棉籽油生物柴油制备的试验研究

【作者】 罗帅；

【导师】 王华； 包桂蓉；

【作者基本信息】 昆明理工大学 ， 化学工程， 2009， 硕士

【摘要】 作者利用棉籽油为原料,利用亚临界水-超临界甲醇两步法制备生物柴油.第一步棉籽油在亚临界水中制备出棉籽油脂肪酸,第二步利用制备得出的棉籽油脂肪酸在超临界甲醇中制备脂肪酸甲酯,即生物柴油.本文详细的研究了物料配比、反应温度、反应压力、反应时间各单因素对制备生物柴油的影响.通过对产物的酸值测定和UPLC(超高效液相色谱)检测.第一步水解反应中,结果表明该反应最适宜的操作条件为：油水体积比1：4,反应时间40min,反应温度290℃,在此条件下生物柴油的收率可达96.69%。通过进行动力学研究分析表明,棉籽油与水在亚临界状态下进行水解反应的平均反应级数为n=1.15,活化能Ea=108.63kJ/mol,频率因子A=2.696x109,动力学模型为：第二步酯化反应中,结果表明该反应最适宜的操作条件为：油水体积比1：3,反应时间30min,反应温度290℃,在此条件下生物柴油的收率可达98.89%。通过UPLC(超高效液相色谱)对产物检测,分析了各影响因素对脂肪酸及脂肪酸甲酯含量的影响。结果表明：(1)不饱和脂肪酸甲酯如油酸甲酯(18：1),以及多聚不饱和脂肪酸甲酯如亚油酸甲酯(18：2)在280℃超临界甲醇下相对含量开始降低了。过高的温度使脂肪酸甲酯产生变化。(2)甲醇的过多的加入并不能使得产物脂肪酸甲酯的量也随着增加。一般在脂肪酸与甲醇体积比1：3为适宜。(3)反应时间的过多增长并不能提高其脂肪酸甲酯的量,因为生产出的脂肪酸甲酯会产生其他副反应。更多还原

【Abstract】 Author use cottonseed oil as raw material to make the biodiesel in the sub-critical water and supercritical methanol. Cottonseed oil in the sub-critical first step in the preparation of cottonseed oil fatty acid in the water, and the second step the use of cottonseed oil fatty acid preparation derived from Supercritical Methanol in the preparation of fatty acid methyl ester, or biodiesel. Cottonseed oil fatty acid is made by cottonseed oil and water in the sub-critical first step,fatty acid methyl ester is made by cottonseed oil fatty acid and methanol in the Supercritical Methanol. In this paper, a detailed study on the single factor of material ratio, reaction temperature, reaction pressure and reaction time impacting in the preparation of biodiesel. The acid value and UPLC testing of the product of measured. The product are measured by the acid value of the product of measured and UPLC testing.The best conditions that the cottonseed oil hydrolysis in sub-critical water is temperature 290℃, oil-water volume ratio 1:4, reaction time 40min, which yields 96.69% of fatty acids. Reaction kinetics analysis shows that the reaction order of hydrolysis reaction is 1.15; activation energy is 108.63kJ/mol, and kinetics equation the most appropriate conditions of esterification are reaction temperature 290℃, reaction time 30min, volume ratio of to methanol 1:3. With the conditions of the test, the yields of fatty acids methyl ester is 98.89%. The adoption of UPLC of tine product testing, analysis of the impact of factors on the fatty acid and fatty acid methyl ester content. The results show that:Unsaturated fatty acid methyl ester such as methyl oleate (18:1), and poly-unsaturated fatty acid methyl esters such as linoleic acid methyl ester (18:2) at 280℃under supercritical methanol relative content began to lower.fatty acid methyl ester changes in high temperature. Fatty acid methyl ester can not increase by adding excess methanol. General fatty acid and methanol in volume ratio 1:3 is Suitable. The excessive reaction time growth can not increase the fatty acid methyl ester, because the production of fatty acid methyl ester will have other side effects.更多还原