CN111205829A - Preparation method and application of phase change-infrared stealth bifunctional composite microcapsule - Google Patents
Preparation method and application of phase change-infrared stealth bifunctional composite microcapsule Download PDFInfo
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- CN111205829A CN111205829A CN202010033458.2A CN202010033458A CN111205829A CN 111205829 A CN111205829 A CN 111205829A CN 202010033458 A CN202010033458 A CN 202010033458A CN 111205829 A CN111205829 A CN 111205829A
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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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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/002—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches with controlled internal environment
- A41D13/005—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches with controlled internal environment with controlled temperature
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
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Abstract
The invention discloses a preparation method and application of a composite microcapsule phase change material with double functions of heat storage and temperature control and infrared stealth. For the sake of simpler explanation, the description first coats the mask inside, and the infrared stealth performance of the mask wearing area and other areas is tested and compared.
Description
Technical Field
The invention relates to the technical field of phase change microcapsule preparation, in particular to a preparation method and application of a phase change-infrared stealth bifunctional composite microcapsule phase change material.
Background
Due to the universality of infrared radiation of objects and the difference between target and background infrared radiation, thermal infrared detection plays an increasingly important role in modern military reconnaissance, and seriously threatens the viability of some military targets. The thermal infrared stealth material can reduce the infrared radiation intensity difference between the target and the background to the extent that the thermal infrared detector cannot identify the difference, thereby achieving the purpose of stealth in relative meaning. Therefore, the thermal infrared stealth technology for the purpose of reducing the radiation intensity on the surface of an object has attracted high attention from the military in various countries. It is known from stefan-boltzmann's law that reducing the intensity of radiation at the target surface can be controlled by reducing the temperature and infrared emissivity of the target surface. In the current research, the infrared stealth coating with low emissivity is mainly widely applied, but the infrared stealth coating which takes infrared emissivity control as a fundamental approach has poor tolerance to the surrounding complex environment, poor stealth effect and easy oxidation and corrosion, and the emissivity is increased along with the increase of the service time, so that the stealth effect is lost, and the stealth time is short.
In summary, how to obtain a thermal infrared stealth material with low emissivity, temperature control, stable performance and long action time is a problem which needs to be researched urgently at present.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a bifunctional composite microcapsule phase change material with a core-shell structure, which is used for solving the problems in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
a preparation method and application of a bifunctional composite microcapsule phase change material with a core-shell structure are provided, wherein the bifunctional composite microcapsule phase change material mainly comprises a core material and a wall material.
Preferably, the core material is stearic acid.
Preferably, the wall material is a mixture of calcium carbonate and nano-iron.
Preferably, the double functions are heat storage and temperature control and infrared stealth functions.
The embodiment of the invention also provides a method for preparing the bifunctional composite microcapsule phase change material, which is an in-situ polymerization method.
Preferably, the preparation steps of the bifunctional composite microcapsule phase change material are as follows:
(1) dissolving a certain amount of stearic acid, sodium dodecyl benzene sulfonate and calcium chloride in a certain amount of deionized water, and stirring at a constant temperature of 70 ℃ for 60min by using a magnetic stirrer to obtain a component A;
(2) dissolving a certain amount of sodium carbonate in a certain amount of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding a certain amount of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with anhydrous ethanol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample.
Preferably, the sodium dodecyl benzene sulfonate plays a role of an emulsifier, and the dosage of the emulsifier is 1% -10% of that of stearic acid.
Preferably, the calcium chloride and the sodium carbonate are raw materials for preparing the calcium carbonate wall material.
Preferably, the mass ratio of the stearic acid to the calcium carbonate is 3: 1.
Preferably, the particle size of the nano iron powder is 30nm, 50nm and 100nm, and the nano iron powder accounts for 0-10% of the using amount of stearic acid.
Preferably, the multifunctional composite microcapsule phase change material is applied to processing the multifunctional composite microcapsule phase change material into an interlayer, and the interlayer is coated on the hollow part of the clothes in a coating treatment mode to obtain the phase change temperature control-infrared stealth night clothes.
The invention has the beneficial effects that:
the stealth effect is better. Stearic acid as an organic phase-change material has the functions of heat storage and temperature control, can control the surface temperature of a target and reduce the temperature difference with the surrounding environment of the target, thereby achieving the purpose of stealth; meanwhile, the nano iron powder is used as a low-emissivity material, the infrared emissivity of the surface of the target can be reduced after doping, the radiation intensity of the surface of the target is reduced from two aspects of surface temperature and surface emissivity, and the stealth effect is better.
The performance is more stable and the action time is long. The microcapsule technology and interlayer treatment can reduce the contact and reaction between the composite stealth material and the external environment, reduce oxidation and corrosion, prevent leakage and coating pollution, prolong the service life and enable the target to achieve the stealth purpose for a long time.
The wearing is more comfortable. The composite stealth material can control the temperature of the surface of a target, so that the temperature difference between the target and the ambient environment can be basically ignored within a certain time range, the adverse effect of the extremely severe environment on the target is eliminated, and the wearing comfort is good.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
FIG. 1 is a flow chart of a process for preparing a sample of microcapsules according to an embodiment of the present invention.
FIG. 2 is a plot of the IR emissivity of a sample of microcapsules according to an embodiment of the present invention.
FIG. 3 is a graph showing the actual stealth effect of the microcapsule sample according to the embodiment of the present invention.
Detailed Description
Fig. 1 is a flow chart of a process for preparing a microcapsule sample according to an embodiment of the present invention, and the following embodiments are provided to illustrate the embodiments of the present invention, and it is obvious that the embodiments described are a part of the embodiments of the present invention, but not all embodiments of the present invention, and those skilled in the art can easily understand other advantages and effects of the present invention from the disclosure of the present specification. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding 0.04g of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with absolute ethyl alcohol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample Fe-SA-1.
Example 2
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding 0.12g of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with absolute ethyl alcohol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample Fe-SA-3.
Example 3
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding 0.20g of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with absolute ethyl alcohol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample Fe-SA-5.
Example 4
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding 0.28g of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with absolute ethyl alcohol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample Fe-SA-7.
Example 5
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding 0.40g of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with absolute ethyl alcohol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample Fe-SA-10.
Comparative examples
(1) Dissolving 4.00g of stearic acid, 0.12g of sodium dodecyl benzene sulfonate and 1.48g of calcium chloride in 100ml of deionized water, and stirring for 60min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain a component A;
(2) dissolving 1.41g of sodium carbonate in 20ml of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) slowly dripping the component B obtained in the step (2) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(4) standing for 12h, filtering microcapsule liquid, washing the residue with anhydrous ethanol and deionized water respectively for 3 times, and drying in drying oven at 60 deg.C for 12h to obtain microcapsule powder sample SA-CaCO3。
In embodiments 1 to 5 of the present invention, the particle size of the nano iron powder is 50nm, and the amount of the nano iron powder is 1% to 10% of the amount of stearic acid.
In the comparative example of the invention, the content of the nano iron powder is 0%, which is in contrast to examples 1 to 5.
In the embodiment of the invention, the dosage of the sodium dodecyl benzene sulfonate is 3% of that of stearic acid.
In the embodiment of the invention, the stearic acid is provided by the chemical corporation of Shingan chemical industry, the purity is analytically pure, the stearic acid has a white and glossy leaf-shaped crystal property, and the phase transition temperature is 52 ℃.
Example 6
The prepared composite microcapsule phase-change material is processed into an interlayer, and the interlayer is coated on the hollow part of the clothes in a coating treatment mode to obtain the phase-change temperature-control infrared stealth night clothes. For the sake of simplicity, this example first coats the mask interior and tests and compares the infrared stealth performance of the mask worn area with that of the other areas.
The infrared emissivity of the composite microcapsule phase change material provided in examples 1 to 5 and comparative example is measured, and the test result is shown in fig. 2, the infrared emissivity of the microcapsule sample is between 0.39 and 0.86, and decreases with the increase of the mass ratio of nano iron to stearic acid. When the mass ratio of the nano-iron to the stearic acid is 10 percent, namely the Fe-SA-10 infrared emissivity in the example 5 is the minimum, compared with the undoped nano-iron, namely the SA-CaCO in the comparative example3The reduction of 54.7 percent, and the doping of the nano iron well improves the infrared stealth performance of the microcapsule sample.
Taking Fe-SA-5 in example 3 as an example, FIG. 3 shows the infrared imaging photographs before and after the microcapsule phase change material is added to the mask. When no filling material is added into the mask, the mask shows obvious infrared characteristics under the action of the body temperature of a human body, compared with the naked human body skin, the infrared radiation intensity of the human body skin can be only slightly reduced, and the infrared radiation intensity is almost consistent with the infrared radiation intensity of the human body surface after the mask is worn for about 30min along with the time. After Fe-SA-5 is coated inside the mask, the infrared characteristics of the part of a person wearing the mask are basically consistent with those of the environment background, and when the wearing time exceeds 150min, the infrared characteristics of the wearer gradually appear.
The microcapsule sample prepared in the embodiment has good heat storage and temperature control performance of the phase change material, the temperature of the surface of a human body is basically the same as that of the ambient environment within a certain time range, meanwhile, the doped nanometer iron powder has lower surface infrared emissivity, the infrared radiation intensity is greatly reduced, the infrared characteristics of the surface of the human body are basically consistent with those of the ambient environment, and the microcapsule sample has good infrared stealth performance. When the mass ratio of the nano iron to the stearic acid is 5%, the stealth time can reach 150 min.
The prepared microcapsule phase change material is processed into an interlayer, and the interlayer is coated on the hollow part of the clothes in a coating treatment mode, so that the phase change temperature control-infrared stealth night suit can be obtained, and the phase change temperature control-infrared stealth night suit has good infrared stealth performance. Meanwhile, due to the special temperature control capability of the microcapsule phase change material, the microcapsule phase change material is used on a target in a coating or barrier shielding mode, and the surface temperature of the target is reduced by absorbing heat emitted by the target, so that the heat infrared radiation is reduced, and the stealth effect is achieved. Therefore, the bifunctional composite microcapsule phase change material has a great application prospect.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (11)
1. The preparation method and the application of the difunctional composite microcapsule phase change material with the core-shell structure are characterized in that the difunctional composite microcapsule phase change material mainly comprises a core material and a wall material.
2. The bifunctional composite microcapsule phase-change material according to claim 1,
the core material is Stearic Acid (SA).
3. The bifunctional composite microcapsule phase-change material according to claim 1,
the wall material is calcium carbonate (CaCO)3) And nano iron (Fe).
4. The bifunctional composite microcapsule phase-change material according to claim 1,
the double functions are heat storage and temperature control and infrared stealth functions.
5. A method for preparing the bifunctional composite microcapsule phase change material as claimed in claim 1, wherein the method is an in-situ polymerization method.
6. The method of claim 5,
the preparation steps of the bifunctional composite microcapsule phase change material are as follows:
(1) dissolving a certain amount of stearic acid, sodium dodecyl benzene sulfonate and calcium chloride in a certain amount of deionized water, and stirring at a constant temperature of 70 ℃ for 60min by using a magnetic stirrer to obtain a component A;
(2) dissolving a certain amount of sodium carbonate in a certain amount of deionized water, and stirring for 10min at room temperature to obtain a component B;
(3) adding a certain amount of nano iron powder into the component B in the step (2), and ultrasonically dispersing for 120min by adopting an ultrasonic instrument to obtain a component C;
(4) slowly dripping the component C obtained in the step (3) into the component A obtained in the step (1), and stirring for 120min at a constant temperature of 70 ℃ by adopting a magnetic stirrer to obtain microcapsule liquid;
(5) standing for 12h, filtering the microcapsule liquid, washing the filter residue with anhydrous ethanol and deionized water respectively for 3 times, and finally drying in a drying oven at 60 ℃ for 12h to obtain a microcapsule powder sample.
7. The method of claim 6,
the Sodium Dodecyl Benzene Sulfonate (SDBS) plays a role of an emulsifier, and the dosage of the emulsifier is 1% -10% of that of stearic acid.
8. The method of claim 6,
the calcium chloride (CaCl)2) And sodium carbonate (Na)2CO3) Is a raw material for preparing calcium carbonate wall materials.
9. The method of claim 6,
the mass ratio of the stearic acid to the calcium carbonate is 3: 1.
10. The method of claim 6,
the grain size of the nano iron powder is 30nm, 50nm and 100nm, and the dosage of the nano iron powder is 0-10% of that of stearic acid.
11. The bifunctional composite microcapsule phase-change material according to claim 1,
the application is that the phase-change temperature-control infrared invisible night suit is processed into an interlayer, and the interlayer is coated on the hollow part of the suit in a coating treatment mode to obtain the phase-change temperature-control infrared invisible night suit.
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| CN112574719A (en) * | 2020-12-29 | 2021-03-30 | 凯盛石墨碳材料有限公司 | Preparation method of phase change energy storage material based on calcium carbonate nano vesicles |
| CN112946014A (en) * | 2021-01-29 | 2021-06-11 | 中国人民解放军国防科技大学 | Method for rapidly evaluating infrared stealth performance of high-temperature stealth component based on energy contrast method |
| CN113230990A (en) * | 2021-06-15 | 2021-08-10 | 南通大学 | Microcapsule with infrared and radar stealth functions and preparation method and application thereof |
| CN115323794A (en) * | 2022-07-07 | 2022-11-11 | 合肥市盛文信息技术有限公司 | Preparation method and application of infrared stealth fabric coating fabric |
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| CN112574719A (en) * | 2020-12-29 | 2021-03-30 | 凯盛石墨碳材料有限公司 | Preparation method of phase change energy storage material based on calcium carbonate nano vesicles |
| CN112946014A (en) * | 2021-01-29 | 2021-06-11 | 中国人民解放军国防科技大学 | Method for rapidly evaluating infrared stealth performance of high-temperature stealth component based on energy contrast method |
| CN113230990A (en) * | 2021-06-15 | 2021-08-10 | 南通大学 | Microcapsule with infrared and radar stealth functions and preparation method and application thereof |
| CN115323794A (en) * | 2022-07-07 | 2022-11-11 | 合肥市盛文信息技术有限公司 | Preparation method and application of infrared stealth fabric coating fabric |
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