CN106753261A - A kind of microencapsulated phase change material and preparation method thereof - Google Patents
A kind of microencapsulated phase change material and preparation method thereof Download PDFInfo
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- 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
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Abstract
The invention provides a kind of microencapsulated phase change material, core is wrapped up, wall material is provided with the outside of described core, aluminum nanoparticles and graphite nano-particles are contained in described core and wall material.Present invention also offers a kind of preparation method of microencapsulated phase change material, including one the step of weigh core and wall material；One the step of prepare aluminum nanoparticles and graphite nano-particles mixture；The step of one determination Nanocomposites amount；One the step of prepare core composite solution；The step of one the first wall material composite solution of preparation；The step of one microcapsules is molded；The dry step of one microcapsules washing.The present invention by improving three kinds of characteristics simultaneously to clad aluminum and graphite nano-particles are added in core and wall material, i.e. the density of regulation microencapsulated phase change material particle, raising thermal conductivity factor, reduction degree of supercooling, obtain the microencapsulated phase change material of a kind of high density, high thermal conductivity coefficient, low degree of supercooling, clad aluminum and graphite nano-particles.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of phase-change material, in particular to a kind of microcapsule phase-change material
Material and preparation method thereof.
Background technology
Microencapsulated phase change material particle refers to that phase-change material is encapsulated in into densification and with one by Micro-Encapsulation Technique
Novel materials particle in the high molecular polymer shell of fixed elasticity, its particle diameter generally in the range of 1 μm -1000 μm, has been reported
Road can accomplish smaller particle diameter.Phase-change microcapsule suspension is then that the microencapsulated phase change material particle that will be prepared is scattered in list
Phase fluid（Such as water, conduction oil）The suspension of middle formation.
Microcapsules technology research starts from the thirties in last century, and be attended by the most momentous results the fifties.In whole evolution
In, the research in the U.S. is constantly in leading position, and Japan also gradually has caught up with the 60-70 ages.
The preparation method of microencapsulated phase change material substantially res divisibiles logos, polymerisation method, phase separation method three major types.Physics
Method is, by the physical change of microcapsule wall material, microencapsulation to be carried out using certain mechanical processing toolses, mainly has spraying dry
Dry method.For polymerisation method, can according to microencapsulation when prepare that raw material used by wall material is different, the difference of polymerization methodses,
It is divided into situ aggregation method, interfacial polymerization and suspensoid cross method.Phase separation rule is the physicochemical properties for utilizing polymer, i.e.,
The property of phase separation, so being also called physical-chemical process, mainly there is Simple coacervation, complex coacervation.In microencapsulated phase change material
In preparation, frequently with method have situ aggregation method, interfacial polymerization, spray drying process and complex coacervation.
1st, situ aggregation method.
Situ aggregation method be will be formed wall material monomer and initiator be all scattered in PCMs emulsion droplets inside or
, there is polymerisation in outside, monomer is solvable in continuous phase, and the polymer of generation is insoluble, is covered in drop in droplet surface
Surface coating forms microcapsules.Situ aggregation method applies more when phase-change microcapsule is prepared, and its key is the polymer to be formed
How to precipitate and be coated on the surface of core.
2nd, interfacial polymerization.
Interfacial polymerization is two kinds of different activities monomers containing double (many) functional groups, is dissolved in respectively not miscible
In dispersed phase and continuous phase, core is dissolved in dispersion phase solvent, two kinds of polymerization reaction monomers are respectively from inside two-phase to emulsification
The Interface Moving of drop, and polycondensation reaction is carried out on two-phase interface rapidly, core is wrapped up, form microcapsules.
3rd, spray drying process.
Spray drying process is a kind of physical method.Phase-change material micro-capsule is prepared with spray drying process, is first had to core
Material is dispersed in wall material solution, is then atomized this mixed liquor in high temperature gas flow, the solvent of dissolving wall material is evaporated rapidly,
So that wall material solidifies and is coated on core.Spray drying process is suitable to the microencapsulation of lipophile liquid material, and core is dredged
Aqueous stronger, embedding effect is better.
4th, complex coacervation.
Complex coacervation refers to do wall material by two or more macromolecular materials with opposite charges, and core is dispersed in into wall
In material solution, under proper condition（Such as change ph values or temperature）So that there is electrostatic interaction between the polymer of opposite charges.Band
After the macromolecular material of opposite charges interacts, solution solubility is reduced and produces phase separation, and cohesion forms microcapsules.
Microencapsulated phase change material particle above has many good qualities in application:
（1）The temperature difference is adjusted as construction material, the comfort level that people live indoors is improved.
（2）The clothes of cold and hot regulatory function are made as textile material additive.
（3）Recyclable waste heat, improves energy utilization rate.
（4）Microencapsulated phase change material particle is made the refrigerating of suspension（Heat）Ability is stronger than water, can be used for augmentation of heat transfer Jie
Matter and heat accumulating.
Microencapsulated phase change material possesses the outstanding advantages of the above, has very wide application in using energy source and field of heat exchange
Prospect.As heat transfer medium, it can apply to the therrmodynamic systems such as Aero-Space, electronics, central air-conditioning, chemical industry, power plant, cooling
System and heat exchanger, as heat-storing material it can apply to the fields such as central air-conditioning, Solar use storage it is cold/heat accumulation system
System.Microencapsulated Phase Change Material Suspension storage density is high, there is application potential higher in terms of solar energy heat-storage, is conducive to economy to build
If, social development, expand renewable energy utilization rate.
But the microencapsulated phase change material particle applied in the market, still suffers from certain defect, receive its practical application
To certain limitation, defect is as follows：
（1）Because the density of microencapsulated phase change material particle is big with water difference, suspension as energy storage is configured to by base fluid of water
Easily it is layered during the material of material or augmentation of heat transfer, physical stability is poor.
（2）Because the preparing raw material of existing microencapsulated phase change material particle is generally paraffin, high-molecular organic material etc., lead
Hot coefficient is smaller, limits its application in terms of augmentation of heat transfer.
（3）Due to solidification（Liquid is changed into solid）Temperature is less than melting（Solid is changed into liquid）Temperature, it may appear that supercooling is existing
As.This can be such that latent heat is discharged within the scope of the temperature of lower temperature or bigger, be unfavorable for the storage of energy.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of microencapsulated phase change material and its preparation side
It is steady that method, described this microencapsulated phase change material and preparation method thereof will solve microencapsulated phase change material particle of the prior art
Qualitative difference, poor thermal conductivity, energy are unfavorable for the technical problem of storage.
The invention provides a kind of microencapsulated phase change material, including core, wall material, institute are provided with the outside of described core
Contain aluminum nanoparticles and graphite nano-particles in the core and wall material stated.
The invention provides a kind of preparation method of microencapsulated phase change material, comprise the following steps：
1）One the step of weigh core and wall material, be 2-5 according to core wall mass ratio:1 weighs core and wall material, wherein wall material by
Two kinds of material compositions of first wall material and the second wall material, its mass ratio is 1:1；Add water dissolves standby second wall material；
2）One the step of weigh composite nanoparticle, described composite nanoparticle is by aluminum nanoparticles and graphite nano-particles
Mix, be any mass ratio between described aluminum nanoparticles and graphite nano-particles, described composite nanoparticle
Quality is the 3%-5% of core wall gross mass；
3）One the step of prepare core composite solution, by step 2）In aluminum nanoparticles pressed with graphite nano-particles mixture
According to step 1）Middle identical core wall mass ratio 2-5:1 is divided into two parts, by aluminum nanoparticles of the core with 2-5 parts and Nano graphite grain
Sub- mixture mixing, adds the water of meltage, and core composite solution is obtained using ultrasonic processor dispersion；
4）One prepare the first wall material composite solution the step of, take step 1) in the first wall material, step 3）Middle residual Al nanoparticle
Son mixes with graphite nano-particles mixture, adds the water of meltage, and obtaining the first wall material using ultrasonic processor dispersion is combined
Solution；
5）The step of one microcapsules is molded, by step 3）In core composite solution be added to step 4）In the first wall material answer
Close in solution, constant temperature high speed shearing emulsification is continuously added the aqueous solution of the second wall material in emulsion process, first adjusted using first kind PH
Section agent adjusts pH value to 4.0-4.5, cooling cohesion, then adds crosslinking agent, then using Equations of The Second Kind PH conditioning agents adjust pH value to
9-11, rises warm hardening；
6）The dry step of one microcapsules washing, by the solution natural cooling in 4), treats that particle is precipitated, and filtering supernatant is right
Precipitation carries out filtering and washing, dries, and obtains microencapsulated phase change material.
Further, the core is selected from n-octadecane, aliphatic hydrocarbon, paraffin, aliphatic acid, fatty acid ester etc..
Further, first wall material is any one in gelatin or Arabic gum.
Further, second wall material is any one in Arabic gum or gelatin.
Further, the first kind PH conditioning agents are sulfuric acid, hydrochloric acid, citric acid etc..
Further, the crosslinking agent is formaldehyde, glutaraldehyde, tannic acid etc..
Further, the Equations of The Second Kind PH conditioning agents are NaOH, calcium hydroxide, ammoniacal liquor etc..
The present invention by be combined two kinds of nano-particles of material, while improving three kinds of characteristics.
(1) density of microencapsulated phase change material particle of the present invention is changed by two kinds of nano-particles being combined.Existing micro- glue
The density of capsule phase-change material particle can be adjusted by the 3rd class material of introducing and the 4th class material.Determine to add by calculating
Enter amount, the density of microencapsulated phase change material particle can be made same or like with required base fluid density, so as to suppress microcapsules phase
Become material granule to be layered in base fluid, improve the physical stability of suspension.
(2) thermal conductivity factor of microencapsulated phase change material particle of the present invention can be changed by the two kinds of nano-particles for adding.
The thermal conductivity factor of existing microencapsulated phase change material particle is smaller, and the 3rd class material and the 4th class material thermal conductivity factor phase of introducing
To larger.The thermal conductivity factor of microencapsulated phase change material particle, enhanced heat exchange can be effectively improved.
(3) microencapsulated phase change material particle of the present invention, can be used as microcapsule phase-change because there is two kinds of additions of nano-particle
Core solidification in material granule（Liquid is changed into solid）When nucleator, so as to reduce degree of supercooling.
The present invention is compared with prior art, and its technological progress is significant.The present invention is added by core and wall material
Clad aluminum and graphite nano-particles to improve three kinds of characteristics simultaneously, that is, adjust the density of microencapsulated phase change material particle, raising and lead
Hot coefficient, reduction degree of supercooling, obtain the micro- of a kind of high density, high thermal conductivity coefficient, low degree of supercooling, clad aluminum and graphite nano-particles
Capsule phase change material.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of the microencapsulated phase change material particle prepared using the present invention.Wherein：1st, wall material；2nd, core
Material；3rd, aluminum nanoparticles；4th, graphite nano-particles.
Specific embodiment
Below in conjunction with the accompanying drawings, the present invention is described in further detail：
Such as Fig. 1, a kind of microencapsulated phase change material of the invention, including core 2, the outside of described core 2 are provided with wall material 1,
Contain aluminum nanoparticles 3 and graphite nano-particles 4 in described wall material 1.
The invention provides three preparating examples of microencapsulated phase change material：
Embodiment 1
1）One the step of weigh core and wall material, be 2 according to core wall mass ratio:1 weighs core n-octadecane 40g and wall material
20g；Wherein wall material is by the first wall material gelatin 10g and the second wall material Arabic gum 10g；Add water dissolves standby in the second wall material
With；
2）The step of one determination Nanocomposites amount, it is total that the aluminum nanoparticles compound quantity total with graphite nano-particles accounts for core wall
The 3% of quality, i.e. 1.8g；
3）One the step of prepare aluminum nanoparticles and graphite nano-particles mixture, aluminum nanoparticles are pressed with graphite nano-particles
Mass ratio 1:1, take 0.9g aluminum nanoparticles 0.9g graphite nano-particles and obtain aluminum nanoparticles and graphite nano-particles mixture；
4）One the step of prepare core composite solution, coring material, 1.2g3）In aluminum nanoparticles and graphite nano-particles mix
Compound, core, part aluminum nanoparticles are mixed with graphite nano-particles mixture, add the water of meltage, at ultrasound
Reason device dispersion obtains core composite solution；
5）The step of one the first wall material composite solution of preparation, the first wall material, 3 in taking 1)）In remaining 0.6g aluminum nanoparticles
With graphite nano-particles mixture, by 3）Middle remaining aluminum nanoparticles and graphite nano-particles mixture are mixed with the first wall material
Close, add the water of meltage, the first wall material composite solution is obtained using ultrasonic processor dispersion；
6）The step of one microcapsules is molded, by 4）In core composite solution be added to 5）In the first wall material composite solution
In, constant temperature high speed shearing emulsification is continuously added the aqueous solution of the second wall material in emulsion process, first using citric acid adjust pH value to
Then 4.0-4.5, cooling cohesion adds crosslinking agent glutaraldehyde, then adjusts pH value to 9-11 using NaOH, rises warm hardening；
7）The dry step of one microcapsules washing, by the solution natural cooling in 4), treats that particle is precipitated, and filtering supernatant is right
Precipitation carries out filtering and washing, dries, and obtains microencapsulated phase change material.
Embodiment 2
1）One the step of weigh core and wall material, be 3 according to core wall mass ratio:1 weighs core paraffin 60g and wall material 20g；Its
Middle wall material is by the first wall material gelatin 10g and the second wall material Arabic gum 10g；Add water dissolves standby in the second wall material；
2）The step of one determination Nanocomposites amount, it is total that the aluminum nanoparticles compound quantity total with graphite nano-particles accounts for core wall
The 5% of quality, i.e. 4g；
3）One the step of prepare aluminum nanoparticles and graphite nano-particles mixture, aluminum nanoparticles are pressed with graphite nano-particles
Mass ratio 1:3, take 1g aluminum nanoparticles 3g graphite nano-particles and obtain aluminum nanoparticles and graphite nano-particles mixture；
4）One the step of prepare core composite solution, by core and 3g3）In aluminum nanoparticles mix with graphite nano-particles
Thing mixes, and adds the water of meltage, and core composite solution is obtained using ultrasonic processor dispersion；
5）One the step of prepare the first wall material composite solution, by the first wall material, 3 in 1)）In remaining 1g aluminum nanoparticles with
Graphite nano-particles mixture mixes, and adds the water of meltage, and the first wall material composite solution is obtained using ultrasonic processor dispersion；
6）The step of one microcapsules is molded, by 4）In core composite solution be added to 5）In the first wall material composite solution
In, constant temperature high speed shearing emulsification is continuously added the aqueous solution of the second wall material in emulsion process, first using hydrochloric acid adjust pH value to
Then 4.0-4.5, cooling cohesion adds crosslinking agent formaldehyde, then adjusts pH value to 9-11 using calcium hydroxide, rises warm hardening；
7）The dry step of one microcapsules washing, by the solution natural cooling in 4), treats that particle is precipitated, and filtering supernatant is right
Precipitation carries out filtering and washing, dries, and obtains microencapsulated phase change material.
Embodiment 3
1）One the step of weigh core and wall material, be 5 according to core wall mass ratio:1 weighs core hexadecane 50g and wall material
10g；Wherein wall material is by the first wall material gelatin 5g and the second wall material Arabic gum 5g；Add water dissolves standby in the second wall material；
2）The step of one determination Nanocomposites amount, it is total that the aluminum nanoparticles compound quantity total with graphite nano-particles accounts for core wall
The 5% of quality, i.e. 3g；
3）One the step of prepare aluminum nanoparticles and graphite nano-particles mixture, aluminum nanoparticles are pressed with graphite nano-particles
Mass ratio 2:1, take 2g aluminum nanoparticles 1g graphite nano-particles and obtain aluminum nanoparticles and graphite nano-particles mixture；
4）One the step of prepare core composite solution, by core and 2.5g3）In aluminum nanoparticles and graphite nano-particles mix
Compound mixes, and adds the water of meltage, and core composite solution is obtained using ultrasonic processor dispersion；
5）One the step of prepare the first wall material composite solution, by the first wall material, 3 in 1)）In remaining 0.5g aluminum nanoparticles
Mix with graphite nano-particles mixture, add meltage water, using ultrasonic processor dispersion obtain the first wall material be combined it is molten
Liquid；
6）The step of one microcapsules is molded, by 4）In core composite solution be added to 5）In the first wall material composite solution
In, constant temperature high speed shearing emulsification is continuously added the aqueous solution of the second wall material in emulsion process, first using sulfuric acid adjust pH value to
Then 4.0-4.5, cooling cohesion adds crosslinking agent tannic acid, then adjusts pH value to 9-11 using ammoniacal liquor, rises warm hardening；
7）The dry step of one microcapsules washing, by the solution natural cooling in 4), treats that particle is precipitated, and filtering supernatant is right
Precipitation carries out filtering and washing, dries, and obtains microencapsulated phase change material.
Claims (8)
1. a kind of microencapsulated phase change material, it is characterised in that：Parcel core, is provided with wall material on the outside of described core, described
Core and wall material in contain aluminum nanoparticles and graphite nano-particles.
2. the preparation method of a kind of microencapsulated phase change material described in claim 1, it is characterised in that comprise the following steps：
1）One the step of weigh core and wall material, be 2-5 according to core wall mass ratio:1 weighs core and wall material, wherein wall material by
Two kinds of material compositions of first wall material and the second wall material, its mass ratio is 1:1；Add water dissolves standby second wall material；
2）One the step of weigh composite nanoparticle, described composite nanoparticle is by aluminum nanoparticles and graphite nano-particles
Mix, be any mass ratio between described aluminum nanoparticles and graphite nano-particles, described composite nanoparticle
Quality is the 3%-5% of core wall gross mass；
3）One the step of prepare core composite solution, by step 2）In aluminum nanoparticles pressed with graphite nano-particles mixture
According to step 1）Middle identical core wall mass ratio 2-5:1 is divided into two parts, by aluminum nanoparticles of the core with 2-5 parts and Nano graphite grain
Sub- mixture mixing, adds the water of meltage, and core composite solution is obtained using ultrasonic processor dispersion；
4）One prepare the first wall material composite solution the step of, take step 1) in the first wall material, step 3）Middle residual Al nanoparticle
Son mixes with graphite nano-particles mixture, adds the water of meltage, and obtaining the first wall material using ultrasonic processor dispersion is combined
Solution；
5）The step of one microcapsules is molded, by step 3）In core composite solution be added to step 4）In the first wall material answer
Close in solution, constant temperature high speed shearing emulsification is continuously added the aqueous solution of the second wall material in emulsion process, first adjusted using first kind PH
Section agent adjusts pH value to 4.0-4.5, cooling cohesion, then adds crosslinking agent, then using Equations of The Second Kind PH conditioning agents adjust pH value to
9-11, rises warm hardening；
6）The dry step of one microcapsules washing, by the solution natural cooling in 4), treats that particle is precipitated, and filtering supernatant is right
Precipitation carries out filtering and washing, dries, and obtains microencapsulated phase change material.
3. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：Core is selected from positive ten
Eight alkane, aliphatic hydrocarbon, paraffin, aliphatic acid, fatty acid ester etc..
4. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：The first described wall
Material is any one in gelatin or Arabic gum.
5. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：The second described wall
Material is any one in Arabic gum or gelatin.
6. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：The first kind PH
Conditioning agent is sulfuric acid, hydrochloric acid or citric acid.
7. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：The crosslinking agent is
Formaldehyde, glutaraldehyde or tannic acid.
8. the preparation method of a kind of microencapsulated phase change material according to claim 2, it is characterised in that：The Equations of The Second Kind PH
Conditioning agent is NaOH, calcium hydroxide or ammoniacal liquor.
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| CN107384326A (en) * | 2017-07-25 | 2017-11-24 | 延安大学 | Gelatin chitosan nano silicon multinuclear microcapsules of storing energy through phase change preparation method |
| CN110777737A (en) * | 2019-10-16 | 2020-02-11 | 天津大学 | Anti-freezing core wall phase change clay for winter construction process and construction method thereof |
| WO2020127078A1 (en) | 2018-12-17 | 2020-06-25 | Saltx Technology Ab | Heat storage using phase change material coated with nanoparticles |
| CN113355054A (en) * | 2021-05-26 | 2021-09-07 | 中国地质大学（武汉） | Phase change energy storage microcapsule applied to inorganic cementing material and preparation method thereof |
| CN116063996A (en) * | 2023-04-03 | 2023-05-05 | 西南石油大学 | Phase-change heat storage microcapsule material suitable for cooling drilling fluid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107384326A (en) * | 2017-07-25 | 2017-11-24 | 延安大学 | Gelatin chitosan nano silicon multinuclear microcapsules of storing energy through phase change preparation method |
| CN107384326B (en) * | 2017-07-25 | 2020-08-04 | 延安大学 | Preparation method of gelatin chitosan-nano silicon dioxide multi-core phase change energy storage microcapsule |
| WO2020127078A1 (en) | 2018-12-17 | 2020-06-25 | Saltx Technology Ab | Heat storage using phase change material coated with nanoparticles |
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| CN110777737A (en) * | 2019-10-16 | 2020-02-11 | 天津大学 | Anti-freezing core wall phase change clay for winter construction process and construction method thereof |
| CN110777737B (en) * | 2019-10-16 | 2021-08-27 | 天津大学 | Anti-freezing core wall phase change clay for winter construction process and construction method thereof |
| CN113355054A (en) * | 2021-05-26 | 2021-09-07 | 中国地质大学（武汉） | Phase change energy storage microcapsule applied to inorganic cementing material and preparation method thereof |
| CN113355054B (en) * | 2021-05-26 | 2022-04-01 | 中国地质大学（武汉） | Phase change energy storage microcapsule applied to inorganic cementing material and preparation method thereof |
| CN116063996A (en) * | 2023-04-03 | 2023-05-05 | 西南石油大学 | Phase-change heat storage microcapsule material suitable for cooling drilling fluid and preparation method thereof |
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