CN105199675A - Composite phase change material set by oxidized graphene and preparing method thereof - Google Patents
Composite phase change material set by oxidized graphene and preparing method thereof Download PDFInfo
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- CN105199675A CN105199675A CN201510592852.9A CN201510592852A CN105199675A CN 105199675 A CN105199675 A CN 105199675A CN 201510592852 A CN201510592852 A CN 201510592852A CN 105199675 A CN105199675 A CN 105199675A
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Abstract
The invention relates to a composite phase change material set by oxidized graphene and a preparing method thereof. The preparing method includes the following steps that oxidized graphene is ultrasonically dispersed in deionized water to prepare an oxidized graphene solution with certain concentration; the phase change material is ground into powder and added into the oxidized graphene solution, a microwave reactor is used for heating at the temperature higher than the melting point of the phase change material, and intense stirring is carried out along with heating to obtain a solution mixed evenly; the solution is put into a vacuum drying oven and dried to constant weight to obtain the composite phase change material. Compared with the prior art, the oxidized graphene is used as a supporting material, so that the composite phase change material has the setting effect, and the thermal property of the phase change material is improved. The composite phase change material has the advantages of being high in heat-conducting property, heat storage capacity and stability. The preparing method is easy to operate, short in synthesis time and low in cost.
Description
Technical field
The present invention relates to shaped composite phase-change material and preparation method thereof.Particularly, strengthen the phase change materials such as polyoxyethylene glycol using graphene oxide as propping material thus obtain a kind of graphene oxide sizing composite phase-change material.
Background technology
21 century, along with the fast development of economy, the environmental problem that the shortage of the energy and the burning of fossil oil cause has attracted a large amount of concern.Tap a new source of energy, improve efficiency of energy utilization, minimizing waste heat discharge becomes problem demanding prompt solution.Store and utilize thermal source to become the emphasis of research and development.
Phase change material is a kind of latent heat materials, and it absorbs or discharges a large amount of heats in the process undergone phase transition, and keeps the temperature of material self that too large change does not occur simultaneously.It can realize storage and the release of energy, is with a wide range of applications in space flight and aviation, building, intelligent temperature-regulation garment, refrigeration equipment and communication electric power etc.
Phase change material can be divided into according to phase transition process: solid-solid phase change material, solid-liquid phase change material, solids-gases phase change material, fluid-gas phase change material etc.Wherein, solid-liquid phase change material is because its high energy storage density and wide variety are studied widely.
Be suitable for as a kind of green, nontoxic, transformation temperature and high organic hydration (hydrophilic) the solid-liquid phase change material of energy storage capacity, polyoxyethylene glycol can be widely used in the application.But similar to other organic solid-liquid phase change material, polyoxyethylene glycol has the shortcoming that thermal conductivity is little, phase transition process can not be shaped, and brings obstruction to its practical application.
The matrix material that sizing phase-change material is made up of phase change material and propping material.Because propping material is to the restriction of phase change material and provide protection, phase change material also can keep original shape to reach the effect of sizing after being melted down.But generally propping material does not produce thermal change in phase change material phase transition process, so the unit heat content of composite phase-change material can be caused to reduce.For these problems, be generally propping material and the phase change material Homogeneous phase mixing of looking for a kind of good heat conductivity, improve its heat conductivility and ensure sizing simultaneously.
Graphene is a kind of Two-dimensional Carbon material arranged with polynuclear plane by monolayer carbon atom, because its quality is light, physical strength and hardness is large, good heat conductivity, is desirable propping material.Particularly the thermal conductivity of Graphene is up to 5000W/m*k, is the material that thermal conductivity is the highest in the world at present.But the natural hydrophobicity of Graphene and hardly by most of organic solvent dissolution, make it and phase change material be difficult to uniform mixing, this has a significant impact the performance of matrix material.The character of graphene oxide and Graphene basic simlarity, also have excellent calorifics and mechanical property.It is the product that the inner and edge of graphene sheet layer contains a large amount of hydrophilic oxygen-containing functional group (hydroxyl, carboxyl and epoxy group(ing) etc.) and modifies that the structure of graphene oxide can regard as.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist deficiency and a kind of graphene oxide shaped composite phase-change material and preparation method thereof is provided.
The present invention, using graphene oxide as a kind of propping material, utilizes microwave reactor to assist and graphene oxide is mixed uniformly with polyoxyethylene glycol, obtain shaped composite phase-change material.Wherein graphene oxide plays the effect of sizing and increased thermal conductivity energy simultaneously, and graphene oxide sheet interlayer spacing under microwave-assisted increases, and is conducive to better and phase change material Homogeneous phase mixing.The unit heat enthalpy value of this composite phase-change material PEG4 reaches 95.6% of pure polyoxyethylene glycol, and circulation 50 heat enthalpy value changes are later only 1.3%, prove the cyclical stability that composite phase-change material has had.It is easier and greatly raise the efficiency and save the advantage such as cost that the method for preparation has operation compared with traditional method.
The present invention can be realized by following technical scheme: a kind of graphene oxide shaped composite phase-change material and preparation method thereof, and described graphene oxide shaped composite phase-change material is prepared by following method:
(1) configure graphene oxide solution: graphene oxide powder is added in deionized water, ultrasonic and stir make it dispersed, be configured to graphene oxide solution;
(2) organic phase change material is joined in the graphene oxide solution of step (1) gained, and transfer in microwave reactor, heat with vigorous magnetic stirring under higher than organic phase change material melt temperature, obtain the solution be dispersed in deionized water;
(3) solution that step (2) obtains is put into vacuum drying oven and be dried to constant weight, obtain composite phase-change material.
In step (1), the concentration of the graphene oxide solution of preparation is 0.2mg/ml ~ 1mg/ml.
Described in step (2), organic phase change material is polyoxyethylene glycol, (number average molecular weight is 200 ~ 10000).
The consumption of organic phase change material and graphene oxide solution is to make the massfraction of graphene oxide in the composite phase-change material that obtains be 1% ~ 5%.
Ultrasonic in step (1) is 10-50 minute with churning time, and the magnetic agitation time described in step (2) is 1-10 minute.
The temperature that in step (2), heating is stirred with vigorous magnetic under higher than organic phase change material melt temperature is 70-100 DEG C.
The present invention has following advantage and positively effect:
1. the present invention adopts wetting ability graphene oxide as propping material, graphene oxide not only has the good heat conductivility similar to Graphene character, and surface is containing a large amount of functional groups, can and phase change material molecular chain between form hydrogen bond, be conducive to keep matrix material shape in phase transition process.
2. utilize microwave reaction to assist, the sheet interlayer spacing of graphene oxide improves greatly, is conducive to graphene oxide and mixes more uniformly with phase change material, to improve the thermal property of composite phase-change material.The performance of composite phase-change material can be regulated and controled by the add-on controlling propping material graphene oxide.
3. the building-up process of present method compared with prior art, easier, quick, energy-conservation, is convenient to large-scale production and application.Do not contain toxic substance in whole matrix material simultaneously, there is environment friendly.
Accompanying drawing explanation
Fig. 1 is building-up process schematic diagram;
Fig. 2 is schematic diagram of the present invention;
Fig. 3 is the infrared spectrogram of the composite phase-change material obtained in each embodiment;
Fig. 4 is the DSC figure of the composite phase-change material PEG1 obtained in embodiment 1;
Fig. 5 is the DSC figure of the composite phase-change material PEG2 obtained in embodiment 2;
Fig. 6 is the DSC figure of the composite phase-change material PEG3 obtained in embodiment 3;
Fig. 7 is the DSC figure of the composite phase-change material PEG4 obtained in embodiment 4;
Fig. 8 is the DSC figure of the composite phase-change material PEG5 obtained in embodiment 5.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.Be understandable that, concrete case study on implementation described herein is only for explaining the application, but not the restriction to the application.
Graphene oxide powder as shown in Figure 1, first adds in deionized water by the preparation process of graphene oxide shaped composite phase-change material of the present invention, ultrasonic and stir and make it dispersed in 10-50 minute, is configured to graphene oxide solution; Organic phase change material is joined in the graphene oxide solution of gained, and transfer in microwave reactor, heat with vigorous magnetic stirring 1-10 minute under higher than organic phase change material melt temperature (70-100 DEG C), obtain the solution be dispersed in deionized water; The solution obtained is put into vacuum drying oven and is dried to constant weight, compression molding obtains composite phase-change material sample.
As shown in Figure 2, the graphene oxide of sheet is after mixing with polyoxyethylene glycol (number average molecular weight is 200 ~ 10000), and through ultrasonic and effect that is microwave-assisted, its sheet interlayer spacing increases greatly, is so more conducive to mixing for principle of the present invention.The molecular chain of polyoxyethylene glycol to be mixed with graphene oxide lamella by the physical action such as hydrogen bond and capillary force and oxidized graphene sheet layer wraps up, and reaches the effect of sizing.
embodiment 1
(1) configuration of graphene oxide solution: the graphene oxide powder taking 20mg, joins in 70ml secondary deionized water, and magnetic agitation also with ultrasonic 30 minutes, makes graphene oxide disperse uniformly in deionized water;
(2) Macrogol 4000 of 1.98g is joined in above-mentioned graphene oxide solution, and transfer in microwave reactor, stirring 10 minutes higher than organic phase change material melt temperature (80 DEG C) heating with vigorous magnetic, obtain the solution be dispersed in deionized water;
(3) solution obtained is put into vacuum drying oven to be dried to sample and to reach constant weight, obtain composite phase-change material.
Its infared spectrum of composite phase-change material PEG1 FT-IR result prepared by the present embodiment is as shown in a curve in Fig. 3, and its DSC result picture as shown in Figure 4.
embodiment 2
By preparation process and the reaction process of embodiment 1, just change the quality of graphene oxide and Macrogol 4000 into 40mg and 1.96g, its infared spectrum of the composite phase-change material PEG2 FT-IR result obtained is as shown in b curve in Fig. 3, and its DSC result as shown in Figure 5.
embodiment 3
By preparation process and the reaction process of embodiment 1, just change the quality of graphene oxide and Macrogol 4000 into 60mg and 1.94g, its infared spectrum of the composite phase-change material PEG3 FT-IR result obtained is as shown in c curve in Fig. 3, and its DSC result as shown in Figure 6.
embodiment 4
By preparation process and the reaction process of embodiment 1, just change the quality of graphene oxide and Macrogol 4000 into 80mg and 1.92g, its infared spectrum of the composite phase-change material PEG4 FT-IR result obtained is as shown in d curve in Fig. 3, and its DSC result as shown in Figure 7.
embodiment 5
By preparation process and the reaction process of embodiment 1, just change the quality of graphene oxide and Macrogol 4000 into 100mg and 1.90g, its infared spectrum of the composite phase-change material PEG5 FT-IR result obtained is as shown in e curve in Fig. 3, and its DSC result as shown in Figure 8.
embodiment 6
By preparation process and the reaction process of embodiment 1, just change Macrogol 4000 into Liquid Macrogol.
embodiment 7
By preparation process and the reaction process of embodiment 1, just change Macrogol 4000 into Macrogol 2000.
Above-described embodiment is illustrative principle of the present invention and effect only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art and usually know that the knowledgeable modifies or changes not departing from all that complete under disclosed spirit and technological thought, still covered by claim of the present invention.
Claims (8)
1. a preparation method for the composite phase-change material of graphene oxide sizing, is characterized in that, comprise the following steps:
(1) graphene oxide powder is added in deionized water, ultrasonic and stir make it dispersed, be configured to graphene oxide solution;
(2) organic phase change material is joined in the graphene oxide solution of step (1) gained, and transfer in microwave reactor, heat with vigorous magnetic stirring under higher than organic phase change material melt temperature, obtain the solution be dispersed in deionized water;
(3) solution that step (2) obtains is put into vacuum drying oven and be dried to constant weight, obtain composite phase-change material.
2. preparation method according to claim 1, is characterized in that, the concentration of graphene oxide solution is 0.2mg/ml ~ 1mg/ml.
3. preparation method according to claim 1 and 2, is characterized in that, described in step (2), organic phase change material is polyoxyethylene glycol.
4. preparation method according to claim 3, is characterized in that, described polyoxyethylene glycol to be number-average molecular weight be 200 ~ 10000 polyoxyethylene glycol.
5. preparation method according to claim 1 and 2, is characterized in that, the consumption of organic phase change material and graphene oxide solution is to make the massfraction of graphene oxide in the composite phase-change material that obtains be 1% ~ 5%.
6. preparation method according to claim 1 and 2, is characterized in that, ultrasonic in step (1) is 10-50 minute with churning time, and the magnetic agitation time described in step (2) is 1-10 minute.
7. preparation method according to claim 1 and 2, is characterized in that, the temperature that in step (2), heating is stirred with vigorous magnetic under higher than organic phase change material melt temperature is 70-100 DEG C.
8. the composite phase-change material of the graphene oxide sizing obtained by method described in claim 1 or 2 or 3 or 4 or 5 or 6 or 7.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106010458A (en) * | 2016-06-03 | 2016-10-12 | 大连理工大学 | Magnetic thermal-photothermal double-drive energy conversion and storage polymer nano composite phase-change energy-storage material and preparation method thereof |
| CN106085368A (en) * | 2016-06-22 | 2016-11-09 | 桂林电子科技大学 | Composite phase-change energy storage material for microcapsule that a kind of nano heat-conductive strengthens and preparation method thereof |
| CN106118610A (en) * | 2016-08-02 | 2016-11-16 | 陕西理工大学 | The preparation method of Polyethylene Glycol/Graphene sizing phase-change material |
| CN106634850A (en) * | 2016-10-19 | 2017-05-10 | 北京恒通绿建节能科技有限公司 | Heat-conducting composite solid-solid phase-change material and preparation method therefor |
| CN106928906A (en) * | 2017-05-02 | 2017-07-07 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN107963626A (en) * | 2017-12-21 | 2018-04-27 | 东南大学 | A kind of preparation method of photothermal conversion composite setting phase-change material |
| CN108822805A (en) * | 2018-07-11 | 2018-11-16 | 东华大学 | Composite phase-change material and preparation method thereof based on spongy graphene oxide |
| CN111253913A (en) * | 2020-02-29 | 2020-06-09 | 复旦大学 | Heat storage material based on graphene composite framework structure and preparation method thereof |
| CN112194942A (en) * | 2020-09-18 | 2021-01-08 | 沪宝新材料科技（上海）股份有限公司 | Waterproof and heat-insulating middle coating for outer wall and preparation method thereof |
| CN113456814A (en) * | 2020-03-11 | 2021-10-01 | 北京石墨烯研究院 | Graphene-based composite material, preparation method and application |
| CN115678088A (en) * | 2021-07-23 | 2023-02-03 | 中国科学院大连化学物理研究所 | Porous polymer-graphene-based composite shaping phase-change material and preparation and application thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106010458B (en) * | 2016-06-03 | 2018-12-21 | 大连理工大学 | A kind of magnetic heat-photo-thermal is double to drive energy conversion and the polymer nanocomposite composite phase-change energy storage material of storage and preparation method thereof |
| CN106010458A (en) * | 2016-06-03 | 2016-10-12 | 大连理工大学 | Magnetic thermal-photothermal double-drive energy conversion and storage polymer nano composite phase-change energy-storage material and preparation method thereof |
| CN106085368A (en) * | 2016-06-22 | 2016-11-09 | 桂林电子科技大学 | Composite phase-change energy storage material for microcapsule that a kind of nano heat-conductive strengthens and preparation method thereof |
| CN106085368B (en) * | 2016-06-22 | 2019-08-06 | 桂林电子科技大学 | A kind of composite phase-change energy storage material for microcapsule and preparation method thereof of nano heat-conductive enhancing |
| CN106118610A (en) * | 2016-08-02 | 2016-11-16 | 陕西理工大学 | The preparation method of Polyethylene Glycol/Graphene sizing phase-change material |
| CN106118610B (en) * | 2016-08-02 | 2019-03-12 | 陕西理工大学 | Polyethylene glycol/graphene sizing phase-change material preparation method |
| CN106634850A (en) * | 2016-10-19 | 2017-05-10 | 北京恒通绿建节能科技有限公司 | Heat-conducting composite solid-solid phase-change material and preparation method therefor |
| CN106928906A (en) * | 2017-05-02 | 2017-07-07 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN106928906B (en) * | 2017-05-02 | 2019-08-02 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN107963626A (en) * | 2017-12-21 | 2018-04-27 | 东南大学 | A kind of preparation method of photothermal conversion composite setting phase-change material |
| CN108822805A (en) * | 2018-07-11 | 2018-11-16 | 东华大学 | Composite phase-change material and preparation method thereof based on spongy graphene oxide |
| CN111253913A (en) * | 2020-02-29 | 2020-06-09 | 复旦大学 | Heat storage material based on graphene composite framework structure and preparation method thereof |
| CN111253913B (en) * | 2020-02-29 | 2021-09-17 | 复旦大学 | Heat storage material based on graphene composite framework structure and preparation method thereof |
| CN113456814A (en) * | 2020-03-11 | 2021-10-01 | 北京石墨烯研究院 | Graphene-based composite material, preparation method and application |
| CN113456814B (en) * | 2020-03-11 | 2022-10-21 | 北京石墨烯研究院 | Graphene-based composite material, preparation method and application |
| CN112194942A (en) * | 2020-09-18 | 2021-01-08 | 沪宝新材料科技（上海）股份有限公司 | Waterproof and heat-insulating middle coating for outer wall and preparation method thereof |
| CN112194942B (en) * | 2020-09-18 | 2022-02-01 | 沪宝新材料科技（上海）股份有限公司 | Waterproof and heat-insulating middle coating for outer wall and preparation method thereof |
| CN115678088A (en) * | 2021-07-23 | 2023-02-03 | 中国科学院大连化学物理研究所 | Porous polymer-graphene-based composite shaping phase-change material and preparation and application thereof |
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Application publication date: 20151230 |