CN108467711B - Inorganic composite phase change material and preparation method thereof - Google Patents
Inorganic composite phase change material and preparation method thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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Abstract
The invention discloses an inorganic composite phase-change material and a preparation method thereof, wherein the phase-change material comprises a main thermal agent, a nucleating agent, a pH regulator, an anti-corrosion agent, a thermal conducting agent and water, the mass of the nucleating agent is 3-6% of that of the main thermal agent, the mass of the pH regulator is 0-3% of that of the main thermal agent, and the mass of the anti-corrosion agent is main heat, sodium acetate, calcium chloride and sodium stearate are subjected to high-temperature hydrothermal reaction under the condition of the pH regulator to prepare eutectic salt, so that the phase-change temperature range of the obtained eutectic salt is reduced to 5-10 ℃, and the prepared product directly generates a self-organization framework to form gel eutectic salt, thereby the system does not need to add a thickening agent and a sizing agent, the supercooling degree of the product is greatly reduced, and the ternary eutectic salt has the characteristic of being special in structure, the organic phase-change material is not easy to delaminate, the super-cooling is not easy to generate, and simultaneously, the inorganic phase change material has the advantage of high latent heat value.
Description
Technical Field
The invention relates to the technical field of phase change material preparation, in particular to an inorganic composite phase change material and a preparation method thereof.
Background
A Phase Change Material (PCM-Phase Change Material) refers to a substance that changes state of a substance with a Change in temperature and can provide latent heat. The process of changing physical properties is called a phase change process, and in this case, the phase change material absorbs or releases a large amount of latent heat. Once the material is widely applied to human life, the material becomes an optimal green environment-friendly carrier for energy conservation and environmental protection, and is listed as a national research and development utilization sequence in China.
Phase change materials have the ability to change their physical state over a range of temperatures. Taking solid-liquid phase change as an example, when the material is heated to a melting temperature, the material generates phase change from a solid state to a liquid state, and in the melting process, the phase change material absorbs and stores a large amount of latent heat; when the phase change material is cooled, the stored heat is dissipated to the environment within a certain temperature range, and reverse phase change from liquid to solid is carried out. In both phase change processes, the stored or released energy is called latent heat of phase change. When the physical state changes, the temperature of the material is almost kept unchanged before the phase change is completed, a wide temperature platform is formed, and although the temperature is unchanged, the latent heat absorbed or released is quite large.
The classification of phase change materials mainly includes three types of inorganic PCM, organic PCM, and composite PCM. Wherein, the inorganic PCM mainly comprises crystalline hydrated salts, molten salts, metals or alloys and the like; the organic PCM mainly comprises paraffin, acetic acid and other organic matters; the composite phase-change heat storage material has the advantages that the defects of a single inorganic or organic phase-change heat storage material can be effectively overcome, the application effect of the phase-change material can be improved, and the application range of the phase-change material can be expanded. Therefore, the development of composite phase-change heat storage materials has become a hot research topic in the field of heat storage materials. However, the mixed phase change material may also cause disadvantages such as a decrease in latent heat of phase change, or easy denaturation during a long-term phase change.
With the high development of Chinese cold-chain logistics, particularly medicine and vaccine specialized cold-chain logistics, the use of phase-change materials for cold-chain transportation has increasingly become an attractive focus of the Chinese logistics community. In the cold chain transportation process of foods, medicines and the like, the phase change material can enable the foods and the medicines to be in a low-temperature environment, so that the fluctuation of storage and transportation temperature in the transportation process is solved, and the quality of the products is effectively controlled. The cold chain transportation of drugs, vaccines, blood products and medical devices, and in particular the transportation of vaccines, is subject to strict regulations, and the temperature during the transportation of vaccines is usually kept between 2 ℃ and 8 ℃, and if there is a temperature deviation, the effect of the vaccine should be lost.
At present, a lot of organic phase change materials are researched, which have inflammability, and can still become a fire hazard even though being subjected to flame retardant treatment. The inorganic hydrated salt phase-change material has incombustibility, but has poor supercooling degree and cycle performance. In addition, the corrosion problem of eutectic salt in the inorganic phase-change material to the heat exchanger is serious, the actual application value is influenced, and the popularization and the application are not facilitated.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an inorganic composite phase change material and a preparation method thereof for solving the application problem.
The invention is realized by the following technical scheme:
the invention discloses an inorganic composite phase change material which comprises a main thermal agent, a nucleating agent, a pH regulator, an anti-corrosion agent, a heat conducting agent and water, wherein the mass of the nucleating agent is 3-6% of that of the main thermal agent, the mass of the pH regulator is 0-3% of that of the main thermal agent, the mass of the anti-corrosion agent is 0.5-2% of that of the main thermal agent, the mass of the heat conducting agent is 0.5-1% of that of the main thermal agent, and the mass of the water is 30-75% of that of the main thermal agent.
The invention discloses an inorganic composite phase change material which is characterized in that a main heating agent is eutectic salt of sodium acetate, calcium chloride and sodium stearate, wherein the mass ratio of the sodium acetate to the calcium chloride to the sodium stearate is 50-65:45-33: 5-2.
The invention also discloses a preparation method of the inorganic composite phase-change material, which comprises the following steps:
1) heating water to 70-80 ℃, adding sodium acetate, and uniformly stirring to form a transparent solution; adding calcium chloride, and stirring to form a transparent solution; adding sodium stearate, slowly adding pH regulator under stirring, maintaining reaction for 2 hr to make the whole system become transparent solution again, cooling, and stirring to obtain gel;
2) heating the product obtained in the step 1) to 70-80 ℃ again to obtain a transparent solution, slowly adding the nucleating agent and the corrosion inhibitor into the solution obtained in the step 1), uniformly stirring, and controlling the temperature of the solution at 70-80 ℃ for half an hour;
3) adding the heat-conducting agent into the solution obtained in the step 2), uniformly stirring, and filling the solution into a container for storage when the temperature of the solution is controlled to be 50-60 ℃.
As a further improvement, the nucleating agent is one or a composition of more of borax, sodium hexametaphosphate and sodium pyrophosphate.
As a further improvement, the pH regulator disclosed by the invention is one or a combination of two of boric acid and phosphoric acid.
As a further improvement, the corrosion inhibitor is a compound product of benzotriazole and triethanolamine, wherein the weight ratio of triethanolamine: the mass ratio of the benzotriazole is 2: 1.
As a further improvement, the heat conducting agent is one or a composition of more of nano silicon dioxide, nano titanium dioxide and graphene.
The invention has the following beneficial effects:
the invention discloses an inorganic composite phase-change material and a preparation method thereof, wherein a main heating agent is eutectic salt of sodium acetate, calcium chloride and sodium stearate, wherein the phase-change temperature of sodium acetate trihydrate is 58 ℃, the phase-change temperature of calcium chloride hexahydrate is 29 ℃, and the two substances have the defect of large supercooling degree as the phase-change material. According to the preparation method, sodium acetate, calcium chloride and sodium stearate are subjected to high-temperature hydrothermal reaction under a pH regulator to prepare the eutectic salt, the phase transition temperature range of the obtained eutectic salt is reduced to 5-10 ℃, and the prepared product directly generates a self-organization framework to form a gel eutectic salt, so that a thickening agent and a shaping agent are not required to be added to a system, and the supercooling degree of the product is greatly reduced (the supercooling degree is less than 0.5 ℃). And because the ternary eutectic salt has a special structure, the ternary eutectic salt has the advantages that the organic phase-change material is not easy to delaminate and generate supercooling, and simultaneously has the advantage of high latent heat value of the inorganic phase-change material.
In the invention, because of the existence of chloride ions, in actual use, in order to avoid the corrosion of the chloride ions, the corrosion inhibitor is added, and the excellent corrosion resistance is obtained by compounding the benzotriazole and the triethanolamine, thereby having wide market prospect.
The invention also adds nucleating agent and heat-conducting agent, especially adding heat-conducting agent, which finds that in the ternary eutectic salt of the system, because the ternary eutectic salt has unique self-organizing gel structure, after one or more of nano-level nano-silicon dioxide, nano-titanium dioxide and graphene are added, hydrate with complex structure can be formed, the phase-change temperature time is prolonged, and the phase-change potential is increased. Meanwhile, a complex internal inorganic network is formed, so that the heat conductivity coefficient of the phase change material is greatly increased, and the phase change material has the advantage different from a common inorganic salt phase change material.
Detailed Description
The invention is further illustrated, but not limited, by the following specific examples.
Example 1
1) Heating 75 parts by weight of water to 70-80 ℃, adding 50 parts by weight of sodium acetate, and uniformly stirring to form a transparent solution; then adding 45 parts by weight of calcium chloride, and stirring to form a transparent solution; then 5 parts by weight of sodium stearate is added, 1 part by weight of phosphoric acid as a pH regulator is slowly added under stirring, and the reaction is maintained for 2 hours, so that the whole system becomes a transparent solution again. Cooling, and stirring to obtain gel.
2) And (2) heating the product obtained in the step 1) to 70-80 ℃ again to obtain a transparent solution, wherein 6 parts by weight of nucleating agent borax and 2 parts by weight of corrosion inhibitor (triethanolamine: the mass ratio of benzotriazole is 2:1), slowly adding the benzotriazole into the solution obtained in the step 1), uniformly stirring, and controlling the temperature of the solution at 70-80 ℃ for half an hour;
3) adding 1 part by weight of thermal conductive agent nano silicon dioxide into the solution obtained in the step 2), uniformly stirring, and filling the solution into a container for storage when the temperature of the solution is controlled to be 50-60 ℃.
The phase change material provided by the invention is tested for phase change temperature and supercooling degree according to a step cooling curve method, phase change enthalpy value is tested, and corrosion rates of aluminum and stainless steel in the phase change material are examined (the temperature is selected to be 71 +/-2 ℃). And simultaneously, the long-term stability condition of the product is detected again after the cold-hot phase change circulation is carried out for 1000 times in the high-low temperature circulation box.
The test result shows that: the phase-change material is white gel-like solid, the phase-change temperature is 7-10 ℃, the phase-change enthalpy is 240J/g, and the corrosion rate of the metallic aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement. After 1000 times of phase change circulation, the phase change material is white gel solid, the phase change temperature is 7-10 ℃, the phase change enthalpy is 229J/g, and the corrosion rate of the metal aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement.
Example 2
1) Heating 30 parts by weight of water to 70-80 ℃, adding 65 parts by weight of sodium acetate, and uniformly stirring to form a transparent solution; adding 33 parts by weight of calcium chloride, and stirring to form a transparent solution; then adding 2 parts by weight of sodium stearate, slowly adding 3 parts by weight of pH regulator boric acid under stirring, and maintaining the reaction for 2 hours to ensure that the whole system becomes transparent solution again. Cooling, and stirring to obtain gel.
2) And (2) heating the product obtained in the step 1) to 70-80 ℃ again to obtain a transparent solution, wherein 3 parts by weight of nucleating agent sodium hexametaphosphate and 0.5 part by weight of corrosion inhibitor (triethanolamine: the mass ratio of benzotriazole is 2:1), slowly adding the benzotriazole into the solution obtained in the step 1), uniformly stirring, and controlling the temperature of the solution at 70-80 ℃ for half an hour;
3) adding 0.5 part by weight of heat-conducting agent nano titanium dioxide into the solution obtained in the step 2), uniformly stirring, and filling the solution into a container for storage when the temperature of the solution is controlled to be 50-60 ℃.
The phase change material provided by the invention is tested for phase change temperature and supercooling degree according to a step cooling curve method, phase change enthalpy value is tested, and corrosion rates of aluminum and stainless steel in the phase change material are examined (the temperature is selected to be 71 +/-2 ℃). And simultaneously, the long-term stability condition of the product is detected again after the cold-hot phase change circulation is carried out for 1000 times in the high-low temperature circulation box.
The test result shows that: the phase-change material is white gel-like solid, the phase-change temperature is 8-11 ℃, the phase-change enthalpy is 249J/g, and the corrosion rate of the metallic aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement. After 1000 times of phase change circulation, the phase change material is white gel solid, the phase change temperature is 8-11 ℃, the phase change enthalpy is 235J/g, and the corrosion rate of the metallic aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement.
Example 3
1) Heating 50 parts by weight of water to 70-80 ℃, adding 58 parts by weight of sodium acetate, and uniformly stirring to form a transparent solution; then adding 38 parts by weight of calcium chloride, and stirring to form a transparent solution; then, 4 parts by weight of the sodium stearate component was added thereto, and the reaction was maintained for 2 hours with stirring, so that the whole system became a transparent solution again. Cooling, and stirring to obtain gel.
2) And (2) heating the product obtained in the step 1) to 70-80 ℃ again to obtain a transparent solution, wherein 4.5 parts by weight of nucleating agent sodium pyrophosphate and 1 part by weight of corrosion inhibitor (triethanolamine: the mass ratio of benzotriazole is 2:1), slowly adding the benzotriazole into the solution obtained in the step 1), uniformly stirring, and controlling the temperature of the solution at 70-80 ℃ for half an hour;
3) adding 1 part by weight of a heat conducting agent graphene material into the solution obtained in the step 2), uniformly stirring, and filling the solution into a container for storage when the temperature of the solution is controlled to be 50-60 ℃.
The phase change material provided by the invention is tested for phase change temperature and supercooling degree according to a step cooling curve method, phase change enthalpy value is tested, and corrosion rates of aluminum and stainless steel in the phase change material are examined (the temperature is selected to be 71 +/-2 ℃). And simultaneously, the long-term stability condition of the product is detected again after the cold-hot phase change circulation is carried out for 1000 times in the high-low temperature circulation box.
The test result shows that: the phase-change material is yellow or black gel-like solid, the phase-change temperature is 8-10 ℃, the phase-change enthalpy is 258J/g, and the corrosion rate of the metallic aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement. After 1000 times of phase change circulation, the phase change material is yellow or black gelatinous solid, the phase change temperature is 8-10 ℃, the phase change enthalpy is 248J/g, and the corrosion rate of the metallic aluminum and the stainless steel meets the SH/T0085-91 corrosion test requirement.
The foregoing is merely an example of the embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (2)
1. The inorganic composite phase change material is characterized by comprising a main thermal agent, a nucleating agent, a pH regulator, an anti-corrosion agent, a heat conducting agent and water, wherein the mass of the nucleating agent is 3-6% of that of the main thermal agent, the mass of the pH regulator is 0-3% of that of the main thermal agent, the mass of the anti-corrosion agent is 0.5-2% of that of the main thermal agent, the mass of the heat conducting agent is 0.5-1% of that of the main thermal agent, the mass of the water is 30-75% of that of the main thermal agent, the main thermal agent is eutectic salt of sodium acetate, calcium chloride and sodium stearate, the mass ratio of the sodium acetate, the calcium chloride and the sodium stearate is 50-65:45-33:5-2, the nucleating agent is one or a combination of borax, sodium hexametaphosphate and sodium pyrophosphate, and the pH regulator is boric acid, sodium hexametaphosphate and sodium pyrophosphate, One or two of phosphoric acid, the corrosion inhibitor is a compound product of benzotriazole and triethanolamine, wherein the weight ratio of triethanolamine: the mass ratio of benzotriazole is 2:1, and the heat conducting agent is one or a combination of several of nano silicon dioxide, nano titanium dioxide and graphene.
2. The preparation method of the inorganic composite phase-change material as claimed in claim 1, characterized by comprising the following steps:
1) heating water to 70-80 ℃, adding sodium acetate, and uniformly stirring to form a transparent solution; adding calcium chloride, and stirring to form a transparent solution; adding sodium stearate, slowly adding pH regulator under stirring, maintaining reaction for 2 hr to make the whole system become transparent solution again, cooling, and stirring to obtain gel;
2) heating the product obtained in the step 1) to 70-80 ℃ again to obtain a transparent solution, slowly adding the nucleating agent and the corrosion inhibitor into the solution obtained in the step 1), uniformly stirring, and controlling the temperature of the solution at 70-80 ℃ for half an hour;
3) adding the heat-conducting agent into the solution obtained in the step 2), uniformly stirring, and filling the solution into a container for storage when the temperature of the solution is controlled to be 50-60 ℃.
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| CN110878199B (en) * | 2018-09-06 | 2021-09-14 | 陕西久维电力工程有限公司 | Composite phase change material |
| CN111518520B (en) * | 2018-12-30 | 2021-05-28 | 纯钧新材料(深圳)有限公司 | Composition as coolant and method for preparing same |
| CN109723488A (en) * | 2019-03-05 | 2019-05-07 | 重庆大学 | Utilize the gas pumping method and extraction system of phase-change material auxiliary liquid nitrogen fracturing |
| CN111718690B (en) * | 2019-03-19 | 2021-08-31 | 中国科学院大连化学物理研究所 | Preparation and application of composite energy storage material |
| CN113861944B (en) * | 2021-10-19 | 2023-10-27 | 佛山市顺德区美的洗涤电器制造有限公司 | Inorganic hydrated salt phase-change material composition, inorganic hydrated salt phase-change material, and preparation method and application thereof |
| CN113861943B (en) * | 2021-10-19 | 2023-11-10 | 佛山市顺德区美的洗涤电器制造有限公司 | Phase change material composition, phase change material, preparation method and application thereof |
| CN113881405A (en) * | 2021-10-19 | 2022-01-04 | 佛山市顺德区美的洗涤电器制造有限公司 | Phase-change material composition, phase-change material, and preparation method and application thereof |
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| CN101982518A (en) * | 2010-09-14 | 2011-03-02 | 中国科学技术大学 | Nano solid-liquid phase change energy storage composite material |
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| CN104371658A (en) * | 2014-10-29 | 2015-02-25 | 桂林电子科技大学 | Packaging shape-stabilizing method of inorganic hydrated salt phase-change heat storage material |
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