The effects that both soap concentration and base oil viscosity exert on the rheology of lubricating greases and its relationship with grease microstructure are discussed in this work. With this aim, different lubricating grease formulations were manufactured by modifying the concentration of lithium 12-hydroxystearate and the viscosity of the base oil, according to an RSM statistical design. These lubricating greases were rheologically characterized through small-amplitude oscillatory shear (SAOS) and viscous flow measurements. In addition to these, scanning electronic microscopy (SEM) observations and mechanical stability tests were also carried out. It has been found that the structural skeleton (size and shape of the disperse phase particles) was highly influenced by the base oil viscosity. In this sense, the values of the viscoelastic functions in the linear viscoelastic region and the mechanical stability of the lubricating greases increase as the viscosity of the base oil decreases. An opposite tendency was observed during viscous flow tests at high shear rates, when the grease microstructure was mostly destroyed. On the other hand, the microstructural network of these greases becomes stronger as soap concentration increases. These results have been explained taking into account the balance between the solvency of the thickener in the base oil and the level of entanglements formed by soap fibers, which influence the lubricating grease network.
Thermal-induced changes in the viscous and viscoelastic responses of lubricating greases have been investigated through different rheological techniques in a temperature range of 0-175°C. Small-amplitude oscillatory shear and viscous flow measurements were carried out on a model conventional lithium lubricating grease prepared by inducing the in situ saponification reaction between 12-hydroxystearic acid and hydrated lithium hydroxide. The linear viscoelasticity functions dramatically decrease above 110°C, but not below this critical temperature, which determines the maximum recommended operating temperature in relation to its durability and resistance under working conditions. Two different regions, below and above this critical temperature, in the plateau modulus versus temperature plot have been detected. From this thermal dependence, a much larger thermal susceptibility of the lubricating grease at temperatures above 110°C is apparent. The thermo-mechanical reversibility of this material has been studied by applying different combined stress-temperature protocols. Regarding the viscous flow, a minimum in the shear stress versus shear rate plots appeared at temperatures above 60°C, more pronounced as temperature increases, resulting from material instabilities. The experimental results obtained have been explained on the basis of the thermo-mechanical degradation of the lubricating grease microstructure.
Nowadays, different types of natural carbohydrates such as sugars, starch, cellulose and their derivatives are widely used as renewable raw materials. Vegetable oils are also considered as promising raw materials to be used in the synthesis of high quality products in different applications, including in the adhesive field. According to this, several bio-based formulations with adhesion properties were synthesized first by inducing the functionalization of cellulose acetate with 1,6-hexamethylene diisocyanate and then mixing the resulting biopolymer with a variable amount of castor oil, from 20% to 70% (wt). These bio-based adhesives were mechanically characterized by means of small-amplitude oscillatory torsion measurements, at different temperatures, and standardized tests to evaluate tension loading (ASTM-D906) and peel strength (ASTM-D903). In addition, thermal properties and stability of the synthesized bio-polyurethane formulations were also analyzed through differential scanning calorimetry and thermal gravimetric analysis. As a result, the performance of these bio-polyurethane products as wood adhesives were compared and analyzed. Bio-polyurethane formulations exhibited a simple thermo-rheological behavior below a critical temperature of around 80-100 • C depending on the castor oil/cellulose acetate weight ratio. Formulation with medium castor oil/biopolymer weight ratio (50:50 % wt) showed the most suitable mechanical properties and adhesion performance for bonding wood.
There is a growing interest on the development of new materials based on recycled polymers from plastics waste, since the use of such plastics represents a low-cost source of raw material. The purpose of the present work is to evaluate, from a comparative point of view, the effect that different waste and virgin polymers, used as viscosity modifier additives, exert on the rheological properties of standard lithium lubricating greases. Grease formulations containing diverse polymers, differing in nature and/or origin, were manufactured and rheologically characterized. Particularly, the influences of the type of polymer, the molecular weight and the presence of carbon black, used as filler in recycled polymers, have been evaluated. Small-amplitude oscillatory shear (SAOS) and viscous flow measurements were carried out, as well as calorimetric and thermogravimetric analysis. In general, recycled polymers induce a more important rheological modification than virgin polymers of the same nature. Thus, the addition of some recycled polymers such as HDPE, LDPE, PP, and EVA copolymer to lithium lubricating grease significantly increases the values of the rheological parameters analyzed. The crystallinity degree, mainly dependent on the nature of the polymer, and the carbon black content of recycled polymers have been pointed out as the most highly influencing parameters on the rheology of the lubricating greases studied. However, an apparent loss in mechanical stability for lubricating greases containing recycled polymers has been found when they were submitted to a severe mechanical treatment.
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