CN106947434A - A kind of hydrated salt modified expanded graphite composite phase-change material and preparation method thereof - Google Patents
A kind of hydrated salt modified expanded graphite composite phase-change material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of hydrated salt modified expanded graphite composite phase-change material and preparation method thereof, including block shape hydrophilic modifying expanded graphite and absorption the hydrated salt in the block shape hydrophilic modifying expanded graphite；The density of the block shape hydrophilic modifying graphite is 300~600kg/m3.The composite phase-change material that the present invention is provided significantly improves adsorbance of the expanded graphite to hydrated salt, so as to improve the energy storage density of composite phase-change material using the expanded graphite absorption hydrated salt of hydrophilic modifying；And hydrated salt is adsorbed using the modified expanded graphite of block shape, the energy storage density of unit volume composite phase-change material is further increased.Experiment shows that the mass fraction of hydrated salt can reach 85% in the composite phase-change material that the present invention is provided, and energy storage density can reach 300MJ/m3, thermal conductivity factor can reach 9.86 (Wm‑1·K‑1)。
Description
Technical field
The present invention relates to the technical field of phase-change material, more particularly to a kind of hydrated salt-modified expanded graphite composite phase-change
Material and preparation method thereof.
Background technology
Phase-change material can absorb or discharge substantial amounts of heat in phase transition process with keeping body system temperature in the process
Phase transition temperature or so is substantially constant at, so that the purpose to temperature effectively control and the hidden heat energy storage of surrounding is reached, according to material
Phase-change material can be divided into inorganic and organic phase-change material by material composition.It is small to there is thermal conductivity factor in simple phase-change material,
Solid liquid phase, which becomes different, occurs the shortcomings of liquid leaks, and composite phase-change heat-storage material can not only overcome the defect of single phase-change heat-storage material, and
And the application effect of phase-change material can be improved and its application is expanded.
Expanded graphite is the loose porous vermiform material being made up of graphite microcrystal, and it is good except crystalline flake graphite is remained
Thermal conductivity outside, also with good adsorptivity, phase-change thermal storage material is adsorbed in the cavernous structure of expanded graphite constitute it is multiple
It is current most common method to close phase-change material.
Inorganic phase-changing material can be divided into hydrated salt, simple metal and alloy etc. according to material composition, and wherein hydrated salt has storage
Can density it is big, thermal conductivity is high, it is cheap, widely distributed the advantages of, but with expanded graphite carry out compound tense, expanded graphite
Adsorptivity to inorganic phase-changing material is poor, causes the energy storage density of composite phase-change material and can not further improve, limits water
Close the application of salt phase-change material.
The content of the invention
In view of this, present invention aims at provide hydrated salt-modification that a kind of hydrated salt adsorbance is high, energy storage density is big
Expanded graphite composite phase-changing material and preparation method thereof.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of hydrated salt-modified expanded graphite composite phase-change material, including block shape hydrophilic modifying are swollen
The hydrated salt of swollen graphite and absorption in the block shape hydrophilic modifying expanded graphite；The block shape hydrophilic modifying graphite it is close
Spend for 300~600kg/m3。
It is preferred that, in the composite phase-change material mass ratio of block shape hydrophilic modifying expanded graphite and hydrated salt be 15~
30:70~85.
It is preferred that, the hydrated salt is in calcium chloride hexahydrate, magnesium chloride hexahydrate, magnesium nitrate hexahydrate and ten sulfate dihydrate aluminium ammonium
One or more of mixtures.
The invention provides a kind of preparation side of hydrated salt described in such scheme-modified expanded graphite composite phase-change material
Method, comprises the following steps：
Hydrophilic modifying expanded graphite is suppressed, block shape hydrophilic modifying expanded graphite is obtained；
The block shape hydrophilic modifying expanded graphite and molten state hydrated salt are subjected to mixing and absorption, hydrated salt-change is obtained
Property expanded graphite composite phase-changing material.
It is preferred that, the temperature of the compacting is 10~40 DEG C；The pressure of the compacting is 5~30MPa.
It is preferred that, the time of the mixing and absorption is 1~5h.
It is preferred that, the preparation method of the hydrophilic modifying expanded graphite comprises the following steps：
Ultrasound after wetting agent and expanded graphite, polar solvent are mixed, obtains hydrophilic modifying expanded graphite.
It is preferred that, the wetting agent is Triton X-100, lauryl sodium sulfate, neopelex
With one or more of mixtures in cetyl ammonium bromide.
It is preferred that, the mass ratio of the wetting agent and expanded graphite is 5~30:70~95.
It is preferred that, the ultrasonic time is 3~20min.
The invention provides a kind of hydrated salt-modified expanded graphite composite phase-change material, including block shape hydrophilic modifying are swollen
The hydrated salt of swollen graphite and absorption in block shape hydrophilic modifying expanded graphite；The density of the block shape hydrophilic modifying graphite is
300~600kg/m3.The composite phase-change material that the present invention is provided significantly is carried using the expanded graphite absorption hydrated salt of hydrophilic modifying
High adsorbance of the expanded graphite to hydrated salt, so as to improve the energy storage density of composite phase-change material；And utilize block shape
Modified expanded graphite absorption hydrated salt, further increase the composite phase-change material energy storage density of unit volume.Furthermore, it is hydrophilic
Modified expanded graphite thermal conductivity factor is high, for thermal conductivity factor of the thermal conductivity factor compared to single-phase hydrated salt of composite phase-change material
It is significantly increased.Embodiment shows that the mass fraction of hydrated salt can reach 85% in the composite phase-change material that the present invention is provided,
Energy storage density can reach 300MJ/m3, thermal conductivity factor is 7~15 times of single-phase hydrated salt thermal conductivity factor.
The invention provides a kind of preparation side of hydrated salt described in such scheme-modified expanded graphite composite phase-change material
Method, the preparation method is simple, and step is few, and energy consumption is low, environmentally friendly, easily carries out industrialized production.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention 1 in before modified after Porous Structure of Expanded Graphite electron scanning micrograph；
Fig. 2 be the embodiment of the present invention 1 in before modified after expanded graphite infrared spectrogram；
Fig. 3 be the embodiment of the present invention 1 in before modified after expanded graphite water contact angle figure；
Fig. 4 be in the embodiment of the present invention 1 before modified after expanded graphite to the absorption property figure of hydrated salt；
Fig. 5 is that the SEM of hydrated salt-modified expanded graphite composite phase-change material in the embodiment of the present invention 1 is shone
Piece.
Embodiment
The invention provides a kind of hydrated salt-modified expanded graphite composite phase-change material, including block shape hydrophilic modifying are swollen
The hydrated salt of swollen graphite and absorption in block shape hydrophilic modifying expanded graphite；The density of the block shape hydrophilic modifying graphite is
300~600kg/m3。
The hydrated salt that the present invention is provided-modified expanded graphite composite phase-change material includes modified expanded graphite.In the present invention
In, the modified expanded graphite is the expanded graphite of hydrophilic modifying.In the present invention, the expanded graphite hydrophily of hydrophilic modifying
Good, the abundant hydrophilic functional group of area load, Adsorption is more, and the expanded graphite by the use of hydrophilic modifying is used as composite phase-change
The matrix of material, significantly improves the adsorbance to hydrous salt phase change material, so as to improve the energy storage density of composite phase-change material.
In the present invention, the hydrophilic modifying expanded graphite is block shape hydrophilic modifying expanded graphite；The block shape parent
The density of water modified expanded graphite is 300~600kg/m3, preferably 350~550kg/m3, more preferably 400~500kg/m3；
The present invention does not have particular/special requirement to the specific size of block shape expanded graphite, in a particular embodiment of the present invention, can basis
The phase-change material size needed sets specific size.The present invention is raw material using the hydrophilic modifying expanded graphite of block shape, is entered
One step improves the composite phase-change material energy storage density of unit volume.
In the present invention, the preparation method of the hydrophilic modifying expanded graphite preferably includes following steps：
Ultrasound after wetting agent and expanded graphite, polar solvent are mixed, obtains hydrophilic modifying expanded graphite.
In the present invention, the wetting agent is preferably Triton X-100, lauryl sodium sulfate, dodecyl
One or more of mixtures in benzene sulfonic acid sodium salt and cetyl ammonium bromide；The mixture of the wetting agent is preferably 2~3 kinds
The mixture of the mixture of wetting agent, more preferably Triton X-100 and lauryl sodium sulfate, dodecyl sulphur
The mixture or Triton X-100, neopelex and cetyl of sour sodium and neopelex
The mixture of ammonium bromide；Polyethylene glycol octyl group benzene in the Triton X-100 and the mixture of lauryl sodium sulfate
Base ether and the mass ratio of lauryl sodium sulfate are preferably 1:1~2, more preferably 1:1.3~1.8；The dodecyl sulphate
The mass ratio of lauryl sodium sulfate and neopelex is preferably in the mixture of sodium and neopelex
1:1~2, more preferably 1:1.3~1.8；The Triton X-100, neopelex and hexadecane bromide
The mass ratio for changing Triton X-100, neopelex and cetyl ammonium bromide in the mixture of ammonium is preferred
For 1~3:1~2:1, more preferably 1.5~2.5:1.3~1.8:1.
In the present invention, the polar solvent is preferably one or more of mixtures in water, absolute ethyl alcohol and ether.
In the present invention, the specific surface area of the expanded graphite is preferably 50~200m2/ g, more preferably 100~180m2/
g；The bulk density of the expanded graphite is preferably 0.002~0.005g/cm3, more preferably 0.003~0.004g/cm3.This hair
The no particular/special requirement in the bright source to expanded graphite, the commodity bought using in the market or voluntarily prepared using crystalline flake graphite
Can.
The present invention does not have particular/special requirement to the charging sequence of wetting agent, expanded graphite and polar solvent in mixing, uses this
Charging sequence known to art personnel.In a particular embodiment of the present invention, can be first by wetting agent and polarity
Solvent is mixed, and obtains wetting agent solution, then expanded graphite is added in wetting agent solution.
In the present invention, the mass ratio of the wetting agent and expanded graphite is preferably 5~30:70~95, more preferably 10
~25:75~90, most preferably 15~20:80~85；The mass ratio of the wetting agent and polar solvent is preferably 5~30:500
~1000, more preferably 10~20:600~900, most preferably 15~18:700~800.
In the present invention, the ultrasonic time is preferably 3~20min, more preferably 5~15min, most preferably 8~
12min；The ultrasonic power is preferably 300~500W, more preferably 350~450W, most preferably 380~420W.
After the ultrasound, the present invention preferably dries the expanded graphite after ultrasound.In the present invention, the temperature of the drying
Preferably 80~150 DEG C, most preferably more preferably 90~130 DEG C, 100~120 DEG C；The time of the drying is preferably 12~
24h, more preferably 15~20h, most preferably 17~18h.
Dried expanded graphite is preferably naturally cooled to room temperature by the present invention, obtains hydrophilic modifying expanded graphite.
The composite phase-change material that the present invention is provided includes hydration of the absorption in the block shape hydrophilic modifying expanded graphite
Salt.In the present invention, the hydrated salt absorption is in the hole and layer structure of expanded graphite；The hydrated salt is preferably six water
One or more of mixtures in calcium chloride, magnesium chloride hexahydrate, magnesium nitrate hexahydrate and ten sulfate dihydrate aluminium ammoniums；The hydrated salt
Mixture be preferably 2~3 kinds of hydrated salts mixture, more preferably ten sulfate dihydrate aluminium ammoniums and magnesium chloride hexahydrate mixing
The mixture or magnesium chloride hexahydrate and the mixture of magnesium nitrate hexahydrate of thing, calcium chloride hexahydrate and magnesium chloride hexahydrate；12 water
The mass ratio of magnesium chloride hexahydrate and ten sulfate dihydrate aluminium ammoniums is preferably 1 in the mixture of alum and magnesium chloride hexahydrate:1~3,
More preferably 1:1.5~2.5；Calcium chloride hexahydrate and magnesium chloride hexahydrate in the mixture of the calcium chloride hexahydrate and magnesium chloride hexahydrate
Mass ratio be preferably 1:1~3, more preferably 1:1.5~2.5；In the mixture of the magnesium chloride hexahydrate and magnesium nitrate hexahydrate
The mass ratio of magnesium chloride hexahydrate and magnesium nitrate hexahydrate is preferably 1:1~3, more preferably 1:1.5~2.5.
In the present invention, the mass ratio of the block shape hydrophilic modifying expanded graphite and hydrated salt is preferably 15~30:70
~85, more preferably 18~25:75~82, most preferably 20:80.
The invention provides a kind of preparation side of hydrated salt described in such scheme-modified expanded graphite composite phase-change material
Method, comprises the following steps：
Hydrophilic modifying expanded graphite is suppressed, block shape hydrophilic modifying expanded graphite is obtained；
The block shape hydrophilic modifying expanded graphite and molten state hydrated salt are subjected to mixing and absorption, hydrated salt-change is obtained
Property expanded graphite composite phase-changing material.
The present invention carries out hydrophilic modifying to expanded graphite using wetting agent, and modified expanded graphite is porous lamella knot
Structure, and substantial amounts of hydrophilic radical is attached to, the compatibility of expanded graphite and hydrated salt greatly improved, improves to hydrated salt
Adsorbance, can be such that hydrated salt is evenly distributed in modified expanded graphite in follow-up adsorption process, reduce phenomenon of phase separation
Generation.And the hydrophilic modifying expanded graphite thermal conductivity factor that the present invention is obtained is high, rate of heat transfer increase can enter one after being combined
Step improves the heat conductivity of composite phase-change material, reduces the degree of supercooling of composite phase-change material.
The present invention is suppressed hydrophilic modifying expanded graphite, obtains block shape hydrophilic modifying expanded graphite.In the present invention
In, the temperature of the compacting is preferably 10~40 DEG C, more preferably 20~30 DEG C, most preferably 25 DEG C；The pressure of the compacting
Preferably 5~30MPa, more preferably 10~25MPa, most preferably 15~20MPa.The device that the present invention is used compacting does not have
It is specifically limited, suppressed, pressed present invention preferably uses tablet press machine using device well known to those skilled in the art
System.In the present invention, the density of the block shape hydrophilic modifying expanded graphite is consistent with such scheme, will not be repeated here.
Obtain after block shape hydrophilic modifying expanded graphite, the present invention preferably by the block shape hydrophilic modifying expanded graphite with
Molten state hydrated salt carries out mixing and absorption, obtains hydrated salt-modified expanded graphite composite phase-change material.In the present invention, it is described
The mass ratio of block shape hydrophilic modifying expanded graphite and hydrated salt is preferably 15~30:70~85, more preferably 18~25:75~
82, most preferably 20~80；The species of the hydrated salt is consistent with such scheme, will not be repeated here.
In the present invention, the molten state hydrated salt is preferably obtained by heating melting to hydrated salt；The present invention is to heating
The temperature of melting does not have particular/special requirement, in a particular embodiment of the present invention, and heating melting temperature is determined according to the fusing point of hydrated salt
Degree.In the present invention, the heating melting temperature is preferably above 0.5~50 DEG C of hydrated salt fusing point, is more preferably higher than hydrated
10~35 DEG C of salt fusing point；Hydrated salt is heated and melted by the present invention preferably in closed environment.
In the present invention, the time of the mixing and absorption is preferably 1~5h, more preferably 2~4h, most preferably 2.5~
3.5h；The temperature of the mixing and absorption preferably remains in the heating melting temperature of hydrated salt.
After the mixing and absorption, the present invention obtains hydrated salt-modified expanded stone preferably by the sample natural cooling after absorption
Black composite phase-change material.Sample after absorption is preferably cooled to 10~30 DEG C, more preferably 15~25 DEG C by the present invention.
Hydrated salt-modified expanded graphite the composite phase-change material provided with reference to embodiment the present invention and its preparation side
Method is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
The Triton X-100 (TritonX-100) of 5 mass parts is dissolved into 500 mass parts absolute ethyl alcohols,
The ethanol solution of Triton X-100 is obtained, the expanded graphite of 95 mass parts is added to polyethylene glycol octyl group benzene
In the ethanol solution of base ether, ultrasonic 3min, ultrasonic power 300W, ultrasound after sample be put into 80 DEG C of baking oven dry
Hydrophilic modifying expanded graphite is obtained after 24h, cooling；
Hydrophilic modifying expanded graphite is pressed into density for 300kg/m using tablet press machine3Block, press temperature is 10
DEG C, pressing pressure is 5Mpa, obtains block shape hydrophilic modifying expanded graphite；
Calcium chloride hexahydrate is heated melting in 100 DEG C of closed environment, block shape hydrophilic modifying expanded graphite is added
Adsorbed in the calcium chloride hexahydrate of melting, the mass ratio of wherein block shape hydrophilic modifying expanded graphite and calcium chloride hexahydrate is
10:90, adsorption time is 1h, and temperature maintains 100 DEG C during absorption, and sample is cooled into 10 DEG C after the completion of absorption, is hydrated
Salt-modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, and before adsorbing hydrated salt
The density of block shape hydrophilic modifying expanded graphite is 300kg/m3, illustrate that hydrated salt is adsorbed in block shape hydrophilic modifying expanded graphite
Amount reaches 1700kg/m3, calculating (quality of unit volume hydrated salt adsorbance/unit volume composite phase-change material) must can be combined
The adsorbance of hydrated salt reaches 85wt% in phase-change material；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 27 DEG C, and enthalpy of phase change is 162J/g, degree of supercooling
For 1.3 DEG C, thermal conductivity factor is 3.86 (Wm-1·K-1), energy storage density is 298MJ/m3；
The pore structure of the expanded graphite after before modified is observed using SEM, as a result as shown in figure 1,
Fig. 1 is the electron scanning micrograph of rear Porous Structure of Expanded Graphite before modified, and wherein Fig. 1 (a) is expanded graphite before modified
Pore structure observation figure, Fig. 1 (b) schemes for the pore structure observation of modified expanded graphite；According to Fig. 1 as can be seen that after before modified
Expanded graphite is all porous sheet structure, but modified expanded graphite worm state is not obvious, and lamella distribution is more equal
It is even；
The structure of expanded graphite after before modified is characterized using infrared spectrometric analyzer, acquired results as shown in Fig. 2
Fig. 2 is the infrared spectrogram of rear expanded graphite before modified；According to Fig. 2 as can be seen that modified expanded graphite 1000~
1500-1In the range of stretching vibration be remarkably reinforced, illustrate to be attached to substantial amounts of hydrophilic radical on modified expanded graphite；
The water contact angle of graphite before and after improving is determined using water contact angle measuring instrument, measurement result is as shown in figure 3, Fig. 3 is
The water contact angle figure of expanded graphite after before modified, wherein Fig. 3 (a) is the water contact angle figure of expanded graphite before modified, and Fig. 3 (b) is
The water contact angle figure of modified expanded graphite；According to Fig. 3 as can be seen that the water contact angle of modified expanded graphite is 0 °, relatively change
Greatly reduced before property, illustrate that the hydrophily of modified expanded graphite is greatly improved；
Expanded graphite after before modified is tested the absorption property of six calcium chloride hydrates, acquired results as shown in figure 4,
Fig. 4 is absorption property figure of the rear expanded graphite to hydrated salt before modified；According to Fig. 4 as can be seen that modified expanded graphite pair
The rate of adsorption and adsorbance of hydrated salt, which are obtained for, to be greatly improved；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result as shown in figure 5, Fig. 5 is the electron scanning micrograph of hydrated salt-modified expanded graphite composite phase-change material；According to figure
5 as can be seen that substantial amounts of hydrated salt is attracted to the pore structure and piece interlayer of modified expanded graphite, and hydrated salt is modified expanded
It is evenly distributed in graphite.
Embodiment 2
The Triton X-100 of 30 mass parts is dissolved into 1000 mass parts absolute ethyl alcohols, polyethylene glycol is obtained
The ethanol solution of octyl phenyl ether, then the expanded graphite of 70 mass parts is added to the anhydrous of Triton X-100
In ethanol solution, ultrasonic 20min, ultrasonic power 350W, ultrasound after sample be put into 150 DEG C of baking oven dry 24h, take out it is cold
But hydrophilic modifying expanded graphite is obtained afterwards；
Hydrophilic modifying expanded graphite is pressed into density for 600kg/m3Block, press temperature be 40 DEG C, pressing pressure
For 30Mpa, block shape hydrophilic modifying expanded graphite is obtained；
By calcium chloride hexahydrate in 40 DEG C of closed environment heating and melting, block shape hydrophilic modifying expanded graphite is added molten
Adsorbed in the calcium chloride hexahydrate melted, the mass ratio of wherein block shape hydrophilic modifying mass of expanded graphite and calcium chloride hexahydrate is
30:70, adsorption time is 1h, and temperature maintains 40 DEG C during absorption, and sample is cooled into 20 DEG C after the completion of absorption, is hydrated
Salt-modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 70wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 27 DEG C, and enthalpy of phase change is 126J/g, degree of supercooling
For 0.3 DEG C, thermal conductivity factor is 9.86 (Wm-1·K-1), energy storage density is 258MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 3
The Triton X-100 (TritonX-100) of 17.5 mass parts is dissolved into 750 mass parts absolute ethyl alcohols
In, the ethanol solution of Triton X-100 is obtained, then the expanded graphite of 82.5 mass parts is added to poly- second two
In the ethanol solution of alcohol octyl phenyl ether, ultrasonic 11.5min, ultrasonic power 400W, ultrasound after sample be put into 115 DEG C
18h is dried in baking oven, hydrophilic modifying expanded graphite is obtained after taking out cooling；
Hydrophilic modifying expanded graphite is pressed into density for 450kg/m3Block, press temperature is 25 DEG C, and pressing pressure is
17.5Mpa, obtains block shape hydrophilic modifying expanded graphite；
Calcium chloride hexahydrate is heated in 35 DEG C of closed environment and melted, block shape hydrophilic modifying expanded graphite is added and melted
Calcium chloride in adsorbed, wherein the mass ratio of modified expanded graphite block and calcium chloride hexahydrate be 15:85, adsorption time is
3h, temperature maintains 35 DEG C during absorption, and sample is cooled into 20 DEG C after the completion of absorption, obtains hydrated salt-modified expanded graphite multiple
Close phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 1900kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 76.3wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 27 DEG C, and enthalpy of phase change is 153J/g, degree of supercooling
For 0.8 DEG C, thermal conductivity factor is 6.15 (Wm-1·K-1), energy storage density is 275MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 4
Wetting agent is replaced with into Triton X-100 (TritonX-100) and sodium dodecyl sulfate mixture
(wherein Triton X-100 is 10 mass parts, and lauryl sodium sulfate is 7.5 mass parts), according in embodiment 3
Method prepares hydrophilic modifying expanded graphite；
According to briquetting and absorption is carried out the step of embodiment 3, hydrated salt-modified expanded graphite composite phase-change material is obtained.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 27.3 DEG C, and enthalpy of phase change is 152J/g, supercooling
Spend for 1.3 DEG C, thermal conductivity factor is 5.75 (Wm-1·K-1), energy storage density is 278MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 5
Wetting agent is replaced with into Triton X-100 (TritonX-100), neopelex and 16
(wherein Triton X-100 is 8 mass parts to alkyl bromination ammonium mixture, and neopelex is 5 mass parts, ten
Six alkyl bromination ammoniums are 4.5 mass parts), prepare hydrophilic modifying expanded graphite according to the step in embodiment 3；
According to briquetting and absorption is carried out the step of embodiment 3, hydrated salt-modified expanded graphite composite phase-change material is obtained.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 27.1 DEG C, and enthalpy of phase change is 155J/g, supercooling
Spend for 2.3 DEG C, thermal conductivity factor is 6.75 (Wm-1·K-1), energy storage density is 276MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 6
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；
Hydrophilic modifying expanded graphite is pressed into density for 400kg/m3Block, press temperature is 15 DEG C, and pressing pressure is
5Mpa, obtains block shape hydrophilic modifying expanded graphite；
Magnesium chloride hexahydrate is heated in 125 DEG C of closed environment and melted, block shape hydrophilic modifying expanded graphite is added molten
Adsorbed in the magnesium chloride hexahydrate melted, wherein the mass ratio of modified expanded graphite block and magnesium chloride hexahydrate is 20:80, during absorption
Between be 1.5h, temperature maintains 125 DEG C during absorption, and sample is cooled into 20 DEG C after the completion of absorption, obtains hydrated salt-modified expanded
Graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 80wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 117 DEG C, and enthalpy of phase change is 102J/g, supercooling
Spend for 1.3 DEG C, thermal conductivity factor is 6.78 (Wm-1·K-1), energy storage density is 285MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 7
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；Will be modified expanded according to the method in embodiment 3
Graphite is pressed into block；Hydrated salt is replaced with into magnesium nitrate hexahydrate, adsorbed according to the method for embodiment 3, obtain hydrated salt-
Modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 1990kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.4wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 110 DEG C, and enthalpy of phase change is 136J/g, supercooling
Spend for 0.7 DEG C, thermal conductivity factor is 5.94 (Wm-1·K-1), energy storage density is 286MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 8
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；Will be modified expanded according to the method in embodiment 3
Graphite is pressed into block；Hydrated salt is replaced with into ten sulfate dihydrate aluminium ammoniums, is adsorbed according to the method for embodiment 3, obtains water
Close salt-modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 1998kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 89 DEG C, and enthalpy of phase change is 178J/g, degree of supercooling
For 2.7 DEG C, thermal conductivity factor is 6.24 (Wm-1·K-1), energy storage density is 279MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 9
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；Will be modified expanded according to the method in embodiment 3
Graphite is pressed into block；Hydrated salt is replaced with to mixture (the wherein six water chlorinations of ten sulfate dihydrate aluminium ammoniums and magnesium chloride hexahydrate
Magnesium is 26.25 mass parts, and ten sulfate dihydrate aluminium ammoniums are 63.75 mass parts), adsorbed according to the method for embodiment 3, obtain water
Close salt-modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 56 DEG C, and enthalpy of phase change is 170J/g, degree of supercooling
For 1.7 DEG C, thermal conductivity factor is 6.21 (Wm-1·K-1), energy storage density is 278MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 10
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；Will be modified expanded according to the method in embodiment 3
Graphite is pressed into block；
Hydrated salt is replaced with into the mixture of ten sulfate dihydrate aluminium ammoniums and magnesium chloride hexahydrate, and (wherein magnesium chloride hexahydrate is
29.75 mass parts, ten sulfate dihydrate aluminium ammoniums are 55.25 mass parts), adsorbed, be hydrated according to the method for embodiment 3
Salt-modified expanded graphite composite phase-change material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 59 DEG C, and enthalpy of phase change is 176J/g, degree of supercooling
For 2.1 DEG C, thermal conductivity factor is 6.01 (Wm-1·K-1), energy storage density is 278.5MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
Embodiment 11
Hydrophilic modifying expanded graphite is prepared according to the method in embodiment 3；Will be modified expanded according to the method in embodiment 3
Graphite is pressed into block；
Hydrated salt is replaced with into the mixture of ten sulfate dihydrate aluminium ammoniums and magnesium chloride hexahydrate, and (wherein magnesium chloride hexahydrate is 25.5
Mass parts, ten sulfate dihydrate aluminium ammoniums are 59.5 mass parts), adsorbed according to the method for embodiment 3, obtain hydrated salt-modification
Expanded graphite composite phase-changing material.
The density of gained hydrated salt-modified expanded graphite composite phase-change material is 2000kg/m3, can be calculated and be wherein hydrated
The adsorbance of salt reaches 77.5wt%；
The phase transition temperature of gained hydrated salt-modified expanded graphite phase-change material is 57 DEG C, and enthalpy of phase change is 172J/g, degree of supercooling
For 1.9 DEG C, thermal conductivity factor is 5.99 (Wm-1·K-1), energy storage density is 285MJ/m3；
Structure, water contact angle and the absorption property of rear expanded graphite before modified are carried out according to the method described in embodiment 1
Characterize, acquired results and embodiment 1 are similar；
Gained hydrated salt-modified expanded graphite composite phase-change material is observed using SEM, gained
As a result it is similar with embodiment 1.
As seen from the above embodiment, the energy storage for hydrated salt-modified expanded graphite composite phase-change material that the present invention is provided is close
Degree is big, and thermal conductivity factor is high, and degree of supercooling is low；And the hydrophily of modified expanded graphite strengthens, good surface activity, water contact angle can reach
0 °, and modified expanded graphite is high to the adsorbance of hydrated salt, hydrated salt is evenly distributed inside modified expanded graphite.
As seen from the above embodiment, the present invention the above be only the preferred embodiment of the present invention, it is noted that for
For those skilled in the art, under the premise without departing from the principles of the invention, can also make it is some improvement and
Retouching, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of hydrated salt-modified expanded graphite composite phase-change material, including block shape hydrophilic modifying expanded graphite and absorption exist
Hydrated salt in the block shape hydrophilic modifying expanded graphite；The density of the block shape hydrophilic modifying graphite be 300~
600kg/m3。
2. composite phase-change material according to claim 1, it is characterised in that block shape is hydrophilic in the composite phase-change material
The mass ratio of modified expanded graphite and hydrated salt is 15~30:70~85.
3. composite phase-change material according to claim 1 or 2, it is characterised in that the hydrated salt is calcium chloride hexahydrate, six
One or more of mixtures in aqueous magnesium chloride, magnesium nitrate hexahydrate and ten sulfate dihydrate aluminium ammoniums.
4. the preparation method of hydrated salt described in claims 1 to 3 any one-modified expanded graphite composite phase-change material, including
Following steps：
Hydrophilic modifying expanded graphite is suppressed, block shape hydrophilic modifying expanded graphite is obtained；
The block shape hydrophilic modifying expanded graphite and molten state hydrated salt are subjected to mixing and absorption, hydrated salt-modification is obtained swollen
Swollen graphite composite phase-change material.
5. preparation method according to claim 4, it is characterised in that the temperature of the compacting is 10~40 DEG C；The pressure
The pressure of system is 5~30MPa.
6. preparation method according to claim 4, it is characterised in that the time of the mixing and absorption is 1~5h.
7. preparation method according to claim 4, it is characterised in that the preparation method bag of the hydrophilic modifying expanded graphite
Include following steps：
Ultrasound after wetting agent and expanded graphite, polar solvent are mixed, obtains hydrophilic modifying expanded graphite.
8. preparation method according to claim 7, it is characterised in that the wetting agent be Triton X-100,
One or more of mixtures in lauryl sodium sulfate, neopelex and cetyl ammonium bromide.
9. the preparation method according to claim 7 or 8, it is characterised in that the mass ratio of the wetting agent and expanded graphite
For 5~30:70~95.
10. the preparation method according to claim 7 or 8, it is characterised in that the ultrasonic time is 3~20min.
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