No abstract

With cassava starch as a raw material and octenyl succinic anhydride as an esterifying agent, octenyl succinic anhydride modified starch (OSA–starch) was prepared in an aqueous medium and treated by water‐bath heating and microwave radiation at a certain temperature, respectively. The reaction kinetics of esterification were studied. The structural analysis and synthesis mechanism of OSA–starch were investigated by means of scanning electron microscopy and Fourier transform infrared spectroscopy. The differences in the esterification reaction kinetics between starches treated with water‐bath heating and microwave radiation were observed. Under the condition of water‐bath heating, the apparent activation energy of the esterification reaction was 52.22 ± 1.21 kJ/mol, and the pre‐exponential factor was 9018.20/min−1. Under the condition of microwave radiation, the apparent activation energy of the esterification reaction was 50.13 ± 1.16 kJ/mol, and the pre‐exponential factor was 4510.21/min−1. We found that microwave radiation could reduce both the activation energy of the reaction and the pre‐exponential factor. The lowering effect of the apparent activation energy was greater than that of the pre‐exponential factor under the condition of microwave radiation, and this resulted in increased reaction rates. The change in the esterification reaction kinetics was a nonthermal effect of microwave radiation on the esterification of cassava starch. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43909.

To discover new synthesis technology and increase the degree of substitution (DS) of carboxymethyl starch (CMS), ultrasound‐modified CMS (U‐CMS) was successfully prepared under ultrasonic irradiation in the alkali condition with corn starch (CS) as the raw material, ethyl alcohol as the solvent, and monochloroacetic acid as the carboxymethylated reagent. The effects of ultrasound conditions (ultrasonic action sequence, ultrasonic radiation time, and ultrasonic power) and etherification time after ultrasonic irradiation on DS of U‐CMS were studied separately through single‐factor experiments. Meanwhile, the granule morphology, crystal type, and molecular structure of U‐CMS were studied by scanning electron microscopy (SEM), X‐ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT‐IR). The results showed that DS of U‐CMS prepared under certain conditions (ultrasonic radiation time before alkalization, 40 min; ultrasonic radiation temperature, 35°C; ultrasonic power, 170 W; and etherification time, 180 min) improved 38.7% compared with that without ultrasonic radiation. The SEM, XRD, and FT‐IR results illustrated that crystal‐type change of the starch granule after ultrasonic irradiation was not obvious. However, the number of sunken points and holes on the granule surface increased, so that the specific surface expanded, which improved the carboxymethylation.

Using native cassava starch as raw materials, carboxymethyl starch (CMS) was prepared by ethanol solvent method under the ultrasound‐microwave synergistic interaction. And the structure of CMS was characterized employing Fourier transform infrared (FTIR) spectrometer, scanning electron microscopy (SEM), X‐ray diffraction (XRD) and thermogravimetric analyzer. Typically, the optimal synthesis conditions for the preparation process confirmed by orthogonal experiment L18 (61 × 36) were shown as follows: the ultrasonic treatment temperature was fixed to 35°C and two steps alkalization was employed; the ultrasonic time was 40 min before alkalizing and the ultrasonic power was 220 W; the amount of sodium hydroxide was 8.8 g, the microwave alkalization time was 2 min; the amount of monochloroacetic acid was 11.34 g; the amount of 95% (v/v) ethanol was 70 mL; the microwave etherification time was 3 min. The degree of substitution of prepared CMS was 1.089 ± 0.041, which was increased 30.4% compared with the prepared sample without ultrasound‐microwave synergistic treatment. FTIR results showed that the strong COO characteristic absorption peaks of the stretching vibration were observed at 1613 and 1421 cm−1, which proved that the carboxymethylation of cassava starch was occurred. SEM results suggested that there were many cracks and dents on CMS granules; and, XRD results indicated that the carboxymethylation of starch occurred both in amorphous region and crystalline region, the noticeable damage of crystalline region by carboxymethylation was observed. Thermogravimetric analysis (TG) and derivative TG showed that thermal stability of CMS changed better compared with native starch. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40906.