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以自制三羟甲基己烷为原料 ,采用自制的负载磷钨酸催化剂催化合成一系列三羟甲基己烷脂肪酸酯。通过大量实验研究了影响催化剂活性和酯化率的因素 ,筛选出最佳催化剂并确定了适宜的酯化工艺条件。最佳催化剂制备条件 :载体与活性物质量比 1/ 6 ,浸渍时间 5h ,烘焙温度 32 0℃。适宜的酯化工艺条件 :反应时间 12 0min ,反应温度2 2 0℃ ,压力 0 0 2～ 0 0 4MPa,催化剂质量分数 1 8%,庚酸 /三羟甲基己烷摩尔比 3 7/ 1 0。在此条件下酯化率可达96 0 %以上 ,而且催化剂可重复使用。通过质量检测及光谱分析 ,对目标产物进行了确证。
A series of trimethylolhexane fatty acid esters were synthesized by using self-made trimethylolpropane as catalyst. Through a large number of experiments to study the factors that affect the catalyst activity and esterification rate, screening out the best catalyst and determine the appropriate esterification process conditions. The best catalyst preparation conditions: the ratio of carrier to active material 1/6, immersion time 5h, baking temperature 32 0 ℃. The suitable esterification conditions were as follows: reaction time 12 0min, reaction temperature 220 ℃, pressure 0 0 2 ~ 0 0 4MPa, catalyst mass fraction 1 8%, heptanoic acid / trimethylolpropane molar ratio 3 7/1 0. In this condition, the esterification rate can reach more than 96 0%, and the catalyst can be reused. Through the quality inspection and spectral analysis, the target product was confirmed.