CN113214795A - Preparation method of ionic liquid phase-change microcapsule - Google Patents
Preparation method of ionic liquid phase-change microcapsule Download PDFInfo
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- CN113214795A CN113214795A CN202110085100.9A CN202110085100A CN113214795A CN 113214795 A CN113214795 A CN 113214795A CN 202110085100 A CN202110085100 A CN 202110085100A CN 113214795 A CN113214795 A CN 113214795A
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Abstract
本发明涉及一种包覆离子液体相变微胶囊的制备方法，属于新型相变功能材料及制备技术领域。离子液体相变微胶囊的壁材是具有优异化学稳定性、导热性、机械性能和高抗温蠕变性的聚合物，芯材是具有相变储热性能、种类多样的离子液体。离子液体具有宽液程、大热容以及优异的热和化学稳定性等优点，是现有相变储热材料的理想介质之一。将相变离子液体封闭在球形胶囊中，可增加传质接触面积，避免离子液体的流失，并实现离子液体相变材料的多次循环利用，拓宽了离子液体在相变储热技术的应用领域。The invention relates to a preparation method of coated ionic liquid phase-change microcapsules, and belongs to the technical field of novel phase-change functional materials and preparation. The wall material of ionic liquid phase change microcapsules is a polymer with excellent chemical stability, thermal conductivity, mechanical properties and high temperature creep resistance, and the core material is a variety of ionic liquids with phase change heat storage properties. Ionic liquids have the advantages of wide liquid path, large heat capacity, and excellent thermal and chemical stability, and are one of the ideal media for existing phase change heat storage materials. Enclosing the phase change ionic liquid in a spherical capsule can increase the mass transfer contact area, avoid the loss of the ionic liquid, and realize the multiple recycling of the ionic liquid phase change material, which broadens the application field of the ionic liquid in the phase change heat storage technology. .
Description
Technical Field
The invention relates to a method for preparing a phase change energy storage material by utilizing a microcapsule technology, in particular to a technology for surface coating of an ionic liquid phase change heat storage material, which can realize the production of phase change materials with different phase change temperatures.
Background
The ionic liquid is a salt which is composed of organic cation and inorganic or organic anion and is liquid at room temperature or near room temperature. Compared with the traditional phase change energy storage material, the ionic liquid as the phase change energy storage material has the following advantages: (1) the melting point of the ionic liquid has strong designability, and corresponding structural adjustment can be made according to the target phase transition temperature; (2) the organic energy storage material has good thermal stability and higher decomposition temperature, is higher than the prior organic energy storage material, can not be decomposed or generate other changes after being subjected to multiple phase change cycles, and is suitable for being used as a heat storage material of a high-grade heat source; (3) the pH is controllable, and the excellent pH adjustability of the ionic liquid is beneficial to forming a multi-component system with other substances with higher requirements on the pH environment; (4) the density of the ionic liquid is stable and easy to adjust, and the density of the ionic liquid is stable in different environments and is not influenced by factors such as temperature, humidity and the like. (5) The hydrophilicity and hydrophobicity are adjustable, and an oil-in-water or water-in-oil system can be formed according to the microcapsule preparation method. Therefore, the wide liquid range, large heat capacity and excellent thermal and chemical stability of the ionic liquid are one of the ideal media of the existing heat storage materials.
Because the phase change process of the ionic liquid is easily influenced by impurities (such as water, absorbed gas and the like), the development of a functional material which not only has the phase change advantage of the ionic liquid but also can improve the phase change stability of the ionic liquid has important significance for the application of the ionic liquid in the aspect of heat storage. The ionic liquid phase-change microcapsule technology is characterized in that the microcapsule technology is applied to the preparation of ionic liquid phase-change materials, phase-change ionic liquid is sealed in spherical capsules, the phase-change advantage of the ionic liquid is kept, the loss of the ionic liquid is prevented, and the problem of phase-change stability of the ionic liquid is solved, so that the application performance of the ionic liquid phase-change materials is improved, and the application field of the phase-change heat storage technology is widened.
Description of the drawings:
FIG. 1 is an electron microscope image of 1-decyl-3-methylimidazolium chloride-polyurethane ionic liquid microcapsule; FIG. 2 is DSC curve diagram of ionic liquid-paraffin composite phase-change microcapsule.
Disclosure of Invention
The invention aims to provide a preparation method of an ionic liquid phase-change heat storage material, which utilizes a microcapsule technology to seal phase-change ionic liquid in a microcapsule so as to ensure that the phase-change material is not leaked and the reversibility of a phase-change process is ensured. The phase-change heat storage material prepared by the method can be processed into an automatic temperature regulating material suitable for the fields of medical sanitation, construction, decoration, military facilities and the like.
The ionic liquid phase-change microcapsule consists of an outer wall material and a phase-change heat storage ionic liquid core material which is coated inside.
The outer wall material of the ionic liquid microcapsule is a polymer with acid and alkali resistance, solvent resistance, stable chemical and mechanical properties and good heat transfer property.
The ionic liquid phase change microcapsule core material has the characteristics of good phase change performance, high heat capacity, high heat energy storage density, high heat stability and the like. The combination of these properties can constitute a large number of ionic liquid core materials of varying properties and uses.
The outer wall material of the ionic liquid phase change microcapsule is one or more of phenolic resin, urea resin, polyacrylate, polyurethane, polylactic acid and the like.
The phase change temperature of the core material of the ionic liquid phase change microcapsule is in the range of 0-100 ℃, and the melting phase change enthalpy is more than 60J/g.
The ionic liquid microcapsule core material comprises but is not limited to 1-decyl-3-methyl imidazole chloride, 1-methyl imidazole trifluoromethanesulfonic acid, 1-ethyl-3-methyl imidazole nitrate, 1-hexyl-2, 3-dimethyl imidazole bromide or 1-octyl-3-methyl imidazole tetrafluoroborate.
The ionic liquid core material can be a compound of one, two or more ionic liquids, and also can be a compound of the ionic liquid and paraffin so as to realize the regulation and control of different phase transition temperatures.
The preparation method of the ionic liquid microcapsule comprises the following steps:
(1) dissolving an ionic liquid core material in an organic solvent, and ultrasonically forming a homogeneous and uniform dispersed phase solution, wherein the mass percentage content of the ionic liquid is 5-10%;
(2) preparing a continuous phase solution, wherein the continuous phase solution is an aqueous solution containing wall materials and a surfactant, and the mass percentage content of the surfactant is 0.1-1%;
(3) microencapsulation: mixing and stirring the dispersed phase and the continuous phase to form an oil-in-water or water-in-oil system, adding a polymerization agent to solidify the polymer film material to form a coating on the ionic liquid;
(4) and (3) washing the obtained novel phase-change ionic liquid microcapsule with water for three times, filtering, and drying in the air for 24 hours to obtain the coated ionic liquid phase-change microcapsule.
The preparation method of the ionic liquid phase change microcapsule comprises the following steps of selecting one or more organic solvents from dichloromethane, trichloromethane, ethyl acetate, petroleum ether, cyclohexane and n-hexane; the surfactant is one or more of polyvinyl alcohol, polyoxyethylene, polythioether and alkyl sodium sulfonate; the polymerization agent is one or more of benzoyl peroxide, lauroyl peroxide and azobisisobutyronitrile.
Detailed description of the preferred embodiments
The invention will now be illustrated by the following examples
Example 11-decyl-3-methylchloroimidazole-polyurethane Ionic liquid phase-Change microcapsules
The composition of the microcapsule is as follows: wall material: a polyurethane; ionic liquid: the preparation method of the 1-decyl-3-methyl imidazole chloride comprises the following steps: the method for preparing the microcapsule phase change material by adopting an interfacial polymerization method comprises the following specific steps: firstly, weighing 2.0g of sodium dodecyl benzene sulfonate powder, pouring into 200mL of deionized water, and uniformly stirring, wherein the prepared system is marked as a system I; then, 25g of 1-decyl-3-methylimidazolium chloride and 75g of 2, 4-tolylene diisocyanate were mixed uniformly, and the oil phase system thus prepared was designated as system II. Putting the system I into a shearing emulsifying machine (the rotating speed is 7000r/min), then pouring the system II into the system I for continuous emulsification for 15min, transferring the obtained suspension into a three-neck flask, adding 10mL of 4.5g triethanolamine solution into the system under the condition of continuous stirring, preserving heat at 40 ℃ for 1h, preserving heat at 60 ℃ for reaction for 2h, and preserving heat at 70 ℃ for reaction for 3 h. And finally, cooling and discharging, washing and filtering the obtained microcapsule product, and drying at 60 ℃ for 12 hours to obtain microcapsule powder. The surface topography is shown in the attached figure 1 of the specification.
Example 21 octyl-3-methylimidazolium tetrafluoroborate Ionic liquid-polylactic acid phase Change microcapsules
The composition of the microcapsule is as follows: wall material: polylactic acid; ionic liquid: 1-octyl-3-methylimidazolium tetrafluoroborate. The preparation method comprises the following steps: the preparation method of the polylactic acid coated 1-octyl-3-methylimidazole tetrafluoroborate ionic liquid phase-change microcapsule comprises the steps of firstly preparing 1-6% by mass of polylactic acid and 1-octyl-3-methylimidazole tetrafluoroborate which are added into dichloromethane to form a uniform solution, wherein the solution is an oil phase. Then 0.5-4% by mass of sodium dodecyl sulfate is added to deionized water, and the solution is water phase. And after the two solutions are completely dissolved, mixing the oil phase and the water phase in a ratio of 1:10, uniformly stirring at room temperature and low speed for emulsification reaction, then raising the temperature to 60 ℃ to volatilize dichloromethane to obtain white emulsion, carrying out centrifugal precipitation on the emulsion, and finally carrying out vacuum drying to obtain the 1-octyl-3-methylimidazole tetrafluoroborate ionic liquid phase-change microcapsule.
Example 31-hexyl-2, 3-dimethylimidazolium bromide Ionic liquid-Paraffin composite phase Change microcapsule
The composition of the microcapsule is as follows: wall material: methyl methacrylate; ionic liquid: 1-hexyl-2, 3-dimethylimidazolium bromide.
The preparation method comprises the following steps: preparation of the aqueous phase: 1.5g of emulsifier polyvinylpyrrolidone and 200mL of deionized water were weighed into a three-necked flask and stirred at a low speed at 60 ℃. Preparation of oil phase: 30g of paraffin, 20g of 1-hexyl-2, 3-dimethylimidazolium bromide, 17.8g of monomeric methyl methacrylate, 2.2g of crosslinking agent pentaerythritol tetraacrylate and 0.5g of initiator azobisisobutyronitrile were weighed. Paraffin is put into a 100mL single-neck flask and heated and melted at 60 ℃, then ionic liquid, monomer and cross-linking agent are sequentially added, and finally initiator powder is added to dissolve the ionic liquid, monomer and cross-linking agent. The oil phase was poured into the aqueous phase and was emulsified by mechanical stirring at 1500rpm for 10 min. The temperature is increased to 80 ℃, and the reaction is carried out for 5 hours under the mechanical stirring of 700rpm, so that the polymerization reaction is carried out. And carrying out suction filtration on the obtained sample while the sample is hot, washing the sample with 70 ℃ water and ethanol for three times respectively, and finally putting the obtained product into a 50 ℃ oven to dry the product to constant weight. The DSC phase transition process of the ionic liquid-paraffin composite phase transition microcapsule is shown in figure 2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113893793A (en) * | 2021-10-25 | 2022-01-07 | 浙江大学 | Size-controllable flexible ionic liquid nano microcapsule and preparation method and application thereof |
| CN115260993A (en) * | 2022-06-29 | 2022-11-01 | 东莞理工学院 | MXene stable ionic liquid based phase change emulsion and preparation method thereof |
| CN116836556A (en) * | 2023-05-10 | 2023-10-03 | 西北工业大学 | A kind of toughened clove oil/ionic liquid material for bay leaves and its preparation and use method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101670256A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of phase change material microcapsule |
| CN107779173A (en) * | 2017-10-12 | 2018-03-09 | 北京宇田相变储能科技有限公司 | A kind of microcapsules for improving thermal storage performance and combinations thereof formed body |
-
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- 2021-01-21 CN CN202110085100.9A patent/CN113214795A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101670256A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of phase change material microcapsule |
| CN107779173A (en) * | 2017-10-12 | 2018-03-09 | 北京宇田相变储能科技有限公司 | A kind of microcapsules for improving thermal storage performance and combinations thereof formed body |
Non-Patent Citations (1)
| Title |
|---|
| 王立久等: "《新型屋面材料》", 31 October 2012, 中国建材工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113893793A (en) * | 2021-10-25 | 2022-01-07 | 浙江大学 | Size-controllable flexible ionic liquid nano microcapsule and preparation method and application thereof |
| CN113893793B (en) * | 2021-10-25 | 2022-12-09 | 浙江大学 | A flexible ionic liquid nanocapsule with controllable size and its preparation method and application |
| CN115260993A (en) * | 2022-06-29 | 2022-11-01 | 东莞理工学院 | MXene stable ionic liquid based phase change emulsion and preparation method thereof |
| CN115260993B (en) * | 2022-06-29 | 2024-06-07 | 东莞理工学院 | A MXene-stabilized ionic liquid-based phase change emulsion and preparation method thereof |
| CN116836556A (en) * | 2023-05-10 | 2023-10-03 | 西北工业大学 | A kind of toughened clove oil/ionic liquid material for bay leaves and its preparation and use method |
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