CN107513375B - Phase-change microcapsule coated with silicon dioxide and preparation method and application thereof - Google Patents
Phase-change microcapsule coated with silicon dioxide and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a phase-change microcapsule coated by silicon dioxide, a preparation method and application thereof, wherein the phase-change microcapsule comprises a core material and a wall material; the core material comprises a phase-change material, and the wall material is silicon dioxide; the enthalpy retention rate of the phase change microcapsule coated by the silicon dioxide is 20-99%; the average particle size of the microcapsules is 0.1-100 microns; the phase-change material coated by silicon dioxide is obtained in one step through sol-gel reaction on an emulsion interface; no toxic substance is generated in the preparation process, and the preparation process is green and environment-friendly; the prepared phase change energy storage microcapsule has high coating rate and low breakage rate, effectively reduces the supercooling degree of the phase change material, has no volatile gas, is safe to use, and expands the application range of the phase change material; the preparation method has simple process and low cost, and the used raw materials are cheap and easy to obtain and are easy to realize industrialization; the phase change energy storage microcapsule can be widely applied to the fields of textile, building energy conservation, electronic component heat management, waste heat recovery and the like.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a phase change microcapsule coated by silicon dioxide, and a preparation method and application thereof.
Background
With the continuous improvement of living standard of people, the problem of the shortage of non-renewable energy sources is getting more and more serious. In recent years, in order to reduce energy consumption and further achieve the purposes of energy conservation and energy storage, researchers invest a large amount of time, manpower and material resources. In the research of phase change energy storage technology, the development of phase change energy storage materials is the most concerned. The application of the room temperature phase change material in the aspect of building energy conservation can effectively reduce the indoor temperature fluctuation and reduce the energy consumption.
The phase-change energy storage material (hereinafter referred to as phase-change material) is a material which achieves the purposes of storing and releasing heat energy by absorbing and releasing energy in a phase-change process within a specific temperature range. The phase-change material can be used for storing energy and adjusting the temperature by utilizing heat energy provided by the environment in the phase-change process, can be repeatedly used for a long time, and has important application prospects in the fields of energy-saving and energy storage, building materials, textiles, aerospace, military and the like.
In recent years, phase change microcapsules and preparation techniques thereof have been patented, and the microcapsules can be classified into organic wall materials and inorganic wall materials according to the difference of the coated wall materials.
The organic wall material takes amino resin and a modified material system thereof as main bodies. The Chinese patent CN1903971A takes a solid-liquid phase change material as a core material, an emulsifier is directly dissolved in a melamine-formaldehyde resin prepolymer solution, and the phase change microcapsule is prepared by adopting the processes of prepolymerization, emulsification and coating in sequence, so that the problem of emulsion breaking in the coating process is effectively avoided. The Chinese patent CN1570014A takes alkane solid-liquid phase change materials as core materials, and the outer layers of the core materials are respectively coated with melamine-formaldehyde resin and PEG200 modified melamine-formaldehyde resin, so that the phase change microcapsule with complete appearance is prepared, and the sealing performance and the crushing resistance of the phase change microcapsule are improved. Although the organic wall material has a good coating effect, most of the organic wall materials are flammable, and a large amount of volatile organic compounds (such as formaldehyde) remain in the coated phase-change material, so that a great deal of potential safety hazards are brought to the practical application of the phase-change material.
Compared with organic wall materials, the inorganic wall material can not burn, and has better safety performance; in addition, the phase-change material coated by the inorganic material has the advantages of constant phase-change temperature, high energy storage density, high thermal conductivity and the like. Therefore, the phase change microcapsule coated by the inorganic material has better application prospect in the aspect of energy-saving building materials. But the mass preparation of the phase-change microcapsules coated by the inorganic material is still difficult to realize in the aspect of productivity; furthermore, there are reported phase change microcapsules coated with an inorganic material, in which the amount of the coated phase change material is much lower than that of the phase change material coated in the phase change microcapsules coated with an organic material; these defects severely limit their practical application in practical production.
Disclosure of Invention
In order to solve the defects of the prior art, one of the purposes of the invention is to provide a phase change microcapsule coated by silicon dioxide, which has extremely high enthalpy retention rate and excellent thermal property, and greatly improves the application prospect in energy-saving building materials.
The second purpose of the invention is to provide a preparation method of the phase-change microcapsule coated by the silicon dioxide; the method can efficiently control the proportion of the phase-change material and the silicon dioxide, has short production period and simple process, and is convenient for control and industrial production.
The invention also aims to provide application of the silicon dioxide coated phase change microcapsule.
The purpose of the invention is realized by the following technical scheme:
a phase change microcapsule coated with silicon dioxide, which comprises a core material and a wall material; the core material comprises a phase-change material, and the wall material is silicon dioxide; the enthalpy retention rate of the phase change microcapsule coated by the silicon dioxide is 20-99%; the average particle size of the microcapsules is 0.1-100 microns.
Preferably, the enthalpy retention rate of the phase-change microcapsule is 75-99%.
Still preferably, the enthalpy retention rate of the phase-change microcapsule is 75-95%.
More preferably, the enthalpy retention rate of the phase change microcapsule is 80-93%.
In the invention, the enthalpy retention rate of the phase-change microcapsule coated by the silicon dioxide is consistent with the coating rate and the core material content, and can be calculated by melting enthalpy or crystallization enthalpy, and the calculation method comprises the following steps:
enthalpy retention rate (coating rate) core material content (delta H)m/ΔHm0×100％；
The content of wall materials is 100 percent to the content of core materials;
wherein, Δ Hm0Is the phase transition point enthalpy, Δ H, of the core material of the phase transition microcapsulemIs the enthalpy value of the phase change point of the phase change microcapsule.
Preferably, the average particle size of the phase-change microcapsule is 1-10 microns.
Still preferably, the average particle size of the phase-change microcapsule is 2-5 microns.
According to the invention, the phase-change material is a solid-liquid phase-change material and can comprise at least one of alcohol compounds, organic acid compounds, ester compounds and alkane compounds.
Preferably, the alcohol compound is at least one selected from the group consisting of glycerol, erythritol, dodecanol, tetradecanol, hexadecanol, and erythritol.
Preferably, the organic acid compound is at least one selected from caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, lauric acid, palmitic acid, and stearic acid.
Preferably, the ester compound is at least one selected from the group consisting of cellulose laurate and cetyl stearate.
Preferably, the alkane compound is at least one selected from paraffin (melting point 14-80 ℃), aromatic hydrocarbon, and aliphatic hydrocarbon (carbon number is 8-100, such as n-octadecane).
According to the invention, the phase change temperature of the phase change microcapsule coated by the silicon dioxide is 14-52 ℃; preferably 20 to 40 ℃.
According to the invention, the latent heat of phase change of the silicon dioxide coated phase change microcapsule is 30J/g to 240J/g, preferably 100J/g to 230J/g, and preferably 110J/g to 220J/g.
The invention also provides a preparation method of the phase-change microcapsule coated by the silicon dioxide, which comprises the following steps:
1) preparing a dispersed phase, namely dissolving a silicon-containing inorganic substance reaction precursor in a molten phase-change material;
2) preparing a continuous phase, including dissolving an emulsifier in a polar solvent;
3) dispersing the dispersed phase prepared in the step 1) in the continuous phase prepared in the step 2), and emulsifying under the action of an emulsifier to form emulsion;
4) carrying out interface reaction on the emulsion prepared in the step 3) at normal temperature or under a heating condition to prepare the phase-change microcapsule coated by the silicon dioxide.
According to the invention, in step 1), said silicon-containing inorganic reactive precursor comprises R1CnH2n-Si or R1CnH2n-Si(R2)m(R3)2-mAt least one of; wherein m and n are integers, n is more than or equal to 0 and less than or equal to 127, and m is more than or equal to 0 and less than or equal to 2; the R is1Selected from H, fatty alkyl, phenyl, vinyl, amino, -CN, -NHCONH2、-Cl、-NH(CH2)2NH22, 3-epoxypropoxy, methacryloxy or mercapto; r2、R3Identical or different, independently of one another, from the group-Cl, -CH3、-OCyH2y+1or-OC2H4OCH3(ii) a said-OCyH2y+1Wherein y is an integer of 1 to 20.
Preferably, the silicon-containing inorganic substance reaction precursor comprises at least one of ethyl orthosilicate, epoxypropyltrimethoxysilane, phenyltriethoxysilane, aminopropyltrimethoxysilane, phenyltrimethoxysilane and n-octyltriethoxysilane.
According to the invention, in the step 1), the mass ratio of the silicon-containing inorganic substance reaction precursor to the phase-change material is 1: 0.1-100; preferably 1:1 to 50.
According to the invention, in the step 2), in order to regulate the hydrolysis-condensation speed of the silicon-containing inorganic substance reaction precursor, the pH value of the continuous phase is regulated by acid or alkali to 1-14, preferably 2-12.
Preferably, the choice of the acid or the base and the concentration thereof are not particularly limited and may be applied to the reaction system of the present invention. Illustratively, the acid is selected from at least one of hydrochloric acid, sulfuric acid and nitric acid, and the base is selected from at least one of sodium hydroxide, potassium hydroxide and ammonia water.
According to the invention, in step 2), the emulsifier comprises sodium salt hydrolysate of ethylene methyl ether-maleic anhydride copolymer, sodium salt hydrolysate of isobutylene-maleic anhydride copolymer, sodium salt hydrolysate of styrene-maleic anhydride copolymer, sodium salt hydrolysate of ethylene-maleic anhydride copolymer, copolymer obtained by copolymerizing acrylic acid or methacrylic acid with styrene, ethylene, vinyl alcohol, vinyl acetate, methacrylamide, isobutylene, acrylate, methacrylate or acrylonitrile, polyvinylbenzenesulfonic acid, sodium polyvinylbenzenesulfonate, emulsifier OP-5, emulsifier OP-10, Tween20 (Tween20), Tween60 (Tween60), Tween80 (Tween80), polyethylene glycol octylphenyl ether X-100(Triton X-100), sodium lauryl sulfate, sodium lauryl sulfonate, sodium lauryl sulfate, at least one of sodium dodecylbenzene sulfonate, hexadecyl trimethyl ammonium bromide and dioctyl sodium sulfosuccinate.
According to the invention, in step 2), the polar solvent comprises at least one of water, methanol, ethylene glycol, propylene glycol, glycerol, tetrahydrofuran, and N, N-dimethylformamide.
According to the invention, in the step 3), the volume ratio of the dispersed phase to the continuous phase is 1: 1-100; preferably 1:1 to 50.
According to the invention, in the step 3), the amount of the emulsifier is 0.5-30% of the mass of the emulsion, and preferably 1-20%.
According to the invention, in step 3), the emulsification can be high-speed shearing emulsification or ultrasonic emulsification; the shearing speed of the high-speed shearing emulsification is within the range of 1000-25000 r/min, and the shearing time is within the range of 0.5-30 min; the ultrasonic frequency during ultrasonic emulsification is within the range of 1000 Hz-40000 Hz, and the ultrasonic emulsification time is within the range of 10 minutes-60 minutes.
According to the invention, in step 4), the reaction temperature of the interfacial reaction is 20-90 ℃ and the reaction time is 0.5-72 hours.
According to the invention, the method further comprises a post-processing step, the post-processing comprising: and (3) carrying out centrifugation or suction filtration on the phase change microcapsule mixed system mixed with the silicon dioxide coating to obtain a solid phase product, washing and drying to obtain the silicon dioxide coated phase change microcapsule.
Preferably, when a centrifugal method is selected to obtain a solid-phase product, the centrifugal speed is 3000-15000 rpm, and the centrifugal time is 2-30 minutes; when a solid-phase product is obtained by selecting a suction filtration method, the aperture of the filter paper for suction filtration is 50-500 mu m.
According to the invention, the method comprises the following steps:
a) dispersing a silicon-containing inorganic substance reaction precursor into a molten solid-liquid phase-change material to obtain a uniform dispersion system, and taking the dispersion system as a dispersion phase;
b) adding an emulsifier into water, dispersing to obtain a uniform dispersion system, taking the dispersion system as a continuous phase, and simultaneously adjusting the pH value of the continuous phase by using acid or alkali;
c) mixing the dispersed phase and the continuous phase, and forming emulsion through emulsification under the action of an emulsifier;
d) carrying out interface reaction at normal temperature or under heating condition to obtain phase change microcapsule coated by silicon dioxide;
e) and separating, washing and drying to obtain the phase change microcapsule dry powder coated by the silicon dioxide.
The invention also provides application of the phase change microcapsule coated by the silicon dioxide, which can be used in the fields of textile, building energy conservation, electronic component heat management, waste heat recovery and the like.
The invention has the beneficial effects that:
the invention provides a phase-change microcapsule coated by silicon dioxide, a preparation method and application thereof, wherein the phase-change microcapsule comprises a core material and a wall material; the core material comprises a phase-change material, and the wall material is silicon dioxide; the enthalpy retention rate of the phase change microcapsule coated by the silicon dioxide is 20-99%; the average particle size of the microcapsules is 0.1-100 microns; in the phase change energy storage microcapsule material taking a phase change material as a core material and silicon dioxide as a wall material and the preparation method thereof in the prior art, the phase change material coated by the silicon dioxide is obtained in one step through sol-gel reaction on an emulsion interface; no toxic substance is generated in the preparation process of the phase change microcapsule coated by the silicon dioxide, and the preparation process is green and environment-friendly; the phase change energy storage microcapsule prepared by the preparation method has high coating rate and low breakage rate, and effectively reduces the supercooling degree of the phase change material, so that the obtained phase change material has no volatile gas, is safe to use, and expands the application range of the phase change material; the preparation method has simple process and low cost, and the used raw materials are cheap and easy to obtain and are easy to realize industrialization; the phase change energy storage microcapsule can be widely applied to the fields of textile, building energy conservation, electronic component heat management, waste heat recovery and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a phase change microcapsule coated with silicon dioxide according to example 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the description of the present invention, and such equivalents also fall within the scope of the invention.
Example 1
6g of ethyl orthosilicate, 0.5g of epoxypropyltrimethoxysilane and 0.5g of phenyltriethoxysilane are added to 30g of octadecane and mixed thoroughly to form an oil phase. 1g of Tween80 was added to 50g of water as an aqueous phase. Adding the water phase into the oil phase, shearing and emulsifying at 10000rpm for 10min by using a high-speed shearing emulsifying machine, transferring the obtained emulsion into a three-mouth bottle, and reacting for 12 hours at 70 ℃ under mechanical stirring. The phase-change microcapsule dry powder is obtained by separation, washing and further drying.
The enthalpy retention rate of the phase-change microcapsule coated with silicon dioxide prepared by the embodiment is 90.5 percent
The scanning electron micrograph of the phase change microcapsule coated with silica prepared in this example is shown in fig. 1. As can be seen from fig. 1, the phase change material coated with silica prepared in this example has uniform particle size and good coating property.
In the phase change material coated with silicon dioxide prepared in this embodiment, the mass percentage of the core material in the phase change microcapsule is 90.5%; the wall material accounts for 9.5 percent of the mass of the phase-change microcapsule; the phase change temperature of the phase change microcapsule coated by the silicon dioxide is 28.2 ℃; the latent heat of phase change of the phase change microcapsule coated by the silicon dioxide is 141.2J/g; the particle size of the phase change microcapsule coated by the silicon dioxide is 2-10 microns; the coating rate of the phase change microcapsule coated by the silicon dioxide is 90.5%.
Example 2
10g of ethyl orthosilicate, 0.5g of aminopropyltrimethoxysilane and 0.5g of n-octyltriethoxysilane were added to 30g of octadecane, and the mixture was thoroughly mixed to obtain an oil phase. 1g of Tween80 was added to 50g of water as an aqueous phase. Adding the water phase into the oil phase, shearing and emulsifying at 10000rpm for 10min by using a high-speed shearing emulsifying machine, transferring the obtained emulsion into a three-mouth bottle, and reacting for 12 hours at 70 ℃ under mechanical stirring. The phase-change microcapsule dry powder is obtained by separation, washing and further drying.
The enthalpy retention rate of the phase change microcapsule coated with silica prepared in the embodiment is 90.7%.
In the phase change material coated with silicon dioxide prepared in this embodiment, the mass percentage of the core material in the phase change microcapsule is 90.7%; the wall material accounts for 9.3 percent of the mass of the phase-change microcapsule; the phase change temperature of the phase change microcapsule coated by the silicon dioxide is 28.0 ℃; the latent heat of phase change of the phase change microcapsule coated by the silicon dioxide is 142.5J/g; the particle size of the phase change microcapsule coated by the silicon dioxide is 2-10 microns; the coating rate of the phase change microcapsule coated by the silicon dioxide is 90.7%.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (15)
1. The preparation method of the phase-change microcapsule coated by the silicon dioxide is characterized in that the phase-change microcapsule coated by the silicon dioxide comprises a core material and a wall material; the core material comprises a phase-change material, and the wall material is silicon dioxide; the coating rate of the phase change microcapsule coated by the silicon dioxide is 90.5-99%; the average particle size of the microcapsules is 2-10 microns; the coating rate is equal to the content of the core material;
the preparation method comprises the following steps:
1) preparing a dispersed phase, namely dissolving a silicon-containing inorganic substance reaction precursor in a molten phase-change material;
2) preparing a continuous phase, including dissolving an emulsifier in a polar solvent;
3) dispersing the dispersed phase prepared in the step 1) in the continuous phase prepared in the step 2), and emulsifying under the action of an emulsifier to form emulsion;
4) carrying out interface reaction on the emulsion prepared in the step 3) at normal temperature or under a heating condition to prepare the phase-change microcapsule coated by the silicon dioxide;
the phase-change material is a solid-liquid phase-change material, the solid-liquid phase-change material comprises at least one of alcohol compounds, organic acid compounds, ester compounds and alkane compounds, and the alcohol compounds are selected from at least one of glycerol, erythritol, dodecanol, tetradecanol, hexadecanol and erythritol;
the organic acid compound is at least one selected from caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, lauric acid, myristic acid, palmitic acid and stearic acid;
the ester compound is selected from at least one of lauric acid cellulose ester and stearic acid hexadecyl ester;
the alkane compound is at least one of paraffin with a melting point of 14-80 ℃, aromatic hydrocarbon and aliphatic hydrocarbon with 8-100 carbon atoms;
in the step 1), the silicon-containing inorganic substance reaction precursor comprises at least one of ethyl orthosilicate, epoxypropyl trimethoxy silane, phenyl triethoxy silane, aminopropyl trimethoxy silane, phenyl trimethoxy silane and n-octyl triethoxy silane;
in the step 2), in order to regulate and control the hydrolysis-condensation speed of the silicon-containing inorganic substance reaction precursor, the pH value of the continuous phase is regulated by acid or alkali to be 1-14;
in the step 3), high-speed shearing emulsification or ultrasonic emulsification is selected for emulsification; the shearing speed of the high-speed shearing emulsification is within the range of 1000-25000 r/min, and the shearing time is within the range of 0.5-30 min; the ultrasonic frequency during ultrasonic emulsification is within the range of 1000 Hz-40000 Hz, and the ultrasonic emulsification time is within the range of 10 minutes-60 minutes;
in the step 4), the reaction temperature of the interfacial reaction is 20-90 ℃, and the reaction time is 0.5-72 hours.
2. The method for preparing the phase-change microcapsule coated with silicon dioxide according to claim 1, wherein the coating rate of the phase-change microcapsule coated with silicon dioxide is 90.5% -93%.
3. The method for preparing the silica-coated phase-change microcapsule according to claim 1, wherein the average particle size of the silica-coated phase-change microcapsule is 2 to 5 μm.
4. The method for preparing the phase-change microcapsule coated with silicon dioxide according to claim 1, wherein the phase-change temperature of the phase-change microcapsule coated with silicon dioxide is 14 to 52 ℃.
5. The method for preparing the silica-coated phase-change microcapsule according to claim 1, wherein the silica-coated phase-change microcapsule has a latent heat of phase change of 30 to 240J/g.
6. The method for preparing the phase-change microcapsule coated with silicon dioxide according to claim 1, wherein in the step 1), the mass ratio of the silicon-containing inorganic substance reaction precursor to the phase-change material is 1: 0.1-100.
7. The method of preparing silica-coated phase-change microcapsules of claim 1, wherein in step 2), the acid is at least one selected from hydrochloric acid, sulfuric acid and nitric acid, and the base is at least one selected from sodium hydroxide, potassium hydroxide and ammonia water.
8. The method of preparing the silica-coated phase-change microcapsule according to claim 1, wherein in step 2), the emulsifier comprises a copolymer obtained by copolymerizing acrylic acid with at least one of: styrene, ethylene, vinyl alcohol, vinyl acetate, methacrylamide, isobutylene, acrylates, methacrylates or acrylonitrile, methacrylic acid copolymerized with at least one of the following: styrene, ethylene, vinyl alcohol, vinyl acetate, methacrylamide, isobutylene, acrylate, methacrylate or acrylonitrile, sodium salt hydrolysate of an ethylene methyl ether-maleic anhydride copolymer, sodium salt hydrolysate of an isobutylene-maleic anhydride copolymer, sodium salt hydrolysate of a styrene-maleic anhydride copolymer, sodium salt hydrolysate of an ethylene-maleic anhydride copolymer, polyvinylbenzenesulfonic acid, sodium polyvinylbenzenesulfonic acid, emulsifier OP-5, emulsifier OP-10, Tween20, Tween60, Tween80, polyethylene glycol octylphenyl ether X-100, sodium lauryl sulfate, sodium lauryl sulfonate, sodium dodecylbenzenesulfonate, hexadecyltrimethylammonium bromide and dioctyl sodium sulfosuccinate.
9. The method for preparing the silica-coated phase-change microcapsule according to claim 1, wherein in the step 2), the polar solvent comprises at least one of water, methanol, ethylene glycol, propylene glycol, glycerol, tetrahydrofuran, and N, N-dimethylformamide.
10. The method for preparing the silica-coated phase-change microcapsule according to claim 1, wherein in the step 3), the volume ratio of the dispersed phase to the continuous phase is 1:1 to 100.
11. The method for preparing the phase-change microcapsule coated with silicon dioxide according to claim 1, wherein in the step 3), the amount of the emulsifier is 0.5-30% of the mass of the emulsion.
12. The method for preparing silica-coated phase-change microcapsules according to claim 1, further comprising a post-treatment step, wherein the post-treatment step comprises: and (3) carrying out centrifugation or suction filtration on the phase change microcapsule mixed system mixed with the silicon dioxide coating to obtain a solid phase product, washing and drying to obtain the silicon dioxide coated phase change microcapsule.
13. The method for preparing the silica-coated phase-change microcapsule according to claim 12, wherein when a centrifugation method is selected to obtain a solid-phase product, the centrifugation speed is 3000 to 15000rpm, and the centrifugation time is 2 to 30 minutes; when a solid-phase product is obtained by selecting a suction filtration method, the aperture of the filter paper for suction filtration is 50-500 mu m.
14. The method for preparing silica-coated phase-change microcapsules according to claim 1, comprising the steps of:
a) dispersing a silicon-containing inorganic substance reaction precursor into a molten solid-liquid phase-change material to obtain a uniform dispersion system, and taking the dispersion system as a dispersion phase;
b) adding an emulsifier into water, dispersing to obtain a uniform dispersion system, taking the dispersion system as a continuous phase, and simultaneously adjusting the pH value of the continuous phase by using acid or alkali;
c) mixing the dispersed phase and the continuous phase, and forming emulsion through emulsification under the action of an emulsifier;
d) carrying out interface reaction at normal temperature or under heating condition to obtain phase change microcapsule coated by silicon dioxide;
e) and separating, washing and drying to obtain the phase change microcapsule dry powder coated by the silicon dioxide.
15. The application of the phase change microcapsule coated with silicon dioxide prepared by the preparation method of the phase change microcapsule coated with silicon dioxide according to claim 1 in the fields of textile, building energy conservation, electronic component heat management and waste heat recovery.
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555401B (en) * | 2008-04-10 | 2011-12-21 | 中国科学院化学研究所 | Microcapsule of organic phase change energy storage material and preparation method thereof |
| US20100143422A1 (en) * | 2008-12-04 | 2010-06-10 | Lewis Michael Popplewell | Microcapsules Containing Active Ingredients |
| CN101503618A (en) * | 2009-03-09 | 2009-08-12 | 中国科学技术大学 | Silicon dioxide gel micro-encapsulated phase change energy storage material and preparation thereof |
| CN101824307B (en) * | 2010-04-30 | 2012-07-25 | 北京化工大学 | Composite phase-change energy storage material for microcapsule and preparation method thereof |
| CN102677471A (en) * | 2012-05-29 | 2012-09-19 | 东华大学 | Method for preparing temperature regulation textile by sol-gel technology |
| CN104152115A (en) * | 2014-07-18 | 2014-11-19 | 东南大学 | Paraffin-SiO2-TiO2 phase change microcapsule and preparation method thereof as well as application of microcapsule in preparing heat-accumulation thermal insulation coating |
| CN104650929A (en) * | 2015-01-27 | 2015-05-27 | 上海应用技术学院 | Halogen-free flame-retardant temperature controlled microcapsules and preparation method thereof |
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