CN110452667A - Graphene, which enhances phase transformation material preparation method and graphene, enhances phase-change material - Google Patents
Graphene, which enhances phase transformation material preparation method and graphene, enhances phase-change material Download PDFInfo
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- CN110452667A CN110452667A CN201910798282.7A CN201910798282A CN110452667A CN 110452667 A CN110452667 A CN 110452667A CN 201910798282 A CN201910798282 A CN 201910798282A CN 110452667 A CN110452667 A CN 110452667A
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Abstract
The embodiment of the present application provides a kind of graphene enhancing phase transformation material preparation method and graphene enhancing phase-change material, solves the problems, such as that the heating conduction of conventional phase change material is low and closing is difficult.It includes: to prepare graphene dispersing solution that the graphene, which enhances phase transformation material preparation method, wherein the graphene dispersing solution concentration is 1mg/mL-20mg/mL；The graphene dispersing solution is restored to obtain graphene hydrogel using amine curing agent, wherein the concentration of the amine curing agent is 0.1mmol-0.5mmol；Solvent replacement process and constant pressure and dry process are carried out to obtain graphene aerogel to the graphene hydrogel；And organic phase change material is filled into inside the graphene aerogel to obtain the graphene enhancing phase-change material, wherein the mass ratio of the phase-change material and the graphene aerogel is 10-30:1.
Description
Technical field
This application involves technical field of composite materials, and in particular to a kind of graphene enhancing phase transformation material preparation method and stone
Black alkene enhances phase-change material.
Background technique
There is intermittent, fluctuation and randomness feature using wind energy, solar energy as the renewable energy of representative, be stranded always
The development for disturbing renewable energy, finding ideal energy storage solution seems particularly significant.Thermal energy storage, as a kind of cleaning
Efficient energy storage mode provides good thinking for the difficult point for solving to encounter in renewable energy utilization.Phase-changing energy storage material benefit
Store heat with latent heat, have energy storage density big, the features such as phase transition process temperature is nearly constant, be widely used in space flight, building,
In the thermal energy storage system in the fields such as refrigeration equipment.But traditional phase-change material heating conduction is low, affects phase-change material and exists
Heat transfer efficiency in storage/discharge thermal process.In addition, traditional organic phase change material, due to having certain fluidity, there is also envelopes
Close problem, it is difficult to be widely applied in each application scenarios.
Summary of the invention
In view of this, the embodiment of the present application provides a kind of graphene enhancing phase transformation material preparation method and graphene enhancing
Phase-change material solves the problems, such as that the heating conduction of conventional phase change material is low and closing is difficult.
According to the one aspect of the application, a kind of graphene that one embodiment of the application provides enhances phase-change material preparation side
Method includes: to prepare graphene dispersing solution, wherein the graphene dispersing solution concentration is 1mg/mL-20mg/mL；It is solid using amine
Agent restores the graphene dispersing solution to obtain graphene hydrogel, wherein the concentration of the amine curing agent is 0.1mmol-
0.5mmol；Solvent replacement process and constant pressure and dry process are carried out to obtain graphene aerogel to the graphene hydrogel；With
And organic phase change material is filled into inside the graphene aerogel to obtain the graphene enhancing phase-change material, wherein
The mass ratio of the phase-change material and the graphene aerogel is 10-30:1.
In one embodiment of the application, it is described prepare graphene aerogel dispersion liquid include: raw graphite is added to it is mixed
It closes to form the first mixed liquor in acid solution, stirring is greater than 30 minutes；KMnO is added in first mixed liquor4, stirring is greater than
30 minutes, wherein the KMnO4Weight and the raw graphite weight ratio be 2-5:1；The KMnO will be had4Institute
It states the first mixed liquor and is warming up to 40 DEG C -60 DEG C, stirring is greater than 12 hours；After first mixed liquor is cooled to room temperature, by institute
It states the first mixed liquor and imports ice water, and hydrogen peroxide is added dropwise.
In one embodiment of the application, the raw graphite selects one of following material or a variety of: expanded graphite, squama
Piece graphite, Pintsch process graphite, graphene powder and carbon nanotube.
In one embodiment of the application, the mix acid liquor be the concentrated sulfuric acid and concentrated phosphoric acid mixed liquor, the concentrated sulfuric acid and
The ratio of concentrated phosphoric acid is 5-20:1；Wherein, the ratio of the weight of the weight and raw graphite of the mix acid liquor is 10-
500:1。
In one embodiment of the application, the volume of the ice water is 3-5 times of first mixeding liquid volume, the dioxygen
The volume of water and the ice water volume ratio are 1:150-200.
In one embodiment of the application, it is described using amine curing agent restore the graphene dispersing solution include: will be described
Graphene dispersing solution is mixed to carry out the reduction reaction with the anhydrous ethylenediamine, and is carried out at homogenization by ultrasonic procedure
Reason, wherein the temperature range of the reduction reaction is 120 DEG C -160 DEG C, and the time of the reduction reaction is -6 hours 3 hours；
Gel Jing Guo the reduction reaction is placed in subzero 18 DEG C and is once refrigerated to solid-state；And by the solid gel thaw with
Obtain the graphene hydrogel.
In one embodiment of the application, the solvent replacement process includes: by the graphene hydrogel in deionized water
Middle flushing, and dialysis -6 hours 3 hours is carried out with ethyl alcohol and the mixed solution of deionized water, wherein ethyl alcohol and deionized water
Volume ratio is 1:50-150.
In one embodiment of the application, the constant pressure and dry process includes: will be by described in the volume replacement process
Graphene hydrogel is dried in 60 DEG C or more of environment.
It is described that organic phase change material is filled into inside the graphene aerogel to obtain in one embodiment of the application
The graphene enhancing phase-change material includes: to mix the graphene aerogel with organic phase change material to have obtained the second mixing
Liquid；Second mixed liquor is placed in vacuum environment and is heated, wherein the vacuum degree of the vacuum environment is greater than 20kpa, it is described
The temperature of heating process is higher than 3 DEG C -5 DEG C of the organic phase change material fusing point, and time of the heating process is 12 hours -24 small
When.
In one embodiment of the application, the organic phase change material includes one of following different materials or a variety of groups
It closes: paraffin, decyl alcohol, tetradecyl alchohol and hexadecanol.
According to further aspect of the application, a kind of graphene that one embodiment of the application provides enhances phase-change material, adopts
With it is preceding it is any as described in method be prepared.
A kind of graphene enhancing phase transformation material preparation method and graphene provided by the embodiments of the present application enhance phase-change material,
It is to play the basis material played a supporting role to phase-change material, and phase-change material is filled into graphene with graphene aerogel
To play energy storage/exothermic effects inside aeroge, the overall mechanical properties of material are not only increased, the experiment proved that, it can also phase
Than the thermal conductivity that simple phase-change material improves 10%-35%.Meanwhile using graphene airsetting prepared by the embodiment of the present application
Glue also effectively limits the mobility of phase-change material as basis material using internal micro-structure duct, is not only does this facilitate and mentions
The thermal stability of high phase-change material also solves the closing problem of phase-change material.The experiment proved that being mentioned using the embodiment of the present application
A kind of graphene of graphene enhancing phase transformation material preparation method preparation supplied enhances phase-change material, is higher than phase transition temperature in temperature
Without obvious fluid seepage in 0 DEG C -10 DEG C, illustrate that this method is significantly improved for the thermal conductivity raising of phase-change material, for
The encapsulation of phase-change material also has positive effect.
Detailed description of the invention
Fig. 1 show a kind of process signal of graphene enhancing phase transformation material preparation method of one embodiment of the application offer
Figure.
Fig. 2 show in a kind of graphene enhancing phase transformation material preparation method of one embodiment of the application offer and prepares graphite
The flow diagram of alkene dispersion liquid.
Fig. 3 show in a kind of graphene enhancing phase transformation material preparation method of one embodiment of the application offer and uses amine
The flow diagram of curing agent reduced graphene dispersion liquid.
Fig. 4 is shown phase transformation material in a kind of graphene enhancing phase transformation material preparation method of one embodiment of the application offer
Material is filled into inside graphene aerogel to obtain the flow diagram of graphene enhancing phase-change material.
The process that Fig. 5 show a kind of graphene enhancing phase transformation material preparation method that another embodiment of the application provides is shown
It is intended to.
Fig. 6 show a kind of structural schematic diagram of constant temperature composite construction of one embodiment of the application offer.
Fig. 7 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.
Heat provides layer and is evenly heated layer in a kind of constant temperature composite construction that the embodiment of the application one shown in Fig. 8 provides
Structural schematic diagram.
Fig. 9 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.
Figure 10 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.
Figure 11 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.
Specific embodiment
Many details are explained in the following description in order to fully understand the application.But the application can be with
Much it is different from other way described herein to implement, those skilled in the art can be without prejudice to the application intension the case where
Under do similar popularization, therefore the application is not limited by following public specific implementation.
The term used in this specification one or more embodiment be only merely for for the purpose of describing particular embodiments,
It is not intended to be limiting this specification one or more embodiment.In this specification one or more embodiment and appended claims
The "an" of singular used in book, " described " and "the" are also intended to including most forms, unless context is clearly
Indicate other meanings.It is also understood that term "and/or" used in this specification one or more embodiment refers to and includes
One or more associated any or all of project listed may combine.
It will be appreciated that though may be retouched using term first, second etc. in this specification one or more embodiment
Various information are stated, but these information should not necessarily be limited by these terms.These terms are only used to for same type of information being distinguished from each other
It opens.For example, first can also be referred to as second, class in the case where not departing from this specification one or more scope of embodiments
As, second can also be referred to as first.Depending on context, word as used in this " if " can be construed to
" ... when " or " when ... " or " in response to determination ".
Application is summarized
As described above, the heating conduction of existing phase-change material is low, phase-change material is affected in storage/discharge thermal process
Heat transfer efficiency.In addition, traditional organic phase change material, due to having certain fluidity, there is also closing problems, it is difficult to practical
It is applied to concrete application scene.
For the above technical issues, the basic conception of the application is to propose to make using graphene aerogel as support is played
Basis material, and phase-change material is filled into inside graphene aerogel to play energy storage/exothermic effects, it is consequently formed one
The novel graphene of kind enhances phase-change material.For graphene as a kind of Novel Carbon Nanomaterials, it has unique two dimensional crystal
Structure and high charge migration rate, while graphene also has stable large specific surface area, chemical property, high-termal conductivity and height
The advantages that mechanical strength.Graphene aerogel is that have three by what graphene oxide layer interconnection and recombination constructed out
The new material for tieing up structure, with gap abundant and open cellular structure.Graphene aerogel and phase-change material are combined,
It can use graphene aerogel and adequately adsorb phase-change material, the thermal conductivity of phase-change material is improved using graphene high-termal conductivity
Rate is limited the mobility of phase-change material by the micro-structure duct of graphene, improves the thermal stability of phase-change material, can effectively solve
The certainly closing problem of organic phase change material.
It should be noted that graphene prepared by graphene enhancing phase transformation material preparation method provided herein
Enhancing phase-change material can be applied under any energy storage/heat release scene.For example, under living scene, in order to realize a kind of constant temperature
Mattress, so that it may realize storage using graphene enhancing phase-change material prepared by graphene enhancing phase transformation material preparation method
Energy/heat release, and provide layer as heat still in a manner of carbon fiber exothermic wire and provide heat source for graphene enhancing phase-change material.
Concrete application field of the application to graphene enhancing phase-change material prepared by graphene enhancing phase transformation material preparation method
Scape is without limitation.
After describing the basic principle of the application, carry out the various non-limits for specifically introducing the application below with reference to the accompanying drawings
Property embodiment processed.
Exemplary embodiment
The process that Fig. 1 show a kind of preparation method of graphene enhancing phase-change material of one embodiment of the application offer is shown
It is intended to.As shown in Figure 1, the preparation method of graphene enhancing phase-change material includes the following steps:
Step 101: preparing graphene dispersing solution, wherein graphene dispersing solution concentration is 1mg/mL-20mg/mL.In this Shen
In an embodiment, please be used to prepare graphene enhancing phase-change material graphene dispersing solution concentration can for 2mg/mL, 4mg/mL,
6mg/mL, 8mg/mL, 10mg/mL, 12mg/mL, 14mg/mL, 16mg/mL or 18mg/mL.
In one embodiment of the application, as shown in Fig. 2, the process for preparing graphene dispersing solution may include following steps:
Step 1011: raw graphite being added in mix acid liquor to form the first mixed liquor, stirring is greater than 30 minutes.
Raw graphite may be selected one of following material or a variety of: expanded graphite, crystalline flake graphite, Pintsch process graphite,
Graphene powder and carbon nanotube.Mix acid liquor can be the mixed liquor of the concentrated sulfuric acid and concentrated phosphoric acid, the ratio of the concentrated sulfuric acid and concentrated phosphoric acid
For 5-20:1 (for example, can be 8:1,10:1,12:1,14:1,15:1,16:1 or 18:1)；Wherein, the weight of mix acid liquor with
The ratio of the weight of raw graphite is 10-500:1 (may be, for example, 50:1,100:1,200:1,300:1 or 400:1).However it answers
Work as understanding, the originally specific choice of graphite and mix acid liquor can need condition for peace according to actual scene and adjust, the application couple
This does not do considered critical.
Step 1012: KMnO is added in the first mixed liquor4, stirring was greater than 30 minutes, wherein KMnO4Weight and raw material
The ratio of graphite weight is 2-5:1 (may be, for example, 3:1,3.5:1 or 4:1).
Step 1013: KMnO will be had4The first mixed liquor be warming up to 40 DEG C -60 DEG C, stirring is greater than 12 hours.By prolonging
Grow the degree of oxidation that graphite synusia can be improved 40 DEG C -60 DEG C of reaction time.
Step 1014: after the first mixed liquor is cooled to room temperature, the first mixed liquor being imported into ice water, and hydrogen peroxide is added dropwise.
The volume of ice water can be 3-5 times of the first mixeding liquid volume, the volume and ice water volume ratio of hydrogen peroxide for 1:150-200 (such as
It can be 1:160,1:170,1:180 or 1:190).
Step 102: using amine curing agent reduced graphene dispersion liquid to obtain graphene hydrogel, wherein amine-type cure
The concentration of agent be 0.1mmol-0.5mmol (may be, for example, 0.175mmol, 0.25mmol, 0.325mmol, 0.4mmol or
0.475mmol)。
In one embodiment of the application, as shown in figure 3, can be wrapped using the process of amine curing agent reduced graphene dispersion liquid
Include following steps:
Step 1021: graphene dispersing solution being mixed with anhydrous ethylenediamine to carry out reduction reaction, and passes through ultrasonic procedure
Carry out Homogenization Treatments, wherein the temperature range of reduction reaction is 120 DEG C -160 DEG C, and time of reduction reaction is 3 hours -6 small
When.
Step 1022: the gel Jing Guo reduction reaction being placed in subzero 18 DEG C and is once refrigerated to solid-state.
Step 1023: solid gel is thawed to obtain graphene hydrogel.
Step 103: solvent replacement process and constant pressure and dry process are carried out to obtain graphene airsetting to graphene hydrogel
Glue.
Specifically, solvent replacement process can include: graphene hydrogel is rinsed in deionized water, and with ethyl alcohol and
The mixed solution of deionized water carries out dialysis -6 hours 3 hours, wherein ethyl alcohol and the volume ratio of deionized water are 1:50-150
(may be, for example, 1:75,1:100 or 1:125).Constant pressure and dry process can include: by the graphene water-setting Jing Guo volume replacement process
Glue is dried in 60 DEG C or more of environment.
Step 104: organic phase change material is filled into inside graphene aerogel to obtain graphene enhancing phase-change material,
Wherein, the mass ratio of phase-change material and graphene aerogel be 10-30:1 (may be, for example, 12:1,14:1,16:1,18:1,20:
1,22:1,24:1,26:1 or 28:1).
In one embodiment of the application, as shown in figure 4, organic phase change material is filled into inside graphene aerogel to obtain
Detailed process to graphene enhancing phase-change material may include following steps:
Step 1041: graphene aerogel being mixed with organic phase change material and has obtained the second mixed liquor.
In one embodiment of the application, organic phase change material includes one of following different materials or multiple combinations: stone
Wax, decyl alcohol, tetradecyl alchohol and hexadecanol.It should be appreciated, however, that the specific choice of organic phase change material can be according to actual scene need
Condition for peace and adjust, the application does not do considered critical to this.
Step 1042: the second mixed liquor being placed in vacuum environment and is heated, wherein the vacuum degree of vacuum environment is greater than 20kpa
(may be, for example, 30kpa), the temperature of heating process are higher than 3 DEG C -5 DEG C of organic phase change material fusing point, and the time of heating process is 12
- 24 hours hours.
One embodiment of the application also provides a kind of graphene enhancing phase-change material, using the stone as described in preceding any embodiment
Black alkene enhancing phase transformation material preparation method is prepared.
A kind of graphene enhancing phase transformation material preparation method and graphene provided by the embodiments of the present application enhance phase-change material,
It is to play the basis material played a supporting role to phase-change material, and phase-change material is filled into graphene with graphene aerogel
To play energy storage/exothermic effects inside aeroge, the overall mechanical properties of material are not only increased, the experiment proved that, it can also phase
Than the thermal conductivity that simple phase-change material improves 10%-35%.Meanwhile using graphene airsetting prepared by the embodiment of the present application
Glue also effectively limits the mobility of phase-change material as basis material using internal micro-structure duct, is not only does this facilitate and mentions
The thermal stability of high phase-change material also solves the closing problem of phase-change material.The experiment proved that being mentioned using the embodiment of the present application
A kind of graphene of graphene enhancing phase transformation material preparation method preparation supplied enhances phase-change material, is higher than phase transition temperature in temperature
Without obvious fluid seepage in 0 DEG C -10 DEG C, illustrate that this method is significantly improved for the thermal conductivity raising of phase-change material, for
The encapsulation of phase-change material also has positive effect.
Fig. 5 show a kind of process of the preparation method for graphene enhancing phase-change material that another embodiment of the application provides
Schematic diagram.
Step 501: it weighs raw material crystalline flake graphite and is added in the concentrated sulfuric acid and the mixed liquor of concentrated phosphoric acid (volume ratio 10:1),
Magnetic agitation 30min, the weight and raw graphite weight ratio of mix acid liquor are 100 times, and the ratio of the concentrated sulfuric acid and concentrated phosphoric acid is
15:1.
Step 502: being slowly added to KMnO4, (KMnO4Weight ratio be 3 times of raw material crystalline flake graphite weight), continue to stir
30min。
Step 503: being warming up to 40 DEG C -60 DEG C, stir 12 hours.
Step 504: after being cooled to room temperature, above-mentioned mixed liquor importeding into ice water to (ice water volume is the 3 of mixeding liquid volume
Times), and a certain amount of hydrogen peroxide (dioxygen water volume is the 1/150 of ice water volume) is added dropwise, wherein ice water volume is mixeding liquid volume
3-5 times.The preparation of graphene aerogel dispersion liquid, concentration 10mg/ml are completed since then.
Step 505: graphene dispersing solution and 0.25mmol anhydrous ethylenediamine that concentration is 10mg/mL are mixed, and
Channel ultrasound obtains homogeneous system, restores 3-6 hours under 120 DEG C of -150 DEG C of degree.
Step 506: the gel that step 505 is obtained is placed in 18 degrees below zero following temperature environment and is refrigerated to complete solid,
It thaws after taking-up.
Step 507: with deionized water repeated flushing, and with ethyl alcohol and the mixed solution of deionized water carry out dialysis 3-6 it is small
When, the ratio of ethyl alcohol and deionized water is 1:100, and is completely dried in 60 DEG C of environment above.So far graphene airsetting is obtained
Glue, pore-size distribution is between 40um-120um.
Step 508: selection hexadecanol is organic phase change material, by graphene aerogel obtained in above-mentioned steps and 16
The mass ratio of alcohol mixing, hexadecanol and graphene aerogel is 12:1；Above-mentioned mixed liquor is placed in vacuum tank, vacuum degree is
30kpa, temperature setting are 50 DEG C；After 12-24 hours, extra organic phase change material is removed to get graphene reinforced phase is arrived
Become material.
It is characterized, is measured by the thermal conductivity that thermal conductivity instrument enhances phase-change material to the graphene that above-mentioned steps are prepared
Thermal conductivity is 0.33W/ (M.K), and the thermal conductivity of hexadecanol is 0.25W/ (M.K) in contrast, it can be seen that passes through the application reality
The thermal conductivity for applying the enhancing phase-change material of graphene provided by example improves 32%.Graphene enhances phase-change material for phase transformation material
The closed performance of material is tested by the way that composite material is placed on placement 30min on 50 DEG C of temperature platforms, and test result is shown,
Material surface does not obviously leak, and illustrates that the enhancing phase-change material of graphene provided by the embodiment of the present application has phase-change material
Good closure.
In one embodiment of the application, graphene enhancing prepared by above-mentioned graphene enhancing phase transformation material preparation method
Phase-change material can be used as the whole or part of phase change composite material layer 100, be used in a kind of constant temperature composite construction.
Specifically, Fig. 6 show a kind of structural schematic diagram of constant temperature composite construction of one embodiment of the application offer.Such as
Shown in Fig. 6, which includes: phase change composite material layer 100, heat offer layer 200 and heat reflecting layer 300.
Specifically, phase change composite material layer 100 is configured to undergo phase transition from the heat offer absorption heat of layer 200 to store heat, and
Heat is discharged by reverse transformation process to maintain constant temperature.Heat provides layer 200 and is arranged in 100 side of phase change composite material layer, structure
It makes to provide heat to phase change composite material layer 100.The setting of heat reflecting layer 300 is compound far from phase transformation in heat offer layer 200
The side of material layer 100 is configured to reflection heat and provides the heat that layer 200 and heat offer layer 200 discharge.
Phase change composite material layer 100 may include backing material and the phase-change material that is filled in backing material.Phase-change material
It undergoes phase transition with heat is absorbed to store heat, and heat is discharged to maintain constant temperature by reverse transformation process.Due to phase transformation
Phase-change material may become liquid in the process, and backing material can wrap the phase-change material of liquid without arbitrarily flowing, together
When keep solid appearance presentation, to meet the appearance or mechanical property requirements of concrete application scene.It should be appreciated that phase transformation is compound
The specific material selection of material layer 100 and internal structure can be adjusted according to specific application scenarios demand, for example, phase transformation is compound
The material of material layer 100 may include one of following several phase change composite materials or a variety of combinations: with graphene aerogel
For backing material, using organic phase change material as the phase change composite material of packing material；Using foam metal as backing material, with organic
Phase-change material is the phase change composite material of packing material；And using high molecular polymer as backing material, with organic phase change material
For the phase change composite material of packing material.The application does not do stringent limit to the specific material and internal structure of phase change composite material
It is fixed.
In one embodiment of the application, when the product that the constant temperature composite construction is applicable in is needed with human contact, it can lead to
It crosses and adjusts the material and internal structure of phase change composite material layer 100 in the constant temperature composite construction to meet and want with human contact
It asks.Such as the product that the living scenes such as personal clothing or mattress are used, by adjusting the material of phase change composite material layer 100
With internal structure so that the phase transition temperature of phase change composite material layer 100 is 25 DEG C to 45 DEG C, constant temperature time is maintained to be less than or equal to 8
Hour.Specifically, 31 DEG C, 33 can be adjusted to the phase transition temperature of phase change composite material layer 100 according to actual application scenarios
DEG C, 35 DEG C, 37 DEG C or 39 DEG C, by maintain constant temperature time be adjusted to 2 hours, 4 hours or 6 hours.
It is also understood that the specific implementation that heat provides layer 200 can also specifically answering according to the constant temperature composite construction
It is adjusted with the wanting condition for peace of scene.In one embodiment of the application, heat, which provides layer 200, can be used carbon fiber exothermic wire friendship
The network being made into.Carbon fiber exothermic wire use Far-infrared radiation heating, have heating safety, electric heating high conversion rate it is excellent
Point；Meanwhile the constant temperature can also be met using the network being woven into and meet structure for gas permeability and anti-fracture equal mechanical property
The requirement of energy.In the other embodiments of the application, in order to meet better mechanical property requirements, heat provides layer 200 can also
Using other heating methods, for example, by using metal material calandria.The application provides heat and specifically heats used by layer 200
Mode does not also do considered critical.
It is also understood that the specific implementation in heat reflecting layer 300 can also specifically answering according to the constant temperature composite construction
It is adjusted with the material for wanting condition for peace and heat offer layer 200 and phase change composite material layer 100 of scene.In the application
In one embodiment, heat reflecting layer 300 may include infrared reflecting layer.For example, metallic aluminium can be used in the material of the infrared reflecting layer
One of film, metal zirconium film, metal titanium membrane, metal silverskin, stainless steel membrane or a variety of combinations.The application reflects the heat
The specific material of layer 300 does not do considered critical equally.
Fig. 7 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.Compared to Fig. 6
Shown in constant temperature composite construction, constant temperature composite construction shown in Fig. 7 can further comprise: being evenly heated layer 400, be arranged in heat
It provides between layer 200 and phase change composite material layer 100, passes to being configured to provide heat the even heat that layer 200 generates
Phase change composite material layer 100 provides the absorption effect of heat to improve phase change composite material layer 100 and provide layer 200 for heat
Rate.
It should be appreciated that the heating method that the material for being evenly heated layer 400 can provide layer 200 according to heat adjusts, as long as energy
It plays and provides heat to the even heat that layer 200 generates and pass to phase change composite material layer 100.For example, when heat provides
When layer 200 is heated using carbon fiber exothermic part 201, being evenly heated layer 400 can also be used carbon fiber realization, to play uniformly
Heat transfer and the effect for blocking radiation.The application to the specific material and internal structure for being evenly heated layer 400 without limitation.
In one embodiment of the application, as shown in figure 8, heat provides multiple heaters that layer 200 may include array arrangement
201, it is evenly heated multiple heat carriers 401 that layer 400 includes array arrangement.Multiple heat carriers 401 are arranged in multiple heaters 201
Gap above.It is not the layer of whole face tiling, multiple array arrangements since heat provides layer 200 and is evenly heated layer 400 all
Multiple heaters 201 between have gap, and also have gap between multiple heat carriers 401, to can help to ensure that constant temperature is multiple
The gas permeability of structure is closed, to meet the needs of some living scene products (such as personal clothing or bedding).But due to more
There are gap between a heater 201, the heat transfer efficiency of the position in gap may be cannot be guaranteed, therefore by multiple heat carriers
401 are arranged in above the gap of multiple heaters 201, can effectively improve the heat transfer efficiency between heater 201 at interstitial site.
It can be seen that providing layer 200 by heat shown in Fig. 8 and being evenly heated the overlaying structure of layer 400, it can be achieved that gas permeability and biography
Hot balance improves user experience to improve the constant temperature composite construction for the applicability of living scene product.
Fig. 9 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.Compared to Fig. 7
Shown in constant temperature composite construction, constant temperature composite construction shown in Fig. 9 can further comprise: insulating 500, be arranged in heat
Reflecting layer 300 provides the side of layer 200 far from heat, is configured to trap heat and scatters and disappears.
It should be appreciated that the specific material and internal structure of insulating 500 can also be according to the tools of the constant temperature composite construction
Body application scenarios want condition for peace and heat to provide the material of layer 200 and phase change composite material layer 100 and adjust.At this
Apply in an embodiment, one of following heat preservation material or multiple combinations: boron nitride can be used in the material of insulating 500
Fibrofelt, Zirconium oxide fibre felt, polycrystalline mullite fibre felt, alumina fiber blanket, carbon fiber felt.In a preferred embodiment
In, it is contemplated that the application scenarios of the constant temperature composite construction may need and human contact, in order to avoid the constant temperature composite construction institute
Applicable product generates high temperature spontaneous combustion because of failure, which can be used aerogel heat-insulating felt.Aerogel heat-insulating felt
Not only there is excellent heat-proof quality, can effectively avoid heat loss, be also high resistant combustible material, it is compound that the constant temperature can be effectively improved
The flame-retarding performance of structure.
In one embodiment of the application, insulating 500 may include with one of lower thermal insulating layer or multiple combinations: gas
Gel felt insulation, with a thickness of 2mm-20mm；Polyurethane foam pad, with a thickness of 10mm-50mm；Polystyrene foam pad, with a thickness of
10mm-50mm；And asbestos pad, with a thickness of 10mm-50mm；And felt, with a thickness of 10mm-50mm.
Figure 10 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.Compared to figure
Constant temperature composite construction shown in 9, constant temperature composite construction shown in Fig. 10 can further comprise: the top surface of cladding constant temperature composite construction
With the worsted fabric layer 700 of bottom surface.Constant temperature composite construction and human contact's sense of touch can be improved in worsted fabric layer 700, guarantees simultaneously
Gas permeability, encapsulation and certain mechanical property requirements.It should be understood that the material and internal structure of worsted fabric layer 700 can also roots
It adjusting according to specific application scenarios, worsted fabric layer 700 can be used the super suede of crystal and realize in one embodiment of the application, however
The application to the specific material and internal structure of worsted fabric layer 700 without limitation.
Figure 11 show a kind of structural schematic diagram for constant temperature composite construction that another embodiment of the application provides.Compared to figure
Constant temperature composite construction shown in 9, in order to further increase the homogeneity of heat transfer, constant temperature composite construction shown in Figure 11 can be into
One step includes: the thermally conductive fixing layer 600 being arranged between phase change composite material layer 100 and worsted fabric layer 700.In the application one
In embodiment, which can be one of following material or multiple combinations: carbon fiber felt, glass mat and
Alumina silicate fiber felt.
In one embodiment of the application, in order to meet the specific requirements of concrete application scene, phase change composite material layer 100 can
Multi-layer phase change layer including superposition, wherein the multi-layer phase change layer uses a variety of combinations in following phase change composite material with reality
It is promoted in existing comprehensive performance: compound as the phase transformation of packing material using organic phase change material using graphene aerogel as backing material
Material；Using foam metal as backing material, using organic phase change material as the phase change composite material of packing material；With high molecular polymerization
Object is backing material, using organic phase change material as the phase change composite material of packing material；And using polymer plastic material bag as container,
The phase change composite material of inside filling phase-change material, wherein the phase-change material includes solid-liquid phase change material or solid-solid phase change material
Material.
In one embodiment of the application, solid-liquid phase change material above-mentioned can be by solid paraffin, atoleine and heat filling
Composition.The fusing point of solid paraffin is within the scope of 48 DEG C -65 DEG C, and atoleine fusing point is in 3 DEG C -8 DEG C, solid paraffin and liquid stone
The mass ratio of wax is 100:5-30, and heat filling can be graphene, expanded graphite, fibrous carbon dust, flakey carbon dust, nano oxygen
Change aluminium or silicon carbide etc..The quality of heat filling and the mass ratio of gross mass are 1-15:100.The preparation of the solid-liquid phase change material
Method can are as follows: various raw materials are added to heating container according to mass ratio, are heated to 70 DEG C, until after solid paraffin all melts
It is mixed, the preparation of the solid-liquid phase change material can be completed after mixing evenly.
Solid-solid phase change material can be by polyethylene or polypropylene and above-mentioned solid-liquid phase change material.Polyethylene or polypropylene with
The mass ratio of solid-liquid phase change material is 20-50:100, and heat filling can be graphene, expanded graphite, fibrous carbon dust, flakey
Carbon dust, nano aluminium oxide or silicon carbide etc., the quality of heat filling and the mass ratio of gross mass are 1-15:100.The solid-solid phase change
The preparation method of material can are as follows: various raw materials are added to heating container according to mass ratio, are heated to selected polyethylene or poly- third
Alkene fusing point can be added to fixing mould molding until solid-state material is mixed after all melting after mixing evenly, i.e., complete
At the preparation of the solid-solid phase change material of fixed shape, above-mentioned process transfer to double screw extruder can also be completed.
In another embodiment of the application, in order to meet the specific requirements of concrete application scene, phase change composite material layer 100
Can include: the first phase change region and second phase change region adjacent with the first phase change region；Wherein the first phase change region is used
Phase change composite material thermal conductivity coefficient lower than phase change composite material used by the second phase change region thermal conductivity coefficient.Such
The heat transfer efficiency of one phase change region can be lower than the second phase change region, to meet the diversified demand of concrete application scene.For example, working as
When the phase change composite material layer 100 is suitable for a kind of bedding, it is contemplated that the temperature in human limb region is usually to be lower than
Chest, abdomen and head, therefore can be true by the region corresponding with human chest, abdomen and head of phase change composite material layer 100
It is set to the first phase change region, and handle region corresponding with four limbs is determined as the second phase change region, since the first phase change region is adopted
The thermal conductivity coefficient of phase change composite material is lower than the thermal conductivity coefficient of phase change composite material used by the second phase change region, in this way
Aloowing user, whole body maintains uniform temperature when in use, avoids the occurrence of the cool situation of the cool foot of hand, further increases
The user experience of product.
One embodiment of the application also provides a kind of constant temperature mattress, using the constant temperature composite junction as described in preceding any embodiment
Structure.Constant temperature mattress provided by the embodiments of the present application, the storage and release for realizing heat by phase change composite material layer 100 are to maintain
Constant temperature avoids the problem of existing thermostat needs to rely on the uninterrupted heat supply of electric energy and leads to security risk.Simultaneously as adopting
The stepped construction of layer 200 and heat reflecting layer 300 is provided with phase change composite material layer 100, heat, it is simple for structure and do not need
The radiators such as liquid circulation, easy to produce and use.In addition, by setting heat reflecting layer 300, it can be by phase change composite material
Layer 100 and heat provide the side that the heat that layer 200 generates reflexes to constant temperature composite construction, multiple so as to effectively improve the constant temperature
Close the heating efficiency of structure.
The above description of disclosed aspect is provided so that any person skilled in the art can make or use this
Application.Various modifications in terms of these are readily apparent to those skilled in the art, and are defined herein
General Principle can be applied to other aspect without departing from scope of the present application.Therefore, the application is not intended to be limited to
Aspect shown in this, but according to principle disclosed herein and the consistent widest range of novel feature.
In order to which purpose of illustration and description has been presented for above description.In addition, this description is not intended to the reality of the application
It applies example and is restricted to form disclosed herein.Although already discussed above multiple exemplary aspects and embodiment, this field skill
Its certain modifications, modification, change, addition and sub-portfolio will be recognized in art personnel.
The foregoing is merely the preferred embodiments of the application, not to limit the application, all essences in the application
Within mind and principle, made any modification, equivalent replacement etc. be should be included within the scope of protection of this application.
Claims (10)
1. a kind of preparation method of graphene enhancing phase-change material characterized by comprising
Prepare graphene dispersing solution, wherein the graphene dispersing solution concentration is 1mg/mL-20mg/mL；
The graphene dispersing solution is restored using amine curing agent to obtain graphene hydrogel, wherein the amine curing agent
Concentration is 0.1mmol-0.5mmol；
Solvent replacement process and constant pressure and dry process are carried out to obtain graphene aerogel to the graphene hydrogel；And
Organic phase change material is filled into inside the graphene aerogel to obtain the graphene enhancing phase-change material,
In, the mass ratio of the phase-change material and the graphene aerogel is 10-30:1.
2. the method according to claim 1, wherein the graphene aerogel dispersion liquid for preparing includes:
Raw graphite is added in mix acid liquor to form the first mixed liquor, stirring is greater than 30 minutes；
KMnO is added in first mixed liquor4, stirring was greater than 30 minutes, wherein the KMnO4Weight and the raw material
The ratio of graphite weight is 2-5:1；
The KMnO will be had4First mixed liquor be warming up to 40 DEG C -60 DEG C, stirring is greater than 12 hours；
After first mixed liquor is cooled to room temperature, first mixed liquor is imported into ice water, and hydrogen peroxide is added dropwise.
3. according to the method described in claim 2, it is characterized in that, the raw graphite selects one of following material or more
Kind: expanded graphite, crystalline flake graphite, Pintsch process graphite, graphene powder and carbon nanotube.
4. according to the method described in claim 2, it is characterized in that, the mix acid liquor is the mixing of the concentrated sulfuric acid and concentrated phosphoric acid
The ratio of liquid, the concentrated sulfuric acid and concentrated phosphoric acid is 5-20:1；Wherein, the weight of the mix acid liquor and the raw graphite
The ratio of weight is 10-500:1.
5. according to the method described in claim 2, it is characterized in that, the volume of the ice water is first mixeding liquid volume
3-5 times, the volume of the hydrogen peroxide and the ice water volume ratio are 1:150-200.
6. the method according to claim 1, wherein described restore the graphene dispersion using amine curing agent
Liquid includes:
The graphene dispersing solution is mixed with the anhydrous ethylenediamine to carry out the reduction reaction, and by ultrasonic procedure into
Row Homogenization Treatments, wherein the temperature range of the reduction reaction is 120 DEG C -160 DEG C, and the time of the reduction reaction is 3 small
When -6 hours；
Gel Jing Guo the reduction reaction is placed in subzero 18 DEG C and is once refrigerated to solid-state；And
The solid gel is thawed to obtain the graphene hydrogel.
7. the method according to claim 1, wherein the solvent replacement process includes:
The graphene hydrogel is rinsed in deionized water, and dialysis 3 is carried out with ethyl alcohol and the mixed solution of deionized water
Hours -6 hours, wherein ethyl alcohol and the volume ratio of deionized water are 1:50-150.
8. the method according to claim 1, wherein the constant pressure and dry process includes:
The graphene hydrogel Jing Guo the volume replacement process is dried in 60 DEG C or more of environment.
9. the method according to claim 1, wherein described be filled into the graphene gas for organic phase change material
Include: to obtain the graphene enhancing phase-change material inside gel
The graphene aerogel is mixed with organic phase change material and has obtained the second mixed liquor；
Second mixed liquor is placed in vacuum environment and is heated, wherein the vacuum degree of the vacuum environment is greater than 20kpa, it is described
The temperature of heating process is higher than 3 DEG C -5 DEG C of the organic phase change material fusing point, and time of the heating process is 12 hours -24 small
When.
10. a kind of graphene enhances phase-change material, which is characterized in that using the method system as described in any in claim 1 to 9
It is standby to form.
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Application publication date: 20191115 |