酯交换法制备硬脂酸高碳醇酯的研究

发布时间：2018-07-17 19:10

【摘要】：硬脂酸高碳醇酯分子结构中同时含有一个酯基和异构长链烷基,凝固点低,可以用于聚氯乙烯的增塑剂,化妆品中的延展剂,高级润滑油的添加剂,塑料加工润滑剂,聚碳酸酯脱膜剂。因此,研究硬脂酸高碳醇酯的合成方法具有较高的理论和现实意义。本文以硬脂酸甲酯和异辛醇、2-己基-1-癸醇、2-辛基十二醇为原料,以二丁基氧化锡为催化剂,研究了酯交换合成硬脂酸高碳醇酯的反应规律。详细考察了原料配比,催化剂用量、反应温度等因素的影响,确定了酯交换反应的最佳反应条件:异辛醇、2-己基-1-癸醇、2-辛基十二醇与硬脂酸甲酯的醇酯摩尔比均为1.5,催化剂用量均为硬脂酸甲酯物质量的1.14%,反应温度分别为140℃,170℃,170℃,保护氮气流速为30ml/min,相应三种高碳醇酯的收率分别为92.0%,91.5%,90.0%。 使用二丁基氧化锡催化酯交换制备硬脂酸异辛酯工艺中,探讨了二丁基氧化锡的再生方法,结果表明,乙醇和水作为沉淀剂再生效果最佳,催化剂的回收率是82.5%,催化剂循环使用三次,催化活性基本保持不变。对反应前后的Bu_2SnO进行了FTIR和XRD表征,结果表明:用水和乙醇作沉淀剂沉淀出的催化剂大部分仍为Bu_2SnO。 本论文还探索使用其它催化剂催化该反应。例如用二丁基氧化锡与甲磺酸,对苯甲磺酸反应制备了两种新的有机锡化合物—二丁基锡(Ⅳ)甲磺酸酯(Sn-ME),和二丁基锡(Ⅳ)对甲基苯磺酸酯(Sn-MBE),并利用紫外、红外、核磁共振技术对其进行了表征,研究了他们对酯交换反应的催化活性。研究表明:在酯交换制备硬脂酸高碳醇酯的反应中,由于磺酸基的强吸电子效应增强了Sn-ME,Sn-MBE中的Sn的Lewis酸性,导致其催化活性比Bu_2SnO高,并且磺酸基上取代基的吸电子能力越强,催化剂中Sn的Lewis酸性越强,其催化活性也就越高。
[Abstract]:The molecular structure of stearic acid high carbon alcohol ester contains one ester group and isomerization long chain alkyl, low freezing point. It can be used as plasticizer for PVC, extender for cosmetics, additive for high grade lubricating oil, plastic processing lubricant. Polycarbonate debonding agent. Therefore, it is of great theoretical and practical significance to study the synthetic method of stearic acid high carbon alcohol ester. The synthesis of high carbon alcohol stearate by transesterification was studied using methyl stearate and isooctyl 2-hexyl -1-decyl alcohol as raw materials and two Ding Ji tin oxide as catalyst. The effects of the ratio of raw materials, the amount of catalyst and the reaction temperature were investigated in detail. The optimum reaction conditions for transesterification were determined as follows: the molar ratio of isooctanol 2-hexyl-1-decanol 2-octyl dodecanol to methyl stearate was 1.5, the amount of catalyst was 1.14% of the mass of methyl stearate, and the reaction temperature was 140 鈩，

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