CN107586537A - A kind of composite phase-change material and preparation method thereof - Google Patents
A kind of composite phase-change material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of composite phase-change material and preparation method thereof, and three-dimensional sleeve-shaped graphene is prepared by hydro-thermal method, three-dimensional grapheme and salt-mixture is obtained into composite phase-change material by the way that vacuum impregnation technology is compound, salt-mixture includes borax and Na2SO4·10H2O, borax and Na in salt-mixture2SO4·10H2O mass ratio is (0~1):25, the mass ratio of three-dimensional grapheme and salt-mixture is 1:(7~10).Compared with prior art, the three-dimensional sleeve-shaped graphene-structured of the present invention be applied to inorganic hydrated salt it is compound in, to solving to be separated new thinking is provided with the problems such as supercooling, the application field of inorganic hydrated salt has been widened significantly, have a extensive future, and three-dimensional grapheme of the present invention/inorganic hydrated salt composite phase-change material can be used as phase transformation large capsule to be applied to the fields such as building ecological energy-conservation.
Description
Technical field
The present invention relates to composite phase-change material field, and in particular to a kind of composite phase-change material and preparation method thereof.
Background technology
Graphene there are a series of superiority to obtain researchers earnestly pay close attention to.Two-dimensional graphene has that specific surface area is big,
The characteristics of surface energy is high, easily reunite, limit its application in actual production.Three-dimensional grapheme (3D-rGO) has
There is stable mechanical property, remain some excellent properties of two-dimensional graphene, therefore three-dimensional graphite and its composite have
Wide application prospect.
Inorganic hydrated salt, which is used as phase-change material, has the advantages that latent heat of phase change is high, and phase transition temperature is low, and environmental pollution is small, can be with
Applied to fields such as cold chain transportation, ecotecture energy-conservations.Na2SO4·10H2O is typical low-temperature phase-change material, fusing point 32.4
DEG C, latent heat of phase change is higher, and chemical stability is good, nontoxic, and raw material easily obtain, cheap, can be applied to solar energy, industry more than
The storage of heat.But there is phenomenon of phase separation and have larger degree of supercooling in inorganic hydrated salt, seriously limit its extensive use.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of mechanical property and lead
Outstanding composite phase-change material of heating rate and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:A kind of composite phase-change material, the phase-change material bag
The salt-mixture for including three-dimensional grapheme and being filled between three-dimensional grapheme, the salt-mixture include borax and Na2SO4·
10H2O, borax and Na in the salt-mixture2SO4·10H2O mass ratio is (0~1):25, the three-dimensional grapheme and mixing
The mass ratio of salt is 1:The amount of (7~10), wherein borax is not 0.
In the material, three-dimensional grapheme provides excellent mechanical property and structural stability, meanwhile, graphene can have
Effect improves the thermal conductivity without salification, improves the uniformity of inorganic hydrated salt, reduces problem of phase separation, and column vertical bottom face
There is certain anisotropy, and the Na that the present invention uses on direction with parallel bottom surface direction electric conductivity and thermal conductivity2SO4·
10H2Borax is added in O as nucleator, can effectively solve Na2SO4·10H2The problem of O degree of supercoolings are low.
A kind of preparation method of composite phase-change material as described above, including following steps:
(1) using such as Chen J, Yao B, Li C, et al.An improved Hummers method for eco-
friendly synthesis of graphene oxide[J].Carbon,2013,64(11):225-229. described changes
Graphite oxide solution is prepared in the Hummers methods entered, ultrasound, is dried under hyperbaric environment, and then cooling obtains three-dimensional grapheme
Hydrogel;
(2) the three-dimensional grapheme hydrogel precooling for obtaining step (1), is then freeze-dried under vacuum environment, obtains three
Tie up sleeve-shaped graphene aerogel;
(3) by borax and Na2SO4·10H2O is well mixed to obtain salt-mixture, with the three-dimensional sleeve-shaped graphite of step (2) gained
Alkene aeroge mixes, and then heated sealed, makes salt-mixture fully melt and be totally submerged three-dimensional sleeve-shaped graphene aerogel;
(4) the three-dimensional sleeve-shaped graphene aerogel that the mixed salt that step (3) obtains submerges is placed on vacuum condition
Under, constant temperature is kept, and is then cooled down, is produced the composite phase-change material.
The concentration of graphite oxide solution described in step (1) is 5~8mg/mL.
The ultrasonic time described in step (1) is 1~2h.
The temperature dried described in step (1) is 160~180 DEG C, and drying time is 12~24h, under the temperature, pressure,
Graphite can be transformed into three-dimensional grapheme.
The temperature of precooling described in step (2) is -15~-30 DEG C, and the time of precooling is 2~4h.
When being freeze-dried described in step (2), the environment vacuum degree holding≤100Pa, the temperature of freeze-drying is -10
~-30 DEG C, the time of freeze-drying is 24~36h.
The temperature of heated sealed described in step (3) is 50~70 DEG C, and the time of heated sealed is 2~4h.
Vacuum condition is 0.075~0.085MPa in step (4), and the temperature that constant temperature is kept is 50~70 DEG C, and constant temperature is kept
Time be 0.5~2h.
Reaction in step (1) is:Graphite obtains graphite oxide under strong oxidizer effect in improved hummers methods;
Peeled off by ultrasound, graphite oxide is peeled off to the graphene oxide for turning into few layer;Under the HTHP that hydrothermal reaction kettle provides,
Graphene oxide is reduced, and forms the graphene aerogel with 3-D solid structure.
In step (2):By freeze-drying, the three-dimensional structure of hydrogel in (1) is maintained, obtains utilizable having
The three-dimensional grapheme aeroge of mechanical strength.
In step (3):Three-dimensional grapheme aeroge provides multilayer interstitial structure as filling skeleton, to a certain degree
On play a part of slowing down inorganic salts phase separation.
In step (4):Using vacuum impregnation technology, inorganic salts are sufficient filling with three-dimensional grapheme it is compound, cool down band is multiple
Close phase-change material.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects:
(1) by three-dimensional sleeve-shaped graphene-structured be applied to inorganic hydrated salt it is compound in, to solve be separated and mistake
The problems such as cold, provides new thinking, has widened the application field of inorganic hydrated salt significantly, has had a extensive future;
(2) present invention prepared by three-dimensional grapheme/inorganic hydrated salt composite in three-dimensional grapheme provide it is excellent
Mechanical property and structural stability, meanwhile, graphene can be effectively improved the thermal conductivity of no salification, improve inorganic hydrated salt
Uniformity, problem of phase separation is reduced, and had on column vertical bottom face direction with parallel bottom surface direction electric conductivity and thermal conductivity
There is certain anisotropy, therefore three-dimensional grapheme/inorganic hydrated salt composite phase-change material that the invention obtains can be used as phase transformation
Large capsule is applied to the fields such as building ecological energy-conservation.
Brief description of the drawings
Fig. 1 is composite phase-change material Cross Section Morphology figure of the present invention;
Fig. 2 is that the present invention meets phase change material releases heat conditional curve;
Fig. 3 is the T-T temperature lowering curves of different composite phase-change material;
Fig. 4 is 3D-rGO/Na2SO4·10H2O/2%Na2B4O7·10H2O composite phase-change material DSC curve figures.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
Graphite oxide solution is prepared using improved Hummers methods laboratory, graphite oxide solution is diluted to
Ultrasonic 1h, takes 60mL to be placed in water heating kettle after 5mg/ml, and 180 DEG C of insulation 16h, are cooled to room temperature, obtain in vacuum drying chamber
Three-dimensional grapheme hydrogel.By hydrogel pre-freeze 2h, in vacuum freeze-drying machine under holding≤100Pa vacuums, freeze-drying
24h, obtain three-dimensional sleeve-shaped graphene aerogel.
By the Na of excess2SO4·10H2O is placed in beaker with three-dimensional grapheme, adds Na2SO4·10H2O amount meets
Na2SO4·10H2Three-dimensional grapheme can be totally submerged by O after melting.The sealing of beaker preservative film is placed in vacuum drying chamber
In, drying box temperature setting is 70 DEG C, heated at constant temperature 2h, makes Na2SO4·10H2O fully melts.Beaker is taken out, uses syringe needle
Rupture disk is pricked about 30~60, hole, even air hole distribution by head.
Beaker is still placed in vacuum drying chamber, the lower 70 DEG C of constant temperature 0.5h of vacuum condition, makes Na2SO4·10H2O solution with
Three-dimensional grapheme is fully compound, is cooled to room temperature, obtains uniform composite phase-change material.(a), (b) are three-dimensional sleeve-shaped in Fig. 1
Graphene SEM photograph, (c), (d) are 3D-rGO/Na2SO4·10H2O composite phase-change material SEM photographs.Novel three-dimensional sleeve-shaped
Structure graphite alkene provides good memory space, wherein three-dimensional grapheme volumetric porosity about 94%, phase transformation material for phase-change material
Material uniformly and stably can be stored in sleeve-like configuration in phase transition process, effectively alleviate inorganic hydrated salt problem of phase separation.
Embodiment 2
Graphite oxide solution is prepared using improved Hummers methods laboratory.The graphite oxide of above-mentioned preparation is molten
Liquid is diluted to ultrasonic 2h after 8mg/ml, takes 60ml to be placed in water heating kettle, and 180 DEG C of insulation 24h, are cooled to room in vacuum drying chamber
Temperature, obtain three-dimensional grapheme hydrogel.By hydrogel pre-freeze 3h, in vacuum freeze-drying machine under holding≤100Pa vacuums, freezing
36h is dried, obtains three-dimensional sleeve-shaped graphene aerogel.
By Na2SO4·10H2O is placed in beaker with three-dimensional grapheme, adds Na2SO4·10H2O amount meets
Na2SO4·10H2Three-dimensional grapheme can be totally submerged by O after melting.The sealing of beaker preservative film is placed in vacuum drying chamber
In, drying box temperature setting is 60 DEG C, heated at constant temperature 3h, makes Na2SO4·10H2O fully melts.Beaker is taken out, uses syringe needle
Rupture disk is pricked about 50, hole, even air hole distribution by head.
Beaker is still placed in vacuum drying chamber, the lower 60 DEG C of constant temperature 1.5h of vacuum condition, makes Na2SO4·10H2O solution with
Three-dimensional grapheme is fully compound, is cooled to room temperature, obtains uniform composite phase-change material.To Na2SO4·10H2O raw materials and 3D-
rGO/Na2SO4·10H2O composite phase-change materials do DSC thermal performance analysis, as shown in Figure 2.3D-rGO/Na2SO4·10H2O is compound
The phase transition temperature of phase-change material is less than Na2SO4·10H2O phase transition temperature, it follows that 3D-rGO can effectively improve phase transformation material
The heat conductivility of material.
Embodiment 3
Graphite oxide solution is prepared using improved Hummers methods laboratory.The graphite oxide of above-mentioned preparation is molten
Liquid is diluted to ultrasonic 2h after 7mg/ml, takes 45ml to be placed in water heating kettle, and 160 DEG C of insulation 12h, are cooled to room in vacuum drying chamber
Temperature, obtain three-dimensional grapheme hydrogel.By hydrogel at -30 DEG C pre-freeze 4h, holding≤100Pa vacuum in vacuum freeze-drying machine
Under degree, -30 DEG C of freeze-drying 24h, three-dimensional sleeve-shaped graphene aerogel is obtained.
By borax, Na2SO4·10H2O presses 1 respectively:100、1:50、1:33、1:25 mass ratioes are well mixed, by mixture
It is placed in three-dimensional grapheme in beaker, the amount for adding mixture meets to be totally submerged three-dimensional grapheme after thawing.Will
The sealing of beaker preservative film is placed in vacuum drying chamber, and drying box temperature setting is 70 DEG C, heated at constant temperature 4h, makes Na2SO4·
10H2O fully melts.Beaker is taken out, rupture disk is pricked into about 40, hole, even air hole distribution with syringe needle.
Beaker is still placed in vacuum drying chamber, the lower 50 DEG C of constant temperature 2h of vacuum condition, makes mixture solution and three-dimensional graphite
Alkene is fully compound, is cooled to room temperature, obtains uniform composite phase-change material.Fig. 3 is that the T-T coolings of different composite phase-change material are bent
Line, as seen from the figure, 3D-rGO, Na2B4O7·10H2O can effectively reduce the degree of supercooling of phase-change material, wherein, 3D-rGO with
Na2B4O7·10H2O collective effect effects are more obvious, when borax and Na2SO4·10H2O mass ratioes are 1:When 50, degree of supercooling drop
Low is 2.5 DEG C.
Embodiment 4
Graphite oxide solution is prepared using improved Hummers methods laboratory.The graphite oxide of above-mentioned preparation is molten
Ultrasonic 1.5h after liquid dilution finite concentration 6mg/ml, takes 60ml to be placed in water heating kettle, 160 DEG C of insulation 14h in vacuum drying chamber,
Room temperature is cooled to, obtains three-dimensional grapheme hydrogel.By hydrogel in -15 DEG C of pre-freeze 2h, kept in vacuum freeze-drying machine≤
Under 100Pa vacuums, 24h is freeze-dried at -10 DEG C, obtains three-dimensional sleeve-shaped graphene aerogel.
By borax, Na2SO4·10H2O presses 1:50 mass ratioes are well mixed, and mixture and three-dimensional grapheme are placed in into beaker
In, add Na2SO4·10H2O amount meets in Na2SO4·10H2Three-dimensional grapheme can be totally submerged by O after melting.It will burn
The sealing of cup preservative film is placed in vacuum drying chamber, and drying box temperature setting is 50 DEG C, heated at constant temperature 4h, makes Na2SO4·10H2O
Fully melt.Beaker is taken out, rupture disk is pricked into about 30, hole, even air hole distribution with syringe needle.
Beaker is still placed in vacuum drying chamber, the lower 70 DEG C of constant temperature 1h of vacuum condition, makes mixture solution and three-dimensional graphite
Alkene is fully compound, is cooled to room temperature, obtains uniform composite phase-change material.Fig. 4 is 3D-rGO/Na2SO4·10H2O/2%
Na2B4O7·10H2O composite phase-change material DSC curve figures, the degree of supercooling of phase-change material is about 8 DEG C, because DSC tests have necessarily
Hysteresis quality, by the figure can draw composite phase-change material degree of supercooling can by with 3D-rGO/Na2B4O7·10H2O is compound to be obtained
To being effectively improved.
Claims (9)
1. a kind of composite phase-change material, it is characterised in that the phase-change material includes three-dimensional grapheme and is filled in three-dimensional graphite
Salt-mixture between alkene, the salt-mixture include borax and Na2SO4·10H2O, borax and Na in the salt-mixture2SO4·
10H2O mass ratio is (0~1):25, the mass ratio of the three-dimensional grapheme and salt-mixture is 1:(7~10).
2. a kind of preparation method of composite phase-change material as claimed in claim 1, it is characterised in that including following step
Suddenly:
(1) graphite oxide solution is prepared using improved Hummers methods, ultrasound, dried, then cooling obtains three-dimensional graphite
Alkene hydrogel;
(2) the three-dimensional grapheme hydrogel precooling for obtaining step (1), is then freeze-dried under vacuum environment, obtains three-dimensional set
Tubular graphene aerogel;
(3) by borax and Na2SO4·10H2O is well mixed to obtain salt-mixture, with the three-dimensional sleeve-shaped graphene gas of step (2) gained
Gel mixes, and then heated sealed, makes salt-mixture fully melt and be totally submerged three-dimensional sleeve-shaped graphene aerogel;
(4) the three-dimensional sleeve-shaped graphene aerogel that the mixed salt for obtaining step (3) submerges is placed under vacuum, permanent
Temperature is kept, and is then cooled down, is produced the composite phase-change material.
3. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (1)
The concentration of graphite oxide solution is 5~8mg/mL.
4. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (1)
The time of ultrasound is 1~2h.
5. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (1)
Dry temperature is 160~180 DEG C, and drying time is 12~24h.
6. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (2)
The temperature of precooling is -15~30 DEG C, and the time of precooling is 2~4h.
7. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (2)
During freeze-drying, the environment vacuum degree holding≤100Pa, the temperature of freeze-drying is -10~-30 DEG C, freeze-drying when
Between be 24~36h.
8. the preparation method of a kind of composite phase-change material according to claim 2, it is characterised in that described in step (3)
The temperature of heated sealed is 50~70 DEG C, and the time of heated sealed is 2~4h.
A kind of 9. preparation method of composite phase-change material according to claim 2, it is characterised in that vacuum in step (4)
Condition is 0.075~0.085MPa, and the temperature that constant temperature is kept is 50~70 DEG C, and the time that constant temperature is kept is 0.5~2h.
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CN109929518A (en) * | 2019-03-29 | 2019-06-25 | 同济大学 | A kind of graphite oxide aerogel heat chemistry heat accumulation composite material and preparation method |
CN110499145A (en) * | 2019-08-26 | 2019-11-26 | 张立强 | Aeroge adsorbs phase-change accumulation energy powder, preparation method and applications |
CN110564374A (en) * | 2019-09-18 | 2019-12-13 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
CN110564374B (en) * | 2019-09-18 | 2021-08-03 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
CN115305059A (en) * | 2022-01-28 | 2022-11-08 | 兰州理工大学 | Preparation method and application of hexadecylamine three-dimensional graphene composite material |
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