论文部分内容阅读
以甘油和苯甲醛为原料,对甲苯磺酸为催化剂,制备了甘油苯甲醛缩醛,产物分为2种:4-羟甲基-2-苯基-1,3-二氧戊环(五元环)和2-苯基-1,3-二氧六环-5-醇(六元环)。分别研究了原料摩尔比、带水剂用量、催化剂用量及反应时间对反应的影响。结果表明,在n(甘油)∶n(苯甲醛)=1.2∶1,带水剂体积为15 m L,催化剂质量为0.15 g,反应时间为4 h的较优反应条件下,得到了缩醛产物最大收率为97%(以苯甲醛计)。利用气相色谱(GC)、气相色谱-质谱联用仪(GC-MS)、核磁共振氢谱(1H-NMR)对目标产物进行了定量和定性分析。
Glycerol benzaldehyde acetal was prepared by using glycerol and benzaldehyde as raw materials and p-toluenesulfonic acid as catalyst. The product was divided into two kinds: 4-hydroxymethyl-2-phenyl-1,3-dioxolane Membered ring) and 2-phenyl-1,3-dioxan-5-ol (six membered ring). The effects of molar ratio of raw materials, amount of water-carrying agent, amount of catalyst and reaction time on the reaction were studied respectively. The results showed that under the optimal reaction conditions of n (glycerol): n (benzaldehyde) = 1.2:1, water-entraining agent volume 15 m L, catalyst mass 0.15 g and reaction time 4 h, The maximum yield of the product was 97% (based on benzaldehyde). The target products were quantitatively and qualitatively analyzed by gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (1H-NMR).