CN104925787B - A kind of method that constant pressure and dry prepares graphene aerogel - Google Patents
A kind of method that constant pressure and dry prepares graphene aerogel Download PDFInfo
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Abstract
The present invention provides a kind of method that constant pressure and dry prepares graphene aerogel, hydrogel is prepared as raw material using the aqueous dispersions of graphene oxide first in this method, handled again by freezing thawing, re-assembly its internal structure, the structure formed is enough to resist structure collapses caused by gas-liquid interface tension force during constant pressure and dry, finally realizes that constant pressure and dry prepares graphene aerogel.Compared with being freeze-dried with supercritical drying drying method, present invention greatly enhances the preparation efficiency of graphene aerogel, production cost is reduced, is expected to realize the industrialized production of graphene aerogel.In addition, the present invention provides a kind of new graphene aerogel, the characteristic of its macropore and super rebound will be applied in many fields.
Description
【Technical field】
The present invention relates to a kind of method that constant pressure and dry prepares graphene aerogel, belong to aeroge preparing technical field.
【Background technology】
Aeroge (Aerogel) is also known as xerogel, is with surpassing with extra-low density, high-specific surface area, high hole ratio
The nano material of the multi-branched nanoporous three-dimensional net structure of high pore volume rate, the medium being full of in its space net structure are
Gas, appearance are in solid-like.The appearance of carbon aerogels is that have initiative progress in aerogel material research, it is by aeroge
The non-conductor of material from electricity extend to electric conductor, start the new application field of aerogel material.
Graphene (Graphene) is made of sp2 hydbridized carbon atoms, in cycle honeycomb lattice structure, is had well
The physical properties such as conduction, heat conduction, mechanics.The thickness of graphene is only 0.34 ran, and its two-dimensional is from tens nanometers
Differed to tens microns, therefore porous, ultralight graphene aerogel can be assembled into by certain method.Different systems
Preparation Method determines the different internal networking structure of graphene aerogel, also gives its different performance, such as high intensity
Brittleness aeroge and soft elastic aeroge.Graphene aerogel is with ultralight, porous, conductive, hydrophobic oleophilic oil and flexibly
The characteristics such as mechanical performance, can be applied in fields such as catalyst carrier, conductive devices, oily waste treatment and energy snubbers.
Graphene can be obtained graphene oxide (Oxide graphene) first by graphite by oxidizing process, then be led to again
The method for crossing chemistry or heat reduces to obtain.Surface of graphene oxide has abundant oxy radical, can stable dispersion in water.
Therefore the preparation of graphene aerogel is usually all that graphene oxide dispersion is prepared first by raw material of graphene oxide
Or graphene wet gel, then remove solvent by freeze-drying or supercritical drying again and obtain.For example, Chinese patent
CN102239114A is prepared for using the dispersion liquid or wet gel of graphene oxide by freeze-drying or supercritical drying first
Graphene oxide and graphene aerogel.
Graphene oxide aqueous dispersions are reduced using reducing agent first in CN101941693A to obtain graphene hydrogel,
Then aeroge is prepared by freeze-drying.Why people without using method dry under normal pressure are primarily due to graphene film
The hole of layer assembling is smaller, and capillarity is obvious, and gas-liquid interface tension force easily makes pore space structure cave in during gas evaporation,
The after-contraction of drying is obvious；And freeze-drying and supercritical drying can be to avoid this point, therefore airsetting can be kept well
The volume and shape of glue.But the environment that offer low temperature and low pressure are provided is freeze-dried, the overcritical environment for needing to provide high pressure,
And special equipment is required for, it is of high cost, and low production efficiency, it is impossible to prepare in large quantity, therefore constrain graphite
The extensive use of alkene aeroge.A kind of constant pressure and dry is provided in patent CN102774824A and prepares the organic gas of graphene cross-linking type
The method of gel and charcoal-aero gel, illustrates that constant pressure and dry prepares the significance of aeroge.But graphene is only in the patent
It is as crosslinking agent, is not the material of main part of aeroge, performance and graphene aerogel difference is larger.Therefore done using normal pressure
The aeroge that dry method prepares full graphene has very important practical significance.
【The content of the invention】
[technical problems to be solved]
It is an object of the invention to provide a kind of method that constant pressure and dry prepares graphene aerogel；
The present invention also aims to provide a kind of purposes that this method is used for graphene aerogel preparation.
[technical solution]
As it was previously stated, special equipment is required in the preparation process of the graphene aerogel of the prior art, it is of high cost, and
And low production efficiency, it is impossible to prepare in large quantity, therefore constrain the extensive use of graphene aerogel.Only use normal pressure
Drying, which prepares graphene aerogel, could fundamentally simplify the production technology of graphene aerogel, reduce cost, realize industry
Metaplasia is produced.But when dry under condition of normal pressure, due to the tension force that gas-liquid interface produces, gel network structure easily produce cave in,
Phenomena such as contraction.But when the three-dimensional network hole that graphene sheet layer assembling is built is sufficiently large, hole wall is sufficiently thick, it becomes possible to support
This tension force is driven, volume and shape during hydrogel is substantially kept, obtains the graphene aerogel of constant pressure and dry.This hair
Bright technical solution provides a kind of method that constant pressure and dry prepares graphene aerogel, and this method is with the moisture of graphene oxide
Dispersion liquid is reaction system, and adding reducing agent, either crosslinking agent or use high pressure hydro-thermal method, the moisture of redox graphene dissipate
Liquid, and the reducing degree of graphene oxide can be controlled by controlling time and the temperature of prereduction reaction, prepare first
The graphene oxide hydrogel of prereduction is obtained, graphene three-dimensional network is then made by the method for melting hydrogel freezing again
Structure re-assemblies, and obtains resisting the structure of tension force produced by gas-liquid interface during constant pressure and dry, further reduces
Hydrogel, consolidates the three-dimensional structure of hydrogel, finally realizes dry graphene hydrogel under normal pressure, prepares almost non-shrinking stone
Black alkene aeroge.
The present invention is achieved through the following technical solutions.
A kind of method that constant pressure and dry prepares graphene aerogel, it is characterised in that this method is with the moisture of graphene oxide
Dispersion liquid is reaction system, and by adding reducing agent in the aqueous dispersions, either prepared by crosslinking agent or use high pressure hydro-thermal method
The hydrogel of prereduction graphene oxide, prereduction degree need to control in a certain range, can be changed by fixed reaction temperature
Become the reaction time to realize.Then melted again after the hydrogel is freezed under -30 to 0 degrees Celsius, which is melted
After process is repeated more than once, then by the hydrogel, further reduction becomes graphene hydrogel, finally does under normal pressure
It is dry to obtain graphene aerogel.
Another kind preferred embodiment according to the present invention, wherein the monolithic layer of the graphene oxide is 0.2~50
Micron, the concentration of graphene oxide aqueous dispersions is 0.5~10 milligram every milliliter.
Another kind preferred embodiment according to the present invention, wherein the reducing agent is hydrazine hydrate, vitamin C and iodate
Hydrogen.
Another kind preferred embodiment according to the present invention, wherein the crosslinking agent is ethylenediamine.
Another kind preferred embodiment according to the present invention, wherein drying means are selected from direct drying under normal pressure.
Method as described before, it is characterised in that this method comprises the following steps：
(1) graphene oxide aqueous dispersions are prepared；
(2) by adding reducing agent either crosslinking agent or use high pressure hydro-thermal in the graphene oxide aqueous dispersions
Method prepares the hydrogel of prereduction graphene oxide；
(3) hydrogel for the prereduction graphene oxide for preparing step (2) freezes under -30 to -10 degrees Celsius, then
Make its thawing, repeated freezing thawing step more than 1 time at room temperature；
(4) hydrogel prepared by step (3) is further reduced, the prereduction method in the same step of restoring method (2), after
Continuous heating reaction to reduction reaction terminates；
(5) hydrogel washing by soaking more than 2 times in a solvent for preparing step (4), solvent are selected from water, ethanol and acetone
In one or more；
(6) hydrogel that 20-100 degrees Celsius of drying steps (5) is prepared under normal pressure obtains graphene aerogel.
Another kind preferred embodiment according to the present invention, it is characterised in that in the step (1), graphene oxide water
The preparation method of dispersion liquid is unlimited, and it is method commonly used in the art that wherein Hummer ' s chemical methods, which prepare graphite oxide,.
Another kind preferred embodiment according to the present invention, it is characterised in that in the step (2), prepare prereduction oxygen
The method of graphite alkene hydrogel is unlimited, preferably, using the method for adding reducing agent or high pressure hydro-thermal.
Another kind preferred embodiment according to the present invention, it is characterised in that in the step (2), control prereduction oxygen
C/O mole atoms ratio in graphite alkene is 3.0 to 5.0.
Another kind preferred embodiment according to the present invention, it is characterised in that in the step (3), control cryogenic temperature
At -20 to -15 degrees Celsius, freezing melts number control at 1 to 3 times.
Another kind preferred embodiment according to the present invention, it is characterised in that in the step (4), stone after control reduction
C/O atomic molars ratio in black alkene is 6.0 to 10.0.
Application of the method in graphene aerogel is prepared.
[beneficial effect]
The present invention has the following advantages due to taking above-mentioned technical proposal：
1st, constant pressure and dry prepares graphene aerogel, volume and shape before most can keeping dry, with freezing
Drying prepares graphene aerogel with supercritical drying and compares, and technique is simpler, cost is lower, and solves graphene gas
Gel is prepared on a large scale the problem of production, is expected to realize industrialized production.
2nd, the graphene aerogel prepared by the present invention has extraordinary mechanical performance and electric conductivity.Such as prepare
Graphene aerogel has super resilience, and maximum compression ratio can reach 93%, and can reply well, for compression at present
Than maximum graphene aerogel, permanent deformation is nearly free from after compression reaction more than 1,000 times.Conductance when its is uncompressed
Rate can be to reach 13S m-1.Therefore the graphene aerogel prepared by the present invention can be applied to the conductive sensor of large deformation
Field.
3rd, the graphene aerogel prepared by the present invention has oleophilic drainage characteristic, may be used as oil suction decontamination material, and
And it can recycle.
4th, the graphene aerogel prepared by the present invention has ultralight characteristic, and density range arrives 10mg cm 1-3。
5th, the present invention can prepare graphene aerogel of different shapes, meet the needs of different field.
【Brief description of the drawings】
Fig. 1 is the photo in kind of aeroge after the obtained graphene hydrogel of the present invention and constant pressure and dry；
Fig. 2 is the obtained graphene aerogel of different shapes of the present invention；
Fig. 3 is the scanning electron microscope (SEM) photograph of the obtained graphene aerogel of the present invention；
Fig. 4 is the compression reaction test curve figure of the obtained graphene aerogel of the present invention；
Fig. 5 is the displaying figure that the obtained graphene aerogel of the present invention has oleophilic drainage performance, it can pass through pressure
The oil that contracting extrusion absorbs recycles；
Fig. 6 is the photo in kind of graphene aerogel prepared by embodiment 5 and comparative example 1；
【Embodiment】
The present invention is further described with reference to embodiment, it should be understood that these embodiments are merely to illustrate this hair
It is bright, rather than limit the scope of the invention.
Embodiment 1.
Using the crystalline flake graphite of 325 mesh as raw material, graphene oxide is prepared by improved Hummer ' s chemical methods, is obtained
To 10 milligrams every milliliter of graphene oxide (GO) solution, take 5 milliliters of GO solution to be added in cylindrical glass bottle, add 5 millis
Deionized water is risen, GO solution concentrations are made into 5 milligrams every milliliter, then takes the hydrazine hydrate solution of 100 microlitres of mass fractions 35%, is added
Enter into GO solution, be ultrasonically treated 5 minutes, hydrazine hydrate is uniformly dispersed, circular glass bottle is jumped a queue sealing, is put into 95 degrees Celsius
It is lower reaction 0.5 it is small when form gel.Then stop reaction, after gel drops to room temperature, which is put into refrigerator and is freezed, ice
After about -18 degrees Celsius, two hours of the temperature of case, after gel freezes completely, which is taken at room temperature, is melted completely
Afterwards, then with identical condition freezing melt once, when hydrogel then being placed in reaction 2 is small under 95 degrees Celsius again, reaction terminates
Hydrogel is rinsed twice with alcohol afterwards, finally will obtain graphene gas when drying 24 is small under hydrogel in an oven 60 degrees Celsius
Gel.
Embodiment 2.
Technological process is with embodiment 1, the difference is that GO solution concentrations are made into 4 milligrams every milliliter, 10 milliliters of total amount, is hydrated
Hydrazine adds 80 microlitres, when the reaction time 1 is small, and after forming gel, cryogenic temperature is -30 degrees Celsius.After freezing thawing has been handled, then
React 1.5 it is small when.
Embodiment 3.
Technological process is with embodiment 1, the difference is that GO solution concentrations are made into 3 milligrams every milliliter, 10 milliliters of total amount, is hydrated
Hydrazine addition is 90 microlitres.
Embodiment 4.
Technological process is with embodiment 1, the difference is that changing 325 mesh crystalline flake graphites into 180 mesh crystalline flake graphites.
Embodiment 5.
Technological process is with embodiment 1, the difference is that GO solution concentrations are made into 4 milligrams every milliliter, 10 milliliters of total amount, adds
80 milligrams of vitamin Cs replace hydrazine hydrate, and ultrasonic 2 minutes vitamin Cs are completely dissolved, and when then the reaction time 1 is small, form gel,
Freezing melt handled after, then react 5 it is small when.
Embodiment 6.
Technological process, the difference is that when the reaction time 2 is small, forms gel with embodiment 5, after freezing thawing has been handled, then
React 4 it is small when.
Embodiment 7.
Technological process is with embodiment 5, the difference is that cryogenic temperature is -30 degrees Celsius.
Embodiment 8.
Technological process is with embodiment 1, the difference is that GO solution concentrations are made into 3 milligrams every milliliter, 10 milliliters of total amount, adds
40 microlitres of ethylenediamines replace hydrazine hydrate, when then 90 degrees Celsius of reactions 8 are small, form gel, after freezing thawing has been handled, then react
8 it is small when.
Embodiment 9.
Technological process is with embodiment 8, the difference is that adding 80 microlitres of ethylenediamines, when the reaction time 12 is small, forms gel, cold
Freeze -30 degrees Celsius of temperature, freezing melt handled after, then react 4 it is small when.
Embodiment 10.
Technological process is with embodiment 1, the difference is that GO solution concentrations are made into 3 milligrams every milliliter, 10 milliliters of total amount, is not added with
Any reducing agent and crosslinking agent, when reaction 2 is small under 180 degrees Celsius in autoclave, form gel, freezing, which is dissolved, have been handled
Afterwards, then react 13 it is small when.
Comparative example 1.
Technological process handles this step with embodiment 5, the difference is that melting without freezing, when directly reaction 6 is small, then
Oven drying.
From figure 1 it appears that the invention can prepare graphene aerogel by constant pressure and dry, and can portion big absolutely
Divide the volume and shape before keeping dry.Fig. 2 illustrates that the invention can prepare graphene aerogel of different shapes.Fig. 3 is shown
The morphosis of graphene aerogel prepared by the invention, the three-dimensional hole of graphene assembling 100 to 500 microns it
Between, belong to bigger hole, and graphene wall orientations, gas-liquid interface institute during constant pressure and dry can be resisted well
The tension force of generation, the overwhelming majority keep the volume and shape before drying.Fig. 4 illustrates the graphene aerogel tool of patent offer
There is super-elasticity, its maximum compression ratio can reach 93%, be the compression ratio of current graphene aerogel maximum, compression reaction 1,000
Permanent deformation is nearly free from after secondary.Fig. 5 illustrates performance of the graphene aerogel with oleophilic drainage of patent offer, and
And it can be recycled by compressing the oil of extrusion absorption.Fig. 6 embodies the crucial work that processing is melted in freezing as a comparison case
With.Its left figure is to melt the aeroge pictorial diagram handled prepared by this step by freezing, and right figure eliminates pair of this step
Than embodiment 1, occurs serious shrinkage phenomenon during constant pressure and dry.
Claims (8)
1. a kind of method that constant pressure and dry prepares graphene aerogel, it is characterised in that this method is dissipated with the moisture of graphene oxide
Liquid is reaction system, by adding reducing agent either crosslinking agent or pre- using the preparation of high pressure hydro-thermal method in the aqueous dispersions
The hydrogel of redox graphene, the C/O atomic molars of prereduction graphene oxide 3.0 to 5.0, then should than control
Hydrogel melts at room temperature again after being freezed under -30 to -10 degrees Celsius, which is repeated more than once
Afterwards, by the hydrogel, further reduction becomes graphene hydrogel, finally dries the graphene hydrogel under normal pressure and obtains stone
Black alkene aeroge；
The wherein described constant pressure and dry is direct drying under normal pressure, and drying temperature is 20-100 degrees Celsius.
2. the method as described in claim 1, the control of the reducing degree of prereduction graphene oxide passes through fixed reaction temperature
Change reaction time realization.
3. the method as described in claim 1, wherein the monolithic layer of the graphene oxide is 0.2~50 micron, aoxidizes stone
The concentration of black alkene aqueous dispersions is 0.5~10 milligram every milliliter.
4. the method as described in claim 1, wherein the reducing agent in hydrazine hydrate, vitamin C and hydrogen iodide one
Kind is several, wherein the crosslinking agent is ethylenediamine.
5. the method as described in claim 1, it is characterised in that this method comprises the following steps：
(1) graphene oxide aqueous dispersions are prepared；
(2) by adding reducing agent either crosslinking agent or use high pressure hydro-thermal legal system in the graphene oxide aqueous dispersions
The hydrogel of standby prereduction graphene oxide, the C/O atomic molars of prereduction graphene oxide are than controlling 3.0 to 5.0；
(3) hydrogel for the prereduction graphene oxide for preparing step (2) freezes under -30 to -10 degrees Celsius, then in room
Make its thawing, repeated freezing thawing step more than 1 time under temperature；
(4) hydrogel prepared by step (3) is further reduced, the prereduction method in the same step of restoring method (2), continues to add
Thermal response to reduction reaction terminates；
(5) hydrogel washing by soaking more than 2 times in a solvent for preparing step (4), solvent is in water, ethanol and acetone
It is one or more；
(6) hydrogel that 20-100 degrees Celsius of drying steps (5) is prepared under normal pressure obtains graphene aerogel.
6. method as claimed in claim 5, it is characterised in that in the step (3), control cryogenic temperature is -20 to -15
Degree Celsius, freezing melts number control at 1 to 3 times.
7. method as claimed in claim 5, it is characterised in that in the step (4), the C/O after control reduction in graphene
Atomic molar ratio is 6.0 to 10.0.
8. application of the method described in claim 1 in graphene aerogel is prepared.
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