CN114369448B - Reversible thermochromic nano capsule and preparation method thereof - Google Patents
Reversible thermochromic nano capsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a reversible thermochromic nano-capsule and a preparation method thereof, belonging to the field of nano-capsule preparation, wherein the thermochromic nano-capsule is prepared by an external immobilized particle mode, a phase change nano-capsule core material is n-tetradecyl alcohol nucleating agent modified octadecane, a shell material is silicon dioxide modified by a silane coupling agent, the core material of the external immobilized particle on the surface of the shell material is a reversible thermochromic compound prepared based on intermolecular electron transfer, the shell material is polymethyl methacrylate, and the preparation of the reversible thermochromic compound and a prepolymer of polymethyl methacrylate is finally completed according to a certain mass ratio; the thermochromic nanocapsule prepared by the method has the advantages of simple operation steps, single required processing equipment, energy saving of products and obvious color change effect, and can be widely applied to various fields such as color change fiber films, coatings and the like.
Description
Technical Field
The invention relates to the field of phase change nanocapsules, in particular to a preparation method of reversible thermochromic phase change nanocapsules.
Background
The reversible thermochromic nano capsule is a phase change energy storage material capable of controlling color change through a phase change temperature interval of a solvent in a thermochromic compound. Thermochromic capsules can be classified into low, medium and high temperatures according to temperature intervals. Thermochromic capsules can be classified into reversible and irreversible according to thermochromic properties. The reversible thermochromic nanocapsules are prepared by a method of selecting external immobilized particles because the nanocapsules have smaller volume. The patent ZL201010572467.5 relates to a philosophy and other people to prepare the thermochromic microcapsule by an in-situ polymerization method. Patent ZL201510217133.9 Zheng Lihui et al invents an organic thermochromic microcapsule with long service life and large color change gap. Meanwhile, the reversible thermochromic nanocapsules can be applied to various fields such as anti-counterfeiting coatings, cotton fabrics, fiber membranes and the like. However, thermochromic microcapsules are more, larger in particle size, smaller in specific surface area and single in preparation method.
Disclosure of Invention
In order to overcome the phenomenon that the phase change process is slowed down after the phase change material is shelled, the invention aims to: the reversible thermochromic nano capsule and the preparation method thereof are provided, and the heat transfer characteristic of the capsule is improved while the thermochromic capsule is embodied; the assembly is carried out by immobilizing particles outside the nanocapsules. The phase-change nanocapsule is prepared by a microemulsion polymerization method and internally contains a phase-change energy storage material. The core material of the external immobilized nano particle is a thermochromic compound, and the shell material is polymethyl methacrylate prepolymer. Has the temperature change warning function while storing energy, has wide application field,
in order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the preparation method of the reversible thermochromic nanocapsules specifically comprises the following steps:
step one: mixing a certain amount of n-octadecane and a nucleating agent n-tetradecanol, wherein the n-tetradecanol accounts for 5-15% of the mass fraction of the mixed solution. Sequentially adding tetraethoxysilane, a silane coupling agent, ethanol and a surfactant according to a certain proportion of 1:0.5:14.2-16:0.3-0.4, emulsifying for 2-4 min at a speed of 8000-7000r/min to form microemulsion, adding ammonia water after ultrasonic oscillation dispersion, reacting and stirring for 13-17h at a speed of 250-350r/min, and finally filtering and drying to obtain the modified phase change nanocapsule.
Step two: heating and stirring the solvent and the leuco agent for 2-7min, then adding the color-developing agent, continuously mechanically stirring, fully mixing in the heating process of heating to 70-90 ℃ to obtain transparent liquid, and stirring for 1-2h at constant temperature. Finally cooling to obtain the solid thermochromic compound.
Step three: taking a certain amount of the phase-change nanocapsules prepared in the laboratory in the first step and the thermochromic compound in the second step and distilled water according to the ratio of 1-2:1-2:50, and stirring for 3-4h in a water bath kettle at a speed of 500-600r/min under a heating environment of 50-60 ℃. Subsequently, the emulsifier sodium lauryl sulfate was added and stirred at the same speed and at the same temperature for 3-4h. And then adding an initiator and a shell material prepolymer, heating the water bath kettle to 80-90 ℃, stirring for 5-6 hours, and then filtering and drying to finally obtain the immobilized reversible thermochromic nano-capsules.
Wherein the mass ratio of the emulsifier to the thermochromic compound to the shell material prepolymer is 3-5:5:5-10.
In the second step, the mass ratio of the leuco agent to the color developing agent to the solvent is 1:3-5:50-70. Preferably the mass ratio is 1:3:50.
In the third step, the mass ratio of the emulsifier to the thermochromic compound is 3-10:5-10. Preferably the mass ratio is 3:5. The mixing amount of the initiator is 2-3% of the shell material prepolymer; preferably, the incorporation is 2%.
In the third step, the mass ratio of the thermochromic compound to the prepolymer of polymethyl methacrylate is 1:1-2.
In the first step, the nucleating agent comprises at least one of metal nano particles, alcohols and alkanes.
In the first step, the surfactant comprises cationic surfactants such as cetyl trimethyl ammonium bromide, cetyl dimethyl chloridizing discourager, stearyl trimethyl chloridizing discourager and the like.
In the second step, the solvent is one of fatty alcohol and fatty ester.
In the second step, the leuco agent is one of crystal violet lactone, tetramethyl diaminotriphenylmethane, o-cresol red and other triarylmethane compounds and phthalides thereof.
In the second step, the color reagent is one of phenol compounds such as bisphenol A, 4-dihydroxydiphenyl methane and the like.
In the third step, the initiator is azobisisobutyronitrile.
In order to achieve the above object, another technical scheme adopted by the present invention is as follows: the reversible thermochromic nano-capsule is prepared by externally immobilizing particles, and comprises a core material and a shell material, wherein the core material is n-tetradecyl alcohol nucleating agent modified octadecane, and the shell material is silicon dioxide modified by a silane coupling agent; the external immobilized particles comprise particle core materials and particle shell materials, wherein the particle core materials are reversible thermochromic compounds prepared based on intermolecular electron transfer, and the particle shell materials are polymethyl methacrylate; and the external immobilized particles are attached to the surface of the phase-change nanocapsule modified by the silane coupling agent, and finally the preparation of the reversible thermotropic hue-thinning nanocapsule is completed.
Compared with the prior art, the invention has the following advantages:
(1) The phase change nanocapsules of the external immobilized particles and the silane coupling agent modified shell material are nano-sized, the average particle diameter is 300-400nm, and the heat conductivity coefficient is 1.93W/m.K. Therefore, the material has the characteristics of thermochromic property, large specific surface area, high heat transfer efficiency and the like, and can be widely applied to the fields of medical treatment, food and the like.
(2) In the phase-change nanocapsule, the core material is modified by 15% of n-tetradecanol by mass fraction to reduce the supercooling degree, and meanwhile, the heat conductivity coefficient is improved, and compared with an unmodified phase-change nanocapsule, the supercooling degree is reduced by 49.00%, and the heat conductivity coefficient is improved by 13.76%.
(3) When the external immobilized particle shell material is formed, the emulsifier sodium dodecyl sulfate with higher chemical stability is selected, which is more favorable for the synthesis of nano-scale particles.
(4) The invention increases the color-changing warning function of the phase-change nanocapsules, and can simultaneously have energy storage capacity and color-changing effect.
Drawings
Fig. 1 is a SEM Scanning Electron Microscope (SEM) morphology diagram of the reversible thermochromic nanocapsules of example 1.
Fig. 2 is a chart of the reversible thermochromic nanocapsules DSC differential scanning calorimeter test of example 1.
Detailed Description
The present invention will be further illustrated by the following examples, but the present invention is not limited thereto.
The embodiment discloses a reversible thermochromic nano-capsule, which is prepared by an external immobilized particle mode, wherein the phase-change nano-capsule comprises a core material and a shell material, the core material is octadecane modified by a n-tetradecyl alcohol nucleating agent, and the shell material is silicon dioxide modified by a silane coupling agent; the external immobilized particles comprise particle core materials and particle shell materials, wherein the particle core materials are reversible thermochromic compounds prepared based on intermolecular electron transfer, and the particle shell materials are polymethyl methacrylate; and the external immobilized particles are attached to the surface of the phase-change nanocapsule modified by the silane coupling agent, and finally the preparation of the reversible thermochromic nanocapsule is completed.
Example 1:
mixing 4g of n-octadecane and 0.7g of n-tetradecanol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 2min at the rate of 8000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 83.2ml of ammonia water to react, stirring for 16h at the rate of 300r/min, and finally filtering and drying to obtain the modified phase-change nanocapsule.
Heating and stirring 6g of n-tetradecanol and 0.12g of crystal violet lactone for 2min, then adding 0.36g of bisphenol A, continuing to mechanically stir, fully mixing in the heating process of heating to 90 ℃ to obtain transparent liquid, stirring at a constant temperature for 1h, and finally cooling to obtain the thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath kettle at a speed of 500r/min for 3 hours at a water bath temperature of 50 ℃. Subsequently, 0.6g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. Then 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate are added, the water bath kettle is heated to 80 ℃ and stirred for 6 hours, and filtration and drying are carried out to obtain the immobilized reversible thermochromic phase change nanocapsules.
The heat storage performance of the thermally induced color change nanocapsules prepared by the method is shown in the figure 2, and the result shows that the thermally induced color change nanocapsules have heat absorption and release capability after external immobilization, the phase change temperature range is 21-33 ℃, the enthalpy value is highest compared with other examples, the thermally induced color change nanocapsules are shown in the table 1, and the color difference value delta E=23.44 before and after color change can be widely applied to the low-temperature field (< 100 ℃) in the thermally induced color materials.
Example 2:
mixing 4g of n-octadecane and 0.7g of n-tetradecyl alcohol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 4min at the speed of 7000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 100ml of ammonia water to react, stirring for 17h at the speed of 250r/min, and finally filtering and drying to obtain the modified phase-change nanocapsule.
6g of n-tetradecanol and 0.12g of crystal violet lactone are heated and stirred for 3min, then 0.36g of bisphenol A is added for continuous mechanical stirring, and the mixture is fully mixed in the heating process of raising the temperature to 80 ℃ to obtain transparent liquid, and the transparent liquid is stirred for 2h at constant temperature. Finally cooling to obtain the solid thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath kettle at a speed of 500r/min for 3 hours at a water bath temperature of 50 ℃. Subsequently, 0.6g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. Then 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate are added, the water bath kettle is heated to 80 ℃ and stirred for 6 hours, and filtration and drying are carried out to obtain the immobilized reversible thermochromic phase change nanocapsules.
Example 3:
mixing 4g of n-octadecane and 0.4g of n-tetradecanol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 3min at the speed of 7500r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 80ml of ammonia water to react, stirring for 17h at the speed of 300r/min, and finally filtering and drying to obtain the modified phase change nanocapsule.
5.6g of n-tetradecanol and 0.08g of crystal violet lactone are heated and stirred for 5min, then 0.24g of bisphenol A is added for continuous mechanical stirring, and the mixture is fully mixed in the heating process of raising the temperature to 85 ℃ to obtain transparent liquid, stirred at constant temperature for 1.5h, and finally cooled to obtain the solid thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath at a water bath temperature of 55 ℃ for 3 hours at a speed of 500 r/min. Subsequently, 0.8g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. And adding 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate, heating to 85 ℃ in a water bath, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic nanocapsules.
Example 4:
mixing 4g of n-octadecane and 0.4g of n-tetradecanol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 3min at the speed of 7500r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 80ml of ammonia water to react, stirring for 13h at the speed of 350r/min, and finally filtering and drying to obtain the modified phase change nanocapsule.
4g of n-tetradecanol and 0.08g of crystal violet lactone are heated and stirred for 5min, then 0.4g of bisphenol A is added for continuous mechanical stirring, and the mixture is fully mixed in the heating process of raising the temperature to 70 ℃ to obtain transparent liquid, and the transparent liquid is stirred for 2h at constant temperature. Finally cooling to obtain the solid thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath at a water bath temperature of 55 ℃ for 3 hours at a speed of 500 r/min. Subsequently, 0.8g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. And adding 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate, heating to 85 ℃ in a water bath, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic nanocapsules.
Example 5:
mixing 4g of n-octadecane and 0.2g of n-tetradecyl alcohol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 4min at the speed of 7000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 77ml of ammonia water to react, stirring for 16h at the speed of 300r/min, and finally filtering and drying to obtain the modified phase-change nanocapsule.
14g of n-tetradecanol and 0.2g of crystal violet lactone are heated and stirred for 7min, then 1g of bisphenol A is added for continuous mechanical stirring, and the mixture is fully mixed in the heating process of heating to 90 ℃ to obtain transparent liquid, and the transparent liquid is stirred for 1h at constant temperature. Finally cooling to obtain the solid thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath at a water bath temperature of 55 ℃ for 4 hours at a speed of 500/min. Subsequently, 1g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. And adding 0.04g of azodiisobutyronitrile and 2ml of methyl methacrylate, heating to 90 ℃ in a water bath, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic nanocapsules.
Example 6:
mixing 4g of n-octadecane and 0.2g of nano alumina, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 2min at the rate of 8000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 84ml of ammonia water to react, stirring for 16h at the rate of 300r/min, and finally filtering and drying to obtain the modified phase-change nano capsule.
6g of n-tetradecanol and 0.12g of tetramethyl diaminotriphenylmethane are heated and stirred for 2min, then 0.36g of bisphenol A is added for continuous mechanical stirring, and the mixture is fully mixed in the heating process of heating to 90 ℃ to obtain transparent liquid, and the transparent liquid is stirred for 1h at constant temperature. Finally cooling to obtain the solid thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred for 3 hours at a water bath temperature of 50 ℃ in a water bath kettle at a speed of 550/min. Subsequently, 0.6g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. And adding 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate, heating to 80 ℃ in a water bath, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic nanocapsules.
The average particle diameter of the sample obtained in this example was 600nm. Compared to example 1, the thermal conductivity is reduced by 7% and the supercooling degree is increased by 0.8 ℃, so that the nucleating agent is preferably n-tetradecanol.
Example 7:
mixing 4g of n-octadecane and 0.7g of n-tetradecanol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 2min at the rate of 8000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 83.2ml of ammonia water to react, stirring for 16h at the rate of 300r/min, and finally filtering and drying to obtain the modified phase-change nanocapsule.
Heating and stirring 6g of n-tetradecanol and 0.12g of crystal violet lactone for 2min, then adding 0.36g of bisphenol A, continuing to mechanically stir, fully mixing in the heating process of heating to 90 ℃ to obtain transparent liquid, stirring at a constant temperature for 1h, and finally cooling to obtain the thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath kettle at a speed of 500r/min for 3 hours at a water bath temperature of 50 ℃. Subsequently, 0.6g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. And adding 0.04g of azodiisobutyronitrile and 2ml of methyl methacrylate, heating the water bath to 80 ℃, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic phase change nanocapsules.
Example 8:
mixing 4g of n-octadecane and 0.7g of n-tetradecyl alcohol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 64ml of ethanol and 1.4g of hexadecyl trimethyl ammonium bromide to emulsify for 2min at the rate of 8000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 83.2ml of ammonia water to react, stirring for 16h at the rate of 300r/min, and finally filtering and drying to obtain the modified phase-change nanocapsule.
Heating and stirring 6g of n-tetradecanol and 0.12g of crystal violet lactone for 2min, then adding 0.36g of bisphenol A, continuing to mechanically stir, fully mixing in the heating process of heating to 90 ℃ to obtain transparent liquid, stirring at a constant temperature for 1h, and finally cooling to obtain the thermochromic compound.
1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water are mixed and stirred in a water bath kettle at a speed of 500r/min for 3 hours at a water bath temperature of 50 ℃. Subsequently, 0.6g of sodium dodecyl sulfate was added and stirred at the same speed and at the same temperature for 4 hours. Then 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate are added, the water bath kettle is heated to 80 ℃ and stirred for 6 hours, and filtration and drying are carried out to obtain the immobilized reversible thermochromic phase change nanocapsules.
Table 1: examples 1-8 enthalpy value comparison Table
Comparative example 1:
this comparative example, based on example 1, replaces the emulsifier with 0.05-1g of span 80 or tween 80 emulsifier, and the result shows that the discoloration fails, which proves that the emulsifier is sodium dodecyl sulfate with excellent chemical stability, and is more practical for the invention.
The above embodiments are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereto, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the present invention.
Claims (1)
1. The preparation method of the reversible thermochromic nanocapsules is characterized by comprising the following steps of:
mixing 4g of n-octadecane and 0.7g of n-tetradecanol, adding 4g of tetraethoxysilane, 2g of silane coupling agent, 56.8ml of ethanol and 1.312g of cetyl trimethyl ammonium bromide to emulsify for 2min at the rate of 8000r/min to form microemulsion, then performing ultrasonic vibration dispersion, adding 83.2ml of ammonia water to react, stirring for 16h at the rate of 300r/min, and finally filtering and drying to obtain modified phase-change nanocapsules;
heating and stirring 6g of n-tetradecanol and 0.12g of crystal violet lactone for 2min, then adding 0.36g of bisphenol A, continuing to mechanically stir, fully mixing in the heating process of heating to 90 ℃ to obtain transparent liquid, stirring at a constant temperature for 1h, and finally cooling to obtain a thermochromic compound;
mixing 1g of phase-change nanocapsules, 1g of thermochromic compound and 50ml of distilled water, stirring at the water bath temperature of 50 ℃ in a water bath kettle at the speed of 500r/min for 3 hours, and then adding 0.6g of sodium dodecyl sulfate and stirring at the same speed and the same temperature for 4 hours; and adding 0.02g of azodiisobutyronitrile and 1ml of methyl methacrylate, heating the water bath to 80 ℃, stirring for 6 hours, and filtering and drying to obtain the immobilized reversible thermochromic phase change nanocapsules.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109575911A (en) * | 2018-12-29 | 2019-04-05 | 江南大学 | Strawberry shape thermochromism energy storage material and the preparation method and application thereof |
| CN110951465A (en) * | 2019-12-13 | 2020-04-03 | 天津优米优科技有限公司 | Novel phase change capsule and preparation method thereof |
| CN113025285A (en) * | 2021-03-15 | 2021-06-25 | 深圳华力兴新材料股份有限公司 | Phase-change energy-storage microcapsule and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109575911A (en) * | 2018-12-29 | 2019-04-05 | 江南大学 | Strawberry shape thermochromism energy storage material and the preparation method and application thereof |
| CN110951465A (en) * | 2019-12-13 | 2020-04-03 | 天津优米优科技有限公司 | Novel phase change capsule and preparation method thereof |
| CN113025285A (en) * | 2021-03-15 | 2021-06-25 | 深圳华力兴新材料股份有限公司 | Phase-change energy-storage microcapsule and preparation method and application thereof |
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| Title |
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