CN105271212B - A kind of graphene aerogel material and preparation method thereof - Google Patents
A kind of graphene aerogel material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene aerogel material and preparation method thereof, methods described comprises the following steps：(1) precursor solution is prepared：Graphene oxide and skeleton filler are mixed and stirred for uniformly, to obtain precursor solution；(2) graphene hydrogel is prepared：Catalyst is added to the precursor solution and is stirred, and is subsequently poured into the mould for being placed with reinforcing fiber and is sealed, by mould heating response, obtains fibre-reinforced graphene hydrogel；(3) graphite ketenes gel is prepared：The graphene hydrogel is placed in progress solvent displacement in acetone soln, obtains graphite ketenes gel；(4) graphene aerogel is prepared：The graphite ketenes gel is taken out and dried, obtains fibre-reinforced graphene aerogel material.The invention further relates to the graphene aerogel material as made from methods described, the material has lower thermal conductivity and high intensity, can be used as high temperature insulating material.
Description
Technical field
The invention belongs to technical field of composite materials, is related to a kind of preparation method of composite, more particularly to one kind
The preparation method of graphene aerogel material and the graphene aerogel material according to made from methods described.
Background technology
Aerogel material is that a kind of the receiving with network structure formed is mutually built up by colloidal particle or high-polymer molecular
Rice porous solid material, due to its aperture (<50nm) it is less than the mean free path (~70nm) of air molecule, thus in airsetting
Glue does not have cross-ventilation in hole, has extremely low gaseous heat conduction；Aeroge has high porosity, body shared by solid simultaneously
Product ratio is very low, and solid-state heat transfer is also very low.Carbon-based aeroge resistance to elevated temperatures in various aeroges is best (>=1600 DEG C),
High Mach number aircraft thermal protection field has the superiority that can not be substituted.However, the insufficient strength of pure aerogel material, typically
It is required for reinforcing material such as fiber to improve its intensity.
Graphene is a kind of nano-carbon material for the two-dimensional slice structure being made up of carbon atom, has high-specific surface area.It is high
The characteristics such as mechanical property, high thermal conductivity.At this stage, graphene aerogel material (Chinese patent:CN101941693 A) it is main logical
Preparation graphene oxide water solution is crossed, then obtained by processes such as sol gel reaction, dryings.Graphite prepared by the process
Alkene aeroge is by graphene sheet layer build stack, and the graphene aerogel intensity being prepared is high, but thermal conductivity is also high,
It can not be used directly as heat-barrier material.The research about graphene aerogel mainly utilizes the height of graphene in the prior art
Mechanical property and high heat conductance improve the mechanical property and thermal conductivity of gained aerogel material.For example,
CN201210191045.2 discloses a kind of method that constant pressure and dry prepares graphene cross-linking type organic aerogel and charcoal-aero gel,
It mainly solves the problems, such as that the shrinkage factor of aeroge made from constant pressure and dry is excessive using the strong mechanical performance of graphene.Again
For example, CN201310085977.3 provides a kind of graphene oxide/organic aerogel composite with low-shrinkage, wherein
The mechanical property of gained graphene organic aerogel composite is provided by the use of graphene as framework material in itself.Example again
Such as, CN201310504175.1, which is disclosed, provides a kind of preparation method of graphene aerogel, and this method is by graphene oxide
The aqueous solution and polymer：The aqueous solution mixing of polytetrafluoroethylene (PTFE), polyvinyl alcohol, Kynoar or sodium carboxymethylcellulose,
Graphene oxide construction unit is set to be physically connected to form graphene oxide colloidal sol, then with polymer unit by cementation
Graphene aerogel is obtained by drying, reduction, graphene is excellent to lead so that aeroge can be played farthest
The performances such as electricity, heat conduction, mechanics.
But there is presently no can keep or reduce aerogel material while Mechanical Properties of Aerogels is improved
The aeroge preparation method of thermal conductivity.
The content of the invention
The present inventor has found by studying, although it is well known that graphene has high thermal conductivity, when by stone
Black alkene and framework material can improve the intensity of aeroge especially reinforcing fiber composite aerogel when being applied in combination
While can also reduce the lower thermal conductivity of aeroge.In other words, the use of framework material can reduce graphene aerogel material
Thermal conductivity.
Then, it is an object of the present invention to overcome existing graphene aerogel material thermal conductivity high the problem of, there is provided
A kind of preparation method of graphene aerogel material and graphene aerogel material obtained by this method.
In a first aspect, the invention provides a kind of preparation method of graphene aerogel material, wherein, methods described bag
Include following steps：
(1) precursor solution is prepared：Graphene oxide and skeleton filler are mixed and stirred for uniformly, it is molten to obtain presoma
Liquid；
(2) graphene hydrogel is prepared：Catalyst is added to the precursor solution and is stirred, and is subsequently poured into placement
Have in the mould of reinforcing fiber and seal, by mould heating response, obtain fibre-reinforced graphene hydrogel；
(3) graphite ketenes gel is prepared：The graphene hydrogel is placed in progress solvent displacement in acetone soln, obtained
Graphite ketenes gel；
(4) graphene aerogel is prepared：The graphite ketenes gel is taken out and dried, obtains fibre-reinforced graphene
Aerogel material.
In another aspect, present invention also offers the graphene aerogel material as made from methods described.
The beneficial effect of the present invention compared with prior art：
The present invention prepares graphene aerogel material, while using graphene to improve mechanical strength, significantly changes
The defects of being apt to high original graphene aerogel thermal conductivity, heat-proof quality difference, so as to be advantageous to graphene aerogel material conduct
The widespread adoption of heat-barrier material.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Embodiment
As described above, the present invention provides a kind of preparation method of graphene aerogel material in first aspect.In a word
Come, the method described in the present invention mainly comprises the following steps：Prepare precursor solution, sol gel reaction, solvent displacement and do
Dry (such as shown in Fig. 1).
More specifically, method of the present invention may include steps of：
(1) precursor solution is prepared：Graphene oxide and skeleton filler are mixed and stirred for uniformly, it is molten to obtain presoma
Liquid；
(2) graphene hydrogel is prepared：Catalyst is added to the precursor solution and is stirred, and is subsequently poured into placement
Have in the mould of reinforcing fiber and seal, by mould heating response, obtain fibre-reinforced graphene hydrogel；
(3) graphite ketenes gel is prepared：The graphene hydrogel is placed in progress solvent displacement in acetone soln, obtained
Graphite ketenes gel；
(4) graphene aerogel is prepared：The graphite ketenes gel is taken out and dried, obtains fibre-reinforced graphene
Aerogel material.
In some embodiments, the graphene oxide in step (1) is the form of graphene aqueous solution, preferably
, the graphene oxide in the graphene aqueous solution concentration 0.05mg/ml to 20mg/ml (be, for example, 0.05,
0.1st, 1,10 or 20mg/ml).In some embodiments, the concentration is 0.1 to 10mg/ml.In other embodiment
In, the concentration is 1 to 5mg/ml.
In some embodiments, in step (2) by the mould be heated to 60 DEG C to 90 DEG C (be, for example, 60 DEG C, 70
DEG C, 80 DEG C or 90 DEG C), temperature is too low, and reaction speed is slow, too high temperature then excessive consumed energy and to a certain extent
The thermal conductivity of resulting materials may be improved.In some preferred embodiment, the mould is positioned in baking oven and carried out,
It is further preferred that the reaction time is 48 hours to 72 hours (being, for example, 48,54,60,66 or 72 hours).If overlong time,
Then, consumed energy is excessive；If the time is too short, precursor solution may not react complete, cause gel strength poor.
In some embodiments, in step (3), the solvent, which is replaced into, changes an acetone for 2 days, replaces 3 times altogether.
In some embodiments, in step (4), the drying is preferably supercritical drying.Relative to supercritical drying
For dry, other conventional drying methods easily crack, so as to easily be had undesirable effect to material property.
In general, in some embodiments, present invention preferably uses the framework material body for finally giving carbon aerogels
System.In some embodiments, the skeleton filler is selected from by group that such as lower skeleton filler systems form：Resorcinol+formaldehyde；
Melamine+formaldehyde；Phenolic resin+formaldehyde；Cresols+formaldehyde；Poly- isocyanide ester；1,3,5-trihydroxybenzene+formaldehyde；Resorcinol+
Poly- N hydroxymethyl acrylamide.In one preferred embodiment, the quality of the skeleton filler and the graphene oxide
Than for 1：10-10：10 (be, for example, 1:1、1:2、1:3、1:4、1:5、1:6、1:7、1:8、1:9 or 1:10).If the skeleton
The dosage of filler is too low, then can not fully reduce thermal conductivity, if the dosage of the framework material is excessive, reduces gained
The intensity of material, so as to which high intensity caused by graphene can not be given full play to.Skeleton filler is by two kinds of things as described above
In the case that matter forms, the skeleton filler is preferably that the mol ratio of two kinds of materials is 1：2 mixture.
In some embodiments, the catalyst is selected from by sodium borohydride, hydrazine hydrate, ethylenediamine, ascorbic acid, hydrogen
Change aluminium lithium, p-phenylenediamine, hydroiodic acid, diethylamine, propane diamine, butanediamine, diethylenetriamine, triethylene tetramine, TEPA
The group of composition；Preferably, the mass ratio of the graphene oxide and the catalyst is 1：1-200：1 (be, for example, 1,10,
20、50、60：1).If catalyst ratio is too small, presoma can not gel, if ratio is excessive, catalyst it is remaining and for example
Cause to waste.In addition, the inventors discovered that, in body series, such as ammoniacal liquor or other strong acid and strong bases are unable to gel, thus uncomfortable
Cooperate as catalyst.
The present invention has no particular limits to reinforcing fiber, such as in some embodiments, the reinforcing fiber can be with
Selected from the group being made up of carbon fiber, Zirconium oxide fibre, mullite fiber and alumina fibre；Preferably, the reinforcing fiber
Mass ratio with the precursor solution is 80：20-90：10, for example, 80：20、85:15 or 90：10.If reinforcing fiber is used
Measure too small, then may influence whether the intensity of resulting materials；If reinforcing fiber dosage is much, gained material may be influenced whether
The high material of the thermal conductivity of material.
In the second aspect of the present invention, there is provided graphene aerogel material made from the method described in first aspect present invention
Material.
Below in conjunction with Fig. 1 and instantiation, the present invention is described in detail.
Embodiment 1
Using 0.2mg/ml graphene oxide solution, resorcinol+formaldehyde systems are as skeleton filler, graphene oxide
Mass ratio with skeleton filler is 10：1, after the two is well mixed, add the p-phenylenediamine of 50 times of graphene oxide quality, stirring
After uniformly, pour into the mould that placed carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80：20, sealing
Afterwards, it is placed in baking oven, 80 DEG C are reacted 2 days, have obtained graphene hydrogel.Graphene hydrogel after sol-gel is taken out,
It is placed in acetone soln, carries out solvent displacement, change within 2 days an acetone, replaces 3 times altogether, obtain the graphite ketenes of acetone solvent
Gel.Graphite ketenes gel is taken out, by supercritical drying, fibre-reinforced graphene aerogel material is prepared.So
The thermal conductivity and the strength of materials (compressive strength, similarly hereinafter) of resulting materials are measured afterwards.
Thermal conductivity measurements are according to GB/T 10295-2008《Technology of Steady State Thermal Resistance of Thermal Insulating Material and the measure heat about characteristic
Flowmeter method》Carry out；
The measuring method of the strength of materials is according to GB/T 8813-2008《The measure of rigid foam compression performance》Carry out.
Embodiment 2
Using 0.5mg/ml graphene oxide solution, melamine+formaldehyde systems are as skeleton filler, graphene oxide
Mass ratio with skeleton filler is 10：1, after the two is well mixed, add the ethylenediamine of 100 times of graphene oxide quality, stirring
After uniformly, pour into the mould that placed carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80：20, sealing
Afterwards, it is placed in baking oven, 80 DEG C are reacted 2 days, have obtained graphene hydrogel.Graphene hydrogel after sol-gel is taken out,
It is placed in acetone soln, carries out solvent displacement, change within 2 days an acetone, replaces 3 times altogether, obtain the graphite ketenes of acetone solvent
Gel.Graphite ketenes gel is taken out, by supercritical drying, fibre-reinforced graphene aerogel material is prepared.So
The thermal conductivity and the strength of materials of resulting materials are measured afterwards.
Embodiment 3
Using 1mg/ml graphene oxide solution, phenolic resin+formaldehyde systems as skeleton filler, graphene oxide with
The mass ratio of skeleton filler is 10：1, after the two is well mixed, the diethylenetriamine of 100 times of graphene oxide quality is added, is stirred
After mixing uniformly, pour into the mould that placed carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80：20, it is close
It is honored as a queen, is placed in baking oven, 80 DEG C is reacted 2 days, have obtained graphene hydrogel.Graphene hydrogel after sol-gel is taken
Go out, be placed in acetone soln, carry out solvent displacement, change within 2 days an acetone, replace 3 times altogether, obtain the graphene of acetone solvent
Ketone gel.Graphite ketenes gel is taken out, by supercritical drying, fibre-reinforced graphene aerogel material is prepared.
Then the thermal conductivity and the strength of materials of resulting materials are measured.
Embodiment 4
Using 2mg/ml graphene oxide solution, cresols+formaldehyde systems as skeleton filler, graphene oxide with
The mass ratio of skeleton filler is 10：1, after the two is well mixed, the hydrazine hydrate of 100 times of graphene oxide quality is added, stirring is equal
After even, pour into the mould that placed carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80：20, after sealing,
It is placed in baking oven, 90 DEG C are reacted 2 days, have obtained graphene hydrogel.Graphene hydrogel after sol-gel is taken out, put
In acetone soln, solvent displacement is carried out, changes within 2 days an acetone, replaced 3 times altogether, the graphite ketenes for obtaining acetone solvent coagulates
Glue.Graphite ketenes gel is taken out, by supercritical drying, fibre-reinforced graphene aerogel material is prepared.Then
Measure the thermal conductivity and the strength of materials of resulting materials.
Embodiment 5
Using 5mg/ml graphene oxide solution, 1,3,5-trihydroxybenzene+formaldehyde systems as skeleton filler, graphene oxide with
The mass ratio of skeleton filler is 10：1, after the two is well mixed, the ascorbic acid of 50 times of graphene oxide quality is added, stirring is equal
After even, pour into the mould that placed carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80：20, after sealing,
It is placed in baking oven, 60 DEG C are reacted 3 days, have obtained graphene hydrogel.Graphene hydrogel after sol-gel is taken out, put
In acetone soln, solvent displacement is carried out, changes within 2 days an acetone, replaced 3 times altogether, the graphite ketenes for obtaining acetone solvent coagulates
Glue.Graphite ketenes gel is taken out, by supercritical drying, fibre-reinforced graphene aerogel material is prepared.Then
Measure the thermal conductivity and the strength of materials of resulting materials.
Embodiment 6 to 17
Except being otherwise noted, otherwise using method same as Example 1 according to raw material as shown in table 1 below and technique bar
Part prepares graphene aerogel material, then measures the thermal conductivity and the strength of materials of resulting materials.The results listed in the following table.
Wherein, when skeleton filler is two kinds of materials, the skeleton filler is that two kinds of material mol ratios are 1：2 mixture.
Embodiment 17 is according to document report (Zhang X., Sui Z., Xu B., Yue S., Luo Y., Zhan W., et
al.Mechanically strong and highly conductive graphene aerogel and its use as
electrodes for electrochemical power sources.J Mater Chem.2011,21(18):6494-
6497.) graphene aerogel preparation method, fiber reinforced graphite alkene aerogel material, remaining step and the phase of embodiment 5 are prepared
Together, obtained graphene aerogel material property contrasts with material made from embodiment 5, it is found that its thermal conductivity is higher, be not suitable for
As materials'use.
To sum up, the preparation method of this patent and document report associated materials is contrasted, and skeleton filler and stone is used in combination
Black alkene, the good graphene aerogel material of heat-proof quality can be prepared.
Unspecified part of the present invention is known to the skilled person technology.
Claims (13)
1. a kind of preparation method of graphene aerogel material, it is characterised in that methods described comprises the following steps：
(1) precursor solution is prepared：Graphene oxide and skeleton filler are mixed and stirred for uniformly, to obtain precursor solution；
(2) graphene hydrogel is prepared：Catalyst is added to the precursor solution and is stirred, and is subsequently poured into and is placed with increasing
In the mould of strong fiber and seal, by mould heating response, obtain fibre-reinforced graphene hydrogel；
(3) graphite ketenes gel is prepared：The graphene hydrogel is placed in progress solvent displacement in acetone soln, obtains graphite
Ketenes gel；
(4) graphene aerogel is prepared：The graphite ketenes gel is taken out into simultaneously supercritical drying, obtains fibre-reinforced graphite
Alkene aerogel material；
Wherein, the skeleton filler is selected from by group that such as lower skeleton filler systems form：Resorcinol+formaldehyde；Melamine+first
Aldehyde；Phenolic resin+formaldehyde；Cresols+formaldehyde；Poly- isocyanide ester；1,3,5-trihydroxybenzene+formaldehyde；Resorcinol+poly- N- methylols third
Acrylamide.
2. according to the method for claim 1, it is characterised in that in step (1), the graphene oxide is graphene water
The form of solution.
3. according to the method for claim 2, it is characterised in that the graphene oxide is in the graphene aqueous solution
Concentration 0.05mg/ml to 20mg/ml.
4. according to the method in any one of claims 1 to 3, it is characterised in that in step (2), the mould is added
Heat is to 60 DEG C to 90 DEG C.
5. according to the method for claim 4, it is characterised in that the mould is positioned in baking oven and carried out.
6. according to the method for claim 5, it is characterised in that the reaction time is 48 hours to 72 hours.
7. according to the method in any one of claims 1 to 3, it is characterised in that in step (3), the solvent displacement
An acetone was changed for 2 days, is replaced 3 times altogether.
8. according to the method in any one of claims 1 to 3, it is characterised in that the skeleton filler and the oxidation stone
The mass ratio of black alkene is 1：10-10：10.
9. according to the method in any one of claims 1 to 3, it is characterised in that the catalyst is selected from by hydroboration
Sodium, hydrazine hydrate, ethylenediamine, ascorbic acid, lithium aluminium hydride reduction, p-phenylenediamine, hydroiodic acid, diethylamine, propane diamine, butanediamine, diethyl
Alkene triamine, triethylene tetramine, the group of TEPA composition.
10. according to the method for claim 9, it is characterised in that the mass ratio of the graphene oxide and the catalyst
For 1：1 to 200：1.
11. according to the method in any one of claims 1 to 3, it is characterised in that the reinforcing fiber selects free carbon fine
The group that dimension, Zirconium oxide fibre, mullite fiber and alumina fibre form.
12. according to the method for claim 1, it is characterised in that the reinforcing fiber and the quality of the precursor solution
Than being 80：20 to 90：10.
13. graphene aerogel material made from the method according to any one of claim 1 to 12.
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| CN101941693B (en) * | 2010-08-25 | 2012-07-25 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN101948296B (en) * | 2010-09-28 | 2013-08-21 | 航天特种材料及工艺技术研究所 | High-performance thermal insulation material and preparation method thereof |
| CN102774824B (en) * | 2012-06-11 | 2014-08-20 | 北京化工大学 | Method for preparing graphene crosslinked type organic aerogel and carbon aerogel by normal-pressure drying |
| WO2014163403A1 (en) * | 2013-04-02 | 2014-10-09 | 주식회사 관평기술 | Coating composition containing composite aerogel and method for manufacturing same |
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