CN109266314A - A kind of flexible compound phase-change material and preparation method thereof - Google Patents
A kind of flexible compound phase-change material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of flexible compound phase-change material, belong to phase-change heat-storage material field.The present invention using water in freezing dry process is formed by ice crystal as template and prepares the carbon nanotube base aeroge carrier of loose porous three-dimensional net structure, obtain flexible structure, strong hydrogen bond action between polyvinyl alcohol, chitosan and phase transformation core material, more phase transformation core materials can be loaded, the raising of phase transformation core material load capacity, improve the energy storage density of material, utilize the matching between phase transformation core material and the duct of carbon nanotube-based material, the flexibility of material can be made still to remain behind, using the high thermal conductivity of carbon nanotube, keep the thermal conductivity of material more preferable.
Description
Technical field
The invention belongs to technical field of phase change heat storage more particularly to a kind of flexible compound phase-change material and its preparation sides
Method.
Background technique
With the development of electronic technology, increasing simultaneously in the heat radiation power of electronic chip and heat radiation density, to it
The requirement of thermal control is also higher and higher.Phase-change accumulation energy thermal control is since energy storage density is high, temperature fluctuation is small, system is simple and convenient to operate
The advantages that, it has also become one of most important passive thermal control means of electronic device.But the solid-liquid phase change material generallyd use at present
Due in phase transition process, oneself became and restricted phase transformation thermal control difficult to install caused by solid-liquid variation, the problems such as easily leaking out
Key is because of rope.The scheme to solve the above problems using shaping phase-change material is proposed in spite of researcher, but is still had at present
Many critical issues do not solve, and are mainly reflected in: energy storage density is low and lacks flexibility, and phase transformation thermal control component is in complicated shape
It is difficult to install on thermal control surface.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of flexible compound phase-change materials and its preparation method and application.
Flexible compound phase-change material flexibility produced by the present invention is super good, and energy storage density is high.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of flexible compound phase-change material, comprising the following steps:
Chitosan-acetic acid solution is provided；
Polyvinyl alcohol water solution is provided；
Carbon nanotube is mixed with water, obtains carbon nano tube suspension；
The carbon nano tube suspension is added in chitosan-acetic acid solution, mixed solution is obtained；
The mixed solution is mixed with polyvinyl alcohol water solution, obtains precursor solution；
The precursor solution is freeze-dried, carbon nanotube base aeroge carrier is obtained；
The carbon nanotube base aeroge carrier is impregnated with phase transformation core material solution, obtains flexible compound phase-change material, it is described
Phase transformation core material solution is polyglycol solution, octadecyl alcolol solution or octadecylamine solution.
Preferably, in the carbon nanotube in the carbon nano tube suspension and chitosan-acetic acid solution chitosan mass ratio
For 1:1~1:10.
Preferably, the concentration of the carbon nano tube suspension is 4~35mg/mL, the quality of the chitosan-acetic acid solution
Score is 1~5%.
Preferably, in the carbon nanotube in the carbon nano tube suspension and polyvinyl alcohol water solution polyvinyl alcohol quality
Than for 1:1~1:20.
Preferably, the mass fraction of the polyvinyl alcohol water solution is 2~25%.
Preferably, the mass ratio of phase transformation core material and carbon nanotube base aeroge carrier is 0.5 in the phase transformation core material solution:
9.5~5:5.
Preferably, the molecular weight of the polyethylene glycol is 2000~20000.
Preferably, the temperature of the freeze-drying is -20~-196 DEG C, and the time is 2~12h, and pressure is 25~95mT.
The present invention also provides flexible compound phase-change material made from preparation method described in above-mentioned technical proposal, the flexibility
Composite phase-change material includes phase transformation core material and carbon nanotube base aeroge carrier, and the phase transformation core material is supported on the carbon nanotube
In the three-dimensional hole of base aeroge carrier.
Preferably, the load capacity of the phase transformation core material is 50~95%.
The present invention provides a kind of preparation methods of flexible compound phase-change material, comprising the following steps: provides chitosan vinegar
Acid solution；Polyvinyl alcohol water solution is provided；Carbon nanotube is mixed with water, obtains carbon nano tube suspension；By the carbon nanometer
Pipe suspension is added in chitosan-acetic acid solution, obtains mixed solution；The mixed solution is mixed with polyvinyl alcohol water solution,
Obtain precursor solution；The precursor solution is freeze-dried, carbon nanotube base aeroge carrier is obtained；With phase transformation core
Material solution impregnates the carbon nanotube base aeroge carrier, obtains flexible compound phase-change material, the phase transformation core material solution is poly-
Ethylene glycol solution, octadecyl alcolol solution or octadecylamine solution.The present invention using water in freezing dry process be formed by ice crystal as
Template prepares the carbon nanotube base aeroge carrier of loose porous three-dimensional net structure, obtains flexible structure, polyvinyl alcohol, shell
Strong hydrogen bond action between glycan and phase transformation core material, enters phase transformation core material in the duct of tridimensional network, and make phase transformation
Core material, which is bound in, prevents the generation of leakage in duct；The size in aperture is controlled using freeze-drying；Utilize carbon nanotube
Suspension controls the thickness and flexibility of composite phase-change material, can load more phase transformation core materials, the load capacity of phase transformation core material
It increases, improves the energy storage density of material, it, can be with using the matching between phase transformation core material and the duct of carbon nanotube-based material
It remains behind the flexibility of material still, using the high thermal conductivity of carbon nanotube, keeps the thermal conductivity of material more preferable.The present invention mentions
The preparation method of confession has many advantages, such as low in cost, easy to operate.Embodiment statistics indicate that, flexible compound produced by the present invention
Phase-change material is tested by compression resilience, and maximum compressibility can revert to original 99% up to 99%；It is surveyed by flexibility
Examination, composite phase-change material is bent respectively, folded and distorted, can return to the original form completely under the effect of external force；
Mechanical property is excellent, is tested by BET, is multistage by the available carbon nanotube based support material of nitrogen adsorption desorption curve
Hole, micron openings is relatively more, is very beneficial for the encapsulation of phase-change material, and enthalpy of phase change is up to 149J/g.
Detailed description of the invention
Fig. 1 is that the SEM of 1 carbon nanotube base aeroge carrier of embodiment schemes；
Fig. 2 is that the SEM of 1 flexible compound phase-change material of embodiment schemes；
Fig. 3 is the DSC curve figure of 1 flexible compound phase-change material of embodiment；
Fig. 4 is that 1 flexible compound phase-change material of embodiment carries out bending property test photo；
Fig. 5 is that the SEM of 3 flexible compound phase-change material of embodiment schemes；
Fig. 6 is that the SEM of 4 flexible compound phase-change material of embodiment schemes；
Fig. 7 is the DSC curve figure of 5 flexible compound phase-change material of embodiment；
Fig. 8 is the DSC curve figure of 6 flexible compound phase-change material of embodiment.
Specific embodiment
The present invention provides a kind of preparation methods of flexible compound phase-change material, comprising the following steps:
Chitosan-acetic acid solution is provided；
Polyvinyl alcohol water solution is provided；
Carbon nanotube is mixed with water, obtains carbon nano tube suspension；
The carbon nano tube suspension is added in chitosan-acetic acid solution, mixed solution is obtained；
The mixed solution is mixed with polyvinyl alcohol water solution, obtains precursor solution；
The precursor solution is freeze-dried, carbon nanotube base aeroge carrier is obtained；
The carbon nanotube base aeroge carrier is impregnated with phase transformation core material solution, obtains flexible compound phase-change material, it is described
Phase transformation core material solution is polyglycol solution, octadecyl alcolol solution or octadecylamine solution.
The present invention provides chitosan-acetic acid solution.In the present invention, the mass fraction of the chitosan-acetic acid solution is preferred
It is 1~5%, more preferably 2~4%.The present invention preferably adds chitosan into and prepares chitosan-acetic acid solution in acetic acid.At this
In invention, the molar concentration of the acetic acid is preferably 1~5mol/L.In the present invention, the dissolubility of the chitosan is good, and flexible
It is good.
In the present invention, it prepares chitosan-acetic acid solution preferably to carry out under the conditions of ultrasonic agitation, at the ultrasonic agitation
The time of reason is preferably 60min, and the speed of ultrasonic agitation is preferably 600r/min.
The present invention provides polyvinyl alcohol water solution.In the present invention, the mass fraction of the polyvinyl alcohol water solution is preferred
It is 2~25%, more preferably 15%.In the present invention, polyvinyl alcohol water solution is prepared preferably to carry out under agitation, it is described
The time of stir process is preferably 60min, and the speed of stirring is preferably 600r/min.
The present invention mixes carbon nanotube with water, obtains carbon nano tube suspension.In the present invention, the mixing preferably exists
It is carried out under ultrasound condition, the time of the ultrasonic treatment is preferably 60min, and ultrasonic power is preferably 500~1000W.
In the present invention, the concentration of the carbon nano tube suspension is preferably 4~35mg/mL, more preferably 5~10mg/
mL.In the present invention, preferably, the reunion for utmostly reducing carbon nanotube is existing for dispersibility in chitosan for the carbon nanotube
As the flexibility and high-termal conductivity of carbon nanotube can give full play of.The present invention is to the source of the carbon nanotube without spy
Different restriction, using commercial goods well known to those skilled in the art.
The carbon nano tube suspension is added in chitosan-acetic acid solution the present invention, obtains mixed solution.In the present invention
In, in the carbon nanotube and chitosan-acetic acid solution in the carbon nano tube suspension mass ratio of chitosan be preferably 1:1~
1:10, more preferably 1:3~1:7.
In the present invention, the carbon nano tube suspension preferably includes to be ultrasonically treated after being added in chitosan-acetic acid solution.
The present invention does not have special restriction to the parameter of the ultrasonic treatment, can make carbon nano tube suspension and chitosan-acetic acid solution
It is uniformly mixed.
After obtaining mixed solution, the present invention mixes the mixed solution with polyvinyl alcohol water solution, and it is molten to obtain presoma
Liquid.In the present invention, in the carbon nanotube in the carbon nano tube suspension and polyvinyl alcohol water solution polyvinyl alcohol quality
Than being preferably 1:1~1:20, more preferably 1:5~1:15.In the present invention, polyvinyl alcohol water solution can be coupled carbon nanotube.
After the completion of mixing, gained mixed system is preferably carried out ultrasonication by the present invention, obtains precursor solution.In this hair
In bright, the time of the ultrasonication is preferably 45~60min, and the power of ultrasonication is preferably 500~1000W.
After obtaining precursor solution, the precursor solution is freeze-dried by the present invention, obtains carbon nanotube base gas
Gel carrier.In the present invention, the temperature of the freeze-drying is preferably -20~-196 DEG C, more preferably -60~-196 DEG C；
The time of the freeze-drying is preferably 2~12h, more preferable 2~10h；The pressure of the freeze-drying is preferably 25~95mT,
More preferably 36mT.The present invention is formed by ice crystal using water in freezing dry process and prepares loose porous three-dimensional as template
The carbon nanotube base aeroge carrier of network structure, obtains flexible structure.
After obtaining carbon nanotube base aeroge carrier, the present invention impregnates the carbon nanotube base airsetting with phase transformation core material solution
Glue carrier, obtains flexible compound phase-change material, and the phase transformation core material solution is polyglycol solution, octadecyl alcolol solution or octadecylamine
Solution.In the present invention, phase transformation core material and the mass ratio of carbon nanotube base aeroge carrier are preferred in the phase transformation core material solution
For 0.5:9.5~5:5.
The present invention does not have special restriction to the solvent of the phase transformation core material solution, can make for polyethylene glycol, octadecyl alcolol
It is completely dissolved with octadecylamine, the present invention does not have special restriction, energy to the concentration and dosage of the phase transformation core material solution
Phase transformation core material and the mass ratio of carbon nanotube base aeroge carrier is enough set to reach above-mentioned requirements.
In the present invention, the molecular weight of the polyethylene glycol is preferably 2000~20000.
The present invention also provides flexible compound phase-change material made from preparation method described in above-mentioned technical proposal, the flexibility
Composite phase-change material includes phase transformation core material and carbon nanotube base aeroge carrier, and the phase transformation core material is supported on the carbon nanotube
In the three-dimensional hole of base aeroge carrier.
In the present invention, the load capacity of the phase transformation core material is preferably 50~95%.
A kind of flexible compound phase-change material provided by the invention and preparation method thereof is carried out below with reference to embodiment detailed
Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) chitosan is put into molar concentration is to carry out ultrasonic agitation processing in 5mol/L acetum, stirs 60min,
Mixing speed is 600r/min, obtains the chitosan solution that uniform mass fraction is 1%；
(2) above-mentioned chitosan solution 100mL is added in the carbon nano tube suspension 20mL of the 5mg/mL of ultrasonic 60min, surpassed
Sound stirs 60min, obtains mixed solution, spare；
(3) ultrasonic powder in above-mentioned mixed solution is added in the polyvinyl alcohol water solution 10mL that the mass fraction of preparation is 15%
It is broken, precursor solution is made；
(4) precursor solution is put into liquid nitrogen and is freezed, cryogenic temperature is -196 DEG C, cooling time 2h, freeze-drying
Pressure is 36mT；The carbon nanotube base aeroge carrier of the dry obtained loose and porous structure of freeze dryer is put into after freezing completely；
(5) final flexible compound phase-change material, poly- second will be prepared with infusion process after Polyethylene glycol-2000 (PEG) dissolution
The mass ratio of glycol and carbon nanotube base aeroge carrier material is 95:5.
SEM test is carried out to carbon nanotube base aeroge carrier, as shown in Figure 1.As seen from Figure 1, carbon obtained is received
Mitron base aeroge carrier has the layer structure of orientation, and using end-to-end mechanism, carbon nanotube connects into three-dimensional net structure,
Porosity is high.
SEM test is carried out to flexible compound phase-change material, as shown in Figure 2.As seen from Figure 2, load phase transformation core material it
Afterwards, the surface of composite phase-change material becomes smooth, illustrates that phase transformation core material has been successfully entered in duct.
Fig. 3 is the DSC curve figure of flexible compound phase-change material, and enthalpy of phase change is an important ginseng of phase-change material thermal storage performance
Number, it is directly related to the storage density of phase-change material.As seen from Figure 3, by being carried out to the suction exothermic peak in DSC curve
Integral calculation obtains, when the mass fraction of PEG is 95%, has a very high load capacity, enthalpy of phase change 149J/g, pure PEG's
Enthalpy of phase change is 156J/g, consistent with result.
Bending property test is carried out to the flexible compound phase-change material of embodiment 1, as a result as shown in figure 4, can be seen by Fig. 4
Out, flexible compound phase-change material obtained is flexible, and excellent in mechanical performance.
Embodiment 2
It is same as Example 1, the difference is that: carbon nanotube concentration is changed as 10mg/mL.
(1) chitosan is put into molar concentration is to carry out ultrasonic agitation processing in 10mol/L acetum, is stirred
60min, mixing speed 600r/min obtain the chitosan solution that uniform mass fraction is 1%；
(2) above-mentioned chitosan solution 100mL is added in the carbon nano tube suspension 20mL of the 10mg/mL of ultrasonic 60min, surpassed
Sound stirs 60min, obtains mixed solution, spare；
(3) ultrasonic powder in above-mentioned mixed solution is added in the polyvinyl alcohol water solution 10mL that the mass fraction of preparation is 15%
It is broken, precursor solution is made；
(4) precursor solution is put into liquid nitrogen and is freezed, cryogenic temperature is -196 DEG C, cooling time 2h, freeze-drying
Pressure is 36mT；The carbon nanotube base aeroge carrier of the dry obtained loose and porous structure of freeze dryer is put into after freezing completely；
(5) final flexible compound phase-change material, poly- second will be prepared with infusion process after Polyethylene glycol-2000 (PEG) dissolution
The mass ratio of glycol and carbon nanotube base aeroge carrier material is 95:5.
Embodiment 2 has probed into the influence flexible of the concentration of carbon nanotube base aeroge carrier of carbon nanotube, by macroscopic view
Flexible test can proper carbon nanotube concentration be 10mg/mL when, compare embodiment 1, can be bigger with curved angle, can be with kinking
Degree it is bigger, illustrate the good mechanical property of carbon nanotube, have greatly improved to the flexibility of carrier material.
Embodiment 3
It is same as Example 1, the difference is that: it is -60 DEG C by cryogenic temperature variation.
(1) chitosan is put into molar concentration is to carry out ultrasonic agitation processing in 5mol/L acetum, stirs 60min,
Mixing speed is 600r/min, obtains the chitosan solution that uniform mass fraction is 1%；
(2) above-mentioned chitosan solution 100mL is added in the carbon nano tube suspension 20mL of the 5mg/mL of ultrasonic 60min, surpassed
Sound stirs 60min, obtains mixed solution, spare；
(3) ultrasonic powder in above-mentioned mixed solution is added in the polyvinyl alcohol water solution 10mL that the mass fraction of preparation is 15%
It is broken, precursor solution is made；
(4) precursor solution is put into liquid nitrogen and is freezed, cryogenic temperature is -60 DEG C, cooling time 10h, freeze-drying
Pressure is 36mT；The carbon nanotube base aeroge carrier of the dry obtained loose and porous structure of freeze dryer is put into after freezing completely；
(5) final flexible compound phase-change material, poly- second will be prepared with infusion process after Polyethylene glycol-2000 (PEG) dissolution
The mass ratio of glycol and carbon nanotube base aeroge carrier material is 95:5.
Embodiment 4
It is same as Example 1, the difference is that: it is -20 DEG C by cryogenic temperature variation.Other steps are as example 1.
Embodiment 3~4 has probed into influence of the height to pore size of cryogenic temperature, and Fig. 5 is compound made from embodiment 3
The SEM spectrogram of phase-change material, Fig. 6 are the SEM spectrogram of composite phase-change material made from embodiment 4, pass through contrast scans electron microscope
(Fig. 2, Fig. 5 and Fig. 6) can be seen that the reduction with cryogenic temperature, and aperture is smaller and smaller, when discovery cryogenic temperature is -20 DEG C,
Aperture is too big, is unfavorable for the load of phase-change material.
Embodiment 5
It is same as Example 1, the difference is that: phase transformation core material is changed as octadecylamine.
(1) chitosan is put into molar concentration is to carry out ultrasonic agitation processing in 5mol/L acetum, stirs 60min,
Mixing speed is 600r/min, obtains the chitosan solution that uniform mass fraction is 1%；
(2) above-mentioned chitosan solution 100mL is added in the carbon nano tube suspension 20mL of the 5mg/mL of ultrasonic 60min, surpassed
Sound stirs 60min, obtains mixed solution, spare；
(3) ultrasonic powder in above-mentioned mixed solution is added in the polyvinyl alcohol water solution 10mL that the mass fraction of preparation is 15%
It is broken, precursor solution is made；
(4) precursor solution is put into liquid nitrogen and is freezed, cryogenic temperature is -196 DEG C, cooling time 2h, freeze-drying
Pressure is 36mT；The carbon nanotube base aeroge carrier of the dry obtained loose and porous structure of freeze dryer is put into after freezing completely；
(5) final flexible compound phase-change material, polyethylene glycol and carbon nanometer are prepared after dissolving octadecylamine with infusion process
The mass ratio of pipe base aeroge carrier material is 95:5.
Embodiment 5 has probed into influence of the different phase transformation core material of load to enthalpy of phase change, tests discovery (Fig. 7) by DSC, bears
The polyethylene glycol that the enthalpy of phase change relative molecular weight after octadecylamine is 2000 is carried to decrease, probe into be molecular weight be 2000 it is poly-
The size of ethylene glycol is more matched with the aperture of carrier material.
Embodiment 6
It is same as Example 1, the difference is that: phase transformation core material is changed as octadecyl alcolol.Other steps are as example 1.
Embodiment 6 is the influence for having probed into the different phase transformation core material of load to enthalpy of phase change, tests discovery (Fig. 8) by DSC,
Enthalpy of phase change after load octadecyl alcolol is increased with respect to octadecylamine, and the hydrogen bond action of octadecyl alcolol and carrier material is more stronger.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flexible compound phase-change material, which comprises the following steps:
Chitosan-acetic acid solution is provided；
Polyvinyl alcohol water solution is provided；
Carbon nanotube is mixed with water, obtains carbon nano tube suspension；
The carbon nano tube suspension is added in chitosan-acetic acid solution, mixed solution is obtained；
The mixed solution is mixed with polyvinyl alcohol water solution, obtains precursor solution；
The precursor solution is freeze-dried, carbon nanotube base aeroge carrier is obtained；
The carbon nanotube base aeroge carrier is impregnated with phase transformation core material solution, obtains flexible compound phase-change material, the phase transformation
Core material solution is polyglycol solution, octadecyl alcolol solution or octadecylamine solution.
2. preparation method according to claim 1, which is characterized in that carbon nanotube in the carbon nano tube suspension with
The mass ratio of chitosan is 1:1~1:10 in chitosan-acetic acid solution.
3. preparation method according to claim 1 or 2, which is characterized in that the concentration of the carbon nano tube suspension be 4~
35mg/mL, the mass fraction of the chitosan-acetic acid solution are 1~5%.
4. preparation method according to claim 1, which is characterized in that carbon nanotube in the carbon nano tube suspension with
The mass ratio of polyvinyl alcohol is 1:1~1:20 in polyvinyl alcohol water solution.
5. preparation method according to claim 1 or 4, which is characterized in that the mass fraction of the polyvinyl alcohol water solution
It is 2~25%.
6. preparation method according to claim 1, which is characterized in that phase-change material is received with carbon in the phase transformation core material solution
The mass ratio of mitron base aeroge carrier is 0.5:9.5~5:5.
7. preparation method according to claim 1 or 6, which is characterized in that the molecular weight of the polyethylene glycol be 2000~
20000。
8. preparation method according to claim 1, which is characterized in that the temperature of the freeze-drying is -20~-196 DEG C,
Time is 2~12h, and pressure is 25~95mT.
9. flexible compound phase-change material made from preparation method described in claim 1~8 any one, which is characterized in that described
Flexible compound phase-change material includes phase transformation core material and carbon nanotube base aeroge carrier, and the phase transformation core material is supported on the carbon and receives
In the three-dimensional hole of mitron base aeroge carrier.
10. flexible compound phase-change material according to claim 9, which is characterized in that the load capacity of the phase transformation core material is
50~95%.
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