires also more harshness, more demanding to parameters when handling sample, and it is raw to limit its batch
Production and production cost, are difficult to effectively be promoted in terms of industrialization.
In addition, aeroge is due to its excellent thermal insulation property, graphene heat resistance, makes graphene aerogel heat-insulated in addition
There is good application prospect in field, as Chinese invention patent application (application publication number CN105923641A, apply publication date:
2017-05-03), a kind of preparation method of the thermally conductive aluminium oxide of fire-resistant oxidation resistant/grapheme foam composite material is disclosed.It should
Invention is by compound in a solvent with graphene aerogel by alumina powder, then carries out being freeze-dried obtained aluminium oxide/graphite
Alkene aeroge.The composite material prepared is lower than 60% through 800 DEG C of ablations, 5 hours thermal weight losses under air environment, and thermal conductivity is high
In 9W/m.K.But the method for preparing graphene aerogel material is complicated, due to there is no crosslinking agent or a backing material, only without
Machine ion, the graphene aerogel material structure prepared is loose, frangible, is not easy to realize its value.
To sum up, the orderly and regulatable magnetic graphite alkenyl aeroge not about internal microstructure in the prior art
The report of material.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of magnetic graphite alkenyl aeroge materials for having ordered structure
Material and preparation method thereof.Graphene sheet layer is coated on magnetic Nano fiber surface by the preparation method, and through magnetic field orientating technology,
After orienting Refrigeration Technique processing, the graphene sheet layer for being coated with magnetic polymer nanofiber orients under magnetic field force effect
Arrangement, and continue to align to form apparent ordered three-dimensional frame knot along ice-crystal growth direction in orientation refrigerating process
Structure, the final anisotropy and functionalization for realizing graphene aerogel microstructure.
To achieve the above object, the invention discloses a kind of magnetic graphite alkenyl aerogel material for having ordered structure,
Its internal structure is magnetic polymer nanofiber and the three-dimensional network knot that graphene sheet layer is orderly crosslinked and orientations are formed
Structure, the magnetic graphite alkenyl aerogel material its physical property on different Macroscopic physical directions have anisotropic character.
Specifically, above-mentioned orderly crosslinking refers to that graphene sheet layer, magnetic polymer nanofiber are made by crosslinking agent respectively
With and present have regularity interconnection, form the big lamella of continuous graphene and magnetic polymer bundles of nanofibers, together
When graphene sheet layer and magnetic polymer nanofiber are connected with each other, construct as complete, continuous structural system.
Induce magnetic polymer nanofiber along magnetic field by electromagnetic field orientation technology specifically, above-mentioned orientations refer to
Orientations occur for direction, and drive graphene sheet layer that orientation row occurs in the interior space by magnetic polymer nanofiber
Column, are collectively formed the three-dimensional net structure of orientations.
Specifically, the magnetic polymer nanofiber and graphene sheet layer are in magnetic graphite alkenyl aerogel material
The orientations presented in internal microstructure can be align, partial order arrangement, arrangement of gradients or gradual change arrangement.
Specifically, orientation is that control external condition induces graphene film interlayer or magnetic polymer nanofiber
It is arranged towards a direction, the direction of graphene sheet layer can need not keep identical with the direction of magnetic polymer nanofiber.
Specifically, partial order arrangement mode refers to that internal structure is local order structure, can for graphene sheet layer and
Wherein ordered arrangement occurs magnetic polymer bundles of nanofibers for one-component material, or in the presence of whether there is or not sequence areas in entire scope
Domain, order degree, which is lower than, to be aligned.Its requirement to external inductive condition simultaneously is compared with aligning lower, experimentation more
It is convenient.
Specifically, arrangement of gradients mode or gradual change arrangement mode refer to graphene sheet layer and magnetic polymer nanofiber
The features such as size, thickness, content, orientation, arrangement angle and connection type, is common or shows identical change respectively
Change trend and law characteristic.
Further, the difference of the difference of electromagnetic field directional process and orientation freezing processing can regulate and control magnetic graphite alkenyl
Aerogel material internal microstructure is in specific aligned transfer, therefore can assign the magnetic graphite alkenyl aeroge in difference
The anisotropic character of its physical property on Macroscopic physical direction.
Specifically, the above-mentioned physical property for having anisotropic properties mainly includes mechanical property, electric conductivity, magnetism
Energy is equal.
Specifically, the anisotropic properties of the magnetic graphite alkenyl Mechanical Properties of Aerogels refer to due to graphene film
Different its compression stress, springform on the different directions such as radially, axially of layer, magnetic polymer nanofiber arrangement mode
The characteristics of amount, compression reaction rate, compressive recovery rate and the compression mechanical properties such as cyclical stability show differentiation.
Specifically, the anisotropic properties of the magnetic graphite alkenyl aeroge electric conductivity refer to due to graphene sheet layer
Electric conductivity with magnetic polymer nanofiber is there are bigger difference, and electronics relies primarily on graphene sheet layer and transmitted, therefore
It can make the magnetic graphite alkenyl airsetting according to the difference of graphene sheet layer and magnetic polymer nanofiber arrangement mode, angle etc.
Glue is the characteristics of radially, axially waiting electric properties such as conductivity, electron-transport speed on different directions to show differentiation.
Specifically, the anisotropic properties of the magnetic graphite alkenyl aeroge magnetic behavior refer to that magnetic Nano fiber passes through
Orientations occur along magnetic direction after additional electromagnetic field orientation process, internal magnetization nanofiber can be according to additional electromagnetic field
The difference of direction and processing mode and condition shows different arrangement modes, causes the magnetic graphite alkenyl aeroge along magnetic field
The differentiation feature of magnetic behavior is showed on direction and non-magnetic field direction.
Further, the magnetic polymer nanofiber is the nanofiber by magnetic cytokine regulatory, it is described it is magnetic because
Son is one of strontium ferrite, Ni ferrite, Conjugate ferrite, ferroso-ferric oxide or iron-cobalt-nickel metal.
Further, the mass percent of each component is as follows in the magnetic graphite alkenyl aerogel material: graphene
90%~50%, magnetic polymer nanofiber 25%~5%, PVA is 25%~5%.
In order to preferably realize technical purpose of the invention, the invention discloses a kind of magnetic graphites for having ordered structure
The preparation method of alkenyl aerogel material, it includes the following steps:
1) polymer nanofiber master batch is mixed with the magnetic polymer nano particle through demagnetization processing, is squeezed through melting
Out, it emulsifies, shear obtained magnetic polymer nanofiber dispersion liquid；
2) take magnetic polymer nanofiber dispersion liquid, graphene oxide water solution and PVA (polyvinyl alcohol) aqueous solution mixed
Uniform mixed liquor is closed, mixed liquor is placed in electromagnetic field and stands and carry out directional process, it will be after electromagnetic field orientation process
Mixed liquor is oriented freezing processing using liquid nitrogen, continues to be freeze-dried the magnetic oxygenated of obtained internal microstructure ordered arrangement
Graphene aerogel；
3) it takes magnetic oxygenated graphene aerogel to be placed in hydrazine hydrate atmosphere under confined conditions and carries out vapour phase reduction processing,
Magnetic graphite alkenyl aeroge is made.
Preferably, the internal microstructure ordered arrangement in step 2) includes arrangement, gradual change arrangement, partial order in gradient
It arranges or aligns.
Further, the electromagnetic field intensity in step 2) is 0.01~2T, and magnetic direction is vertical direction or horizontal direction.
Specifically, magnetic field orientating technology acts on to provide magnetic field force using electromagnetic field, driven under magnetic field force effect magnetic
Displacement occurs for the factor, and drives polymer nanofiber, graphene sheet layer that ordered arrangement occurs in turn.And it can pass through
The orientation and spread pattern for adjusting magnetic field angle control polymer nanofiber, when by adjusting magnetic field strength and orientation
Between, number etc. may be implemented that finally magnetic size controls to magnetic graphite alkenyl aeroge.
Further, the orientation freezing processing in step 2) are as follows: 0~90 ° of angle, cooling time 0.5~2 hour of freezing.
Specifically, orientation Refrigeration Technique, which can be fixed quickly and effectively and reinforce lower obtain of externally-applied magnetic field effect, is orientated knot
The ordered arrangement of structure further strengthens the ordered three-dimensional frame structure inside graphene aerogel.And it is cold by adjusting orientation
Various ordered structures can be obtained by freezing angle, realize the anisotropic in graphene aerogel structure.
Further, the freeze-drying in step 2) are as follows: -20 DEG C~-80 DEG C of cryogenic temperature, cooling time 12~72 is small
When, drying time 20~90 hours.
Further, the magnetic factor is strontium ferrite, Ni ferrite, Conjugate ferrite, four in magnetic polymer nano particle
One of Fe 3 O or iron-cobalt-nickel metal.
Further, the graphene oxide water solution is made for improved Hummers method.Specific preparation process is such as
Under:
It is dispersed with stirring uniformly, is added after being warming up to 80 DEG C natural after potassium peroxydisulfate, phosphorus pentoxide are added into the concentrated sulfuric acid
Graphite powder, insulation reaction must pre-oxidize graphene, continue to be warming up to after the concentrated sulfuric acid, potassium permanganate is added into pre-oxidation graphene
45 DEG C of insulation reactions are slow added into deionized water to no gas after process and release, are warming up to 95 DEG C of continuation insulation reactions,
Reaction solution is transferred in deionized water, is vigorously stirred simultaneously, hydrogen peroxide is added dropwise dropwise after reaction solution is cooling to reacting molten
Liquid is generated without color change and gas, successively use mass fraction for 10% dilute hydrochloric acid solution, deionized water washs to sample
For neutrality, and it is stand-by to be configured to the evenly dispersed graphene oxide water solution that concentration is 1~15mg/mL.
Preferably, graphene oxide water solution concentration is 1~15mg/mL.
Preferably, PVA aqueous solution mass fraction is 0.5%~5%.
Further, the material of the polymer nanofiber master batch be PVA-co-PE (ethylene-vinyl alcohol copolymer),
POE (polyolefin elastomer), PA6 (nylon 6), PA66 (nylon66 fiber), PET (polyethylene terephthalate) or (poly- pair of PPT
At least one of benzene dicarboxylic acid trimethylene glycol ester).
Further, the condition of vapour phase reduction processing is carried out in hydrazine hydrate atmosphere are as follows: reduction temperature is 50~90 DEG C, reduction
Time is 1~6 hour.
Specifically, using the advantage of above-mentioned restoring method to obtain the magnetic oxygenated graphite of ordered structure by directional process
After alkene aeroge because it has great porosity and specific surface area, under gas phase condition hydrazine hydrate can sufficiently into
Enter inside magnetic oxygenated graphene aerogel and come into full contact with, and graphene oxide layer is effectively restored, is not influencing
The enhancing of electric conductivity is realized on the basis of its structure and mechanical property.
Further, magnetic polymer nanofiber be polymer nanofiber master batch is dissolved in alcohol-water system heat it is molten
Xie Hou, add through demagnetization processing magnetic polymer nano particle, be stirred, Precipitation, shearing dispersion after answered
Close particle, then composite particles are mixed with cellulose acetate-butyrate through melting extrusion, emulsification, shearing and etc. be prepared it is uniform
The magnetic polymer nanofiber dispersion liquid of dispersion.
The beneficial effects are mainly reflected as follows following aspects:
1, present invention design assigns polymer nanofiber magnetic, and drives packet using the induction in magnetic factor pair magnetic field
Oriented alignment occurs for the graphene sheet layer for being covered with magnetic polymer nanofiber, and realizes orientation texture in orientation refrigerating process
Fixed and reinforcement, the graphene aerogel that the internal microstructure of formation aligns has broader in aerogel material field
Application prospect；
2, the preparation method that the present invention designs can be by strong to treatment conditions such as magnetic field on the basis of realizing ordered structure
The arrangement of gradients of graphene aerogel internal microstructure, gradual change row are realized in the regulation of degree, magnetic direction, orientation freezing angle etc.
Column, partial order arrange, align etc. a variety of ordered structures independences or and the structural system deposited, it is good to prepare mechanical property
Good magnetic controllable grapheme aeroge lays the foundation.
Detailed description of the invention
Fig. 1 is the SEM image of magnetic polymer nanofiber prepared by the present invention；
Fig. 2 is the TEM image of magnetic polymer nanofiber prepared by the present invention；
Fig. 3 is the macro morphology of the magnetic graphite alkenyl aerogel material prepared by the present invention for having ordered structure；
Fig. 4 is the microcosmic ordered structure figure of magnetic graphite alkenyl aerogel material prepared by the present invention；
Fig. 5 is the orientation structure figure of magnetic graphite alkenyl aerogel material prepared by the present invention；
Fig. 6 is the arrangement of gradients structural schematic diagram of magnetic graphite alkenyl aerogel material of the invention；
Fig. 7 is the gradual change arrangement architecture schematic diagram of magnetic graphite alkenyl aerogel material of the invention.
Wherein, figure label is as follows:
Magnetic polymer nanofiber 1, graphene sheet layer 2；
And in figure symbol H indicate be magnetic direction.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
Embodiment 1:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, and 10mL is dense
Degree is the magnetic polymer nanofiber dispersion liquid of 5mg/mL in beaker, and the PVA solution that 10mL concentration is 5mg/mL is added,
Agitated, ultrasonic disperse obtains mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations are opened, set the magnetic field strength that magnetizes as 1T, circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be through overcharging
Magnetic aligning treated mixed solution is placed in rapidly orientation freezing die tip, is oriented mixed solution using liquid nitrogen cold
Jelly processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely,
It is 90 hours dry under conditions of vacuum degree is 15Pa, obtain the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 2:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 1mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 1mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 3:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 4:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 0.01T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be through overcharging
Magnetic aligning treated mixed solution is placed in rapidly orientation freezing die tip, is oriented mixed solution using liquid nitrogen cold
Jelly processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely,
It is 90 hours dry under conditions of vacuum degree is 15Pa, obtain the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 5:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 2T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 6:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 1 time, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 7:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 3 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 8:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 45 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 9:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 6 times, and magnetic direction is 90 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 90 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
Embodiment 10:
A kind of preparation method of magnetic graphite alkenyl aerogel material is present embodiments provided, specific preparation process is as follows:
1) preparation of graphene oxide solution: with natural graphite powder, the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, permanganic acid
Potassium is that by improved Hummers method graphene oxide is prepared in raw material, is dispersed in deionized water and obtains concentration and be
The graphene oxide water solution of 5mg/mL.
2) preparation of magnetic polymer nanofiber dispersion liquid: polymer P VA-co-PE master batch is heated in alcohol-water system
After dissolution, the magnetic polymer nano particle (ferroferric oxide nano granules) through demagnetization processing, agitated mixing, precipitating is added
It is precipitated, obtains composite particles after shearing dispersion, by composite particles and cellulose acetate-butyrate powder according to certain mass mixing
By melting extrusion, emulsification, shearing and etc. evenly dispersed magnetic polymer nanofiber dispersion liquid is prepared.
3) preparation of magnetic graphite alkenyl aeroge: taking 20mL concentration is the graphene oxide solution of 5mg/mL, 5mL concentration
For 5mg/mL magnetic polymer nanofiber dispersion liquid in beaker, and be added 5mL concentration be 5mg/mL PVA solution, warp
Stirring, ultrasonic disperse obtain mixed solution.The beaker for filling mixed solution is placed in electromagnetic coil central sample platform position, is opened
Cooling cycle water installations set the magnetic field strength that magnetizes as 1T, and circulation magnetizes orientation 6 times, and magnetic direction is 30 °.It will be by magnetizing
Mixed solution after orientation process is placed in rapidly orientation freezing die tip, is oriented freezing to mixed solution using liquid nitrogen
Processing, orientation freezing angle is 0 °, and solution to be mixed continues freezing 24 hours under the conditions of being transferred to -60 DEG C after freezing completely, in
Vacuum degree is 90 hours dry under conditions of being 15Pa, obtains the magnetic graphite alkenyl aeroge for having ordered structure.
4) the vapour phase reduction processing of magnetic graphite alkenyl aeroge: 2mL hydrazine hydrate solution is added into 25mL beaker, will fill
The 25mL beaker for having hydrazine hydrate and the magnetic oxygenated graphene aerogel being prepared are transferred in 500mL beaker, encapsulation process
Afterwards, 80 DEG C of heating water bath 2h take out after cooled to room temperature.
In conjunction with Fig. 1, Fig. 2 it is found that magnetic polymer is received in magnetic polymer nanofiber made from the embodiment of the present invention 1
Rice grain is distributed among fiber, so that polymer nanofiber has magnetism.
Fig. 3 is the macro morphology of aerogel material made from embodiment 1；The aerogel material surface is smooth, structural integrity.
In conjunction with Fig. 4, Fig. 5, Fig. 6 and Fig. 7 it is found that by regulation magnetic field orientating technology and orientation Refrigeration Technique to control magnetism
Different ordered three-dimensional frame structure inside graphene-based aeroge.
It wherein, is 1T in magnetic field strength when Fig. 4 is graphene oxide, magnetic polymer nanofiber mass ratio is 2:1,
Further orientation freezes the micro- of obtained interior microscopic ordered arrangement under 45 ° after magnetic field angle is orientated 6 times under the conditions of being 45 °
Mirror diagram.It can be found that the magnetic polymer nanofiber for being oxidized graphene coated presents a degree of orderly row
Column, but still will appear a degree of tangling phenomenon when magnetic polymer nanofiber too high levels.
It is 1T, magnetic field angle in magnetic field strength when Fig. 5 is graphene oxide, magnetic polymer nanofiber mass ratio is 4:1
Degree further orients freezing after being orientated 6 times under the conditions of being 90 ° under 90 °, can obviously observe magnetic polymer nanofiber
Oriented alignment has occurred, realizes the anisotropy of magnetic graphite alkenyl aeroge.But orientation is not limited to Fig. 5,
Graphene sheet layer and magnetic polymer nanofiber can also be arranged according to different directions.
As shown in fig. 6, by adjusting external inductive condition, graphene sheet layer 2 and magnetic polymer nanofiber 1 can be made
Arrangement of gradients is presented in the features such as size, thickness, content, orientation, arrangement angle and connection type.
As shown in fig. 7, by adjusting external inductive condition, graphene sheet layer 2 and magnetic polymer nanofiber 1 can be made
Gradual change arrangement is presented in the features such as size, thickness, content, orientation, arrangement angle and connection type.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment
Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention
It is required that protection scope.
Claims (10)
1. a kind of magnetic graphite alkenyl aerogel material for having ordered structure, internal is magnetic polymer nanofiber and stone
The three-dimensional net structure that black alkene lamella is orderly crosslinked and orientations are formed, the magnetic graphite alkenyl aerogel material is in difference
Its physical property has anisotropic character on Macroscopic physical direction.
2. having the magnetic graphite alkenyl aerogel material of ordered structure according to claim 1, it is characterised in that: the magnetic
Property polymer nanofiber and the graphene sheet layer in the internal microstructure of magnetic graphite alkenyl aerogel material in ladder
Degree arrangement, gradual change arrangement, partial order arrangement align.
3. the magnetic graphite alkenyl aerogel material according to claim 1 or claim 2 for having ordered structure, it is characterised in that: institute
Stating magnetic polymer nanofiber is the nanofiber by magnetic cytokine regulatory, and the magnetism factor is strontium ferrite, ferronickel oxygen
One of body, Conjugate ferrite, ferroso-ferric oxide or iron-cobalt-nickel metal.
4. having the preparation method of the magnetic graphite alkenyl aerogel material of ordered structure described in a kind of claim 1, it includes
Following steps:
1) polymer nanofiber master batch is mixed with the magnetic polymer nano particle through demagnetization processing, through melting extrusion, cream
Change, shear obtained magnetic polymer nanofiber dispersion liquid；
2) magnetic polymer nanofiber dispersion liquid, graphene oxide water solution is taken to be uniformly mixed to obtain mixed liquor with PVA aqueous solution,
Mixed liquor is placed in electromagnetic field and stands and carry out directional process, by the mixed liquor after electromagnetic field orientation process using liquid nitrogen into
Row orientation freezing processing, continues the magnetic oxygenated graphene aerogel for being freeze-dried obtained internal microstructure ordered arrangement；
3) it takes magnetic oxygenated graphene aerogel to be placed in hydrazine hydrate atmosphere under confined conditions and carries out vapour phase reduction processing, be made
Magnetic graphite alkenyl aeroge.
5. having the preparation method of the magnetic graphite alkenyl aerogel material of ordered structure, feature according to claim 4
Be: the electromagnetic field intensity in step 2) is 0.01~2T, and magnetic direction is vertical direction or horizontal direction.
6. having the preparation method of the magnetic graphite alkenyl aerogel material of ordered structure, feature according to claim 4
It is: the orientation freezing processing in step 2) are as follows: 0~90 ° of angle, cooling time 0.5~2 hour of freezing.
7. having the preparation method of the magnetic graphite alkenyl aerogel material of ordered structure, feature according to claim 4
It is: the freeze-drying in step 2) are as follows: -20 DEG C~-80 DEG C of cryogenic temperature, cooling time 12~72 hours, drying time 20
~90 hours.
8. having the preparation method of the magnetic graphite alkenyl aerogel material of ordered structure, feature according to claim 4
It is: the condition that vapour phase reduction is handled in step 3) are as follows: reduction temperature is 50~90 DEG C, and the recovery time is 1~6 hour.
9. having the preparation of the magnetic graphite alkenyl aerogel material of ordered structure according to claim 4 or 5 or 6 or 7 or 8
Method, it is characterised in that: in the magnetic polymer nano particle the magnetic factor be strontium ferrite, Ni ferrite, Conjugate ferrite,
One of ferroso-ferric oxide or iron-cobalt-nickel metal.
10. having the system of the magnetic graphite alkenyl aerogel material of ordered structure according to claim 4 or 5 or 6 or 7 or 8
Preparation Method, it is characterised in that: the material of the polymer nanofiber master batch be PVA-co-PE, POE, PA6, PA66, PET or
At least one of PPT.
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