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高酸值花椒籽油酯化脱酸的工艺研究
Study on Reduce High Acidity of Prickly Ash Seed Oil with Esterification
【作者】 詹玉新;
【导师】 齐玉堂;
【作者基本信息】 武汉工业学院 , 食品科学与工程, 2010, 硕士
【摘要】 本研究以花椒籽油为基本原料,花椒籽油一般颜色较深、酸价较高,本文有针对性的先对花椒籽油进行脱色,再以酯化脱酸的方法对花椒籽油进行精炼,最后对酯化油进行必要的后处理,精炼效果较好。在脱色工艺的研究中,以活性炭结合活性白土作为混合脱色剂,重点研究活性炭占混合脱色剂比例、混合脱色剂用量、脱色时间、脱色温度四个脱色影响因素,结合单因素试验和响应面优化试验,最终得出最佳的脱色条件为∶活性炭占混合脱色剂比例∶15.5%;混合脱色剂用量∶2%;脱色时间∶22min;脱色温度∶93℃,在此条件下脱色率为79.71%。在酯化脱酸工艺研究中,对五种传统的酯化催化剂进行比较筛选,结果表明ZnO催化效果最好。选定ZnO作为酯化反应的催化剂,对酯化反应时间、酯化反应温度、ZnO添加量、单甘酯/甘油(1∶1,w/w)添加量进行单因素试验考察,并进行正交试验分析。通过正交试验分析并结合单因素试验情况,综合考虑酯化温度对酯化油色泽的影响和经济适用性,最终确定最佳的酯化条件为∶酯化时间6h、酯化温度200℃、ZnO添加量为0.2%、单甘酯/甘油(1∶1,w/w)添加量为理论添加量的150%,在此条件下得到的酯化油的酸价为3.57mgKOH/g,酯化油中单甘酯、甘二酯的含量分别为3.25%、13.64%。酯化油的后处理主要是对甘油三酯进行纯化,纯化采用溶剂萃取法,萃取条件为∶萃取剂采用乙醇,浓度为85%;乙醇溶液/混合油(w/w)比例为0.8∶1;萃取温度为40℃,最终得到的甘油三酯中单甘酯含量为0.88%,甘二酯含量为4.62%,酸价降至1.73 mgKOH/g。
【Abstract】 In this study, the basic raw material was prickly ash seed oil, prickly ash seed oil was generally dark in color, and had higher acid value, the text targeted for decolorizing the prickly ash seed oil pertinencily, then refining oil by the way of acid esterification, finally depickling with esterificating the oil post-processing necessarily, that refined results were better.In the study of discolor process, activated carbon combined with activated clay as a mixed-decolorizing agent, focused on four decolorizing factors,including of activated carbon accounting for the mixed-decolorizing agent , mixed-decolorizing agent dosage,decolorizing time, and decolorizing temperature. Combining single factor experiment and response surface optimization experiments , ultimately optimum decolorizing conditions were as follow∶activated carbon accounting for the mixed- decolorizing agent 15.5% ; mixed-decolorizing dosage 2% ; decolorizing time 22min ; decolorizing temperature 93℃, under the optimum conditions,the decolorizing rate was 79.71%.In the study of depickling with esterification process , by comparing five traditional esterification catalyst screening,the results showed that the catalyst ZnO was the best. Selected ZnO as a catalyst for esterification, we used the reaction time on esterification, esterification temperature, the dosage of ZnO, the addition of monoglyceride / glycerine (1∶1,w/w) as the single factor experiment for observation and analysis of orthogonal test. Through orthogonal test analysis of single factor experiments combined with the situation, considering the effect on oil color by reaction temperature on the esterification and economic applicability,finally determined the optimal reaction conditions were as follows∶reaction temperature 200℃, the dosage of ZnO 0.2%,monoglyceride / glycerine (1∶1,w/w) content 150% of the theoretical value, under this condition, the acid ester oil price was 3.57mgKOH / g, the yield of monoglyceride and diglyceride in the ester oil were 3.25% and 13.64% respectively.In the post-processing of oil esterification,mainly purified triglyceride by solvent extraction, extraction conditions were as follow∶extraction solvent 85% ethanol concentration; ethanol / mixed oil (w/w) percentage was0.8∶1; extraction temperature 40℃, finally the content of triglycerides in monoglyceride was 0.88%, the content of diglyceride was 4.62%, acid value dropped to 1.73 mgKOH / g.
【Key words】 prickly ash seed oil; decolor; depickling with esterification; menstruum distill;