相变温度可调的储能微胶囊的制备及其性能研究
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摘要
相变储能材料是一种非常有应用价值的热能存储材料。相变储能微胶囊的出现，使相变储能材料的应用范围更加广泛。本文运用不同的聚合方法成功制得了一系列以相变蜡/硬脂酸正丁酯二元复合体系为芯材的相变温度可调的储能微胶囊。该微胶囊相变温度的调节可以通过改变其芯材的组成来实现，通过改变相变蜡和硬脂酸正丁酯的相对比例，微胶囊的熔化峰值温度在28~35oC之间可调。
首先，研究了相变蜡/硬脂酸正丁酯组成的二元复合体系的相变储热性能。该二元复合体系在固-液相变过程中都分别只有一个明显的熔化和结晶峰；通过改变相变蜡和硬脂酸正丁酯的相对比例，可以使二元复合体系的相变温度在相变蜡和硬脂酸正丁酯的相变温度之间调节。同时，傅立叶红外光谱结果表明，相变蜡和硬脂酸正丁酯组成的二元复合体系为物理混合物，两组分之间没有发生化学反应。
其次，选用聚氨酯或甲基丙烯酸酯基单体，对二元复合体系进行微胶囊化，制得了一系列相变储热性能很好的微胶囊。一方面，运用界面聚合法制得了聚氨酯/聚脲双层壳包覆复合芯材的相变储能微胶囊。在该体系中，硬脂酸正丁酯本身作为储能材料不仅表现出了很好的相变储热性能，而且它还起助溶的作用，从而省去了丙酮等助溶剂的加入，使制得的微胶囊的包覆率可以进一步提高到60wt%以上。另一方面，为了提高微胶囊的热稳定性及储热可靠性，选取了四种不同种类的丙烯酸酯基交联剂参与形壳反应，对微胶囊的壳材进行优化。其中制得的性能最好微胶囊在经过了500次熔化–结晶的高低温循环热处理后，保持了很好的储热稳定性，经过上述热处理后其包覆率仅下降了约1wt%。
最后，研究了其它不同种类的相变储能材料组成的二元或三元复合体系，及其微胶囊化后得到的相变储能微球的相变储热性能。选用了另外两种酯类的相变储能材料甲基丙烯酸月桂酯和甲基丙烯酸十八酯，分别与相变蜡和硬脂酸正丁酯复合。同时，将该复合体系微胶囊化后，制得了一系列粒径在10~80μm之间，熔化焓值在30~65J/g的相变储能微球。
研究表明，相变蜡/硬脂酸正丁酯二元复合芯材相变储能微胶囊是很好的热能存储材料，具有很好的相变储热性能。制得相变储能微胶囊的相变温度不仅可以通过其复合芯材组成的改变来调节。而且，经过了上百次高低温循环后，大多数相变储能微胶囊依然保持了很好的储热可靠性。
Phase change materials (PCMs) have a good application value as thermalenergy storage materials. Microencapsulated phase change materials(micro-PCMs) make PCMs more widely available. Using differentpolymerization methods, a series of micro-PCMs are prepared which containingparaffin and butyl stearate as their binary cores. The phase change temperatureof these micro-PCMs could be adjusted by regulating the composition of thebinary cores, and the melting peak temperature of the micro-PCMs could beregulated from28oC to35oC.
First, the phase change properties and chemical structures of the binarysystems are studied. The binary systems composed of paraffin and butyl stearatedisplay excellent phase change performances. The binary systems respectivelyshow one melting and freezing peak during solid-liquid phase transition process.Besides, FT-IR results indicat that paraffin and butyl stearate do not react with eachother, and the binary core materials exist as physical mixtures.
Second, the binary cores are microencapsulated using polyurethane oracrylate-based co-polymer shells, the preparation process and phase changeproperties of these micro-PCMs are studied. Using interfacial polymerizationmethods, polyurea/polyurethane double shell micro-PCMs containing paraffinand butyl stearate are synthesized. Using butyl stearate that functionalizes as:co-solvent for improving compatibility of the paraffin and PU shell; componentof binary core for regulating phase change temperature in the range from28to35oC. The microencapsulation ratios of these as-prepared micro-PCMs are morethan60wt%. Moreover, in order to improve the thermal stabilities and thermalreliabilities of these microcapsules, four kinds of acrylate-based cross-linkingagents are respectively introduced into the microencapsulation process. After500times thermal cycling test, these as-prepared micro-PCMs keep goodstabilities that the microencapsulation ratio loss of the best-performedmicrocapsules are only about1wt%.
In addition, octadecyl methacrylate and dodecyl2-methylacrylate are respectively introduced to form binary or ternary systems with paraffin and butyl stearate. Thermalproperties of these mixtures are investigated. Moreover, these binary or ternary systemsare microencapsulated with P(MMA-co-DVB) shells. Since different compositions ofthe core and shell materials, a series of microspheres are synthesized with the diameterranging from10μm to80μm, and the melting enthalpy is in the range of30J/g to65J/g.
All the results reveal that the paraffin/butyl strearate micro-PCMs with different shellmaterials have good application value as thermal energy storage materials. The phasechange temperature of these as-prepared micro-PCMs not only could be adjusted byregulating the composition of their binary core, but the micro-PCMs show good thermalreliability after500times thermal cycling test.
首先，研究了相变蜡/硬脂酸正丁酯组成的二元复合体系的相变储热性能。该二元复合体系在固-液相变过程中都分别只有一个明显的熔化和结晶峰；通过改变相变蜡和硬脂酸正丁酯的相对比例，可以使二元复合体系的相变温度在相变蜡和硬脂酸正丁酯的相变温度之间调节。同时，傅立叶红外光谱结果表明，相变蜡和硬脂酸正丁酯组成的二元复合体系为物理混合物，两组分之间没有发生化学反应。
其次，选用聚氨酯或甲基丙烯酸酯基单体，对二元复合体系进行微胶囊化，制得了一系列相变储热性能很好的微胶囊。一方面，运用界面聚合法制得了聚氨酯/聚脲双层壳包覆复合芯材的相变储能微胶囊。在该体系中，硬脂酸正丁酯本身作为储能材料不仅表现出了很好的相变储热性能，而且它还起助溶的作用，从而省去了丙酮等助溶剂的加入，使制得的微胶囊的包覆率可以进一步提高到60wt%以上。另一方面，为了提高微胶囊的热稳定性及储热可靠性，选取了四种不同种类的丙烯酸酯基交联剂参与形壳反应，对微胶囊的壳材进行优化。其中制得的性能最好微胶囊在经过了500次熔化–结晶的高低温循环热处理后，保持了很好的储热稳定性，经过上述热处理后其包覆率仅下降了约1wt%。
最后，研究了其它不同种类的相变储能材料组成的二元或三元复合体系，及其微胶囊化后得到的相变储能微球的相变储热性能。选用了另外两种酯类的相变储能材料甲基丙烯酸月桂酯和甲基丙烯酸十八酯，分别与相变蜡和硬脂酸正丁酯复合。同时，将该复合体系微胶囊化后，制得了一系列粒径在10~80μm之间，熔化焓值在30~65J/g的相变储能微球。
研究表明，相变蜡/硬脂酸正丁酯二元复合芯材相变储能微胶囊是很好的热能存储材料，具有很好的相变储热性能。制得相变储能微胶囊的相变温度不仅可以通过其复合芯材组成的改变来调节。而且，经过了上百次高低温循环后，大多数相变储能微胶囊依然保持了很好的储热可靠性。
Phase change materials (PCMs) have a good application value as thermalenergy storage materials. Microencapsulated phase change materials(micro-PCMs) make PCMs more widely available. Using differentpolymerization methods, a series of micro-PCMs are prepared which containingparaffin and butyl stearate as their binary cores. The phase change temperatureof these micro-PCMs could be adjusted by regulating the composition of thebinary cores, and the melting peak temperature of the micro-PCMs could beregulated from28oC to35oC.
First, the phase change properties and chemical structures of the binarysystems are studied. The binary systems composed of paraffin and butyl stearatedisplay excellent phase change performances. The binary systems respectivelyshow one melting and freezing peak during solid-liquid phase transition process.Besides, FT-IR results indicat that paraffin and butyl stearate do not react with eachother, and the binary core materials exist as physical mixtures.
Second, the binary cores are microencapsulated using polyurethane oracrylate-based co-polymer shells, the preparation process and phase changeproperties of these micro-PCMs are studied. Using interfacial polymerizationmethods, polyurea/polyurethane double shell micro-PCMs containing paraffinand butyl stearate are synthesized. Using butyl stearate that functionalizes as:co-solvent for improving compatibility of the paraffin and PU shell; componentof binary core for regulating phase change temperature in the range from28to35oC. The microencapsulation ratios of these as-prepared micro-PCMs are morethan60wt%. Moreover, in order to improve the thermal stabilities and thermalreliabilities of these microcapsules, four kinds of acrylate-based cross-linkingagents are respectively introduced into the microencapsulation process. After500times thermal cycling test, these as-prepared micro-PCMs keep goodstabilities that the microencapsulation ratio loss of the best-performedmicrocapsules are only about1wt%.
In addition, octadecyl methacrylate and dodecyl2-methylacrylate are respectively introduced to form binary or ternary systems with paraffin and butyl stearate. Thermalproperties of these mixtures are investigated. Moreover, these binary or ternary systemsare microencapsulated with P(MMA-co-DVB) shells. Since different compositions ofthe core and shell materials, a series of microspheres are synthesized with the diameterranging from10μm to80μm, and the melting enthalpy is in the range of30J/g to65J/g.
All the results reveal that the paraffin/butyl strearate micro-PCMs with different shellmaterials have good application value as thermal energy storage materials. The phasechange temperature of these as-prepared micro-PCMs not only could be adjusted byregulating the composition of their binary core, but the micro-PCMs show good thermalreliability after500times thermal cycling test.
引文
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