CN112940689A - Composite phase change material for diving suit and preparation method thereof - Google Patents

Composite phase change material for diving suit and preparation method thereof Download PDF

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CN112940689A
CN112940689A CN202110159792.7A CN202110159792A CN112940689A CN 112940689 A CN112940689 A CN 112940689A CN 202110159792 A CN202110159792 A CN 202110159792A CN 112940689 A CN112940689 A CN 112940689A
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microcrystalline cellulose
bentonite
chitosan
change material
solution
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CN112940689B (en
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赵旭
陈妍
王晓伟
李浩佳
谢云龙
刘琴
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Zhejiang Ocean University ZJOU
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B63SHIPS OR OTHER WATERBORNE VESSELS; RELATED EQUIPMENT
    • B63CLAUNCHING, HAULING-OUT, OR DRY-DOCKING OF VESSELS; LIFE-SAVING IN WATER; EQUIPMENT FOR DWELLING OR WORKING UNDER WATER; MEANS FOR SALVAGING OR SEARCHING FOR UNDERWATER OBJECTS
    • B63C11/00Equipment for dwelling or working underwater; Means for searching for underwater objects
    • B63C11/02Divers' equipment
    • B63C11/04Resilient suits

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Abstract

The invention provides a composite phase change material for diving suit, which is prepared by the following steps: s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution to obtain a microcrystalline cellulose solution; s2, adding chitosan into an acetic acid aqueous solution, stirring, adding bentonite, and uniformly mixing to obtain a bentonite-chitosan solution; s3, mixing the microcrystalline cellulose solution with the bentonite chitosan solution, and stirring to obtain hydrogel; s4, freezing and drying the hydrogel to obtain aerogel powder; s5, removing residual sodium hydroxide and urea from the aerogel powder, and freeze-drying to obtain bentonite-chitosan-microcrystalline cellulose aerogel; s6, immersing bentonite-chitosan-microcrystalline cellulose aerogel into the melted n-decanoic acid under a vacuum environment to obtain a mixture; s7, adsorbing excessive n-capric acid on the mixture on filter paper. The invention also provides a preparation method of the composite phase change material. The composite phase-change material provided by the invention fixes the phase-change material in the aerogel, and has better thermal stability.

Description

Composite phase change material for diving suit and preparation method thereof
Technical Field
The invention relates to a phase change material, in particular to a composite phase change material for diving suit and a preparation method thereof.
Background
Current wetsuits are classified into wet wetsuits, jellyfish suits, dry wetsuits:
1. the wet-type diving suit can enter water, is not suitable for deep diving, is easy to cause body temperature imbalance and causes life danger;
2. jellyfish clothes are the most basic diving suit and are usually made of thin materials. The jellyfish clothes basically have no cold-proof effect mainly to avoid being scratched and sting by jellyfishes or other aquatic organisms carelessly;
3. the dry-type diving suit is very thick and heavy, heavy to wear, and expensive, and domestic three thousand plays, and foreign eight thousand plays. Therefore, the development of the novel diving suit is urgent.
A phase change material is a chemical material that uses latent heat of phase change to store and release energy, accompanied by an endothermic or exothermic phenomenon. In recent years, the application of phase change materials in the field of textile and clothing, particularly in the field of temperature-adjusting textiles and clothing, has attracted more and more attention. The temperature-regulating textile is a novel intelligent textile, and can absorb heat from the environment and store the heat in the textile or emit the heat stored in the textile according to the reversible change of liquid-solid or solid-solid of a phase-change material contained in the textile according to the change of the external environment temperature, so that microclimate with basically constant temperature is formed around the textile, and the temperature regulating function is realized. The research and development of the temperature-regulating textile and the temperature-regulating clothing phase-change material have positive practical significance for improving the wearing comfort of clothing and maintaining the physical and psychological health of human beings.
The phase change material applied to the clothing should meet the following requirements: firstly, the phase transition temperature of the phase transition material should be close to the body temperature of a human body, and the phase transition temperature is about 30 ℃ generally. The human body can regulate the heat production and the heat dissipation through self-regulation behaviors such as sweating, body surface capillary vessel expansion or contraction, muscle tension, shivering and the like, so that the core temperature of the human body is maintained in a basically normal range. When the environmental temperature is seriously deviated from 30 ℃, a human body must control the heat flow between the human body and the environment by means of the enclosure structure, a microclimate area with proper temperature is formed between the surface of the human body and the enclosure structure, so that the human body has proper body temperature and comfortable feeling, clothing, bedding, tents, houses and auxiliary air conditioning equipment are typical enclosure structures, and obviously, if the phase change temperature of the phase change material is excessively higher or lower than 30 ℃, the phase change material cannot play a role in regulating the body temperature. Secondly, the heat capacity is large, that is, not only the latent heat of phase change needs to be high, but also the latent heat of phase change per unit mass and unit volume needs to be large enough. And thirdly, the glass must be melted and solidified at a constant temperature, namely reversible phase change is required, and supercooling phenomenon (or small supercooling degree) does not occur. Fourthly, the crystal is nontoxic and noncorrosive to human bodies, has higher crystallization speed and crystal growth speed, smaller volume expansion rate, higher density, easily purchased raw materials and low price. The phase-change temperature, the price and the source of raw materials and the non-toxicity are key factors influencing the application of the phase-change material.
The organic phase-change material has the advantages of low price, good chemical stability and thermal stability, no supercooling and phase separation phenomenon, low corrosivity and toxicity and the like, and becomes the most concerned phase-change material in current research and use. However, the organic phase-change material has the problem that the liquid phase is easy to leak in the solid-liquid phase-change process, so that the application of the organic phase-change material is limited. Therefore, finding a carrier material capable of well encapsulating the organic phase change material becomes a key technology for promoting the popularization and application of the carrier material.
Disclosure of Invention
The invention aims to provide a composite phase change material for diving suit, which is fixed in aerogel and has better thermal stability.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a composite phase change material for wetsuits, which is prepared by the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution, stirring for 60-120 minutes, adding bentonite, and stirring until the mixture is uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 with the bentonite chitosan solution obtained in the step S2, and stirring until the mixture is in a gel state to obtain hydrogel;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 1-3 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 1-3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid in a vacuum environment, soaking for 10 minutes, then turning on a vacuum pump for 10 minutes, then cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Further, the sodium hydroxide urea aqueous solution comprises sodium hydroxide, urea and water in a mass ratio of 7:14:79, and the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is (2-4) g:100mL:1g:100mL:500 mg.
Further, in step S2 of the present invention, the volume fraction of the aqueous acetic acid solution was 1%, and the stirring speed was 300 r/min.
Further, in step S3 of the present invention, the volume ratio of the microcrystalline cellulose solution to the bentonite-chitosan solution is 1: 1.
Further, in step S6 of the present invention, the weight ratio of the n-decanoic acid to the bentonite-chitosan-microcrystalline cellulose aerogel is 15: 1.
Another technical problem to be solved by the present invention is to provide a method for preparing the above composite phase change material for diving suit.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of a composite phase change material for diving suits comprises the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution, stirring for 60-120 minutes, adding bentonite, and stirring until the mixture is uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 with the bentonite chitosan solution obtained in the step S2, and stirring until the mixture is in a gel state to obtain hydrogel;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 1-3 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 1-3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid in a vacuum environment, soaking for 10 minutes, then turning on a vacuum pump for 10 minutes, then cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Further, the sodium hydroxide urea aqueous solution comprises sodium hydroxide, urea and water in a mass ratio of 7:14:79, and the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is (2-4) g:100mL:1g:100mL:500 mg.
Further, in step S2 of the present invention, the volume fraction of the aqueous acetic acid solution was 1%, and the stirring speed was 300 r/min.
Further, in step S3 of the present invention, the volume ratio of the microcrystalline cellulose solution to the bentonite-chitosan solution is 1: 1.
Further, in step S6 of the present invention, the weight ratio of the n-decanoic acid to the bentonite-chitosan-microcrystalline cellulose aerogel is 15: 1.
Compared with the prior art, the invention has the following beneficial effects:
1) according to the invention, bentonite-chitosan-microcrystalline cellulose aerogel is used as a carrier, and the phase-change material n-decanoic acid is mixed with the carrier by a vacuum impregnation method and then is placed in a vacuum environment together, so that air in the original aerogel is pumped out, and the n-decanoic acid can enter the carrier more easily, thus the composite phase-change material capable of being used for diving suit is prepared. Wherein, the bentonite and the chitosan can play a role in expansion, the water absorption of the aerogel is improved, and the microcrystalline cellulose has high adhesion, so that the adsorption quantity of the aerogel on the n-capric acid can be improved.
2) The vacuum impregnation method used in the invention belongs to one of physical adsorption, but compared with common physical adsorption, the vacuum impregnation method can greatly improve the adsorption capacity and the thermal stability of the phase-change material, and actual tests show that the load capacity of the bentonite-chitosan-microcrystalline cellulose aerogel prepared by the invention is about 90%.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a TGA profile of example 1 of the present invention with n-decanoic acid;
FIG. 2 is a diffraction scan of example 1 of the present invention with n-decanoic acid;
FIG. 3 is an infrared spectrum of bentonite-chitosan-microcrystalline cellulose aerogel and n-decanoic acid in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, and the exemplary embodiments and descriptions thereof herein are provided to explain the present invention but not to limit the present invention.
Example 1
The composite phase change material for the diving suit is prepared according to the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution consisting of sodium hydroxide, urea and water in a mass ratio of 7:14:79, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution with the volume fraction of 1%, stirring at the speed of 300r/min for 90 minutes, adding bentonite, and stirring until the bentonite and the chitosan are uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 and the bentonite chitosan solution obtained in the step S2 in a volume ratio of 1:1, and stirring the mixture until the mixture is gelatinous to obtain hydrogel, wherein the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is 3g:100mL:1g:100mL:500 mg;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 2 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 2 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid according to the weight ratio of 1:15 in a vacuum environment, soaking for 10 minutes, turning on a vacuum pump for 10 minutes, cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Example 2
The composite phase change material for the diving suit is prepared according to the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution consisting of sodium hydroxide, urea and water in a mass ratio of 7:14:79, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution with the volume fraction of 1%, stirring at the speed of 300r/min for 60 minutes, adding bentonite, and stirring until the bentonite and the chitosan are uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 and the bentonite chitosan solution obtained in the step S2 in a volume ratio of 1:1, and stirring the mixture until the mixture is gelatinous to obtain hydrogel, wherein the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is 4g:100mL:1g:100mL:500 mg;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 1 day to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid according to the weight ratio of 1:15 in a vacuum environment, soaking for 10 minutes, turning on a vacuum pump for 10 minutes, cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Example 3
The composite phase change material for the diving suit is prepared according to the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution consisting of sodium hydroxide, urea and water in a mass ratio of 7:14:79, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution with the volume fraction of 1%, stirring at the speed of 300r/min for 120 minutes, adding bentonite, and stirring until the mixture is uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 and the bentonite chitosan solution obtained in the step S2 in a volume ratio of 1:1, and stirring the mixture until the mixture is gelatinous to obtain hydrogel, wherein the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is 2g:100mL:1g:100mL:500 mg;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 3 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 1 day to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid according to the weight ratio of 1:15 in a vacuum environment, soaking for 10 minutes, turning on a vacuum pump for 10 minutes, cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Example 4
The composite phase change material for the diving suit is prepared according to the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution consisting of sodium hydroxide, urea and water in a mass ratio of 7:14:79, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution with the volume fraction of 1%, stirring at the speed of 300r/min for 75 minutes, adding bentonite, and stirring until the bentonite and the chitosan are uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 and the bentonite chitosan solution obtained in the step S2 in a volume ratio of 1:1, and stirring the mixture until the mixture is gelatinous to obtain hydrogel, wherein the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is 3.5g:100mL:1g:100mL:500 mg;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 2 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid according to the weight ratio of 1:15 in a vacuum environment, soaking for 10 minutes, turning on a vacuum pump for 10 minutes, cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
Experimental example 1: thermal stability test
The TGA graph obtained by thermogravimetric analysis of example 1 and n-decanoic acid is shown in FIG. 1, and the detailed data is shown in Table 1:
Figure BDA0002935967690000071
TABLE 1
Thermal stability is an essential parameter of phase change materials. As shown in fig. 1 and table 1, the mass loss of both the n-decanoic acid and example 1 during thermal decomposition was accomplished in only one step. The mass of the n-decanoic acid was only 4.3% remaining, whereas the remaining mass of example 1 was 27.6%. Considering that 90% of the n-decanoic acid is contained in the composite phase change material, this indicates that the distribution of the n-decanoic acid in the composite phase change material prepared by the present invention is uniform. When the temperature is lower than 300 ℃, almost no weight loss of the n-decanoic acid is caused in the example 1, and when the temperature is increased to about 390 ℃, the quality of the pure decanoic acid is rapidly reduced due to the disintegration of the molecular chain of the n-decanoic acid, and the obvious decomposition reaction is not found in the process of 20 ℃ to 375 ℃ in the example 1, which shows that the composite phase change material prepared by the invention has good thermal stability at 375 ℃.
Experimental example 2: test of crystallization Property
Diffraction scanning was performed on example 1 and n-decanoic acid, and the range 2 θ was from 10 to 60 ° as shown in fig. 2. As can be seen from fig. 2, the peaks at about 19 °, 22 °, 26 ° and 37 ° belong to the n-decanoic acid crystals, whereas the typical amorphous structure of the composite phase change material is found between 20 ° and 30 ° for the broad peaks. A sharp diffraction peak of n-decanoic acid was observed in example 1, indicating that the crystal structure of n-decanoic acid was not disrupted. These findings confirm that no chemical reaction occurs between the n-decanoic acid and the bentonite-chitosan-microcrystalline cellulose aerogel, but that it is physically bound.
Experimental example 3: chemical property test
Infrared spectroscopy can provide useful information about the way the molecules are made, and can reveal the binding mode and chemical properties of n-decanoic acid/bentonite-chitosan-microcrystalline cellulose aerogel and n-decanoic acid. The infrared spectra of the bentonite-chitosan-microcrystalline cellulose aerogel and n-decanoic acid in example 1 are shown in FIG. 3, and can be seen from FIG. 3 at 964cm-1And 2880cm-1In which C-H and-CH appear2Typical stretching vibration peaks. The influence of the i group causes n-decanoic acid to be 474cm-1、845cm-1And 1110cm-1Where a vibration occursA similar vibration peak occurred in example 1. Comparing the infrared spectrum of example 1 with that of n-decanoic acid and bentonite-chitosan-microcrystalline cellulose aerogel, it can be seen that the peak values of all major peaks of n-decanoic acid and bentonite-chitosan-microcrystalline cellulose aerogel are not observed with a clear new peak except for some slight changes, indicating that there is only physical adsorption between n-decanoic acid and bentonite-chitosan-microcrystalline cellulose aerogel.
Experimental example four: load capacity test
The loading of the composite phase change materials obtained in examples 1-4 was calculated according to the following formula:
load capacity (mass of composite phase change material obtained in step S7-mass of bentonite-chitosan-microcrystalline cellulose aerogel added in step S6)/mass of composite phase change material obtained in step S7 × 100%
The test results are shown in table 2:
load (%)
Example 1 90.3
Example 2 90.1
Example 3 90.0
Example 4 90.2
TABLE 2
As can be seen from Table 2, the loading amounts of the embodiments 1 to 4 of the present invention all reach more than 90%, which indicates that the encapsulation of the n-decanoic acid by using the method of the present invention can reach higher loading amounts.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A composite phase change material for a wetsuit, comprising: the preparation method comprises the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution, stirring for 60-120 minutes, adding bentonite, and stirring until the mixture is uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 with the bentonite chitosan solution obtained in the step S2, and stirring until the mixture is in a gel state to obtain hydrogel;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 1-3 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 1-3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid in a vacuum environment, soaking for 10 minutes, then turning on a vacuum pump for 10 minutes, then cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
2. The composite phase change material for wetsuits according to claim 1, wherein: the sodium hydroxide urea aqueous solution comprises sodium hydroxide, urea and water in a mass ratio of 7:14:79, and the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is (2-4) g:100mL:1g:100mL:500 mg.
3. The composite phase change material for wetsuits according to claim 1, wherein: in the step S2, the volume fraction of the acetic acid aqueous solution is 1%, and the stirring speed is 300 r/min.
4. The composite phase change material for wetsuits according to claim 1, wherein: in the step S3, the volume ratio of the microcrystalline cellulose solution to the bentonite-chitosan solution is 1: 1.
5. The composite phase change material for wetsuits according to claim 1, wherein: in the step S6, the weight ratio of the n-decanoic acid to the bentonite-chitosan-microcrystalline cellulose aerogel is 15: 1.
6. The method for preparing a composite phase change material for wetsuits according to any one of claims 1 to 5, wherein the method comprises the following steps: the method comprises the following steps:
s1, adding microcrystalline cellulose into a sodium hydroxide urea aqueous solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a microcrystalline cellulose solution;
s2, adding chitosan into an acetic acid aqueous solution, stirring for 60-120 minutes, adding bentonite, and stirring until the mixture is uniformly mixed to obtain a bentonite-chitosan solution;
s3, mixing the microcrystalline cellulose solution obtained in the step S1 with the bentonite chitosan solution obtained in the step S2, and stirring until the mixture is in a gel state to obtain hydrogel;
s4, pouring the hydrogel obtained in the step S3 into a polytetrafluoroethylene beaker, and freeze-drying for 1-3 days to obtain aerogel powder;
s5, soaking the aerogel powder obtained in the step S4 in an ethanol water solution for 12 hours, taking out the aerogel powder, soaking the aerogel powder in deionized water for 12 hours, removing residual sodium hydroxide and urea, and freeze-drying for 1-3 days to obtain bentonite-chitosan-microcrystalline cellulose aerogel;
s6, heating n-decanoic acid to 65 ℃ to melt the n-decanoic acid, immersing the bentonite-chitosan-microcrystalline cellulose aerogel obtained in the step S5 into the melted n-decanoic acid in a vacuum environment, soaking for 10 minutes, then turning on a vacuum pump for 10 minutes, then cooling for 10 minutes, circulating for 3 times, and taking out to obtain a mixture;
s7, placing the mixture obtained in the step S6 on weighing paper at room temperature, and adsorbing excessive n-capric acid adsorbed on the surface of the bentonite-chitosan-microcrystalline cellulose aerogel on the filter paper until the mass of the mixture is not changed any more to obtain the composite phase-change material for the diving suit.
7. The method for preparing a composite phase change material for wetsuits according to claim 6, wherein: the sodium hydroxide urea aqueous solution comprises sodium hydroxide, urea and water in a mass ratio of 7:14:79, and the ratio of the microcrystalline cellulose to the sodium hydroxide urea aqueous solution to the chitosan to the acetic acid aqueous solution to the bentonite is (2-4) g:100mL:1g:100mL:500 mg.
8. The method for preparing a composite phase change material for wetsuits according to claim 6, wherein: in the step S2, the volume fraction of the acetic acid aqueous solution is 1%, and the stirring speed is 300 r/min.
9. The method for preparing a composite phase change material for wetsuits according to claim 6, wherein: in the step S3, the volume ratio of the microcrystalline cellulose solution to the bentonite-chitosan solution is 1: 1.
10. The method for preparing a composite phase change material for wetsuits according to claim 6, wherein: in the step S6, the weight ratio of the n-decanoic acid to the bentonite-chitosan-microcrystalline cellulose aerogel is 15: 1.
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