A series of homogeneous samples with high sugar-surfactant content (sucrose fatty acid ester/water and sucrose fatty acid ester/glycerol/water systems) were prepared with well-controlled processes and investigated by DSC, polarized microscopy, X-ray scattering and rheology. Meanwhile the accuracy of the preparation process is confirmed gas chromatography. The polarized microscopy indicates that the ordering degree of the network structure composed of the liquid crystals may be reduced by the glycerol addition. The results of DSC revealed that 50% glycerol solution could significantly inhibit the crystallization of sucrose fatty acid ester and resulted in a significant widening of the temperature interval for the transformation of the liquid crystal phase into the gel phase. In order to further evaluate the effect of glycerol molecules versus water molecules on the liquid crystal structure of sucrose fatty acid ester, we comparatively analyzed the X-ray scattering data from two perspectives: the mass fraction and molar fraction. It was found that 50% glycerol solution could inhibit the crystallization of sucrose fatty acid ester through changing the water-head group interaction of surfactant, facilitates the integration of sucrose fatty acid ester with different alkyl chain length and may reduce the regularity of liquid crystal, both from the perspective of surfactant mass and molar fraction. Furthermore, the addition of 50% glycerol (w/w) does not significantly impede the liquid crystal formation of sucrose fatty acid ester in aqueous solution. However, from the perspective of surfactant mass fraction, glycerol incorporation could reduce the effective cross-sectional areas of the hydrophilic part of sucrose fatty acid ester in aqueous solution and induce the phase transition of hexagonal liquid crystals to aggregates with less positive curvature, while an opposite tendency could be obtained from the perspective of surfactant molar fraction. The conclusions are also confirmed by subsequent rheological test. Moreover, the results of rheological measurements reveals that the interactions among cylindrical units of the hexagonal liquid crystalline phase become weaker and the surfactant molecules aggregate more loosely in the cylindrical unit with the glycerol incorporation. Moreover, the above-mentioned influence of glycerol on the liquid crystal structure of sucrose fatty acid ester in aqueous solution would be similar but more prominent from the perspective of the molar fraction.
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