CN106634855A - Preparation method of hybrid graphene gel/phase-change heat-conducting composite material - Google Patents
Preparation method of hybrid graphene gel/phase-change heat-conducting composite material Download PDFInfo
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- CN106634855A CN106634855A CN201610965453.7A CN201610965453A CN106634855A CN 106634855 A CN106634855 A CN 106634855A CN 201610965453 A CN201610965453 A CN 201610965453A CN 106634855 A CN106634855 A CN 106634855A
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The invention relates to a preparation method of a hybrid graphene gel/phase-change heat-conducting composite material. The preparation method comprises the following steps that 1, graphite oxide is taken and dispersed in water and is prepared into an oxidized graphene solution; 2, the oxidized graphene solution obtained in the step 1 is put in a reaction kettle, and hydrothermal reaction and drying are performed to obtain graphene gel; 3, then a solid-liquid organic phase-change material and the graphene gel prepared in the step 2 are put under vacuum condition, heating is performed to remove excessive solid-liquid organic phase-change material, and cooling is performed to obtain the graphene gel/phase-change heat-conducting composite material. Compared with the prior art, the prepared composite material has excellent thermal conductivity, electrical conductivity and thermal stability, the problems of low thermal conductivity, electrical insulation and the like of phase-change energy storage materials existing in the prior art are solved, and the preparation method is simple, low in cost, good in repeatability and the like.
Description
Technical field
The present invention relates to graphene nanocomposite material technical field, more particularly, to a specific admixture Graphene gel/phase
Become the preparation method of heat-conductive composite material.
Background technology
At present, energy problem becomes the bottleneck that restriction human material and cultural life are further improved.Phase-change material exists
In its phase transition process, heat can be absorbed or released from environment such that it is able to storage and release heat energy, be effectively improved the energy
Utilization rate.Thus in recent years, phase-changing energy storage material is increasingly becoming the focus in terms of using energy source and investigation of materials.Can be extensive
It is applied to the fields such as solar thermal utilization, building energy conservation and heat management.Organic phase change material have phase transition temperature adaptability it is good,
Latent heat of phase change is big, stable chemical performance many advantages, such as, thus widely studied.But organic phase change material heat conductivility
Relatively low, Volume Changes are big in phase transition process, easily reveal so being subject to certain restrictions in application process.It is high with heat conductivility,
The Material cladding of stable performance is current effectively solution into the heat conductivility that phase change composite material has improved material.
Graphene is a kind of two-dimentional new carbon.Its unique structure imparts many excellent performances of Graphene.Stone
Black alkene has high thermal conductivity and electrical conductivity, and has good heat endurance.This ideal for causing it and becoming Heat Conduction Material is filled out
Material, the shortcoming for overcoming single phase transformation material thermal conductivity low improves heat exchange efficiency, realizes composite heat transfer and heat accumulation integration.
But it is uneven that Graphene has a dispersion as filler, easily stacking the problems such as limit its application.Thus by Graphene self assembly
Into three-dimensional network material for the practical application of Graphene has value.Three-dimensional grapheme cross-linked network has stable thermal conductivity
Rate, low-density and chemical stability etc., are suitable as the carrier of heat filling and phase-change material.By three-dimensional grapheme material and phase
Become Material cladding to be conducive to improving the heat conductivility and heat endurance of phase-change material.Such as the disclosure of Chinese patent 201610209084.9
A kind of high heat conduction gel film and preparation method thereof, the high heat conduction gel film includes silicone oil matrix and heat filling；The silicone oil
Matrix is vinyl-terminated silicone fluid and end containing hydrogen silicone oil；The heat filling is metal oxide or/and hydroxide or/and graphite
Alkene.
Chinese patent 201610049411.9 discloses a kind of three-dimensional phase-change material based on Graphene and preparation method thereof.
Certain density graphene oxide water solution is put into snap frozen in liquid nitrogen, then graphene oxide is obtained by freeze-drying
Aeroge, sends into and carry out under an inert atmosphere in high temperature furnace 500 DEG C of -3000 DEG C of heat treatments of high temperature, is then immersed in variable concentrations
Paraffin dichloromethane solution in, after fully absorbing, then be put in 30 DEG C of vacuum drying ovens be dried, obtain based on Graphene three
Dimension phase-change material.
The content of the invention
The purpose of the present invention is exactly the defect in order to overcome above-mentioned prior art to exist and provides a specific admixture Graphene and coagulate
The preparation method of glue/heat conduction with phase change composite.
The purpose of the present invention can be achieved through the following technical solutions：
The preparation method of one specific admixture Graphene gel/heat conduction with phase change composite, comprises the following steps：
(1) take graphite oxide to be dispersed in water, be made into graphene oxide solution；
(2) graphene oxide solution that step (1) is obtained is placed in reactor, hydro-thermal reaction, is dried, obtain Graphene
Gel；
(3) solid-liquid organic phase change material and Graphene gel obtained in step (2) be placed under vacuum condition again, heated,
Unnecessary solid-liquid organic phase change material is removed, is cooled down, that is, obtain Graphene gel/heat conduction with phase change composite.
Preferably, the concentration of graphene oxide solution is 2-4mg/mL in step (1).
Preferably, the temperature of hydro-thermal reaction is 160-200 DEG C in step (2), and the time is 12-24h.
Preferably, the drying in step (2) is：Reacted Graphene column is taken out, using vacuum freeze-drying machine vacuum
Lyophilized 24h.
Preferably, in step (3)：Before heating, it is ensured that mix Graphene gel and have been placed in 1-2h under vacuum condition.
Preferably, the temperature of heating is 80 DEG C in step (3).
Solid-liquid organic phase change material described in step (3) is hexadecylic acid.
Step (1) obtains also carrying out following process after graphene oxide solution：
Graphene nanometer sheet is additionally added toward graphene oxide solution, graphene oxide/graphene solution is obtained after dispersion,
Graphene oxide/graphene solution is placed in reactor again, carries out step (2) and step (3) process.
In graphene oxide/graphene solution, graphene oxide is not less than 1 with the mass ratio of graphene nanometer sheet:1.
The present invention in order to solve prior art in there are problems that phase-changing energy storage material thermal conductivity it is low, with oxidation
Graphene is surfactant, and dispersed graphite alkene nanometer sheet obtains homodisperse graphene/graphene oxide solution, and leads to
Hydrothermal reduction reaction is crossed, makes graphene oxide reduce to form the three-dimensional grapheme gel for mixing.By vacuum impregnation so that phase transformation
Material is filled in graphene three-dimensional structure, effectively prevents the seepage flow of phase-change material, and with the stone of excellent heat conducting performance
Black alkene nanometer sheet can further improve the heat conductivility of phase-change material as heat filling, and absorption phase-change material improves phase transformation material
The heat endurance of material.Additionally, due to unique Graphene hybrid structure, the heat storage capacity of composite is also improved.Using
Composite prepared by the present invention has excellent thermal conductivity, electric conductivity and heat endurance.
Graphene oxide has amphipathic, surface-active of the present invention first with graphene oxide so as to as dispersion
Agent, dispersed graphite alkene nanometer sheet obtains homodisperse graphene/graphene oxide solution.Therefore different quality can be added
Graphene nanometer sheet, but the mass ratio of graphene nanometer sheet does not exceed 1:1, it is impossible to formed homodisperse Graphene/
Graphene oxide solution.And both mass ratioes are prepared for for 1:0 solution, that is, be added without graphene nanometer sheet, is carried out with this
Contrast, compares impact of the graphene nanometer sheet to composite.
The solution for mixing is reduced by hydro-thermal, the temperature of hydro-thermal reaction is 160-200 DEG C, and the time is 12-24h.
Due to the poor thermal conductivity of graphene oxide, can be reduced by hydro-thermal reaction, and be formed the network of three-dimensional.Graphene oxide
Reducing degree it is relevant with reaction temperature and time, using the condition in the present invention, graphene oxide is obtained effectively reduction.
Again by vacuum impregnation cause phase-change material and the Graphene gel for mixing it is compound (vacuum 0.09Mpa～
0.01Mpa, reacts 1-2h).The air mixed under vacuum condition in the hole of graphene three-dimensional structure is pumped, the phase transformation material of melting
Material can be filled in three-dimensional structure.
Graphene nanometer sheet has excellent heat conductivility in the present invention, therefore the addition of graphene nanometer sheet makees can it
For the heat conductivility that heat filling improves phase-change material.And due to the peptizaiton of graphene oxide, stone in preparation process
Black alkene nanometer sheet can be uniformly dispersed in three-dimensional structure, form more thermal conducting paths, improve material heat conductivility and
Its heat endurance.
Compared with prior art, the present invention has advantages below：
(1) with graphene oxide as surfactant, dispersed graphite alkene nanometer sheet obtains homodisperse graphite to the present invention
Alkene/graphene oxide solution, and reacted by hydrothermal reduction, make graphene oxide obtain graphene nanometer sheet while reduction equal
The even scattered three-dimensional grapheme gel for mixing.Its structure can be adjusted by the volume of graphene nanometer sheet.The present invention
The performance of composite can be adjusted by different nanometer sheet additions.
(2) different from the three-dimensional grapheme obtained by hydro-thermal method, graphene film is dispersed in three-dimensional knot in the present invention
In structure.Graphene nanometer sheet with excellent heat conducting performance can further improve the thermal conductivity of phase-change material as heat filling
Can, and adsorb the heat endurance that phase-change material improves phase-change material.Phase change composite material prepared by the present invention is not only increased
Heat conductivility, its thermal storage performance is also improved.
(3) preparation method of the present invention is simple, with low cost, favorable repeatability.Using mix Graphene gel as heat conduction, lead
Electric template, is combined with the organic material of solid-liquid phase-changeable, and thermal conductivity, electrical conductivity and the heat that can be effectively improved phase change composite material is steady
It is qualitative, and the technical problem of energy effectively solving easily leakage, it is adaptable to industrialized production, with good application prospect.
Description of the drawings
Fig. 1 is field emission scanning electron microscope figure of the Graphene gel of the preparation of embodiment 1 under different amplification；
Fig. 2 is field emission scanning electron microscope figure of the Graphene gel of the preparation of embodiment 2 under different amplification；
Fig. 3 is the DSC curve figure of composite prepared by embodiment 1-4 and hexadecylic acid；
Fig. 4 is the thermal conductivity figure of composite prepared by embodiment 1-4 and hexadecylic acid；
Fig. 5 is the resistivity of composite prepared by embodiment 1-4.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in detail with specific embodiment.
Embodiment 1
(1) it is graphite oxide is soluble in water, 60min, ultrasonic 2h are stirred, certain density graphene oxide solution is made into,
Concentration range is 4mg/ml；
(2) take 50ml graphene oxide solutions to be placed in reactor, hydro-thermal reaction 24h at 180 DEG C.Reaction terminates
Graphene column is taken out afterwards, using vacuum freeze-drying machine vacuum freeze-drying 24h is carried out, obtain Graphene gel.
(3) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1h, heat at 80 DEG C, melt phase-change material, take out after 2h.Unnecessary phase-change material is filtered
Fall, treat that sample drops to room temperature and obtains mixing Graphene gel phase change composite material.
Embodiment 2
(1) it is graphite oxide is soluble in water, 60min, ultrasonic 2h are stirred, certain density graphene oxide solution is made into,
Concentration range is 4mg/ml；
(2) 50ml graphene oxide solutions are taken, (graphene oxide is received with Graphene to add a certain amount of graphene nanometer sheet
The mass ratio of rice piece is 4：1), 30min, ultrasonic 2h are stirred, obtains graphene oxide/graphene solution.
(3) it is placed in reactor, hydro-thermal reaction 24h at 180 DEG C.Reaction takes out Graphene column after terminating,
Vacuum freeze-drying 24h is carried out using vacuum freeze-drying machine, obtains mixing Graphene gel.
(4) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1h, heat at 80 DEG C, melt phase-change material, take out after 2h.Unnecessary phase-change material is filtered
Fall, treat that sample drops to room temperature and obtains mixing Graphene gel phase change composite material.
Fig. 1 and Fig. 2 are respectively in embodiment 1 ESEM for mixing Graphene gel in Graphene gel and embodiment 2
Figure.The Graphene gel of preparation can be seen and mix Graphene gel and be as three-dimensional porous shape, but be mixed in Graphene gel
Can see that graphene film is dispersed in mesh skeleton.
Embodiment 3
(1) it is graphite oxide is soluble in water, 60min, ultrasonic 2h are stirred, certain density graphene oxide solution is made into,
Concentration range is 4mg/ml；
(2) 50ml graphene oxide solutions are taken, (graphene oxide is received with Graphene to add a certain amount of graphene nanometer sheet
The mass ratio of rice piece is 2：1), 30min, ultrasonic 2h are stirred, obtains graphene oxide/graphene solution.
(3) it is placed in reactor, hydro-thermal reaction 24h at 180 DEG C.Reaction takes out Graphene column after terminating,
Vacuum freeze-drying 24h is carried out using vacuum freeze-drying machine, obtains mixing Graphene gel.
(4) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1h, heat at 80 DEG C, melt phase-change material, take out after 2h.
Embodiment 4
(1) it is graphite oxide is soluble in water, 60min, ultrasonic 2h are stirred, certain density graphene oxide solution is made into,
Concentration range is 4mg/ml；
(2) 50ml graphene oxide solutions are taken, (graphene oxide is received with Graphene to add a certain amount of graphene nanometer sheet
The mass ratio of rice piece is 1：1), 30min, ultrasonic 2h are stirred, obtains graphene oxide/graphene solution.
(3) it is placed in reactor, hydro-thermal reaction 24h at 180 DEG C.Reaction takes out Graphene column after terminating,
Vacuum freeze-drying 24h is carried out using vacuum freeze-drying machine, obtains mixing Graphene gel.
(4) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1h, heat at 80 DEG C, melt phase-change material, take out after 2h
The DSC curve of the composite in embodiment is as shown in Figure 3, it can be seen that the phase transition temperature of composite is hardly
Become, enthalpy of phase change does not lose.Thermal conductivity and resistivity such as Fig. 4 of composite, shown in 5, the heat conductivility of composite and
Electric conductivity is improved significantly.
The composite prepared in above-described embodiment 1-4 and the hot property of hexadecylic acid are specifically shown in table 1 below.
Table 1
| Sample | Tm(℃) | ΔHm(J/g) | Tf(℃) | ΔHf(J/g) |
| Hexadecylic acid | 63.08 | 194.4 | 59.98 | 187.3 |
| Embodiment 1 | 63.59 | 202.4 | 60.45 | 201 |
| Embodiment 2 | 63.45 | 213.2 | 59.99 | 212 |
| Embodiment 3 | 63.13 | 201.3 | 60.5 | 199.5 |
| Embodiment 4 | 63.19 | 206.2 | 60.69 | 203 |
Embodiment 5
(1) it is graphite oxide is soluble in water, 45min, ultrasonic 1.5h are stirred, it is made into certain density graphene oxide molten
Liquid, concentration range is 3mg/ml；
(2) 50ml graphene oxide solutions are taken, (graphene oxide is received with Graphene to add a certain amount of graphene nanometer sheet
The mass ratio of rice piece is 6：1), 45min, ultrasonic 1.5h are stirred, obtains graphene oxide/graphene solution.
(3) it is placed in reactor, hydro-thermal reaction 18h at 160 DEG C.Reaction takes out Graphene column after terminating,
Vacuum freeze-drying 24h is carried out using vacuum freeze-drying machine, obtains mixing Graphene gel.
(4) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1.5h, heat at 80 DEG C, melt phase-change material, take out after 2h.By unnecessary phase-change material mistake
Filter, treat that sample drops to room temperature and obtains mixing Graphene gel phase change composite material.
Embodiment 6
(1) it is graphite oxide is soluble in water, 45min, ultrasonic 1.5h are stirred, it is made into certain density graphene oxide molten
Liquid, concentration range is 3mg/ml；
(2) 50ml graphene oxide solutions are taken, (graphene oxide is received with Graphene to add a certain amount of graphene nanometer sheet
The mass ratio of rice piece is 8：1), 45min, ultrasonic 1.5h are stirred, obtains graphene oxide/graphene solution.
(3) it is placed in reactor, hydro-thermal reaction 12h at 200 DEG C.Reaction takes out Graphene column after terminating,
Vacuum freeze-drying 24h is carried out using vacuum freeze-drying machine, obtains mixing Graphene gel.
(4) will be placed in vacuum drying chamber using hexadecylic acid as phase-change material and Graphene gel, be vacuumized.
Maintain under vacuum condition after 1.5h, heat at 80 DEG C, melt phase-change material, take out after 2h.By unnecessary phase-change material mistake
Filter, treat that sample drops to room temperature and obtains mixing Graphene gel phase change composite material.
The above-mentioned description to embodiment is that invention is understood that and used for ease of those skilled in the art.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel announcement of the invention, the improvement made without departing from scope and modification all should be the present invention's
Within protection domain.
Claims (9)
1. the preparation method of a specific admixture Graphene gel/heat conduction with phase change composite, it is characterised in that comprise the following steps：
(1) take graphite oxide to be dispersed in water, be made into graphene oxide solution；
(2) graphene oxide solution that step (1) is obtained is placed in reactor, hydro-thermal reaction, is dried, obtained Graphene and coagulate
Glue；
(3) solid-liquid organic phase change material and Graphene gel obtained in step (2) be placed under vacuum condition again, heated, removed
Unnecessary solid-liquid organic phase change material, cooling, that is, obtain Graphene gel/heat conduction with phase change composite.
2. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that the concentration of graphene oxide solution is 2-4mg/mL in step (1).
3. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that the temperature of hydro-thermal reaction is 160-200 DEG C in step (2), and the time is 12-24h.
4. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that the drying in step (2) is：Reacted Graphene column is taken out, using vacuum freeze-drying machine vacuum freeze-drying 24h.
5. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is, in step (3)：Before heating, it is ensured that mix Graphene gel and have been placed in 1-2h under vacuum condition.
6. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that the temperature of heating is 80 DEG C in step (3).
7. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that the solid-liquid organic phase change material described in step (3) is hexadecylic acid.
8. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 1, its feature
It is that step (1) obtains also carrying out following process after graphene oxide solution：
Graphene nanometer sheet is additionally added toward graphene oxide solution, graphene oxide/graphene solution is obtained after dispersion, then will
Graphene oxide/graphene solution is placed in reactor, carries out step (2) and step (3) process.
9. the preparation method of specific admixture Graphene gel/heat conduction with phase change composite according to claim 8, its feature
It is that in graphene oxide/graphene solution, graphene oxide is not less than 1 with the mass ratio of graphene nanometer sheet:1.
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