CN106832758B - A kind of graphene/phenolic resin heat-conductive composite material and preparation method thereof - Google Patents
A kind of graphene/phenolic resin heat-conductive composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of composite materials, disclose a kind of preparation method of graphene/phenolic resin heat-conductive composite material.With graphene oxide and water, while reducing agent is added, obtains graphene hydrogel by hydrothermal reduction method, be freeze-dried later, obtains grapheme foam；Using phenol, formaldehyde, water as raw material, sodium hydroxide prepares phenolic resin suspension as basic catalyst；By the phenolic resin suspension vacuum suck grapheme foam of preparation, solidify 1 ~ 2h at 160 ~ 200 DEG C later to get target product graphene/phenolic resin heat-conductive composite material.Gained thermal conductivity of composite materials is excellent, the drawback that conventional thermal conductive density of material can be overcome big, the limitation for the discontinuity that also powdery graphite alkene can be overcome thermally conductive, and under the premise of not influencing heat-conducting effect, has the characteristics that intensity is high.Preparation method of the invention, raw material is cheap and easy to get, and preparation process is simple, convenient for industrial production.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of graphene/phenolic resin heat-conductive composite material
Preparation method.
Background technique
As human being's production level is continuously improved, the development that various fields are advanced by leaps and bounds especially is sent a telegram here in recent years
Sub-information industry flourishes, and the requirement for electronic device in life is higher and higher, and heat management and thermal transpiration have become
It is more and more important.The favor of novel lightweight, high thermal conductivity high molecular material increasingly by vast consumption market.
Conventional thermal conductive material is big, perishable because of its density, is difficult to the reasons such as processing and forming, and application is increasingly limited
System, with the development of technical level, Polymer composite heat conduction material is initially entered in everybody sight.External industrially developed country
It is more early to the development of macromolecule thermal-conducting composite material, the latter stage sixties is started from, the mid-1970s start to put into industrial applications,
Development speed is extremely swift and violent.The U.S. is to the demand of highly heat-conductive material every year with 20 ~ 30% speed increase.It is related high in Japan
The research topic of molecular composite material has been put into ten among " the 21 century Industry Foundation technical research exploitation " that 1987 work out
The research of polymer composite has also been included in national " the Seventh Five-Year Plan " weight by one of preferential scientific research project of binomial, at the same time, China
Point key scientific and technological projects and project of national nature science fund project.
For graphene as fullerene family member, this kind of material is the graphite of monoatomic thickness.Since 2004 by Geim
Since the discovery such as Novoselov, by the concern of whole world researchers.As a kind of new material, graphene has uniqueness
Mechanics, optics, calorifics and electric property, such as the quantum hall effect of non-integer, the Young's modulus of superelevation, thermal conductivity and ratio
Surface area etc..As various advantageous properties of graphene are found, how to make full use of the property of graphene by numerous researchs
The attention of scholar.
Since graphene is individual layer laminated structure, scattering of the heating conduction not only by graphene planes boundary is limited, and
And it causes to lead due to the influence of its structure in the strong limitation that will receive interlayer Van der Waals force perpendicular to graphene planes direction
The discontinuity of heat, therefore heat conduction governing has certain difficulty, this be also the slow reason of the thermally conductive progress of research of graphene it
One.
Summary of the invention
It is an object of the invention to a kind of graphene/phenolic resin heat-conductive composite material preparation method, gained composite woods
Material has the good capacity of heat transmission, and preparation method is simple.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of preparation method of graphene/phenolic resin heat-conductive composite material, comprising the following steps:
The preparation of S1, grapheme foam: graphene oxide and water are used, while reducing agent is added, is obtained by hydrothermal reduction method
It to graphene hydrogel, is freeze-dried later, obtains grapheme foam；
The preparation of S2, phenolic resin suspension: using phenol, formaldehyde, water as raw material, sodium hydroxide as basic catalyst,
Prepare phenolic resin suspension；
S3, graphene/phenolic resin heat-conductive composite material preparation: by the phenolic resin suspension vacuum suck stone of preparation
Black alkene foam solidifies 1 ~ 2h at 160 ~ 200 DEG C later to get target product graphene/phenolic resin heat-conductive composite material.
Preferably, it in S3, counts in mass ratio, grapheme foam: phenolic resin suspension=1 ~ 2g: 3 ~ 5g.
Preferably, the step of S1 are as follows:
S1.1, graphene oxide is dissolved in the water, ultrasonic disperse；
S1.2, the graphene oxide water solution after ultrasonic disperse is taken out, is placed in hydrothermal reaction kettle, ascorbic acid is added,
First in 100 ~ 120 DEG C of 30 ~ 50min of heat preservation, 150 ~ 200 DEG C of 24 ~ 48h of heat preservation are then heated to, graphene hydrogel is obtained；
S1.3, graphene hydrogel is taken out, is freeze-dried, obtain grapheme foam；
Wherein, based on mass volume ratio, graphene oxide: water: ascorbic acid=80 ~ 120mg: 40 ~ 60mL: 2 ~ 12mg.
Preferably, in S1.2, ascorbic acid is added in the form of its aqueous solution.
Preferably, the step of S2 are as follows:
S2.1, phenol, water, sodium hydroxide are condensed back 20 ~ 30min under the conditions of 40 ~ 60 DEG C；
S2.2,60 ~ 65 DEG C are then warming up to, every 10 ~ 15min points of 3 ~ 4 addition solid formaldehydes；
S2.3, after solid formaldehyde is added, 4 ~ 5h of insulation reaction then heats to 70 ~ 80 DEG C, the reaction was continued 4 ~
4.5h；
S2.4,50 ~ 60 DEG C are cooled to, the p-methyl benzenesulfonic acid aqueous solution that mass fraction is 60 ~ 70% is added, adjust pH value to 7
~ 8, obtain phenolic resin suspension；
Wherein, it counts in mass ratio, phenol: sodium hydroxide: water: solid formaldehyde=90 ~ 100g: 5 ~ 10g: 5 ~ 10g: 105 ~
120g, solid formaldehyde is in terms of its gross mass.
In the present invention, passes through hydrothermal reduction method first with graphene oxide, while reducing agent is added, obtain graphene water-setting
Glue, then be freeze-dried to obtain grapheme foam, phase is carried out with the phenolic resin suspension prepared followed by by grapheme foam
The solidification of pass controls curing time and solidification temperature, obtains graphene of the invention/phenolic resin heat-conductive composite material.Wherein,
The introducing of reducing agent ascorbic acid plays a dual role of abundant redox graphene and adjustment graphene-structured.
The utility model has the advantages that the present invention first prepares grapheme foam, then method is entered by vacuum absorption and introduces phenolic resin, solidification
Afterwards, phenolic resin is evenly distributed in graphene, therefore gained graphene/phenolic resin heat-conductive composite material thermal coefficient is excellent
Drawback good, that conventional thermal conductive density of material can be overcome big, the limit for the discontinuity that also powdery graphite alkene can be overcome thermally conductive
System.Graphene high-heat-conductive composite material of the invention can be used for the thermally conductive field of polymer, overcome tradition to lead to a certain extent
The drawbacks of hot material, and under the premise of not influencing heat-conducting effect, have the characteristics that intensity is high.Preparation method of the invention,
Raw material is cheap and easy to get, and preparation process is simple, convenient for industrial production.
Specific embodiment
The present invention is further introduced below in conjunction with body embodiment.
Embodiment 1
A kind of preparation method of graphene/phenolic resin heat-conductive composite material, comprising the following steps:
The preparation of S1, grapheme foam:
S1.1,80mg graphene oxide is dissolved in 40mL deionized water, ultrasonic disperse 30min；Compound concentration simultaneously
For the aqueous ascorbic acid of 2mg/mL；
S1.2, the graphene oxide water solution after ultrasonic disperse is taken out, is placed in ptfe autoclave liner,
It is separately added into aqueous ascorbic acid by 1 dosage of table, inner liner of reaction kettle is put in reaction kettle, vacuum drying oven is then placed in
In, adjustment temperature is 100 DEG C, keeps the temperature 40min, then heats to 180 DEG C of heat preservations for 24 hours, obtains graphene hydrogel；
S1.3, hydrogel is taken out, is freeze-dried, obtain grapheme foam；
The preparation of S2, phenolic resin suspension:
S2.1, phenol 90g, sodium hydroxide 5g, water 5g, control system temperature are 43 DEG C, are condensed back 30min；
S2.2,60 DEG C then are warming up to, are added three times solid formaldehyde every 10min, solid formaldehyde 35g is added every time；
S2.3, after solid formaldehyde is added, insulation reaction 4h is warming up to 80 DEG C, the reaction was continued 4h；
S2.4,55 DEG C are cooled to, the p-methyl benzenesulfonic acid aqueous solution that mass fraction is 70% is added, adjusted pH value to 7, obtain phenol
Urea formaldehyde suspension；
S3, the preparation of graphene/phenolic resin composite:
Count in mass ratio, grapheme foam: graphene bubble end is placed in phenolic resin and hanged by phenolic resin suspension=1g: 3g
It in supernatant liquid, is then vacuumized using circulating vacuum pump, the phenolic resin suspension of preparation is sucked into grapheme foam, Zhi Hou
Solidify 1.5h at 180 DEG C to get target product graphene/phenolic resin heat-conductive composite material.
Table 1 is shadow of the dosage to gained graphene hydrogel density of reducing agent in the present embodiment (aqueous ascorbic acid)
Variation is rung, can be seen that the content increase with ascorbic acid from table, the density of graphene hydrogel is in a certain range
Fluctuation, is intended to 1g/cm3, density is lower than common metal Heat Conduction Material, therefore passes through the Heat Conduction Material of grapheme foam preparation
The drawback that conventional thermal conductive density of material can be overcome big.
Graphene/phenolic resin heat-conductive composite material of test 3mL aqueous ascorbic acid dosage preparation is thermally conductive respectively
Coefficient and compression strength, as a result are as follows: the thermal coefficient of composite material is about 0.4W/ (mK), and the compression strength of composite material is about
1.0Mpa；Consulting literatures are it is found that the thermal coefficient of phenolic resin is the left and right 0.023 W/ (mK).The result shows that: composite material
The high-termal conductivity that can make full use of three-dimensional shape graphene has the characteristics that intensity is high under the premise of not influencing heat-conducting effect.
This is because: this patent passes through the method for hydrothermal reduction graphene oxide, can make to realize self assembly between graphene sheet layer, from
And graphene three-dimensional structure is formed, the boundary of graphene film interlayer Van der Waals force, graphene sheet layer is reduced to a certain extent
Influence of the scattering process to the thermal conductivity of graphene makes graphene continuity in phenolic resin is thermally conductive to be achieved；It is same with this
When, it is compound by being carried out with phenolic resin, the intensity of three-dimensional grapheme can be improved to a certain extent, can overcome self assembly
Obtain the lower disadvantage of the grapheme material intensity of three-dimensional structure.
Reference examples 2
With the difference of embodiment 1, it is " without the hydrothermal reduction self assembly of graphene oxide ", i.e. omission step
S1, while S3 step is changed are as follows: it counts in mass ratio, powdery graphite alkene: phenolic resin suspension=1g: 3g, by the phenolic aldehyde of preparation
Resin is blended with powdery graphite alkene, solidifies 1.5h at 180 DEG C later to get graphene/phenolic resin composite.
Graphene/phenolic resin composite of reference examples preparation does not have thermal coefficient, this is because powdery graphite
Alkene is thermally conductive to have discontinuity, thus after the powdered graphene of doping, there is no apparent effects for thermal coefficient.
Reference examples 3
With the difference of embodiment 1, it is " solidification is directly blended in the graphene hydrogel of preparation with phenolic resin ",
Step S1.3 is omitted, while S3 step is changed are as follows: count in mass ratio, graphene hydrogel: phenolic resin suspension=1g: 3g,
The phenolic resin of preparation is blended with graphene hydrogel, solidifies 1.5h at 180 DEG C later to get graphene/phenolic resin
Composite material.
Graphene/phenolic resin composite thermal coefficient of reference examples preparation is a changing value, thermal coefficient
Change as position is different, this is because vacuumizing sucking phenolic resin suspension, phenol without using circulating vacuum pump
Urea formaldehyde is not dispersed in graphene hydrogel, therefore thermal coefficient is not single, related with position, and due to wherein containing
There is a large amount of water, the compression strength of gained composite material is lower (< 1Mpa).
Claims (4)
1. a kind of graphene/phenolic resin heat-conductive composite material preparation method, which comprises the following steps:
The preparation of S1, grapheme foam:
S1.1, graphene oxide is dissolved in the water, ultrasonic disperse；
S1.2, the graphene oxide water solution after ultrasonic disperse is taken out, be placed in hydrothermal reaction kettle, ascorbic acid is added, first exists
100 ~ 120 DEG C of 30 ~ 50min of heat preservation then heat to 150 ~ 200 DEG C of 24 ~ 48h of heat preservation, obtain graphene hydrogel；
S1.3, graphene hydrogel is taken out, is freeze-dried, obtain grapheme foam；
Wherein, based on mass volume ratio, graphene oxide: water: ascorbic acid=80 ~ 120mg: 40 ~ 60mL: 2 ~ 12mg；
The preparation of S2, phenolic resin suspension: using phenol, formaldehyde, water as raw material, sodium hydroxide is as basic catalyst, preparation
Phenolic resin suspension out；
S3, graphene/phenolic resin heat-conductive composite material preparation: by the phenolic resin suspension vacuum suck graphene of preparation
Foam solidifies 1 ~ 2h at 160 ~ 200 DEG C later to get target product graphene/phenolic resin heat-conductive composite material.
2. preparation method as described in claim 1, which is characterized in that in S3, count in mass ratio, grapheme foam: phenolic aldehyde tree
Rouge suspension=1 ~ 2g: 3 ~ 5g.
3. preparation method as described in claim 1, it is characterised in that: in S1.2, ascorbic acid is added in the form of its aqueous solution.
4. preparation method as described in claim 1, which is characterized in that the step of S2 are as follows:
S2.1, phenol, water, sodium hydroxide are condensed back 20 ~ 30min under the conditions of 40 ~ 60 DEG C；
S2.2,60 ~ 65 DEG C are then warming up to, every 10 ~ 15min points of 3 ~ 4 addition solid formaldehydes；
S2.3, after solid formaldehyde is added, 4 ~ 5h of insulation reaction then heats to 70 ~ 80 DEG C, the reaction was continued 4 ~ 4.5h；
S2.4,50 ~ 60 DEG C are cooled to, the p-methyl benzenesulfonic acid aqueous solution that mass fraction is 60 ~ 70% is added, adjusts pH value to 7 ~ 8,
Obtain phenolic resin suspension；
Wherein, it counts in mass ratio, phenol: sodium hydroxide: water: solid formaldehyde=90 ~ 100g: 5 ~ 10g: 5 ~ 10g: 105 ~ 120g, Gu
Body formaldehyde is in terms of its gross mass.
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