CN113355055A - Microcapsule with high phase change enthalpy and preparation method thereof - Google Patents
Microcapsule with high phase change enthalpy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a microcapsule with high phase change enthalpy and a preparation method thereof, wherein the phase change energy storage microcapsule takes straight-chain alkane phase change material as an inner core and takes polyurea with stable chemical property formed by polymerization of diisocyanate and polyamine at an interface as a shell layer; the stable high phase change enthalpy microcapsule with the phase change temperature of-10-60 ℃, the average size of 5-100 microns and the phase change enthalpy of 200J/g is formed. The preparation method comprises the following steps: firstly, directly mixing a certain amount of alkane core materials and diisocyanate which is one of wall material reaction monomers, then adding the mixture into water solution containing an emulsifier for high-speed shearing emulsification, slowly heating, simultaneously adding a certain amount of amine reaction monomers, and after the reaction is finished, cleaning, filtering, drying and the like are carried out on the product to obtain the polyurea phase change energy storage microcapsule. The energy storage microcapsule prepared by the method has the advantages of adjustable phase change temperature, controllable particle size, high coating efficiency and phase change enthalpy up to 200J/g. Has better application prospect in the aspects of temperature regulation, energy storage, heat preservation and the like.
Description
Technical Field
The invention belongs to the field of phase change microcapsules, and particularly relates to a microcapsule with high phase change enthalpy and a preparation method thereof.
Background
The phase change process of the phase change energy storage material is utilized to realize the absorption or release of heat energy from the external environment, and the storage and the release of the heat energy can be effectively carried out, so that the difference between the energy supply and the energy use is made up, the energy utilization efficiency is effectively improved, and the energy waste is reduced. Not only meets the technical and economic requirements of people in engineering and products, but also improves the utilization rate of energy. Nowadays, PCM is not only applied to the effective utilization of renewable energy, but also widely used in energy-saving and thermal regulation systems, such as building energy conservation, refrigeration of pharmaceutical or biological products, temperature control of electronic parts or equipment, textiles with temperature regulation function, thermal buffering of lithium ion batteries, thermal comfort of vehicles, and the like.
The phase change energy storage microcapsule is formed by coating a phase change energy storage material by using a microcapsule technology and adopting a material with stable chemical properties as a shell material, so that the microsphere with a core-shell structure is formed, various problems of the phase change energy storage material in practical application, such as leakage, difficult processability, corrosivity, instability and the like, are effectively solved, and the application field of the phase change energy storage material is expanded. In recent years, the application of phase change energy storage materials in building materials has become a hot spot of research and attention. The energy storage phase change material is combined with reasonable utilization of solar energy, so that the comfort level of a building is improved, the energy consumption is reduced, and the influence caused by negative environment can be reduced.
At present, the main methods for preparing phase change microcapsules include interfacial polymerization, in-situ polymerization, spray drying, etc., and the in-situ polymerization is most commonly used. Such as melamine-formaldehyde resins, PMMA, etc., but are environmentally and health hazards due to the presence of unreacted monomers, such as formaldehyde, in both resins. The microcapsule taking polyurea resin as a shell material does not contain free formaldehyde, has little harm to the environment and health and good environmental protection, so the polyurea resin microcapsule receives more and more attention. Chinese patent application CN107903877A discloses a preparation method of polyurea resin phase change microcapsules, wherein an interfacial polymerization method is adopted to prepare the polyurea phase change microcapsules, the prepared microcapsules have good thermal stability, but the phase change enthalpy is only 95.81J/g. Therefore, how to prepare the phase-change microcapsule with good thermal stability, excellent use effect and low cost becomes a technical problem which needs to be solved urgently.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide the microcapsule with high phase-change enthalpy and the preparation method thereof, so that the microcapsule with high phase-change enthalpy has good thermal stability, excellent use effect and low cost, and the energy-storage microcapsule prepared by the method has adjustable phase-change temperature, controllable particle size and high coating efficiency, and the phase-change enthalpy can reach 200J/g. Has better application prospect in the aspects of temperature regulation, energy storage, heat preservation and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a microcapsule with high phase change enthalpy is characterized in that a straight-chain alkane phase change material is used as an inner core, polyurea is formed by interfacial polymerization of diisocyanate and polyamine and is used as a shell layer, and the phase change energy storage microcapsule with a core-shell structure is formed, wherein the phase change temperature of the microcapsule is-30-60 ℃, the average size of the microcapsule with high phase change enthalpy is 5-100 micrometers, and the phase change enthalpy of the microcapsule is at least 200J/g. The present invention forms a dimensionally stable microcapsule structure.
Preferably, the phase-change core material adopted by the inner core is C14～C25At least one of the straight-chain alkanes with the phase transition temperature of-10 ℃ to 60 ℃.
Preferably, the mass fraction of the phase-change core material in the total mass of the phase-change microcapsule is 50-90%.
The invention relates to a preparation method of a microcapsule with high phase change enthalpy, which comprises the following steps:
(1) directly mixing an alkane core material and a diisocyanate monomer into an oil phase;
(2) preparing an amine monomer into an aqueous solution to obtain an amine monomer aqueous solution;
(3) dissolving an emulsifier in deionized water to prepare an emulsifier aqueous solution;
(4) dripping the oil phase prepared in the step (1) into the emulsifier aqueous solution obtained in the step (3), shearing and stirring for 1-30 min, controlling the stirring speed to be 600-20000 rpm, and obtaining a stable emulsion after stirring;
(5) slowly heating the emulsion obtained in the step (4) to 30-90 ℃, simultaneously dripping the amine monomer aqueous solution obtained in the step (2) to obtain a reactant mixed solution, and carrying out heat preservation reaction for 1-12 h to obtain a product solution;
(6) and (3) washing, filtering and drying the product solution obtained in the step (5) to obtain the alkane-coated polyurea phase-change microcapsule.
Preferably, in the step (1), the mass ratio of the usage amount of the diisocyanate monomer to the usage amount of the alkane core material is 10-50%; preferably, the material of the diisocyanate monomer is at least one of MDI, IPDI and NDI.
Preferably, in the step (2), the mass fraction of the amine monomer in the amine monomer aqueous solution is 5-60%; preferably, the amine monomer material is polyamine with 2-8 carbon atoms. Further preferably, in the step (2), the amine monomer material is at least one of ethylenediamine, diethylenetriamine, triethylenetetramine and melamine.
Preferably, in the step (3), the mass fraction of the emulsifier in the emulsifier aqueous solution is 1-20%; preferably, the emulsifier is at least one of SDBS, SDS, SMA, GA, Tween80, Span 20.
Preferably, in the step (4), the mass ratio of the usage amount of the diisocyanate monomer to the usage amount of the emulsifier is 6-400%; preferably, the stirring is carried out at a rotation speed of 600 to 10000 rpm.
Preferably, in the step (5), the amount of the amine monomer is 50-300% of that of the diisocyanate monomer by mass percentage; preferably, the reaction is carried out for 2-8 h at the temperature of 45-70 ℃ to obtain a product solution.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the polyurea phase-change microcapsule has good compactness and thermal stability of shell materials;
2. the phase change enthalpy of the polyurea phase change microcapsule is high and can reach 200J/g, and a better using effect can be brought;
3. the polyurea phase change microcapsule prepared by the invention does not contain free formaldehyde and has no harm to the environment and health; the polyurea phase-change microcapsule prepared by the invention adopts an interfacial polymerization method, has the advantages of no violent reaction, simple process, good control of product quality and easy realization of industrial production and application.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in the embodiment, the microcapsule with high phase change enthalpy takes a straight-chain alkane phase change material as an inner core, polyurea is formed by polymerization of diisocyanate and polyamine at an interface as a shell layer, and the phase change energy storage microcapsule with a core-shell structure is formed, wherein the phase change temperature is-30-60 ℃, the average size of the microcapsule with high phase change enthalpy is 5-100 microns, and the phase change enthalpy is not lower than 200J/g.
In this embodiment, a method for preparing a microcapsule with high phase change enthalpy includes the following steps:
(1) directly mixing 8g of tetradecane and 4g of MDI to form an oil phase;
(2) preparing 5g of diethylenetriamine monomer into an aqueous solution with the mass fraction of 5% to obtain an amine monomer aqueous solution;
(3) dissolving 1g of SMA emulsifier in 100g of deionized water to prepare an emulsifier aqueous solution;
(4) dripping the oil phase prepared in the step (1) into the emulsifier aqueous solution obtained in the step (3), shearing and stirring for 30min, controlling the stirring speed to be 600rpm, and obtaining stable emulsion after stirring;
(5) slowly heating the emulsion obtained in the step (4) to 45 ℃, simultaneously dripping the amine monomer aqueous solution obtained in the step (2) to obtain a reactant mixed solution, and carrying out heat preservation reaction for 2 hours to obtain a product solution;
(6) and (3) washing, filtering and drying the product solution obtained in the step (5) to obtain the alkane-coated polyurea phase-change microcapsule.
The phase change energy storage microcapsule prepared by the embodiment takes alkane phase change materials as a core, and polyurea with stable chemical properties formed by interfacial polymerization as a shell layer; forming a dimensionally stable microcapsule structure. The polyurea phase-change microcapsule has high phase-change enthalpy, the phase-change enthalpy is not lower than 200J/g, and the polyurea phase-change microcapsule has good application potential in the aspects of temperature regulation, energy storage, heat preservation and the like.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in the embodiment, the microcapsule with high phase change enthalpy takes a straight-chain alkane phase change material as an inner core, polyurea is formed by polymerization of diisocyanate and polyamine at an interface as a shell layer, and the phase change energy storage microcapsule with a core-shell structure is formed, wherein the phase change temperature is-30-60 ℃, the average size of the microcapsule with high phase change enthalpy is 5-100 microns, and the phase change enthalpy is not lower than 200J/g.
In this embodiment, a method for preparing a microcapsule with high phase change enthalpy includes the following steps:
(1) mixing 10g octadecane with 2g NDI directly into an oil phase;
(2) preparing 2g of ethylene diamine monomer into an aqueous solution with the mass fraction of 20% to obtain an amine monomer aqueous solution;
(3) dissolving 10g of SDBS emulsifier in 90g of deionized water to prepare an emulsifier aqueous solution;
(4) dripping the oil phase prepared in the step (1) into the emulsifier aqueous solution obtained in the step (3), shearing and stirring for 30min, controlling the stirring speed to be 6000rpm, and obtaining stable emulsion after stirring;
(5) slowly heating the emulsion obtained in the step (4) to 65 ℃, simultaneously dripping the amine monomer aqueous solution obtained in the step (2) to obtain a reactant mixed solution, and carrying out heat preservation reaction for 4 hours to obtain a product solution;
(6) and (3) washing, filtering and drying the product solution obtained in the step (5) to obtain the alkane-coated polyurea phase-change microcapsule.
The phase change energy storage microcapsule prepared by the embodiment takes alkane phase change materials as a core, and polyurea with stable chemical properties formed by interfacial polymerization as a shell layer; forming a dimensionally stable microcapsule structure. The polyurea phase-change microcapsule has high phase-change enthalpy, the phase-change enthalpy is not lower than 200J/g, and the polyurea phase-change microcapsule has good application potential in the aspects of temperature regulation, energy storage, heat preservation and the like.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in the embodiment, the microcapsule with high phase change enthalpy takes a straight-chain alkane phase change material as an inner core, polyurea is formed by polymerization of diisocyanate and polyamine at an interface as a shell layer, and the phase change energy storage microcapsule with a core-shell structure is formed, wherein the phase change temperature is-30-60 ℃, the average size of the microcapsule with high phase change enthalpy is 5-100 microns, and the phase change enthalpy is not lower than 200J/g.
In this embodiment, a method for preparing a microcapsule with high phase change enthalpy includes the following steps:
(1) mixing 6g hexadecane with 6g eicosane, 0.6g MDI, 0.6g IPDI directly to form an oil phase;
(2) preparing 1.2g of diethylenetriamine monomer into an aqueous solution with the mass fraction of 60% to obtain an amine monomer aqueous solution;
(3) dissolving 20g of Tween80 emulsifier in 80g of deionized water to prepare an emulsifier aqueous solution;
(4) dripping the oil phase prepared in the step (1) into the emulsifier aqueous solution obtained in the step (3), shearing and stirring for 30min, controlling the stirring rotation speed to be 10000rpm, and obtaining stable emulsion after stirring;
(5) slowly heating the emulsion obtained in the step (4) to 70 ℃, simultaneously dripping the amine monomer aqueous solution obtained in the step (2) to obtain a reactant mixed solution, and carrying out heat preservation reaction for 8 hours to obtain a product solution;
(6) and (3) washing, filtering and drying the product solution obtained in the step (5) to obtain the alkane-coated polyurea phase-change microcapsule.
The phase change energy storage microcapsule prepared by the embodiment takes alkane phase change materials as a core, and polyurea with stable chemical properties formed by interfacial polymerization as a shell layer; forming a dimensionally stable microcapsule structure. The polyurea phase-change microcapsule has high phase-change enthalpy, the phase-change enthalpy is not lower than 200J/g, and the polyurea phase-change microcapsule has good application potential in the aspects of temperature regulation, energy storage, heat preservation and the like.
In summary, the microcapsules with high phase change enthalpy in the above embodiments use linear alkane phase change materials as the inner core, and polyurea with stable chemical properties formed by polymerization of diisocyanate and polyamine at the interface as the shell layer; the phase transition temperature is-10-60 ℃, the average particle size is 5-100 microns, and the phase transition enthalpy can reach 200J/g. According to the preparation method of the embodiment, firstly, a certain amount of diisocyanate which is one of the wall material reaction monomers is directly mixed with the alkane core material, then the mixture is added into water solution containing an emulsifier for high-speed shearing emulsification, the temperature is slowly increased, meanwhile, a certain amount of amine reaction monomers are added, and after the reaction is finished, the product is cleaned, filtered, dried and the like, so that the polyurea phase change energy storage microcapsule is obtained. The energy storage microcapsule prepared by the method of the embodiment has the advantages of adjustable phase change temperature, controllable particle size, high coating efficiency, high phase change enthalpy, low cost and easy realization. Has better application prospect in the aspects of temperature regulation, energy storage, heat preservation and the like.
While the embodiments of the present invention have been described, the present invention is not limited to the above embodiments, and various changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the present invention may be made in the form of equivalent substitutions without departing from the technical principle and inventive concept of the present invention.
Claims (10)
1. A microcapsule with high phase change enthalpy is characterized in that: taking a straight-chain alkane phase change material as an inner core, forming polyurea as a shell layer through the interfacial polymerization of diisocyanate and polyamine, and forming the phase change energy storage microcapsule with a core-shell structure, wherein the phase change temperature is-30-60 ℃; the average size of the microcapsules with high phase change enthalpy is 5-100 microns, and the phase change enthalpy of the microcapsules is at least 200J/g.
2. A microcapsule with high enthalpy of phase change according to claim 1, characterized in that: the phase change core material adopted by the inner core is C14～C25At least one of the straight-chain alkanes with the phase transition temperature of-10 ℃ to 60 ℃.
3. The microcapsule with high phase change enthalpy according to claim 1, wherein the mass fraction of the phase change core material in the total mass of the phase change microcapsule is 50-90%.
4. A process for the preparation of microcapsules of high enthalpy of phase change according to claim 1, comprising the following steps:
(1) directly mixing an alkane core material and a diisocyanate monomer into an oil phase;
(2) preparing an amine monomer into an aqueous solution to obtain an amine monomer aqueous solution;
(3) dissolving an emulsifier in deionized water to prepare an emulsifier aqueous solution;
(4) dripping the oil phase prepared in the step (1) into the emulsifier aqueous solution obtained in the step (3), shearing and stirring for 1-30 min, controlling the stirring speed to be 600-20000 rpm, and obtaining a stable emulsion after stirring;
(5) slowly heating the emulsion obtained in the step (4) to 30-90 ℃, simultaneously dripping the amine monomer aqueous solution obtained in the step (2) to obtain a reactant mixed solution, and carrying out heat preservation reaction for 1-12 h to obtain a product solution;
(6) and (3) washing, filtering and drying the product solution obtained in the step (5) to obtain the alkane-coated polyurea phase-change microcapsule.
5. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 4, characterized in that: in the step (1), the mass ratio of the diisocyanate monomer to the alkane core material is 10-50%;
or the material of the diisocyanate monomer is at least one of MDI, IPDI and NDI.
6. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 4, characterized in that: in the step (2), the mass fraction of the amine monomer in the amine monomer aqueous solution is 5-60%;
or the amine monomer material is polyamine with 2-8 carbon atoms.
7. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 6, characterized in that: in the step (2), the amine monomer material is at least one of ethylenediamine, diethylenetriamine, triethylenetetramine and melamine.
8. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 4, characterized in that: in the step (3), the mass fraction of the emulsifier in the emulsifier aqueous solution is 1-20%;
or the emulsifier is at least one of SDBS, SDS, SMA, GA, Tween80 and Span 20.
9. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 4, characterized in that: in the step (4), the mass ratio of the usage amount of the diisocyanate monomer to the usage amount of the emulsifier is 6-400%;
or when stirring, controlling the stirring speed to be 600-10000 rpm.
10. The process for the preparation of microcapsules of high enthalpy of phase change according to claim 4, characterized in that: in the step (5), the amount of the amine monomer is 50-300% of the diisocyanate monomer by mass percent.
Or, carrying out heat preservation reaction for 2-8 h at the temperature of 45-70 ℃ to obtain a product solution.
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