CN105271212A - Graphene aerogel material and preparation method thereof - Google Patents
Graphene aerogel material and preparation method thereof Download PDFInfo
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- CN105271212A CN105271212A CN201510846174.4A CN201510846174A CN105271212A CN 105271212 A CN105271212 A CN 105271212A CN 201510846174 A CN201510846174 A CN 201510846174A CN 105271212 A CN105271212 A CN 105271212A
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Abstract
The invention discloses a graphene aerogel material and a preparation method thereof. The preparation method comprises the following steps: (1) preparing a precursor solution, namely mixing graphene oxide with a framework filler, and stirring uniformly to obtain the precursor solution; (2) preparing graphene hydrogel, namely adding a catalyst into the precursor solution, stirring uniformly, then pouring into a mold containing reinforcing fibers, sealing the mold, and heating the mold for reaction, thereby obtaining fiber reinforced graphene hydrogel; (3) preparing graphene ketone gel, namely putting the graphene hydrogel into an acetone solution to perform solvent replacement so as to obtain the graphene ketone gel; and (4) preparing graphene aerogel, namely taking out the graphene ketone gel, and drying to obtain a fiber reinforced graphene aerogel material. The invention also relates to the graphene aerogel material prepared by the method, and the graphene aerogel material is low in heat conductivity and high in strength, and can be used as a high-temperature heat insulating material.
Description
Technical field
The invention belongs to technical field of composite materials, relate to a kind of preparation method of matrix material, particularly relate to a kind of preparation method of graphene aerogel material and the graphene aerogel material obtained according to described method.
Background technology
Aerogel material mutually builds up by colloidal particle or high-polymer molecular a kind of nanoporous solid material with network structure formed, because its aperture (< 50nm) is less than the mean free path (~ 70nm) of air molecule, thus in aerogel pores, do not have convection of air, there is extremely low gaseous heat conduction; Aerogel has high porosity simultaneously, and shared by solid, volume ratio is very low, and solid state heat conduction is also very low.Carbon back aerogel resistance to elevated temperatures in various aerogel best (>=1600 DEG C), has in High Mach number aircraft thermal protection field the superiority that can not be substituted.But the insufficient strength of pure aerogel material, generally all needs strongthener such as fiber to improve its intensity.
Graphene is a kind of nano-carbon material of the two-dimentional laminated structure be made up of carbon atom, has high-specific surface area.The characteristic such as strong mechanical performance, high thermal conductivity.Present stage, graphene aerogel material (Chinese patent: CN101941693A) mainly through preparation graphene oxide water solution, then obtains through the process such as sol gel reaction, drying.Graphene aerogel prepared by this process is by graphene sheet layer build stack, and the graphene aerogel intensity prepared is high, but thermal conductivity is also high, can not directly use as lagging material.About the research of graphene aerogel mainly utilizes the strong mechanical performance of Graphene and high heat conductance to improve mechanical property and the thermal conductivity of gained aerogel material in prior art.Such as, CN201210191045.2 discloses a kind of method that constant pressure and dry prepares Graphene cross-linking type organic aerogel and charcoal-aero gel, and it mainly utilizes the strong mechanical performance of Graphene to solve the excessive problem of the shrinking percentage of the aerogel that constant pressure and dry obtains.Again such as, CN201310085977.3 provides a kind of graphene oxide/organic aerogel composite with low-shrinkage, wherein utilizes Graphene itself as framework material to provide the mechanical property of gained Graphene organic aerogel composite.Again such as, CN201310504175.1 discloses the preparation method providing a kind of graphene aerogel, the method is by graphene oxide water solution and polymkeric substance: the aqueous solution of tetrafluoroethylene, polyvinyl alcohol, polyvinylidene difluoride (PVDF) or Xylo-Mucine, by cohesive action, graphene oxide structural unit be connected with polymer unit physics and form graphene oxide colloidal sol, then obtain graphene aerogel by dry, reduction, make aerogel farthest can play the performances such as the excellent conduction of Graphene, heat conduction, mechanics thus.
But, also there is no the aerogel preparation method that can keep or reduce the thermal conductivity of aerogel material while improving Mechanical Properties of Aerogels at present.
Summary of the invention
The present inventor is found by research, although it is well known that, Graphene has high thermal conductivity, but when the lower thermal conductivity by aerogel can also be reduced when the combinationally using of Graphene and framework material while the intensity improving aerogel especially fortifying fibre composite aerogel.In other words, the use of framework material can reduce the thermal conductivity of graphene aerogel material.
So one object of the present invention is to overcome the high problem of existing graphene aerogel material thermal conductivity, provides a kind of preparation method of graphene aerogel material and graphene aerogel material obtained by this method.
In first aspect, the invention provides a kind of preparation method of graphene aerogel material, wherein, described method comprises the steps:
(1) precursor solution is prepared: graphene oxide and skeleton filler are mixed and stirred, obtains precursor solution;
(2) prepare Graphene hydrogel: add catalyzer to described precursor solution and stir, then to pour in the mould being placed with fortifying fibre and to seal, mold heated being reacted, obtains fibre-reinforced Graphene hydrogel;
(3) prepare graphite ketenes gel: described Graphene hydrogel is placed in acetone soln and carries out solvent exchange, obtain graphite ketenes gel;
(4) graphene aerogel is prepared: taken out and drying by described graphite ketenes gel, obtain fibre-reinforced graphene aerogel material.
In yet another aspect, present invention also offers the graphene aerogel material obtained by described method.
The present invention's beneficial effect compared with prior art:
The present invention prepares graphene aerogel material, utilizing Graphene to while improving mechanical strength, significantly improve the defect that original graphene aerogel thermal conductivity is high, heat-proof quality is poor, thus be conducive to the widespread adoption of graphene aerogel material as lagging material.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
As mentioned above, the present invention provides a kind of preparation method of graphene aerogel material in first aspect.Generally speaking, described method of the present invention mainly comprises the steps: to prepare precursor solution, sol gel reaction, solvent exchange and drying (such as shown in Fig. 1).
More particularly, method of the present invention can comprise the steps:
(1) precursor solution is prepared: graphene oxide and skeleton filler are mixed and stirred, obtains precursor solution;
(2) prepare Graphene hydrogel: add catalyzer to described precursor solution and stir, then to pour in the mould being placed with fortifying fibre and to seal, mold heated being reacted, obtains fibre-reinforced Graphene hydrogel;
(3) prepare graphite ketenes gel: described Graphene hydrogel is placed in acetone soln and carries out solvent exchange, obtain graphite ketenes gel;
(4) graphene aerogel is prepared: taken out and drying by described graphite ketenes gel, obtain fibre-reinforced graphene aerogel material.
In some embodiments, described graphene oxide in step (1) is the form of graphene aqueous solution, preferably, the concentration 0.05mg/ml to 20mg/ml of described graphene oxide in described graphene aqueous solution (be such as 0.05,0.1,1,10 or 20mg/ml).In some embodiments, described concentration is 0.1 to 10mg/ml.In other embodiment, described concentration is 1 to 5mg/ml.
In some embodiments, in step (2) by described mold heated to 60 DEG C to 90 DEG C (they being such as 60 DEG C, 70 DEG C, 80 DEG C or 90 DEG C), temperature is too low, speed of response is slow, the consumed energy that too high temperature is then excessive and may improve the thermal conductivity of resulting materials to a certain extent.At some preferred embodiment, described mould is positioned in baking oven and carries out, it is further preferred that the reaction times is 48 little of 72 hours (being such as 48,54,60,66 or 72 hours).If overlong time, then, consumed energy is excessive; If the time is too short, then precursor solution may not react completely, and causes gel-strength poor.
In some embodiments, in step (3), described solvent exchange is within 2 days, change an acetone, altogether displacement 3 times.
In some embodiments, in step (4), described drying is preferably supercritical drying.For supercritical drying, other conventional drying methods easily crack, thus easily cause detrimentally affect to material property.
In general, in some embodiments, the present invention preferably uses the framework material system finally obtaining carbon aerogels.In some embodiments, described skeleton filler is selected from the group be made up of such as lower skeleton filler systems: Resorcinol+formaldehyde; Trimeric cyanamide+formaldehyde; Resol+formaldehyde; Mixture cresol+formaldehyde; Poly-isocyanide ester; Phloroglucinol monomethyl ether+formaldehyde; Resorcinol+poly-N hydroxymethyl acrylamide.In one preferred embodiment, the mass ratio of described skeleton filler and described graphene oxide is 1: 10-10: 10 (being such as 1: 1,1: 2,1: 3,1: 4,1: 5,1: 6,1: 7,1: 8,1: 9 or 1: 10).If the consumption of described skeleton filler is too low, then cannot reduce thermal conductivity fully, if the consumption of described framework material is excessive, then reduce the intensity of resulting materials, thus the high strength that Graphene brings cannot be given full play to.Skeleton filler is when being made up of two kinds of materials as above, and the mol ratio that described skeleton filler is preferably two kinds of materials is the mixture of 1: 2.
In some embodiments, described catalyzer is be selected from the group be made up of sodium borohydride, hydrazine hydrate, quadrol, xitix, lithium aluminum hydride, Ursol D, hydroiodic acid HI, diethylamine, propylene diamine, butanediamine, diethylenetriamine, triethylene tetramine, tetraethylene pentamine; Preferably, the mass ratio of described graphene oxide and described catalyzer is 1: 1-200: 1 (being such as 1,10,20,50,60: 1).If catalyst ratio is too small, presoma cannot gel, if ratio is excessive, then and catalyzer residue and such as cause waste.In addition, the present inventor finds, in body series, such as ammoniacal liquor or other strong acid and strong bases can not gels, are thus not suitable as catalyzer.
The present invention has no particular limits fortifying fibre, and such as in some embodiments, described fortifying fibre can be selected from the group be made up of carbon fiber, Zirconium oxide fibre, mullite fiber and sapphire whisker; Preferably, the mass ratio of described fortifying fibre and described precursor solution is 80: 20-90: 10, such as, be 80: 20,85: 15 or 90: 10.If fortifying fibre consumption is too small, then may have influence on the intensity of resulting materials; If fortifying fibre consumption is much, then may have influence on the material that the thermal conductivity of resulting materials is high.
In a second aspect of the present invention, provide the graphene aerogel material that the method described in first aspect present invention obtains.
Below in conjunction with Fig. 1 and specific examples, the present invention is described in detail.
Embodiment 1
Adopt the graphene oxide solution of 0.2mg/ml, Resorcinol+formaldehyde systems is as skeleton filler, and the mass ratio of graphene oxide and skeleton filler is 10: 1, after the two mixes, add the Ursol D of 50 times of graphene oxide quality, after stirring, pour into and placed in the mould of carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80: 20, after sealing, be placed in baking oven, 80 DEG C are reacted 2 days, obtain Graphene hydrogel.Taken out by Graphene hydrogel after sol-gel, be placed in acetone soln, carry out solvent exchange, within 2 days, change an acetone, displacement 3 times, obtains the graphite ketenes gel of acetone solvent altogether.Graphite ketenes gel is taken out, through supercritical drying, prepares fibre-reinforced graphene aerogel material.Then thermal conductivity and the strength of materials (compressive strength, lower same) of resulting materials is measured.
Thermal conductivity measurements is carried out according to GB/T10295-2008 " the mensuration heat flowmeter method of Technology of Steady State Thermal Resistance of Thermal Insulating Material and related characteristics ";
The measuring method of the strength of materials is carried out according to GB/T8813-2008 " mensuration of rigid foam compression performance ".
Embodiment 2
Adopt the graphene oxide solution of 0.5mg/ml, trimeric cyanamide+formaldehyde systems is as skeleton filler, and the mass ratio of graphene oxide and skeleton filler is 10: 1, after the two mixes, add the quadrol of 100 times of graphene oxide quality, after stirring, pour into and placed in the mould of carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80: 20, after sealing, be placed in baking oven, 80 DEG C are reacted 2 days, obtain Graphene hydrogel.Taken out by Graphene hydrogel after sol-gel, be placed in acetone soln, carry out solvent exchange, within 2 days, change an acetone, displacement 3 times, obtains the graphite ketenes gel of acetone solvent altogether.Graphite ketenes gel is taken out, through supercritical drying, prepares fibre-reinforced graphene aerogel material.Then thermal conductivity and the strength of materials of resulting materials is measured.
Embodiment 3
Adopt the graphene oxide solution of 1mg/ml, resol+formaldehyde systems is as skeleton filler, and the mass ratio of graphene oxide and skeleton filler is 10: 1, after the two mixes, add the diethylenetriamine of 100 times of graphene oxide quality, after stirring, pour into and placed in the mould of carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80: 20, after sealing, be placed in baking oven, 80 DEG C are reacted 2 days, obtain Graphene hydrogel.Taken out by Graphene hydrogel after sol-gel, be placed in acetone soln, carry out solvent exchange, within 2 days, change an acetone, displacement 3 times, obtains the graphite ketenes gel of acetone solvent altogether.Graphite ketenes gel is taken out, through supercritical drying, prepares fibre-reinforced graphene aerogel material.Then thermal conductivity and the strength of materials of resulting materials is measured.
Embodiment 4
Adopt the graphene oxide solution of 2mg/ml, mixture cresol+formaldehyde systems is as skeleton filler, and the mass ratio of graphene oxide and skeleton filler is 10: 1, after the two mixes, add the hydrazine hydrate of 100 times of graphene oxide quality, after stirring, pour into and placed in the mould of carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80: 20, after sealing, be placed in baking oven, 90 DEG C are reacted 2 days, obtain Graphene hydrogel.Taken out by Graphene hydrogel after sol-gel, be placed in acetone soln, carry out solvent exchange, within 2 days, change an acetone, displacement 3 times, obtains the graphite ketenes gel of acetone solvent altogether.Graphite ketenes gel is taken out, through supercritical drying, prepares fibre-reinforced graphene aerogel material.Then thermal conductivity and the strength of materials of resulting materials is measured.
Embodiment 5
Adopt the graphene oxide solution of 5mg/ml, Phloroglucinol monomethyl ether+formaldehyde systems is as skeleton filler, and the mass ratio of graphene oxide and skeleton filler is 10: 1, after the two mixes, add the xitix of 50 times of graphene oxide quality, after stirring, pour into and placed in the mould of carbon fiber in advance, the mass ratio of its carbon fiber and precursor solution is 80: 20, after sealing, be placed in baking oven, 60 DEG C are reacted 3 days, obtain Graphene hydrogel.Taken out by Graphene hydrogel after sol-gel, be placed in acetone soln, carry out solvent exchange, within 2 days, change an acetone, displacement 3 times, obtains the graphite ketenes gel of acetone solvent altogether.Graphite ketenes gel is taken out, through supercritical drying, prepares fibre-reinforced graphene aerogel material.Then thermal conductivity and the strength of materials of resulting materials is measured.
Embodiment 6 to 17
Except being otherwise noted, otherwise adopting the method identical with embodiment 1 to prepare graphene aerogel material according to raw material as shown in table 1 below and processing condition, then measuring 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, this skeleton filler is two kinds of material mol ratios is the mixture of 1: 2.
Embodiment 17 is according to bibliographical information (ZhangX., SuiZ., XuB., YueS., LuoY., ZhanW., etal.Mechanicallystrongandhighlyconductivegrapheneaeroge landitsuseaselectrodesforelectrochemicalpowersources.JMa terChem.2011, 21 (18): 6494-6497.) graphene aerogel preparation method, prepare fiber reinforced graphite alkene aerogel material, all the other steps are identical with embodiment 5, the material contrast that obtained graphene aerogel material property and embodiment 5 obtain, find that its thermal conductivity is higher, be not suitable as materials'use.
To sum up, the preparation method of this patent and bibliographical information associated materials contrasts, conbined usage skeleton filler and Graphene, can prepare the graphene aerogel material that heat-proof quality is good.
The unspecified part of the present invention is known to the skilled person technology.
Claims (10)
1. a preparation method for graphene aerogel material, is characterized in that, described method comprises the steps:
(1) precursor solution is prepared: graphene oxide and skeleton filler are mixed and stirred, obtains precursor solution;
(2) prepare Graphene hydrogel: add catalyzer to described precursor solution and stir, then to pour in the mould being placed with fortifying fibre and to seal, mold heated being reacted, obtains fibre-reinforced Graphene hydrogel;
(3) prepare graphite ketenes gel: described Graphene hydrogel is placed in acetone soln and carries out solvent exchange, obtain graphite ketenes gel;
(4) graphene aerogel is prepared: taken out and drying by described graphite ketenes gel, obtain fibre-reinforced graphene aerogel material.
2. method according to claim 1, it is characterized in that, in step (1), described graphene oxide is the form of graphene aqueous solution, preferably, the concentration 0.05mg/ml to 20mg/ml of described graphene oxide in described graphene aqueous solution.
3. method according to claim 1 and 2, is characterized in that, in step (2), by described mold heated to 60 DEG C to 90 DEG C, preferably, described mould is positioned in baking oven and carries out, it is further preferred that the reaction times is 48 little of 72 hours.
4. according to the method in any one of claims 1 to 3, it is characterized in that, in step (3), described solvent exchange is within 2 days, change an acetone, altogether displacement 3 times.
5. method according to any one of claim 1 to 4, is characterized in that, in step (4), described drying is supercritical drying.
6. method according to any one of claim 1 to 5, is characterized in that, described skeleton filler is selected from the group be made up of such as lower skeleton filler systems: Resorcinol+formaldehyde; Trimeric cyanamide+formaldehyde; Resol+formaldehyde; Mixture cresol+formaldehyde; Poly-isocyanide ester; Phloroglucinol monomethyl ether+formaldehyde; Resorcinol+poly-N hydroxymethyl acrylamide.
7. method according to any one of claim 1 to 6, is characterized in that, the mass ratio of described skeleton filler and described graphene oxide is 1: 10-10: 10.
8. method according to any one of claim 1 to 7, it is characterized in that, described catalyzer is be selected from the group be made up of sodium borohydride, hydrazine hydrate, quadrol, xitix, lithium aluminum hydride, Ursol D, hydroiodic acid HI, diethylamine, propylene diamine, butanediamine, diethylenetriamine, triethylene tetramine, tetraethylene pentamine; Preferably, the mass ratio of described graphene oxide and described catalyzer is 1: 1 to 200: 1.
9. method according to any one of claim 1 to 8, is characterized in that, described fortifying fibre is selected from the group be made up of carbon fiber, Zirconium oxide fibre, mullite fiber and sapphire whisker; Preferably, the mass ratio of described fortifying fibre and described precursor solution is 80: 20 to 90: 10.
10. the graphene aerogel material that method according to any one of claim 1 to 9 is obtained.
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