CN109370535A - A kind of starch expanded graphite phase change composite material and preparation method thereof - Google Patents
A kind of starch expanded graphite phase change composite material and preparation method thereof Download PDFInfo
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- CN109370535A CN109370535A CN201811399851.2A CN201811399851A CN109370535A CN 109370535 A CN109370535 A CN 109370535A CN 201811399851 A CN201811399851 A CN 201811399851A CN 109370535 A CN109370535 A CN 109370535A
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- starch
- expanded graphite
- composite material
- phase change
- change composite
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
Abstract
The present invention relates to a kind of starch expanded graphite phase change composite materials and preparation method thereof, phase-change material, the microcapsules being wrapped in outside phase-change material including middle part and the particle being connected on microcapsules outer wall, phase-change material is paraffin, microcapsules are the mixture of modified starch and expanded graphite, particle includes starch granules and expanded graphite particles, and the mass fraction of expanded graphite is 5%~12% in microcapsules.Compared with prior art, the present invention has excellent heating conduction and structural stability, and with the increase of expanded graphite, the thermal coefficient of starch expanded graphite phase change composite material is gradually increased.
Description
Technical field
The present invention relates to energy storage and energy conversion techniques fields, and in particular to a kind of starch expanded graphite phase transformation composite wood
Material and preparation method thereof.
Background technique
Energy problem is the significant problem of 21 century facing mankind, and each aspect of human production life be unable to do without energy
Source.Meanwhile with the fast development of world economy, demand of the mankind to the energy is higher and higher.And the tellurian energy is limited
, it is increasingly of practical significance so heat-conserving energy-saving multi material just seems to the reasonable utilization and saving of the energy.Thermal energy storage system
Appearance, not only contribute to reduce the dependence to fossil fuel, and facilitate using efficient and benignly for the energy.It is at this
In system, thermal energy can be stored in a manner of sensible heat and latent heat.It is stored compared to sensible heat, material phase required for latent heat stores
It is smaller to volume.Therefore hidden heat energy storage receives more concerns.Latent heat heat accumulation is also known as phase-change thermal storage.Phase-change material is in phase transformation
Cheng Zhongneng absorbs and releases a large amount of latent heat of phase change, is widely used in thermal energy storage and domain of control temperature.By material property
Difference, phase-change material can be divided into inorganic phase-changing material and organic phase change material.Organic phase change material has high latent heat of phase change, mistake
It is cold to spend the advantages that small, without mutually separating, it is widely used, but there are small and easy leakages of thermal conductivity etc. to ask for organic phase change material
Topic.Nowadays different solutions has been proposed to overcome these problems.
For phase-change material leakage problem, solution is mostly to prepare phase-change material micro-capsule at present.Microcapsules are by phase transformation
Material package prevents the leakage of phase-change material.Dao and Jeong is the solution of 5% graphene using concentration, and it is hard to prepare graphene
Resin acid (SA) nucleocapsid composite micro-capsule.While thermal conductivity increases by 26% compared to SA, phase-change material leakage problem is changed significantly
It is kind.East etc. is coated in microcapsule composite material using graphene oxide as cyst wall, by paraffin phase change material is stable.Needle
The problem low to the thermal conductivity of phase-change material, most commonly used solution are to increase thermal conducting material.Such as metal powder, carbon materials
Material or inorganic material.In addition three dimentional heat conduction network structure is prepared, phase-change material is immersed in heat conduction network, it can also be effective
Raising phase-change material heating conduction.Finally, phase-change material it is high with thermal conductivity in the form of microcapsules porous material it is compound,
Also phase-change material thermal conductivity can be improved and achieve the purpose that further to encapsulate phase-change material.
The stability of the acquired microcapsule phase-change composite materials of many researchs be not very well, trace it to its cause may be because
More thin for microcapsules shell, during undergoing phase transition, the volume change as caused by solid-liquid transformation causes phase-change material
The rupture of microcapsule phase-change material shell.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of heating conduction and
Starch expanded graphite phase change composite material having good stability and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions: a kind of starch expanded graphite phase change composite material,
The phase change composite material includes the phase-change material at middle part, the microcapsules being wrapped in outside phase-change material and is connected to outside microcapsules
Particle on wall, the phase-change material are paraffin, and the microcapsules are the mixture of modified starch and expanded graphite, the particle
Including starch granules and expanded graphite particles, the mass fraction of expanded graphite is 5%~12% in the microcapsules.
The transformation of molecular structure can occur in boiling process for starch granules, and straight chain molecule therein spirals into spiral knot
Structure, polar lipid, which moves to, forms stable composite construction in straight chain molecule helical structure.Polar lipid is usually by polar head
With non-polar tail form, therefore this compound substance have it is amphiphilic, can be used as surfactant occur emulsification.Its
It is secondary, be added expanded graphite when, due to chemical structure similitude, composites of starch matter in the form of intermolecular force and expansion stone
Ink combines.When phase-change material is added, starch in expanded graphite conjugate together as microcapsules shell coating phase-change materials.
The main function of starch is that emulsification can occur in order to form amphiprotic substance, so as to form microcapsule structure.Expand stone
The addition of ink is primarily to improve the thermal conductivity of phase-change material.With the progress of reaction process, the remnants to suspend in water form sediment
Powder and expanded graphite accumulation to microcapsules shell to increase wall layer thickness, in this way since the stability of microcapsules more may be used
It leans on, also has great help to the thermal conductivity for increasing phase-change material.
The modified starch is the starch boiled.Starch granules is mainly by amylose, amylopectin and some polarity
Lipid composition, polar lipid are usually made of polar head and non-polar tail.During ebuillition of heated, in order to reduce surface
Can, amylose molecule spirals into helical structure, and polar lipid, which moves to, forms stable substance in amylose spiral.This
Kind of compound has amphiphilic, can be used as surfactant and emulsification occurs.Therefore amphipathic using the Starch formation boiled
Substance is easily formed microcapsules to play emulsification.
A kind of preparation method of starch expanded graphite phase change composite material as described above, comprising the following steps:
(1) in deionized water by starch dispersion, it heats and boils while magnetic agitation, obtain starch suspension；
(2) starch suspension is transferred in high-speed shearing machine, expanded graphite is then added, in the effect of high-speed shearing machine
Under be vigorously stirred, obtain mixing suspension；
(3) heating paraffin is melted, then the paraffin of melting is added in the mixing suspension obtained to step (2),
It is vigorously stirred under high-speed shearing machine effect, obtains crude samples；
(4) by crude samples filtering, dry, cooling to get the starch expanded graphite phase change composite material.
As previously mentioned, starch after boiling has amphiphilic, one has hydrophobicity, and one has hydrophily, in high speed
In shear history, hydrophobicity one end meeting coating phase-change materials form core-shell structure, and hydrophily one end is molten in water.With reaction
It carries out, expanded graphite can be supported on microcapsule shell layer surface to extra starch granules.
Preferably, temperature needed for the starch boiling is 90~100 DEG C, continues 10~20min after boiling.
Preferably, the mass ratio of starch is (0.4~0.06) in the expanded graphite and starch suspension: 1.
Preferably, the stirring rate of high-speed shearing machine described in step (2) is 8000~12000rpm, mixing time 10
~20min.
Preferably, the fusion temperature of the paraffin is 70~90 DEG C, and the melt paraffin of addition and the mass ratio of starch are (2
~18): 1.
Preferably, the stirring rate of high-speed shearing machine described in step (3) is 8000~12000rpm, mixing time 10
~20min.
Preferably, temperature dry described in step (4) is 30~40 DEG C, and the cooling carries out at room temperature.
The purpose that starch solution is boiled is to be conducive to that emulsification occurs, thus shape to form the amphiphilic substance of starch
At microcapsule structure.The purpose of high speed shear is to give maximum system energy, and quickening forms microcapsule structure.Dry purpose is
In order to remove micro moisture.
Compared with prior art, the beneficial effects of the present invention are embodied in following several respects:
(1) starch expanded graphite phase change composite material prepared by this technology has excellent thermal conductivity compared with phase-change material
Energy and structural stability；With the increase of expanded graphite, the thermal coefficient of starch expanded graphite phase change composite material is gradually increased；
The ratio of starch is also to gradually increase, and after increasing to certain numerical value, starch expanded graphite phase change composite material is in microcapsules ball
Shape plays good encapsulation to phase-change material.
(2) special starch expanded graphite phase change composite material is prepared for the first time, has widened the application of phase-change material significantly
Field.
Detailed description of the invention
Fig. 1 is the FTIR figure of starch, expanded graphite, paraffin and phase change composite material；
Fig. 2 is the SEM photograph of the starch expanded graphite phase change composite material of different amplification；
Fig. 3 is starch expanded graphite phase change composite material thermal conductivity figure.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Starch expanded graphite phase change composite material is mainly synthesized by the preparation of starch, expanded graphite and phase-change material.Originally it grinds
Study carefully the paraffin used to be provided by Sinopharm Chemical Reagent Co., Ltd., specification is that chemistry is pure, and 48-52 DEG C of fusing point, density is
0.86g/cm3.Unmodified food grade cornstarch is bought from Henan grace seedling food Co., Ltd.Expanded graphite (Expanded
Graphite, EG) it is provided by Baoding Lian Xing hard alloy Co., Ltd, expansion rate 150ml/g, average grain diameter before expanding
For 0.18mm.
Embodiment 1
(1) starch dispersion of 1g is weighed in 100ml deionized water, and constant temperature blender with magnetic force temperature is set in 90 DEG C.
Starch suspension is placed under magnetic stirring apparatus and is heated, after its boiling, continues to boil 15min.
(2) boiling starch suspension transfer is set under high-speed shearing machine.Then it is added immediately in boiling starch suspension
0.5-1g expanded graphite is vigorously stirred starch expanded graphite mixing suspension with 10000rpm revolving speed under high-speed shearing machine, stirs
Fully dispersed suspension is formed after 15min.
(3) 9g paraffin is placed in 70 DEG C of vacuum ovens and is heated, until fusing.
(4) melt paraffin is added in the suspension in (2), and violent with the revolving speed of 10000rpm under high-speed shearing machine
Stir 15min.
(5) by sample filtering, after removing its ionized water.It is placed in 35 DEG C of dryings in baking oven, solidification paraffin drop and makes starch
Consolidation.Through detecting, EG volume is 5% in this example.
Embodiment 2
(1) starch dispersion of 1g is weighed in 100ml deionized water, and constant temperature blender with magnetic force temperature is set in 90 DEG C.
Starch suspension is placed under magnetic stirring apparatus and is heated, after its boiling, continues to boil 15min.
(2) boiling starch suspension transfer is set under high-speed shearing machine.Then it is added immediately in boiling starch suspension
0.5g expanded graphite is vigorously stirred starch expanded graphite mixing suspension with 10000rpm revolving speed under high-speed shearing machine, stirs
Fully dispersed suspension is formed after 15min.
(3) 4.45g paraffin is placed in 70 DEG C of vacuum ovens and is heated, until fusing.
(4) melt paraffin is added in the suspension in (2), and violent with the revolving speed of 10000rpm under high-speed shearing machine
Stir 15min.
(5) by sample filtering, after removing its ionized water.It is placed in 35 DEG C of dryings in baking oven, solidification paraffin drop and makes starch
Consolidation.Through detecting, EG volume is 8.4% in this example.
The composite material that the present embodiment is prepared carries out electron-microscope scanning, and result is as shown in Fig. 2, we can from figure
With discovery, starch expanded graphite phase change composite material is in microencapsulated.
Embodiment 3
(1) starch dispersion of 1g is weighed in 100ml deionized water, and constant temperature blender with magnetic force temperature is set in 90 DEG C.
Starch suspension is placed under magnetic stirring apparatus and is heated, after its boiling, continues to boil 15min.
(2) boiling starch suspension transfer is set under high-speed shearing machine.Then it is added immediately in boiling starch suspension
0.5g expanded graphite is vigorously stirred starch expanded graphite mixing suspension with 10000rpm revolving speed under high-speed shearing machine, stirs
Fully dispersed suspension is formed after 15min.
(3) 2.97g paraffin is placed in 70 DEG C of vacuum ovens and is heated, until fusing.Starch, expanded graphite, paraffin and
The scanning electron microscope (SEM) photograph figure of phase change composite material is shown in Fig. 2.Figure A is the starch expanded graphite phase change composite material of dispersion, can
To find out particle in spherical, size is about 200 μm or so.Scheming B, C and D is compacting sample.Starch expanded graphite phase is shown in figure
Change composite material is in spherical or ellipsoid, and size distribution is more uniform, and size is about 200-300 μm.
(4) melt paraffin is added in the suspension in (2), and violent with the revolving speed of 10000rpm under high-speed shearing machine
Stir 15min.
(5) by sample filtering, after removing its ionized water.It is placed in 35 DEG C of dryings in baking oven, solidification paraffin drop and makes starch
Consolidation.Through detecting, EG volume is 11% in this example.
The starch expanded graphite phase change composite material that the present embodiment is obtained carries out FTIR spectrum detection, as a result such as
Shown in Fig. 1.For expanded graphite spectrum, 3435,1644 and 1082cm of absorption peak-1.The major absorbance peak of paraffin about 3435,
2959,1467 and 721cm-1Place, it is related with the vibration of-CH2 and-CH3 group respectively.In starch spectrum, 1163,1082 and
Bands of a spectrum at 1018cm-1 are related with C-O stretching, in 3435 and 1644cm-1The peak at place is attributed to-OH stretching and bending vibration.?
Typical paraffin and starch bands of a spectrum are observed in composite phase-change material, new peak do not occur, there is no displacement, tables for the position at peak
It is not chemically bonded between alum wax, starch and EG.
Comparative example 1
(1) starch dispersion of 1g is weighed in 100ml deionized water, and constant temperature blender with magnetic force temperature is set in 90 DEG C.
Starch suspension is placed under magnetic stirring apparatus and is heated, after its boiling, continues to boil 15min.
(2) boiling starch suspension transfer is set under high-speed shearing machine.Then it is added immediately in boiling starch suspension
0.5g expanded graphite is vigorously stirred starch expanded graphite mixing suspension with 10000rpm revolving speed under high-speed shearing machine, stirs
Fully dispersed suspension is formed after 15min.
(3) 17.86g paraffin is placed in 70 DEG C of vacuum ovens and is heated, until fusing.
(4) melt paraffin is added in the suspension in (2), and violent with the revolving speed of 10000rpm under high-speed shearing machine
Stir 15min.
(5) by sample filtering, after removing its ionized water.It is placed in 35 DEG C of dryings in baking oven, solidification paraffin drop and makes starch
Consolidation.Through detecting, EG volume is 2.6% in this example.
Examples 1 to 3, comparative example 1 are prepared into resulting composite material and pure phase-change material carries out thermal conductivity test,
As a result as shown in figure 3, wherein 0 thermal conductivity for representing pure phase-change material, from the figure we can see that, when expanded graphite volume is small
When 8.4ms%, with gradually increasing for expanded graphite volume, the thermal conductivity of phase change composite material is obviously gradually increased.When swollen
When swollen graphite volume is 8.4ms%, the thermal conductivity of phase change composite material is 0.607WK-1m-1, paraffin refined wax is compared, thermal conductivity increases
Add 190%.When expanded graphite volume is greater than 8.4ms%, the thermal conductivity speedup of phase change composite material is slow.When expanded graphite is mixed
When amount is 11ms%, the thermal conductivity of phase change composite material is 0.625WK-1m-1, thermal conductivity increase by 200%.
Claims (9)
1. a kind of starch expanded graphite phase change composite material, which is characterized in that the phase change composite material includes the phase transformation material at middle part
The microcapsules expect, being wrapped in outside phase-change material and the particle being connected on microcapsules outer wall, the phase-change material are paraffin,
The microcapsules are the mixture of modified starch and expanded graphite, and the particle includes starch granules and expanded graphite particles, institute
The mass fraction for stating expanded graphite in microcapsules is 5%~12%.
2. a kind of starch expanded graphite phase change composite material according to claim 1, which is characterized in that the modified shallow lake
Powder is the starch boiled.
3. a kind of preparation method of starch expanded graphite phase change composite material as claimed in claim 1 or 2, which is characterized in that packet
Include following steps:
(1) in deionized water by starch dispersion, it heats and boils while magnetic agitation, obtain starch suspension；
(2) starch suspension is transferred in high-speed shearing machine, expanded graphite is then added, it is acute under the action of high-speed shearing machine
Strong stirring, obtains mixing suspension；
(3) heating paraffin is melted, then the paraffin of melting is added in the mixing suspension obtained to step (2), in high speed
It is vigorously stirred under cutter effect, obtains crude samples；
(4) by crude samples filtering, dry, cooling to get the starch expanded graphite phase change composite material.
4. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that institute
Temperature needed for stating starch boiling is 90~100 DEG C, continues 10~20min after boiling.
5. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that institute
The mass ratio for stating starch in expanded graphite and starch suspension is (0.4~0.6): 1.
6. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that step
Suddenly the stirring rate of high-speed shearing machine described in (2) is 8000~12000rpm, and mixing time is 10~20min.
7. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that institute
The fusion temperature for stating paraffin is 70~90 DEG C, and the melt paraffin of addition and the mass ratio of starch are (2~18): 1.
8. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that step
Suddenly the stirring rate of high-speed shearing machine described in (3) is 8000~12000rpm, and mixing time is 10~20min.
9. a kind of preparation method of starch expanded graphite phase change composite material according to claim 3, which is characterized in that step
Suddenly temperature dry described in (4) is 30~40 DEG C, and the cooling carries out at room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111960411A (en) * | 2020-08-19 | 2020-11-20 | 浙江锂宸新材料科技有限公司 | Large-aperture graphite negative electrode material and preparation method thereof |
| CN114058228A (en) * | 2021-11-30 | 2022-02-18 | 德清绿能热电有限公司 | Heat-conducting coating, preparation method thereof, water pipe and boiler steam waste heat collecting system |
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| CN108048045A (en) * | 2017-11-28 | 2018-05-18 | 大连理工大学 | A kind of enhanced thermal conduction organic composite shaping phase-change material and preparation method thereof |
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2018
- 2018-11-22 CN CN201811399851.2A patent/CN109370535A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108048045A (en) * | 2017-11-28 | 2018-05-18 | 大连理工大学 | A kind of enhanced thermal conduction organic composite shaping phase-change material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| NUNO VITORINO，ET AL.: "《Highly conducting core–shell phase change materials for thermal regulation》", 《APPLIED THERMAL ENGINEERING》 * |
| 饶中浩等: "《储能技术概论》", 31 January 2017, 中国矿业大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111960411A (en) * | 2020-08-19 | 2020-11-20 | 浙江锂宸新材料科技有限公司 | Large-aperture graphite negative electrode material and preparation method thereof |
| CN114058228A (en) * | 2021-11-30 | 2022-02-18 | 德清绿能热电有限公司 | Heat-conducting coating, preparation method thereof, water pipe and boiler steam waste heat collecting system |
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