CN114214040B - Preparation method of organic phase-change composite material and prepared phase-change composite material - Google Patents
Preparation method of organic phase-change composite material and prepared phase-change composite material Download PDFInfo
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- CN114214040B CN114214040B CN202210095435.3A CN202210095435A CN114214040B CN 114214040 B CN114214040 B CN 114214040B CN 202210095435 A CN202210095435 A CN 202210095435A CN 114214040 B CN114214040 B CN 114214040B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Abstract
The invention belongs to the technical field of phase change material preparation, in particular relates to a preparation method of an organic phase change composite material and the prepared phase change composite material, and aims to solve the problems of local supercooling or overheating of a system and reduced heat storage performance caused by low thermal conductivity of the existing organic phase change material. The preparation method of the organic phase-change composite material comprises the following steps: step one: immersing polymer aerogel in carbohydrate water solution, freeze-drying and carbonizing at low temperature to form carbon-coated aerogel material; step two: and (3) vacuum impregnating the aerogel material into the organic phase change material melt by adopting a vacuum impregnation method, and heating to remove the organic phase change material which is not adsorbed to obtain the polymer aerogel organic phase change composite material. The aerogel organic phase change composite material prepared by the method increases the wettability of the aerogel carrier and the organic phase change material, and simultaneously increases the heat conductivity coefficient of the material.
Description
Technical Field
The invention belongs to the technical field of phase change material preparation, and particularly relates to a preparation method of an organic phase change composite material and the prepared phase change composite material.
Background
The energy crisis is attracting more and more attention worldwide due to the shortage of fossil energy and the shortage of energy. Thermal storage is becoming one of the most effective methods for reasonably and efficiently utilizing existing energy. In all heat storage methods, latent heat storage is widely studied and used in many fields due to its excellent phase change characteristics and high heat storage capacity. The phase change material is a heat storage material that can store and release latent heat by adjusting its phase change according to the change of the ambient temperature. In recent years, phase change materials have been widely used in battery thermal management, building energy conservation, textile temperature regulation, solar energy, heat recovery systems, and the like.
Phase change materials are largely classified into organic phase change materials (such as paraffin, lauric acid, and alkane) and inorganic phase change materials (including alloys, metals, salts, and salt hydrates). The organic phase change material has the advantages of strong latent heat storage capacity, good chemical stability, low cost, no corrosiveness, no toxicity, no phase separation, good molding in solid state and the like. However, the organic phase-change material has low thermal conductivity, is easy to cause local supercooling or overheating of the system, and is easy to leak in the phase-change process, so that the heat storage performance of the heat storage system is reduced, and the application range of the heat storage system is limited.
Disclosure of Invention
The invention provides a preparation method of an organic phase-change composite material, which is used for solving the problems that the thermal conductivity of the organic phase-change material prepared by the existing method is low, so that the system is partially supercooled or overheated and the heat storage performance is reduced.
In order to alleviate the technical problems, the technical scheme provided by the invention is as follows:
the preparation method of the organic phase-change composite material comprises the following steps:
step one: immersing polymer aerogel in carbohydrate water solution, freeze-drying and carbonizing at low temperature to form carbon-coated aerogel material;
step two: and (3) vacuum impregnating the aerogel material into the organic phase change material melt by adopting a vacuum impregnation method, and heating to remove the organic phase change material which is not adsorbed to obtain the polymer aerogel organic phase change composite material.
Still further, polymeric aerogels include polyimides, polyamides, polyurethanes, polyphosphazenes, polybenzazoles, or polyaryletherketones.
Still further, the polymer aerogel comprises one or more of polyimide, poly (paraphenylene terephthalamide), polybenzimidazole, polybenzoxazole, polybenzothiazole, polyetherketone, polyetheretherketone; the polymer aerogel is in the form of powder, fiber, lamellar structure or block.
Still further, the carbohydrate includes a monosaccharide, disaccharide, oligosaccharide or polysaccharide.
Further, the carbohydrate comprises one or more of glucose, fructose, galactose, maltose, sucrose, lactose, starch, and pectin; the mass concentration of the carbohydrate aqueous solution is 0.5-50%; preferably 5 to 25%.
Further, the reaction condition of the impregnation in the first step is that the impregnation is carried out for 0.5 to 36 hours at room temperature and normal pressure or at room temperature and vacuum, so that the network structure of the polymer aerogel is completely impregnated; the dipping process is carried out under the ultrasonic condition, the ultrasonic power is 200-600W, and the ultrasonic time is 0.5-3 hours. The purpose of this step is to fully impregnate the network structure of the polymer aerogel with the carbohydrate solution.
Furthermore, the low-temperature carbonization reaction in the first step is preferably carried out in a tube furnace, and the carbonization temperature is 250-450 ℃ for 1-10 hours under the atmosphere of inert gas; the flow rate of the inert gas is 1-100 mL/min. The inert gas is one, two or more of nitrogen, argon and helium.
Further, in the second step, the organic phase change material includes paraffin, fatty acid or polyalcohol; preferably, one, two or more of lauric acid, stearic acid, palmitic acid, myristic acid, capric acid, pentaerythritol, neopentyl glycol, paraffin of 17-36 carbon atoms and polyethylene glycol of average molecular weight 600-10000 are included.
Further, the organic phase change material melt is a phase change material in a state of 10-30 ℃ above the melting point of the organic phase change material, and the dipping time is 6-36 hours.
The polymer aerogel organic phase change composite material is prepared by adopting the preparation method of the organic phase change composite material.
The preparation method of the organic phase-change composite material and the prepared polymer aerogel organic phase-change composite material have the following beneficial effects:
1. according to the preparation method of the polymer aerogel organic phase change composite material, the polymer nanofiber aerogel is soaked in a carbohydrate solution and carbonized at low temperature, a carbon layer is coated on the outer wall of the fiber, and then the organic phase change material is soaked in vacuum to prepare the aerogel organic phase change composite material, so that the preparation method is economical and environment-friendly;
2. the carbon layer coated outside the polymer aerogel not only increases the wettability of the aerogel carrier and the organic phase change material, but also increases the heat conductivity coefficient of the material;
3. according to the invention, polymer aerogel with higher thermal decomposition temperature is used as a carrier material, so that the thermal stability of the phase-change composite material is improved;
4. because the polymer aerogel has extremely low density, extremely high porosity and specific surface area, the encapsulation rate (namely, the loading rate, which refers to the mass ratio of the organic phase change material to the whole composite material) can be greatly improved by adopting the polymer aerogel as the carrier material of the phase change material;
5. the polymer aerogel is easy to form, can be used for preparing nano particles, fibers or lamellar structures, and can be designed according to different requirements so as to meet different application scenes;
6. the polymer aerogel organic phase change composite material provided by the invention has the advantages of high encapsulation rate, high heat conductivity, high phase change latent heat, good circulation stability and the like, and can be used in the fields of solar energy utilization, novel green building, industrial heat recovery, communication, clothing and the like;
7. the preparation method of the organic phase-change composite material has the advantages of simple process, convenient operation, low equipment requirement, large-scale preparation and industrial production application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the related art, the drawings that are required to be used in the description of the embodiments or the related art will be briefly described, and it is apparent that the drawings in the description below are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort for those skilled in the art.
FIG. 1 is a graph of a sample of polymer aerogel impregnated with sucrose solutions of varying concentrations after carbonization;
FIG. 2 is a scanning electron microscope image of the polymer aerogel coated with the carbon layer and its organic phase change composite material of example 1;
FIG. 3 is a DSC profile of the polymer aerogel organic phase change composite prepared in example 1;
FIG. 4 is a graph of the thermal weight loss spectrum of the polymer aerogel organic phase change composite prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention, i.e., the embodiments described are merely some, but not all, of the embodiments of the invention.
Thus, the following detailed description of the embodiments of the invention, as provided, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
Example 1:
immersing the poly-p-phenylene terephthalamide aerogel (porosity 94.7%) in a sucrose solution (sucrose 15g, water 85 g), vacuumizing, putting the system in an ultrasonic cleaner (200W) for 1.5 hours, taking out, and freeze-drying; and then placing the sucrose-impregnated poly-p-phenylene terephthalamide aerogel into a quartz tube of a tube furnace, and filling argon into the system at the argon flow of 10-20 mL/min to ensure that the quartz tube is free of active gases such as oxygen and the like, wherein the carbonization temperature is 350 ℃ and the carbonization time is 3 hours, so as to form the carbon-coated aerogel material.
Vacuum impregnation is adopted, the aerogel material coated by carbon is subjected to vacuum impregnation in polyethylene glycol (average molecular weight 4000) melt (80 ℃), the aerogel material impregnated with polyethylene glycol is taken out after 24 hours, and is placed into a 100 ℃ oven to be heated to constant weight, so that the polymer aerogel organic phase change composite material is obtained, and the mark is C1.
As a result of carbonization treatment of the prepared polymer aerogel with 10%, 15% and 30% sucrose solutions, respectively, referring to fig. 1, it can be seen that the higher the concentration of the impregnated sucrose solution, the thicker the coated carbon layer.
Referring to fig. 2, the left image is a scanning electron microscope image of the polymer aerogel coated with the carbon layer, and the outer wall of the network structure of the polymer aerogel is coated with the carbon layer; the right image is a scanning electron microscope image of the organic phase-change composite material C1 obtained after immersing in polyethylene glycol.
Referring to fig. 3, a DSC diagram of the polymer aerogel organic phase-change composite material C1 prepared in example 1 is shown, gray is a first thermal cycle curve, black is a DSC curve after 100 cycles, and it can be seen that the organic phase-change composite material C1 has high enthalpy, strong heat absorbing and releasing capability, and good Chu Reneng force.
The encapsulation efficiency of the polymer aerogel organic phase change composite C1 prepared in example 1 was 91.8% by weighing, and the encapsulation efficiency obtained by the test was 92.57%, please refer to fig. 4, which is specifically described as follows:
1. c1 has no thermal weight loss within 350 ℃, which indicates that the material has good thermal stability;
2. the weight loss gradually occurs after the temperature exceeds 350 ℃, the decomposition of the phase change material is completed at about 600 ℃, the weight loss reaches 92.57%, the encapsulation rate of the phase change material is up to 92.57%, and the test result is basically consistent with the calculation result.
Example 2:
this example is similar to example 1, except that the sucrose solution concentration is changed to 10g sucrose and 90g water, and the conditions are the same, to obtain a polymer aerogel organic phase change composite, labeled C2.
Example 3:
immersing the poly (paraphenylene terephthalamide) aerogel (porosity 94.7%) in a glucose solution (glucose 25g, water 75 g), vacuumizing, putting the system in an ultrasonic cleaner (300W) for 1.5 hours, taking out, and freeze-drying; and then placing the poly-p-phenylene terephthalamide aerogel impregnated with glucose into a quartz tube of a tube furnace, filling argon into the system, wherein the flow rate of the argon is 10-20 mL/min, so that the quartz tube is free of active gases such as oxygen and the like, the carbonization temperature is 350 ℃, and the time is 4 hours, and forming the carbon-coated aerogel material.
Vacuum impregnation is adopted, the aerogel material coated by carbon is vacuum impregnated in polyethylene glycol (average molecular weight 4000) melt (80 ℃), after 18 hours, the aerogel material impregnated with polyethylene glycol is taken out, and is put into a 100 ℃ oven to be heated to constant weight, so that the polymer aerogel organic phase change composite material is obtained, and the mark is C3.
Example 4:
immersing polyimide aerogel (porosity 91%) in starch solution (starch 5g, water 95 g), vacuumizing, placing the system in an ultrasonic cleaner (300W) for 1.5 hours, taking out, and freeze-drying; and then placing the polyimide aerogel impregnated with the starch into a quartz tube of a tube furnace, and filling argon into the system, wherein the flow rate of the argon is 10-20 mL/min, so that the quartz tube is free of active gases such as oxygen and the like, the carbonization temperature is 400 ℃, and the carbonization time is 3 hours, thereby forming the carbon-coated aerogel material.
Vacuum impregnation is adopted, the aerogel material coated by the carbon is subjected to vacuum impregnation in an octadecanol melt (80 ℃), the aerogel material impregnated with the octadecanol is taken out after 18 hours, and is placed into an oven at 80 ℃ to be heated to constant weight, so that the polymer aerogel organic phase change composite material is obtained, and the mark is C4.
Example 5:
the starch solution in example 4 was changed to sucrose solution (sucrose 15g, water 85 g), the carbonization temperature was 300 ℃, the time was 5 hours, and other conditions were unchanged, to obtain a polymer aerogel organic phase change composite material, labeled C5.
Comparative example 1:
and directly dipping the poly (p-phenylene terephthalamide) aerogel in a polyethylene glycol (average molecular weight 4000) melt (80 ℃) in vacuum by adopting a vacuum dipping method, taking out the aerogel material dipped with the polyethylene glycol after 24 hours, and heating the aerogel material in a 100 ℃ oven to constant weight to obtain the polymer aerogel organic phase change composite material, wherein the mark is C6.
Comparative example 2:
and directly dipping polyimide aerogel in a stearyl alcohol melt (80 ℃) in vacuum by adopting a vacuum dipping method, taking out the aerogel material dipped with stearyl alcohol after 18 hours, and heating the aerogel material in an oven at 80 ℃ to constant weight to obtain the polymer aerogel organic phase-change composite material, wherein the mark is C7.
The encapsulation rate, latent heat of phase change, phase change temperature and heat conductivity coefficient of the polymer aerogel organic phase change composite materials prepared in each example and comparative example are shown in the following table:
as can be seen from the above table, comparative example 1 was not immersed in a carbohydrate solution, was not coated with a carbon layer, and the thermal conductivity was significantly reduced as compared with examples 1 to 3. Compared with example 2 and example 4 and example 5, the thermal conductivity is significantly reduced without immersing in the carbohydrate solution and without coating the carbon layer.
It will be appreciated by persons skilled in the art that the above embodiments are provided for illustration only and not for limitation of the invention, and that variations and modifications of the above described embodiments are intended to fall within the scope of the claims of the invention as long as they fall within the true spirit of the invention.
Claims (6)
1. The preparation method of the organic phase-change composite material is characterized by comprising the following steps of:
step one: immersing polymer aerogel in carbohydrate water solution, freeze-drying and carbonizing at low temperature to form carbon-coated aerogel material;
step two: vacuum dipping the aerogel material into an organic phase change material melt by adopting a vacuum dipping method, and then heating to remove the organic phase change material which is not adsorbed to obtain a polymer aerogel organic phase change composite material;
the polymer aerogel comprises one or more of polyimide, poly (paraphenylene terephthalamide), polybenzimidazole, polybenzoxazole, polybenzothiazole, polyether ketone and polyether ether ketone;
the polymer aerogel is in the form of powder, fiber, lamellar structure or block;
the carbohydrate comprises a monosaccharide, disaccharide, oligosaccharide or polysaccharide;
the low-temperature carbonization reaction condition in the first step is that the carbonization temperature is 250-450 ℃ for 1-10 hours under the inert gas atmosphere;
the flow rate of the inert gas is 1-100 mL/min.
2. The method for preparing an organic phase-change composite material according to claim 1, wherein,
the carbohydrate comprises one or more of glucose, fructose, galactose, maltose, sucrose, lactose, starch and pectin;
the mass concentration of the carbohydrate aqueous solution is 0.5-50%.
3. The method for preparing an organic phase-change composite material according to claim 2, wherein,
the reaction condition of the dipping in the first step is dipping for 0.5 to 36 hours under room temperature and normal pressure or room temperature and vacuum;
the dipping process is carried out under the ultrasonic condition, the ultrasonic power is 200-600W, and the ultrasonic time is 0.5-3 hours.
4. The method for preparing an organic phase-change composite material according to claim 1, wherein,
in the second step, the organic phase change material comprises paraffin, fatty acid or polyalcohol.
5. The method for preparing an organic phase change composite material according to claim 4, wherein,
the organic phase change material melt is a phase change material in a state of 10-30 ℃ above the melting point of the organic phase change material, and the dipping time is 6-36 hours.
6. A polymer aerogel organic phase change composite prepared by the method of preparing an organic phase change composite according to any one of claims 1 to 5.
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