【作者】 曹建平；

【导师】 李浔；

【作者基本信息】 长沙理工大学 ， 有机化学， 2011， 硕士

【摘要】 生物柴油作为一种极有发展前景的生物质能源,越来越受到世界各国的关注,并得到了大力的发展。其副产物甘油的大量生成使得甘油的深度开发已成为人们重点研究的对象。本文制备了磁性固体碱催化剂用于合成生物柴油和甘油,研究了甘油制备环氧氯丙烷过程中催化剂的制备及反应条件的优化。制备了SO₄^2-/ZrO₂固体酸用于甘油与HCl的反应,制备二氯丙醇。将KF了附载于γ-Al₂O₃上制备出的KF/γ-Al₂O₃固体碱催化二氯丙醇的环化反应制备环氧氯丙烷也良好的实验结果。1.用Fe₃O₄作为磁基质与镁铝水滑石合成磁性固体碱。从镁与铝的物质的量,镁与铁（Ⅱ）物质的量,反应温度,反应时间,催化剂用量及醇油比对产物产率的影响,探索在无溶剂情况下磁性固体碱催化酯化反应的最佳反应条件,利用磁场将磁性固体碱与反应体系进行有效分离回收。2.用正交实验法优化了制备固体酸的条件。考察了反应时间、反应温度、催化剂寿命等因素对甘油氯化反应的影响.研究结果表明,最佳制备催化剂的条件为1.0mol/L硫酸浸渍,500℃下煅烧4h.以此条件制备的催化剂在130℃下,催化甘油氯化反应4h,产率可达到82.1%。固体酸催化剂可重复使用6次以上,且具有良好的再生性。3.制备了固体碱KF/γ-Al₂O₃制备环氧氯丙烷。考察了KF浸渍浓度、煅烧时间、煅烧温度对催化活性的影响。分析了环化反应的最佳制备条件。研究结果表明:KF负载量为20%,浸渍时间4 h,焙烧温度500℃此时获得的KF/γ-Al₂O₃的催化剂催化效果最好。于85℃下催化二氯丙醇环化反应4h,可获得81.2%的产率。更多还原

【Abstract】 As a promising biomass, biodiesel has attracted much attention allover the word and increased produced. Couple with the vigorous development of biodiesel industry, surplus glycerol immerges and deep exploration of this glycerol has been focused. In this paper, solid base nano-catalysts were prepared and used in the production of biodiesel, and the preparation of catalysts for conversion of glycerol into epichlorohydrin and optimizing of relative factors were investigated; SO₄^2-/ZrO₂ solid super acid were synthesized and evaluated in the production of dichlorohydrin from glycerol and HCl; solid base catalyst KF/γ-Al₂O₃ with KF loaded onγ-Al2O3 were tested in the Cyclization of dichloropropanol in order to Preparation of epichlorohydrin.1.Fe3O4 as magnetic matrix were combined with Mg-Al hydrotalcites to synthesize magnetic solid base catalyst. Effect of Mg/Al and Mg/Fe mole ratio, reaction temperature, reaction time, catalyst concentration, and alcohol/oil on the biodiesel yield was studied and the optimum reaction conditions of transesterification reaction over magnetic solid base without solvent were obtained. The catalyst could be effectively recycled in magnetic fields.2. Orthogonal experiment method was introduced to optimized the preparation condition of solid acid. Effect of reaction time, reaction temperature, lifetime of catalysts on the chlorination reaction of glycerol was investigated. The results revealed that after 4h of reaction time, a yield as high as 82.1% was achieved over the catalyst dipped by H₂SO₄ and calcined at 500℃for 4h, with 130℃of reaction temperature. The solid acid catalyst could be recycled more than 6 times, which indicated its good durability.3. Solid based catlyst KF/γ-Al₂O₃ was prepared and screened in the synthesis of dichlorohydrin. Factors including dosage of KF, calcination temperature and time were investigated. And the cyclization conditions were optimized. Obtained results showed that catalyst with a KF dosage of 20%,dipping time of 4h, and calcination of 500℃posses best activity. A yield of 81.2% was accomplished under the condition of 85℃of reaction temperature and 4h of reaction time.更多还原