Summary: Polyurethane foam nanocomposites were formed via in-situ copolymerisations, in which polyether polyol/water-montmorillonite mixtures were reacted with toluene diisocyanate. The unmodified Na þ -montmorillonite (MMT) was swollen in polyol/water using an ultrasound technique resulting in intercalated layers with increased basal spacings of 2.3 AE 0.1 nm. Measurements of quasi-adiabatic temperature rise showed higher reaction rates as MMT loading increased from 0 to 10 wt.-%. Forced-adiabatic FTIR spectroscopy was used to determine the kinetics of both the copolymerisation and of the microphase separation between poly(ether-urethane) soft segments and polyurea hard segments. The apparent microphase-separation transition time decreased from 70 AE 3 to 42 AE 2 s upon addition of 10 wt.-% MMT, but at reaction times >100 s there was significant retardation of the development of hydrogen bonding in the urea groups of the hard-segment phase.

Interactions between sodium montmorillonite (Na-MMT) and a variety of probes, some of which are intended to model components of a polyurethane system, have been studied. Particular attention was given to the effect of preadsorbed water on the adsorption behavior of the probes. Flow microcalorimetry (FMC), diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS), and wide-angle X-ray scattering (WAXS) were used to monitor the adsorption process. The probe set included alcohols, amines, ethers, poly(propylene glycol) monobutyl ethers (PPG), and 4-ethylphenyl isocyanate (4-EPI). FMC revealed that the preadsorbed water molecules on undried Na-MMT hindered the adsorption of alcohol and ether probes, but had little effect on the adsorption of amines. Drying of Na-MMT to less than 0.3% w/w H2O led to an increase in heat of adsorption and generally greater retention of the probes. PPG showed strong interaction with Na-MMT due to multipoint adsorption. With dried Na-MMT, WAXS revealed that PPG of molecular weight (MW) 1000 was partly intercalated into the gallery while lower molecular weight PPG (MW 340) did not intercalate the Na-MMT. DRIFTS spectra of 4-EPI adsorbed on undried Na-MMT revealed urea linkages, indicating formation of N,N'-bis(4-ethylphenyl) urea. In contrast, with dried Na-MMT the 4-EPI formed a urethane linkage with hydroxyl groups present at the edges of the silicate platelets.

Gedi (Abelmoschus Manihot L.) is a tropical plant in the Malvaceae family, one of the groups of plants in the herbal community. Gedi plants are known to contain flavonoids, hormones, alkaloids, tannins and phenolic compounds. An ultrasonic extraction tool is used in the extraction process of Gedi leaves. The objective of the study is to know the yield and analyze Gedi leaf extract, including proximate analysis and active substance components with LCMS-QTof. The material used is Gedi leaves from Manado. Ultrasonic extraction was carried out with a dry Gedi leaf ratio and Ethanol 1:40 (m/v) with a time of 30 minutes. The concentration of the extract is with a rotary evaporator temperature of 50-60°C. The yield of the extract of Gedi leaf is 9.86 %. Study of the proximity of dried Gedi leaf powder revealed 27.135% protein, 41.675% carbohydrate, 329 kcal energy, 11.235% water and 13.83% ash material. Meanwhile for proximity products, the Gedi leaf extract contains 0.635% protein, 1.27% carbohydrate, 9.26% total energy, 7.1% water, and 0.635% ash. The active compounds in the Gedi extract have been analyzed using LCMS. Trigonelline, Gentiatibetine, Harman, Periplocoside C, and Biotin were detected using the positive-ionization mode, whereas Chloramphenicol was detected with negative-ionization mode.

Unmodified Na-montmorillonite (MMT) was swollen in a polyol/water mixture using an ultrasound technique. Polyurethane (PU) foam nanocomposites were formed via reaction of these polyol/water/Na-MMT mixtures with toluene diisocyanate (TDI). Forced-adiabatic attenuated total reflectance FTIR spectroscopy was used to determine the kinetics of both the PU copolymerisation and of the microphase separation between poly(ether-urethane) soft segments and polyurea hard segments. Consumption of TDI during the initial stages of the copolymerisation was accelerated significantly by the addition of 10 wt% Na-MMT. The initial rate of formation of urea groups also increased significantly upon addition of Na-MMT, but at reaction times >100 s a significant retardation occurred in the development of hydrogen bonding within the urea groups of the hard-segment phase that was recovered only after 1000 s. The reasons for this extensive disruption in structure development were investigated using flow microcalorimetry (FMC), diffuse reflectance Fourier-transform infrared spectroscopy (DRIFTS), and wide angle X-ray scattering (WAXS) to monitor the adsorption process and any chemical reaction between hydrated Na-MMT and a model monoisocyanate; 4-ethylphenyl isocyanate (4-EPI). DRIFTS spectra of 4-EPI adsorbed on Na-MMT revealed urea groups, indicating formation of N,N -bis(4-ethylphenyl) urea. FMC indicated that a significant quantity of this urea formed at the surface and then desorbed. In addition, DRIFTS spectra indicated that the 4-EPI reacted with hydroxyl groups present at the edges of the silicate platelets to form urethane linkages. Thus, in a PU-foam reaction mixture, the water will tend to associate with the Na-MMT, either within the galleries or on the surfaces of silicate lamellae. Upon reaction with isocyanate, the presence of the Na-MMT both promotes the formation of urea and generates urethane linkages between silicate lamellae and the polyurethane.