CN110305634A - A kind of preparation method of carbon ball base composite phase-change material - Google Patents
A kind of preparation method of carbon ball base composite phase-change material Download PDFInfo
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- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The present invention provides a kind of preparation methods of carbon ball base composite phase-change material comprising following steps: dopamine being put into phosphate buffer solution and is stirred, and obtains poly-dopamine microballoon；Poly-dopamine microballoon, which is placed in tube furnace, to be pyrolyzed, and mesoporous carbon spheres (MCMS) is obtained；Using polyethylene glycol as core material, using the MCMS as carrier, by the hydrogen bond action between polyethylene glycol and dopamine, and realize polyethylene glycol is immobilized in carbon-based composite phase-change material (PEG/MCMS) in the hole of the mesoporous carbon spheres, is made.The invention patent synthesizes poly-dopamine micron particles using bionic method, poly-dopamine micron particles are pyrolyzed to obtain novel MCMS, and using this MCMS as the carrier preparation NEW TYPE OF COMPOSITE shaping phase-change material that thermal conductivity is good, enthalpy of phase change is high, preparation method has many advantages, such as easy to operate, mild condition, nonhazardous.
Description
Technical field
The invention belongs to the fields of phase-change material preparation, are more particularly to a kind of carbon ball base composite phase-change material and its preparation
Method.
Background technique
Organic phase change energy storage material because its energy storage density is big, corrosivity is small, small toxicity, it is at low cost the advantages that be widely used
With energy storage field；But the disadvantages of organic phase change material thermal coefficient is small, easy leakage hinders its wider application space.
In order to supply the short slab that organic phase change material and inorganic phase-changing material easily leak, thermal coefficient is small and are easily subcooled, can have pure
Machine or inorganic phase-changing material and another one or more functional material be combined with each other by specific method prepare it is a kind of newly
Stable phase-change material.Currently, the mesoporous materials such as mesoporous silicon, mesoporous carbon are good, mechanical strong because having large specific surface area, absorption property
Spending the advantages that high is applied to organic phase change material carrier and prepares shaping phase-change material.However, current mesoporous material preparation is still deposited
The defects of preparation process is complicated, at high cost.
Summary of the invention
The object of the present invention is to provide a kind of good shaping phase-change materials and preparation method thereof of thermal conductivity.
According to an aspect of the invention, there is provided a kind of preparation method of carbon ball base composite phase-change material comprising with
Under several steps:
Dopamine is put into phosphate buffer solution and is stirred, poly-dopamine microballoon is obtained；
Poly-dopamine microballoon, which is placed in tube furnace, to be pyrolyzed, and mesoporous carbon spheres (MCMS) is obtained；
Using polyethylene glycol as core material, using the MCMS as carrier, pass through the hydrogen bond between polyethylene glycol and dopamine
Effect, and realize polyethylene glycol is immobilized in carbon-based composite phase-change material (PEG/ in the hole of the mesoporous carbon spheres, is made
MCMS)。
In some embodiments, the preparation method of the MCMS includes:
Configuration pH value is 7.0-8.5 phosphate buffer solution；
Dopamine is added in phosphate buffer solution, is stirred under dark condition, filters, drying, gained is poly- DOPA
Amine microballoon；
Poly-dopamine microballoon is placed in the heating rate in tube furnace with 5-10 DEG C and is warming up to 800-850 DEG C and in 800-
850 DEG C of holding 120-180min, gained is mesoporous carbon spheres.
In some embodiments, the input amount 1g:100mL-10g of the dopamine and the phosphate buffer solution:
100mL。
In some embodiments, the mixing time is 24-48h, and the drying temperature is 45-55 DEG C, drying time
For 24-48h.
In some embodiments, the preparation method of the PEG/MCMS includes:
Mesoporous carbon spheres are placed in vacuum environment, and polyglycol solution is added, 4-8h is stirred at a temperature of 65-80 DEG C；
Then it dries, obtains phase change composite material.
In some embodiments, the solvent in the polyglycol solution is ethyl alcohol, the input amount of the PEG and ethyl alcohol
The ratio between be 2g:1000mL-2g:100mL.
In some embodiments, the mass ratio of the polyethylene glycol in the polyglycol solution and the MCMS are 4:1-
3:2, preferably 7:3.
In some embodiments, 1-3h is stirred under vacuum, by heating water bath to stirring 4- at a temperature of 65-85 DEG C
8h, then place it in 45-60 DEG C of thermostatic drying chamber and dry 24-48h to ethyl alcohol evaporating completely.
It has the advantage that: the invention patent synthesizes poly-dopamine micron particles using bionic method, poly-dopamine is micro-
Rice grain is pyrolyzed to obtain novel MCMS, and shapes by the carrier preparation NEW TYPE OF COMPOSITE that thermal conductivity is good, enthalpy of phase change is high of this MCMS
Phase-change material, preparation method have many advantages, such as easy to operate, mild condition, nonhazardous.
The present invention synthesizes poly-dopamine micron particles by bionic method, poly-dopamine micron particles is pyrolyzed to obtain novel
MCMS, and using its as carrier prepare NEW TYPE OF COMPOSITE shaping phase-change material, this novel MCMS is for easy to operate, condition temperature
The advantages that with nonhazardous.The NEW TYPE OF COMPOSITE shaping phase-change material of preparation has the advantages such as thermal conductivity is good, enthalpy of phase change is high.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) photo of the mesoporous carbon spheres MCMS used in the embodiment of the present invention 1；
Fig. 2 is the SEM photograph of 1 obtained phase change composite material (PEG/MCMS) of the embodiment of the present invention；
Fig. 3 is Fu of pure PEG, mesoporous carbon spheres MCMS and phase change composite material PEG/Dop-SBA15 in the embodiment of the present invention 1
In leaf infrared spectrogram；
Fig. 4 is that the wide-angle X of pure PEG, mesoporous carbon spheres MCMS and phase change composite material PEG/MCMS in the embodiment of the present invention 1 are penetrated
Ray diffraction diagram spectrum；
Fig. 5 is the phase-change material PEG/ of pure PEG and phase change composite material PEG/MCMS in the embodiment of the present invention 1, comparative example
The differential scanning calorimetry change curve map of Dop-SBA15；
Fig. 6 is pure PEG in present example 1, is obtained with the poly-dopamine microballoon not being pyrolyzed directly as the fixed PEG of carrier
The phase-change material of phase-change material (PEG/PDAMS), phase-change material (PEG/MCMS) obtained in embodiment 1 thermal conductivity comparison
Figure.
Specific embodiment
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned attached drawing.
The preparation method of phase change composite material provided by the invention will be described further below.
A kind of preparation method of carbon ball base composite phase-change material comprising dopamine following steps: is put into phosphoric acid
It is stirred in buffer solution, obtains poly-dopamine microballoon；Poly-dopamine microballoon, which is placed in tube furnace, to be pyrolyzed, and mesoporous carbon spheres are obtained
(MCMS)；The hole of the mesoporous carbon spheres is for loading subsequent polyethylene glycol.Using polyethylene glycol as core material, with the MCMS
As carrier, by the hydrogen bond action between polyethylene glycol and dopamine, and realize polyethylene glycol is immobilized in the mesoporous carbon
In the hole of ball, carbon-based composite phase-change material (PE) is made.
The preparation method of the MCMS includes: that configuration pH value is 7.0-8.5 phosphate buffer solution；In phosphate buffer solution
Dopamine is added, 24-48h is stirred under dark condition, filters, drying.Gained is poly-dopamine microballoon；Poly-dopamine is micro-
The heating rate that ball is placed in tube furnace with 5-10 DEG C is warming up to 800-850 DEG C and in 800-850 DEG C of holding 120-180min, institute
It must be mesoporous carbon spheres.Wherein, the input amount 1g:100mL-10g:100mL of the dopamine and the phosphate buffer solution.Institute
State drying temperature be 45-55 DEG C, drying time 24-48h.
The preparation method of the PE includes: mesoporous carbon spheres to be placed in vacuum environment, and polyglycol solution is added, in 65-
4-8h is stirred at a temperature of 80 DEG C；Then it dries, obtains phase change composite material.Wherein, by polyglycol solution and mesoporous carbon spheres
It is first placed in the purpose stirred under vacuum environment to be, diffuses to polyglycol solution rapidly in the hole of mesoporous carbon spheres and fills
It is full, make to form stronger hydrogen bond action between amino and catechol group in polyethylene glycol and dopamine.And then in
It is stirred under normal pressure, the obtained phase change composite material is made to more tend to stablize.Wherein, the solvent in the polyglycol solution is second
The ratio between input amount of alcohol, the PEG and ethyl alcohol is 2g:1000mL-2g:100mL.Poly- second two in the polyglycol solution
Alcohol and mesoporous carbosphere/copper microballoon mass ratio are 4:1-3:2, preferably 7:3.Stir 1-3h under vacuum, by water-bath plus
Heat is to stirring 4-8h at a temperature of 65-85 DEG C, then to place it in dry 24-48h in 45-60 DEG C of thermostatic drying chamber complete to ethyl alcohol
Evaporation.
Compared with prior art, in the preparation method of phase change composite material provided by the invention, mesoporous carbon spheres are first prepared,
Then again by polyethylene glycol by in dopamine amino and catechol functional group formed hydrogen bond and it is immobilized in mesoporous carbon
In the hole of ball, phase change composite material is obtained.In the preparation method, prepare mesoporous carbon spheres process and immobilized polyethylene glycol
Process does not use organic solvent, and without the operation such as flow back is carried out, low energy consumption, and without the toxic solvents such as toluene residual
In duct, secondary pollution not will form, nonhazardous, in addition modifying process is simple, the period is short, mild condition, and at low cost.It should
Preparation method is suitble to large-scale industrial production.
In the obtained phase change composite material, polyethylene glycol passes through as core material, mesoporous carbon spheres as carrier, polyethylene glycol
Hydrogenbond is formed between the amino and catechol group in dopamine, enhances its effect between mesoporous carbon spheres
Power, thus the crystallization behavior of polyethylene glycol can be regulated and controled, the enthalpy of phase change of the final obtained phase change composite material, thermal conductivity and
Biggish raising can be obtained in thermal stability, and can prevent polyethylene glycol liquid phase from leaking.
Hereinafter, will further illustrate in conjunction with specific embodiments.
Embodiment 1
The preparation of poly-dopamine micron particles
In beaker, the dopamine of 0.5g is dissolved in the phosphate buffer solution of reaction medium pH most 7.0 of 50mL,
And continue to stir, it reacts under dark condition and room temperature (25 DEG C) and is filtered afterwards for 24 hours, obtained dark precipitate object is dried
Dry, drying temperature is 45 DEG C, drying time is for 24 hours, to obtain the poly-dopamine micron particles of black powder.
It is pyrolyzed poly-dopamine micron particles
Poly-dopamine micron particles are placed in tube furnace, are risen under the protection of nitrogen with the heating rate of 5 DEG C/min
800 DEG C, and in 800 DEG C of holding 120min, the product finally obtained is New Type of Mesoporous carbon ball (MCMS).
The preparation of NEW TYPE OF COMPOSITE shaping phase-change material
With polyethylene glycol (PEG) for core material, NEW TYPE OF COMPOSITE fixed phase change material is prepared as carrier using the poly-dopamine after being pyrolyzed
Material, the specific steps are as follows: 0.35gPEG is dissolved in 15ml ethyl alcohol, it is poly- more after 0.15g pyrolysis is added after it is completely dissolved
Bar amine, and the suspension is stirred into 1h under vacuum conditions；Then 4h will be stirred at a temperature of 65 DEG C of this suspension heating water bath；
After by mixture be placed in 45 DEG C of thermostatic drying chambers it is dry for 24 hours, make ethyl alcohol evaporating completely, the solid product finally obtained is i.e.
For NEW TYPE OF COMPOSITE shaping phase-change material (PEG/MCMS).
The mesoporous carbon spheres MCMS and composite phase-change material PEG/MCMS that embodiment 1 is obtained carry out following characterization, as a result see
Fig. 1-Fig. 5.By Fig. 1 and Fig. 2 as it can be seen that PEG success is combined to together with through the modified mesoporous carbon spheres MCMS of dopamine.It can by Fig. 3
See, compares the curve corresponding to phase change composite material and the curve corresponding to mesoporous carbon spheres, corresponding to the curve of pure PEG, it can
See, apparent new peak is not observed in the curve of phase change composite material, this illustrates that the interaction of PEG and MCMS is physics
, and this interaction can prevent phase change composite material from revealing in phase transition process.From fig. 4, it can be seen that pure PEG exists
Two strong diffraction maximums are shown at 19.13 ° and 23.47 °, this shows the highly crystalline structure of pure PEG material.And phase transformation is compound
The diffraction maximum position of material PEG/MCMS material is substantially identical as pure PEG material, this illustrates that the introducing of mesoporous material does not influence
The crystal structure of PEG, the i.e. crystallinity without influencing PEG.As seen from Figure 5, pure PEG shows endothermic fusion peak at 65.24 DEG C,
Melting enthalpy is 190.2J/g, shows that exothermic crystallization peak, solidification enthalpy are 175.2J/g at 35.20 DEG C.And 1 phase transformation of embodiment is compound
Material PEG/MCMS shows that endothermic fusion peak, melting enthalpy 112.08J/g show heat release knot at 36.78 DEG C at 62.19 DEG C
Brilliant peak, solidification enthalpy are 107.34J/g.As it can be seen that 3 phase change composite material PEG/MCMS heat enthalpy value with higher of embodiment, this is said
It is bright to prepare shaping phase-change material using mesoporous carbon spheres MCMS for the fixed PEG of carrier, it can not only be sent out in phase transition process to avoid PEG
Raw leakage, and will not influence the thermal storage performance of PEG.As seen from Figure 6, the thermal conductivity of pure PEG is 0.251；It is poly- with what is be not pyrolyzed
Dopamine microballoon is 0.288 directly as the phase-change material of the obtained phase-change material (PEG/PDAMS) of the fixed PEG of carrier；Implement
The thermal conductivity of phase-change material obtained in example 1 (PEG/MCMS) is 0.304.
Embodiment 2
The preparation of poly-dopamine micron particles
In beaker, the dopamine of 0.5g is dissolved in the phosphate buffer solution of reaction medium pH most 8.5 of 25mL,
And continue to stir, it is filtered after reacting 36h under dark condition and room temperature (25 DEG C), obtained dark precipitate object is dried
Dry, drying temperature is 55 DEG C, drying time 36h, obtains the poly-dopamine micron particles of black powder.
It is pyrolyzed poly-dopamine micron particles
Poly-dopamine micron particles are placed in tube furnace, are risen under the protection of nitrogen with the heating rate of 5 DEG C/min
800 DEG C, and in 850 DEG C of holding 120min, the product finally obtained is New Type of Mesoporous carbon ball (MCMS).
The preparation of NEW TYPE OF COMPOSITE shaping phase-change material
With polyethylene glycol (PEG) for core material, NEW TYPE OF COMPOSITE fixed phase change material is prepared as carrier using the poly-dopamine after being pyrolyzed
Material, the specific steps are as follows: 0.35gPEG is dissolved in 20mL ethyl alcohol, the poly- DOPA after 0.2g pyrolysis is added after it is completely dissolved
Amine, and the suspension is stirred into 2h under vacuum conditions；Then 8h will be stirred at a temperature of 65 DEG C of this suspension heating water bath；Knot
Mixture, which is placed in drying in 45 DEG C of thermostatic drying chambers, after beam for 24 hours, makes ethyl alcohol evaporating completely, the solid product finally obtained is
NEW TYPE OF COMPOSITE shaping phase-change material (PEG/MCMS).
Embodiment 3
The preparation of poly-dopamine micron particles
In beaker, the dopamine of 0.5g is dissolved in the phosphate buffer solution of reaction medium pH most 8.0 of 50mL,
And continue to stir, it is filtered after reacting 48h under dark condition and room temperature (25 DEG C), obtained dark precipitate object is dried
Dry, drying temperature is 45 DEG C, drying time 48h, obtains the poly-dopamine micron particles of black powder.
It is pyrolyzed poly-dopamine micron particles
Poly-dopamine micron particles are placed in tube furnace, are risen under the protection of nitrogen with the heating rate of 5 DEG C/min
800 DEG C, and in 800 DEG C of holding 180min, the product finally obtained is New Type of Mesoporous carbon ball (MCMS).
The preparation of NEW TYPE OF COMPOSITE shaping phase-change material
With polyethylene glycol (PEG) for core material, NEW TYPE OF COMPOSITE fixed phase change material is prepared as carrier using the poly-dopamine after being pyrolyzed
Material, the specific steps are as follows: 0.35gPEG is dissolved in 35ml ethyl alcohol, the poly- DOPA after 0.1g pyrolysis is added after it is completely dissolved
Amine, and the suspension is stirred into 3h under vacuum conditions；Then 6h will be stirred at a temperature of 75 DEG C of this suspension heating water bath；Knot
Mixture is placed in 45 DEG C of thermostatic drying chambers dry 48h after beam, makes ethyl alcohol evaporating completely, the solid product finally obtained is
NEW TYPE OF COMPOSITE shaping phase-change material (PEG/MCMS).
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of carbon ball base composite phase-change material comprising following steps:
Dopamine is put into phosphate buffer solution and is stirred, poly-dopamine microballoon is obtained；
The poly-dopamine microballoon is placed in tube furnace and is pyrolyzed, mesoporous carbon spheres (MCMS) is obtained；
Using polyethylene glycol (PEG) as core material, using the MCMS as carrier, pass through the hydrogen bond between polyethylene glycol and dopamine
Effect, and realize polyethylene glycol is immobilized in carbon-based composite phase-change material (PEG/MCMS) in the hole of the MCMS, is made.
2. the preparation method of carbon-based composite phase-change material according to claim 1, which is characterized in that the preparation of the MCMS
Method includes:
Configuration pH value is 7.0-8.5 phosphate buffer solution；
Dopamine is added in phosphate buffer solution, is stirred under dark condition, filters, drying, gained is that poly-dopamine is micro-
Ball；
Poly-dopamine microballoon is placed in the heating rate in tube furnace with 5-10 DEG C and is warming up to 800-850 DEG C and at 800-850 DEG C
120-180min is kept, gained is mesoporous carbon spheres.
3. the preparation method of carbon-based composite phase-change material according to claim 2, which is characterized in that the dopamine and institute
State the input amount 1g:100mL-10g:100mL of phosphate buffer solution.
4. the preparation method of carbon-based composite phase-change material according to claim 2, which is characterized in that the mixing time is
24-48h, the drying temperature is 45-55 DEG C, drying time 24-48h.
5. the preparation method of carbon-based composite phase-change material according to claim 1, which is characterized in that
The preparation method of the PEG/MCMS includes:
Mesoporous carbon spheres are placed in vacuum environment, and polyglycol solution is added, 4-8h is stirred at a temperature of 65-80 DEG C；Then
It is dry, obtain phase change composite material.
6. the preparation method of carbon-based composite phase-change material according to claim 5, which is characterized in that the polyethylene glycol is molten
Solvent in liquid is ethyl alcohol, and the ratio between the PEG and the input amount of ethyl alcohol are 2g:1000mL-2g:100mL.
7. the preparation method of carbon-based composite phase-change material according to claim 5, which is characterized in that the polyethylene glycol is molten
The mass ratio of polyethylene glycol and the MCMS in liquid is 4:1-3:2, preferably 7:3.
8. the preparation method of carbon-based composite phase-change material according to claim 5, which is characterized in that stir 1- under vacuum
3h by heating water bath to stirring 4-8h at a temperature of 65-85 DEG C, then places it in dry 24- in 45-60 DEG C of thermostatic drying chamber
48h is to ethyl alcohol evaporating completely.
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| CN111394067A (en) * | 2020-05-09 | 2020-07-10 | 中国科学院化学研究所 | Metal fluoride high-temperature phase change energy storage microcapsule and preparation method and application thereof |
| CN113789158A (en) * | 2021-10-21 | 2021-12-14 | 中国矿业大学 | Preparation method of waste plastic modified and shaped phase-change material heat storage working medium |
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Application publication date: 20191008 |