CN103131395A - Paraffin-graphite foam composite shape-stabilized phase change material and preparation method thereof - Google Patents
Paraffin-graphite foam composite shape-stabilized phase change material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a composite shape-stabilized phase change material and a preparation method of the material. The composition of the material comprises 60 wt% to 72 wt% of paraffin, 7 wt% to 9 wt% of high density polyethylene, 3 wt% to 4 wt% of styrene butadiene styrene block copolymer (SEBS) and 15 wt% to 30 wt% of graphite foam, wherein the paraffin is packaged in the graphite foam through the high density polyethylene and the SEBS. The method comprises: feed composition is weighed; the paraffin is heated and melted so that the temperature of the paraffin can reach to between 150 DEG C to 180 DEG C; the high density polyethylene and the SEBS are added to fluid paraffin, the fluid paraffin is stirred mechanically so that the fluid paraffin is dissolved evenly; the graphite foam is placed in a mold, obtained liquid mixture is poured to the graphite foam so as to fill the gaps of the graphite foam, and therefore the composite shape-stabilized phase change material is obtained after cooling. The composite shape-stabilized phase change material is capable of efficiently converting solar energy and electric energy to heat energy at the same time, the heat energy is stored in phase change materials, and the composite shape-stabilized phase change material is an optical-electric composite shape-stabilized phase change material.
Description
Technical field
The present invention relates to a kind of take paraffin as energy storage material, high density polyethylene(HDPE) (HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer (SEBS) are encapsulants, graphite foam has composite shape-setting phase-change material of excellent heat conductivity rate, extinction and conduction property and preparation method thereof for encapsulation setting skeleton.
Background technology
Phase change material is subject to extensive concern as a kind of thermal energy storage material of clean and effective, and it has broad application prospects at aspects such as sun power utilization, building energy conservation, power peak regulations.The paraffin class phase change material due to adjustable transformation temperature, larger latent heat of phase change, the advantages such as cold-peace is separated without crossing, good cycle, cost is low and reserves are abundant are widely used, but the encapsulation problem after melted paraffin wax and the low thermal conductivity of paraffin have limited the further use of paraffin.
At present, utilize the technology of polymer melting mixing packaging phase change material to receive publicity because its packaging effect is good.Inaba etc. (Heat and transfer, 1997,32,307) are the pioneers of this encapsulation technology, and the high density polyethylene(HDPE) hybrid package that begun one's study fusing point is the paraffin of 54 ℃, and has studied its thermophysical property in great detail, and wherein the content of paraffin is 74%.The people such as Xia Dingguo are in patent CN1635044A, further developed this encapsulation technology, use high density polyethylene(HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer (SEBS) encapsulation paraffin, simultaneously add wherein expanded graphite, utilize the vesicular structure of expanded graphite to improve packaging effect and utilize the high heat conductance of expanded graphite to strengthen the heat conductivility of composite shape-setting phase-change material.But due to expanded graphite be discontinuous existence in composite shape-setting phase-change material, so composite shape-setting phase-change material integral body is not possess conduction property, this has also weakened the application of composite shape-setting phase-change material in power peak regulation.
Summary of the invention
The purpose of this invention is to provide a kind of paraffin-graphite foam composite shape-setting phase-change material and preparation method thereof, do not need container encloses, and have simultaneously good heat conductivility, photo absorption performance and conductivity, sun power and electric energy can be converted into thermal energy storage efficiently in phase change material.
Its composition of composite shape-setting phase-change material of the present invention is that massfraction is the paraffin of 60%-72%, the high density polyethylene(HDPE) of 7%-9% (HDPE), the graphite foam of polystyrene-poly ethene-polybutene of 3%-4%-polystyrene block copolymer (SEBS) and 15%-30%, wherein paraffin is packaged in graphite foam by high density polyethylene(HDPE) and SEBS.
The method of the above-mentioned composite shape-setting phase-change material of preparation that the present invention proposes comprises the following steps:
1) take feed composition, its massfraction is respectively: the paraffin of 60%-72%, the high density polyethylene(HDPE) of 7%-9% (HDPE), polystyrene-poly ethene-polybutene of 3%-4%-polystyrene block copolymer (SEBS), and the graphite foam of 15%-30%;
2) with the heating paraffin fusing, make its temperature reach 150-180 ℃;
3) high density polyethylene(HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer being joined step 2) in the gained liquid paraffin, mechanical stirring makes its uniform dissolution;
4) graphite foam is placed in mould, is cast in step 3) gained liquid form mixt on graphite foam and makes its hole that is full of graphite foam, obtain paraffin-graphite foam composite shape-setting phase-change material after cooling.
The described churned mechanically time is preferably 0.3-1 hour.
Described graphite foam prepares by prior art, its method is: phase, synthetic mesophase phase or coal tar mesophase pitch in the middle of petroleum asphalt based are added in reactor, be warming up to 260-400 ℃ with 1-5 ℃/min speed, pressurising 2-6Mpa, be warming up to 350-550 ℃ with 1-2 ℃/min speed again, constant temperature 15min-2 hour, the employing difference is cooling obtained bituminous froth with the venting mode; Be warming up to 950-1100 ℃, omnidistance nitrogen protection charing gets the charing bituminous froth; Be warming up to 2600-3000 ℃ again under argon shield and carry out greying, naturally cooling obtains high heat conducting foam material of graphite; Its aperture is 80-800 μ m, and density is 0.28-0.75g/cm
3
Characteristics of the present invention are, in graphite foam, graphite interconnects, so the composite shape-setting material has very high thermal conductivity, more than can reaching 100W/ (mK); Because graphite has good photo absorption performance, composite shape-setting phase-change material can absorb sunlight solar energy highly effective is converted into thermal energy storage in phase change material; Graphite due to three-dimensional communication makes composite shape-setting phase-change material have good conductivity simultaneously, is that thermal energy storage is in phase change material with the electric energy Efficient Conversion in the making alive situation.
The present invention adopts paraffin as heat accumulating, encapsulate paraffin by high density polyethylene(HDPE) (HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer (SEBS), reach the purpose that paraffin is not revealed, and adopt graphite foam as support frame, make phase change material have good heat conduction, extinction and conductivity, can be with sun power and luminous energy Efficient Conversion thermal energy storage in phase change material, can be widely used in building the fields such as temperature-controlling energy-saving, power peak regulation, sun power utilization, waste heat recovery.
Description of drawings
Fig. 1 is the macropore graphite foam photo of preparation in the embodiment of the present invention 1.
Fig. 2 is the aperture graphite foam photo of preparation in the embodiment of the present invention 2.
Fig. 3 is the electron micrograph of the X500 of the aperture graphite foam of preparation in the embodiment of the present invention 2.
Fig. 4 is the electron micrograph of the X150 of the aperture graphite foam of preparation in the embodiment of the present invention 2.
Fig. 5 is the heat flow curve of the differential scanning calorimeter of composite phase-change material in the embodiment of the present invention 1 and embodiment 2.
Fig. 6 is the temperature variation curve of composite shape-setting phase-change material sample under making alive of the embodiment of the present invention 1 preparation.
Fig. 7 is the temperature variation curve of composite shape-setting phase-change material sample under making alive of the embodiment of the present invention 2 preparations.
Embodiment
Below by specific embodiment, and coordinate accompanying drawing, the present invention is described in detail.
Embodiment 1:
Prepare graphite foam by prior art: phase, synthetic mesophase phase or coal tar mesophase pitch in the middle of petroleum asphalt based are added in reactor, being warming up to 260 ℃ with 1-5 ℃/min speed (can in 260-400 ℃ of scope, the present embodiment adopts 260 ℃), pressurising 2-6Mpa, being warming up to 350 ℃ with 1-2 ℃/min speed again (can in 350-550 ℃ of scope, the present embodiment adopts 350 ℃), constant temperature 15min-2 hour, then cooling and venting obtained bituminous froth; Be warming up to 950 ℃ (in 950-1100 ℃ of scopes can, the present embodiment adopts 950 ℃), omnidistance nitrogen protection charing gets the charing bituminous froth; Being warming up to 2600 ℃ under argon shield (can in 2600-3000 ℃ of scope again; 2600 ℃ of the present embodiment employings) carry out greying; naturally cooling; must arrive by adjusting cooling and deflation course the foam material of graphite that the aperture is about 600 μ m; its pattern photo as shown in Figure 1, electron micrograph is as shown in Figure 3 and Figure 4.
The heating paraffin of getting the 8.5g fusing point and be 35 ℃ melts and makes its temperature reach 150 ℃, then gets 1g high density polyethylene(HDPE) and 0.4gSEBS and joins in paraffin, and mechanical stirring makes its uniform dissolution half an hour.The 1.8g graphite foam is placed in mould, and then above-mentioned liquid form mixt being cast in and preparing the Quality of Paraffin Waxes mark on graphite foam is 72% paraffin-graphite foam composite shape-setting phase-change material.
As shown in Figure 5, the phase transformation starting temperature of using the French Setaram 131evo of company differential scanning calorimeter to record paraffin, high density polyethylene(HDPE) and SEBS matrix material is 32.8 ℃, and the phase transformation heat content is 102.8J/g.Due to the good heat conductivility of graphite foam, more than the thermal conductivity of composite shape-setting phase-change material can reach 100W/ (mK).Due to the graphite foam excellent conductive performance, electric energy can be converted into thermal energy storage efficiently in composite shape-setting phase-change material simultaneously.
Fig. 6 is the temperature variation curve according to composite shape-setting phase-change material sample under making alive of the present embodiment preparation.As can be seen from the figure, the flex point that heats up has appearred during at the phase change material fusing point at the heating curve of sample after the making alive of composite shape-setting phase-change material two ends, therefore electric energy conversion is heat energy and phase change material is melted, and this has illustrated that composite shape-setting phase-change material can be effectively that thermal energy storage is in phase change material with electric energy conversion.
Embodiment 2:
Prepare graphite foam by prior art: phase, synthetic mesophase phase or coal tar mesophase pitch in the middle of petroleum asphalt based are added in reactor, be warming up to 400 ℃ with 1-5 ℃/min speed, pressurising 2-6Mpa, heat up 550 ℃ with 1-2 ℃/min speed again, constant temperature 15min-2 hour, then cooling and venting obtained bituminous froth; Be warming up to 1100 ℃, omnidistance nitrogen protection charing gets the charing bituminous froth; Be warming up to 3000 ℃ again under argon shield and carry out greying, naturally cooling must arrive by adjusting cooling and deflation course the foam material of graphite that the aperture is about 200 μ m, its pattern photo as shown in Figure 2, electron micrograph is as shown in Figure 3 and Figure 4.
The heating paraffin of getting the 8.5g fusing point and be 35 ℃ melts and makes its temperature reach 180 ℃, then gets 1g high density polyethylene(HDPE) and 0.5gSEBS and joins in paraffin, and mechanical stirring makes its uniform dissolution half an hour.The 4.3g graphite foam is placed in mould, and then above-mentioned liquid form mixt being cast in and preparing the Quality of Paraffin Waxes mark on graphite foam is 60% paraffin-graphite foam composite shape-setting phase-change material.
As shown in Figure 5, the phase transformation starting temperature of using the French Setaram 131evo of company differential scanning calorimeter to record paraffin, high density polyethylene(HDPE) and SEBS matrix material is 32.8 ℃, and the phase transformation heat content is 102.8J/g.Due to the good heat conductivility of graphite foam, more than the thermal conductivity of composite shape-setting phase-change material can reach 100W/ (mK).Due to graphite foam good extinction and conductivity, sun power and electric energy can be converted into thermal energy storage efficiently in composite shape-setting phase-change material simultaneously.
Fig. 7 is the temperature variation curve according to composite shape-setting phase-change material sample under making alive of the present embodiment preparation.As can be seen from the figure, the flex point that heats up has appearred during at the phase change material fusing point at the heating curve of sample after the making alive of composite shape-setting phase-change material two ends, therefore electric energy conversion is heat energy and phase change material is melted, and this has illustrated that composite shape-setting phase-change material can be effectively that thermal energy storage is in phase change material with electric energy conversion.
Embodiment 3:
Prepare graphite foam by prior art: phase, synthetic mesophase phase or coal tar mesophase pitch in the middle of petroleum asphalt based are added in reactor, be warming up to 260 ℃ with 1-5 ℃/min speed, pressurising 2-6Mpa, be warming up to 350 ℃ with 1-2 ℃/min speed again, constant temperature 15min-2 hour, then cooling and venting obtained bituminous froth; Be warming up to 950 ℃, omnidistance nitrogen protection charing gets the charing bituminous froth; Be warming up to 2600 ℃ again under argon shield and carry out greying, naturally cooling must arrive by adjusting cooling and deflation course the foam material of graphite that the aperture is about 600 μ m, its pattern photo as shown in Figure 1, electron micrograph is as shown in Figure 3 and Figure 4.
The heating paraffin of getting the 8.5g fusing point and be 35 ℃ melts and makes its temperature reach 150 ℃, then gets 1g high density polyethylene(HDPE) and 0.5gSEBS and joins in paraffin, and mechanical stirring makes its uniform dissolution half an hour.The 2.9g graphite foam is placed in mould, and then above-mentioned liquid form mixt being cast in and preparing the Quality of Paraffin Waxes mark on graphite foam is 66% paraffin-graphite foam composite shape-setting phase-change material.
Above embodiment is only in order to technical scheme of the present invention to be described but not be limited; those of ordinary skill in the art can modify or be equal to replacement technical scheme of the present invention; and not breaking away from the spirit and scope of the present invention, protection scope of the present invention should be as the criterion so that claim is described.
Claims (8)
1. composite shape-setting phase-change material, it is characterized in that, its composition is the paraffin of 60-72wt%, the high density polyethylene(HDPE) of 7-9wt%, the graphite foam of polystyrene-poly ethene-polybutene of 3-4wt%-polystyrene block copolymer and 15-30wt%, wherein paraffin is packaged in graphite foam by high density polyethylene(HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer.
2. composite shape-setting phase-change material as claimed in claim 1, is characterized in that, the aperture of described graphite foam is 80-800 μ m, and density is 0.28-0.75g/cm
3
3. the preparation method of the described composite shape-setting phase-change material of claim 1, its step comprises:
1) take feed composition, be respectively: the paraffin of 60-72wt%, the high density polyethylene(HDPE) of 7-9wt%, polystyrene-poly ethene-polybutene of 3-4wt%-polystyrene block copolymer, and the graphite foam of 15-30wt%;
2) with the heating paraffin fusing, make its temperature reach 150 ~ 180 ℃;
3) high density polyethylene(HDPE) and polystyrene-poly ethene-polybutene-polystyrene block copolymer being joined step 2) in the gained liquid paraffin, mechanical stirring makes its uniform dissolution;
4) graphite foam is placed in mould, is cast in step 3) gained liquid form mixt on graphite foam and makes its hole that is full of graphite foam, obtain paraffin-graphite foam composite shape-setting phase-change material after cooling.
4. preparation method as claimed in claim 3, it is characterized in that, the preparation method of described graphite foam is: phase, synthetic mesophase phase or coal tar mesophase pitch in the middle of petroleum asphalt based are added in reactor, be warming up to 260-400 ℃ with 1-5 ℃/min speed, pressurising 2-6Mpa, be warming up to 350-550 ℃ with 1-2 ℃/min speed again, constant temperature 15min-2 hour, the employing difference is cooling obtained bituminous froth with the venting mode; Be warming up to 950-1100 ℃, omnidistance nitrogen protection charing gets the charing bituminous froth; Be warming up to 2600-3000 ℃ again under argon shield and carry out greying, obtain high heat conducting foam material of graphite after naturally cooling.
5. preparation method as claimed in claim 3, is characterized in that, the aperture of described graphite foam is 80-800 μ m, and density is 0.28-0.75g/cm
3
6. preparation method as claimed in claim 3, is characterized in that, the described churned mechanically time is 0.3-1 hour.
The described composite shape-setting phase-change material of claim 1 be used for converting solar energy into heat energy and with thermal energy storage in this composite shape-setting phase-change material.
The described composite shape-setting phase-change material of claim 1 be used for electric energy conversion be heat energy and with thermal energy storage in this composite shape-setting phase-change material.
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Cited By (17)
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| CN104371666A (en) * | 2014-12-04 | 2015-02-25 | 西南科技大学 | Preparation method of high-thermal-conductivity low-leakage phase-change composite |
| CN104893672A (en) * | 2015-05-21 | 2015-09-09 | 沈阳建筑大学 | High-density polyethylene/paraffin composite phase-change material and preparation method thereof |
| CN104893674A (en) * | 2015-06-03 | 2015-09-09 | 中国科学院空间应用工程与技术中心 | Foamy carbon/paraffin type phase-change composite material and encapsulation method thereof |
| CN106501221A (en) * | 2016-10-09 | 2017-03-15 | 东北石油大学 | A kind of experimental provision of the measurement solar energy transmissison characteristic of glass structure containing olefin material |
| CN106905927A (en) * | 2015-12-23 | 2017-06-30 | 上海邦中高分子材料有限公司 | A kind of composite shape-setting phase-change material and preparation method |
| CN107383662A (en) * | 2017-09-01 | 2017-11-24 | 重庆卡美伦科技有限公司合川分公司 | A kind of energy-saving heat preserving polrvinyl benzene composite board material and preparation method thereof |
| CN108531140A (en) * | 2018-05-31 | 2018-09-14 | 华中科技大学 | A kind of preparation method of paraffinic base sizing phase change plate |
| CN109489278A (en) * | 2018-11-22 | 2019-03-19 | 湖南省农村科技发展中心 | Grapheme foam/paraffin wax phase change energy storage material production solar water heater water tank |
| CN110305635A (en) * | 2019-07-19 | 2019-10-08 | 天津工业大学 | A kind of forming heat accumulating and preparation method thereof |
| CN110336097A (en) * | 2019-06-05 | 2019-10-15 | 华南理工大学 | A kind of cascaded structure battery heating system based on electric heating composite phase-change material |
| CN111117575A (en) * | 2019-12-31 | 2020-05-08 | 中国电子科技集团公司第三十八研究所 | Modification method of phase change energy storage material |
| CN112063370A (en) * | 2020-08-31 | 2020-12-11 | 华南理工大学 | Self-repairing composite phase change material with enhanced heat conduction and preparation method and application thereof |
| CN112351650A (en) * | 2020-10-30 | 2021-02-09 | 西南电子技术研究所（中国电子科技集团公司第十研究所） | Design method of missile-borne transient thermal control electronic module composite phase change cold plate |
| CN113105871A (en) * | 2021-04-09 | 2021-07-13 | 中国科学院山西煤炭化学研究所 | Phase-change heat storage material with bionic structure and preparation method and application thereof |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113667459A (en) * | 2021-08-31 | 2021-11-19 | 华南理工大学 | Electric heating flexible composite phase change material, preparation method thereof and application of electric heating flexible composite phase change material as thermal therapy product |
| CN114316913A (en) * | 2021-10-26 | 2022-04-12 | 江苏大学 | Organic composite phase-change heat storage material and preparation method thereof |
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| CN104371666A (en) * | 2014-12-04 | 2015-02-25 | 西南科技大学 | Preparation method of high-thermal-conductivity low-leakage phase-change composite |
| CN104893672A (en) * | 2015-05-21 | 2015-09-09 | 沈阳建筑大学 | High-density polyethylene/paraffin composite phase-change material and preparation method thereof |
| CN104893674A (en) * | 2015-06-03 | 2015-09-09 | 中国科学院空间应用工程与技术中心 | Foamy carbon/paraffin type phase-change composite material and encapsulation method thereof |
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| CN106905927A (en) * | 2015-12-23 | 2017-06-30 | 上海邦中高分子材料有限公司 | A kind of composite shape-setting phase-change material and preparation method |
| CN106501221A (en) * | 2016-10-09 | 2017-03-15 | 东北石油大学 | A kind of experimental provision of the measurement solar energy transmissison characteristic of glass structure containing olefin material |
| CN106501221B (en) * | 2016-10-09 | 2019-07-02 | 东北石油大学 | A kind of experimental provision measuring the solar energy of glass structure containing olefin material transmissison characteristic |
| CN107383662A (en) * | 2017-09-01 | 2017-11-24 | 重庆卡美伦科技有限公司合川分公司 | A kind of energy-saving heat preserving polrvinyl benzene composite board material and preparation method thereof |
| CN108531140A (en) * | 2018-05-31 | 2018-09-14 | 华中科技大学 | A kind of preparation method of paraffinic base sizing phase change plate |
| CN109489278A (en) * | 2018-11-22 | 2019-03-19 | 湖南省农村科技发展中心 | Grapheme foam/paraffin wax phase change energy storage material production solar water heater water tank |
| CN110336097B (en) * | 2019-06-05 | 2022-10-25 | 华南理工大学 | Series structure battery heating system based on electric heating composite phase change material |
| CN110336097A (en) * | 2019-06-05 | 2019-10-15 | 华南理工大学 | A kind of cascaded structure battery heating system based on electric heating composite phase-change material |
| CN110305635A (en) * | 2019-07-19 | 2019-10-08 | 天津工业大学 | A kind of forming heat accumulating and preparation method thereof |
| CN111117575A (en) * | 2019-12-31 | 2020-05-08 | 中国电子科技集团公司第三十八研究所 | Modification method of phase change energy storage material |
| CN112063370A (en) * | 2020-08-31 | 2020-12-11 | 华南理工大学 | Self-repairing composite phase change material with enhanced heat conduction and preparation method and application thereof |
| CN112351650A (en) * | 2020-10-30 | 2021-02-09 | 西南电子技术研究所（中国电子科技集团公司第十研究所） | Design method of missile-borne transient thermal control electronic module composite phase change cold plate |
| CN113105871A (en) * | 2021-04-09 | 2021-07-13 | 中国科学院山西煤炭化学研究所 | Phase-change heat storage material with bionic structure and preparation method and application thereof |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113667459A (en) * | 2021-08-31 | 2021-11-19 | 华南理工大学 | Electric heating flexible composite phase change material, preparation method thereof and application of electric heating flexible composite phase change material as thermal therapy product |
| CN114316913A (en) * | 2021-10-26 | 2022-04-12 | 江苏大学 | Organic composite phase-change heat storage material and preparation method thereof |
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