RESUMEN
Reversible colour change of leuco dye-based composites is in general closely related to their phase change, thus the two phenomena should occur at around the same temperature and should be influenced similarly. However, spatial confinement of the analysed sample affects the change in colour differently compared to its phase transition and the most pronounced effects can be observed during cooling. The bulk composite is coloured while still liquid and the colour hysteresis does not exhibit a loop. In an open-porous medium the colouration coincides well with the crystallization and the colour hysteresis widens to about 4 °C. Microencapsulated composite exhibits two crystallization processes, one of them taking place at the bulk crystallization temperature and the other one at about 20 °C lower. Under such conditions the composite is coloured just before the onset of the second crystallization, i.e. about 15 °C below crystallization in the bulk, and the corresponding colour hysteresis widens to 18 °C. The two crystallization forms are thermally independent and have the same crystalline structure. These effects should be taken into account when designing future applications where the phase-changing materials are implemented.
RESUMEN
Paraffinic phase change materials (PCM) were microencapsulated by in situ polymerization of melamine-formaldehyde prepolymers. Partly methylated trimethylolmelamine was used as an aminoaldehyde prepolymer for the microcapsule wall, a styrene-maleic acid anhydride copolymer as an emulsifier and modifying agent, and ammonia as a scavenger for reducing residual formaldehyde. For the determination of residual formaldehyde in a ppm concentration range, EDANA and malachite green analytical methods were studied, and the EDANA 210.1-99 was applied for the determination of residual formaldehyde in 25 samples of microcapsules, produced in a 200-L reactor. A linear correlation was observed between the added ammonia scavenger concentration and the reduction of residual formaldehyde concentration. Compared with 0.45% (4500 ppm) formaldehyde in a non-treated microcapsule suspension, with ammonia scavenger concentrations 0.80, 0.90 and 1.35%, the concentration of residual formaldehyde dropped to 0.27, 0.20 and 0.09% (i.e. 2700, 2000 and 900 ppm), respectively. Morphological characterisation of microcapsules by SEM and microcapsule wall permeability measurements by gravimetry / mass loss at an elevated temperature (135 °C) suggested that ammonia positively contributed to the wall elasticity / durability, while microcapsules with no ammonia scavenger added tended to have more brittle walls, and were more prone to cracking.