CN111548771A - Method for preparing low-temperature phase-change material by utilizing tetradecane and expanded graphite - Google Patents
Method for preparing low-temperature phase-change material by utilizing tetradecane and expanded graphite Download PDFInfo
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- CN111548771A CN111548771A CN202010439961.8A CN202010439961A CN111548771A CN 111548771 A CN111548771 A CN 111548771A CN 202010439961 A CN202010439961 A CN 202010439961A CN 111548771 A CN111548771 A CN 111548771A
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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
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- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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Abstract
The invention belongs to the technical field of phase-change material preparation, and particularly discloses a method for preparing a low-temperature phase-change material by utilizing tetradecane and expanded graphite, which comprises the following steps: (1) placing expandable graphite in an oven, drying at 100 ℃ for 2 hours, taking out and paving in a crucible, calcining the crucible, taking out and cooling to prepare the completely expanded expandable graphite; (2) weighing expanded graphite, adding the expanded graphite into a beaker, pouring tetradecane into the beaker, and placing the beaker in a water bath kettle for stirring; (3) filtering the stirred uniform mixture by suction; (4) and (4) putting the solid obtained by suction filtration into an oven for drying, taking out the solid at intervals of half an hour, weighing, and observing the surface drying state of the solid. And (4) until the mass loss rate of the material is reduced, and the sample is loose and granular, namely the preparation of the composite material is finished. The scheme is mainly used for preparing the low-temperature phase-change material which can be widely used in the anti-freezing cement concrete pavement, and solves the problems of complex process and high cost of preparing the low-temperature phase-change material in the prior art.
Description
Technical Field
The invention belongs to the technical field of phase-change material preparation, and particularly discloses a method for preparing a low-temperature phase-change material by utilizing tetradecane and expanded graphite.
Background
China is vast in territory, large in south-north span and east-west span, most of the interior of China belongs to ice and snow areas, and the problem of snow accumulation and icing on the road surface is common. In the early winter and the early spring of the ice and snow area, and in the winter of the middle part of the area, the ice and the cold are alternated day and night, so that the ice condensation problem occurs on the surface of a building or a cement concrete road under the action of temperature, humidity and vehicle load, and the durability of the building and the driving safety of the road are seriously influenced. If the composite phase-change material is used for the cement concrete pavement, the pavement ice condensation can be prevented, the traffic safety problem of the ice condensation pavement can be effectively solved, traffic accidents can be avoided as far as possible, and the road traffic capacity and the operation benefit can be improved.
Phase Change Materials (PCM), or phase change energy storage materials, refer to materials that change their phase state (e.g., from solid to liquid or from liquid to solid) within a temperature range of one point, i.e., a phase change temperature range, and absorb, store or release a large amount of heat in the form of latent heat while the temperature itself remains constant. The phase-change material has the characteristics of heat energy storage and temperature regulation control, so that the phase-change material has application values in many fields, such as solar energy utilization, electric power peak regulation, waste heat utilization, cross-season heat storage and cold storage, food preservation, building heat insulation and preservation, electronic device heat protection, textile clothing, agriculture and the like. However, the application of phase change materials in the field of road traffic is still under the research and research stage.
Phase change materials are widely used in cement concrete, and are generally divided into three purposes: one is that phase change materials are used for heat preservation and insulation of building walls, and the phase change materials in the walls absorb heat through phase change when the external temperature is higher, so as to achieve the purpose of temperature peak clipping and reduce energy consumption; one is to utilize phase change material to absorb heat to reduce hydration heat release of mass concrete in the forming process and eliminate temperature crack caused by temperature difference inside and outside the concrete. The phase-change material applicable under the two kinds of use conditions generally has the phase-change temperature of 20-30 ℃, and the material selection range is wide. The last type is to mix the phase-change material into cement concrete to achieve the effect of snow melting and ice melting, and the phase-change temperature is usually 0-5 ℃.
Chinese patent CN101029216A "a self-temperature-regulating highway phase-change material and its production method" proposes a phase-change material compounded by ten materials of fatty acid, potassium sulfate, chitosan, polyacrylamide, cenospheres, brucite, pyrophyllite, organosilicon emulsion, paraffin and sodium hydroxide according to a certain mass ratio.
Chinese patent CN108130047A 'preparation method of low-temperature regulator for asphalt based on tetradecane/tetradecanol/melamine modified urea-formaldehyde resin', provides a preparation method of temperature regulator using tetradecane/tetradecanol/melamine modified urea-formaldehyde resin as temperature regulating material. The method comprises the steps of mixing n-tetradecane and tetradecanol in a certain proportion, coating the mixture by melamine/urea/formaldehyde resin to obtain microcapsules under the premise of selecting a proper emulsifier, and recoating the microcapsules by high-temperature-resistant phenolic aldehyde modified epoxy resin to obtain the final self-temperature-regulating material for asphalt. But the application range is limited to asphalt mixture, and the process is relatively more complicated.
Disclosure of Invention
The invention aims to provide a method for preparing a low-temperature phase-change material by utilizing tetradecane and expanded graphite, so as to solve the problems of complex process and high cost of the preparation of the low-temperature phase-change material in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for manufacturing a low-temperature phase-change material by utilizing tetradecane and expanded graphite comprises the following steps:
(1) placing expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded graphite;
(2) weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring a phase change main material tetradecane into the beaker to enable the phase change main material tetradecane to completely submerge the expanded graphite; placing the beaker in a 60 ℃ water bath kettle, stirring for 30min by a constant speed stirrer at a rotating speed of 160rad/min, and scraping off expanded graphite which is stirred and raised and is stuck on the wall of the beaker during the stirring so as to ensure the full contact and complete adsorption of the materials;
(3) pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips from the bottom of the funnel, repeatedly washing the beaker with the filtrate and carrying out suction filtration until no expanded graphite residue exists in the beaker;
(4) and (3) putting the solid obtained by suction filtration into an oven for forced air drying at the temperature of 80 ℃, taking out the solid at intervals of half an hour, weighing the solid, and observing the surface drying state of the solid. And (4) until the mass loss rate of the material is reduced, and the sample is loose and granular, namely the preparation of the composite material is finished.
Further, the phase change carrier material in the step (1) uses expandable graphite, and the phase change host material in the step (2) is tetradecane.
Furthermore, the composite phase change material can be used as a low-temperature regulator for anti-freezing cement concrete pavements.
The working principle and the beneficial effects of the technical scheme are as follows:
(1) the adsorption shaping of tetradecane and expanded graphite is only simple physical mixing, no chemical reaction occurs, and the chemical compatibility is good;
(2) the composite phase change aggregate has low phase change rate, can keep longer heat release time, enables the environmental temperature to slowly and uniformly rise, and is suitable for long-time low-temperature environment;
(3) the composite phase-change aggregate has excellent hydrophobicity, a very large contact angle is kept when the material is contacted with water, tetradecane does not leak, and the adsorption stability in the concrete construction process can be ensured;
(4) the invention has simple synthesis process, low cost and wide prospect.
Drawings
FIG. 1 is a scanning electron microscope image of expanded graphite illustrating the microstructure of the expanded graphite;
FIG. 2 is a graph showing the FT-IR test results of the composite phase change material;
FIG. 3 is a DSC curve of tetradecane/expanded graphite illustrating the heat storage capacity and operating range of the composite phase change aggregate;
FIG. 4 is a photograph of the final product;
FIG. 5 shows a phase change cement concrete made from the final product instead of a portion of the aggregate.
Detailed Description
The following is further detailed with reference to fig. 1, fig. 2, fig. 3, fig. 4, and fig. 5 by the specific embodiments:
the final product of the invention is a composite low-temperature phase-change material which can be mixed into cement concrete.
The invention provides a preparation method of a tetradecane/expanded graphite-based low-temperature phase-change material, which comprises the steps of placing expandable graphite in an oven for drying for several hours, taking out the expandable graphite to be thinly paved in a crucible, placing the crucible in a muffle furnace for calcining for a period of time, taking out the crucible and cooling to prepare the completely expanded graphite; the melting point of tetradecane is 5.5 ℃, tetradecane/expanded graphite is mixed according to a certain proportion, the mixture is stirred at a certain temperature and within a certain pressure range, so that the two materials are fully contacted and completely adsorbed, after the mixture is uniformly mixed, the mixture is poured into a funnel, a vacuum pump is connected for suction filtration until no liquid drips at the bottom of the funnel, and a beaker is repeatedly washed by filtrate and suction filtration is carried out until no expanded graphite residue exists in the beaker. And (3) putting the solid obtained by suction filtration into an oven for forced air drying at the temperature of 80 ℃, taking out the solid at intervals of half an hour, weighing the solid, and observing the surface drying state of the solid. And (4) until the mass loss rate of the material is reduced, and the sample is loose and granular, namely the preparation of the composite material is finished. The product of the patent is subjected to DSC test, the phase change starting temperature of the material in the temperature rising process is 5.2 ℃, the ending temperature is 10.7 ℃, the peak temperature is 9.2 ℃, and the phase change latent heat is 201.4J/g; the initial temperature of phase change in temperature reduction is 4.1 ℃, the final temperature is-2.4 ℃, the peak temperature is 0.3 ℃, and the latent heat of phase change is 198.9J/g. The invention provides a preparation method of tetradecane/expanded graphite low-temperature phase change aggregate, which comprises the following specific steps:
(1) and (3) placing the expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded expandable graphite.
(2) Weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring a phase change main material tetradecane into the beaker to completely submerge the expanded graphite. Placing the beaker in a 60 ℃ water bath kettle, stirring for 30min by a constant speed stirrer at a rotating speed of 160rad/min, and scraping off the expanded graphite which is stirred and raised and is stuck on the wall of the beaker during the stirring so as to ensure the full contact and complete adsorption of the materials.
(3) And pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips from the bottom of the funnel, repeatedly washing the beaker with the filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker.
(4) And (3) putting the solid obtained by suction filtration into an oven for forced air drying at the temperature of 80 ℃, taking out the solid at intervals of half an hour, weighing the solid, and observing the surface drying state of the solid. And (4) until the mass loss rate of the material is reduced, and the sample is loose and granular, namely the preparation of the composite material is finished.
In the invention, the expanded graphite in the step (1) is a loose and porous vermicular substance obtained by intercalating, washing, drying and high-temperature expanding natural graphite flakes, and has stable property, cold and heat resistance, corrosion resistance, more than 99 percent of carbon content and 400 times of expansion ratio. The tetradecane in the step (2) has a melting point of 5.5 ℃, is in a liquid state at normal temperature, has a proper phase-change temperature, large phase-change latent heat and good phase-change circulation stability, and is a proper anti-freezing phase-change material. And (4) ensuring that the filtrate in the step (3) is tetradecane residual solution after complete adsorption, and filtering out the tetradecane residual solution without adding other impurities. And (4) the mass ratio of the tetradecane to the expanded graphite in each part of the composite phase-change material obtained in the step (4) is about 10: 1.
The embodiments in this scheme all operate as described above.
Example 1
(1) And (3) putting the expanded graphite in an oven at 100 ℃ for 2h, and fully drying.
(2) 10g of fully dried expanded graphite is weighed into a beaker, and the phase change host material is poured into the beaker so that the phase change host material completely submerges the expanded graphite. Placing the beaker in a 60 ℃ water bath kettle, stirring for 30min by a constant speed stirrer at a rotating speed of 160rad/min, and scraping off the expanded graphite which is stirred and raised and is stuck on the wall of the beaker during the stirring so as to ensure the full contact and complete adsorption of the materials.
(3) And pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips from the bottom of the funnel, repeatedly washing the beaker with the filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker.
(4) And (3) putting the solid obtained by suction filtration into an oven for forced air drying at the temperature of 80 ℃, taking out the solid at intervals of half an hour, weighing the solid, and observing the surface drying state of the solid. And when the mass loss rate of the material is reduced, the sample is loose and granular, and the preparation of the composite material is considered to be finished.
(5) And repeating the steps to obtain multiple groups of composite phase change aggregates.
And uniformly spreading the prepared tetradecane/expanded graphite in three batches on filter paper, and placing the filter paper indoors. After 13 days, the mass was weighed and the filter paper was observed for signs of tetradecane leakage. The mass changes are shown in Table 1.
TABLE 1 Long-term storage stability of tetradecane/expanded graphite at Room temperature
Putting tetradecane/expanded graphite into a beaker, adding a proper amount of distilled water, stirring with a glass rod for 2min, and simulating the mixing process of cement concrete. The stirred mixture was poured into a funnel, filtered with a vacuum pump and all filtrates were collected. The mass and volume of the filtrate were measured and the density was calculated. And comparing and interpolating the calculated mixture density with an actual density curve of tetradecane-distilled water to obtain the content of tetradecane in the mixture, and judging the tetradecane leakage condition. The tetradecane/expanded graphite adsorption rate used in the test is 92.5%, and the test data are shown in Table 2.
TABLE 2 tetradecane/expanded graphite Water adsorption stability test data
Fig. 1 is a scanning electron microscope image of expanded graphite. FIG. 2 is the FT-IR test result of the composite phase change material, and it can be seen that the adsorption shaping of tetradecane and expanded graphite is only simple physical mixing, no chemical reaction occurs, and the chemical compatibility is good; the expanded graphite is 500-4000cm-1Mainly has 4 absorption peaks at 1400cm-1、3100cm-1Predominantly methyl (CH)3-) and methylene (-CH)2-) caused by carbon-hydrogen bond stretching vibration; 1610cm-1Mainly caused by stretching vibration of carbonyl (C ═ O); 3450cm-1Is caused by the stretching vibration of hydroxyl (-OH). Tetradecane 3000-2800cm-1Is a saturated carbon-hydrogen bond (C-H) contraction vibration absorption peak, 1465--1Is a bending vibration peak of saturated carbon-hydrogen bond (C-H). The infrared spectrum curve of the tetradecane/expanded graphite is the superposition of the tetradecane and the expanded graphite, and no new characteristic peak appears or disappears. It can be concluded that the adsorptive shape of tetradecane and expanded graphite is simply a physical mixture, no chemical reaction occurs, and chemical compatibility is good. Fig. 3 is a DSC curve of tetradecane/expanded graphite illustrating the heat storage capacity and operating range of the composite phase change aggregate. Fig. 4 is a photograph of the final product. FIG. 5 shows a phase change cement concrete made from the final product instead of a portion of the aggregate.
Example 2: the same as in example 1, except that the temperature of the water bath in step (2) was changed to 30 ℃.
Example 3: the same as example 1, but the step (2) was changed to a step of charging the fully dried expanded graphite and tetradecane into a conical flask in sequence under a water bath condition of 60 ℃, connecting a vacuum pump, and stirring with a magnetic stirrer at a rotation speed of still 160rad/s for 30 min. And (3) keeping the vacuum pump running in the stirring process, stopping stirring after 4min when the air pressure in the conical flask is less than 0.3MPa, removing a connecting pipe of the vacuum pump, recovering the air pressure in the container to the atmospheric pressure, and keeping for 1 min. The steps of suction filtration and drying are the same as the normal pressure adsorption test.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (3)
1. A method for manufacturing a low-temperature phase-change material by utilizing tetradecane and expanded graphite is characterized by comprising the following steps of:
(1) placing expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and paving in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded graphite;
(2) weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring a phase change main material tetradecane into the beaker to enable the phase change main material tetradecane to completely submerge the expanded graphite; placing the beaker in a 60 ℃ water bath kettle, stirring for 30min by a constant speed stirrer at a rotating speed of 160rad/min, and scraping off expanded graphite which is stirred and raised and is stuck on the wall of the beaker during the stirring so as to ensure the full contact and complete adsorption of the materials;
(3) pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips from the bottom of the funnel, repeatedly washing the beaker with the filtrate and carrying out suction filtration until no expanded graphite residue exists in the beaker;
(4) and (3) putting the solid obtained by suction filtration into an oven for forced air drying at the temperature of 80 ℃, taking out the solid at intervals of half an hour, weighing the solid, and observing the surface drying state of the solid. And (4) until the mass loss rate of the material is reduced, and the sample is loose and granular, namely the preparation of the composite material is finished.
2. The method of claim 1, wherein the phase change carrier material in step (1) is expandable graphite, and the phase change host material in step (2) is tetradecane.
3. The application of the tetradecane and the expanded graphite in preparing the low-temperature phase-change material according to the claim 1, wherein the composite phase-change material can be used as a low-temperature regulator for anti-icing cement concrete pavement.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113307578A (en) * | 2021-06-24 | 2021-08-27 | 江苏创为交通科技发展有限公司 | Multifunctional UHPC and preparation method thereof |
| CN113652207A (en) * | 2021-08-25 | 2021-11-16 | 云南师范大学 | Adsorptive phase-change material for cold-chain logistics and preparation method thereof |
| CN115181548A (en) * | 2021-04-02 | 2022-10-14 | 中国科学院化学研究所 | Photo-thermal phase change composite material, preparation method thereof and application thereof in anti-icing and deicing |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115181548A (en) * | 2021-04-02 | 2022-10-14 | 中国科学院化学研究所 | Photo-thermal phase change composite material, preparation method thereof and application thereof in anti-icing and deicing |
| CN113307578A (en) * | 2021-06-24 | 2021-08-27 | 江苏创为交通科技发展有限公司 | Multifunctional UHPC and preparation method thereof |
| CN113652207A (en) * | 2021-08-25 | 2021-11-16 | 云南师范大学 | Adsorptive phase-change material for cold-chain logistics and preparation method thereof |
| CN113652207B (en) * | 2021-08-25 | 2023-11-17 | 云南师范大学 | Adsorptive phase change material for cold chain logistics and preparation method thereof |
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