CN105950121B - A kind of intelligent adjustable phase-change material and preparation method thereof of Nano capsule - Google Patents
A kind of intelligent adjustable phase-change material and preparation method thereof of Nano capsule Download PDFInfo
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Abstract
The invention discloses a kind of intelligent adjustable phase-change materials and preparation method thereof of Nano capsule.The material is using organic phase change material as core, and the carbon nanotube (CNTs) crossed through nitric acid treatment is shell, and benzene and dehydrated alcohol are solvent, prepares Nano capsule intelligently adjustable phase-change material by self-diffusion under vacuum state, the internal diameter of capsule is 20~50 nm.The partial size of the capsule is smaller, has biggish specific surface area, can further improve heat conduction efficiency, and reduce destruction of the biggish volume change of phase transition process to capsule structure, improve stability.It selects a series of organic phase change material of different molecular weights to be filled into carbon nanotube, controls the loading of organic phase change material, it is intelligently adjustable to realize phase transition temperature, while guaranteeing that phase-change material is not revealed in storage/exothermic process.Using the high latent heat of phase change and CNTs high thermal conductivity characteristic of organic phase change material, intelligently adjustable phase-change material is widely used in the fields such as solar energy storage, industrial afterheat recovery, microelectronic device cooling and power-saving technology to the Nano capsule of preparation.
Description
Technical field
The present invention relates to phase-change material technical field, more particularly to a kind of Nano capsule intelligently adjustable phase-change material and its
Preparation method.
Background technique
In the research of phase-change material (PCM) it can be seen that have researcher by phase-changing energy storage material be wrapped in other materials it
In, form capsule PCM.According to the size of capsule, capsule PCM can be divided into three classes: large capsule (1 millimeter or more)；Microcapsules
(0-1000 microns)；Nano capsule (0-1000 nanometers).PCM, which is encapsulated, is isolated it with ambient enviroment in the application,
Sufficiently can have the advantages that latent heat of phase change using it, and avoid other as corrosivity, flammability, soluble, volatile etc. no
The feature of benefit.For organic phase-change material, although most of all do not have corrosivity, substantially thermally conductive coefficient is all very
It is low, it is easy to be detached from wall surface after the volume change of multiple phase transition process and influence using effect in application.Select nanometer
The available small size of encapsulated PCM, bigger serface and high thermal conduction rate etc. are very beneficial for the spy of heat transfer
Point.
The thermal coefficient of carbon nanotube (CNTs) is very high, generally 2000-6000Wm-1K-1, while being also equipped with open circles
The special property such as rod structure receives researcher in recent years and widely pays close attention to.Material is filled into carbon nanotube, is needed
Want its surface tension lower than 200mNm-1, such as water, polymer and paraffin meets this condition.According to institute in application
The operating temperature needed can choose the organic phase-change material of different phase transition temperatures, so that the corresponding phase transformation for managing interior packing material
Property has certain adjustability.
Carbon nano-tube filled technology develops very rapid.It studies earlier, is to fusing metal, salt or oxide
Filling.Later, there is the research much for water-soluble liquid stream and organic blended object filling carbon nano-pipe.Last decade has researcher sharp
Carbon nanotube has been filled into pressure and thermodynamic-driven water.These researchs are all gradually pushing filling technique in carbon nanotube
Development.Hereafter, carbon nanotube inner stuffing is gradually extended to the organic matters such as polymer and paraffin, can be applied to phase transformation neck
Domain.If high latent heat of phase change and application of the carbon nanotube high thermal conductivity characteristic for phase-change material of organic phase change material can be utilized
Have very important significance, but related filling experimental study is also only in the primary exploratory experiment stage, how to prepare compared with
The nano capsule phase change material of high stability and higher compactedness will become the research hotspot of special application field.
Summary of the invention
Based on the above issues, the present invention provides a kind of higher stability and the Nano capsule of higher compactedness intelligently can phase modulation
Become material.Further, a kind of preparation method of the intelligent adjustable phase-change material of Nano capsule is provided.
A kind of intelligent adjustable phase-change material of Nano capsule, intelligently adjustable phase-change material is with organic phase-change to the Nano capsule
Material is core, and carbon nanotube is the Nano capsule of shell, and the internal diameter of the Nano capsule is 20~50 nm.
In one or more embodiments of the invention, the organic phase change material is that phase transition temperature is 53~55 DEG C
Stearic one kind that lauric acid that paraffin, phase transition temperature are 41~45 DEG C, phase transition temperature are 55~60 DEG C.
In one or more embodiments of the invention, the carbon nano pipe purity > 95wt%, outer diameter 30-60nm are interior
Diameter 20-50nm, length are 1-10 μm.
A kind of preparation method of the intelligent adjustable phase-change material of Nano capsule, includes the following steps:
A, organic phase change material, solvent are 1:4 mixing in mass ratio, obtain organic phase change material-solvent mixture；
B, ultrasonic under 1000~1500 revs/min of mixing speed by the mixture oil bath heating to 60~80 DEG C
Vibration 10 minutes is clarified until solution becomes；
C, by acid, treated that carbon nanotube is added in aryballos, 80 DEG C of oil bath heatings, by vacuum pump by aryballos
In air and carbon nanotube in air take away, keep aryballos in vacuum time be 10-20 minutes；
D, organic phase change material-solvent mixture is added in aryballos, 80 DEG C of oil bath heating vacuum self-diffusion reactions
30 minutes, isolate and purify to obtain Nano capsule intelligently adjustable phase-change material, the Nano capsule intelligently adjustable phase-change material be with
Organic phase change material is core, and carbon nanotube is the Nano capsule of shell, and the internal diameter of the Nano capsule is 20~50 nm.
In one or more embodiments of the invention, the solvent is respectively one kind of benzene and dehydrated alcohol.
In one or more embodiments of the invention, the organic phase change material-solvent mixture be paraffin/benzene,
Lauric acid/dehydrated alcohol, stearic acid/benzene one kind.
In one or more embodiments of the invention, the acidification step of the carbon nanotube is into concentrated nitric acid
Carbon nanotube is added, flows back 4 hours for 120 DEG C in magnetic agitation heater, is filtered with 0.22 μm of teflon membrane filter,
And be washed with distilled water after neutral, it is 24 hours dry in 60 DEG C of drying boxes.
In one or more embodiments of the invention, described the step of isolating and purifying are as follows: after reaction, to 80
DEG C reaction solution be added hot solvent wash 2-3 time, 0.22 μm of teflon membrane filter of the mixed liquor after washing is filtered, dry
After obtain Nano capsule intelligently adjustable phase-change material.
In one or more embodiments of the invention, the hot solvent is respectively one kind of benzene and dehydrated alcohol.
In one or more embodiments of the invention, the step of the drying is to be dried in vacuo 2 hours at 40 DEG C.
Beneficial effects of the present invention: the preparation method that the present invention provides the intelligent adjustable phase-change material of Nano capsule is with organic
Phase-change material is core, and the carbon nanotube (CNTs) crossed through nitric acid treatment is shell, and benzene and dehydrated alcohol are solvent, is led under vacuum state
It crosses self-diffusion and prepares Nano capsule intelligently adjustable phase-change material, the internal diameter of capsule is 20~50 nm.The partial size of the capsule is smaller,
With biggish specific surface area, heat conduction efficiency can further improve, and reduce the biggish volume change of phase transition process to capsule
Structural damage improves stability.It selects a series of organic phase change material of different molecular weights to be filled into carbon nanotube, controls
It is intelligently adjustable to realize phase transition temperature for the loading of organic phase change material processed, while guaranteeing phase-change material in storage/exothermic process
It does not reveal.Using the high latent heat of phase change and carbon nanotube high thermal conductivity characteristic of organic phase change material, the Nano capsule of preparation intelligently may be used
Phase-change material is adjusted to be widely used in the fields such as solar energy storage, industrial afterheat recovery, microelectronic device cooling and power-saving technology.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) figure of carbon nanotube after acid processing in embodiment；
Fig. 2 is transmission electron microscope (TEM) figure of carbon nanotube after acid processing in embodiment；
Fig. 3 is transmission electron microscope (TEM) figure of the intelligent adjustable phase-change material of 1 Nano capsule of embodiment；
Fig. 4 is transmission electron microscope (TEM) figure of the intelligent adjustable phase-change material of 1 Nano capsule of embodiment；
Fig. 5 is transmission electron microscope (TEM) figure of the intelligent adjustable phase-change material of 1 Nano capsule of embodiment；
Fig. 6 is differential scanning calorimetry (DSC) figure of the intelligent adjustable phase-change material of 1 Nano capsule of embodiment；
Fig. 7 is differential scanning calorimetry (DSC) figure of 1 paraffin refined wax of embodiment；
Fig. 8 is differential scanning calorimetry (DSC) figure of the intelligent adjustable phase-change material of 2 Nano capsule of embodiment；
Fig. 9 is embodiment 2 lauric differential scanning calorimetry (DSC) figure；
Figure 10 is differential scanning calorimetry (DSC) figure of the intelligent adjustable phase-change material of 3 Nano capsule of embodiment；
Figure 11 is embodiment 3 stearic differential scanning calorimetry (DSC) figure.
Specific embodiment
Further explanation is made to the present invention combined with specific embodiments below.
The acidification of carbon nanotube is as follows in the embodiment:
3.0g carbon nanotube is added in 400 mL concentrated nitric acids, 120 DEG C of reflux 4 are small in magnetic agitation heater
When, it is filtered with 0.22 μm of teflon membrane filter, and be washed with distilled water after neutral, dry 24 in 60 DEG C of drying boxes
Hour.
It as depicted in figs. 1 and 2, is all opening through peracid treated carbon nanotube, so that liquid organic phase becomes material
It is quickly filled in carbon nanotube.Arrow 1 indicate open end, arrow 2 indicate inside be it is empty, arrow 3 indicates that there is corrosion in inside.
A kind of preparation method of the intelligent adjustable phase-change material of Nano capsule, includes the following steps:
Paraffin and benzene are that 1:4 is mixed to get mixture in mass ratio, by the mixture oil bath heating to 60~80 DEG C,
Ultrasonic vibration 10 minutes under 1000~1500 revs/min of mixing speed are clarified until solution becomes；
By acid, treated that carbon nanotube is added in aryballos, and 80 DEG C of oil bath heatings will be in aryballos by vacuum pump
Air and carbon nanotube in air take away, keep aryballos in vacuum time be 10-20 minutes；
Paraffin-benzol mixture is added in aryballos, 80 DEG C of oil bath heating vacuum self-diffusions are reacted 30 minutes, reaction
After, benzene is added to 80 DEG C of reaction solutions and washs 2-3 times, by 0.22 μm of teflon membrane filter of the mixed liquor after washing
It filters, Nano capsule intelligently adjustable phase-change material is obtained after being dried in vacuo 2 hours at 40 DEG C.
Paraffin filling carbon nano-pipe Nano capsule manufactured in the present embodiment intelligently adjustable phase-change material internal diameter be 20~50
Nm, the TEM under different multiples are imaged as shown in Fig. 3, Fig. 4 and Fig. 5, and arrow indicates the paraffin of filling in carbon nanotube.
As shown in Figure 6 and Figure 7, it is tested through DSC, the above-mentioned Nano capsule being prepared intelligently adjustable phase-change material and paraffin
Latent heat be respectively 20.12 Jg-1With 123.9 Jg-1, according to latent heat of phase change value, can calculate and be filled in carbon nanotube
The mass fraction of middle paraffin is 16.24%.After 500 cold cyclings, the latent heat of the intelligent adjustable phase-change material of Nano capsule
18.26Jg can still be maintained-1, illustrate that the thermal stability of the intelligent adjustable phase-change material of the Nano capsule is higher.
A kind of preparation method of the intelligent adjustable phase-change material of Nano capsule, includes the following steps:
Lauric acid and dehydrated alcohol are that 1:4 is mixed to get mixture in mass ratio, by the mixture oil bath heating to 60
~80 DEG C, ultrasonic vibration 10 minutes under 1000~1500 revs/min of mixing speed are clarified until solution becomes；
By acid, treated that carbon nanotube is added in aryballos, and 80 DEG C of oil bath heatings will be in aryballos by vacuum pump
Air and carbon nanotube in air take away, keep aryballos in vacuum time be 10-20 minutes；
Lauric acid-dehydrated alcohol mixture is added in aryballos, 80 DEG C of oil bath heating vacuum self-diffusions react 30 points
Clock is added dehydrated alcohol to 80 DEG C of reaction solutions and washs 2-3 times after reaction, and the mixed liquor after washing is poly- with 0.22 μm
Tetrafluoroethene filter membrane filters, and Nano capsule intelligently adjustable phase-change material is obtained after being dried in vacuo 2 hours at 40 DEG C.
As shown in Figure 8 and Figure 9, it is tested through DSC, the above-mentioned Nano capsule being prepared intelligently adjustable phase-change material and laurel
The latent heat of acid is respectively 16.78 Jg-1With 198.2 Jg-1, according to latent heat of phase change value, can be calculated by and be filled in carbon and receive
The mass fraction of paraffin is 8.47% in mitron.After 500 cold cyclings, the intelligent adjustable phase-change material of Nano capsule
Latent heat can still maintain 15.38Jg-1, illustrate that the thermal stability of the intelligent adjustable phase-change material of the Nano capsule is higher.
Embodiment 3
A kind of preparation method of the intelligent adjustable phase-change material of Nano capsule, includes the following steps:
Stearic acid and benzene are that 1:4 is mixed to get mixture in mass ratio, by the mixture oil bath heating to 60~80 DEG C,
Ultrasonic vibration 10 minutes under 1000~1500 revs/min of mixing speed are clarified until solution becomes；
By acid, treated that carbon nanotube is added in aryballos, and 80 DEG C of oil bath heatings will be in aryballos by vacuum pump
Air and carbon nanotube in air take away, keep aryballos in vacuum time be 10-20 minutes；
Stearic acid-benzol mixture is added in aryballos, 80 DEG C of oil bath heating vacuum self-diffusions are reacted 30 minutes, reaction
After, benzene is added to 80 DEG C of reaction solutions and washs 2-3 times, by 0.22 μm of teflon membrane filter of the mixed liquor after washing
It filters, Nano capsule intelligently adjustable phase-change material is obtained after being dried in vacuo 2 hours at 40 DEG C.
As shown in Figure 10 and Figure 11, it is tested through DSC, the intelligent adjustable phase-change material and hard of the above-mentioned Nano capsule being prepared
The latent heat of resin acid is respectively 55.94 Jg-1And 216.3Jg-1, according to latent heat of phase change value, can be calculated by and be filled in carbon
The mass fraction of paraffin is 25.86% in nanotube.After 500 cold cyclings, the intelligent adjustable phase-change material of Nano capsule
Latent heat can still maintain 53.85Jg-1, illustrate that the thermal stability of the intelligent adjustable phase-change material of the Nano capsule is higher.
It is that above-mentioned preferred embodiment should be regarded as application scheme embodiment for example, all with application scheme thunder
Same, approximate or technology deduction, replacement, improvement for making based on this etc., are regarded as the protection scope of this patent.
Claims (7)
1. a kind of preparation method of the intelligent adjustable phase-change material of Nano capsule, which is characterized in that the Nano capsule is intelligently adjustable
Phase-change material is using organic phase change material as core, and carbon nanotube is the Nano capsule of shell, the internal diameter of the Nano capsule is 20~
50nm, the organic phase change material is the phase transition temperature lauric acid that is 41~45 DEG C, phase transition temperature is 55~60 DEG C of stearic acid
One kind；Carbon nano pipe purity > the 95wt%, 30~60nm of outer diameter, 20~50nm of internal diameter, length are 1~10 μm；It is prepared
Method includes the following steps:
A, organic phase change material, solvent are 1:4 mixing in mass ratio, obtain organic phase change material-solvent mixture；
B, by the mixture oil bath heating to 60~80 DEG C, the ultrasonic vibration under 1000~1500 revs/min of mixing speed
It 10 minutes, is clarified until solution becomes；
C, by acid, treated that carbon nanotube is added in aryballos, and 80 DEG C of oil bath heatings will be in aryballos by vacuum pump
Air in air and carbon nanotube is taken away, and keeping the vacuum time in aryballos is 10~20 minutes；
D, organic phase change material-solvent mixture is added in aryballos, 80 DEG C of oil bath heating vacuum self-diffusions react 30 points
Clock isolates and purifies to obtain Nano capsule intelligently adjustable phase-change material.
2. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 1, which is characterized in that described molten
Agent is one kind of benzene or dehydrated alcohol.
3. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 2, which is characterized in that the matter
Amount is lauric acid/dehydrated alcohol, stearic acid/benzene one kind than being 1:4 organic phase change material-solvent mixture.
4. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 1, which is characterized in that the carbon
The acidification step of nanotube is that carbon nanotube is added into concentrated nitric acid, and 120 DEG C of reflux 4 are small in magnetic agitation heater
When, it is filtered with 0.22 μm of teflon membrane filter, and be washed with distilled water until dry 24 is small in 60 DEG C of drying boxes after neutral
When.
5. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 1, which is characterized in that described point
The step of from purifying are as follows: after reaction, hot solvent is added to 80 DEG C of reaction solutions and washs 2~3 times, by the mixed liquor after washing
It is filtered with 0.22 μm of teflon membrane filter, obtains Nano capsule intelligently adjustable phase-change material after dry.
6. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 5, which is characterized in that the heat
Solvent is one kind of benzene or dehydrated alcohol.
7. the preparation method of the intelligent adjustable phase-change material of Nano capsule according to claim 5, which is characterized in that described dry
Dry step is to be dried in vacuo 2 hours at 40 DEG C.
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| CN106701029A (en) * | 2016-12-06 | 2017-05-24 | 太仓大唐化纤厂 | Phase-changing temperature-adjusting fiber and preparation method of phase-changing temperature-adjusting microcapsule |
| CN108251063B (en) * | 2016-12-28 | 2021-05-11 | 有研工程技术研究院有限公司 | High-performance composite phase-change material and preparation method thereof |
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