| Vitamin E(VE) has a notable function of oxidation, clearing up free radical, enhancing the immunity of organization and so on.6-hydroxyl of natural VE is very easily oxidized into quinone to cause rapid deactivity. By means of modification, the protective group is connected to the6-hydroxyl of VE in order to enhance its stability, which is beneficial to the development and application of VE products.In this study, carboxymethyl cellulose (CMC) was used as carrier for its safe and reliable characteristics, and then VE was connected to the molecular skeleton of CMC to prepare the antioxidant cellulose derivatives--VE cellulose ester. The synthesis conditions and structural characteristics, stability, oxidation resistance and physicochemical properties of the product were studied.The synthesis reaction of Vitamin E cellulose ester was divided into two steps: preparation of carboxymethyl cellulose acyl chloride and synthesis of VE cellulose ester. The optimized reaction conditions were obtained through the single-factor experiments and response surface methodology.â‘ DMF catalysis-improved method:the acidification of nitric acid concentration was20%,1g CMC, amount of DMF and SOCl2were20mL and3mL respectively, reaction time was2h, reaction temperature was110-120℃, the maximum conversion of chloride could reached60.11%.â‘¡The results showed that the optimal conditions for chemical synthesis of VE cellulose ester were as follow:the reaction temperature was45℃, the ratio of VE and carboxymethyl cellulose acyl chloride was1:2.5, the mass ratio of the catalyst was5%, after reacting for2h the yield of product reached18.03%.The molecular structure, chemical structure and surface morphology of the synthetic products were characterized by IRã€UV and SEM. The infrared spectrum of the polymer found the characteristic bands of C=O at1750.73cm-1~1725.73cm-1, indicating the formation of esters. The UV spectrum showed that the products have the medium intensity of absorption band around240-300nm. It was proved that there exists benzene ring structure. The surface of the material was eroded. The broken-honeycomb-like structure appeared on the surface of product under SEM. There was the fault-block formed in many small caves by scanning electron microscopic studies.The effect of moisture, temperature, ultraviolet radiation, pH value and lipase were studied to investigate the chemical stability of the product. The results of stability experiments showed that the product was stable in the low temperature and neutral solution, while it was unstable in the weak acid and alkaline solution of high-temperature, accompanying with some dissociation. In the system containing lipase, the liberation of the product was almost easy. Ultraviolet radiation had no effect on product.This study laid foundation for further research about antioxidant activity of VE cellulose ester. Under the condition of simulated chemical system, the reducing activity was analyzed. The scavenging activity towards superoxide anion free radical and hydroxyl radical were studied. The results of antioxidant experiments showed that VE cellulose ester has some reducing activity and the capacity of clearing superoxide anion radical and hydroxyl radical. Both had good concentration-effect relationship. It was proved that the product reserved antioxidation group, having oxidation resistance.The physical and chemical safety of synthetic product were detected according to several project of burning crumbs(index was sulfate), acidity, arsenic(index was As) and lead(index was Pb). The results of all the detection indexes met the requirement.In a word, synthetic product not only had antioxidant activity, but had safe, stable and nontoxic ability. It would lay a foundation for preparing new functional polymer which had new activity. |