【摘要】：硬脂酸高碳醇酯分子結構中同時含有一個酯基和異構長鏈烷基,凝固點低,可以用于聚氯乙烯的增塑劑,化妝品中的延展劑,高級潤滑油的添加劑,塑料加工潤滑劑,聚碳酸酯脫膜劑。因此,研究硬脂酸高碳醇酯的合成方法具有較高的理論和現(xiàn)實意義。本文以硬脂酸甲酯和異辛醇、2-己基-1-癸醇、2-辛基十二醇為原料,以二丁基氧化錫為催化劑,研究了酯交換合成硬脂酸高碳醇酯的反應規(guī)律。詳細考察了原料配比,催化劑用量、反應溫度等因素的影響,確定了酯交換反應的最佳反應條件:異辛醇、2-己基-1-癸醇、2-辛基十二醇與硬脂酸甲酯的醇酯摩爾比均為1.5,催化劑用量均為硬脂酸甲酯物質(zhì)量的1.14%,反應溫度分別為140℃,170℃,170℃,保護氮氣流速為30ml/min,相應三種高碳醇酯的收率分別為92.0%,91.5%,90.0%。 使用二丁基氧化錫催化酯交換制備硬脂酸異辛酯工藝中,探討了二丁基氧化錫的再生方法,結果表明,乙醇和水作為沉淀劑再生效果最佳,催化劑的回收率是82.5%,催化劑循環(huán)使用三次,催化活性基本保持不變。對反應前后的Bu_2SnO進行了FTIR和XRD表征,結果表明:用水和乙醇作沉淀劑沉淀出的催化劑大部分仍為Bu_2SnO。 本論文還探索使用其它催化劑催化該反應。例如用二丁基氧化錫與甲磺酸,對苯甲磺酸反應制備了兩種新的有機錫化合物—二丁基錫(Ⅳ)甲磺酸酯(Sn-ME),和二丁基錫(Ⅳ)對甲基苯磺酸酯(Sn-MBE),并利用紫外、紅外、核磁共振技術對其進行了表征,研究了他們對酯交換反應的催化活性。研究表明:在酯交換制備硬脂酸高碳醇酯的反應中,由于磺酸基的強吸電子效應增強了Sn-ME,Sn-MBE中的Sn的Lewis酸性,導致其催化活性比Bu_2SnO高,并且磺酸基上取代基的吸電子能力越強,催化劑中Sn的Lewis酸性越強,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，

本文編號：2130653