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Study On The Synthesis Process Of Vitamin E Unsaturated Fatty Acid-Ester Of Camellia Oil

Posted on:2009-08-17Degree:MasterType:Thesis
Country:ChinaCandidate:M X JingFull Text:PDF
GTID:2121360245967770Subject:Chemical processes
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Vitamin E has many functions such as notable oxidation resisting, clearing up free radical, stimulating the circulation of blood, preventing cancer, enhancing the immunity of organization, and so on. However, Vitamin E is easily oxidized in the course of process and storage, especially under the condition of oxygen, metal ion or ultraviolet light. In order to reduce Vitamin E'deficiency or improve it's properties, the properties of Vitamin E could be improved By linking the protective group to the 6-hydroxy of Vitamin E. The way of chemical modification can not only enhance the chemical stability of Vitamin E, but also provide Vitamin E with new functions.This thesis was divided into four parts, and the main work and its results are showed as followed:1. Techniques of alcoholysis of vitamin E acetate were studied: Some key technique parameters such as methanol-vitamin E acetate weight ratio, reaction temperature, reaction time, dosage of catalyst, et al. were discussed and analyzed theoretically. The optimum parameters for the alcoholysis were determined by orthogonal method, showed as followed: at 65℃alcohol-ester weight ratio = 2:1, in the presence of 1.1% NaOH which was the weight of vitamin E acetate as catalyst, the alcoholysis of vitamin E acetate exceeded 99.7% after 2 hours of reaction. The purity of Vitamin E was 97.0% with a yield of 80.2%.2. Enrichment of unsaturated fatty acid in camellia oil with urea adduct method was studied: Factors affecting the reaction such the ratio fatty acid and urea, the ratio fatty acid and ETOH, adduction temperature, adduction time, refluxing time were investigated by the single-variable experiment. By orthogonal design method, the optimal reaction conditions have been determined as follows: the ratio urea and fatty acid was 2.5: 1, the ratio ETOH and fatty acid was20:l, adduction temperature was 5℃, and adduction time was 4h. Under these optimum conditions, the iodine value was increased from 85.4 to 111.5, the yield is 39%.3. Synthesis of Vitamin E unsaturated fatty acid-ester of camellia oil was studied: Factors affecting the reaction such as the material ratio, the amounts of catalyst (triethylamine), reaction temperature, reaction time were investigated by the single-variable experiment. By orthogonal design method, the optimal reaction conditions have been determined as follows: materials ration of oleic chloride to vitamin E was 4.5:1, the amount of catalyst was 0.2mL (0.002mol V_E), reaction temperature was 45℃, and reaction time was 4h.4. A HPLC method for the determination of Vitamin E linolenate, Vitamin E Linoleate was established, meanwhile the HPLC method for the determination of Vitamin E oleate was improved. The condition of HPLC method was as following: the mobile phase was methonal: tetrahydrofuran=65:35(V/V), UV wave length was 285nm, flow speed was 1mL/min, temperature was 30℃, loading sample was 15μL. The retention times of Vitamin E Oleate, Vitamin E Linoleate and Vitamin E linolenate were 9.672min, 8.612min, 7.817min.
Keywords/Search Tags:Vitamin E, Vitamin E unsaturated fatty acid-ester of camellia oil, synthesis, urea adduct method, HPLC
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